United States
           Environmental Protection
           Agency
            Environmental Monitoring and
            Support Laboratory
            Cincinnati OH 45268
EPA/600/4-84/013{R 10)
December 1987
Revision
           Research and Development
&EPA
USEPA Manual of
Methods for Virology

Chapter 10
Revised December 1987

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                                                                                                 December 1987
                                                 Chapter 10
                 Cell Culture Procedures for Assaying Plaque-Forming Viruses
1.   Introduction


  This chapter outlines procedures to
detect waterborne viruses by use of
the plaque assay system. Use of the
method has been described by Dul-
becco (1952), Dulbecco and Vogt
(1954), Hsiung and Melnick (1955)
and Dahling and Wright (1986). The
principle of the system is based simply
on allowing virus particles to adsorb to
the host cells, adding agar medium to
localize virus growth and a vital stain
such  as neutral red to enhance visual-
ization of the cells. Localized lesions
(plaques) developing some days after
viral infection are then counted. These
counts are reported as plaque forming
units, whose number is  proportionate
to the amount of virus inoculated.  A
detailed method, verifying virus etiol-
ogy of a plaque fay "picking" followed
by passage in cell culture monolayer
with liquid medium overlay and then
observing the monolayer for develop-
ment of a  cytopathic effect, is pre-
sented in the next chapter.
  Chapter 10 is solely intended as
guidance for the investigator who  is
preparing to isolate and  enumerate
waterborne viruses utilizing either the
cell monolayer or the suspended cell
plaque assay technique. The proce-
dures outlined in this chapter are for
use with the Buffalo green monkey
(BGM) kidney cell line. The method
may also be applied to the Madin and
Darby bovine kidney (MDBK) cell line,
which has been effectively used for
the plaque assay of reoviruses, or
when deemed preferable to other cell
lines that may be  used in the plaque
assay of these animal viruses. How-
ever, it should be  noted that water-
borne viruses do not all form plaques.
  Chapter 9, Section 7 provides the
procedures for preparation of cell cul-
tures  used for virus assay in this chap-
ter. Cells should be planted three to
six days prior to their use in these
analyses.
  The detection methodology pre-
sented here has focused on labora-
tories with a small-scale virus assay
requirement. Where the quantities of
cell cultures, media and  reagents set
forth in this chapter are not sufficient
for processing the test sample concen-
trates, the prescribed measures may
be increased proportionately to meet
the demands of more expansive test
regimes.
2.   Cell Monolayer Procedure

2.1  Sample Inoculation of Cell
Monolayer for Virus Assay

2.1.1  Apparatus and materials.

(a)  Glassware, Pyrex glass, clear
    (Corning Glass Works, or
    equivalent).
     Storage vessel must be
    equipped with airtight closures.

(b) Cornwall syringe, or equivalent
   with cannula or syringe needle.
     A pipetting device will expedite
   virus assay when large volumes of
   cells, media or reagents must be
   handled.

(c)  Magnetic stirrer and stir bars.

(d) Waterbath set at 36.5 ± 1 °C.

(e) Sterilizing filter—0.22-/um pore
   size with a 47-mm diameter to
   sterilize stock antibiotic solutions
   from Section 2.1.3 (Millipore
   Corp., GS series, or equivalent).
     The 47-mm sterilizing filter may
   also be used for the verification of
   medium and reagent sterility in
   Section 2.4.

(f) Sterilizing filter—0.22-jt/m pore
   size with a 142-mm diameter to
   sterilize ELAH—Earle's  base solu-
   tion from Section 2.1.4 (Millipore
   Corp., GS series, or equivalent).
     Where the volumes of media
   and reagents prepared have been
   for large-scale viral analyses,  the
   use of a 293-mm diameter steril-
   izing filter may be more
   appropriate.

