SEPA EPA/600/R-10/056 | September 2010 | www.epa.gov/ord United States Environmental Protection Agency Standard Analytical Protocol for Escherichia coli 0157:H7 in Water Office of Research and Development National Homeland Security Research Center ------- ------- Standard Analytical Protocol for Escherichia coli 0157:H7 in Water U.S. ENVIRONMENTAL PROTECTION AGENCY OFFICE OF RESEARCH AND DEVELOPMENT NATIONAL HOMELAND SECURITY RESEARCH CENTER CINCINNATI, OH 45268 Office of Research and Development National Homeland Security Research Center ------- ------- Acknowledgments This Standard Analytical Protocol is based on procedures evaluated by BioVir Laboratories. Inc.. under direction of the National Homeland Security Research Center within the U.S. Environmental Protection Agency's (EPAs) Office of Research and Development under the direction of Sanjiv R. Shah for analysis of E. coli 0157:H7 in water samples. Technical support and data evaluation were provided by Computer Sciences Corporation under EPA Contract EP-C- 05-045. The contributions of the following persons and organizations arc gratefully acknowledged: Study Workgroup Participants • Ayaad Assaad (EPA, Office of Pesticide Programs) • Michele Burgess and Marissa Mull ins (EPA, Office of Emergency Management) • Stephanie Harris (EPA, Region 10) • Malik Ray nor (EPA, Office of Water, Water Security Division) • James Sinclair (EPA, Office of Water, Office of Ground Water and Drinking Water) Subject Matter Experts • Cheryl Bopp (Centers for Disease Control and Prevention) • Diana Cantrell and Robert Mandrell (U.S. Department of Agriculture) • Victor Cook, Bill Cray, Mike Grant, and Steve Weagant (U.S. Food and Drug Administration) Volunteer Participant Laboratory • Rick Danielson. Rosie Newton, and JimTruscott (BioVir Laboratories, Inc.) ------- Disclaimer This document has been reviewed in accordance with EPA policy and approved for publication. Mention of trade names or commercial products docs not constitute endorsement or recommendation for use. Neither the United States Government nor any of its employees, contractors, or their employees make any warranty, expressed or implied, or assume any legal liability or responsibility for any third party's use of or the results of such use of any information, apparatus, product, or process discussed in this document, or represent that its use by such party would not infringe on privately owned rights. The procedures described in this document arc intended for use in laboratories when analyzing environmental samples in support of remediation efforts following a homeland security incident. The (culture-based) procedures provide viability determination and identification as either qualitative or quantitative results. The sample preparation procedures arc deemed the most appropriate for the wide variety of matrices to be examined. To the extent possible, these procedures were developed to be consistent with other federal agency procedures. These procedures do not include the sample collection, rapid screening, field techniques, or molecular techniques that may accompany laboratory analysis. Questions concerning this document or its application should be addressed to: Sanjiv R. Shah National Homeland Security Research Center U.S. Environmental Protection Agency 1200 Pennsylvania Avenue, NVV USEPA-8801RR Washington. DC 20460 (202) 564-9522 shah. saniiv@epa. gov If you have difficulty accessing this PDF document, please contact Kathy Nickel (Nickel.Kathv@epa.gov) or Amelia McCall (McCall.Amelia@epa.gov) for assistance. ------- Contents Acknowledgments iii Disclaimer iv I.0 Scope and Application 1 2.0 Summary of Protocol 3 3.0 Acronyms and Abbreviations 5 4.0 Interferences and Contamination 7 5.0 Safety 9 5.1 Laboratory Hazards 9 5.2 Recommended Precautions 9 6.0 Equipment and Supplies 11 7.0 Reagents and Standards 13 8.0 Calibration and Standardization 19 9.0 Quality Control 21 9.1 General 21 9.2 Negative Controls 21 9.3 Positive Controls 21 9.4 Method Blank 21 9.5 Media Sterility Check 22 10.0 Procedures 23 10.1 Qualitative Sample Analysis 23 10.2 Quantitative Sample Analyses 23 10.3 Immunomagnetic Separation and Concentration 23 10.4 Isolation on Selective Agars 24 10.5 Serological Analyses 24 10.6 Isolation on TSA Plates 24 10.7 Biochemical Analyses 24 10.8 Summary of Positive and Negative Control, and /•'. coli 0157:H7 Results 25 II.0 Data Analy sis and Bacterial Density Calculation 27 11.1 Most Probable Number (MPN) Technique 27 11.2 Calculation of MPN 27 12.0 Protocol Performance 33 13.0 Pollution Prevention 35 14.0 Waste Management 37 V ------- 15.0 References 16.0 Flowcharts and Diagrams. vi ------- 1.0 Scope and Application 1.1 This Standard Analytical Protocol (SAP) is for the identification, confirmation, and enumeration of Escherichia coli 0157:H7 (E. coli 0157:H7) in water samples using selective and non-selective media followed by biochemical characterization and serological confirmation. 1.2 This protocol has been adapted from the journal article "Evaluation of Techniques for Enrichment and Isolation of Escherichia coli 0157:H7 from Artificially Contaminated Sprouts" by Weagant and Bound (Reference 15.1), and is for use by laboratories when analyzing samples in support of U.S. Environmental Protection Agency (EPA) homeland security efforts. 1.3 E. coli 0157:H7 is the causative agent of entcroheinorrhagic diarrhea. Due to the infectious nature of the bacterium and the potential for transmission to humans, all procedures should be performed in laboratories that use. at a minimum, biological safety level (BSL)-2 practices (Reference 15.2). Use of a biological safety cabinet (BSC) is recommended for any aerosol-generating procedures. 1.4 All sample handling, analysis, and reporting of results must be performed in accordance with established guidelines. Laboratories must have requisite resources in place prior to use of these procedii 1.5 This protocol is not intended for use as a test for microorganisms other than E. coli 0157:H7 and the matrices described. 1 ------- 2 ------- 2.0 Summary of Protocol 2.1 E. coli 0157:H7 can be identified in a variety of water samples using selective media, and biochemical and serological analyses. Bacterial densities can be estimated using the most probable number (MPN) approach. 2.2 For qualitative results, samples arc diluted 1:1 in double-strength modified buffered peptone water (mBPVV). Samples arc incubated at 36.0°C ± 1.0°C for 2 - 2.5 hours followed by incubation at 42.0°C ± 0.5°C for a total of 20 - 24 hours. 2.3 For quantitative results, samples arc analy/cd as received. All samples arc analy/cd using the MPN technique in mBPVV and incubated at 36.0°C ± 1.0°C for 2 - 2.5 hours followed by incubation at 42.0°C ± 0.5°C for a total of 20 - 24 hours. 2.4 Broth cultures (MPN and qualitative analyses tubes) with positive growth (turbidity) arc submitted to immunomagnetic separation (IMS) and sub-cultured onto tellurite cefixime sorbitol MacConkcy (TC-SMAC) and Rainbow® agars. 2.5 After growth at 42.0°C ± 0.5°C for 18 - 24 hours, TC-SMAC plates arc examined for 2 - 3 mm colorlcss/gray colonics typical of E. coli 0157:H7. On Rainbow® plates, typical colonics arc black/gray. Isolated typical colonics arc submitted to biochemical and serological confirmation. Serological confirmation is by agglutination using E. coli 0157 and H7 antiserum, followed by biochemical characterization using commercially available test strips (e.g., API 20E® or equivalent) or with a group of selected individual biochemical tests. 