vvEPA
   United States
   Environmental Protection
   Agency
  Method A: Enterococci in Water by
  TaqMan® Quantitative Polymerase Chain
  Reaction (qPCR) Assay


  April 2010
  Note that this method will be updated following it's validation in marine
  and fresh ambient waters.

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U.S. Environmental Protection Agency
      Office of Water (4303T)
   1200 Pennsylvania Avenue, NW
      Washington, DC 20460
        EPA-821-R-10-004

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                                 Acknowledgments

This method was developed under the direction of Rich Haugland, Kevin Oshima and Alfred P. Dufour of
the U.S. Environmental Protection Agency's (EPA) Human Exposure Research Division, National
Exposure Research Laboratory, Cincinnati, Ohio.

The following laboratories are gratefully acknowledged for their participation in the single laboratory
validation of this method in fresh and marine waters:

Participant Laboratories

•  New York State Department of Health, Environmental Biology Laboratory: Ellen Braun-Howland
   and Stacey Chmura

•  Mycometrics, LLC: King-Teh Lin and Pi-shiang Lai

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                                        Disclaimer

Neither the United States Government nor any of its employees, contractors, or their employees make any
warranty, expressed or implied, or assumes any legal liability or responsibility for any third party's use of
apparatus, product, or process discussed in this method, or represents that its use by such party would not
infringe on privately owned rights.  Mention of trade names or commercial products does not constitute
endorsement or recommendation for use.

Questions concerning this method or its application should be addressed to:

    Robin K. Oshiro
    Engineering and Analysis Division (4303T)
    U.S. EPA Office of Water, Office of Science and Technology
    1200 Pennsylvania Avenue, NW
    Washington, DC 20460
    oshiro.robin@epa.gov or OSTCWAMethods@epa.gov
                                              IV

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                                       Introduction

Enterococci are commonly found in the feces of humans and other warm-blooded animals. Although
these organisms can be persistent in the environment, the presence of enterococci in water is an indication
of fecal pollution and the possible presence of enteric pathogens. Epidemiological studies have led to the
development of criteria for promulgating recreational water standards based on established relationships
between the measured density of enterococci colony forming units (CPU) in the water by culture based
methods and the risk of gastrointestinal illness (GI) associated with swimming in the water (References
17.3, 17.6,  17.7, and 17.8).

Method A describes a quantitative polymerase chain reaction (qPCR) procedure for the detection of DNA
from enterococci bacteria in ambient water matrices based on the amplification and detection of a specific
region of the large subunit ribosomal RNA gene (IsrRNA, 23S rRNA) from these organisms. The
advantage of this method over currently accepted culture methods that require 24-48 hr to obtain results is
its relative rapidity. Results can be obtained by this method in 3-4 hr, allowing same-day notifications of
recreational water quality. While measurements of enterococci DNA by Method  A and  enterococci CPU's
by culture methods such as EPA Method 1600 are performed for essentially the same purpose, i.e., to
indicate fecal pollution, the results of these two approaches may not always be correlated with each other
due to potential differences in the ratios of viable  and non-viable bacteria in different water environments.
Never-the-less, more recent epidemiological studies conducted at freshwater recreational beaches
(Reference 17.3) have demonstrated similar or improved positive correlations between enterococci DNA
measurements  by this method and swimming-associated GI illness rates compared with those established
for enterococci CPU measurements.

In Method A, water samples are filtered to collect enterococci on membranes. Following filtration, total
DNA is solubilized from the retentate using a bead beater. Enterococci target DNA sequences present in
the clarified homogenate are detected by the  real time polymerase chain reaction technique using
TaqMan® Universal Master Mix PCR reagent and the TaqMan® probe system.  The TaqMan® system
signals the formation of PCR products by a process involving enzymatic hydrolysis of a fluorogenically-
labeled oligonucleotide probe when it hybridizes to the target sequence.

Method A uses an arithmetic formula, the comparative  cycle threshold (CT) method, to calculate the ratio
of Enterococcus IsrRNA gene target sequences (target sequences) recovered in total DNA extracts from
water samples  relative to those in similarly-prepared extracts of calibrator samples containing a known
quantity of Enterococcus cells.  Mean estimates of the absolute quantities of target sequences in the
calibrator sample extracts are then used to  determine the absolute quantities of target sequences in the
water samples.  CT values for sample processing control (SPC) sequences added in equal quantities to
both the water  filtrate and calibrator samples before DNA extraction are used to normalize results for
potential differences in DNA recovery or to signal inhibition or fluorescence quenching of the PCR
analysis caused by a sample matrix component or possible technical error.

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                                  Table of Contents




1.0    Scope and Application	1




2.0    Summary of Method	1




3.0    Definitions	1




4.0    Interferences	2




5.0    Safety	3




6.0    Equipment and Supplies	3




7.0    Reagents and Standards	5




8.0    Sample Collection, Handling, and Storage	8




9.0    Quality Control	9




10.0   Calibration and Standardization of Method-Related Instruments	11




11.0   Procedure	11




12.0   Data Analysis and Calculations	20




13.0   Sample Spiking Procedure	23




14.0   Method Performance	23




15.0   Pollution Prevention	24




16.0   Waste Management	24



17.0   References	25




18.0   Acronyms
                                             VI

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                              List of Appendices



Appendix A:   ABI 7900 and ABI 7500 Sequence Detector Operation



Appendix B:   Cepheid Smart Cycler® Operation
                                        vi i

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   Method A:  Enterococci in Water by Quantitative Polymerase  Chain
                              Reaction (qPCR) Assay


                                       April  2010

1.0   Scope and Application

1.1    Method A describes a quantitative polymerase chain reaction (qPCR) procedure for the
       measurement of large subunit ribosomal RNA (IsrRNA, 23 S rRNA) gene sequences (target
       sequences) from all known species of enterococci bacteria in water. This method is based on the
       collection of enterococci on membrane filters, extraction of total DNA using a bead beater, and
       detection of enterococci target sequences in the supernatant by real time polymerase chain
       reaction using TaqMan® Universal Master Mix PCR reagent and the TaqMan® probe system.
       The TaqMan® system signals the formation of PCR products by a process involving the
       enzymatic hydrolysis of a labeled fluorogenic probe that hybridizes to the target sequence.

1.2    Enterococci are commonly found in the feces of humans and other warm-blooded animals.
       Although DNA from these organisms can be persistent in the environment, its presence in water
       is an indication of fecal pollution and the possible presence of enteric pathogens.

1.3    The Method A test is recommended as  a measure of ambient fresh and marine recreational water
       quality. Epidemiological studies have been conducted at freshwater and marine water beaches
       has been conducted that may lead to the potential development of criteria that can be used to
       promulgate recreational water standards based on established relationships between health effects
       and water quality measurements by this method. The significance of finding Enterococcus DNA
       target sequences in recreational water samples stems from the direct relationship between the
       density of these sequences and the risk of gastrointestinal illness associated with swimming in the
       water that have been observed thus far  in the epidemiological studies (Reference and 17.9).

1.4    This method assumes the use of an ABI Sequence Detector as the  default platform. The Cepheid
       Smart Cycler® may also be used. The  user should refer to the platform specific instructions for
       these instruments in the Appendices. Users should thoroughly read the method in its entirety
       before preparation of reagents and commencement of the method to identify differences in
       protocols for different platforms.

2.0   Summary of Method

       The method is initiated by filtering a water sample through a membrane filter. Following
       filtration, the membrane containing the bacterial cells and DNA is placed in a microcentrifuge
       tube with glass beads and buffer, and then agitated to extract the DNA into solution. The
       supernatant is used for PCR amplification and detection of target sequences using the  TaqMan®
       Universal Master Mix PCR reagent and probe system.

3.0   Definitions

3.1    Enterococci: all species of the genus Enterococcus for which IsrRNA gene nucleotide  sequences
       were reported in the GenBank database (http://www.ncbi.nlm.nih/gov/Genbank) at the time of
       method development.

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                                                                                      Method A
3.2    Target sequence: A segment of the Enterococcus IsrRNA gene containing nucleotide sequences
       that are homologous to both the primers and probe used in the Enterococcus qPCR assay and that
       are common only to species within this genus.

3.3    Sample processing control (SPC) sequence (may also be referred to as reference sequence): A
       segment of the ribosomal RNA gene operon, internal transcribed spacer region 2 of chum salmon,
       Oncorhynchus keta, containing nucleotide sequences that are homologous to the primers and
       probe used in the SPC qPCR assay. SPC sequences are added as part of a total salmon DNA
       solution in equal quantities to all water sample filtrate and calibrator samples prior to extracting
       DNA from the samples.

3.4    DNA standard: A purified, RNA-free and  spectrophotometrically quantified and characterized E.
       faecalis strain ATCC #29212 genomic DNA preparation. Used to generate standard curves for
       determination of performance characteristics of the qPCR assays and instrument with different
       preparations of master mixes containing TaqMan® reagent, primers and probe as described in
       Section 9.6. Also used for quantifying target sequences in calibrator sample extracts as described
       in Section 12.2.

3.5    Calibrator sample: Samples containing constant added quantities of E. faecalis strain ATCC
       #29212 cells and SPC sequences that are extracted and analyzed in the same manner as water
       sample filtrates. Calibrator sample analysis results are used as positive controls for the
       Enterococcus target sequence and SPC qPCR assays and as the basis for target sequence
       quantification in water sample filtrates using the AACT comparative cycle  threshold calculation
       method as described in Section 12.4. Analysis results of these samples provide corrections for
       potential daily or weekly method-related variations in Enterococcus cell lysis, target sequence
       recovery and PCR efficiency. QPCR analyses for SPC sequences from these samples are also
       used to correct for variations in total DNA recovery in the extracts of water sample filtrates that
       can be caused by contaminants in these filtrates as described in Section 12.4 and/or to signal
       potentially significant PCR inhibition  caused by these contaminants as described in Section 9.8.

3.6    AACT comparative cycle threshold calculation method (AACT method): A calculation method
       derived by Applied Biosy stems (Reference 17.1) for calculating the ratios of target sequences in
       two DNA samples  (e.g., a calibrator and water filtrate sample) that normalizes for differences in
       total DNA recovery from these samples using qPCR analysis CT values for a reference (SPC)
       sequence that is initially present in equal quantities prior to DNA extraction.

3.7    Amplification factor (AF): A measure of the average efficiency at which target or SPC sequences
       are copied and detected by their respective primer and probe assays during each thermal cycle of
       the qPCR reaction that is used in the comparative cycle threshold calculation methods. AF values
       can range from 1 (0 % of sequences copied and detected) to 2 (100 % of sequences copied and
       detected) and are calculated from a standard curve as described in Section 12.2.

4.0   Interferences

       Water samples containing colloidal  or suspended particulate materials can clog the membrane
       filter and prevent filtration. These materials can also interfere with DNA recovery and with the
       PCR analysis by inhibiting the enzymatic activity of the Taq DNA polymerase, and/or inhibiting
       the annealing of the primer and probe  oligonucleotides to sample target DNA, enzyme or
       quenching of hydrolyzed probe fluorescence.

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                                                                                       Method A
5.0   Safety

5.1    The analyst / technician must know and observe the normal safety procedures required in a
       microbiology and/or molecular biology laboratory while preparing, using, and disposing of
       cultures, reagents, and materials, and while operating sterilization equipment.
5.2    Where possible, facial masks should be worn to prevent sample contamination.
5.3    Mouth-pipetting is prohibited.


6.0   Equipment and Supplies


6.1    Separated, and dedicated workstations for reagent preparation and for sample preparation,
       preferably with HEPA-filtered laminar flow hoods and an Ultraviolet (UV) light source, each
       having separate supplies (e.g., pipettors, tips, gloves, etc.). Note: The same workstation may be
       used for the entire procedure provided that it has been cleaned with bleach and UV sterilized as
       specified in section 11.6.1 between reagent and sample preparation.  Under ideal conditions, two
       dedicated workstations are used for sample preparation: one for preparing samples with high
       target sequence DNA concentrations (e.g., DNA standards and calibrator samples) and one for
       preparing samples with expected low target sequence DNA concentrations (e.g., filter blanks and
       ambient water samples).
6.2    Balance capable of accuracy to 0.01 g
6.3    Extraction tubes: semi-conical,  screw cap microcentrifuge tubes, 2.0-mL (e.g., PGC 506-636 or
       equivalent)
6.4    Glass beads, acid washed, 212 - 300 um (e.g., Sigma G-1277 or equivalent)

6.5    Autoclave, capable of achieving and maintaining 121°C [15 Ib pressure per square inch (PSI)] for
       minimally 15 minutes  (optional)
6.6    Workstation for water filtrations, preferably a HEPA-filtered laminar flow hood with a UV light
       source.  This can be the same as used for sample preparation, Section 6.1.
6.7    Sterile bottles/containers for sample collection
6.8    Membrane filtration units (filter base and funnel) for 47 mm diameter filters, sterile glass, plastic
       (e.g. Pall Gelman 4242, or equivalent), stainless steel, or disposable plastic (e.g., Nalgene CN
       130-4045 or CN 145-0045, or equivalent); cleaned and bleach treated (rinsed with 10% v/v
       bleach, then 3 rinses with reagent-grade water), covered with aluminum foil or Kraft paper, and
       autoclaved or UV-sterilized if non-disposable
6.9    Line vacuum, electric vacuum pump, or aspirator for use as a vacuum source.  In an emergency or
       in the field, a hand pump or a syringe equipped with a check valve to prevent the return flow of
       air can be used.
6.10   Flask, filter, vacuum, usually 1  L, with appropriate tubing
6.11   Filter manifold to hold a number of filter bases
6.12   Flask for safety trap placed between the filter flask and the vacuum source
6.13   Forceps, straight or curved, with smooth tips to handle filters without damage, 2 pairs
6.14   Polycarbonate membrane filters, sterile, white, 47 mm diameter, with 0.45 /u,m pore size
       (e.g., GE Osmotics Inc. 04CP04700 or equivalent)

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                                                                                       Method A
6.15   Graduated cylinders, 100-1000-mL, cleaned and bleach treated (rinsed with 10% v/v bleach, then
       3 rinses with reagent-grade water), covered with aluminum foil or Kraft paper and autoclaved or
       UV-sterilized
6.16   Petri dishes, sterile, plastic or glass, 100 x 15 mm with loose fitting lids
6.17   Disposable loops, 1 and 10 uL
6.18   Permanent ink marking pen for labeling tubes
6.19   Visible wavelength spectrophotometer capable of measuring at 595 nm
6.20   Single or 8-place mini bead beater (e.g., Biospec Products Inc. #3110BX or equivalent).
6.21   Microcentrifuge capable of 12,000 x g
6.22   Micropipettors with 10, 20, 200 and 1000 uL capacity.  Under ideal conditions, each workstation
       should have a dedicated set of micropipettors (one micropipettor set for pipetting reagents not
       containing cells or reference DNA and one  set for reagents containing reference DNA and for test
       samples).
6.23   Micropipettor tips with aerosol barrier for 10, 20, 200 and 1000 uL capacity micropipettors.
       Note: All micropipetting should be done with aerosol barrier tips. The tips used for reagents not
       containing DNA should be separate from those used for reagents containing DNA  and test
       samples. Each workstation should have a dedicated supply of tips.
6.24   Microcentrifuge tubes, low retention, clear, 1.7-mL (e.g., GENE MATE C-3228-1 or equivalent)
6.25   Test tube rack for microcentrifuge tubes, use a separate rack for each set of tubes
6.26   Conical centrifuge tubes, sterile, screw cap, 50-mL
6.27   Test tubes, screw cap, borosilicate glass,  16 x 125 mm
6.28   Pipet containers, stainless steel, aluminum or borosilicate glass, for glass pipets
6.29   Pipets, sterile, T.D. bacteriological or Mohr, disposable glass or plastic, of appropriate volume
       (disposable pipets preferable)
6.30   Vortex mixer (ideally one for each work station)
6.31   Dedicated lab coats for each work station
6.32   Disposable powder-free gloves for each work station
6.33   Refrigerator, 4°C (ideally one for reagents and one for DNA samples)
6.34   Freezer, -20°C or -80°C (ideally one for reagents and one for DNA samples)
6.35   Ice, crushed or cubes for temporary preservation of samples and reagents
6.36   Printer (optional)
6.37   Data archiving system (e.g., flash drive or other data storage system)
6.38   UV spectrophotometer capable of measuring wavelengths of 260 and 280 nm using small volume
       capacity (e.g., 0.1-mL) cuvettes or NanoDrop® (ND-1000) spectrophotometer (or equivalent)
       capable of the same measurements at 2 uL sample volumes
6.39   ABI 7900 Sequence Detector
       6.39.1  Optical 96 well PCR reaction tray (e.g., Applied Biosystems N801-0560 or equivalent)
       6.39.2 Optical adhesive PCR reaction tray tape (e.g., Applied Biosystems 4311971 or
               equivalent) or MicroAmp™ caps (e.g., Applied Biosystems N8010534 or  equivalent)

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                                                                                     Method A
       6.39.3 ABI 7900 sequence detector
6.40   Cepheid Smart Cycler® (optional to ABI)
       6.40.1 Smart Cycler® 25 uL PCR reaction tubes (e.g., Cepheid 900-0085 or equivalent)
       6.40.2 Rack and microcentriruge for Smart Cycler® PCR reaction tubes.  Note: Racks and
              microcentrifuge are provided with the Smart Cycler® thermocycler
       6.40.3 Cepheid Smart Cycler® System Thermocycler

7.0   Reagents  and Standards
       Note: The E. faecalls stock culture (Section 7.8), Salmon DNA/extraction buffer (Section 7.12),
       and DNA extraction tubes (Section 7.18), may be prepared in advance.
7.1    Purity of Reagents:  Molecular grade reagents and chemicals shall be used in all tests
7.2    Control Culture
       •   Enterococcus faecalis (E. faecalis} ATCC #29212
7.3    Sample Processing Control (SPC) DNA (source of SPC control sequences)
           Salmon testes DNA (e.g., Sigma D1626 or equivalent)
7.4    Phosphate Buffered Saline (PBS)
       7.4.1  Composition:
                Monosodium phosphate (NaH2PO4)             0.58 g
                Disodium phosphate (Na2HPO4)               2.50 g
                Sodium chloride                             8.50 g
                Reagent-grade water                          1.0   L
       7.4.2  Dissolve reagents in 1 L of reagent-grade water in a flask and dispense in appropriate
              amounts for dilutions in screw  cap bottles or culture tubes, and/or into containers for use
              as rinse water. Autoclave after preparation at!21°C[151b pressure per square inch
              (PSI)] for 15 minutes. Final pH should be 7.4 ± 0.2.
7.5    Brain heart infusion broth (BHIB)
       7.5.1  Composition:
                Calf brains, infusion from 200.0 g              7.7  g
                Beef heart, infusion from 250.0 g               9.8  g
                Proteose peptone                            10.0 g
                Sodium chloride                             5.0  g
                Disodium phosphate (Na2HPO4)               2.5  g
                Dextrose                                    2.0  g
                Reagent-grade water                          1.0  L
       7.5.2  Add reagents to 1 L of reagent-grade water, mix thoroughly, and heat to dissolve
              completely. Dispense 10 mL volumes in screw cap 16  x  125 mm tubes and autoclave at
              121°C  (15 PSI) for 15 minutes. Final pH should be 7.4 ± 0.2.

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                                                                                       Method A
7.6    Brain heart infusion agar (BHIA)
       7.6.1   Composition:
               BHI agar contains the same components as BHIB with the addition of 15.0 g agar per
               liter of BHI broth.
       7.6.2   Add agar to formula for BHIB provided above.  Prepare as in Section 7.5.2. After
               sterilization, dispense 12-15 mL into 100 x 15 mm petri dishes. Final pH should be 7.4 ±
               0.2.
7.7    Sterile glycerol (used for preparation of E. faecalis stock culture as described in section 7.8)
7.8    Preparation of E. faecalis (ATCC #29212) stock culture
       Rehydrate lyophilized E. faecalis per manufacturer's instructions (for ATCC stocks, suspend in
       5-6 mL of sterile BHIB and incubate at 37 °C for 24 hours).  Centrifuge to create pellet.  Using a
       sterile pipet, discard supernatant. Resuspend pellet in 10 mL of fresh sterile BHI broth containing
       15% glycerol and dispense in  1.5-mL aliquots in microcentrifuge tubes. Freeze at -20°C (short
       term storage) or -80°C (long term storage).  Note: Aliquots of suspension may be plated to
       determine CPU concentration as described in section 11.1. Note: It is advisable to verify the E.
       faecalis culture as described, for example, in Section 15 of EPA Method 1600.
7.9    PCR grade water (e.g., OmniPur water from VWR EM-9610 or equivalent). Water must be
       DNA/DNase free.
7.10   Isopropanol or ethanol, 95%, for flame-sterilization
7.11   AE Buffer, pH 9.0 (e.g., Qiagen 19077 or equivalent) (Note: pH 8.0 is acceptable)
       Composition:
       lOmMTris-Cl
       0.5 mM EDTA (Ethylenediaminetetraacetic acid)
7.12   Salmon DNA/extraction buffer
       7.12.1  Composition:
               Stock Salmon testes DNA (10 ug/mL) (Section 7.3)
               AE Buffer (Section 7.11)
       7.12.2  Preparation of stock Salmon testes DNA: Each bottle of Salmon DNA contains a
               differing number of units.  Note the units.  Add an equal volume of PCR grade water to
               dissolve the Salmon testes DNA, and stir, using a magnetic stir bar at low to medium
               speed, until dissolved (2-4 hours if necessary).  The solution at this point will be
               equivalent to 50 ug Salmon testes DNA/mL. Dilute using PCR grade water to a
               concentration of ~ 10  ug/mL. Determine concentration of Salmon testes DNA stock by
               OD26o reading in a spectrophotometer.  An OD26o of 1 is approximately equal to 50
               ug/mL (one Unit). This is your Salmon testes DNA stock solution. Unused portion may
               be  aliquoted and frozen at -20°C.
               Note: For example, if the bottle contains 250 mg of DNA, using sterilized scissors and
               sterilized forceps, cut a piece of DNA to weigh approximately 20 mg (approximately 304
               Units), and place in a sterile weigh boat. After weighing, place the DNA into a sterile 50
               mL tube and add 20 mL PCR grade water.  Cap tightly, and resuspend by 2-4  hours of
               gentle rocking. The concentration should be about 1 mg/mL. Remove three,  10 uL
               aliquots and dilute each to 1 mL with PCR grade water. Check absorbance (OD260) and
               calculate DNA using the assumption 1 Unit DNA is  equal to 1 OD26o, which is then

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                                                                                  Method A
              equivalent to 50 ug/mL DNA. Adjust this stock to 10 ug/mL based on calculated initial
              concentration of 1 mg/mL by diluting with PCR grade water. Aliquot portions of the
              adjusted DNA stock and freeze.
       7.12.3 Dilute Salmon testes DNA stock with AE buffer to make 0.2 ug/mL Salmon
              DNA/extraction buffer. Extraction buffer may be prepared in advance and stored at 4°C
              for a maximum of 1 week.
              Note: Determine the total volume of Salmon DNA/extraction buffer required for each day
              or week by multiplying volume (600 uL) x total number of samples to be analyzed
              including controls, water  samples, and calibrator samples.  For example, for 18 samples,
              prepare enough Salmon/DNA extraction buffer for 24 extraction tubes (18^-6 = 3,
              therefore, 3 extra tubes for water sample filtration blanks (method blanks) and 3 extra
              tubes for calibrator samples). Note that the number of samples is divided by 6 because
              you should conduct one method blank for every 6 samples analyzed.  Additionally,
              prepare excess volume to allow for accurate dispensing of 600 uL per tube, generally 1
              extra tube.  Thus, in this example, prepare sufficient Salmon/DNA extraction buffer for
              24 tubes plus one extra. The total volume needed is 600 uL x 25 tubes = 15,000 uL.
              Dilute the Salmon testes DNA working stock 1:50, for atotal volume needed (15,000 uL)
              + 50 = 300  uL of 10 ug/mL Salmon testes DNA working stock.  The AE buffer needed is
              the difference between the total volume and the Salmon testes DNA working stock. For
              this example, 15,000 uL - 300 uL = 14,700 uL AE buffer needed.
7.13   Bleach solution: 10% v/v bleach (or other reagent that hydrolyzes DNA) (used for cleaning work
       surfaces)
7.14   Sterile water (used as rinse water  for work surface after bleaching)
7.15   TaqMan® Universal PCR Master Mix (e.g., Applied Biosystems 4304437 or equivalent)
       Composition:
       AmpliTaq Gold® DNA Polymerase
       AmpErase® UNG
       dNTPs with dUTP
       Passive Reference 1 (ROX™ fluorescent dye)
       Optimized buffer components (KC1, Tris, EDTA, MgCl2)
7.16   Bovine serum albumin (BSA), fraction V powder (e.g., Sigma B-4287 or equivalent)
       Dissolve in PCR grade water a concentration of 2 mg/mL.
7.17   Primer and probe sets: Primer and probe sets may be purchased from commercial sources.
       Primers should be desalted, probes should be HPLC purified.
       7.17.1  Enterococcus primer and  probe set (Reference 17.5):
              Forward primer: 5'-GAGAAATTCCAAACGAACTTG
              Reverse primer: 5'-CAGTGCTCTACCTCCATCATT
              TaqMan® probe: 5'-FAM-TGGTTCTCTCCGAAATAGCTTTAGGGCTA-TAMRA
       7.17.2 Salmon DNA primer and probe set (Reference 17.4):
              Forward primer: 5'-GGTTTCCGCAGCTGGG
              Reverse primer (Sketa 22): 5'-CCGAGCCGTCCTGGTC