(g) Fiberglass prefilters for use with
   sterilizing filters (Millipore Corp.,
  >AP1 5 and AP20, or equivalent).
     Stack AP20 andAP15 prefilters
   and 0.22-um membrane filter into
    disc filter holder with AP20 prefli-
    ter on top and0.22-/jm membrane
    filter on bottom.
 (h) Membrane filter apparatus for ster-
    ilization—47-mm diameter filter
    holder and 50-mL slip tip syringe
    (Millipore Corp., Swinnex filter,
    product no. SX0047000, or equiv-
    alent for filter holder only).
      Disassemble Swinnex filter
    holder. Place membrane filter and
    prefilters in holder as instructed in
    Section 2.1.1, Step (g).

  (i) Disc filter holders—142-mm  or
    293-mm diameter (Millipore
    Corp., or equivalent).
      Use only pressure type filter
    holders. Place membrane filter
    and prefilters in holder as
    instructed in Section 2.1.1, Step
    (9).

  (j) Autoclavable inner-braided tubing
    with metal quick-disconnect con-
    nectors or with thumbscrew-drive
    clamps for connecting tubing to
    equipment to be used under
    pressure.
      Quick-disconnect connectors
    can be used only after equipment
    has been properly adapted.

 (k) Positively-charged cartridge fil-
    ter—10-inch (Zeta plus TSM,
    product no. 45134-01-600P,  AMF
    Cuno Division, or equivalent).

  (I) Holder for cartridge filter with
    adaptor for 10-inch cartridge  (type
    PL-1, product no. YY1601200,
    Millipore Corp., or equivalent).

(m) Culture capsule filter (product no.
    12140, Gelman Sciences Inc., or
    equivalent).

 (n) Positive pressure air or nitrogen
    source equipped with pressure
    gauge.
      Pressure source, if laboratory
    air line or pump, must be
    equipped with oil filter. Deliver to
    pressure  vessel and filter holder
    no more pressure than recom-
    mended by manufacturer.
                                                     10-1

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 December 1987
  (o) Dispensing pressure vessel—5- or
     20-liter capacity (Millipore Corp.,
     or equivalent).

  (p) Petri dish—50-mm diameter (Fal-
     con Labware Division, or
     equivalent).

  (q) Incubator capable of maintaining
     temperature of cell cultures at
     36.5° ± 1 °C.
 2.1.2  Media and reagents.

  (a) ELAH—Earle's base, with 0.5% lac-
     talbumin hydrolysate and without
     NaHCOa (Hazleton/Kansas City
     Biological, product no. DM-303, or
     equivalent).
       See Section 2.1.4, Step (h) for
     options in sterilization of the
     ELAH—Earle's base solution.

  (b) Sodium bicarbonate (NaHCO3).

  (c) Antibiotics—penicillin G, dihydro-
     streptomycin sulfate, tetracycline
     and amphotericin  B (Sigma Chem-
     ical Co., or equivalent).
       Use antibiotics of at least tissue
     culture grade. See Section 2.1.3
     for preparation of stock antibiotic
     solutions.

 (d) Ascorbic acid.

 (e) Water, deionized, distilled.
       See Chapter 4.

  ({) Nutrient agar(Difco Laboratories,
     or equivalent).

2.1.3  Procedure for preparation of
stock antibiotic solutions.
  If not purchased in sterile form.
stock antibiotic solutions must be
filter-sterilized by the use of0.22-um
membrane fitters.
  Antibiotic stock solutions should be
placed in screw-capped containers
and stored at -20°C until needed.
Once thawed they may be refrozen;
however, to avoid repeated freezing
and thawing of these stock solutions
distribute them In quantities that are
sufficient to support no more than a
week's virus assay work. Stock solu-
tions can be stored for  up to 4 months.
  Quantities prepared in steps (a), (b)
and(c) are sufficient for at least 100
liters of media.

  (a) Preparation of penicillin-
     streptomycin  stock solution.
       The procedure described is for
     preparation often 10-mL volume
    penicillin-streptomycin stock solu-
    tions at concentrations of
    1,000,000 units of penicillin and
    1,OOO mg of streptomycin per 10-
    mL unit. The antibiotic concentra-
    tions listed in step fa. 1) may not
    correspond to the concentrations
    obtained from other lots or from a
    different source.
    (a.1) Add appropriate amounts
         (within 5%) of penicilllin G
         and dihydrostreptomycin sul-
         fate to a 250-mL flask con-
         taining 100 mL of deionized
         distilled water.
           For penicillin supplied at
         1435 units per mg, add 7 g
         of the antibiotic.
           For streptomycin supplied
         at 740 mg per g,  add 14 g of
         the antibiotic.