2.6 Broth cultures (MPN and qualitative analysis tubes) concentrated by IMS may be subjected to real-time polymerase chain reaction (PCR) confirmation in place of biochemical and serological confirmation. 2.7 Quantification of E. coli 0157:H7 is determined using the MPN technique (Flowchart 16.1). Tubes that arc confirmed positive for /•'. coli 0157:H7 arc used to determine MPN. Note: Typing by serology for the H7 antigen or PCR for the H7 gene was not conducted during the single-laboratory verification study. To confirm E. coli 0157:H7, additional serological or PCR analyses would be necessary. 3 ------- ------- 3.0 Acronyms and Abbreviations ASTM ASTM International (formerly American Society for Testing and Materials) ATCC® American Type Culture Collection BSC Biological safety cabinet BSL Biological safety level °C Degrees Celsius CT Cefixime potassium tellurite EPA U.S. Environmental Protection Agency g Gram(s) IMS Immunomagnetic separation L Liter(s) liL Microlitcr(s) \im Micrometer(s) mBPW Modified buffered peptone water mg Milligrain(s) mL Milliliter! s) mm Millimcter(s) MPN Most probable number N Normal NCTC National Collection of Type Cultures NHSRC National Homeland Security Research Center NIST National Institute of Standards and Technology PBS Phosphate buffered saline PGR Polymerase chain reaction PPE Personal protective equipment, i.e., gloves, goggles, laboratory coat, etc. psi Pounds per square inch QC Quality control SAP Standard Analytical Protocol TC-SMAC Tellurite cefixime sorbitol MacConkey agar TSA Tryptic soy agar w/v Weight to volume ratio 5 ------- 6 ------- 4.0 Interferences and Contamination 4.1 Low recoveries of E. coli 0157:H7 may be caused by the presence of either high numbers of competing or inhibitory organisms (e.g., other Entcrobactcriaceac). or toxic substances (e.g., metals, organic compounds). 4.2 A viable but non-culturable state of E. coli 0157:H7 may also account for lower recoveries (Reference 15.3). ------- ------- 5.0 Safety 5.1 Laboratory Hazards To prevent transmission, disposable gloves should be worn when working with this organism. Hands should be washed immediately following removal of gloves. Direct and indirect contact of intact or broken skin with cultures and/or contaminated laboratory surfaces, accidental parenteral inoculation, and rarely, exposure to infectious aerosols are the primary hazards to laboratory personnel. Staff should apply safety procedures used for pathogens when handling all samples. 5.2 Recommended Precautions 5.2.1 E. coli 0157:H7 is a BSL-2 pathogen and all procedures should be performed in laboratories that use, at a minimum, BSL-2 practices (Reference 15.2). This includes prohibiting eating, drinking, smoking, handling contact lenses, applying cosmetics, and storing food and drink in the laboratory. 5.2.2 A Class 11 BSC is recommended for sample manipulations where the risk of aerosol production is high. Production of aerosols should be avoided. 5.2.3 Disposable materials arc recommended for sample manipulation. 5.2.4 Mouth-pipetting is prohibited. 5.2.5 The analyst must know and observe normal safety procedures required in a microbiology laboratory. These procedures must be followed while preparing, using, and disposing of media, cultures, reagents, and materials, and while operating sterilization equipment. 5.2.6 Personal Protective Equipment (PPE) 5.2.6.1 Disposable nitrile gloves should be worn at all times to prevent contact with infectious materials. Gloves should be changed whenever they are visibly soiled. Aseptic technique should be used when removing gloves and other protective clothing. 5.2.6.2 Protective goggles and/or non-breakable, chemical-resistant glasses should be worn, as appropriate. 5.2.6.3 Protective laboratory coats covering arms and clothing and closed in the front should be worn at all times. Laboratory coats that become soiled should be changed. 5.2.7 This protocol docs not address all safety issues associated with its use. Please refer to Biosafety in Microbiological and Biomedical Laboratories (BMBL), 5th Edition (Reference 15.2) for additional safety information. A reference file of Material Safety Data Sheets should be available to all personnel involved in analyses. 9 ------- 10 ------- 6.0 Equipment and Supplies 6.1 Autoclave or steam sterilizer, capable of achieving 121°C (15 pounds per square inch [psi]) for 15 minutes 6.2 Autoclave bags, aluminum foil, or kraft paper 6.3 Balance, analytical, with ASTM Class S reference weights, capable of weighing 20 g ± 0.001 g 6.4 Balance, top loading, with Class S reference weights, capable of weighing 100 g ± 0.1 g 6.5 Bead rotator (Dynabeads® Sample Mixer or equivalent), optional 6.6 Beakers, glass or plastic (assorted sizes) 6.7 Biological safety cabinet. Class 11 (optional) 6.8 Borosilicate glass or plastic screw-cap, wide-mouth bottles, sterile (e.g., 250 inL) 6.9 Borosilicate glass culture tubes, with autoclavable screw or snap caps (25 x 150 mm) 6.10 Erlcnincyer flasks (500 inL. I L, 2 L) 6.11 Filters, for reagent sterilization, sterile (0.22 jim pore size), and filter syringes, sterile 6.12 Graduated cylinders (assorted sizes) 6.13 Gloves, sterile, nitrile or equivalent 6.14 lininunomagnetic separator (Dynal® Bead Separator or equivalent) 6.15 Incubators, microbiological type, maintained at 36.0°C ± 1.0°C and 42.0°C ± 0.5°C 6.16 Inoculation loops, sterile, disposable ------- 6.17 Parafilm™ or equivalent 6.18 Petri dishes, sterile, plastic (15 x 100 mm) 6.19 pH meter 6.20 Pipettes, standard tip. sterile, plastic, disposable (assorted si/cs) 6.21 Pipetting device (automatic or equivalent) 6.22 Stirring hotplates and stir bars 6.23 Test tube racks 6.24 Thermometer, National Institute of Standards and Technology (NIST)-traccable 6.25 Tissues, lint-free (Kimwipes® or equivalent) 6.26 Vortex 6.27 Waterbath, maintained at 45°C - 50°C 6.28 Weigh paper and boats ------- 7.0 Reagents and Standards 7.1 Reagent-grade chemicals must be used in all tests. Unless otherwise indicated, reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society (Reference 15.4). For suggestions regarding the testing of reagents not listed by the American Chemical Society, see AnalaR Standards for Laboratory Chemicals (Reference 15.5) and United States Pharmacopeia and National Formulary 24 (Reference 15.6). 7.2 Whenever possible, use commercially available culture media. The agar used in the preparation of culture media must be of microbiological grade. Storage requirements for prepared media and reagents are provided in Table 2 (Section 7.18). 7.3 Reagent-grade water must conform to specifications in Standard Methods for the Examination of Water and Wastewater, 21" Edition, Section 9020 (Reference 15.7). 7.4 Dilution Water Dilution water is a phosphate buffer and is also commonly referred to as Butterfield buffer or phosphate buffered dilution water. Commercially prepared reagents are recommended (Hardy Diagnostics D699 or equivalent). 7.4.1 Composition of stock phosphate buffer solution: Monopotassium phosphate (KH2P04) Reagent-grade water 7.4.2 Prepare stock phosphate buffer by dissolving 34.0 g monopotassium phosphate in 0.5 L of reagent-grade water. Adjust pH to 7.2 ± 0.5 with 1 N sodium hydroxide and dilute to 1.0 L with reagent-grade water. Sterilize by filtration or autoclave at 121 °C (15 psi) for 15 minutes. 