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                                                                                    Method A


              TaqMan® probe: 5'-FAM-AGTCGCAGGCGGCCACCGT-TAMRA
       7.1 7.3 Preparation of primer/probes: Using a micropipettor with aerosol barrier tips, add PCR
              grade water to the lyophilized primers and probe from the vendor to create stock
              solutions of 500 uM primer and 100 uM probe and dissolve by extensive vortexing.
              Pulse centrifuge to coalesce droplets.  Store stock solutions at -20°C.
7.18   DNA extraction tubes

       Note: It is recommended that tube preparation be performed in advance of water sampling and
       DNA extraction procedures.
       Prepare 1 tube for each sample, and 1 extra tube for every 6 samples (i.e., for method blank) and
       minimum of 3 tubes per week for calibrator samples. Weigh 0.3 ± 0.01 g of glass beads (Section
       6.4) and pour into extraction tube.  Seal the tube tightly, checking to make sure there are no beads
       on the O-ring of the tube. Check the tube for proper O-ring seating after the tube has been closed.
       Autoclave tubes at 121°C (15 PSI) for 15 minutes.
7.19   Purified, RNA-free quantified and characterized E. faecalis genomic DNA preparations for use as
       standards used to generate a standard curve (see Section 1 1.2).
7.20   RNase A (e.g. , Sigma Chemical #R-65 13) or equivalent
       7.20.1 Composition:
              RNase A

              Tris-Cl
              NaCl
       7.20.2 Dissolve 10 mg/mL pancreatic RNase A in  10 mM Tris-Cl (pH 7.5), 15 mM NaCl. Heat
              to 100°C for 15 min.  Allow to cool to room temperature. Dispense into aliquots and
              store at - 20°C.  For working solution, prepare solution in PCR grade water at
              concentration of 5
7.21   DNA extraction kit (Gene-Rite #K102-02C-50 DNA-EZ® RW02 or equivalent)


8.0   Sample Collection, Handling, and Storage

8.1    Sampling procedures are briefly described below. Adherence to sample preservation procedures
       and holding time limits is critical to the production of valid data. Samples not collected
       according to these procedures should not be analyzed.
8.2    Sampling Techniques
       Samples are collected by hand or with a sampling device if the sampling site has difficult access
       such as a dock, bridge or bank adjacent to a surface water.  Composite samples should not be
       collected, since such samples do not display the range of values found in individual samples. The
       sampling depth for surface water samples should be 6-12 inches below the water surface.  Sample
       containers should be positioned such that the mouth of the  container is pointed away from the
       sampler or sample point.  After removal of the container from the water, a small portion of the
       sample should be discarded to provide head space for proper mixing before analyses.
8.3    Storage Temperature and Handling Conditions
       Ice or refrigerate water samples at a temperature of <10°C  during transit to the laboratory. Do
       not freeze the samples. Use insulated containers to assure proper maintenance of storage

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                                                                                       Method A


       temperature.  Take care that sample bottles are tightly closed and are not totally immersed in
       water during transit.
8.4    Holding Time Limitations
       Examine samples as soon as possible after collection. Do not hold samples longer than 6 hours
       between collection and initiation of filtration.
9.0   Quality Control

9.1    Each laboratory that uses Method A is required to operate a formal quality assurance (QA)
       program that addresses and documents instrument and equipment maintenance and performance,
       reagent quality and performance, analyst training and certification, and records storage and
       retrieval. Additional recommendations for QA and quality control (QC) procedures for
       microbiological laboratories are provided in Reference 17.2.
9.2    Media sterility check — The laboratory should test media sterility by incubating one unit (tube
       or plate) from each batch of medium (BHIA/BHIB) as appropriate and observing for growth.
       Absence of growth indicates media sterility.  On an ongoing basis, the laboratory should perform
       a media sterility check every day that samples are analyzed.
9.3    Method blank (water sample  filtration blank) — Filter a 50-mL volume of sterile PBS before
       beginning the sample filtrations. Remove the funnel from the filtration unit.  Using two sterile or
       flame-sterilized forceps, fold the filter on the base of the filtration unit and place it in an
       extraction tube with glass beads as described in Section 7.20. Extract as in Section 11.5. Absence
       of fluorescence growth curve during PCR analysis of these samples (reported as  "0" on
       SmartCycler and "undetermined" on ABI model 7900) indicates the absence of contaminant
       target DNA (see Data Quality  Acceptance, below).  Prepare one method blank filter for every
       six samples.
9.4    Positive controls — The laboratory should analyze positive controls  to ensure that the method is
       performing properly. Fluorescence growth curve (PCR amplification trace) with an appropriate
       cycle threshold (CT) value during PCR indicates proper method performance. On an ongoing
       basis, the laboratory should perform positive control analyses every day that samples are
       analyzed.  In addition, controls should be analyzed when new lots of reagents or filters are used.
       9.4.1   Calibrator samples will serve as the positive control. Analyze as described in Section
               11.0. Note: Calibrator samples contain the same amount of extraction buffer and starting
               amount of Salmon DNA as the test samples; hence E. faecalis calibrator DNA extracts
               (Section 11.3) will be  used as a positive control for both Enterococcus and SPC qPCR
               assays.
       9.4.2   If the positive control  fails to exhibit the appropriate fluorescence growth curve response,
               check and/or replace the associated reagents, and reanalyze.  If positive controls still fail
               to exhibit the appropriate fluorescence growth curve response, prepare new calibrator
               samples and reanalyze (see Section 9.7).
9.5    No template controls — The  laboratory should analyze "No Template Controls" (NTC) to
       ensure that the Master Mix PCR reagents are not contaminated. On an ongoing basis, the
       laboratory should perform NTC analyses every day that samples are analyzed. If greater than
       one-third of the NTC reactions for a PCR master mix exhibit true positive logarithmic
       amplification traces with CT values below 45 (not from chemical degradation of probe with  linear
       kinetics that exhibit rising baseline) or if any one NTC reaction has a CT value lower than 35, the
       analyses should be repeated with new Master Mix working stock preparations.

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                                                                                        Method A
9.6    DNA standards and standard curves -Purified, RNA-free and spectrophotometrically
       quantified E. faecalis genomic DNA should be prepared as described in Section 11.2. Based on
       reported values for it size, the weight of a single E. faecalis genome can be estimated to be -3.6
       fg and there are four IsrRNA gene copies per genome in this species (see the rRNA operon
       database at http://rrndb.cme.msu.edu/rrndb). The concentration of IsrRNA gene copies per uL in
       the standard E. faecalis genomic DNA preparation can be determined from this information and
       from its spectrophotometrically determined total DNA concentration  by the formula:
         Concentration of IsrRNA   Total DNA concentration (fg/uL)   x   4 IsrRNA gene copies
             gene copies per uL = 	   	
                                           3.6fg/genome                       genome


       A composite standard curve should be generated from multiple analyses of serial dilutions of this
       DNA standard using the Enterococcus primer and probe assay and subjected to linear regression
       analysis as described in Section 12.2. From that point on, it is recommended that additional
       standard curves be generated from duplicate analyses of these same diluted standard samples with
       each new lot of TaqMan® master mix reagents or primers and probes to demonstrate comparable
       performance by these  new reagents. The r2 values from regressions of these curves should ideally
       be 0.99 or greater. Comparable performance is assessed by their slopes and y-intercepts which
       should be consistent with those from the initial composite analyses (e.g., within the 95%
       confidence range of the average values). Note: The 95% confidence ranges for these parameters
       in the initial composite standard curve can be generated using the Regression Analysis Tool
       which can be accessed from the "Data Analysis" selection under the "Tools" menu in Excel.
       Subsequent regressions can be performed by plotting the  data using the Chart Wizard in Excel
       and using the "add trend line" selection in the Chart menu and "display equation on chart"
       selection under Options to obtain slope and y-intercept values as illustrated in Section 12.2.
       In the event that the slope value from a subsequent standard curve regression is outside of the
       acceptance range, the  diluted standards should be re-analyzed. If this difference persists, new
       working stocks of the  reagents should be prepared and the same procedure repeated. If the
       differences still persist, the amplification factor values used for calculations of target cell
       numbers, as described in Section 8, should be modified based on the new slope values.  If the
       slopes are within acceptance range but Y-intercepts are not within acceptance range of this
       previous average, new serial dilutions of the DNA standard should be prepared and analyzed as
       described above.
9.7    Calibrator samples — The cell concentration of each cultured E. faecalis stock suspension used
       for the preparation of  calibrator sample extracts should be determined as described in Section
       11.1. A minimum of nine calibrator sample extracts should initially be prepared from three
       different freezer-stored aliquots of these stocks as described in Section 11.2. Dilutions of each of
       these calibrator sample extracts equivalent to the anticipated dilutions of the test samples used for
       analysis (e.g., 1, 5 and/or 25 fold) should be analyzed with the Enterococcus primer and probe
       assay. The  average and standard deviation of the CT values from these composite analyses should
       be determined. From that point on, a minimum of three fresh calibrator sample  extracts should be
       prepared from an additional frozen aliquot of the same stock cell suspension at  least weekly and
       preferably daily before analyses of each batch of test samples. Dilutions of each new calibrator
       sample  extract equivalent to the initial composite dilutions (e.g., 1,5 and/or 25  fold) should be
       analyzed using the Enterococcus primer and probe assay. The average CT value from these
       analyses should not be significantly different from the laboratory's average values from analyses
       of the initial calibrator sample extracts from the same stock cell suspension (i.e., not greater than
                                               10

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                                                                                      Method A
       three standard deviations). If these results are not within this acceptance range, new calibrator
       extracts should be prepared from another frozen aliquot of the same stock cell suspension and
       analyzed in the same manner as described above. If the results are still not within the acceptance
       range, the reagents should be checked by the generation of a standard curve as described in
       Section 9.6.
9.8    Salmon DNA Sample Processing Control (SPC) sequence analyses — While not essential, it
       is good practice to routinely prepare and analyze standard curves from serial dilutions of Salmon
       DNA working stocks in a manner similar to that described for the Enterococcus DNA standards
       in Section 9.6. At this time rRNA gene operon copy numbers per genome have not been reported
       in the literature for the salmon species O. keta. Therefore log-transformed total DNA
       concentration values or dilution factor values can be substituted for target sequence copy numbers
       as the  x-axis values in these plots and regression analyses.
       In general, target DNA concentrations in test samples can be  calculated as described in Section
       12.  However, the Salmon DNA PCR assay results for each test sample's 5 fold dilution should
       be within 3 CT units of the mean of the 5 fold diluted calibrator (and/or method blank) sample
       results. Higher CT values may indicate significant PCR inhibition or poor DNA recovery
       possibly due to physical, chemical, or enzymatic degradation. Repeat the Enterococcus and
       Salmon DNA PCR assays of any samples whose 5 fold dilution exhibits a Salmon DNA PCR
       assay CT value greater than 3 CT units higher than the mean of the calibrator sample results using
       a 5 fold higher dilution (net dilution: 25 fold) of the extracts.  The Enterococcus PCR result from
       assaying the original 5-fold dilution of the sample can be accepted if its Salmon DNA assay CT
       value is lower than that of the corresponding 25 fold dilution of the sample. This pattern of
       results  is indicative of poor recovery of total DNA in the extract rather than PCR inhibition. The
       poor DNA recovery is compensated for by the calculation method. Contrarily, if the Salmon
       PCR assay CT value of the 25-fold dilution of the sample is lower than that of the 5 fold dilution
       of the sample, then the Enterococcus PCR assay result from the 25 fold dilution of the sample is
       considered more accurate. However the Enterococcus PCR results should be reported as
       questionable if the Salmon DNA assay's result is still not within 3 CT units of the mean CT result
       of the 25 fold dilution of the three calibrators.
10.0  Calibration and Standardization of Method-Related  Instruments

10.1   Check temperatures in incubators twice daily with a minimum of 4 hours between each reading to
       ensure operation within stated limits.
10.2   Check thermometers at least annually against a NIST certified thermometer or one that meets the
       requirements of NIST Monograph SP 250-23. Check columns for breaks.
10.3   Spectrophotometer should be calibrated each day of use using OD calibration standards between
       0.01 - 0.5. Follow manufacturer instructions for calibration.
10.4   Micropipettors should be calibrated at least annually and tested for accuracy on a weekly basis.
       Follow manufacturer instructions for calibration.
10.5   Follow manufacturer instructions for calibration of real-time PCR instruments.
11.0  Procedure
       Note: E. faecalis cell suspensions (Section 11.1), and E. faecalis DNA standards (Section 11.2)
       may be prepared in advance. Calibrator samples (Section 11.3) should be prepared at least
       weekly.

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                                                                                       Method A
11.1   Preparation of E. faecalis cell suspensions for DNA standards and calibrator samples
       11.1.1  Thaw an E. faecalis (ATCC #29212) stock culture (Section 7.8) and streak for isolation
               on BHIA plates.  Incubate plates at 37°C ± 0.5°C for 24 ± 2 hours.
       11.1.2  Pick an isolated colony of E. faecalis from BHIA plates and suspend in 1 mL of sterile
               phosphate buffered saline (PBS) and vortex.
       11.1.3  Use 10 uL of the  1-mL suspension of E. faecalis to inoculate a 10-mL BHIB tube.  Place
               the inoculated tube and one uninoculated tube (sterility check) on a shaker set at 250 rpm
               and incubate at 37°C ± 0.5°C for 24 ± 2 hours. Note: It is advisable to verify that the
               selected colony is Enterococcus as described, for example, in section 15 of EPA Method
               1600
       11.1.4  After incubation, centrifuge the BHIB containing E. faecalis for 5 minutes at 6000 x g.
       11.1.5  Aspirate the supernatant and resuspend the cell pellet in 10 mL PBS.
       11.1.6  Repeat the two previous steps twice and suspend final E. faecalis pellet in 5 mL of sterile
               PBS. Label the tube as E. faecalis undiluted stock cell suspension, noting cell
               concentration after determination with one of the  following steps.
       11.1.7  Determination of calibrator sample cell concentrations based on one of the three options
               below.
                  Option 1: Spectrophotometric absorbance - Remove three 0.1-mL aliquots of
                  undiluted cell suspension and dilute each with 0.9 mL of PBS (10"1  dilution).  Read
                  absorbance at 595 nm in spectrophotometer against PBS blank  (readings should
                  range from 0.05 to 0.3 OD).  Calculate cells/mL (Y) in undiluted cell suspension
                  using the formula from the standard curve shown below where  X is the average 595
                  nm spectrophotometer reading.
                         Y = (1 x 109  cells / mL x X) / 0.19
               •   Option 2: Hemocvtometer counts - Serially dilute 10 uL of undiluted cell suspension
                  with PBS to 10"1, 10"2, and 10"3 dilutions and determine cell concentration of 10"2 or
                  10"3 dilutions in a hemocytometer or Petroff Hauser counting chamber under
                  microscope.
               •   Option 3: plating - Note:  BHIA plates should be prepared in advance if this option is
                  chosen. For enumeration of the E. faecalis undiluted cell suspension,  dilute and
                  inoculate according to the following. Note: BHIA plates should be made in advance
                  if this option  is chosen.
                  A)  Mix the E. faecalis undiluted cell suspension by vigorously shaking the 5-mL
                      tube a minimum of 25 times. Use a sterile pipette to transfer 1.0 mL of the
                      undiluted cell suspension to 99 mL of sterile PBS, cap, and mix by vigorously
                      shaking the bottle a minimum of 25 times. This is cell suspension dilution "A".
                      A 1.0-mL volume of dilution "A" is 10"2 mL of the original undiluted cell
                      suspension.
                  B)  Use  a sterile pipette to transfer 11.0 mL of cell suspension dilution "A" to 99 mL
                      of sterile PBS, cap, and mix by vigorously shaking the bottle a minimum of 25
                      times.  This is cell suspension dilution "B".  A 1.0-mL volume of dilution "B" is
                       10"3  mL  of the original undiluted cell suspension.
                  C)  Use  a sterile pipette to transfer 11.0 mL  of cell suspension dilution "B" to 99
                      mL of sterile PBS, cap, and mix by vigorously shaking the bottle  a minimum of
                                               12

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                                                                      Method A
     25 times. This is cell suspension dilution "C". A 1.0-mL volume of dilution
     "C" is 10"4 mL of the original undiluted cell suspension.
D)   Use a sterile pipette to transfer 11.0 mL of cell suspension dilution "C" to 99 mL
     of sterile PBS, cap, and mix by vigorously shaking the bottle a minimum of 25
     times. This is cell suspension dilution "D".  A 1.0-mL volume of dilution "D" is
     10"5 mL of the original undiluted cell suspension.
E)   Use a sterile pipette to transfer 11.0 mL of cell suspension dilution "D" to 99 mL
     of sterile PBS, cap, and mix by vigorously shaking the bottle a minimum of 25
     times. This is cell suspension dilution "E".  A 1.0-mL volume of dilution "E" is
     10"6 mL of the original undiluted cell suspension.
F)   Prepare BHIA (Section 7.6).  Ensure that agar surface is dry. Note: To ensure
     that the agar surface  is dry prior to use, plates should be made several days in
     advance and stored inverted at room temperature or dried using a laminar-flow
     hood.
G)   Each of the following will be conducted in triplicate, resulting in the evaluation
     of nine spread plates:
    •   Pipet 0.1 mL of dilution "C" onto surface of BHIA plate [10"5 mL (0.00001)
        of the original cell suspension].
    •   Pipet 0.1 mL of dilution "D" onto surface  of BHIA plate [10'6 mL (0.000001)
        of the original cell suspension].
    •   Pipet 0.1 mL of dilution "E" onto surface of BHIA plate [ 10"7 mL
        (0.0000001) of the original cell suspension].
H)   For each spread plate, use a sterile bent glass rod or spreader to distribute
     inoculum over surface of medium by rotating  the dish by hand or on a rotating
     turntable.
I)    Allow inoculum to absorb into the medium completely.
J)    Invert plates and incubate at 35°C ± 0.5°C for 24 ± 4 hours.
K)   Count and record number of colonies per plate.  Refer to the equation below for
     calculation of undiluted cell suspension concentration.
                                              ..... + CFUn
      CFU/mLundlluted    =
    Where:

    CFU/mLundliuted =   E. faecalis CFU/mL in undiluted cell suspension
    CPU           =   number of colony forming units from BHIA plates yielding
                       counts within the ideal range of 30 to 300 CPU per plate
    V             =   volume of undiluted sample in each BHIA plate yielding
                       counts within the ideal range of 30 to 300 CPU per plate
    n              =   number of plates with counts within the ideal range
                             13

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                                                                                        Method A
Table 1.  Example Calculations of E. faecalis Undiluted Cell Suspension Concentration
Examples
Example 1
Example 2
CPU / plate (triplicate analyses) from
BHIA plates
10'5 mL plates
275, 250, 301
TNTCb, TNTC,
TNTC
10'6 mL plates
30, 10, 5
TNTC, 299, TNTC
10~7 mL plates
0, 0, 0
12, 109, 32
E. faecalis CPU / mL in undiluted
suspension3
(275+250+30) /(10-5+10-5+10-6) =
5557 (2.1 x10'S) = 26,428,571 =
2.6x107CFU/mL
(299+1 09+32) /(10'6+10-7+10-7) =
440 / (1 .2 x 1 0'6) =366,666,667 =
3.7x108CFU/mL
 Cell concentration is calculated using all plates yielding counts within the ideal range of 30 to 300 CPU per plate
b Too numerous to count


        11.1.8 Divide remainder of undiluted cell suspension (approximately 5 mL) into 6 x 0.5 mL
               aliquots for DNA standard preparations and 100-200 x 0.01 mL (10 i^L) aliquots for
               calibrator samples and freeze at -20°C. Note: Cell suspension should be stirred while
               aliquoting. It is also recommended that separate micropipettor tips be used for each 10
               AiL aliquot transfer and that the volumes in each tip be checked visually for consistency.
11.2    Preparation of E. faecalis genomic DNA standards
        11.2.1  Remove two 0.5  mL undiluted E. faecalis cell suspensions (Section 11.1.8) from freezer
               and thaw completely.
        11.2.2 Transfer cell suspensions to extraction tubes with glass.
        11.2.3 Tightly close the tubes, making sure that the O-rings are seated properly.
        11.2.4 Place the tubes in bead beater and shake for 60 seconds at the maximum rate (5000 rpm).
        11.2.5 Remove the tubes from the mini bead beater and centrifuge at 12,000 x  g for one minute
               to pellet the glass beads and debris.
        11.2.6 Using a 200 uL micropipettor, transfer 350 uL of supernatants to sterile 1.7-mL
               microcentrifuge tubes. Recover supernatants  without disrupting the glass beads at the
               tube bottom.
        11.2.7 Centrifuge crude supernatants at 12,000 x g for 5 minutes and transfer 300 uL of clarified
               supernatant to clean, labeled 1.7-mL low retention microcentrifuge tubes, taking care not
               to disturb the pellet.
        11.2.8 Add  1 uL of 5 ug/uL RNase A  solution to each clarified supernatant, mix by vortexing
               and incubate at 37°C for 1 hour.
               Note: Steps 11.2.9- 11.2.15 may be substituted with an optional method if a DNA
               purification procedure is chosen other than the DNA-EZ purification kit. In such a case,
               manufacturer instructions should be followed rather than these steps. Continue  onward
               from step 11.2.16.
        11.2.9    Add 0.6 mL of binding buffer solution from a DNA-EZ purification kit to each of the
                  RNase A-treated extracts and mix by vortexing. Note: In general, a minimum
                  concentration of 5 x  108 cells is required for this step.
                                               14

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                                                                                       Method A


       11.2.10    If using the DNA-EZ purification kit, perform the following steps. Insert one
                  DNAsure™ column from the DNA-EZ purification kit into a collection tube (also
                  provided with kit) for ea°h of the two extracts. Transfer each of the extract and
                  binding buffer mixtures from section 11.2.9 to a DNAsure™ column and collection
                  tube assembly and centrifuge for 1 min at 12,000 x g.
       11.2.11    Transfer each of the DNAsure™ columns to new collection tubes. Discard previous
                  collection tubes and collected liquid.
       11.2.12    Add 500 uL EZ-Wash Buffer from the DNA-EZ purification kit to each of the
                  DNAsure™ columns and centrifuge at 12,000 x g for 1 minute. Discard the liquid in
                  the collection tube.
       11.2.13    Repeat step 11.2.12.
       11.2.14    Transfer each of the DNAsure™ columns to a clean, labeled 1.7-mL low retention
                  microcentrifuge tube and add 50 uL of DNA elution buffer to each column.
                  Centrifuge for 30 seconds at 12,000  x g.  Repeat this procedure again to obtain a total
                  DNA eluate volume of-100 uL from each column.
       11.2.15    Pool the two eluates to make a total  volume of approximately 200 uL.
       11.2.16    Transfer entire purified DNA eluate volume from each column to a clean and sterile
                  microcuvette for UV spectrophotometer and read absorbance at 260 and 280 nM.
                  (note: the cuvette should be blanked with DNA elution buffer before reading sample.
                  If necessary, the sample may be diluted with elution buffer to reach minimum volume
                  that can be accurately read by the spectrophotometer (see manufacturer's
                  recommendation) however, this may reduce the DNA concentration to  a level that can
                  not be accurately read by the spectrophotometer. If available, readings  can be taken of
                  2 uL aliquots of the sample with aNanoDrop™ Spectrophotometer.
       11.2.17    Sample is acceptable as a standard if ratio of OD26o/OD28o readings is > or = to 1.75.
       11.2.18    Calculate total DNA concentration in sample  by formula:
                  OD260 reading x 50 ng/uL DNA/OD260
       11.2.19    Transfer sample back to labeled 1.7-mL non-retentive microcentrifuge  tube and store
                  at -20°C.
11.3   Extraction of E. faecalis calibrator samples
       11.3.1 A minimum of three calibrator extracts should be prepared during each week of analysis.
              Note: To prevent contamination of water sample filtrates and filter blanks,  this procedure
              should be performed at a different time, and, if possible,  in a different work station than
              the procedures in Sections  11.1 and 11.2 above and Section  11.5 below.
       11.3.2 Remove one tube containing a 10  uL aliquot of E. faecalis undiluted stock cell
              suspension (Section 11.1.8) from the freezer and  allow to thaw completely on ice.
              Note: If using BioBalls for calibrators add a single BioBall™ to each of 3,  100-mL sterile
              PBS blanks, filter (Section 11.4), and extract according to (Section 11.5).