    (a.2) Mix contents of flask on
         magnetic stirrer until antibi-
         otics are dissolved.

    (a.3) Sterilize antibiotics by filtra-
         tion through 0.22-/um mem-
         brane filter.

    (a.4) Dispense the penicilllin-
         streptomycin stock in. 10-mL
         volumes into screw-capped
         containers.

(b)  Preparation of tetracycline stock
    solution.
      The procedure described is for
   preparation of ten 5-mL tetracy-
    cline stock solutions at concentra-
    tions of 0.125 g per 5 mL unit.

   (b.1)  Add 1.25 g of tetracycline
         hydrochloride powder and
         3.75 g of ascorbic acid to a
         125-mL flask containing 50
         mL of deionized distilled
         water.

   (b.2)  Mix contents of flask on
         magnetic stirrer until antibi-
         otic is dissolved.
   (b.3) Sterilize antibiotic by filtra-
        tion through 0.22-//m
        membrane filter.

   (b.4) Dispense the tetracycline
        stock in 5-mL volumes into
        screw-capped containers.

(c) Preparation of amphotericin B (fun-
   gizone) stock solution.
      The procedure described is for
   preparation often2.5-mL fungi-
     zone stock solutions at concentra-
     tions of 0.0125 g per 2.5 mL unit.
    (c.1) Add 0.125 g of fungizone to
         a 50-mL flask containing 25
         mL of deionized distilled
         water.

    (c.2) Mix contents of flask on
         magnetic stirrer until antibi-
         otic is dissolved.

    (c.3) Sterilize antibiotic by filtra-
         tion through 0.22-um mem-
         brane filter.

    (c.4) Dispense the fungizone stock
         in 2.5-mL volumes into
         screw-capped containers.
2.1.4  Preparation of maintenance
medium.

 (a) Determine the volume of ELAH—
    Earle's base solution required.
      The volume of ELAH—Earle's
    base solution needed will be equal
    to the volume of growth medium
    used in propagation of cell cul-
    tures  for the plaque assay proce-
    dure.  Thus, see Table 9-2 in
    Chapters to determine the
    volume required.
      The procedure described is for
    preparation of 1 liter of ELAH—
    Earle's base solution in a IX for-
    mulation and will provide suffi-
    cient media for at least sixty 6-oz
    glass bottles or ninety 25-cm2
    plastic flasks.

 (b) Place  a three-inch stir bar into a
    two-liter flask.


 (c) Add contents of a 1 -liter packet of
    ELAH—Earle's base" reagent irtto
   flask.

(d) Add 890 mL of warmed deionized
   distilled water (50-60°C) to rea-
   gent in flask.

(e) Rinse  medium packet with three
   washes of 20 mL each of warmed
   deionized distilled water and add
   to flask.
     Note measure of deionized dis-
   tilled water is 5% less than
   desired total volume of reagent.

 (f) Mix on magnetic stirrer until rea-
   gent is completely dissolved.

(g) Add 2.25 g of NaHCO3  to the dis-
   solved reagent and continue mix-
   ing for an additional 15 min.
                                                      10-2

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                                                                                                   December 1 987
 (h) Filter reagent under pressure
    through a disc filter stack.
      •This sterilizing step requires the
    use of preiliters in line before the
    final sterilizing filter. Prepare filter
    stack according to instructions in
    Section 2.1.1. Step (g).
      As an alternative, use the car-
    tridge prefilter described in Sec-
    tion 2.1.1, Step (k) and the cap-
    sule sterilizing filter in Section
    2.1.1. Step(m).

 (i) Sterility testing.
      Test each lot of reagent to con-
    firm sterility (see Section 2.4).