7.4.3 Composition of stock magnesium chloride solution: Magnesium chloride hcxahydrate (MgCl;«6H,0) Reagent-grade water 7.4.4 Prepare stock magnesium chloride solution by dissolving 81.1 g of magnesium chloride hcxahydrate in 1.0 L of reagent-grade water. Sterilize by filtration or autoclave at 121 °C (15 psi) for 15 minutes. 7.4.5 After sterilization, store the stock solutions in the refrigerator. Handle aseptically. If evidence of mold or other contamination appears, the affected stock solution should be discarded and a fresh solution should be prepared. 7.4.6 Prepare phosphate buffered dilution water by adding 1.25 inL stock phosphate buffer solution and 5.0 inL stock magnesium chloride solution to 1.0 L of reagent-grade water. Autoclave at 121 °C (15 psi) for 15 minutes. 7.5 Phosphate Buffered Saline (PBS) Prepare reagent according to the following and store at <10°C and above freezing for a maximum of two weeks in tubes with loose caps or three months in screw-cap tubes. 13 34.0 g 0.5 L 81.1 g 1.0 L ------- 7.5.1 Composition: Monosodium phosphate (NaH2P04) 0.58 g Diosodium phosphate (Na2HP04) 2.50 g Sodium chloride 8.50 g Reagent-grade water 1.0 L 7.5.2 Dissolve reagents in 1.0 L reagent-grade water, adjust pH to 7.4 ± 0.2 with 1.0 N hydrochloric acid or 1.0 N sodium hydroxide, and dispense appropriate volumes in screw-cap bottles or tubes and autoclave at 121 °C (15 psi) for 15 minutes. 7.6 Modified Buffered Peptone Water (mBPW) Prepare IX, 2X, and 5X mBPW according to the following and store at <10°C and above freezing for a maximum of two weeks in tubes with loose caps or three months in screw-cap tubes. 7.6.1 Composition: IX 2X 5X Peptone 10.0 g 20.0 g 50.0 g Sodium chloride 5.0 g 10.0 g 25.0 g Disodium phosphate (Na2HP04) 3.6 g 7.2 g 18.0 g Monopotassium phosphate 1.5 g 3.0 g 7.5 g (KH2P04) Casamino acids 5.0 g 10.0 g 25.0 g Yeast extract 6.0 g 12.0 g 30.0 g Lactose 10.0 g 20.0 g 50.0 g Pyruvate 2.0 g 4.0 g 10.0 g Reagent-grade water 1.0 L 1.0 L 1.0 L 7.6.2 Add reagents to 950 niL of reagent-grade water and mix thoroughly using a stir bar. Adjust pH to 7.2 ± 0.2 with 1.0 N hydrochloric acid or 1.0 N sodium hydroxide and bring up to 1.0 L. Dispense 10 niL (IX and 2X) or 5 niL (5X) aliquots in 25 x 150 mm tubes and autoclave at 121 °C for 15 minutes. Cool to room temperature. 7.7 Tellurite Cefixime Sorbitol MacConkey Agar (TC-SMAC) Commercially prepared media is recommended. Dehydrated medium (Oxoid CM0813 or equivalent), with cefixime and potassium tellurite (CT) supplement (Oxoid SR172 or equivalent), or prepared plates (Oxoid P00702 or equivalent) may be used. If commercially prepared media are not available, prepare medium using procedures in Sections 7.7.1 through 7.7.4. 14 ------- 7.7.1 Composition: Peptone 20.0 g D-Sorbitol 10.0 g Bile salts No. 3 1.5 g Sodium chloride 5.0 g Agar 15.0 g Neutral red 0.03 g Crystal violet 0.001 g Reagent-grade water 1.0 L 7.7.2 Add reagents to 950 mL of reagent-grade water and mix thoroughly using a stir bar and hot plate. Boil for one minute with rapid stir bar agitation to dissolve completely. Adjust pH to 7.1 ± 0.2 with 1.0 N hydrochloric acid or 1.0 N sodium hydroxide and bring up to 1.0 L. Autoclave at 121 °C (15 psi) for 15 minutes. Cool to 45°C - 50°C in a waterbath. 7.7.3 Prepare CT supplement according to manufacturer's instructions and filter stcrili/c. 7.7.4 Prepare TC-SMAC plates by adding two reconstituted CT supplement vials to the cooled medium, swirling to mix. Final concentrations for cefixime and tellurite are 0.05 mg/L and 2.5 mg/L, respectively. Aseptically pour 12- 15 niL into each 15 x 100 mm sterile Petri plate. 7.8 Rainbow® Agar Commercially prepared dehydrated medium (Biolog 80101 or equivalent) is recommended. 7.8.1 Add 60.0 g dehydrated reagent to 1.0 L of reagent-grade water and mix thoroughly using a stir bar and hot plate. Boil gently to dissolve and autoclave at 121 °C (15 psi) for 15 minutes. Cool to 45°C - 50°C in a waterbath. 7.8.2 Prepare stock potassium tellurite (Sigma-Aldrich® P0677 or equivalent) solution by dissolving 0.008 g in 10.0 inL reagent-grade water and filter sterilizing. Prepare stock novobiocin (Sigma-Aldrich® N1628 or equivalent) by dissolving 0.010 g in 10 niL reagent-grade water and filter sterilizing. 7.8.3 Prepare plates by adding 1.0 inL each of tellurite and novobiocin stock solutions to the cooled medium, swirling to mix. Final concentrations should be 0.8mg/L and 10.0 mg/L, respectively, with medium pH of 7.9 - 8.3. Aseptically pour 12- 15 inL into each 15 x 100 mm sterile Petri plate. 7.9 Tryptic Soy Agar (ISA) Commercially prepared inediuin is recommended. Prepared plates (BBL™ 221803 or equivalent) or dehydrated media (BBL™ 211043 or equivalent) may be used. If coininercially prepared media are not available, prepare media using procedures in Sections 7.9.1 and 7.9.2. 15 ------- 7.9.1 Composition: Pancreatic digest of casein 15.0 g Papaic digest of soybean meal 5.0 g Sodium chloride 5.0 g Agar 15.0 g Reagent-grade water 1.0 L 7.9.2 Add reagents to 950 niL of reagent-grade water and mix thoroughly using a stir bar and hot plate. Heat to dissolve completely. Adjust pH to 7.3 ± 0.2 with 1.0 N hydrochloric acid or 1.0 N sodium hydroxide and bring up to 1.0 L. Autoclave at 121 °C (15 psi) for 15 minutes and cool to 45°C - 50°C in a waterbath. Ascptically pour 12 - 15 niL into each 15 x 100 mm sterile Petri plate. 7.10 E. coli 0157 IMS beads (Invitogen™ 71004 or equivalent) 7.11 IMS wash buffer: Add 50 jiL Tween® 20 to 100 niL of PBS. ensuring all of the Tween® 20 is expelled from the pipette tip; filter stcrili/c or autoclave at 121 °C (15 psi) for 15 minutes. 7.12 Saline, physiological (0.85% w/v): Dissolve 0.85 g NaCl in 100 niL of reagent-grade water. Autoclave at 121 °C (15 psi) for 15 minutes. Cool to room temperature. 7.13 E. coli 0157 latex agglutination reagent (Oxoid DR0620M or equivalent) 7.14 E. coli H7 latex agglutination reagent (Wellcolex® E. coli 0157:H7 Rapid Latex Agglutination Test or equivalent) 7.15 Biochemical test strip (bioMcrieux API 20E® or equivalent) 7.16 Oxidase reagent (BD™ DrySlide™ 231746 or equivalent) 7.17 Positive and negative control cultures that are to be used in the procedures in Section 10.0 are listed in Table 1, below. Use of these controls is discussed in Section 9.0. ------- Table 1. Positive and Negative Control Cultures for Described Tests Media/Tests Positive Control Negative Control TC-SMAC E. coli 0157:H7 (ATCC® 700728™ /NCTC 12900) E. coli (ATCC® 25922™) Rainbow® E. coli 0157:H7 (ATCC® 700728™ / NCTC 12900) E. coli (ATCC® 25922™) 0157 latex agglutination E. coli 0157:H7 (ATCC® 700728™/NCTC 12900) E. coli (ATCC® 25922™) H7 serum agglutination (Optional) E. coli 0157:H7 (ATCC® 700728™ / NCTC 12900) E. coli (ATCC® 25 922™) Biochemical test strip E. coli 0157:H7 (ATCC® 700728™ / NCTC 12900) Pseudomonas aeruginosa (ATCC® 27853™) Oxidase Pseudomonas aeruginosa (ATCC® 27853™) E. coli 0157:H7 (ATCC® 700728™ / NCTC 12900) 7.18 Storage temperatures and times for prepared media and reagents arc provided in Table 2. Follow manufacturers' guidelines for storage and expiration of all commercially prepared reagents. Table 2. Storage Temperatures and Times for Prepared