       11.3.3 While cell  stock is thawing, using sterile (or flame-sterilized) forceps, place one
              polycarbonate filter (Section 6.14) in an extraction tube with glass beads. Prepare one
              filter for each sample to be extracted in this manner.
                                               15

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                                                                                         Method A
       11.3.4 Dispense 590 uL of Salmon DNA/extraction buffer (Section 7.12) into three extraction
               tubes with glass beads and filters.  Prepare one tube for each of the three calibrator
               samples to be extracted in this manner. Label tubes appropriately.
       11.3.5 When E. faecalis suspension has thawed, transfer 990 uL AE buffer (Section 7.11) to the
               10 uL E. faecalis stock cell tube and mix thoroughly by vortexing.  Pulse microcentrifuge
               tube briefly (1-2 sec.) to coalesce droplets in tube.
       11.3.6 Immediately after vortexing the E. faecalis suspension, spot 10 uL onto the
               polycarbonate filter in a calibrator sample tube.
       11.3.7 Tightly close the tube, making sure that the O-ring is seated properly.
       11.3.8 Repeat Sections 11.3.6 and 11.3.7 for the other two filters to prepare three calibrator
               samples with E. faecalis.
       11.3.9 Place the tubes in the mini bead beater and shake for 60 seconds at the maximum rate
               (5000 rpm).
       11.3.10   Remove the tubes from the mini bead beater and centrifuge at 12,000 x g for one
                  minute to pellet the glass beads and debris.
       11.3.11   Using a 200 uL micropipettor, transfer the crude supernatant to the corresponding
                  labeled sterile  1.7-mL microcentrifuge tube.  Transfer 400 uL of supernatant without
                  disrupting the debris pellet or glass beads at the tube bottom. Note: The filter will
                  normally remain intact during the bead beating and centrifugation process. Generally,
                  400 uL of supernatant can be easily collected. Collect an absolute minimum of 100
                  //L of supernatant.
       11.3.12   Centrifuge at 12,000 x  g for 5 minutes and transfer clarified supernatant to a clean,
                  labeled 1.7-mL tube, taking care not to disturb the pellet. Note: Cell pellet may not be
                  visible in calibrator samples.
       11.3.13   Label the tubes as undiluted or Ix E. faecalis calibrator  extracts. Label additional 1.7-
                  mL tubes for 5  and 25 fold dilutions.  In appropriately labeled tubes, using a
                  micropipettor, add a 50 ^L aliquot of each  Ix E. faecalis calibrator extracts and dilute
                  each with 200  uL AE buffer (Section 7.11) to make 5  fold dilutions. In appropriately
                  labeled tubes using a micropipettor, add a 50 /jL aliquot of each 5 fold dilution and
                  dilute each with 200 uL AE buffer to make 25 fold dilutions.  Store all diluted and
                  undiluted extracts in refrigerator.
       11.3.14   If the extracts are not analyzed immediately, refrigerate. For long term storage, freeze
                  at -20°C or -80°C.
11.4   Water sample filtration
       Note: It is required that one water sample filtration blank (method blank) be prepared for every 6
       water samples (Section 9.3) analyzed by the same procedure.
       11.4.1      Place a polycarbonate  filter (Section 6.14) on the filter base, and attach the funnel to
                   the base  so that the membrane filter is now held between the funnel and the base.
       11.4.2     Shake the sample bottle vigorously 25 times to distribute the bacteria uniformly, and
                   measure 100 mL of sample into the funnel.
       11.4.3     Filter 100 mL of water sample. After filtering the sample, rinse the sides of the funnel
                   with 20-30 mL of sterile PBS (Section 7.4) and continue filtration until all liquid has
                   been pulled through the filter.  Turn off the vacuum and remove the funnel from the
                   filter base.
                                               16

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                                                                                         Method A
       11.4.4    Label an extraction tube with glass beads (Section 7.20) to identify water sample.
                  Leaving the filter on the filtration unit base, fold into a cylinder with the sample side
                  facing inward, being careful to handle the filter only on the edges, where the filter has
                  not been exposed to the sample.  Insert the rolled filter into the labeled extraction
                  tube with glass beads.  Prepare one filter for each sample filtered in this manner.

       11.4.5 Cap the extraction tube. Tubes may be frozen at -20°C or -80°C until analysis.
11.5   DNA extraction of water sample filter extracts and method blanks
       11.5.1  Using a 1000 uL micropipettor, dispense 590 uL of the Salmon DNA/extraction buffer
               (Section 7.11) to each labeled extraction tube with glass beads containing water sample
               or method blank filters  from Section 11.3.4.  Extract the method blank last.
       11.5.2 Tightly close the tubes, making sure that the O-ring is seated properly.
       11.5.3 Place the tubes in the mini bead beater and shake for 60 seconds at the maximum rate
               (5000 rpm).
       11.5.4 Remove the tubes from the mini bead beater and centrifuge at 12,000 x g for 1 minute to
               pellet the glass beads and debris. Note: To further prevent contamination, a new pair of
               gloves may be donned for steps 11.4.5, 11.4.6, and 11.4.7 below.
       11.5.5 Using the 200 uL micropipettor, transfer 400 uL of the  supernatant to corresponding
               labeled sterile 1.7-mL microcentrifuge tube, taking care not to pick up glass beads or
               sample debris (pellet). Note: The filter will normally remain intact during the bead
               beating and centrifugation  process. Generally, 400 uL of supernatant can easily be
               collected. Collect an absolute minimum of 100 ^L of supernatant. Recover the method
               blank supernatant last.
       11.5.6 Centrifuge crude supernatant from Section 11.4.5 for 5  minutes at 12,000 * g. Transfer
               350 uL of the clarified supernatant to another 1.7-mL tube, taking care not to disturb
               pellet. Note: pellet may not be visible in water samples. Recover the method blank
               supernatant last.
       11.5.7 Label the tubes from Section 11.4.6 as undiluted or Ix water sample extracts with sample
               identification. These are the water sample filter extracts. Also label tubes for method
               blanks. Label additional 1.7-mL tubes for 5 and 25 fold dilutions. In appropriately
               labeled tubes, using a micropipettor,  add a 50 /^L aliquot of each Ix water sample extract
               and dilute each with 200 uL AE buffer (Section 7.11) to make 5 fold dilutions. In
               appropriately labeled tubes using a micropipettor, add a 50 //L aliquot of each 5 fold
               dilution and dilute each with 200 uL of AE buffer to make 25 fold dilutions. Dilute the
               method blank supernatant last
       11.5.8 Store all diluted and undiluted extracts in refrigerator. Note: Use of 5 fold diluted
               samples for analysis is currently recommended if only one dilution can be analyzed.
               Analyses of undiluted water sample extracts have been  observed to cause a significantly
               higher incidence of PCR inhibition while analyses of 25 fold dilutions may unnecessarily
               sacrifice sensitivity.
       11.5.9 If the extracts are not analyzed immediately, refrigerate. For long term storage, freeze at
               -20°C or-80°C.
11.6   Preparation of qPCR assay mix
       11.6.1  To minimize environmental DNA contamination, routinely treat all work surfaces with a
               10% bleach solution, allowing the bleach to contact the work surface for a minimum of
                                               17

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                                                                                       Method A
               15 minutes prior to rinsing with sterile water. If available, turn on UV light for 15
               minutes. After decontamination, discard gloves and replace with new clean pair.
       11.6.2  Remove primers and probe stocks from the freezer and verify that they have been diluted
               to solutions of 500 uM primer and 100 uM probe.
       11.6.3  Prepare working stocks ofEnterococcus, and Salmon DNA (Sketa 22) primer/probe
               mixes by adding 10 uL of each Enterococcus or Salmon DNA (Sketa 22) primer stock
               and 4 uL of respective probe stock to 676 uL of PCR grade water,  and vortex.  Pulse
               centrifuge to create a pellet. Use a micropipettor with aerosol barrier tips for all liquid
               transfers. Transfer aliquots of working stocks for single day use to separate tubes and
               store at 4°C.
       11.6.4  Using a micropipettor, prepare assay mix of the Enterococcus, and Salmon DNA (Sketa
               22) reactions in separate, sterile, labeled  1.7-mL microcentrifuge tubes as described in
               Table 2.
Table 2.  PCR Assay Mix Composition
Reagent
Sterile H2O
BSA
TaqMan® master mix
Primer/probe working stock solution
Volume/Sample (multiply by # samples to be analyzed
per day)
1.5|JL
2.5 pL
12.5 pL
3.5 pL
        Note: This will give a final concentration of 1 uM of each primer and 80 nM of probe in the
        reactions.  Prepare sufficient quantity of assay mix for the number of samples to be analyzed per
        day including calibrators and negative controls plus at least two extra samples. Prepare assay
        mixes each day before handling DNA samples.

        11.6.5  Vortex the assay mix working stocks; then pulse microcentrifuge to coalesce droplets.
               Return the primer/probe working stocks and other reagents to the refrigerator.
11.7   ABI 7900 & ABI 7500 (non-Fast) qPCR assay preparation (Reference 17.1)
       Transfer 20 uL of mastermix containing Enterococcus primers and probe to wells of a 96-well
       PCR reaction tray equal to number of samples to be analyze including calibrator and negative
       control samples. (Note: The same tip can be used for pipetting multiple aliquots of the same assay
       mix as long as it doesn't make contact with anything else).
       Example: For the analysis of 18 recreational water samples,  51 wells will require the addition of
       assay mix with Enterococcus primers and probe as follows:  18 samples, two replicates each (36),
       3 method blanks, two replicates each (6), 3  no template controls, one replicate each (3), and 3
       calibrators, 2 replicates each (6) = 51 wells.
       11.7.1  Transfer 20 uL of mastermix containing Enterococcus primers and probe to wells of a
               96-well PCR reaction tray equal to  number of samples to be analyzed including calibrator
               and negative control samples. Pipette into the center of the wells, taking care to not touch
               the well walls with the  pipette tip.   (Note: The same tip can be used for pipetting multiple
               aliquots of the same assay mix as long as it doesn't make contact with anything else).
                                               18

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                                                                                       Method A


       11.7.2 When all wells are loaded, cover tray loosely with aluminum foil or plastic wrap and
              transfer to refrigerator or directly to the PCR preparation station used for handling DNA
              samples (Section 6.1). Note: All aliquoting of assay mixes to reaction trays must be
              performed each day before handling of DNA samples.
       11.7.3 Transfer 5 uL each of the diluted (or undiluted) DNA extracts of method blanks and
              water samples (Section 11.5.7), and then corresponding dilutions of calibrator samples
              (Section 11.3.13), to separate wells of the PCR reaction tray containing Enterococcus
              assay mix. Note: Record positions of each sample.
       11.7.4 Transfer 5 uL each of the diluted (or undiluted) DNA extracts of method blanks and
              water samples (Section 11.5.7), and corresponding diluted calibrator samples (Section
              11.3.13) to separate wells of the PCR reaction tray containing Salmon DNA assay mix.
              Record positions of each sample.
       11.7.5 Transfer 5 uL aliquots of AE buffer to wells of PCR reaction tray containing
              Enterococcus master mix that are designated as no-template controls. Record positions
              of these samples.
       11.7.6 Tightly cap wells of PCR reaction tray containing samples or cover tray and seal tightly
              with optical adhesive PCR reaction tray.
       11.7.7 Run reactions in ABI 7900 & ABI 7500 (non-Fast) sequence detector. For platform-
              specific operation see Appendix A.

11.8   Smart Cycler® qPCR assay preparation
       11.8.1 Label 25 uL Smart Cycler® tubes with sample identifiers and assay mix type (see
              Section 11.7.8 for examples) or order tubes in rack by sample number and label rack with
              assay mix type. It is recommended that the unloaded open SmartCycler® tubes be
              irradiated under ultraviolet light in a PCR cabinet for 15 minutes. Using a micropipettor,
              add 20 uL of the Enterococcus assay mix (section 11.6.5) to labeled tubes. Avoid
              generating air bubbles, as they may interfere with subsequent movement of the liquid into
              the lower reaction chamber.  The same tip can be used for pipetting multiple aliquots of
              the same assay mix as long as it doesn't make contact with anything  else. Repeat
              procedure for Salmon DNA (Sketa 22) assay mix.
       11.8.2 Add 5 uL of AE buffer to no-template control tubes and close tubes tightly.
       11.8.3 Close the other PCR tubes loosely and transfer to refrigerator or directly to the PCR
              preparation station used for handling DNA samples (Section 6.1).  Note: All aliquoting of
              assay mixes to reaction tubes must be performed each day before handling of DNA
              samples.
       11.8.4 Transfer 5 uL each of the diluted (or undiluted) DNA extracts of method blanks and
              water samples (Section 11.5.7), and then corresponding dilutions of calibrator samples
              (Section 11.3.13) to tubes containing Enterococcus and Salmon DNA (Sketa 22) mixes.
              Close each tube tightly after adding sample.  Load the method blank PCR assays last.
              Label the tube tops as appropriate.
       11.8.5 When all Smart Cycler® tubes have been loaded, place them in a Smart Cycler®
              centrifuge, and spin for 2-4  seconds.
       11.8.6 Inspect each tube to verify that the sample has properly filled the lower reaction chamber.
              A small concave meniscus may be visible at the top of the lower chamber, but no air
              bubbles should be present. (If the lower chamber has not been properly filled, carefully
              open and reclose the tube, and re-centrifuge). Transfer the tubes to the thermocycler.
                                               19

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                                                                                      Method A


       11.8.7 For platform-specific operation see Appendix B.

       11.8.8 Suggested sample analysis sequence for Smart Cycler®

              Example: For analyses on a single 16-position Smart Cycler®, calibrator samples and
              water samples will need to be analyzed in separate runs and a maximum of 6 water
              samples (or 2 replicates of 3 samples) can be analyzed per run, as described in Tables 3
              and 4, below.

       Table 3.  Calibrator PCR Run -14 Samples
Sample Description*
3 Calibrators * 2 replicates (1, 5, or 25 fold dilution )
3 Calibrators * 2 replicates (1, 5, or 25 fold dilution )
No template controls (reagent blanks)
Quantity
6
6
2
PCR Assay Master Mix
Enterococcus
Salmon DMA
Enterococcus
        Diluted equivalently to the water samples
       Table 4.  Water Sample PCR Run -14 Samples
Sample Description*
Water samples, (1, 5, or 25 fold dilution )
Method blank, (1, 5, or 25 fold dilution )
Water samples, (1, 5, or 25 fold dilution )
Method blank, (1, 5, or 25 fold dilution )
Quantity
6
1
6
1
PCR Assay Master Mix
Enterococcus
Enterococcus
Salmon DMA
Salmon DMA
       * Use of five-fold diluted samples for analysis is currently recommended if only one dilution can be analyzed.
       Analyses of undiluted water sample extracts have been observed to cause a significantly higher incidence of
       PCR inhibition while 25 fold dilutions analyses may unnecessarily sacrifice sensitivity.
12.0  Data Analysis and Calculations

12.1   Overview: This section describes a method for determining the ratio of the target sequence
       quantities recovered from a test (water filtrate) sample compared to those recovered from
       identically extracted calibrator samples using an arithmetic formula, referred to as the AACT
       comparative cycle threshold calculation method. The AACT relative quantitation method also
       normalizes these ratios for differences in total DNA recovery from the test and calibrator samples
       using qPCR analysis CT values for a reference sequence provided by the SPC DNA. These ratios
       are converted to absolute measurements of total target sequence quantities recovered from the test
       samples by multiplying them by the average total number of target sequences that are normally
       recovered from a constant number of target  organisms that are added to all calibrator samples.
       The complete procedure for determining target sequence quantities in water samples is detailed
       below.
12.2   Generation of CT value vs. target sequence number standard curve: Three replicate serial
       dilutions of a DNA standard, prepared as described in section 9.6 should be prepared to give
       concentrations of 4 x 104, 4 x 103, 4 x 102, 2 x 102 and 1 x  102 IsrRNA gene sequences per 5 uL
       (the standard sample volume  added to the PCR reactions) and the replicates of each dilution
       pooled. Note: a procedure for the determinations of target sequence concentrations  in the DNA
       standard is also provided in Section 9.6.
                                              20

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                                                                                        Method A
       Aliquots of each of these dilutions should be stored at 4°C in low retention microcentrifuge tubes
       and can be reused for repeated qPCR analyses. QPCR analyses of these diluted standards using
       the Enterococcus primer and probe assay should be performed at least three separate times in
       duplicate. CT values from these composite analyses should be subjected to regression analysis
       against the loglO-transformed target sequence numbers per reaction as described in Section 9.6
       with example results illustrated in Figure 1.
                                       234
                                     Log target sequences per reaction
Figure 1: Example plot and regression analysis of qPCR analysis cycle threshold values vs. log target
sequences per reaction.

       Amplification factors (AF) used for subsequent comparative cycle threshold calculations (Section
       12.4) can be calculated from the slope value of this curve by the formula AF = 10A(1 / (-)slope
       value). An example calculation using the slope value from the example regression is shown
       below:
        AF=10A(1 73.4777) = 1.94
12.3   Calculation of average target  sequence recovery in calibrator  sample extracts: A minimum
       of nine calibrator sample extracts should initially be prepared from at least three different freezer-
       stored aliquots of each cultured E. faecalis stock suspension that is prepared as described in
       Section 11.1. Dilutions of each  of these calibrator sample extracts equivalent to the anticipated
       dilutions of the test samples used for analysis (e.g., 1, 5 and/or 25  fold) should be analyzed with
       the Enterococcus primer and probe assay. The average CT value from these analyses should be
       interpolated on the standard curve generated from the DNA standard (Section 12.2) to determine
       the average number of target sequences per 5 uL of extract used in the reactions. An example
       calculation using an average calibrator extract CT value of 25.21 is shown below:
       Average calibrator target sequences/5  uL extract = 10A((25.21-38.44) / -3.477) = 6382
       Note: Four places should be kept from this calculation for the following calculation (i.e.,
       6382.6983). Dividing this value by 5 gives the average calibrator target sequences/ uL extract
       which can be multiplied by the total volume of the extract at the applicable dilution level (e.g.,
       600 uL of original extract volume x 5 = 3000 uL for a 5 fold diluted sample) to determine the
       average total quantity of target sequences recovered in the calibrator sample extracts. An example
       of this calculation using the average calibrator target sequences/reaction value determined
       immediately above is shown below:
                                               21

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                                                                                        Method A
            Average target sequences   =    6382 target sequences   x 3000 uL total extract volume
               Calibrator extract                 5 uL extract

                                      =    3,829,619
       12.3.1  Calculation of average target sequence recovery per Enterococcus cell in calibrator
               sample extracts (optional): In previous studies, measurements of recreational water
               quality by the qPCR method have been reported as Enterococcus calibrator cell
               equivalents (References 17.4). Calculations performed to obtain this reporting unit are
               identical to those described in Section 12.4 except that the ratios of target sequences
               obtained as described in Sections 12.4.1 - 12.4.4 are multiplied by the estimated
               quantities of Enterococcus cells added to the calibrator samples rather than by the
               average target sequences recovered per calibrator extract as described in Section 12.4.5.
               While the use of this reporting unit is no longer recommended because of the false
               impression it creates concerning the cell concentration detection limit of the qPCR
               method, it still may be of value for comparing previous results with those of future
               studies.
               A prerequisite for making such comparisons is to determine that the ratio of the numbers
               of target sequences recovered in calibrator sample extracts to the numbers of
               Enterococcus cells added to these samples is consistent in different studies. For the
               purpose of determining this ratio, it is recommended that the cell concentrations of the
               cultured E. faecalis stock suspension used for the preparation of calibrator samples in
               each laboratory be determined by at least two of the three alternative  methods described
               in Section 11.1 to establish the degree of agreement between these enumeration methods.
               The recommended quantity of cells that are added to each calibrator sample is 100,000.
               Dividing the average target sequences recovered per calibrator extract (determined as
               described in Section 12.3) by this number provides the ratio of target sequence numbers
               to cell numbers. An example  of this calculation using the average target sequences/
               calibrator extract value determined in Section 12.3 is shown below:
               Ratio of target sequence numbers to cell numbers = 3,829,619 /  100,000 = 38.29
12.4   Calculation of target sequence quantities in test samples: A minimum of three fresh calibrator
       samples should be extracted and analyzed at least on a weekly basis and preferably on a daily
       basis in association with each batch of water sample filtrates. QC analysis of the  analysis results
       from these calibrator extracts should be performed as described in Section 9.7. CT values from
       the Enterococcus target sequence and salmon DNA  Sample Processing Control (SPC) qPCR
       assays for both the calibrator and test samples are used in the AACT comparative cycle threshold
       calculation method to  determine the ratios of target sequences in the test and calibrator sample
       extracts and these ratios are converted to absolute measurements of total target sequence
       quantities recovered from the test samples as specified  below and illustrated  in Table 5.
       12.4.1  Subtract the SPC assay CT value (CT,spc) from the target assay CT value (CT,target) for each
               calibrator sample extract to obtain ACT value and calculate the average ACT value for
               these calibrator samples.
       12.4.2 Subtract the SPC assay CT value (CT,spc) from the target assay CT value (CT,target) for each
               water sample filtrate extract to obtain ACT values for each of these test samples. Note: if
               multiple analyses are performed on these samples, calculate the average ACT value.
       12.4.3 Subtract the average ACT value for the calibrator samples from the ACT value (or average
               ACT value) for each of the test samples to obtain AACT values.
                                               22

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                                                                                     Method A
       12.4.4 Calculate the ratio of the target sequences in the test and calibrator samples using the
              formula: AFA("AACT), where AF = amplification factor of the target organism PCR assay,
              determined as described in Section 12.2.
       12.4.5 Multiply the ratio of the target sequences in the test and calibrator samples by the average
              target sequences/calibrator extract, determined as described in Section 12.2, to determine
              absolute numbers of total target sequences/ extract for each of the test samples. Note:
              This calculation can be applied without modification to the analyses of diluted extracts if
              both the test sample and calibrator extracts are equally diluted and equal volumes of
              diluted extracts are analyzed.
Table 5. Exam
              ile Calculations (Amplification factor = 1.94)
Target
sequences
in Sample
3,829,619
Unknown
Sample
Type
Calibrator
Test
Cj.target
25.21
32.53
CT.SPC
30.45
30.65
ACT
-5.24
1.88
AACT
—
7.12
Measured Target Sequences in
Test Sample Extract
(1. 94 -iiCTxavg. target
sequences/calibrator)
—
0.0089x3,829,619 = 34,198
       12.4.6 The geometric mean of the measured target sequences and associated coefficients of
              variation in multiple water samples can be determined from individual sample CT values
              using the following procedure:
              12.4.6.1
              12.4.6.2
              12.4.6.3
                         Use ACT value for each individual water sample extract and the mean
                         calibrator ACT value to calculate the measured target sequence numbers in
                         each water sample extract, as described in Section 12.4.
                         Calculate the logio of the measured target sequence numbers in each water
                         sample (log N)
                         Calculate the mean (M) and standard deviation (S) from the values of log N
                         obtained in the previous step for all of the water sample extracts.

                         Calculate the geometric mean as 10M.

                         The implied coefficient of variation (CV) is calculated, based on the log
                         normal distribution, as the square root of iov/0434 - 1, where V = S2.

12.5   Reporting Results: Where possible, duplicate analyses should be performed on each sample.
       Report the results as Enterococcus (large subunit ribosomal RNA gene) target sequences per
       volume of water sample filtered.
              12.4.6.4
              12.4.6.5
13.0  Sample Spiking Procedure
       [This section will be updated after validation study]

14.0  Method Performance

14.1   Accuracy (Bias)
       The IsrRNA gene (23S rRNA) of Enterococci, which contains the target sequence amplified and
       detected by the primers and probe of the Enterococcus qPCR assay, is present in multiple copies
       in the genome of the different Enterococcus species. Enterococcus faecalis and E. faecium each
       contain 4 and 6 copies of the gene, respectively. The number of IsrRNA gene copies per genome
                                              23

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                                                                                      Method A
       has not been ascertained for all of the Enterococcus species which the Enterococcus qPCR assay
       can amplify and detect.  Hence, the use of E. faecalis cells as a calibrator for relative quantitation
       purposes and E. faecalis DNA as a standard for absolute quantitation purposes creates an inherent
       bias potentially affecting the accuracy of the quantitation depending on the species composition
       of the Enterococcus present in a water sample.
       The Enterococcus qPCR method makes the assumption that the Enterococcus cells present in the
       water sample contain the same number of genomes and IsrRNA gene copies as the E. faecalis
       calibrator cells which have been grown in culture media to a late-log or stationary phase in batch
       culture.  This assumption has not been validated if untrue may bias the accuracy of the results in a
       systematic manner. Bacterial cells contain more than one complete genome during growth and
       cell division phases of their life cycle. The number of genomic copies depends on their growth
       rate and cell division time. More than one cell division cycle is often required to complete
       replication of the genome  during rapid log-phase growth and cell division. The IsrRNA genes are
       replicated early in the cell cycle maximizing the number of IsrRNA gene copies present in cells
       during log phase growth.  This facilitates the enhanced ribosome production needed for the high
       level of protein translation needed during rapid cell growth and division.
       [This section will be updated after validation study]

15.0  Pollution Prevention

15.1   The solutions and reagents used in this method pose little threat to the environment when
       recycled and managed properly.
15.2   Solutions and reagents should be prepared in volumes consistent with laboratory use to minimize
       the  volume of expired materials to be disposed.