Media and Reagents1 Media/Reagents Storage Temperature Storage Time Dilution water, PBS, saline (in screw-cap containers) <10°C and above freezing 3 months Tubes: mBPW <10°C and above freezing 2 weeks in loose-cap tubes 3 weeks in screw-cap tubes Plates: TC-SMAC, Rainbow®2, TSA <10°C and above freezing 2 weeks 1 If media reagent is refrigerated, remove from refrigerator 1-1.5 hours prior to inoculation to ensure that it reaches room temperature prior to use 2 Dehydrated medium is hygroscopic and light-sensitive; store tightly sealed and protected from light ------- 18 ------- 8.0 Calibration and Standardization 8.1 Check temperature in incubators twice daily, a minimum of four hours apart, to ensure operation is within stated limits of the protocol. Record daily measurements in an incubator log book. 8.2 Check temperature in rcfrigcrators/frcc/ers at least once daily to ensure operation is within stated limits of the protocol. Record daily measurements in a refrigcrator/frcc/cr log book. 8.3 Calibrate thermometers and incubators annually against a NIST-ccrtified thermometer or against a thermometer that meets the requirements of NIST Monograph SP 250-23 (Reference 15.8). Check mercury columns for breaks. 8.4 Calibrate pH meter prior to each use with two of three standards (e.g., pH 4.0, 7.0, or 10.0) closest to the range being tested. 8.5 Calibrate analytical and top-loading balances with ASTM Class S reference weights once per month, at a minimum. Check each day prior to use with Class S weights. 8.6 Calibrate micropipettors once per year. Spot-check micropipettor accuracy once per month by weighing a measured amount of reagent-grade water (1 jj.L = 1 mg). 8.7 Re-certify BSCs once per year. Re-certification must be performed by a qualified technician. 19 ------- 20 ------- 9.0 Quality Control 9.1 General Each laboratory that uses this protocol is required to operate a formal quality assurance program that addresses and documents instrument and equipment maintenance and performance, reagent quality and performance, analyst training and certification, and records storage and retrieval. Specific quality control (QC) procedures for use with this protocol arc discussed below. Note: Following testing and validation, this protocol will be updated to include QC criteria for initial and ongoing demonstration of capability as well as matrix spike/matrix spike duplicates. 9.2 Negative Controls 9.2.1 The laboratory should analyze negative controls to ensure that all media and reagents arc performing properly. Negative controls should be analyzed whenever a new batch of media or reagents is used. On an ongoing basis, the laboratory should analyze a negative control every day that samples arc analyzed. Recommended negative control organisms arc provided in Table 1 (Section 7.17), and descriptions of negative results arc provided in Table 3 (Section 10.8). 9.2.2 Analysis of negative controls is conducted by inoculating media and performing biochemical tests with known negative control organisms as described in Section 10.0. The negative control is treated as a sample and submitted to the same analytical procedures. 9.2.3 If a negative control fails to exhibit the appropriate response, check and/or replace the associated media, reagents, and/or the respective negative control organism, and re-analyze the appropriate negative control and corresponding sample(s). 9.2.4 Viability of the negative controls should be demonstrated on a monthly basis, at a minimum, using a non-selective media (e.g., TSA). 9.3 Positive Controls 9.3.1 The laboratory should analyze positive controls to ensure that all media and reagents arc performing properly. Positive controls should be analyzed whenever a new batch of media or reagents is used. On an ongoing basis, the laboratory should analyze a positive control every day that samples are analyzed. Recommended positive control organisms arc provided in Table 1 (Section 7.17), and descriptions of positive results arc provided in Table 3 (Section 10.8). 9.3.2 Analysis of positive controls is conducted by inoculating media and performing biochemical tests with known positive organisms as described in Section 10.0. The positive control is treated as a sample and submitted to the same analytical procedures. 9.3.3 If a positive control fails to exhibit the appropriate response, check and/or replace the associated media, reagents, and/ or the positive control organism, and rc-analy/c the appropriate positive control and corresponding sample(s). 9.4 Method Blank On an ongoing basis, every day that samples arc analyzed, the laboratory should analyze a method blank using sterile dilution water or PBS (Sections 7.4 and 7.5, respectively) to verify the sterility of equipment, materials, and supplies. The method blank is treated as a sample and submitted to the same analytical procedures. Absence of growth indicates freedom from contamination. 21 ------- 9.5 Media Sterility Check Test sterility of dilution water, PBS. mBPW, and TSA by incubating one unit (tube or plate) from each batch at 35.0°C - 37.0°C for 24 ± 2 hours and observing for growth. Test sterility of TC-SMAC and Rainbow* by incubating one unit (tube or plate) from each batch at 42.0°C ± 0.5°C for 24 ± 2 hours and observing for growth. Absence of growth indicates the media arc sterile. On an ongoing basis, a media sterility check should be done every day that samples arc analyzed. ------- 10.0 Procedures Process samples promptly upon receipt, allowing no more than six hours to elapse from the time of sample collection to the start of sample processing, which should be completed within two hours. E. coli 0157:H7 is a pathogen, and all samples should be handled with caution, using appropriate BSL-2 procedures and PPE. A Class 11 BSC is recommended for sample manipulations where the risk of aerosol production is high, such as vigorous shaking. 10.1 Qualitative Sample Analysis Add a sample volume (e.g., 200 inL) to an equal volume of double-strength mBPVV (Section 7.6). Incubate at 36.0°C ± 1.0°C for 2.0 - 2.5 hours, non-shaking. Transfer samples to 42.0°C ± 0.5°C and continue incubation, non-shaking, for a total of 20 - 24 hours. After incubation, proceed to Section 10.4 for selective isolation of E. coli 0157:H7. 10.2 Quantitative Sample Analyses A multiple-tube assay incorporating differential sample volumes is used to estimate E. coli 0157:H7 densities in undiluted or diluted samples. If low levels of E. coli 0157:H7 are suspected, larger sample volumes (20.0 inL of original sample) should be used to inoculate the first row of tubes in the series. If high levels of E. coli 0157:H7 are suspected, additional serial dilutions should be used. See Flowchart 16.1 for an overv iew of the sample dilution and inoculation scheme. A minimum sample volume of 156 inL is required if 20 inL volumes arc used to inoculate the first row of tubes. 10.2.1 Sample inoculation Arrange mBPVV tubes in three rows (5 inL of 5X, 10 inL of 2X, and 10 inL of IX) of five tubes each. Inoculate the first row of tubes (5 inL of 5X mBPVV) with 20 inL of the undiluted sample. Inoculate 10 inL of the undiluted sample into each of the tubes in the second row (5 inL of 3X mBPVV). Inoculate 1 inL from the initial sample into each of the tubes in the third row (IX mBPVV). See Flowchart 16.1 for an overview of the sample inoculation scheme. 10.2.2 Sample dilutions Samples may require serial dilution prior to inoculation due to high levels of E. coli 0157:H7. If analyzing serially diluted samples, 1.0 inL of each dilution will be used to inoculate each tube of IX mBPVV, as appropriate. 10.2.3 Growth Incubate tubes at 36.0°C ± 1.0°C for 2.0 - 2.5 hours, non-shaking. Transfer samples to 42.0°C ± 0.5°C and continue incubation, non-shaking, for a total of 20 - 24 hours. After incubation, proceed to Section 10.3 for selective separation and concentration of E. coli 0157:H7. 10.3 Immunomagnetic Separation and Concentration See Flowchart 16.2 for an overview of the colony identification procedures. From each tube with growth, conduct IMS as follows: 10.3.1 Suspend E. coli 0157:H7 beads by vortexing and add 20 pL of the bead suspension to a sterile. 1.5 inL - 2.0 inL tube. 10.3.2 Gently swirl contents of mBPVV tubes to mix, remove 1.0 inL of mBPVV culture, add to tube with beads, and tightly cap. Mix for 10 minutes at room temperature using the tube rotator. 10.3.3 Place tubes in magnetic holder, inverting tubes several times to ensure that beads arc concentrated in a pellet on the side of the tube; allow beads to settle for three minutes. Carefully aspirate liquid and discard. 10.3.4 Resuspcnd beads in l.O inL IMS wash buffer (Section 7.11) by inverting the tube several times. Place tubes in magnetic holder and allow beads to settle for three minutes. Aspirate wash buffer and resuspcnd the beads in 100 pL of IMS buffer. 23 ------- Note: IMS bead complex may be subjected to real-time PCR confirmation in place of, or in addition to, culture on selective media followed by biochemical and serological confirmation. 10.4 Isolation on Selective Agars 10.4.1 Pipette 50 pL (half the beads) onto Rainbow® agar; use a sterile loop to spread the 50-^iL aliquot over one-third of the plate then streak for isolation on the remaining portion of the plate. Repeat this procedure with the remaining 50 pL onto TC-SMAC. 10.4.2 Incubate Rainbow® and TC-SMAC plates for 18 - 24 hours at 42.0°C ± 0.5°C. On TC-SMAC, typical E. coli 0157:H7 colonics arc colorless and 2-3 mm in diameter. On Rainbow® agar, typical E. coli 0157:H7 colonics arc black/gray. Note: Colonies on Rainbow® agar tend to be much smaller and run together making it difficult to obtain well-isolated colonies for serological and biochemical confirmation. Prolonged incubation of TC-SMAC plates may result in colonies ofE. coli 0157:H7 losing their characteristic colorless appearance. Also, the color of sorbitol-positive colonies can fade, making them difficult to distinguish from sorbitol-negative colonies. Appropriate negative and positive controls should be analyzed to avoid confusion (Sections 9.2 and 9.3, respectively). 10.5 Serological Analyses The procedures for the use of latex agglutination kits arc provided in Sections 10.5.1 and 10.5.2. Section 10.5.3 provides an optional procedure for the use of antiserum for serological confirmation. 10.5.1 E. coli 0157 latex agglutination kit: Choose a well-isolated typical colony from each of the positive TC-SMAC and/ or Rainbow® plates and emulsify growth using sterile physiological saline (Section 7.12). Evaluate according to manufacturer's instructions. 10.5.2 Repeat Section 10.5.1 using H7 latex agglutination reagent. Note: Identification of the H7flagellar antigen is usually conducted by reference laboratories and may be difficult since isolates often require multiple passages in motility medium before the antigen is detected. PCR identification of the gene for the H7 antigen may be conducted in place of serology. Neither of these procedures was verified during the single-laboratory study. 10.5.3 E. coli 0157 or H7 antiserum (optional): Choose a well-isolated typical colony from each of the positive TC-SMAC and/or Rainbow® plates and emulsify growth using sterile physiological saline. Place two discrete drops of emulsified growth onto a slide. To the first drop of emulsified growth, add one drop of 0157 antiserum. To the second drop of emulsified growth, add one drop of sterile saline (as a visual comparison). Observe under magnification for an agglutination reaction, which indicates a positive result. E. coli 0157:H7 is agglutination-positive for 0157 antiserum. Results should be compared with those for positive and negative controls (Table 1) analyzed at the same time. 10.6 Isolation on TSA Plates 10.6.1 Streak one 0157 scralogical-positivc isolate onto a TSA plate from each serology-positive TC-SMAC or Rainbow® plate. For spiked samples with no background, a single scralogical-positivc isolate from each dilution should be streaked onto a TSA plate. Incubate the plates at 36.0°C ± 1.0°C for 24 ± 2 hours. 10.6.2 Seal the TC-SMAC and Rainbow® plates with Parafilm™ and store at <10°C and above freezing for use as backup/ archive plates. Use the TSA plates for biochemical analyses. 10.7 Biochemical Analyses Use a single, isolated, large colony (2-3 mm diameter) from each TSA plate for biochemical test strip and oxidase analyses. ------- 10.7.1 Oxidase Test(BD™ DrySlide™ 231746 or equivalent) Following manufacturer's instructions, transfer a small amount of growth from an isolated colony to the slide. Oxidasc-positivc bacteria turn the reagent dark purple within 20 seconds. E. coli 0157:H7 is oxidasc-ncgativc. Results should be compared with those for positive and negative controls (Table 3) analyzed at the same time. 10.7.2 Biochemical Test Strips (API 20E® or equivalent) Emulsify the remainder of the colony in 0.85% NaCl. Follow manufacturers' instructions to inoculate wells and add appropriate reagents. Incubate test strip according to manufacturers' instructions. Add additional reagents, read, and record results. Note: Individual biochemical tests may be used instead of biochemical test strips to identify E. coli 0157 :H7. 10.8 Summary of Positive and Negative Control, and E. coli 0157:H7 Results Typical results are provided in Table 3. Table 3. Positive and Negative Result Descriptions and K coli 0157:H7 Results Medium/Test K. coli 0157:H7 Results Positive Control Result and Description Negative Control Result and Description TC-SMAC Positive Colorless colonies (sorbitol not fermented) Pink to red colonies (sorbitol fermented) Rainbow® Positive Black to gray colonies (glucoronidase-negative) Pink to magenta colonies (glucoronidase-positive) Oxidase Negative Purple to violet color change within 20 seconds Colorless or very light pink color change over time Biochemical test strip Consult manufacturers' instructions 0157 antiserum Positive Agglutination No agglutination H7 antiserum (Optional) Positive Agglutination No agglutination 25 ------- 26 ------- 11.0 Data Analysis and Bacterial Density Calculation 11.1 Most Probable Number (MPN) Technique Estimation of bacterial densities may be determined based on the number of tubes positive for /•'. coli 0157:H7 by biochemical and serological or by PGR confirmation. 11.2 Calculation of MPN If only three rows of tubes were analyzed. identify appropriate MPN value using either Table 5 or 6, depending on volumes assayed. If more than three rows of tubes were analy/cd. the appropriate rows must be selected and MPN value calculated as described in Sections 11.2.1 and 11.2.2. Table 5 should only be used for volumes of 20.0 mL. 10.0 mL. and 1.0 mL. To select MPN values for volumes of 10.0 mL or less, use Table 6 (Sections 11.2.1 and 11.2.2). 