16.0  Waste Management

16.1   It is the laboratory's responsibility to comply with all federal, state, and local regulations
       governing waste management, particularly the biohazard and hazardous waste identification rules
       and land disposal restrictions, and to protect the air, water,  and land by minimizing and
       controlling all releases from fume hoods and bench operations. Compliance with all sewage
       discharge permits and regulations is also required.
16.2   Samples, reference materials, and equipment known or suspected to have viable enterococci
       attached or contained must be sterilized prior to disposal.
16.3   For further information  on waste management, consult "The Waste Management Manual for
       Laboratory Personnel" and "Less Is Better: Laboratory Chemical Management for Waste
       Reduction," both available from the American Chemical Society's Department  of Government
       Relations and Science Policy, 1155 16th Street NW, Washington, DC 20036.
                                              24

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                                                                                    Method A
17.0  References

17.1   Anonymous. 1997. User Bulletin #2. ABI Prism 7700 Sequence Detection System.  Foster City,
       CA, Applied Biosystems.
17.2   Bordner, R., J.A. Winter, and P.V. Scarpino (eds.). 1978. Microbiological Methods for
       Monitoring the Environment:  Water and Wastes, EPA-600/8-78-017
17.3   Cabelli, V. J., A. P. Dufour, M. A. Levin, L. J. McCabe, and P. W. Haberman. 1979.
       Relationship of Microbial Indicators to Health Effects at Marine Bathing Beaches.  Amer. Jour.
       Public Health. 69:690-696.
17.4   Haugland, R.A., S.C. Siefring, L.J. Wymer, K.P. Brenner, and A. P. Dufour. 2005. Comparison
       of Enterococcus Density Measurements by Quantitative Polymerase Chain Reaction and
       Membrane Filter Analysis at Two Freshwater Recreational Beaches. Water Research 39:559-
       568.
17.5   Ludwig, W. and K.-H. Schleifer.  2000.  How quantitative is quantitative PCR with respect to cell
       counts? System Appl. Microbiol. 23:556-562.
17.6   USEPA.  1983.  Health Effects Criteria for Marine Recreational Waters.  EPA-600/1-80-031.
17.7   USEPA.  1984.  Health Effects Criteria for Fresh Recreational Waters. EPA-600/1-84-004.
17.8   USEPA .  1986.  Ambient water quality criteria for bacteria - 1986. EPA 440/5-84-002.
17.9   Wade, T.J., Calderon, R.L., Sams, E., Beach, M., Brenner, K.P. & Dufour, A.P. 2006. Rapidly
       measured indicators of recreational water quality are predictive of swimming associated
       gastrointestinal illness. Environmental Health Perspectives 114: 24-28.
                                             25

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                                                                                   Method A
18.0  Acronyms


AACT     comparative cycle threshold calculation method
AF       amplification factor
BHIA     brain heart infusion agar
BHIB     brain heart infusion broth
BSA      bovine serum albumin
CPU      colony forming units
DNA     deoxyribonucleic acid
EDTA    ethylenediaminetetraacetic acid
IsrRNA   large subunit ribosomal RNA
NTC      no template control
PBS      phosphate buffered saline
PCR      polymerase chain reaction
qPCR     quantitative polymerase chain reaction
SPC      sample processing control
TNTC    too numerous to count
UV       ultraviolet (light)
                                            26

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                                                 Method A
                  Appendix A:
ABI 7900 and ABI 7500 Sequence Detector Operation
                      27

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                                                                                    Method A
Appendix A - ABI 7900 and ABI 7500 (non-Fast) Sequence Detector
Operation

1.0    ABI 7900 Sequence Detector Operation
       1.0.1   Turn on the ABI Model 7900 sequencer and then the computer.  Launch the SDS 2.2.2
              software program by double clicking on its icon on the computer desktop or from the
              Computer Programs menu. The computer will establish communication with the 7900
              instrument and if the connection is successful, the software will display the Connected
              icon in the status bar when a plate document is opened.
       1.0.2   Under File menu, select New.
       1.0.3   In resulting New Document window that appears, change container selection from 384
              well clear plate to 96 well clear plate using drop down menu. Accept default selections
              of Absolute Quantification and Blank Template.  Click OK to display a new plate
              document.
       1.0.4   Click, hold and drag mouse over all PCR reaction tray wells containing samples in upper
              left window. Selected wells will be outlined with a bold line and their position numbers
              should appear in the results table in the lower left window. To unselect wells, repeat
              above process while holding down control key.
       1.0.5   Above right hand window, click on Setup tab.
       1.0.6   Click on Add Detector button at the bottom of the setup screen. Note: Before any
              analyses are performed, a specific detector for the method must be created. To do this go
              to step 1.6.1. Once the detector has been  created, go to step 1.7.
       1.0.7   Click on New in the pop-up window that appears. Another pop-up window will appears.
              Under Name, type in a name for the detector that will be used by this method (e.g.,
              "Method  1600").  Under Group select Default. Under Reporter select FAM. Under
              Quencher select TAMRA. Click on OK to close second pop-up window. This step only
              needs to be performed before the initial analysis run of the method.  The detector that is
              named is  selected in all subsequent analysis runs as indicated in step 1.7)
       1.0.8   In pop-up window that was opened in step 1.6, select the desired detector under Names
              menu (e.g., Method 1600) and click on Copy to Plate Document button.  Click on Done
              button to  return to setup screen.
       1.0.9   Click on Use box next to FAM detector in right hand window. This box should become
              marked with an X. Name and color code for FAM detector should appear in each of the
              selected well positions in the upper left window and a data column for this detector should
              be created for each of the selected well positions in the results table in the lower left
              window.
       1.0.10 Click on Instrument tab right hand window.
       1.0.11  In instrument screen, change sample volume to 25 uL and choose 9600 emulation.
       1.0.12 Still in instrument screen, click on Connect, then click on Open/Close button in lower
              right hand "Real Time" window to open PCR reaction tray holder door on instrument.
       1.0.13 Insert PCR reaction tray with prepared reactions in holder.
       1.0.14 Click on Open/Close button to close PCR reaction tray holder door on instrument.
       1.0.15 Click on Start button in lower right hand "Real Time" window to start thermal cycling in
              instrument.
                                            A-l

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                                                                                       Method A


       1.0.16 Name run file at prompt.
       1.0.17 At termination of the run, instrument-calculated cycle threshold values should
              automatically appear for each well position and detector entry in the lower left hand
              results table window.
       1.0.18 At termination of the run success complete, choose Analysis Settings from the toolbar.  In
              that box enter a value for the Manual Ct Threshold (see  1.18).  Click on OK.  Click on
              Analyze from the toolbar. You should see Ct values in the Results Table.
       1.0.19 The instrument-selected threshold line is indicated by the bold red line on the plot and the
              value is listed below the window.  This can be manually adjusted by either click-hold and
              dragging the line up or down or entering new values below. Note: based on results thus
              far with the instrument, the threshold value can be adjusted from the default value of 0.2 to
              0.03, however, this should be done only if the threshold line remains above the
              background values (seen before the growth curves) for all of the  samples.
       1.0.20 Calculated CT values for each of the sample tray positions in the  lower left hand "Results
              Table" will automatically be updated following adjustments of the threshold line. Once
              the threshold is adjusted to the desired level, select "Print Report" under the "File" menu.
              Check or uncheck desired report items by clicking on their associated  boxes and the click
              on "Print" button. Note: Minimum report should have both detector boxes, i.e., "FAM"
              checked which will show CT values for all selected tray positions for this detector.
       1.0.21 Export data by clicking on File from the toolbar. From the drop down menu choose
              Export. In the box you will see Look in: and here you choose a directory to send the
              exported file too.  Click on Export.  Save changes to document? will  appear, click on
              Yes. Click OK.
1.1     ABI 7500 (non-Fast) Sequence  Detector Operation
       1.1.1   Turn on the ABI Model 7500 sequencer and then the computer.  Launch the software
              program by double clicking on its icon on the computer desktop or from the Computer
              Programs menu. The computer will establish communication with the  7500 instrument.
              See "How to Set Up a New Experiment Using the ABI  7500" for screen shots.
       1.1.2  Click on either the New Experiment or Advanced Setup button to create a new
              experiment, which will  pull up the Experiment Menu.
       1.1.3  From the Setup menu, select Experimental Properties to select the experiment type and
              give the experiment a name. Enter the experiment name in the asterisked box.
              1.1.3.1     Click on 7500 (96 Wells) to select the instrument type. Note: This protocol is
                         not designed for the 7500 Fast.
              1.1.3.2    Scroll down to access more experiment properties options. Click on
                         Quantitation - Standard Curve to select the experiment type
              1.1.3.3    Click on TaqMan® Reagents to select the reagents used.
       1.1.4  From the Setup menu, select Plate Setup. Click on the Define Targets and Samples tab
              to define the reporter-quencher dye for each target and also to enter the sample
              identifications (e.g., Ent 5X).
              1.1.4.1     Click on Add New Target and enter the name of the target. Under the
                         Reporter heading, click on the drop down menu to select the reporter dye
                         FAM.  Under the Quencher heading,  click on the drop down menu to select
                         TAMRA as the quencher.
                                              A-2

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                                                                                Method A


       1.1.4.2    Repeat the process in Section 1.1.4.1 to add more than one target, e.g., Sketa.
       1.1.4.3    In the Define Samples section, click on Add New Sample and enter the
                  sample name in the Sample 1 box.
       1.1.4.4    Click on the Assign Targets and Sample tab to assign the Target, sample ID
                  and sample type to the wells.
                  1.1.4.5    Drag the mouse over the desired cells to assign the Target, Task
                             and Sample.
                  1.1.4.6    While the cells are highlighted, in the Assign target(s) to the
                             selected wells section, check the box under Assign for the
                             appropriate Target, then under Task, select U for unknown, S for
                             standard or N for negative control.
                  1.1.4.7    In the Assign sample(s) to the selected wells section, check the
                             box under Assign to label the highlighted cells as Sample 1 (e.g.).
       1.1.4.8    Repeat the process in Section 1.1.4.4, dragging the mouse over the appropriate
                  cells, and then assigning them as Unknowns, Standards or Negative Controls,
                  as appropriate. Note that for the Standards, in the Assign target(s) to the
                  selected wells section, if there are 4 different values, each cell will need to be
                  highlighted separately, and a quantity (e.g. 40000.0) typed in the Quantity
                  box.
       1.1.4.9    Click on Print Report at the top of the screen to print a plate  layout for
                  loading master mix and sample extracts.
                  1.1.4.9.1   Select Plate Layout option by clicking on the box next to it.
                  1.1.4.9.2   Click Print Report to print the plate layout.
1.1.5  From the Setup menu, select Run Method to set up the thermo cycling profile.
       1.1.5.1    In the Graphical View tab, change the Reaction Volume Per Well from the
                  default 50|JL to 25|JL by typing in 25.
       1.1.5.2    Under Cycling Stage section, change the Number of Cycles to 45.
       1.1.5.3    Check that the default settings of Temperature and Time for the two Holding
                  Stages and the Cycling Stage are correct. Specifically, these should be:
                  Holding Stage 1: 50.0°C for 2:00 minutes, Holding Stage 2: 95.0°C for 10:00
                  minutes, and Cycling Stage: 95.0°C for 0:15 seconds.
       1.1.5.4    The second step of the Cycling Stage is defaulted at 60.0°C for 1 minute -
                  change the time to 2:00 minutes.
       1.1.5.5    Click on Save at the top of the screen to  save the run before actually running
                  the experiment.
       1.1.5.6    The Save screen will open so that you may select the folder to save the Run
                  Data File.  Type in the Experiment Name (if you did not already do so at the
                  beginning of the Experiment Setup) and  click on Save. If you had previously
                  typed in an Experiment Name and there is no change, click on Save.
1.1.6  From the Experiment menu, select Run to monitor the run in real time.
       1.1.6.1    The Run Status screen will open - click on Start Run. When the run has
                  successfully started, the Start Run button will turn change from green to red.
                                       A-3

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                                                                                 Method A


1.1.7  When the run has completed, from the Setup  menu, select Analysis to export your
       results.  See "How to Export Results from the ABI 7500 Software" for screen shots.
       1.1.7.1     The Analysis Settings for Experiment name screen will open.
       1.1.7.2    Under the CT Settings tab, click on the Target desired to be set from Default
                  to Manual Threshold setting (generally, this would be the Ent).
       1.1.7.3    In the CT Settings for ENT section, uncheck the boxes next to Use Default
                  Settings, and Automatic Threshold.  Enter the desired Threshold (e.g.,
                  0.025).  If more than one target is present, highlight the next target (e.g.,
                  Sketa) and repeat this step.
       1.1.7.4    Click on Apply Analysis Settings to save the changes.
1.1.8  Click on Export at the top of the screen to save the experiment results data and to save the
       selected plots required in the report.  Note that the threshold value will have changed on
       the Amplification curve graphic.
       1.1.8.1     The Export Data screen will open. In the Select data to export section, check
                  all of the boxes (i.e.  Sample Setup, Raw Data, Amplification Data, Results,
                  and Multicomponent Data).
       1.1.8.2    For Select one file or separate files, select One file to export all the data into
                  one file with multiple tabs.
       1.1.8.3    For Export File Name, enter the name of the Experimental data file to be
                  exported, and for File Type, choose *.xls.
       1.1.8.4    For Export File Location, click on Browse to select the folder in which you
                  wish to  export your file.
       1.1.8.5    Click on Start Export. When this is completed, an Export Completed screen
                  will open - click on Close Export Tool to complete this task.
1.1.9  How to interpret your results.  See "How to Interpret Results from the  ABI 7500" for
       screen shots.
       1.1.9.1     After exporting your data, from the Experiment menu, select Analysis.
                  1.1.9.1.1   From the Analysis menu, select Amplification Plot to view the
                             results of the selected  samples at different plot settings..
                  1.1.9.2    Drag the mouse over the desired cells to select the samples to be
                             plotted in the amplification plot.
                  1.1.9.3    In the Amplification Plot section, in the Plot Settings tab, select
                             the plot type (from the drop down menu) and the graph type (from
                             the drop  down menu).
                  1.1.9.4    If the plot requires the display of the Threshold and Baseline, in
                             the Options tab, check the boxes next to Threshold and
                             Baseline. If you want to see the results in tabular format, click on
                             View Well Table, and scroll down or sideways for more samples
                             and analysis parameters.
       1.1.9.5    For the  Standard Curve, select Standard Curve from the Analysis menu to
                  view the results of the same sample (assuming they have the same target) and
                  standards in the plot.
                                       A-4

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                                                                                 Method A


                  1.1.9.6    In the Plot Settings tab, click the drop down menu arrow beside
                             Target to select a different target (if the standards were analyzed
                             in more than one target), and click the drop down menu arrow
                             beside Plot Color to change the plot color.
                  1.1.9.7    The parameter display below the plot (/'.e.  Target, Slope, Y-
                             Inter(cept), R2, and Eff% (percent efficiency) is useful for data
                             analysis.
       1.1.9.8    For Multicomponent plots, click on Multicomponent  Plot from the Analysis
                  menu to view the variation in the fluorescence of the dyes used in the
                  experiment over the ascending repeat of the 45 thermo cycles based on the
                  wells, target, or dye.
                  1.1.9.9    Click on the drop down menu arrow next to Plot Color in the
                             Plot Settings tab to select the parameter for the basis of the graph
                             (e.g., well, target, or dye).
       1.1.9.10   For raw data plots, select Raw Data Plot from the Analysis  menu to view the
                  variation in the emission of fluorescence of the dyes in different filters present
                  over the ascending repeat of the 45 thermo cycles.
                  1.1.9.11   In the Options tab, drag the pointer on the cycle scale to the
                             desired cycle number to view the fluorescence variation through
                             filters of the samples at that cycle.
       1.1.9.12   For quality controls, click on QC Summary from the Analysis  menu to view
                  the analysis summary  of the samples.
       1.1.9.13   To view all the plots, click on Multiple Plots View from the Analysis menu
                  to see all of the plots for the samples in a single window.  Each plot will have
                  its own drop down menu as in Sections  1.1.12-1.1.15.
1.1.10 To print the report, click on Print Report at the top of the screen.
       1.1.10.1   Check all of the boxes (/'. e., Experimental Summary, Results Summary, Plate
                  Layout, Amplification Plot (3 boxes), Standard Curves, Results Table, and
                  QC Summary).
       1.1.10.2   Click on Print Report at the bottom of the screen.
                                       A-5

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             How to Set Up a New Experiment Using the ABI 7500
 7500 Software v2.0.1
File Edit Instrument  Analysis  Too
03 New Experimentl' Jj Open... • -          &
                                                                  Analyze Experiment
                                     Click either button to
                                     create new experiment
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  start

-------
  7500 Software v2.0.1
File  Edit  Instrument Analysis  Tools  Help
   New Experiment - ,_j Open... td Save- Jj Close  ^Export...-  ^ Print Report...
   Experiment Menu«
     Setup
    Experiment Properties
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    Run Method
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     aterials List
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Experiment:  Untitled Type: Standard Curve Reagents: TaqMan® Reagents
                          Experiment Properties
       Her an experiment name, select the i
     PCR reactions and instrument run.
 1. Click "Experiment Properties" to
select the experiment type and give
           an experiment name
  How do you want to identify this experiment?
   * Experiment Name:  j Untitled

   Barcode (Optional):

   User Name (Optional)^

   Comments (Optic
                           WhLh instrument are you using to run the experiment?
             7600 (96 Wells)
        7500 Fast (96 Wells)
                           Set up, run, and analyze an experiment using a 4- or 5-color, 96-well system.
      2.  Enter the
      at type of experiment do you want to set up?
  Experiment Name   p
        Quantitation - Standard Curve
  Quantitation - Relative Standard Cur,
Quantitation - Comparative CT (AACi
                                     Melt Curve
                                                                      Presence/Absence
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  7500 Software v2.0.1
Flip  I—Hit In^tri impnt  i i ril • ••- i •"  Tnnl<;
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START RUN
                      Expe...  NRSA Batch 1 ENT 03 ...  Standard Cur Reag...  TaqMan® Reagen
                          Experiment Properties
                           Enter an experiment name, select the instrument type, select the type of experiment to setup, then select materials and methods fort
                           PCR reactions and instrument run.
                        How do you want to identify this experiment?
                         * Experiment Name:

                         Barcode (Optional):

                         User Name (Optional):

                         Comments (Optional):
                                           NRSA Batch 1 ENT 032310|
                                      7500 (96 Wells)
                                                               7500 Fast (96 Wellsl
                               p, run, and analyze an experiment using a 4- or 5-color, SB-well system.
                               / Quantitation - Standard Curve
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                                                         Quantitation - Relative Standard Curve     Quantitation - Comparative CT (AACi
                                                             Scroll  down for more
                                                             experiment properties
                                                             options
                                                                                               resence/Absence
                                                                                                        Disconnected

-------
  7500 Software v2.0.1
File   Edit  Instrument  Analysis  Tools  Help
   New Experiment -  _j" Open...  ^| Save- uS  Close  ^Export...- £  Print Report...
    Experiment Menu«
      Setup
     Experiment Properties
     Plate Setup
     Rim Method
     Reaction Setup
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      Run
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Experiment:  Untitled Type: Standard Curve  Reagents: TaqMan® Reagents
                             Experiment Properties
                               Which instrument are you using to run the experiment?
START RUM
                                        S 7500 (96 Wells)
                                              7500 Fast (96 Wells i
                               Set up, run, and analyze an experiment using a 4- or 5-color, 96-well system.
                               What type of experiment do you want to set up?
                                   S Quantitation - Standard Curve
                                       Ouantitation - Relative standard Curve      Quantitation - Comparative CT (AACi
                                           Melt C-uu-e
                                                                                 Presence/Absen
                               Use standards to determine the absolute quantity of target nucleic acid sequence in samples.
   Which reagents do you want to use to detect the target sequence':
                                        TaqMan® Reagents
                                            SYBR® Green Reagents
    Other
                               The PCR reactions contain primers designed to amplify the target sequence and a TaqMan® probe designed to detect amplification of th
                               target sequence.
   Click to select
   experiment type
     iich ramp speed do you want to use in the instrument run?
                                (standard (~ 2 hours to complete a run)
                                                                                                                                  v
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-------
  7500 Software v2.0.1
File  Edit  Instrument  Analysis  Tools  Help
   New Experiment - _j" Open...  ^| Save- uS Close   ^Export...- £ Print Report...
    Experiment Menu«
     Setup
     Experiment Properties
     Plate Setup
     Rim Method
     Reaction Setup
       erials List
     Run
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Experiment: Untitled Type: Standard Curve  Reagents: TaqMan® Reagents
                            Experiment Properties
                              Which instrument are you using to run the experiment?
START RUM
                                       S 7500 (96 Wells)
                                            7500 Fast (96 Wells i
                              Set up, run, and analyze an experiment using a 4- or 5-color, 96-well system.
                              What type of experiment do you want to set up?
                                   Quantitation - Standard Curve
                                      Ouantitation - Relative standard Curve     Quantitation - Comparative CT (AACi
                                         Melt C-uu-e
                                                                              Presence/Absen
                              Use standards to determine the absolute quantity of target nucleic acid sequence in samples.
   Which reagents do you want to use to detect the target sequence':
                                       TaqMan® Reagents
                                           SYBR® Green Reagents
    Other
                              The PCR reactions contain primers designed to amplify the target sequence and a TaqMan® probe designed to detect amplification of th
                              target sequence.
   Click on TaqMan® Reagents to
        select the reagents  used
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                                                          11 Microsoft P.,,     .  75005oftw.

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  7500 Software v2.0.1
File  Edit Instrument Analysis Tools  Help

OjT] New Experiment - Jj Open... ^J Save" ;Jj' Close  ^Export...- ^ Print Report...
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                                       START RUM
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               •^^^           I	
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                                                                                     c...

                          Define Biological Replicate Groups
                         IJ Instructions: For each biological replicate group in the reaction plate, click Add Biological Group, then define the biological group.
                           Add Biological Group I Delete Biological OIOLI|J
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                                                                                               | Assign Targets and Samples
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Experiment: Untitled Type: Standard Curve Reagents: TaqMan® Reagents
                                    START RUM
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                                                                                         Assign Targets and Samples
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-------
  7500 Software v2.0.1
File   Edit  Instrument  Analvsis  Tools   Helo
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                                                                                                             START RUM
                           Define Targets and Samples |   Assign Targets and Samples
                                Instructions:  Define the targets to quantify and the samples to test in the reaction plate.
                              Define Targets
                                                                                 Define Samples
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per target DMA (ENT, SKETA)


                                                                                                                 Assign Targets and Samples

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-------
  7500 Software v2.0.1
File  Edit  Instrument Analvsis  Tools  Helo
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                                                                V 7500 Software.
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-------
  7500 Software v2.0.1
File  Edit  Instrument  Analysis  Tools  Help
   New Experiment - _J Open...  ^| Save- L3  Close  ^Export...-  £  Print Report...
    Experiment Menu«
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                                                                     START RUN
   Define
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	•^^^^»^^^^^^^^^^^^™^^^^^^^^^^^^^^^^^J=
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  7500 Software v2.0.1
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        Experime...  NRSA Batch!  ENT03231C Ty...  Standard Curve Reagen... TaqMan® Reagents
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-------
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File  Edit  Instrument  Analysis  Tools  Help
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File  Edit Instrument  Analysis  Tools  Help
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To designate standards,
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                                                                        START RUM
                                    es
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-------
  7500 Software v2.0.1
File  Edit Instrument  Analysis Tools  Help
      Type  in a Quantity for each
      standard  - if there are 4
      different values, highlight
      each  cell  independently and
      fill in  the quantity
                                                         Print Report...
                                    Standard Curve Reagen... TaqMan® Reagents
                                                        START RUM
                                   s and Samples
                                   Standards."
                                   st(s), select"U" (Unknown) as the taskfor each target assignment, then assign a sample.
                                   n target(s), then select "N" (Negative Control) as the task for each target assignment.
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        sign sample(s) of selected well(s) to biological group.
                                             View Plate Layout 1  View Well Table
                           SelectWellsWith:
                                                                                    -Select Item- v
                                                                                -Select Item- v
                                                                 Show in Wells T
                                                                  View Legend
                                                             2
                                                          ~5~ampie i
                                                 ENT5X    S3ENT5X
                                                                                                 4
                                                                                               sampler
                                                               5
                                                            iampie I
                                                                                     ENTSX
                                                   ENT5X   |T|ENT5X
                                                                 Sample 1     Sample 1     Sample 1     Sample 1    Sample 1
                                                                 ISKETASX  QSKETASX  EJSKETASX  DSKETASX  HSKETASX
                                                                D ENT5X
                                                                4E4
                                                                                                                     *
                                                                                                                     a
                                             Wells: lit 10 Unknown f~| 4 Standard [J 0 Negative Control
                                                                                                                82 Empty
       | E Untitled x
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-------
  7500 Software v2.0.1
File  Edit  Instrument  Analysis  Tools  Help
   New Experiment -  \3 Open...  id Save- Jj  close  ^*> Export...
    Experiment Menu«
     Setup
    Experiment Properties
    Plate Setup
    Run Method
    Reaction Setup
       erials List
     Run
     Analysis
  Home  E Urrtitled x
   start
                             4i Print Report...
Ex...  NRSA2009 Batch34 ENTC  ... StanoS^d Cu Rea...  TaqMan® Reager
                                                    START RUM
   Define Targets and
             To set up
             To set up
    Instructions: assign a
             To set u
2. Click on "Print Report" to print a plate
layout for loading master mix and sample
extracts
nt, then

in target
             assignment.
                           Assign target(s) to the selected wells.
                            Assign
             Target

             Entero
  Task
                                     Sketa
                                  | Mixed [iJ Unknown |_J Standard | J Negative (
                                Define and Set Up Standards
Assign sample(s) to the selected wells.