11.2.1 Selection of Tubes If more than three rows of tubes arc inoculated with sample (e.g., volumes/dilutions), select the most appropriate rows of tubes according to the criteria listed in Sections 11.2. l .l to 11.2.1.5. Examples of row selections and MPN/1(H) mL values arc provided in Table 4. 11.2.1.1 Choose the smallest volume or the highest dilution giving positive results in all five tubes inoculated plus the two succeeding lower concentrations. In Example A from Table 4, 10 mL is a smaller volume than 20 mL and is the lowest volume giving positive results in all five tubes. 11.2.1.2 If the largest volume tested has less than five tubes with positive results, select it and the next two smaller volumes (Table 4, Examples B and C). 11.2.1.3 When a positive result occurs in a smaller volume than the three rows selected according to the rules above, change the selection to the largest volume that has less than five positive results and the next two smaller volumes (Table 4, Example D). 11.2.1.4 When the selection rules above have left unsclected any smaller volumes with positive results, add those positive tubes to the row of tubes for the smallest volume selected (Table 4, Example E). 11.2.1.5 If there were not enough lower volumes analyzed to select three dilutions using the rules above, then select the three smallest volumes (Table 4, Example F). Table 4. Examples of Appropriate Tube Selection and MPN/100 mL1 Example 20 mL 10 mL 1.0 mL 0.1 mL Significant Dilutions Table MPN Index MPN/100 mL A 5/5 5/5 3/5 0/5 5-3-0 6 0.792 79.2 B 4/5 5/5 1/5 0/5 4-5-1 5 0.1524 15.24 C 0/5 1/5 0/5 0/5 0-1-0 5 0.0067 0.67 D 5/5 3/5 1/5 1/5 3-1-1 6 0.137 13.7 E 4/5 4/5 0/5 1/5 4-4-1 5 0.1181 11.81 F 5/5 >¦- 5/5 2/5 5-5-2 6 5.422 542.2 1 Appropriate volumes are underlined and the largest sample volumes analyzed are highlighted 27 ------- 11.2.2 For calculation of MPN/100 mL when additional dilutions arc analyzed (e.g., 102, 103), obtain the MPN index value from Table 6 using the number of positive tubes in the three selected dilutions. Calculate MPN/100 mL using the equation below. MPN Index from Table 6 MPN/100 mL = x 100 Middle volume analyzed in the scries used for MPN determination For example, a dilution series of 103, 10 4, 10 5, with the following positive tubes 5, 1, 0, respectively would be: 0.329 MPN /100 mL = x 100 = 3.29 x 105 10"4 28 ------- Table 5. MPN Index and 95% Confidence Limits for Various Combinations of Positive Results When Five Tubes are Used and Sample Inoculation Volumes are 20.0,10.0, and 1.0 mL1 Combination of Positives MPN Index 95% Confidence Limits Combination of Positives MPN Index 95% Confidence Limits Lower Upper Lower Upper 0-0-0 0.006473 .... 0.0223 1-3-0 0.0312 0.0055 0.0678 0-0-1 0.0065 0.0012 0.0223 1-3-1 0.0393 0.0092 0.0821 0-0-2 0.0130 0.0012 0.0352 1 -3-2 0.0475 0.0132 0.0967 0-0-3 0.0195 0.0012 0.0472 1 -3-3 0.0559 0.0173 0.1119 0-0-4 0.0262 0.0033 0.0589 ] -3-4 0.0644 0.0216 0.1277 0-0-5 0.0328 0.0062 0.0706 1-3-5 0.0730 0.0260 0.1444 0-1-0 0.0067 0.0012 0.0228 1-4-0 0.0409 0.0099 0.0849 0-1-1 0.0134 0.0012 0.0360 1-4-1 0.0495 0.0141 0.1002 0-1-2 0.0202 0.0012 0.0483 1-4-2 0.0583 0.0185 0.1163 0-1-3 0.0270 0.0037 0.0604 1-4-3 0.0672 0.0231 0.1331 0-1-4 0.0339 0.0067 0.0725 1-4-4 0.0763 0.0277 0.1509 0-1-5 0.0408 0.0099 0.0847 1-4-5 0.0855 0.0324 0.1700 0-2-0 0.0138 0.0012 0.0367 1 -5-0 0.0517 0.0152 0.1042 0-2.-1 0.0208 0.0012 0.0495 1-5-1 0.0609 0.0199 0.1212 0-2-2 0.0279 0.0040 0.0619 1-5-2 0.0703 0.0247 0.1391 0-2-3 0.0350 0.0072 0.0745 1-5-3 0.0799 0.0296 0.1583 0-2-4 0.0422 0.0106 0.0871 1-5-4 0.0897 0.0346 0.1790 0-2-5 0.0494 0.0141 0.1001 1-5-5 0.0998 0.0397 0.2015 0-3-0 0.0215 0.0012 0.0507 2-0-0 0.0155 0.0012 0.0404 0-3-1 0.0288 0.0044 0.0636 2-0-1 0.0226 0.0018 0.0526 0-3-2 0.0362 0.0077 0.0766 2-0-2 0.0303 0.0051 0.0662 0-3-3 0.0437 0.0113 0.0898 2-0-3 0.0382 0.0087 0.0801 0-3-4 0.0512 0.0051 0.1243 2-0-4 0.0462 0.0125 0.0943 0-3-5 0.0588 0.0095 0.1428 2-0-5 0.0543 0.0165 0.1090 0-4-0 0.0299 0.0049 0.0654 2-1-0 0.0234 0.0022 0.0540 0-4-1 0.0375 0.0084 0.0/89 2-1-1 0.0315 0.0056 0.0683 0-4-2 0.0453 0.0121 0.0927 2-1-2 0.0397 0.0094 0.0827 0-4-3 0.0531 0.0160 0.1069 2-1-3 0.0480 0.0134 0.0976 0-4-4 0.0611 0.0200 0.1216 2-1-4 0.0565 0.0177 0.1131 0-4-5 0.0691 0.0241 0.1369 2-1-5 0.0652 0.0221 0.1293 0-5-0 0.0390 0.0090 0.0814 2-2-0 0.0327 0.0062 0.0705 0-5-1 0.0470 0.0129 0.0958 2-2-1 0.0413 0.0101 0.0856 0-5-2 0.0553 0.0170 0.1107 2-2-2 0.0501 0.0144 0.1013 0-5-3 0.0636 0.0212 0.1262 2-2-3 0.0590 0.0189 0.1176 0-5-4 0.0720 0.0255 0.1425 2-2-4 0.0681 0.0236 0.1349 0-5-5 0.0806 0.0299 0.1596 2-2-5 0.0774 0.0283 0.1533 1-0-0 0.0072 0.0012 0.0241 2-3-0 0.0431 0.0110 0.0887 1-0-1 0.0139 0.0012 0.0369 2-3-1 0.0523 0.0155 0.1053 1-0-2 0.0209 0.0012 0.0497 2-3-2 0.0617 0.0203 0.1227 1-0-3 0.0281 0.0041 0.0623 2-3-3 0.0714 0.0252 0.1412. 1-0-4 0.0353 0.0073 0.0749 2-3-4 0.0813 0.0303 0.1611 1-0-5 0.0425 0.0107 0.0878 2-3-5 0.0914 0.0354 0.1826 1-1-0 0.0144 0.0012 0.0377 2-4-0 0.0547 0.0168 0.1098 1-1-1 0.0217 0.0013 0.0509 2-4-1 0.0647 0.0218 0.1284 1-1-2 0.0290 0.0045 0.0640 2-4-2 0.0750 0.0271 0.1484 1-1-3 0.0365 0.0079 0.0771 2-4-3 0.0855 0.0325 0.1700 1-1-4 0.0441 0.0115 0.0905 2-4-4 0.0964 0.0380 0.1937 1-1-5 0.0517 0.0153 0.1043 2-4-5 0.1076 0.0436 0.2201 1 -2-0 0.0224 0.0017 0.0523 2-5-0 0.0681 0.0235 0.1349 1-2-1 0.0301 0.0050 0.0658 2-5-1 0.079: 0.0292 0.1566 1-2-2 0.0379 0.0085 0.0795 2-5-2 0.0904 0.0349 0.1805 1 -2-3 0.0457 0.0123 0.0935 2-5-3 0.1021 0.0409 0.2070 1-2-4 0.0537 0.0162 0.1079 2-5-4 0.1143 0.0469 0.2372 1-2-5 0.0618 0.0203 0.1229 2-5-5 0.1268 0.0531 0.2725 ------- Table 5. MPN Index and 95% Confidence Limits for Various Combinations of Positive Results When Five Tubes are Used and Sample Inoculation Volumes are 20.0,10.0, and 1.0 mL (cont.)1 Combination of Positives MPN Index 95% Confidence Limits Combination of Positives MPN Index 95% Confidence Limits Lower Upper Lower Upper 3-0-0 0.0255 0.0028 0.0585 4-3-0 0.0797 0.0295 0.1579 3-0-1 0.0330 0.0063 0.0710 4-3-1 0.0937 0.0366 0.1877 .1-0-2 0.0417 0.0103 0.0863 4-3-2 0.1086 0.0441 0.2228 3-0-3 0.0506 0.0147 0.1023 4-3-3 0.1245 0.0520 0.2656 3-0-4 0.0598 0.0193 0.1191 4-3-4 0.1414 0.0602 0.3218 3-0-5 0.0691 0.0241 0.1368 4-3-5 0.1595 0.0686 0.4067 3-1-0 0.0344 0.0069 0.0734 4-4-0 0.1012 0.0404 0.2049 3-1-1 0.0435 0.0112 0.0896 4-4-1 0.1181 0.0489 0.2476 3-1-2 0.0529 0.0159 0.1065 4-4-2 0.1364 0.0578 0.3038 3-1-3 0.0626 0.0207 0.1244 4-4-3 0.1563 0.0672 0.3890 3-1-4 0.0725 0.0258 0.1434 4-4-4 0.1780 0.0770 0.5273 3-1-5 0.0827 0.0310 0.1640 4-4-5 0.2015 0.0873 0.6411 3-2-0 0.0456 0.0122 0.0932 4-5-0 0.1304 0.0549 0.2836 3-2-1 0.0555 0.0171 0.1112 4-5-1 0.1524 0.0653 0.3687 3-2-2 0.0657 0.0223 0.1303 4-5-2 0.1769 0.0766 0.5210 3-2-3 0.0763 0.0277 0.1510 4-5-3 0.2046 0.0886 0.6528 3-2-4 0.0872 0.0333 0.1735 4-5-4 0.2357 0.1015 0.7516 3-2-5 0.0984 0.0390 0.1984 4-5-5 0.2708 0.11 50 0.8426 3-3-0 0.0583 0.0186 0.1164 5-0-0 0.0549 0.0162 0.1116 3-3-1 0.0693 0.0241 0.1371 5-0-1 0.0637 0.0213 0.1265 3-3-2 0.0806 0.0299 0.1597 5-0-2 0.0763 0.0277 0.1510 3-3-3 0.0924 0.0359 0.1847 5-0-3 0.0896 0.0345 0.1787 3-3-4 0.1046 0.0421 0.2128 5-0-4 0.1037 0.0417 0.2107 3-3-5 0.1173 0.0484 0.2452 5-0-5 0.0953 0.0165 0.2234 3-4-0 0.0733 0.0262 0. i 450 5-1-0 0.0678 0.0234 0.1344 3-4-1 0.0856 0.0325 0.1 700 5-1-1 0.0816 0.0304 0.1618 3-4-2 0.0984 0.0390 0.1982 5-1-2 0.0963 0.0379 0.1936 3-4-3 0.1118 0.0457 0.2307 5-1-3 0.1121 0.0459 0.2316 3-4-4 0.1258 0.0526 0.2695 5-1-4 0.1291 0.0542 0.2796 3-4-5 0.1405 0.0597 0.3184 5-1-5 0.1293 0.0304 0.3090 3-5-0 0.0913 0.0354 0.1825 5-2-0 0.0879 0.0337 0.1751 3-5-1 0.1055 0.0426 0.2150 5-2-1 0.1046 0.0421 0.2128 3-5-2 0.1204 0.0500 0.2538 5-2-2 0.1227 0.0511 0.2605 3-5-3 0.1362 0.0577 0.3029 5-2-3 0.1427 0.0608 0.3267 3-5-4 0.1529 0.0656 0.3715 5-2-4 0.1646 0.0710 0.4385 3-5-5 0.1707 0.0738 0.4795 5-2-5 0.1767 0.0503 0.5230 4-0-0 0.0381 0.0082 0.0809 5-3-0 0.1151 0.0474 0.2394 4-0-i 0.0461 0.0125 0.0942 5-3-1 0.1368 0.0580 0.3050 4-0-2 0.0563 0.0175 0.1126 5-3-2 0.1614 0.0695 0.4183 4-0-3 0.0668 0.0229 0.1323 5-3-3 0.1895 0.0821 0.5899 4-0-4 0.0777 0.0284 0.1537 5-3-4 0.2216 0.0957 0.7101 4-0-5 0.0890 0.0342 0.1773 5-3-5 0.2527 0.0814 0.7971 4-1-0 0.0484 0.0136 0.0983 5-4-0 0.1571 0.0676 0.3935 4-1-1 0.0592 0.0190 0.1181 5-4-1 0.1907 0.0826 0.5954 4-1-2 0.0705 0.0248 0.1395 5-4-2 0.2319 0.0999 0.7409 4-1-3 0.0822 0.0308 0.1631 5-4-3 0.2834 0.1196 0.8726 4-1-4 0.0945 0.0370 0.1894 5-4-4 0.3475 0.1417 1.0160 4-1-5 0.1072 0.0434 0.2193 5-4-5 0.4256 0.1437 1.1800 4-2-0 0.0626 0.0207 0.1244 5-5-0 0.2398 0.0762 0.7629 4-2.-! 0.0748 0.0269 0.1479 5-5-1 0.3477 0.1172 1.0160 4-2-2 0.0875 0.0335 0.1742 5-5-2 0.5422 0.1791 1.4190 4-2-3 0.1009 0.0403 0.2041 5-5-3 0.9178 0.2672 2.2010 4-2-4 0.1150 0.0473 0.2392 5-5-4 1.6090 0.3837 4.1030 4-2-5 0.1299 0.0546 0.2820 1.6090 0.3837 .... ^able was developed using the MPN calculator developed by Albert Klee (Reference 15.9) ------- Table 6. MPN Index and 95% Confidence Limits for Various Combinations of Positive Results When Five Tubes are Used and Sample Inoculation Volumes are 10.0,1.0, and 0.1 mL1 Combination of Positives MPN Index 95% Confidence Limits Combination of Positives MPN Index 95% Confidence Limits Lower Upper Lower Upper 0-0-0 0.018 ... 0.063 1 -3-0 0.083 0.012 0.196 0-0-1 0.018 0.003 0.063 1-3-1 0.104 0.020 0.243 0-0-2 0.036 0.003 0.101 1-3-2 0.125 0.029 0.296 0-0-3 0.054 0.003 0.137 1 -3-3 0.147 0.038 0.364 0-0-4 0.072 0.008 0.174 1 -3-4 0.169 0.048 0.460 0-0-5 0.091 0.015 0.212 1-3-5 0.191 0.057 0.566 0-1-0 0.018 0.003 0.063 1-4-0 0.105 0.021 0.245 0-1-1 0.036 0.003 0.101 1-4-1 0.127 0.030 0.300 0-1-2 0.055 0.003 0.138 1-4-2 0.148 0.039 0.370 0-1-3 0.073 0.008 0.175 1-4-3 0.170 0.048 0.468 0-1-4 0.091 0.015 0.214 1-4-4 0.193 0.058 0.575 0-1-5 0.110 0.023 0.256 1-4-5 0.215 0.067 0.657 0-2-0 0.037 0.003 0.102 1 -5-0 0.128 0.030 0.303 0-2-1 0.055 0.003 0.139 1-5-1 0.150 0.040 0.375 0-2-2 0.074 0.008 0.176 1-5-2 0.: 72 0.049 0.477 0-2-3 0.092 0.015 0.215 1 -5-3 0.195 0.058 0.583 0-2-4 0.111 0.023 0.258 1-5-4 0.217 0.068 0.664 0-2-5 0.129 0.031 0.307 1-5-5 0.240 0.077 0.731 0-3-0 0.056 0.003 0.140 2-0-0 0.045 0.003 0.119 0-3-1 0.074 0.009 0.177 2-0-1 0.068 0.006 0.164 0-3-2 0.093 0.016 0.217 2-0-2 0.091 0.015 0.213 0-3-3 0.112 0.023 0.260 2-0-3 0.115 0.025 0.269 0-3-4 0.130 0.031 0.310 2-0-4 0.139 0.035 0.338 0-3-5 0.149 0.039 0.372 2-0-5 0.164 0.046 0.437 0-4-0 0.075 0.009 0.179 2-1-0 0.068 0.006 0.166 0-4-1 0.094 0.016 0.219 2-1-1 0.092 0.015 0.216 0-4-2 0.112 0.024 0.263 2-1-2 0.116 0.025 0.272 0-4-3 0.131 0.032 0.313 2-1-3 0.141 0.036 0.343 0-4-4 0.150 0.040 0.377 2-1-4 0.166 0.046 0.447 0-4-5 0.169 0.048 0.462 2-1-5 0.192 0.057 0.571 0-5-0 0.094 0.016 0.221 2-2-0 0.093 0.016 0.218 0-5-1 0.113 0.024 0.265 2-2-1 0.118 0.026 0.276 0-5-2 0.133 0.032 0.317 2-2-2 0.143 0.036 0.349 0-5-3 0.152 0.040 0.382 2-2-3 0.168 0.047 0.456 0-5-4 0.171 0.048 0.470 2-2-4 0.194 0.058 0.581 0-5-5 0.190 0.056 0.563 2-2-5 0.221 0.069 0.675 1 -0-0 0.020 0.003 0.068 2-3-0 0.119 0.026 0.279 1 -0-1 0.040 0.003 0.108 2-3-1 0.144 0.037 0.355 1-0-2 0.060 0.003 0.149 . 2-3-2 0.170 0.048 0.467 1 -0-3 0.08 i 0.011 0.191 2-3-3 0.197 0.059 0.591 1 -0-4 0.101 0.019 0.236 2-3-4 0.223 0.070 0.683 1 -0-5 0.1 22 0.028 0.287 2-3-5 0.251 0.082 0.759 1-1-0 0.040 0.003 0.109 2-4-0 0.146 0.038 0.361 1-1-1 0.061 0.003 0.150 2-4-1 0.172 0.049 0.477 1-1-2 0.081 0.011 0.192 2-4-2 0.199 0.060 0.600 1-1-3 0.102 0.019 0.238 2-4-3 0.226 0.072 0.692 1-1-4 0.123 0.028 0.290 2-4-4 0.254 0.083 0.768 1-1-5 0.144 0.037 0.354 2-4-5 0.282 0.094 0.836 1 -2-0 0.061 0.003 0.151 2-5-0 0.174 0.050 0.488 1-2-1 0.082 0.012 0.194 2-5-1 0.201 0.061 0.610 1-2-2 0.103 0.020 0.240 0.229 0.073 0.700 1-2-3 0.124 0.029 0.293 2-5-3 0.257 0.084 0.776 1-2-4 0.146 0.038 0.359 2-5-4 0.286 0.095 0.845 1 -2-5 0.167 0.047 0.451 2-5-5 0.315 0.107 0.910 ------- Table 6. MPN Index and 95% Confidence Limits for Various Combinations of Positive Results When Five Tubes are Used and Sample Inoculation Volumes are 10.0,1.0, and 0.1 mL (cont.)1 Combination of Positives MPN Index 95% Confidence Limits Combination of Positives MPN Index 95% Confidence Limits Lower Upper Lower Upper 3-0-0 0.079 0.010 0.1 88 4-3-0 0.2.71 0.090 0.809 3-0-1 0.106 0.021 0.246 4-3-1 0.326 0.111 0.934 3-0-2 0.135 0.033 0.323 4-3-2 0.386 0.132 1.060 3-0-3 0.165 0.046 0.440 4-3-3 0.451 0.154 1.192 3-0-4 0.196 0.059 0.589 4-3-4 0.521 0.176 i .331 3-0-5 0.229 0.073 0.699 4-3-5 0.593 0.196 1.477 3-1-0 0.107 0.022 0.250 4-4-0 0.335 0.114 0.953 3-1-1 0.137 0.034 0.329 4-4-1 0.398 0.137 1.084 3-1-2 0.167 0.047 0.452 4-4-2 0.466 0.159 1.223 3-1-3 0.199 0.060 0.601 4-4-3 0.539 0.181 1.368 3-1-4 0.232 0.074 0.710 4-4-4 0.615 0.202 1.521 3-1-5 0.267 0.088 0.800 4-4-5 0.693 0.223 1.681 3-2-0 0.138 0.035 0.335 4-5-0 0.411 0.141 1.111 3-2-1 0.170 0.048 0.464 4-5-1 0.483 0. i 64 1.256 3-2-2 0.202 0.062 0.613 4-5-2 0.559 0.187 1.409 3-2-3 0.236 0.076 0.720 4-5-3 0.639 0.209 1.570 3-2-4 0.271 0.090 0.810 4-5-4 0.722 0.230 1.739 3-2-5 0.308 0.104 0.894 4-5-5 0.806 0.250 1.916 3-3-0 0.172 0.049 0.477 5-0-0 0.240 0.076 0.763 3-3-1 0.205 0.063 0.624 5-0-1 0.314 0.106 0.908 3-3-2 0.240 0.077 0.731 5-0-2 0.427 0.146 1.142 3-3-3 0.276 0.092 0.821 5-0-3 0.578 0.192 1.446 3-3-4 0.313 0.106 0.906 5-0-4 0.759 0.239 1.816 3-3-5 0.352 0.120 0.989 5-0-5 0.953 0.165 2.234 3-4-0 0.209 0.064 0.636 5-1-0 0.329 0.112 0.940 3-4-1 0.244 0.079 0.742 5-1-1 0.456 0.156 1.202 3-4-2 0.281 0.093 0.833 5-1-2 0.631 0.207 1.553 3-4-3 0.319 0.108 0.918 5-1-3 0.839 0.257 1.985 3-4-4 0.358 0.123 1.002 5-1-4 1.062 0.304 2.485 3-4-5 0.399 0.137 1.086 5-1-5 1.293 0.304 3.090 3-5-0 0.248 0.080 0.753 5-2-0 0.493 0.167 1.276 3-5-1 0.286 0.095 0.844 5-2-1 0.700 0.224 1.694 3-5-2 0.325 0.110 0.931 5-2-2 0.944 0.280 2.213 3-5-3 0.365 0.125 1.017 5-2-3 1.205 0.331 2.843 3-5-4 0.407 0.140 1.103 5-2-4 1.479 0.381 3.714 3-5-5 0.450 0.154 1.189 5-2-5 1.767 0.503 5.230 4-0-0 0.130 0.031 0.311 5-3-0 0.792 0.247 1.886 4-0-1 0.166 0.046 0.445 5-3-1 1.086 0.308 2.544 4-0-2 0.207 0.064 0.631 5-3-2 1.406 0.368 3.445 4-0-3 0.253 0.082 0.764 5-3-3 1.750 0.434 5.131 4-0-4 0.302 0.102 0.881 5-3-4 2.122 0.529 6.798 4-0-5 ¦ 0.355 0.121 0.996 5-3-5 2.527 0.814 7.971 4-1-0 0.169 0.048 0.460 5-4-0 1.299 0.348 3.108 4-1-1 0.212 0.066 0.646 5-4-1 1.724 0.429 4.975 4-1-2 0.258 0.085 0.779 5-4-2 2.212 0.563 7.087 4-1-3 0.310 0.105 0.898 5-4-3 2.781 0.882 8.600 4-1-4 0.365 0.125 1.016 5-4-4 3.454 1.159 10.110 4-1-5 0.425 0.145 1.138 5-4-5 4.256 1.437 11.800 4-2-0 0.216 0.067 0.661 5-5-0 2.398 0.762 7.629 4-2-1 0.264 0.087 0.794 5-5-1 3.477 1.172 10.160 4-2-2 0.317 0.108 0.915 5-5-2 5.422 1.791 14.190 4-2.