Assign

H
B
Sample
Cal-99
Cal-100
View Plate Layout T View Well Table
Select Wells With:
pH Show in Wells...


A
B
C
D
E
F
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1 2 3
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                                        7500 Soft ware v2.0.1

-------
  7500 Software v2.0.1
File  Edit  Instrurnpnt  Analvsis  Tools  HP|Q
I]  New Experiment - ._J  Open...
                                 Save- -J}  Close   ^Export..."  ^  Print Report...
    Experimer
                 Print Report
      Setup
     Experiment Pr
     Plate Setup
     Run Method
     Reaction Setii)
      aterials List
                 Q  Select data for the report. Click"Pr


                  D Experiment Summary


                  ~] Results Summary
      Run
      Analysis
                             1.  Select "Plate  Layout" option  by
                             clicking in the  box next to  it
                                               dev), CT (mean) and CT (std dev).
                                               An illustration of the wells in the reaction plate. Displays the contents assigned to each well.
                  D Amplification Plot (ARn vs. Cycle)  Data collected during the cycling or amplification stage. Displays baseline-corrected
                                               normalized reporter (ARn) plotted against cycle number.
                  D Amplification Plot (Rn vs. Cycle)   Data collected during the cycling or amplification stage. Displays normalized reporter (Rn)
                                               plotted against cycle number.
                  D Amplification Plot (Cr vs. Well)    Data collected during the cycling or amplification stage. Displays CT plotted against well
                                               number.
                                               The best fit line using CT values from the standard reactions plotted against standard
                                               quantities.
                                               Atable of experiment results for each well, including sample, target, task, quantity, ARn and CT.
| Standard Curves

| Results Table (By Well)

| QC Summary
                                               Atable of flags applied to wells in the experin'
                                               occurrence.and a list of flagged wells.

                   Print Preview
                                                                                   2. Click  "Print  Report"
                                                                                   to  print the  plate
                                                                                   layout.
                                                                                                                    Cancel
                                                                                                       ignment, then

                                                                                                       for each target
                                                                                                                            tern- v
                                                                                                                             10   11   12
                                                                                                                             Control
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-------
  7500 Software v2.0.1
File  Edit  Instrument  Analysis  Tools  Help
New Experiment - _j  Open...
                              Save- L3 Close   ^Export...-  ^  Print Report...
    Experiment Menu«
     Setup
     Experiment Properties
     Plate Setup
     Run Method
     Reaction Setup
     Materials List
     Run
     Analysis
        IE3 Urrtitled x
                        Expe...  NRSA Batch 1  ENT03 ...  Standard Cur  Reag... TaqMan® Reagen
                                                                            START RUM
                         Select  "Run  Method"  to set
                         up the  thermo cycling profile
                                                                             md Samples
                                               dards."
                                               selecf'U" (Unknown) as the taskfor each target assignment, then
Instructions:  assign a sample
           To setup negative controls: Select wells, assign target(s), then select "N" (Negative Control) asthetaskfor each target
           assignment.
                            t(s) to the selected wells.
Target
ENT5X
SKETA5X
Tas

k
a
a

n
m

a
a
i

Quantity
1DDJ


                            ed Q] Unknown [^ Standard |_J Negative Control
                            and Set Up Standards
ble(s) to the selected wells.





Sample
Sample 1
Sample 2

:A-
V
                                                                         View Plate Layout |  View Well Table

                                                                              Select Wells With
                                                                                               -SelectItem- v
                                                                              -SelectItem- v
                                                                                Show in Wells...
                                                                                           nlf View Legend
                                                                             sample i
                                                                            IENTSX
                                                                                          sample '
                                                                                                     ENT5X
                                                                                 b a m p i e i

                                                                               EJ ENT5X
                                                                             Sample 1     Sample 1     Sample 1     Sample 1     Sam

                                                                           Q]SKETA5X   OJSKETA5X  0SKETA5X  01SKETA5X  0 SHE
                                                                            Wells: 0] 10 Unknown [~] 4 Standard Q 0 Negative Control   82 E
                                                                                                                 Disconnected

-------
 7500 Software v2.0.1
File Edit Instrument Analysis  Tools  Help
IT] New Experiment - _j" Open...
                     Save- ^3 Close  ^Export...- ^ Print Report...
     Experime...  NRSA Batch! ENT 03231C Ty...  Standard Curve Reagen... TaqMan® Reagents
                                                                            START RUM
       Q Review the reaction volume and the thermal profil

       Graphical View 1  Tabu I ar View^^
       Reaction Volume Per Well
                        25
                                   1.  Change the Reaction Volume Per
                                   Well from the default of 50uL to 25uL
                            D Expert Mode
                                                                              from the library.
         Add Stage T  Add Step T  Delete Selected  Undo "Set Hold Time"             i Collect Data T   Open Run
                                                                          i Method
               Holding Stage
                                Holding Stage
      2. Change the Number of Cycles to 45
Cycling Stage
                                                      Number of Cycles: 45  0
                                                        i i bname Auiouena
3. Confirm that the default Temperature
and Time settings in both Holding
Stages and in step 1 of the Cycling
Stage are  as displayed - if  not, reset
them
                                                                                          v
                                             Delta Off
4. In the data collection step,
change the timeframe from
the default 1  minute to 2
minutes

-------
 7500 Software v2.0.1
File Edit  Instrument Analysis  Tools  Help
  New Experiment •» _/' Open.
   Experiment Menu«
    Setup
    Experiment Properlie
    Plate Setup
     n Metlio'l
    Reaction S"
    Materials Li
    Run
    Analysis
  Home S3 Unfilled x
  start
                       1. Click to save the run
                       before starting the run
                                                  sagen
                                                        START RUN
                     Save inl
                  My Recent
                  Documents
                   Desktop

        3 Comparative Ct Example.eds
          Genotyping Example.eds
        31 Presence Absence Example.eds
          Relative Standard Curve Example.eds
          : Standard Curve Example.eds
                   Personal
                  Documents
  9_\
My Computer
                   *
                  My Network
                   Places
          experiments
                              \
                          2. Select the folder for
                          saving the Run Data file
        File name:
Files of type:  Experiment Document Single files reds)
                                                            Save
                                                            Cancel
                          <^
                      - Legend
                                                                  ethod or select a run
                                                                                    a T i
                                                             6u.O°C

                                                             02:00
                          Dal
           3. Enter the experiment name if not entered at the
           beginning of the experiment setup and click "Save"
           or if already have the appropriate experiment name,
           without making  any changes click "Save"
                  %, 75...   teTD.
                                                                                             ted

-------
 7500 Software v2.0.1
File  Edit  Instrument  Analysis  Tools  Help
New Experiment -  _j Open...  iJ Save-
Close
                                           Export... - £ Print Report...
   Experiment Mem
                     Click "Run" to monitor the run in real-time
     Setup
     Run
      ipliflCiTtJOII Plot
    Temperature Plot
    Rim Method
      ification Settings
H-Home \\^\Untitled x
                                               s: TaqMan® Reagents
                                            Instrument Status
                                                                                             Enable Notifications
        Click to start the run.  The
        green box will turn red when
        the run  has been started
        successfully
                                10

                                1 •

                               0.1

                          c    0.01 '
                          a*
                          ^   0.001

                             0.0001

                            0.00001 J

                            0.000001
                                    Amplification Plot
                                  2 4 6 a 10 12 U 16 18 30 22 24 39 28 30 32 3* 38
                                                Cycle
                         • A   B   C   D

                          E • F BO  • H
                                                                                  ut
                                                                                     - Select Item- v
                                                                                              - Select Item-  v
                                                                                     SFJJI View Leg end
                                       1
                                     Samp... Samp... [3 Ta
                                       |Ta.. 01 Ta.. 1
                                     Samp... Samp... |~] Ta-i [7] Ta..
                                     Samp... Samp... g Ta [~] ja..
                                       lTa.. EOla.. 1    1
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                                          '* 7500Softw...    / iPP BJ

-------
                  How to Export Results from  the ABI 7500 Software
 7500 Software v2.0.1
File  Edit  Instrument  Analysis  Tools Help
 Tl New Experiment -  ,_3  Open... J Save - iJj  Close  ^Export...- ^ Print Report..
   Experiment Menu«
     Setup
     Run
   " Analysis
  NRSA Batch 34 testrur ...Standard C  Rea... TaqMan® Reagt
                                                        Analysis Settings
                       Amplification Plot
                                         <  View Plate Layout | View We 11 Table
Plot Settings
"'-^•ifnr'lm-
Click on the "Analysis" tab in the Experiment Menu
to access the "Analysis Settings"
                               10
                                1
                               0.1
                              0.01
                              O.Q01 •
                             0.0001
                            0.00001
                            0.000001
                           0.0000001
                                        Amplification Plot
        B.1M5I9
                                 O  2  A
                                         a id 12 14 10 1s
                                               Cycle
                                                       22 34 28
                         I A   B
                                C  D   E • F
                        fOptions ~\_
                                     Threshold:
                                              -IIK>
                                                                              3   4   5  6  7  8   9  10  11  12
                                                                    Wells: 0| 40 Unknown 0 16 Standard [TJ 0 Negative Control
                      Analysis Summan/: Total Wells in ... 96 Wells S... 56 Wells Omitted Man... 0 Wells Fla...1 4 Wells Omitted by Ana... 0 Samples ...8 Targets ...2
  Home H NRSA Batch 34...032310 eds.eds X
                                                                                                 Disconnected
 '/ start
                                   * 7500.
                                             Anal..,    s* mi
                                                                                10; 11

-------
  7500 Software v2.0.1
File  Edit  Instrumen
 rj New Experiment -
   Experiment
     Setup
1. To change the threshold setting from
Automatic to Manual, click on "Analysis
Settings"
                                                   Analysis Settings
ifir
     Run
r     Analysis
               | Analysis Settings for NRSA Batch 34 testrun 022310
    Standard Ciirvt
    Mutticomponei
    Raw Data Plot
    QC Summary
    Multiple Plots \
 CT Settings T Flag Settings     Advanced Settings
  Q  Review the default settings for
     different settings for a target, s

   Default CT Settings
  Default CT settings are used to calc

   Threshold: AUTO Baseline St
2. Under the "CT Settings" tab,
click on the Target desired to
be set from Default to Manual
Threshold setting
it Default Settings." To use
3 the settings that are display
                                                                                   .click "Edit Default Settings."
                  Select a Target
                 Tarnet
                              Threshnld
                                          HaSfiliOfi_Start
                                                             Fnrj
ENT
SKETA
AUTO
AUTO
AUTO
AUTO
AUTO
AUTO
                                                                   *
                                                         CT Settings for ENT

                                                        CT Settings to Use
                                                         . : Automatic Baseline

                                                          srlirn Start Cycle f 3 i I End
                                                           3. Uncheck the box next to
                                                           "Use Default Settings"
                Revert to Default Analysis Settings
                                                    Apply Analysis Settings
                                                                                                        1   12
                                                         Cancel i   tontrol
                       Analysis Summary: Total Wells in ...96  Wells S... 56 Wells Omitted Man... 0 Wells Fla... 14 Wells Omitted by Ana... 0 Samples ...8 Targets ...2
  Home 1H NRSA Batch 34...032310 eds.eds x
                                                                                                 Disconnected
                                l^-
                                             *  7500...   H3M...  '  .•; Anal...

-------
  7500 Software v2.0.1
File   Edit  Instrumpnt  Analvsis  Tools   HP!O
I] New Experiment - ,_j  Open...
                               Save '  uS Close  ^Export...- ^  Print Report...
    Experiment Menu«
      Setup
      Run
r      Analysis
                                NRSA Batch 34 testrur ...Standard C  Rea... TaqMan® Reage
                  I  Analysis Settings for NRSA Batch 34 testrun 022310
       •plificvition P
     Standard Curvt
     Mutticomponei
     Raw Data Plot
     QC Summary
     Multiple Plots \
                   CT Settings T  Flag Settings     Advanced Settings
                    Q  Review the default settings for analysis of targets in this experiment. To edit the default settings, click "Edit Default Settings." To use
                        different settings for a target, select the target from the table, deselect "Use Default Settings," then change the settings that are display

                     Default CT Settings
                    Default CT settings are used to calculate the CT for targets without custom settings. To edit the default settings, click "Edit Default Settings."
                      Threshold: AUTO Baseline Start Cycle: AUTO  Baseline End Cycle: AUTO  | Edit Default Settings |
                     Select a Target
                     Target           Threshold

                    ENT            AUTO
                    SKE
 Baseline Start

AUTO
 Baseline End

AUTO
                                                                                        CT Settings for ENT
                          Uncheck the  box  next to
                         "Automatic  Threshold" to
                         enter the desired threshold
CT SettlngstoUse: D UseDif aujifS el ngsj

    utomatic Threshold
                                                                                       Threshold  • .
                                     [7| Automatic Baseline

                                             •tart Cycle: F 3 ; I End C. I-
                    Revert to Default Analysis Settings
                                                                                  Apply Analysis Settings
                                                                                                                      Cancel
                                                                                                                               1   12
                                                                                                                               2 .
                                                                                                                               00 ,
                                                                            ;ontrol
                           Analysis Summary: Total Wells in ...96  Wells S... 56 Wells Omitted Man... 0 Wells Fla... 14 Wells Omitted by Ana... 0  Samples...8  Targets...2
   Home 1H NRSA Batch 34...032310 eds.eds
                                                                                                                       Disconnected
   start
                                         .
                                  •'••   I  ^ ••"•••

-------
  7500 Software v2.0.1
File  Edit  Instrument  Analvsis  Tools  Helo
I] New Experiment -
Open...
                            Save-  L3  Close
                                                   Export... "  ^ Print Report...
    Experiment Menu«
                              NRSA Batch 34 tastmr   Standard C  Raa   TanMan®
                                                                              Analyze
                                                                                                             Analysis Settings
          Analysis Settings for NRSA Batch 34 testrun 022310
'*•£:-
      R
Home
           CT Settings T  Flag Settings  |  Advanced Settings
            Q Review the default settings for analysis of targets in this experiment. To edit the default settings, click"Edit Default Settings." To use different
               settings for a target, select the target from the table, deselect "Use Default Settings," then change the settings that are displayed.

             Default CT Settings
            Default CT settings are used to calculate the Crfortargets without custom settings. To edit the default settings, click"Edit Default Settings."
             Threshold: AUTO  Baseline Start Cycle: AUTO  Baseline End Cycle: AUTO  |  Edit Default Settings
             Select a Target
            Target
                          Threshold
                       Baseline Start
                                                            Baseline End
ENT
SKETA
0.2
0.2
AUTO
AUTO
AUTO
AUTO
                                                                                CT Settings for the 2 Selected Targets
                                                                                  CT Settings to Use:  D Use Default Settings

                                                                                   D Automatic Threshold
                     Enter the  desired  Threshold.
                                                                                   Threshold: 0.025
                                                                                0 Automatic Baseline

                                                                                Baseline si.:
                                                                                                                               ntrol
                           Analysis Summary: Total Wells in ...96 Wells S... 56 Wells Omitted Man... 0 Wells Fla... 40 Wells Omitted by Ana... 0  Samples ...8  Targets... 1
           NRSA Batch 34...032310 eds.eds
                                                                                                                      Disconnected
   start     m *
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                                 *.i 7500

-------
  7500 Software v2.0.1
File  Edit  Instrument  Analvsis  Tools  HP!O
I]  New Experiment - >Jj  Open...
                                 Save ' uS  Close   ^Export...-  ^ Print Report...
    Experiment Menu«
      Setup
      Run
r      Analysis
                                 NRSA Batch 34 testrur ...Standard C Rea... TaqMan® Reage
                  I  Analysis Settings for NRSA Batch 34 testrun 022310
       i|>lifk
-------
  7500 Software v2.0.1
File  Edit  Instrument  Analysis  Tools  Help
   New Experiment-•  LJ  Open...  td Save-  ,_i  Close
                  Export..
                          1 Print Report...
   Experiment Menu«
     Setup
 '*;:
     Run
r     Analysis
      •plification Plot
    Standard Curve
    Miilticomponeirt Plot
    Raw Data Plot
    QC Summary
Click on  "Export" to save experiment results
data and to save the selected plots required
in the report
                                 10
                                          Amplification Plot
       1
     0.1
=    am \
*   0.001
   0.0001
   0.00001
  0.000001
         0,025
                                   2 4 e a 10 12 u ie ia 30 22 21 26
                                                  Cycle
                                                                             Show in Wei...
                                                                      Analysis Settings
                                                                  View Well Table
                                                                  ctltem- v
     -SelectItem- v
                                                               'Hi View Leg end
                                                                                                 9   10   11    12
                                                                          .-_
                                                                          13 ENT
                                                                          98.19
                                                                                                              Q ENT
                                                                                                              228....
 1121
El ENT El ENT Q ENT El ENT
23.78 63.45  400  34.99
    ^.—.  TLB-1231    1
El ENT 4E4   947 g El ENT
12.63 CT:...  _ ,  45.28
                                                                                               E| ENT ^E4  E3 ENT [3 ENT
                                                                                                         265.... 47.65
    Note that the threshold value has changed on the Amplification Plot
                           Options
                          Show: 0 Threshold — D Baseline Start: Well  Target
                                                                                                3042
                                                                                                    4fc3
                                                                                                           ENT
                                                                         Wells: H]40 Unknown [~~] 16 Standard [~]o Negative Control
                        Analysis Summary: Total Wells in ...96 Wells S... 56 Wells Omitted Man... 0 Wells Fla... 35 Wells Omitted by Ana... 0 Samples ...S  Targets ...1
  Home H NRSA Batch 34...032310 eds.eds x
                                          ir
                                                                             Disconnected
                                                                                                           '-  ,  11:16 AM

-------
  7500 Software v2.0.1
File   Edit  Instrument Analvsis  Tools  HP|Q
 3 New Experiment
    Experimen
      Setup
      Run
      Analysis
                                                             Check  the boxes next
                                                             to the desired results to
                  Q Select the type of data to export, selectwhetherto export one file or separatefifesj OVDOrt
                     Click "Customize Export" to change the export format and to select fields ts^xportl     H
                       Export Properties    Customize Export
                      1. Select data to export:
                   0 Raw Data
                   0 Amplification Data
0 Results
0 MulticomponentData
2. Select one file or separate files:
                      3. Enter export file properties:
                                                  One File
     Select to export all data in one file or in separate files for each data t/f
                       Export File Name:
                       Export File Location:
NRSA Batch 34 testrun 02231 0_data

File Type:
® rxls) v-

C:\Applied Biosystems\750Q\experiments
Browse
                         Open file(s) when export is complete
                   j Save current settings as the default
                                                                                Start Export | |  Cancel
                                                                                                   Dlel
                                                                                                    ectltem-
                                                                                                                            10  11  12
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                                                                                                                            r-i
                                                                                                                          Jegative Control
                            Analysis Summary:  Total Wells in ...96  Wells S... 56 Wells Omitted Man... 0  Wells Fla... 24 Wells Omitted by Ana... 0  Samples ...8  Targets ...2
   Home i 0 NRSA Batch 34...032310 eds.eds x
                                                                                                                         Disconnected
                                 ...-  |  ftl-^

-------
  7500 Software v2.0.1
File   Edit  Instrument  Analvsis  Tools  HP!O
 I] New Experiment -  & Open...  j Save- i_i  Close  ^Export...- ^  Print Report.
    Experimen
      Setup
      Run
     Analysis
                   Export Data
                 Q Select the type of data to export, select whetherto export one file or separate files, then enter exportfile properties. (Optional)
                    Click "Customize Export" to change the export format and to select fields to export. Click "Start Export' to export your data.
                                                                               Ible
                      Export Properties    Customize Export
                      1. Select data to export:
  0 Sample Setup

  0 Raw Data
  0 Amplification Data
From the  drop-down menu select
"One File"  to export all data into a
single  file with multiple tabs
                     2. Select one file or separate files
                     3. Enter export file properties:
                      Export File Name:

                      Export File Location:
          [Separate Files
                         Select to export all data in one file or in separate files for each data t/t
NRSA Batch 34 testrun 022310 data
                         File Type:
CWpplied Biosystems\75QO\experiments
                                    Browse
                        Open file(s) when export is complete
                  j Save current settings as the default
                                                            Start Export | | Cancel
                           Analysis Summary: Total Wells in ...96  Wells S... 56 Wells Omitted Man... 0  Wells Fla... 24 Wells Omitted by Ana... 0  Samples ...8  Targets ...2
   Home i 0 NRSA Batch 34...032310 eds.eds x
                                                                                                                     Disconnected
                                :..-   |  ftl-^

-------
  7500 Software v2.0.1
File  Edit   Instrurnpnt  Analvsis   Tools   HP!O
 I] New Experiment - \3 Open...  J Save ' u  Close   ^Export...'  ^ Print Report..
     Experimen
      Setup
      Run
      Analysis
                    Q Select the type of data to export, select whetherto export one file or separate files, then enter exportfile properties. (Optional)
                       Click "Customize Export" to change the export format and to select fields to export. Click "Start Export' to export your data.
Export Properties Customize Export
0 Sample Setup 0 Results
0 Raw Data 0 Multicor
1. Select data to export:
0 Amplification Data
2. Select one file or separate files: One File v Sete
3. Enter export file properties: S
£

Export File Name: I IJIii&l^HiMlliiamiilihhfcilMiBEl

nponentData

Enter the name of the
experiment data file to be
CU
eic^orfec


(File Type: 2s) (*X|s) vj
Export File Location: C:U\pplied Biosystems\750D\experiments Browse

D Open file(s) when export is complete
I >



                     j Save current settings as the default
Start Export  | | Cancel
                      Die
                      ectltem-  v
                                                                                                                                      J   10  11   12
                                                                                                                                         10.. n
                                                                                                                                           1
                                                                                                                                      i   en  m
                                                                                                                                       ..  4E3 "."
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                                                                                                                                       S«^H^
                                                                                                                                         1   Q..
                                                                                                                                      Negative Control
                               Analysis Summary:  Total Wells in ...96  Wells S... 56 Wells Omitted Man... 0  Wells Fla... 24 Wells Omitted by Ana... 0  Samples ...8  Targets ...2
   Home 10 NRSA Batch 34...032310 eds.eds x
                                                                                                                                     Disconnected
                                       ^   |  &»;

-------
  7500 Software v2.0.1
File   Edit  Instrument  Analvsis   Tools  HP!O
 rj New Experiment - \3  Open...  jj  Save- _j  close  ^ Export... -  g Print Report..
    Experimen
      Setup
                  Q Select the type of data to export, select whether to export one file or separate files, then enter exportfile properties. (Optional)
                     Click "Customize Export" to change the export format and to select fields to export. Click "Start Export' to export your data.
      Run
      Analysis
                      Export Properties    Customize Export
                      1. Select data to export:
          0 Sample Setup
          0 Raw Data
          0 Amplification Data
0 Results
0 MulticomponentData
                      2. Select c
                      3. Enteres
Select *.xls (Excel)  from the  "File Type"
drop-down menu
                               UIL nib (Ji
                                      ife files for each data t/t
                       Export File Name:
                       Export File Location:
       NRSA Batch 34 testrun 032310 data
       C:\Applied Biosystems\7500\experiments
                        Open file(s) when export is complete
                   j Save current settings as the default
                                                                      Start Export | |  Cancel
                                                                                         Die
                                                                                          ectltem- v
                                                                                                                         )   10  11  12
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                                                                                           1 i^'iaT
                                                                                                                         Negative Control
                            Analysis Summary: Total Wells in ...96 Wells S... 56 Wells Omitted Man... 0 Wells Fla... 24 Wells Omitted by Ana... 0  Samples ...8 Targets ...2
   Home 10 NRSA Batch 34...032310 eds.eds x
                                                                                                                        Disconnected
                                   ^   |  &»;