-3 0.375 0.129 1.037 5-5-3 9.178 2.672 22.010 4-2-4 0.438 0.150 1.164 5-5-4 16.090 3.837 41.030 4-2-5 0.504 0.171 1.297 5-5-5 i 6.090 3.837 ^able was developed using the MPN calculator developed by Albert Klee (Reference 15.9) ------- 12.0 Protocol Performance Culture-based procedures were evaluated for /•'. coli 0157 in a reference matrix (PBS) and two matrices of interest (drinking water, surface water) during a single-laboratory study. Based on workgroup discussion, a nine-tube MPN as opposed to the standard fifteen-tube MPN was utilized for study analyses. It is expected that the SAP will be implemented using a standard 15-tube MPN. Details regarding laboratory method performance arc provided in the study report (Reference 15.10). Summary results using the optimized (i.e., final) procedure from this study arc provided in Table 7. Additional method performance data will be provided following testing in multiple laboratories. Table 7. K. coli 0157 Verification Results for Drinking Water and Surface Water Analyses using the "Optimized" Procedure Date Sample ID Spike Level (CFU/100 mL) MPN Combo K. coli 0157:H7 (MPN/100 mL) Percent Recovery (corrected for ambient concentrations') PBS Samples 3/16/2009 Unspiked NA 0-0-0 <1.08 Spiked 438 3-3-1 462.2 105 3-3-1 462.2 105 Drinking Water Samples 3/16/2009 Unspiked NA 0-0-0 <1.08 0-0-0 <1.08 Spiked 438 3-3-3 >1099 250 3-3-2 1099 250 3-3-2 1099 250 3-3-1 462.2 105 Surface Water Samples 12/1/2008 Unspiked NA u-u-u <3.008 0-0-0 <3.008 Spiked 863 3-3-2 1099 127 3-1-3 158.8 18 12/3/2008 Unspiked NA 0-0-1 3.008 0-0-1 3.008 Spiked 963 3-3-2 1099 114 3-3-3 >1099 114 12/8/2008 Unspiked NA 3-1-0 42.73 1-0-0 3.61 Spiked 1047 3-3-2 1099 103 3-3-2 1099 103 ------- Date Sample ID Spike Level (CFU/100 mL) MPN Combo K. coli 0157:H7 (MPN/KM) mL) Percent Recovery (corrected for ambient concentrations') 12/15/2008 Unspiked NA 2-1-0 14.69 1-2-2 19.5 Spiked 462 3-3-1 462.2 96 3-3-1 462.2 96 12/22/2008 Unspiked NA 3-1-0 42.73 0-0-1 3.008 Spiked 320 3-2-1 149.4 40 3-3-2 1099 336 1/6/2009 Unspiked NA 3-1-3 158.8 3-1-0 42.73 Spiked 713 3-3-2 1099 140 3-3-2 1099 140 1 Background levels of E. coli 0157 in unspiked surface water samples were subtracted from spiked surface water levels to calculate percent recovery ------- 13.0 Pollution Prevention 13.1 The solutions and reagents used in this protocol pose little threat to the environment when recycled and managed properly. 13.2 Solutions and reagents should be prepared in volumes consistent with laboratory use to minimize the volume of expired materials to be disposed. 35 ------- 36 ------- 14.0 Waste Management 14.1 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. 14.2 Samples, reference materials, and equipment known or suspected to have viable E. coli 0157:H7 attached or contained must be sterilized prior to disposal. 14.3 For further information on waste management, consult The Waste Management Manual for Laboratory Personnel (Reference 15.11) and Less Is Better: Laboratory Chemical Management for Waste Reduction (Reference 15.12), both available from the American Chemical Society's Department of Government Relations and Science Policy. 1155 16th Street NVV, Washington. DC 20036. 37 ------- 38 ------- 15.0 References 15.1 Weagant. S.D. and Bound. A.J. 2001. "Evaluation of Techniques for Enrichment and Isolation of Escherichia coli 0157:H7 from Artificially Contaminated Sprouts." International Journal ofFood Microbiology. 71(1): 87-92. 15.2 U.S. Department of Health and Human Services. Centers for Disease Control and Prevention and National Institutes of Health. 2007. Biosafety in Microbiological and Biomedical Laboratories (BMBL), 5th Edition. Washington. D C.: U.S. Government Printing Office http://www.cdc.gov/OD/ohs/biosftv/bmbl5/bmbl5toc.htm 15.3 Makino. S., Kii. T., Asakura. H.. Shirahata. T., Ikeda. T., Takeshi. K.„ and I toll. K. 2000. "Docs Enterohemorrhagic Escherichia coli 0157:H7 Enter the Viable but Nonculturable State in Salted Salmon RoeT' Applied and Environmental Microbiology. 66(12): 5536-5539. 15.4 American Chemical Society. 2000. Reagent Chemicals, American Chemical Society Specifications. 9th edition. New York. NY: American Chemical Society. 15.5 British Drug Houses. Ltd. 1957. AnalaR Standards for Laboratory Chemicals. 5th Edition. Poole. Dorset. U.K.: BDH. Ltd. 15.6 U nited States Pharmacopeia. 2005. United States Pharmacopeia and National Formulary 24. Rockville. MD: United States Pharmacopcial Convention. 15.7 Bordner, R.H. 2005. "Section 9020 - Quality Assurance/Quality Control." In Standard Methods for the Examination of Water and Wastewater. 21" Edition. A.D. Eaton, L.S. Clcsceri, E.VV. Rice. A.E. Greenbcrg. and M.A.H. Franson (eds.). Washington, D C.: American Public Health Association. American Water Works Association, and Water Environment Federation. 15.8 Wise, J. 1988. NISTMeasurement Services: Liquid-In-Glass Thermometer Calibration Service. SP 250 - 23. U.S. Department of Commerce, National Institute of Standards and Technology. http://ts.iiist.gov/MeasurementServices/Calibrations/upload/SP250-23.pdf 15.9 Klee, A. J. 1993. "A Computer Program for the Determination of the Most Probable Number and its Confidence Limits." Journal of Microbiological Methods. 18(2): 91-98. 15.10 U.S. Environmental Protection Agency. Single-Laboratory Verification of Culture-Based Analytical Procedures for Escherichia coli 0157:H7 in Water. Publication forthcoming; date and number to be determined. 15.11 American Chemical Society (ACS). 1990. The Waste Management Manual for Laboratory Personnel. Washington. DC: American Chemical Society Department of Government Relations and Science Policy. 15.12 American Chemical Society (ACS). 1985. Less Is Better: Laboratory Chemical Management for Waste Reduction. Washington. DC: American Chemical Society Department of Government Relations and Science Policy. 39 ------- 40 ------- Distribution of Sample to mBPW (Sections 10.2.1 and 10.2.2) 1.0 mL to each m tube of 1X mBPW Serial dilutions as necessary 10.0 mL to each tube of 2X mBPW (10 mL) p Incubation at 36.0° ± 1.0°C and 42.0° ± 0.5°C (Section 10.2.3) "\ r > Incubate at 36.0°C ± 1.0°C for 2.0-2.5 hours Transfer tubes and incubate at 42.0°C ± 0.5°C^ for total 20 - hours 24 I I Analysis of positive tubes D c & 3 B) < CD 3> 3 as. < OS W o o 3 0> O 3" CD 3 CD J o £D ST SD Q_ 5 0) CO S 5 C/) ------- p> ks Enrichment in mBPW (Sections 10.1 and 10.2) and IMS Concentration (Section 10.3) or PCR Confirmation Isolation on TC-SMAC and Rainbow® Plates (Section 10.4) Qualitative and Quantitative mBPW analyses after 18-24 hours incubation Conduct IMS on 1 mL aliquot Biochemical and Serological Testing (Sections 10.5, 10.5, and 10.7) TC-SMAC 0 o o 1 2 3 E, coli 0157 latex agglutination 0 o o 1 2 3 Incubate at 42.0'C ± 0.5°C for 18-24 hours Rainbow® agar Incubate at 42.0°C ± 0.5°C for 18-24 hours Streak agglutination- positive colony onto TSA Optional H7 antiserum test Incubate at 36.0eC ± 1.0°C for 24 ± 2 hours a © 3 O fii O 3 S3 3. Biochemical test strip oooooot )000 000( 100000 Incubate test strip at 36°C ± 1°C for 18 - 24 hrs o o o o Oxidase test ------- ------- Printed on 100% recycled/recyclable paper with a minimum of 50% post-consumer fiber using vegetable-based ink. SEPA United States Environmental Protection Agency PRESORTED STANDARD POSTAGE & FEES PAID EPA PERMIT NO. G-35 Office of Research and Development (8101R) Washington, DC 20460 Official Business Penalty for Private Use $300 ------- |