-------
  7500 Software v2.0.1
File  Edit  Instrument  Analvsis  Tools  HP|Q
 JT| New Experiment »  & Open...  j Save-  L3  Close  ^Export...-  ^  Print Report.
    Experimen
      Setup
      Run
      Analysis
                  Q Select the type of data to export, select whetherto export one file or separate files, then enter exportfile properties. (Optional)
                     Click "Customize Export" to change the export format and to select fields to export. Click "Start Export' to export your data.
                       Export Properties    Customize Export
                       1. Select data to export:
  0 Raw Data

  0 Amplification Data
0 Results

0 MulticomponentData
                      2. Select one file or separate files:  One File


                      3. Enter export file properties:
                       v  Select to export all data in one file or in separate files for each data tyi
                       Export File Name:

                       Export File Location:
NRSA Batch 34 testrun 022310  data
                                      File Type:
C:\Applied Biosystems\75QQ\experiments
                                                  Browse
                         Open file(s) when export is complete
                                             Click on "Browse" to select the
                                             folder / location  to export the File
                   j Save current settings as the default
                                                               Start Export | |  Cancel
                                                                                   Die
                                                                                    ectltem-
                                                                                                                           J   10  11   12
                                                              = 10.. m


                                                              ^   ^
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                                                                                   i   ri   nT-

                                                                                       ^ '=*
                                                                                      1   01.
                                                                                   i   rn   r-T-
                                                                                                                           Negative Control
                            Analysis Summary: Total Wells in ...96  Wells S... 56 Wells Omitted Man... 0  Wells Fla... 24 Wells Omitted by Ana... 0 Samples ...8  Targets ...2
   Home i 0 NRSA Batch 34...032310 eds.eds x
                                                                                                                          Disconnected
                                    ^   |  &»;

-------
  7500 Software v2.0.1
File   Edit  Instrument  Analvsis  Tools   HP!O
 I] New Experiment - &  Open...  jj Save-  i_i Close  ^Export...-  ^  Print Report.
    Experimen
      Setup
      Run
      Analysis
                  Q Select the type of data to export, select whetherto export one file or separate files, then enter exportfile properties. (Optional)
                     Click "Customize Export" to change the export format and to select fields to export. Click "Start Export' to export your data.
                      Export Properties    Customize Export
                      1. Select data to export:
0 Sample Setup
0 Raw Data
0 Amplification Data
0 Results
0 MulticomponentData
                      2. Select one file or separate files:  One File
                      3. Enter export file properties:
                    v   Select to export all data in one file or in separate files for each data tyt
                      Export File Name:
                      Export File Location:
NRSA Batch 34 testrun 03231 0_data

File Type:
® (*.xls) v-

C:\Applied Biosystems\7500\experiments
Browse
                        Open file(s) when export is complete
                                                         Click on "Start Export"
                                                         to export  the data to the
                                                         determined  location
                   j Save current settings as the default
                                                                               Die
                                                                               ectltem- v
                                                                                                                        )   10   11   12
                                                            =  10.. m
                                                            ^   ^
                                                            I  Cfl  m
                                                                                                                        i
                                                                                .. 4E3 "."
                                                                                  J?^^
                                                                               p  4E3 r^.
                                                                                  1 ^a^
                                                                                                                        Negative Control
                            Analysis Summary: Total Wells in ...96 Wells S... 56 Wells Omitted Man... 0  Wells Fla... 24 Wells Omitted by Ana... 0 Samples ...8 Targets ...2
   Home 10 NRSA Batch 34...032310 eds.eds x
   start
                                                                                                                       Disconnected
                                                          Micro...    / m E)

-------
  7500 Software v2.0.1
File  Edit Instrurnpnt Analysis  Tools  HP!O
3 New Experiment '  \3 Open...  j Save ~
                  Close
                                              Export. .   Q Print Report...
    Experimen
     Setup
     Run
                   Select the type of data to export, selectwhetherto export one file or separate files, then enter export file properties. (Optional)    ^
                   Click "Customize Export" to change the export format and to select fields to export. Click "Start Export' to export your data.
     Analysis
      ,|flifn alion F
    Standard Curv.
    Mutticomponei
    Raw Data Plot
    OC Summary
    Multiple Plots \
                    Expor
       A pop-up window "Export Completed" appears
       once the exporting of the  file is completed.
                    1. Select data to export:
                                    MulticomponentData
2. Select one file o

3. Enter export file (

Export File Name:

Export File Locatioi
                                 Export Completed
                                                                                         > fifes for eacft c^afa f//
Your file has been exported to :

C:\Applied Biosystems\7500\experiments\NRSA Batch 34 testrun 032310_data.xls


What do you want to do next?   _^^^^_^^^^
                                                 Export More Data
                                           Close Export Tool
                                                                                          Type:
                                                                                                (*.xls)
                                                                                                  Browse
                      Open file(s) when export is complete
                                               Click on "Close Export Tool" to
                                               close the export window once
                                               data file exporting  is completed.
                 ^1 Savs current settings as the default
                                                                       Start Export
                                                                                Cancel
                                                                                        Die
                                                                                                           ectltem-  v
                                                                                                           )   10  11  12
                                                                                                              10.. [— |
                                                                                                               i
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                                                                                        i  m i^..
                                                                                                           Negative Control
                         Analysis Summary:  Total Wells in ...96 Wells S... 56 Wells Omitted Man... 0 Wells Fla... 24 Wells Omitted by Ana... 0 Samples ...8 Targets ...2
       ll]NRSABatch34...032310eds.eds x
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-------
                        How to Interpret  Results  From the ABI 7500
  7500 Software v2.0.1
                                                                                          -  ff X
File  Edit  Instrument  Analysis  Tools  Help
03 New Experiment - J/ Open...
      Save-  j  Close  ^Export...-
                                                        Print Report...
    Experiment Menu«
     Setup
     Run
     Analysis
      ipliifjcatioii Plot
      ii id.ii (I Curve
     unicomponein Plot
    Raw Data Plot
    QC Summary
    Multiple Plots View
A
       Nl
                         Ar.plificatii
              Select "Amplification Plot" to view the results of

              the selected samples at different plot settings
                           Plot Settings
                           Plot Type: JARnvs Cycle  v| Graph Type: Log   v| Plot Co'1
                                          Amplification Plot
                             D.OOOD01 H
                                    2 i e a 10 is « -IB fa an 22 s« ae at ao 3Z3i SB aa *> «s 4«

                                                  Cycle
                          • A   B  C   D   E • F • G • H
                          Show: [3 Threshold — D Baseline Start: Well  Targets  v
select wens witn: |-select item - vi - select item- v
                                                                          [°~~;ShowinWel...
                                                                   i*|fi| View Leg end
                                                                            1   2   3   4   5  6   7   8   9   10  11  12
                                                       2 ^ m-• s-"Sp
                                                       ~i c 11.. 100 ,,,..
                                                                                                          98... 100
                                                                            75...
                                                                         Wells: [7j 40 Unknown |~^ 16 Standard |~~] 0 Negative Control
                        Analysis Summary: Total Wells in ... 96 Wells S... 56 Wells Omitted Man... 0 Wells Fla... 1 3 Wells Omitted by Ana... 0 Samples ...8  Targets ...2
  Home  E3 NRSA Batch 34...032310 eds.eds x
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-------
 7^00 Snftwam v? O 1
2. Select the
"Plot Type"
from the drop-
down  menu
    Run
r    Analysis
    Amplification Plot
    Standard Curve
    Mnlticomponent Plot
   Raw Data Plot
    OC Summary
   Multiple Plots View
                               Analysis Menu-Amplification Plot
Tools  Help
   Save - L3 Close
Export... - £j|  Pi
    NRSA Batch 34 testrur ...Star
3. From the "Graph Type"
drop down menu select either
Log or Linear
                                        ettings
                      Amplification Plot
                                        Graph Type: Log
                              1
   Plot Co —
                                      Amplification Plot
                                2 4 8 a 10 12 li 1fl 13 20 22 2i 26 23 X 32 3i 36 33 4J *2
                        1A  B  C   D   E • F • G • H
                        i diy«L. j i aiyei i *
-------
                              Analysis Menu-Amplification Plot
 7500 Software v2.0.1
File  Edit Instrument Analysis  Tools Help
  New Experiment - ,J/ Open...
   Experiment Menu«
    Setup
    Run
    Analysis
jti,
Select "View Well Table"  to view
the results in a tabular format
                      Amplification Plot
Plot Settings
                       Plot Type: [aRnvs Cycle v| Graph Type: [Log
                              Plot Co—
If the plot requires
the display of the
threshold and
baseline select by
checking the "USE"
boxes  in "Show"
next to Threshold
and Baseline
                                                        >
\&  '-
             Amplification Plot
    :oooi ' J . .—i—•—i—•—.—•—•—i—i—i—•—i—•—.—.—.—i—i—i
       2 i 6 a 1Q 12 W 1S 13 20 22 2i 26 iD JO i2 is 33 ia itl i2 i!
                    Cycle
                           B   C   D   E • F • G • H
                       Options
                                                         A
                       Show: 0 Threshold — Q Baseline Start: Well  Target^ v
                     Analysis Summary: Total Wells in ... 56 Wells
      |HNRSABatch34...032310eds.eds
                               Analysis Settings
                               ®
                                         View Plate
                   Layout
              View Well Table
                                           Select Wells With: - Select Item -
                                   -SelectItem- v
                                        Show in Ta..
                                                                         Group By
                                                                ndAII
                                                                                             -
            1
            2
            3
            4
            5
            6
            7
            3
            9
           10
           11
           12
           13
           14
           15
           16
           17
           18
           19
Well
 A1
 A2
 A3
 A4
 A5
 A6
 A7
 A8
 A9
 A10
 A11
 A12
 B1
 B2
 B3
 B4
 B5
 B6
 B7
                                                  Omit
D
D
P
n
D
D
P
P
n
n
n
                                                    n
                                                    n
                                                    n
                                                    n
 Sample...  Targel
LB-123    ENT
CAL-9925X  ENT
        ENT
GAL-1 DO 5x  SKETA
LB-123    ENT
CAL-9925X  ENT
        ENT
CAL-1 DO 5x  SKETA
537238    ENT
CAL-1 DO 25X ENT
        ENT
CAL-9825X  SKETA
                         Scroll down or sideways
                         for more samples and
                         analysis parameters
                               3...Q SpfrtfSfes
                           ...8 Targets ...2
                                                                                         Disconnected

-------
                                    Analysis Menu- Standard Curve
  7500 Software v2.0.1
File  Edit Instrument  Analysis  Tools Help
03 New Experiment - ,_3 Open...  td  Save ~ LJJ Close  ^Export...-  ^  Print Report...
    Experiment Menu«
    NRSA Batch 34 testrur   Standard C Rea   TaaMan® React
     Setup
     Run
     Analysis
     Amplification Plot
        ara Curve
    Miilticompoiient Plot
    Raw Data Plot
    QC Summary
    Multiple Plots View
Select "Standard Curve" to view the results of
the samples (if same target) and standards in  the
plot
                                      -rtlnqs a sine default
                                        Standard Curve
                            o
     17.5 •

     15.0

     12.5

     10.0

      7.6 •

      5.0
                                 1  2345 10 20 30  100 200   1000     10000     1000Q
                                                Quantity
                             Target: ENT Slope: -3.496 Y-Inter: 21.433 R_2: 0.963 Eff%: 93.222
                            Standard •Unknown   Unknown (Flagged)
                                      Analysis Settings
                                     w Well Table
                                                                                                 n - v
                                          -SelectItem-
                                                                        agend
                                                                             1   2  3
                                                                  5   6   7   8  9  10  11  12
                                                                         Wells: HI 40 Unknown [~116 Standard [~] 0 Negative Control
                        Analysis Summary  Total Wells in ...96  Wells S... 56 Wells Omitted Man... 0  Wells Fla... 1 3 Wells Omitted by Ana... 0 Samples ...8  Targets ...2
   Home  E3 NRSA Batch 34...032310 eds.eds
                                                                                                        Disconnected
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-------
                                Analysis Menu - Standard Curve

Click here to select a different Target (if the
standards were analyzed in  more than  one target)
or change the Plot Color
    Setup
    Run
r    Analysis
    Amplification Plot
     rinil.ir j	

                         I Standard • Unknown  Unknown (Flagged)
                                          View Plate Layout 1 View Well Table
                                             Select Wells With: - Select Item - v
                                                                  -SelectItem-
                                        p^'Show in Wei...
                                                        5*OJ]! View Legend
                                                                      1234567
                                                                      9  10 11  12
                                                                     75... i—i
                                                                   Wells: Ly 40 Unknown [J 16 Standard |J o Negative Control
                      Analysis Summary: Total Wells in ...96 Wells S... 56 Wells Omitted Man... 0 Wells Fla... 1 3 Wells Omitted by Ana... 0 Samples ...8 Targets ...2
  Home ; H NRSA Batch 34...032310 eds.eds x
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                             *, 7500 S..,   ^ Print Re.

-------
                           Analysis Menu - Multicomponent Plot
 7"iOO Snflwam v? O 1
Click on the "Plot Color" drop down menu to select the
parameter based on which the graph required to be plotted
    ixperiment Menu«
    Setup
'•I*
    Run
    Analysis
    Ainplifjcation Plot
     andarcl Curve
    Mutticomponent Plot
    Raw Data Pic.
    QC Summary
    Multiple Plots View
  NRSA Batch 34 testrur ...Standard C  Rea... TaqMan® Reagt
                 Analysis Settings
                     MulticomDonent Plot
Plot Settings \
                       Plot Color

                             Dye
      Well
      Target
                                        ?• 13II It
                               Multicomponent Plot
  1,100.000

  1,000,000 •

   900,000

   300,000

 S  700.000
 C
 S  600,000
 v>
 j|  500,000

 iZ  -TOO .000

   300.000

   200.000

	inn nnn
                                        View Plate Layout 1  View We 11 Table
Select Wells With: -Select Item- v
-SelectItem- v-
                                                                 Show in Wei...
                                                      [7] View Legend
Select "Multicomponent Plot" to view the variation in the
fluorescence of the wells, targets or dyes used over the
ascending repeat of the 45 thermo cycles
                                                                             16 Standard   o Negative Control
                    Analysis Summary: Total Wells in ...96 Wells S... 56 Wells Omitted Man... 0 Wells Fla...1 3 Wells Omitted by Ana... 0  Samples ...8  Targets ...2
  Home 03 NRSA Batch 34...032310 eds.eds x
                                                                                        Disconnected
                          yatri ...   f^ Google .
                              75005...   ^ Print R


-------
                             Analysis Menu - Raw Data Plot
Select "Raw Data Plot" to view the variation in the emission of
fluorescence of the dyes in different filters present over the
ascending repeat of the 45 thermo cycles
                                                       Analysis Settings
    Setup
'_*»*.=
    Run
    Analysis
   Ainplifjcatic n Plot
     andard' .urve
   Multicor Roneirt Plot
   Raw Data Plot
   QC Summary
   Multiple Plots View
                    Raw Data Plot
                                    View Plate Layout 1 View Well Table
                                       Select Wells With: -Select Item- v
                                  -SelectItem-
                                                              : Show in Wei...
                                                                        -r-
                                                 a View Legend
                                                              1234
                                                                11-
                                                                73... 100 *•
                                                             FTI  4E4
                                                          8  9  10  11 12
                                                               ID -' E ..
                                                               98... 100
                                                            m  63...
                                                                                         E3 - Q] .
                                     Drag the pointer on the
                                     cycle scale to the desired
                                     cycle number to view the
                                     variation in the fluorescence
                                     through filters of the
                                     samples at that cycle
                   Analysis Summary Total Wells in ... 96 Wells S... 56 Wells Omitted Man... 0 Wells Fla... 1 3 Wells Omitted by Ana... 0  Samples ...8 Targets ...2
  Home 03 NRSA Batch 34...032310 eds.eds
                                                                                    Disconnected
  start    as it
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-------
                                      Analysis Menu - QC  Summary
  7500 Software v2.0.1
File  Edit  Instrument  Analysis  Tools  Help
03 New Experiment -  ,3 Open...  d Save -  i3  Close  ^Export...- ^ Print Report...
    Experiment Menu«
     Setup
'*»*
     Run
    " Analysis
NRSA Batch 34 testrur  ...Standard C  Rea... TaqMan® Reagt
                          QC Summary
                            C Flag Summary ~\
Total ... 96
Wells...56
Processe... 56  Manually Omitte... 0
Flagged... 13  Analysis Omitte... 0
Targets... 2
Sample...8
                             Flag Details
                              Fl...   Name
                             AMP... Amplification in negative con..
                             BAD...
                             OFF...
                             HIG...
                             NO A..
                             NOI...
                             SPIKE
                             NOS...
                             ni IT
    Bad passive reference signal
    Fluorescence is offscale
    High standard deviation in re.
    No amplification
    Noise higherthan others in
    Noise spikes
    No signal in well
                          F...   Wells
                                                       0
                          11
                      B1.B9.B1.
                              A1.A9
    Select "QC Summary"  to view the
    analysis summary of the samples
    in the experiment
                                                                         Analysis Settings
                                               View Plate Layout 1  View Well Table
                                                   Select Wells With: -Select Item-  v
                                                                            -Select Item- v
Show in Wei...
                                                                [7] View Legend
                                                       l-'QJ.'r
                                                       I.. 100 f
                                                                               ni  73... 100 ££'
                                          B7I  4E4
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                                                                                 m-~I  ^™
                                                                               7 '• 1  E3-
                                                                               75... m  r>T.
                                                                           8   9  10  11   12
                                                                         *m.' a..' 0
                                                                        IE 98... 100 ^.'

                                                                      ra  63... r^  ^.'
                                                 ra
                                                 S    ••
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                                                                              ni  4E4
                                                                              3D.. 4E3
                                                                              39.. 4E3

                                                                              5-  1 "
                                                                              34.. |-^
                                                                             Wells: Hj 40 Unknown H116 Standard [~] o Negative Control
                            ...56 Wells Omitted Man... 0  Wells Fla... 1 3 Wells Omitted by Ana... 0  Samples ...8  Targets ...2
                                                                                                            Disconnected
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-------
                            Analysis Menu - Multiple Plots View
Select "Multiple Plot View" to view all the plots for the
samples in one window
   Experiment Menu«

    Setup
 NRSA Batch 34 testrur ...Standard C  Rea... TaqMan® Reagt
    Run
    Analysis
   Amplification Plot
    tandard Curve
   Multicomponent Plot
   Raw Data Plot
   QC Summary
   Multiple Plots View
                     Multiple Plots View
                       Amplification Plot - ARn... v
                                     >
                           Am pi If l-catlon Plut
- sjogoTd	

• A  B  c  D

JE • F • G • H
                       Multicomponent Plot
                          Multlcotnpo.no lit fltrt
- Legarcl -
 I ROX  TAMRA • FAM
                  Standard Curve
                    Standard      • Unkn

                    Unknown (Flagged)
                  Raw Data Plot
                                              .Knnw OMtM l'li>t
                                          p ijogond

                                          • A  B  C  D

                                          IE • F • G • H
                  Analysis Settings
                                        View Plate Layout 1 View We 11 Table
                                           Select Wells With: -Select Item- v
                      -SelectItem-
                                           Show in Wei...
           :"OEi View Leg end
                                                                  1234
                                                                  9  10  11  12
Each plot has a drop down
menu located on the top to
access various parameters
required to displayed and
also has the toolbar feature
with various options of
printing, saving, and other
parameters
                                          75...
                       71.
                                                               Wells: Q]40 Unknown [3 16 Standard [710 Negative Control
                     Analysis Summary: Total Wells in ...96  Wells S... 56 Wells Omitted Man... 0 Wells Fla... 1 3 Wells Omitted by Ana... 0 Samples ...8  Targets ...2
      I S NRSA Batch 34...032310 ecis.eds
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-------
                                       Analysis - To Print a Data Report
7500 Sol
    t  Instrument  Analysis   Tools  Hel

New Experiment - ,__j  Open...  id Save ~
                                                             )  Print Report..
  Experimen
    Setup
    Run
                  Select data forthe report. Click"Preview Report" to preview the repo
                                                                       ontent. Click "Print Report" to send the report to the printer
  Analysis
                 0 Results Summary

                 0 Plate Layout
Information about the experiment, including experiment name, experiment type, file name,user
name, run information, and comments
At;
dei
An
Click on  "Print Report" to  make  a  hard
copy of the  results with required plots
                 EH Amplification Plot (ARn vs. Cycle)  Da
                                             normalized reporter (ARn) plotted against cycle number.
                 EH Amplification Plot (Rn vs. Cycle)   Data collected during the cycling or amplification stage. Displays normalized reporter (Rn)
                                             plotted against cycle number.
                 EH Amplification Plot (Cr vs. Well)    Data collected during the cycling or amplification stage. Displays CT plotted against well
                                             number.
                 0 Standard Curves

                 0 Results Table (By Well)

                 0 QC Summary
                                           The best fit line using CT values from the standard reactions plotted against standard
                                           quantities.
                                           Atable of experiment results for each well, including sample, target, task, quantity, ARn and CT.

                                           Atable of flags applied to wells in the experiment, including flag description, frequency of
                                           occurrence,and a list of flagged wells.
                 Print Preview  |
                                                                Print Report
                         L
                                                                                                                        pies ...8 Targets ...1
 Home | S3 NRSA Batch 34...032310 eds.eds x
                                                                                                                       Disconnected
                                  /atri Varanasi
                                                                        •"• 7500 Software v2.0,1

-------
  7500 Software v2.0.1
                                                                                                                          _  ff  X
File  Edit  Instrumpnt  Analvsis  Tools  HP!D
I] New Experiment -  i_j Open...
                              Save- L§  Close  ^Export...-
                                         4)  Print Report...
    Experimer
               Print Report
     Setup
     Run
r     Analysis
                Q Select data forthe report. Click"Preview Report" to prev

                                           Information aboutth
       •pliflcation f
     Standard Curv
     Mutticompone
     Raw Data Plot
     QC Summary
     Multiple Plots \
0 Experiment Summary

0 Results Summary

0 Plate Layout

0 Amplification Plot (ARn vs. Cycle]

0 Amplification Plot (Rn vs. Cycle)

0 ^mJpJMcaMnZioIIcn^ Weil

0 Standard Curves

0 Results Table (By Well)

0 QC Summary
1.  Select the required data and
plots to be  printed  by checking
the boxes next to the data and
plot types in which  results can be
printed
                                           rnrTn^nin ipf"rrmti'
                                           Atabie of experimen
                                           dev), Cr(mean) and
                                           An illustration of the

                                           Data collected durin
                                           normalized reporter (ARn) plotted against cycle number.
                                           Data collected during the cycling or amplification stage. Displays normalized reporter (Rn)
                                           plotted against cycle number.
                                           Data collected during the cycling or amplification stage. Displays CT plotted against well
                                           number.
                                           The best fit line using CT values from the standard reactions plotted against standard
                                           quantities.
                                           Atabie of experiment results for each well, including sample, target, task, quantity, ARn and CT.

                                           Atabie of flags applied to wells in the experiment, including flag description, frequency of
                                           occurrence,and a list of flagged wells.

                                                                  E
                                                                           2. Click "Print Report" to
                                                                           print the required data
                                                                                                                             c,
                 Print Preview
                        T
                                                               Print Report
                                                                                                                       .8 Targets ...1
   Home IB NRSA Batch 34...032310 eds.eds x
                                                                                                                  Disconnected
   start     m
                                                                 ji;  7500 Software v2..,   H Microsoft Po"

-------
                                         Method A
         Appendix B
Cepheid Smart Cycler® Operation

-------
                                                                                    Method A
Appendix B - Cepheid Smart Cycler® Operation

1.0    Smart Cycler® Operation

1.1    This protocol is intended to provide only information about critical instrument settings required to
       perform EPA Method A. Further details concerning the operation of the instrument can be
       obtained from the Smart Cycler® Operation Manual, Cepheid Part #D0190, Rev. D.
1.2    Turn on the Smart Cycler®; then the computer.
1.3    Double-click on the Smart Cycler® icon on the computer desktop.
1.4    The following steps for defining a protocol are only required before the initial run of the
       instrument. The protocol that is defined in these steps is used in all subsequent runs of the
       instrument. See "How to Set Up a New Experiment Using the Smart Cycler (Software Version
       2.0" for screen shots.
       1.4.1   Click on the Define Protocols icon to go to Define Protocols screen.
       1.4.2  Click on the New Protocol button to open the Protocol Name? dialog. Enter "EPA
              Enterococcus TaqMan Method" for the new protocol name, and click OK. The protocol
              stages are defined in the series of boxes at the bottom of the Define Protocol screen.
              Make sure the new protocol is highlighted and begin to choose state settings. To define
              Stage 1, click on its drop-down box to display the menu of stage types; then select Hold.
              In the Temp column, enter 50.0, and in Sees column, enter 120, leaving the Optics setting
              as the default Off setting. (Note: This stage is performed to eliminate potential PCR
              carryover products in the reactions using the Amp-Erase® UNG enzyme provided in the
              TaqMan® Universal PCR Master Mix. Note that the optical reading cannot be
              programmed during a Hold stage.).
       1.4.3  To define Stage 2, click on its drop-down box to display the menu of stage types, and
              again select Hold.  In the Temp column, enter 95.0, and in Sees column enter 600. Again,
              leave the Optics setting on Off.  (Note: This stage is performed to inactivate the Amp-
              Erase® UNG enzyme).
       1.4.4  To define Stage 3, select 2-Temperature Cycle from its drop down menu. For the first
              step, enter 95.0 in the first row of the Temp column and 15 in the Sees column, Optics
              column Off. For the second step, enter 60.0 in the second row of the Temp column, 120
              in the Sees column,  and click on the Optics cell to select On from the drop-down menu.
              This sets the detection of the fluorescence signal to occur at the end of the second step in
              each cycle.  Enter 45 in the Repeat field at the top of the Stage 3 box to  specify that it
              should be repeated for 45 cycles. Click the Save Protocol button.
       1.4.5  To display primary curve graphs, click Define Graphs.  Highlight FAM in Graph
              column. Check the box for Automatically add to new runs.  Under Graph Type choose
              Optics from the pull down menu. Under Channels check the box for Ch 1 (FAM).
              Under Show check the boxes for Primary Curve, Threshold (Vertical) and Threshold
              (Horizontal). Under Axes check the box for Fluorescence vs. Cycle. At the bottom of
              the screen click on Save Graph.
1.5    Click on the Create Run icon to open the Create Run screen.  For each new run, enter a unique
       name in the Run Name field. (Note: The software does not allow duplicate run names).
1.6    Enter any additional information about the run in the Notes field. Click the arrow in the Dye Set
       box to display a drop-down menu of the possible selections. Select FTTC25. (Note: This selects
       the dye set: FAM, TET, Tex Red, Cy5, and a 25 uL reaction).
                                             B-l

-------
                                                                                        Method A
1.7    Click the Add/Remove Sites button. The Select Protocols and Sites... dialog will appear.
       Highlight (click on) the "EPA Method A" protocol developed prior to the first run (Section  1.4.2)
       in the Protocols list.  In the Sites list, highlight the sites on the instrument to be used with this
       protocol in the current run by clicking on them with the shift key held down (Note: Sites refer to
       the I-core modules in the Smart Cycler® processing block in which reaction tubes will be placed;
       a total of 16 are possible per block.  When using multiple blocks, the site numbers will be
       preceded by the block letters, e.g., A, B, C);  then click the right pointing arrow to transfer the
       selected sites and protocol to the Selections table.
1.8    Click on the OK button to save the selections, and return to the Create Run screen.
1.9    Place the loaded  Smart Cycler® reaction tubes in the I-core module slots, selected above for
       current run.  The tubes should snap into place. Either the front or back of the caps can face  the
       front of the processing block.
1.10   In one of the View menus that is shown, select Analysis Settings. The displayed table includes
       one row for each of the four possible dye channels defined in the dye set.  Click on the cell in the
       FAM row under the Usage column heading, and select Assay from the drop down menu. Set the
       Usage cells for all other dyes to Unused in the same manner. (Note:  All assays in this protocol
       use FAM as the reporter dye). All other cells in this table should be left at default settings (See
       Smart Cycler® Operation Manual).
1.11   In the other View menu that is shown, select the Results Table. Enter the sample identification
       information  for each site in the Sample ID column (additional information can be entered into the
       Notes column.).  Leave the other columns as default settings (see Smart Cycler® Operation
       Manual.).
1.12   Click on the Start Run button. The orange LEDs on the Smart Cycler® processing block should
       turn on, and the software will automatically switch to the View Results screen.
1.13   To display the real time temperature profiles for all sites, click Temperature in either of the View
       menus. To display real time growth curves for all samples (i.e., the fluorescence signal vs. cycle),
       click FAM in the other View menu.
1.14   At the end of the run, it is recommended to check the cycle threshold values calculated by the
       instrument for each sample by opening the Results Table window by clicking on this selection in
       the upper View menu. It is also recommended to inspect the growth curves in the FAM window
       which can be opened in the same manner from the lower View menu. The default threshold
       fluorescence value is shown in this window as a single horizontal red line and the cycle thresholds
       for each site are shown as vertical red lines.  To view the data for individual sites in this window,
       click on that site  number in the table to the right of the graph. If the default threshold fluorescence
       line is well above all of the growth curve lines prior to visible amplification, the threshold
       fluorescence value can be changed to a lower value. This is done by  reopening the Analysis
       Settings window from the upper View menu and entering a new value in the Manual Thresh
       Fluor Units cell in the FAM row.  Conversely if the default threshold fluorescence line is below
       any of the growth curve lines prior to visible amplification, the threshold fluorescence value
       should be changed to a higher value in the same manner. Previous studies have indicated that a
       threshold value of 8 works well for most analyses. Click on the Update Analysis button to view
       the new threshold line in the FAM window.  The cycle threshold values will be automatically
       updated in the  Results Table.
1.15   Once the threshold fluorescence value is adjusted to an optimal value, click the Save Run button.
       (Note: The Smart Cycler® Software does not give a prompt to save changes before printing or
       exporting. Therefore, it is possible to make changes to the Results Table or Analysis Settings, and
       immediately print or export the data, then close the run without saving the changes.  In this  case,
                                              B-2

-------
                                                                                      Method A
       the data saved in the Smart Cycler® database will not match the printed or exported data. If no
       changes are made in the threshold fluorescence value, the run data is automatically saved as it is
       when the program is closed or a new run is created).
1.16   To set up automatic export of raw data, (see "How To Set Up Automatic Export of Raw Data" for
       screen shots) from the main menu, click on Setup, then System Defaults, then Export Settings.
       From the Export Settings dialog box, check the box beside Results Table and Analysis Settings.
       Click the Browse button to select the folder where you want your raw data saved. Click on the
       radio button next to Automatic export on run completion, then click the OK button.
1.17   To manually save the Results Table and Analysis setting containing the instrument-calculated
       cycle threshold values for each sample (see "How to Manually Export Raw Data" for screen
       shots), click the Export button to display the Export Data dialog box.  Check the box next to the
       heading Export Results Table and Analysis Settings by clicking on it.  Leave all other boxes
       unchecked. Click on Export. A box labeled Export Data will appear with the run name in the
       file name box.  Click on the drop down menu to the right of Save In: at the top left of the screen to
       change the directory where you want your data saved.  Click on Save. Data are exported as
       comma-delimited text (.cvs) files in MS Excel-compatible files to the Export folder in the Smart
       Cycler® folder: C:\Smart Cycler®\Export. Analysts will late save the file as an XLS file.

1.18   To archive a run in the Smart Cycler® program, click on Tools. From the drop down menu click
       on Data Management and then Archive Runs. Click Proceed.  Select the run to be archived by
       clicking on its name in the database list. Click OK and then Proceed. A box labeled Archive Run
       will appear on the screen. There will be a line labeled Save in:. Input which directory you would
       like the run to be saved in. There will be aline File Name:. Enter a file name.  Click Save.  Click
       OK

1.19   To print run data (see "How to Print Run Data" for screen shots), after the run is completed, right
       click on the graph area, and select Print, then Print Graph with Results Table. An Optics Graph
       print preview screen will pop up, click Print.  The screen will switch back to the post run screen.
       To print the generated report, click  Report. A Run Report print preview screen will pop up, click
       Print

1.20   To set up a new analysis (see  "How to Set Up a New Run" for screen shots), from the post run
       screen, click Create Run at the top left. The results of your just completed will disappear and a
       Add/Remove Sites button will appear in the middle of the screen - click it.  A Select Protocols
       and Sites screen will pop up, select EPA Enterococcus TaqMan Method in the Protocols box,
       and highlight the amount of sites needed for the assay (A1-A16) in the Sites box.  Click the right
       arrow to the right of the sites box to move the sights to the Selections box. After double checking
       that the correct protocol is highlighted, click OK.  Add the Run Name in the Run Name box. The
       Site ID, Protocol, Sample ID, Sample Type, Notes (etc.) box will pop up. Enter the Sample ID for
       each site. Under this box, find the Usage column and click on Assay to select Unused for Cy3,
       TxR and Cy5 (leave Assay for FAM).  In the same box, find the Manual Thresh Fluor Units, and
       click on the units for FAM to change it from 30.0 to 8.0 (leave the units at 30.0  for Cy3, TxR and
       Cy5). After loading the Smart Cycler with tubes, click Start Run.  A red light should appear on
       sites that are in use.
                                              B-3

-------
  How to Set Up a New Experiment Using the Smart Cycler (Software version 2.0)
  Smart Cycler
User Logs  Setup  Tools Help
          Create Run
                    Check Status
                                      Slop Run
                                                  View Results
                                                                     Define Graphs
                                                                              Maintenance
                                                  Protocol Name
EPA Method 1606
Ecoli EDO (uidA) TaqMan Assay
Ecoli Scorpion Assay                .
  TTaqManRescue          2. This screen will appear - type in the name of the new protocol
Mtd 1 607 E NT-LAC SPC Scorpion
Demo67
EPA Method 1606 STOP
Enterol-Roche TaqMan
Duplex adv to next stage example
ENTL4C-SPC EC-IC Scorpn OmniHS
demo
2 Step 60
3 Step 60 & 72
rtPCR
3 Step w Melt
Fast 2 Step 60
                                New Protocol
                                          Please enter a new name for the Protocol:
                                                OK
                                               Cancel
                                           2-Ternperature Cycle   ^
                                           _.[ Advance to Next Stage
 Stage 1
  Hold
Temp
Sees
 50.0
        120
Optics
              Off
                    Stage 2
                      Hold
Temp  I  Sees  | Optics
                      95.0
                            600
                                  Off
                                  Stage 3
                                                 Stage 4
                                                                Unused
eg/Seel Tempi Sees | Optics!]
                                                                    3. Click 01
                                                             Stage 5
                                                                                    Unused
Deg/Secl Tempi Sees | Optics
                                                                                 [)K when done
                                        Stage
                            1. Click on "New Protocol"
           — [«—         — r
  New Protocol     Delete Protocol    Duplicate Protocol    Rename Protocol

                                ocumentl - Microsof.

-------
5sT Smart Cycler
User Logs Setup  Tools  Help
         Create Run
               Check Si at us
                      Stoii Run
      View Results
    Define Protocols
Define Graphs
Maintenance
EPA Enterococcus TaqMan Method I
       '
                                             Protocol Name
Ecoli BDG (uidA) TaqMan Assay
Ecoli Scorpion Assay
ENTTaqMan Rescue
Mtd 1607 ENT-LAC SPC Scorpion
Demo67
EPA Method 1606 STOP
Enterol-Roche TaqMan
Duplex adv to next stage example
ENTLAC-SPC EC-IC Scorpn OmniHS
demo
2 Step 60
3 Step 60 &. 72
rtPCR
3 Step w Melt
Fast 2 Step 60
                        1. New Protocol name will appear in list
                        Make sure new protocol is highlighted
                        and begin to choose stage settings
                                    2. Set the Temperature in the
                                    "HOLD" stage to 50.0 degrees and
                                    120 seconds. NOTE optical
                                    readings cannot be programmed
                                    during a HOLD stage
 Stage 1
  Hold
  Temp   Sees | Optics
  50.0
J120
Off
Stage 2
Unused ^
Deg/Sec Tempi Sees | Optics


Stage3
Unused T
Deg/Secl Tempi Sees | Optics

•:-----:----'-'::x::-::y-x:y::--;x-:;::::::x::|
Stage 4
Unused "^
Deg/Secl Tempi Sees | Optics


Stage 5
Unused T
Deg/Secl Tempi Sees | Optics


Stage
Unus
Deg/S

|>



T

  New Protocol
       Delete Protocol
             Duplicate Protocol
Rename Protocol
Save Protocol

-------
5sT Smart Cycler
 User Logs  Setup Tools  Help
            Create Run
                  Check Si at us
                            Stoii Run
       View Results
Define Protocols
Define Graphs
Maintenance
                                                           Protocol Name
EPA Enterococcus TaqMan Method
EPA Method 1606
Ecoli BDG (uidA) TaqMan Assay
Ecoli Scorpion Assay
ENTTaqMan Rescue
Mtd 1607 ENT-LA.C SPC Scorpion
Demo67
EPA Method 1606 STOP
Enterol-Roche TaqMan
Duplex adv to next stage example
ENTLAC-SPC EC-IC Scorpn OmniHS
demo
2 Step 60
3 Step 60 &. 72
rtPCR
3 Step w Melt
Fast 2 Step 60
                                    In Stage 2, set the temperature to 95.0 degrees
                                                           and  600 seconds
  Stage 1
  Hold
   Ternp
  Sees
  50.0
120
 Optics
Off
                 Stage 2
Hold •»•
Temp | Sees
95.0 1600

j Optics
JOff

                                   age 3
                                          nused
eg/Seel Tempi Sees [Optics
                       Stage 4
                                                          Unused
Peg/Seel Tempi Sees [Optics
                        Stage 5
                                               Unused
       Deg/SecjTempi Sees | Optics
              Stage
              Unus
              Deg/ji
New Protocol

Delete Protocol

Duplicate Protocol

Rename Protocol

Save Protocol

-------
^ Smart Cycler
User Logs  Setup Tools  Help
          Create Run
              Check Si at us
                                    Stop Run
                           View Results
                                 Define Protocols
                                         Define Graphs
Maintenance
                                                Protocol Name
EPA Enterococcus TaqMan Method
EPA Method 1606
Ecoli BDG (uidA) TaqMan Assay
Ecoli Scorpion Assay
ENTTaqMan Rescue
Mtd 1607 ENT-LA.C SPC Scorpion
Demo67
EPA Method 1606 STOP
Enterol-Roche TaqMan
Duplex adv to next stage example    FOT the fJTSt tGffiD
ENT UC-SPC EC-IC Scorpn OmniHS "
                    set the temp at  95
2 Step 60
     o&72            degrees for 15 seconds
                                    1. In Stage 3, set the drop down
                                    menu at "2-Temperature Cycle"
                                    to repeat 45 times (cycles).
                     WJth OptlCS OFF.
Fast 2 Step 60
                                                          3. In the second Temp
                                                          cycle, set the temp for 60
                                                          degrees for 120 seconds
                                                          with the optics ON
  Stage 1
  Hold
   Ternp
 Sees
  50.0
120
              Optics^
             Off
              Stage 2
              Hold
 Temp
  Sees
95.0
.600
Off
                                        Stage 3
Repeat 45
times.
2-Temperature Cycle T
Decj/Sec
NA
NA

Temp
95.0
60.0
Sees
15
1120
Optics
Off
On

                                         D Advance to Next Stage
                                                          Stage 5
                                                                               Unused
                                               Deg/SecjTempi Sees | Optics
                                                                        Stage
                                                                              Unus
            Decj/E
                                    wifi
  New Protocol
       Delete Protocol
                           Duplicate Protocol
                     Rename Protocol
                             Save Protocol
                                             4. UIICK oave rroiocoi
                                             when finished

-------
                      How To Set  Up Automatic  Export of Raw Data
W Smart Cycler
User  Logs

Setup Tools  Help
          User Administration
          System Defaults
                         Analysis Settings
                                                                Define Protocols
                                                                     Define Graphs
                         Automatic Backup
                         Export Settings
 NRSA 2009 Batch 25E ENT 091 809
                         Access Options
 User: Default User
 Started: Sep 18,2009 01:30 PM
 Finished: Sep 18,2009 03:37 PM
 Status: Done

 Notes:
                Standard - FAM
 NRSA 2009 ENT Analysis of Batch
 25E
                                                    Bkgnd  Bkgnd   Bkgnd
                                                     Sub  Min Cycle Max Cycle
                                                             Curve Analysis
                                 Thresh Setting
Manual Thresh
 Fluor Units
Auto Thresh
  #SD's
                Results Table
                Analysis Settings
                Protocols
                                                                      Primary Curve  Manual
                                                                      Primary Curve  Manual
                         Standard - Tet
                                                             Primary Curve  Manual
 Dye Set: FCTC25

 Protocols:
                                                             Primary Curve  Manual
    Protocol
     Lot Number
 EPA Method 160..
 Number of Sites: 30
                         Melt
                         FAM
                         Cy3
                         Texas Red
                         Cy5
                         Standard - FAM
To set up automatic export of Raw Data
into computer, click on "SETUP", then
"System Defaults" then "Export Settings"
Save Run

Export

Report

Select Graphs

View Another Run

Delete Ftun(s)

Update Analysis

Impart Std Curve

Compare Run

-------
                                                Optics Data Defaults
                                                 fZl Primary Curve
                                                   2nd Derivative
 Data Export Defaults
  j Optics Data
 1*3 Results Table and Analysis Settings
  J Melt Data
1. Check Results Table and Analysis settings box Melt Data Defauhs
                                                  13 Melt Curve
                                                  Ji5 1st Derivative
Export Path and Filename Defaults
   Browse
                       art CyclerCxportWRSA 2009 CSV Files
Enter a filename to write to the same file each time.
Leave filename blank to create a unique file each time.
Filename:
                                                      2. Choose browse to
                                                      select a folder where
                                                      the raw data will export
                                                      to
Automatic Export Option
   No Automatic export
   Automatic export on run completion
    3. Be sure that Automatic export on run completion is checked
                                                    4. Click OK when finished

                                OK
                                       UJIIl,

-------
                                    How To  Manually  Export Raw  Data
User  Logs  Setup  Tools Help
            Create Run
                            Chech Status
                                              Stop Run
                                                                             Define Protocols
                                                                 Define Graphs
                                                                                                                 Maintenance
Run Name:
 NRSA 2009 Batch 25E ENT 091 809
User: Default User

Started: Sep 18, 2009 01:30 PM
Finished: Sep 18, 2009 03:37 PM

Status: Done

Notes:
 NRSA 2009 ENT Analysis of Batch
 25E
Dye Set: FCTC25

Protocols:
Number of Sites: 30
Protocol
EPA Method 160...
Lot Number


                                   Views
Results Table
Analysis Settings
Protocols
                              Standard - Tet
                              Temperature
Intercalate
Melt
FAM
Cy3
Texas Red
Cy5
Standard - FAM
                                   Views
                              Results Table
                              Analysis Settings
                              Protocols
                              Standard - Tet
Temperature
Intercalate
                              Melt
                              FAM
                 Site
                  ID
     Protocol  Sample ID
                    Sample
                    Type
A1
A2
A3
EPA Met..
EPA Met..
EPA Met.
                                               A4
                 A5
                 A6
LB-96
538480
538248
                                                   EPA Met..
                     EPA Met..
                     EPA Met..
                                                           537352
                             538574
                             53865S
                 A7
                 A3
                 A9
    EPA Met.
    EPA Met.
    EPA Met.
                 A10
                 A11
                     EPA Met.
                     EPA Met.
                 A12
                 A13
    EPA Met.
    EPA Met.
        537351
        538651
                             538655
                             537353
                             538673
        538143
        538045
                                                                      UNKN
                                                                      UN KM
                                                                      UNKN
                                                                      UNKN
                                        UNKN
                                        UNKN
                                        UNKN
                   UNKN
                                        UNKN
                                        UNKN
                                        UNKN
                                                                      UNKN
                                        UNKN
                                                                                  Notes
                                                                              ENT5X
                                                                              ENT5X
                                                                              ENT5X
                                                                              ENT 5X
                                                ENT5X
                                                ENT5X
                                                ENT5X
                           ENT5X
                                                ENT5X
                                                ENT 5X
                                                ENT5X
                                                                              ENT5X
                                                ENT5X
                                                                                           Status
                                                                                           OK
                                                                                           OK
                                                                                           OK
                                                                                           OK
                                                             OK
                                                             OK
                                                             OK
                                        OK
                                                             OK
                                                             OK
                                                             OK
                                                                                           OK
                                            OK
                                       FAM
                                     Std/Res
                                              FAM Ct
                                                                                                NEG
                                                                                                POS
                                                                                                POS
                                                                                                POS
                                                                  POS
                                                                  POS
                                                                  POS
                                                                  POS
                                                                  POS
                                                                  POS
                                                                  POS
                                                                                                POS
                                                                  POS
                                                                                                       0.00
35.00
                                                                                                       35.15
                                                                                                       34.07
                                                                         39.79
                                                                         36.69
                                                                         37.20
                                                    33.64
                                                                         28.93
                                                                         29.32
                                                                         33.75
                                                                                                       36.14
                                                                         36.04
                 Chi  Dye   Usage  Bkgnd   Bkgnd   Bkgnd ' Curve Analysis
                  #  Name         Sub  Min Cycle Max Cycle
                    FAM
                          Assay
                                                  Cy3
                                                  TxR
   Cy5
                                                        Unus...
                                                        Unus..
                          Unus..
                                ON
                                ON
                                                              ON
                                ON
                              40
                                               40
                                                                             40
                                               40
                                      Primary Curve  Manual
                                                                                                 Thresh Setting  Manual Thresh  Auto Thresh
                                                                                                               Fluor Units     #SD's
                                  Primary Curve  Manual
                                  Primary Curve  Manual
                                  Primary Curve  Manual
                                                                               8.0
                                                  30.0
                                                                                                             30.0
                                                                               30.0
                                                                                            NA
                   NA
                                                                                                                          NA
                                                                                            NA
                                                              Once run is finished, click Export
Save Run
Export

Report

Select Graphs

View Another Run

Delete Run(s)

Update Analysis

Import Std Curve

Compare Run

-------
     Export Data
  j Export Optics Data
    Export Results Table and Analysis Settings
    Export Melt Data
  D Export Heater Temperature Data


y Export


Cancel
Check the Export Results Table and Analysis Settings box
then click "Export"

-------
    Export Data
Save In:

PI NRSA 2009 CSV Files ^ ^


ffl
                                                              D-D-
                                                              D-D-
                                                  D
                                                  D
   >A 2009 Batch 20 STDCAL 001009
   iA 2009 Batch 20A ENT 081109
   iA 2009 Batch 20A SKETA 081109
   iA 2009 Batch 20B ENT 081209
   iA 2009 Batch 20B SKETA 001209
                    NRSA Z009 Batch 21 STDCAL 081709
                    NRSA 2009 Batch 21C ENT 082009
                    NRSA 2009 Batch 21C SKETA 082009
                  QQRSA 2009 Batch 21D ENT 082109
                    NRSA 2009 Batch 21D SKETA 082109

   File Name:
   Files of Type:
NRSA 2009 Batch 25E ENT 091 G09.csv|
All Files
                                                  Save
                                             Cancel
Choose the appropriate file folder to save the Raw Data to
and click SAVE. NOTE: All raw data will export in the form of
a CSV file.  Analysts will later save file as an "XLS" file.

-------
                                              How to  Print Run  Data
User  Logs  Setup  Tools  Help
                                                                             Define Protocols
                                                                 Define Graphs
                                                                                  Maintenance
Run Name:
 NRSA 2009 Batch 26B ENT 092409
User: Default User

Started: Sep 24, 2009 02:27 PM
Finished: Sep 24,2009 04:34 PM

Status: Done

Notes:
 NRSA 2009 ENT Analysis of Batch
 26B
Dye Set: FCTC25

Protocols:
Number of Sites: 32
Protocol
EPA Method 160...
Lot Number


                                   Views
                              Results Table
Analysis Settings
Protocols
                              Standard - Tet
                              Temperature
Intercalate
Melt
                 Site  Protocol
                  ID |
                 A1   EPA Met...
                                               A2  .EPA Met...
                 A3
                 A4
                 A5
                     EPA Met.
                     EPA Met..
                                                 EPA Met..
                              Sample ID
                                                           LB-98
                             537973
                                                        53S019
                                                        538031
                                            538277
                                                                    Sample
                                                                     Type
                                                                     UNKN
                                                                     UNKN
                                                       UNKN
                                                       UNKN
                                             UNKN
                                                                                  Notes
                                                                             ENT 5X
                                                                             ENT5X
                                                     ENT5X
                                                     ENT5X
ENT5X
                                                                                           Status
                                                                                           OK
                                                                                           OK
             OK
             OK
OK
                                                                                   FAM
                                                                                  Std/Res
                                                                  NEO
                                                                                                POS
     POS
     POS
POS
                                                                                                        FAM Ct
                                                                                                       0.00
                                                                                                       35.31
       36.99
       34.12
36.54
     Right click on graph  area  and select "Print" then
     "Print Graph with Results Table"
Texa:
ytandard - FAM
                     EPA Met... 5.18466
                     EPA Met.  |53|B360
                 A13  EPA Met... 53:796
                              Results Table
                              Analysis Settings
                              Protocols
                              Standard - Tet
Temperature
Intercalate
                                                                     Reset zoom
                                                                     Show all sites
                                                                     Scale graph
                                                                     Overlay graphs
                              Standard - FAM
                                       Print
                                       Save to file (jpg)
                                                                                      Print Graph only
                                                                                      Print Graph with Results Table
                                                                     Export graph data
                                   Select Graphs
                                                  View Another Run
                                                      Update Analysis
                                                                       Import Std Curve
                                                                                     ID  Protocol [Sampl..r
                                                                                     BEPA Met... 537753 j>
                                                                                     _EPAMet... 538049
                                                                                       EPA Met... 538050
                                                                                       EPA Met... 537253
                                                                                       EPA Met...537517
                                                                                       EPA Met... 537143
                                                                                       EPA Met... 538506
                                                                                       EPA Met... 538496
                                                                                       EPA Met... 538525
                                                                                       EPA Met... 538060
                                                                                       EPA Met... 538060
                                                                                       EPA Met... AE
                                                                                       EPA Met... SAE
                                                                                       EPA Met.^ 1:5375...
                                                                                       EPA Met...5375...
Save Run
Export
Report
                                          Compare Run
                  mart Cycler

-------
Jser  Logs  Setup  Tools  Help
                                Vihisd smart Cycler Custcmer
                                                                Optics Graph
                                Rim Name : NRSA 2009 Batch 26B ENT 092409
                                User Name : Default User
                                Rim Date : Sep 24, 2009 02:27 PM
NRSA 2009 Batch 26B ENT 09240!
Jser: Default User
Started: Sep 24,2009 02:27 PM
-inished: Sep 24,2009 04:34 PM
Status: Done

Yotes:
NRSA 2009 ENT Analysis of Batch
26B
                                                                                                                                    537753
                                                                                                                                    538049
                                                                                                                                    538050
                                                                                                                                    537253
                                                                                                                                    537517
                                                                                                                                    537143
                                                                                                                                    538506
                                                                                                                                    538496
                                                                                                                                    538525
                                                                                                                                    538060
                                                                                                                                    538060
                                                                                                                                    |AE~"
                                                                                                                                    SAE
                                                                                                                                    5375...
                                                                                                                                    5375..
                                                                                                           EPA Met...
                                                                                                           EPA Met...
                                                                                                           EPA Met...
                                                                                                           EPA Met...
                                                                                                           EPA Met...
                                                                                                           EPA Met...
                                                                                                           EPA Met...
                                                                                                           EPA Met...
                                                                                                           EPA Met...
                                                                                                           EPA Met...
                                                                                                           EPA Met...
                                                                                                           EPA Met...
                                                                                                           EPA Met...
                                                                                                           EPA Met...
                                                                                                           EPA Met...
                                Site ID Simple ID
Dye Set: FCTC25
   This  sheet
   will pop  up.
   Click
   "Print" to
Mu
                                     Select Graphs
                                    View Another Run
                                                                                         Update Analysis
Import Std Curve
Compare Run
   start
Smart Cycler
                           Microsoft Word

-------
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            Create Run
                                   ,
              Check Status
                      Stop Run
                           View Results
                           Define Protocols
                           Define Graphs
                                    Maintenance
Run Name:
 NRSA 2009 Batch 26B ENT 092409
User: Default User

Started: Sep 24,2009 02:27 PM
Finished: Sep 24,2009 04:34 PM
Status: Done
Notes:
                                     Views
                               Results Table
                Analysis Settings
                Protocols	
                Standard - Tet
                               Temperature
                Intercalate
                Melt
                FAM
                               Cy3
                               Texas Red
                               Cy5
                                  Site  Protocol
                                   ID
                                     Sample ID
                       A1  EPA Met... LB-98
                       A2  EPA Mel... 537973
                       A3  EPA Met...'53801 9
                                  A4
                       A5
                       A6
                       A7
                                  A8
                                  A3
                                  A10
                           EPA Met..
                 EPA Met.
                 EPA Met.
                 EPA Met.
                           EPA Met.
                           EPA Met.
                           EPA Met.
                         538031
         538277
         520186
         520187
                         538579
                         538561
                         538583
                                     Sample
                                      Type
                                Notes
                                                                        UNKN
                                                                        UNKN
                                                                        UNKN
                    UNKN
UNKN
UNKN
UNKN
                    UNKN
                    UNKN
                    UNKN
                                            ENT5X
                                            ENT5X
                                            ENT5X
         ENT5X
ENT5X
ENT5X
ENT 5X
         ENT5X
         ENT5X
         ENT5X
                       Status
                                          OK
                                          OK
                                          OK
              OK
OK
OK
OK
              OK
              OK
              OK
 NRSA2009ENT Anah
 26B
    To print the generated  report, click on "Report"
Dye Set: FCTC25

Protocols:
                     FAM
                   Std/Res
                            NEO
                            POS
                            POS
     POS
POS
POS
POS
     POS
     POS
     POS
     POS
                                                                                                    POS
                                                                                     NEG
              FAMCt
                          0.00
                          35.31
                          36.99
       34.12
36.54
31.96
34.05
       31.30
       27.40
       32.48
       26.51
                                                                                 38.46
                                                                                 0.00
Protocol
EPA Method 160...
Lol Number


Number of Sites: 32
                Temlerature
                Intejtalate
                Me ||
                Ft
                                    Red
                                tandard - FAM
                                                                                                                    Site ID]  Protocol ISampL
                                                                                                EPA Met...
                                                                                                EPA Met...
                                                                                                EPA Met...
                                                                                                EPA Met...
                                                                                                EPA Met...
                                                                                                EPA Met...
                                                                                                EPA Met...
                                                                                                EPA Met...
                                                                                                EPA Met...
                                                                                                EPA Met...
                                                                                                EPA Met...
                                                                                                EPA Met...
                                                                                                EPA Met...
                                                                                                EPA Met...
                                                                                                EPA Met...
                                                                                              537753
                                                                                              538049
                                                                                              538050
                                                                                              537253
                                                                                              537517
                                                                                              537143
                                                                                              538506
                                                                                              538496
                                                                                              538525
                                                                                              538060
                                                                                              538060
                                                                                              AE
                                                                                              SAE
                                                                                              5375..
                                                                                              5375..
  Save Run
Export
Report
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             Create Run
Run Name:
 NRSA 2009 Batch 26B ENT 09240!
User:  Default User

Started: Sep 24,2009 02:27 PM
Finished: Sep 24,2009 04:34 PM

Status: Done

Notes:
 NRSA 2009 ENT Analysis of Batch
 26B
  Click "Print"
  to print out
i the generated
I run data
  report
Number of Sites: 32

               Vailed Smart Cycler Customer

                                                Run Report
               Run Information
               Run Name: NRSA 2009 Batch 26B ENT 092409
               User Name: Default User
               Run Status: Done
               Dye Set: FCTC25
               Notes: NRSA 2009 ENT Analysis of Batch 26B
               Analysis Settings:
                                                                                                   2009/10/2 11:2(5 AM
                                                                                  Started: 2009/9/24 02:27 PM
                                                                                  Finished: 2009/9/24 04:34 PM
                                                                                  S W Version: 2.Od
                                                                                         Maintenance
                                                                                   ret
Ch#
1
Dye
Name
FAM
Manual
Thresh
Fluor
Unite
8.0
Usage
Assay
Auto
Thresh
#SD's
NA
Bkgnd
Sub
ON
Auto Miii
Cycle
5
BkgndMin
Cycle
5
Auto Max
Cycle
10
Bkgnd Max
Cycle
4ID
Valid
Min
Cycle
3
Curve Analysis
Primary Curve
Valid Max
Cycle
60
Boxcar
Avg Cycles
0
Thresh
Setting
Manual
Target


Piotocol(s):
Name :
Lot Number:
                         EPA Method 1 606 STOP
                         None
                         Stage 1 : Hold 50.0°C for 120 seconds
                         Stage 2 : Hold 95 ITC for 600 seconds
                                ^emperature Cycle repeat for 45 times.
                                          r 15 seconds
                                   60.0'C for'l^O'Sissndswith Optics ON
                                   Advance to Next Stage^tJ^eiisdfler Ch 1
                                   1of3
                                               Previous
                                            Next
Last
Print
Close
                                                                                     Cycle
                                                                                         Site ID
                                                                                                              Protocol |SampL
                                                    il
      EPA Met... 537753
|B3    EPA Met... 538049
   	EPA Met... 538050
|B5    EPA Met... 537253
      EPA Met.'.. 1537517
     _ EPA Met.'.. 537143
|B8    EPA Met... 538506
      EPA Met... 538496
      EPA Met... 538525
      EPA Met... 538060
     _EPAMet... 538060
 313   EPA Met... AE
      EPA Met... SAE
      EPA Met... 5375...
      EPA Met... 5375..
Save Run

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8?T Smart Cycler
 User  LO**°  Cotnn
 Run Name:
 NRSA 2009 Batch 25E ENT 091 809
 User: Default User

 Started: Sep 18,2009 01:30 PM
 Finished: Sep 18,2009 03:37 PM

 Status: Done

 Notes:
 NRSA 2009 ENT Analysis of Batch
 25E
 Dye Set: FCTC25

 Protocols:
     Protocol
Lot Number
 EPA Method 160..
 Number of Sites: 30
                                      Views
              Results Table
              Analysis Settings
              Protocols
                                 Standard - Tet
                                Temperature
              Intercalate
              Melt
              FAM
              Cy3
              Texas Red
              Cy5
              Standard - FAM
                                      Views
                                Results Table
                                Analysis Settings
                                Protocols
                                 Standard - Tet
              Temperature
              Intercalate
                                 Melt
                                 FAM
                                 Cy3
                                Texas Red
                                 Cy5
                                 Standard - FAM
 Site
 ID
                                                  A1
                                                  A2
                                A3
                                A4
A5
A6
A7
A8
A9
A10
A11
                                                  A12
                                A13
                                     Protocol
    EPA Met..
    EPA Met..
    EPA Met..
    EPA Met..
EPA Met..
EPA Met..
EPA Met..
EPA Met..
EPA Met.
EPA Met.
EPA Met.
                                    EPA Met.
    EPA Met.
          Sample ID
        LB-96
        538480
        538248
        537352
538574
538658
537351
538651
538655
537353
538673
             538143
        538045
            Sample
             Type
           UNKN
           UNKN
           UNKN
           UNKN
UNKN
UNKN
UNKN
UNKN
UNKN
UNKN
UNKN
                    UNKN
           UNKN
             Notes
        ENT5X
        ENT5X
        ENT5X
        ENT5X
ENT5X
ENT5X
ENT5X
ENT5X
ENT5X
ENT5X
ENT5X
                    ENT5X
        ENT5X
              Status
              OK
              OK
              OK
              OK
OK
OK
OK
OK
OK
OK
OK
                      OK
              OK
       FAM
      Std/Res
      NEG
      POS
      POS
      POS
POS
POS
POS
POS
POS
POS
POS
                    POS
      POS
         FAMCt
       0.00
       35.00
       35.15
       34.07
39.79
36.69
37.20
33.64
28.93
29.32
33.75
             36.14
       36.04
                                 Ch
     Dye
    Name
                                    FAM
          Assay
                                    Cy3
                                    TxR
    Cy5
      Usage
          Unus...
          Unus...
      Unus...
    Bkgnd   Bkgnd   Bkgnd
     Sub   Min Cycle Max Cycle
            ON
            ON
            ON
   ON
                   40
                   40
                   40
        40
                 Curve Analysis
                     Thresh Setting
        Primary Curve  Manual
        Primary Curve  Manual
        Primary Curve  Manual
        Primary Curve  Manual
                    Manual Thresh
                     Fluor Units
                                          8.0
                                          30.0
                                          30.0
                   30.0
                           Auto Thresh
                              #SD's
                                 NA
                                 NA
                                 NA
                           NA
Save Run

Export

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Import Std Curve

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-------
SsT Smart Cycler
 User  Logs  Setup  Tools  Help
                             Check Status
                                      Stop Run
               View Results      Define Protocols      Define Graphs
                                                                           Maintenance
 Run Name:
 Notes:
  Dye Set:
FCTC25
 Protocols:
       Protocol
            Lot Number
 Graphs:
 Standard-Tet
 Temperature
 Intercalate
 Melt
 FAM
 Cy3
                                        Site ID
                                          Protocol
                     Sample ID  Sample Type
                                             Notes
                                                    FAM Std
                                                     Cone
                                                      Cy3 Std   TxR Std   Cy5 Std
                                                       Cone     Cone    Cone
                                       Click "Add/Remove" Sites
                                       Ch
 Dye
Name
                                          FAM
                                      Assay
                                Cy3
                                          TxR
                                          Cy5
Usage
     Assay
     Assay
                                      Assay
Bkgnd
 Sub
            ON
                                                      ON
                                            ON
            ON
 Bkgnd
Min Cycle
 Bkgnd   Curve Analysis
Max Cycle
Thresh Setting
Manual Thresh
 Fluor Units
                     40
                     40
                     40
                     40
                       Primary Curve  [Manual
                       Primary Curve  Manual
                       Primary Curve
                       Primary Curve
                             Manual
                             Manual
                                         30.0
                                         30.0
                                 30.0
                                 30.0
Auto Thresh
  #SD's
                                              NA
                                              NA
                         NA
                         NA
Auto Min
 Cycle
Auto
 Cyc
                                            10
                                            10
                               10
                               10
Start Run

Cancel Run Setup

Report Run Setup

Select Graphs

Copy Run Setup

-------
                        LMT Tc;;"c:i..." CTC.
User Logs Setup Tools Help
Notes:
 Dye Set:
FCTC25
Protocols:
     Protocol
          Lot Nurr
Graphs:
 Standard-Tet
 Temperature
 Intercalate
 Melt
 FAM
 Cy3
                 EPA Enterococcus TaqMan Method
                iHPAMeUiuU 1000
                 Ecoli BDG (uidA) TaqMan Assay
                 Ecoli Scorpion Assay
                 ENT TaqMan Rescue
                 Mtd 1607 ENT-LAC SPC Scorpion
                 Demo67
                 EPA Method 1606 STOP
                 Ei iterol-Roche TaqMan
A1
A2
A3
A4
A5
A6
A7
A8
                                   Select All Sites
  Start Run
     Cancel Run Setup
    Report Run Setup
Select Graphs
                                                1.  Be sure the correct
                                                protocol is highlighted
                                                before selecting sites
                                                resh
                                                its
                                      Auto Thresh
                                        #SD's
Auto Win
 Cycle
Auto
 Cyc
                           2.  Highlight the amount of
                           sites needed for assay  (AI-
                           MS)
                                                      10
                                                      10
                                                      10
                                                      10
Copy Run Setup
   start
       Smart Cycler
      fir EPA Draft TaqMan En.

-------
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                                                                          wi
                                                                                   CD
Run Name:
Notes:
 Dye Set:
FCTC25
Protocols:
     Protocol
           LotNurr
Graphs:
 Standard-Tet
 Temperature
 Intercalate
 Melt
 FAM
 Cy3
                          Select Protocols and Sites
                           Protocols:
                                                                                                          Maintenance
                                                         Selections:
                  ENT TaqMan FAST STOP
                  EPA Enterococcus TaqMan Method
                  EPA Method 1606
                  Ecoli BDG (uidA) TaqMan Assay
                  Ecoli Scorpion Assay
                  ENT TaqMan Rescue
                  Mtd 1607 ENT-LAC SPC Scorpion
                  Demo67
                  EPA Method 1606 STOP
                  Enterol-Roche TaqMan
                           Sites:
                           A9
A11
A12
A13
A14
A1S
A16
                                      Select All Sites
                                                                        Site
                                                                               Protocol
                                                                                                    td
                                                                                               Cy3 Std
                                                                                                Cone
                                                                                    TxR Std
                                                                                     Cone
                                        Cy5 Std
                                         Cone
Click  "right"  arrow to
move sites to the         I
"Selections"
Cancel

OK
Auto Win
 Cycle
                                                                                                        NA
                                                                                                        NA
                                                                                                        NA
                                                                                                        NA
Auto
 Cyc
                                                                                                                 10
                                                                                                                 10
                                                                                                                 10
                                                                                                                 10
Start Run

Cancel Run Setup

Report Run Setup

Select Graphs

Copy Run Setup
                Smart Cycler
                         *m EPA Draft TaqMan En.
                                                            ntl - Microsof.

-------
^~
?T Smart Cycler _ O X
User Logs Setup Tools Help
ml ^1 1 1 m \ v
|| III Select Protocols and Sites

Run Name:
Notes:



Sites have b<
Protoc Aj-vl Asv|-isM<*c% r*f
w. a
'i^»
Maintenance
Protocols: Selections:
ENT TaqMan FAST STOP H
EPA Enterococcus TaqMan Method
EPA Method 1606
Ecoli FJDG (uidA) TaqMan Assay
Ecoli Scorpion Assay
ENT TaqMan Rescue
Mtd 1607 ENT-LAC SPC Scorpion
Demo67
EPA Method 1606 STOP
Enterol-Roche TaqMan •«•
Sites:


36n rlOVGQ LO

selections coiunm. L/uuuie ^^^
check that th
is selected a
Graphs:
Standard -Tet
Temperature
Intercalate
Melt
FAM
Cy3
ie correct protocol
nd click on "OK"

Site
A1
A2
A3
A4
A5
A6
A7
A8
A9
A10
ft1 1
A12
A13
A14
A15
A16
\


si
Cancel Run Setup Report Run Setup Select Graphs Copy Run Setup

Protocol
EPA Enterococcus Ta...
EPA Enterococcus Ta...
EPA Enterococcus Ta...
EPA Enterococcus Ta...
EPA Enterococcus Ta...
EPA Enterococcus Ta...
EPA Enterococcus Ta...
EPA Enterococcus Ta...
EPA Enterococcus Ta...
EPA Enterococcus Ta...
EPA Enterococcus Ta...
EPA Enterococcus Ta...
EPA Enterococcus Ta...
EPA Enterococcus Ta...
EPA Enterococcus Ta...
^

Cancel OK









td Cy3 Std TxR Std Cy5 Std
D Cone Cone Cone

5

resh Auto Thresh Auto Mi n Auto
its #SD's Cycle Cyc
NA 5 10
NA 5 10
NA 5 10
NA 5 10



|>

. uyh* ^ ^^ i u, .- l-li 1, I EH t.^^^B^^™ 1-^3
.. St art IT Smart Cycler fir EPA Draft TaqMan En. . . EjJ Documentl - Microsof . . . H Doc
1- Microsoft Word / ' R9 *< V . ^O • 11:07 AM

-------
User  Logs  Setup  Tools  Help
                           deck Status
                                          Stop Run
View Results
                                                                          VUl
Define Protocols
Define Graphs
                                                                                                         »*=
Maintenance
                                          EPAEnterococcus
                                          EPAEnterococcus
                                          EPAEnterococcus
                                          EPAEnterococcus
                                          EPAEnterococcus
                                          EPAEnterococcus
                                          EPA Enterococcus
                                          EPAEnterococcus
                                          EPAEnterococcus
                                          EPAEnterococcus
                                     Add.'Remove Sites
                                   Ch   Dye  Usage Bkgnd   Skgnd   Bkgnd  Curve Analysis Thresh Setting  Manual Thresh Auto Thresh  Auto Min Auto
                                                        in Cycle Max Cycle
Dye Set:
Protocols:
Protocol
EPA Enterococcus T...
Lot Number


Graphs:
 Standard-Tet
 Temperature
 Intercalate
 Melt
 FAM
 Cy3
                                        The Sample IDs and  run  name can be entered at this
                                        point
Start Run

Cancel Run Setup

Report Run Setup

Select Graphs

Copy Run Setup
   start
              ° Smart Cycler
                        Tosoft Word

-------
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                       Check Status
                               Stop Run
                  View Results
                                                                   VIA,
                          Define Protocols
                                    Define Graphs
                                              Maintenance
                                                    Sample ID  Sample Type
                                      EPAEntercoccus q
 NRSA 2009 Batch 1 SKETA 092209
                                      EPAEntercoccus q
                                      EPAEntercoccus q
                                      EPAEntercoccus q
                                      EPAEntercoccus q
 NRSA 2009 SKETA Analysis of Batch 1
                                      EPAEntercoccus q
                                      EPAEntercoccus q
                                      EPAEntercoccus q
                                      EPAEntercoccus q
                                      EPAEntercoccus q
                                         Entercoccus
                                                             SKETA 5X
                                                             SKETA5id
                                 Add/Remove Sites
 Dye Set:
FCTC25
Protocols:
Protocol
EPAEntercoccus qP...
Lot Number


Graphs:
 Standard-Tet
 Temperature
 Intercalate
 Melt
 FAM
 Cy3
                               Ch
 Dye
Name
                                  FAM
                               Assay
                          Cy3
                                  TxR
                                  Cy5
Usage
    Assay
                               Ass ^y
Bkgnd
 Sub
          ON
                                            ON
                                    ON
          ON
 Bkgnd
Min Cvcle
 Bkgnd
Max Cvcle
                 40
                 40
                      40
                 40
Curve Analysis
Thresh Setting
                  Primary Curve  Manual
                  Primary Curve [Manual
                        Primary Curve
                  Primary Curve  Manual
                             Manual
Manual Thresh
 Fluor Units
Auto Thresh
  #SD's
                                  30.0
                                  30.0
                                  30.0
                                  30.0
                                      NA
                                      NA
                                      NA
                                      NA
Auto Min
 Cvcle
Auto
 Cvc
                                              10
                                              10
                                              10
                                              10
                         Under the "Usage" column, select "Unused" from the
                         drop down  menu for Cy3,  TxR and Cy5.   Leave the
                         "Assay" on the FAM line for this particular protocol
Start Run

Cancel Run Setup

Report Run Setup

Select Graphs

Copy Run Setup

-------
^ Smart Cycler
User  Logs  Setup  Tools  Help
                        Ilieck Status
                                Stop Run
                     View Results
                                                                    VI
                                Define Protocols
                                          Define Graphs
                                                    Maintenance
 Run Name:
 NRSA 2009 Batch 1 SKETA 092209
 Notes:
 NRSA 2009 SKETA analysis of Batch 1
 Dye Set:
FCTC25
 Protocols:
Protocol
EPAEnterococcusT...
Lot Number


 Graphs:
 Standard-Tet
 Temperature
 Intercalate
 Melt
 FAM
                                 Site ID
                                A1
                                A2
                                A3
                       A4
                       A5
                       A6
                                A7
                                A8
                                A9
                                A10
                                A11
                                   Protocol
                              EPAEnterococcus...
                              EPAEnterococcus...
                              EPAEnterococcus...
      EPAEnterococcus...
      EPAEnterococcus...
      EPAEnterococcus...
                     Sample ID  Sample Type
                    LB-1
                         UNKN
                            UNKN
                            UNKN
                         UNKN
                                                            UNKN
                                                            UNKN
                                          Notes
                              SKETA 5X
                              SKETA 5X
                              SKETA 5X
                              SKETA 5X
                              SKETA 5X
                                   SKETA 5X
                                1. Set the Manual Threshold
                                Fluorescence Units to  8.0 on the
                                FAM line
                                  Add/Remove Sites
Ch
f
 Dye
Name
                                   FAM
                               Assay
                          Cy3
                                   TxR
                                   Cy5
Usage
                                        Unus...
                                Unus...
                                Unus...
 Bkgnd   Bkgnd   Bkgnd
 Sub  Min Cycle Max Cycle
ON    5       40
             ON
             ON
             ON
                      40
                      40
                      40
Curve Analysis
                                Primary Curve Manual
                                                                           Thresh Settinc
                        Primary Curve Manual
                        Primary Curve Manual
                        Primary Curve Manual
Manual Thresh
 Fluor Units
                                                  8.0
                                        30.0
                                        30.0
Auto Thresh
  #SD's
                                                        NA
                                                   NA
                               NA
                               NA
Auto Min
 Cycle
Auto
 Cyc
                                               10
                                               10
                          10
                          10
                                 2. When smart cycler tubes have been put in to
                                 appropriate sites, click "Start Run"  - a red light
                                 should  appear on sites that are in  use
Start Run
[-^ 	
Cancel Run Setup

Report Run Setup

Select Graphs

Copy Run Setup
               Smart Cycler
_J-/:---- -: '- _
^^g
41 :•:'-.•••'•
                                                                           rosoft Word

-------