 (j) Store sterilized reagent in tightly
    stoppered or capped container at
    4°C.
      Reagent may be stored for per-
    iods up to two months.

 (k) Add 1 ml of penicillin-
    streptomycin stock, 0.5 mL of
    tetracycline stock and 0.2 mL of
    fungizone stock (Section 2.1.3) to
    ELAH—Earle's base solution
    immediately before washing of
    cells.
2.1.5  Procedure for inoculating test
sample.
  Cell cultures used for virus assay
are generally found to be at their most
sensitive level between the third and
sixth days after initiation. Those older
than seven days should not be used.

 (a) Decant growth medium from pre-
    viously prepared cell culture test
    vessels.
      To prevent splatter, a gauze-
  ",  covered beaker may be used to
    collect spent medium.
      The medium is changed from
    one to four hours before cultures
    are to be inoculated and carefully
    decanted so as not to disturb the
    cell monolayer.

 (b) Discard growth medium.

 (c) Replace discarded medium with an
    equal volume of maintenance
    medium on day cultures are to be
    inoculated.
      For BGM and MDBK cells use
    antibiotic supplemented ELAH—
    Earle's base solution from Section
    2.1.4, Step (k).  To reduce shock to
    cells, warm maintenance medium
    to 36.5 ± 1°C before placing on
    cell monolayer.
      To prevent disturbing cells with
    the force of the liquid against the
    cell monolayer, add maintenance
    medium to the side of the cell cul-
    ture test vessel opposite the cell
    monolayer.

 (d) Identify cell culture test vessels by
    coding them with an indelible
    marker.

 (e) Return cell culture test vessels to
    36.5 ± 1°C incubator and hold
    vessel at the temperature until the
    cell monolayer is to be inoculated.

 (f) Decant maintenance medium from
    cell culture test vessels.
      Do not disturb the cell
    monolayer.

 (g) Discard maintenance medium.

 (h) Inoculate onto each cell monolayer
    a volume of test sample concen-
    trate appropriate for the cell sur-
    face area of the cell culture test
    vessels used.
      Inoculum volume should be no
    greater than 1 mL for each 40 cm2
    of surface area. Use Table 10-1 as
    a guide for inoculation size.
      A void touching either the can-
    nula or the pipetting device to the
    inside rim of the cell culture test
    vessels to avert the possibility of
    transporting contaminants to the
    remaining culture vessels.

 (i) Rock inoculated cell culture test
    vessels gently to achieve uniform
    distribution of inoculum on sur-
    face of cell monolayers.

 (j) Place cell culture test vessels on a
    level stationary surface at room
    temperature (22-25°C) so that the
    inoculum will remain distributed
    evenly over the cell monolayer.

 (k) Incubate inoculated cell cultures at
    room temperature for 80 min to
    permit viruses to adsorb onto and
    infect cells.
 (I) Proceed immediately to Section
    2.2.

2.2  Agar Overlay Procedure for
Plaque Assay
  If there is a likelihood that a test
sample will be toxic to cell cultures or
may be so darkly colored as to result in
inaccurate plaque counts, the cell
monolayer should be treated in ac-
cordance with the method described in
Chapter 8 (April, 1986 revision).

2.2.1   Apparatus and materials.

 (a) Glassware, Pyrex glass, clear .
    (Corning Glass Works, or
    equivalent).

 (b) Magnetic stirrer and stir bars.

 (c) Autoclavable inner-braided tubing
    with metal quick-disconnect  con-
    nectors,or with thumbscrew-drive
    clamps for connecting tubing to
    equipment to be used under
    pressure.
      Quick-disconnect connectors
    can be used only after equipment
    has been properly adapted.

 (d) Positive pressure air or nitrogen
    source equipped with pressure
    gauge.
      Pressure source, if laboratory
    air-line or pump, must be
    equipped with oil filter.  Deliver to
   pressure vessel and filter holder
   no more pressure than recom-
   mended by manufacturer.

(e) Dispensing pressure vessel—5- or
   20-liter capacity (Millipore Corp.,
   or equivalent).

 (f) Waterbath set at 36° ± 1 °C.
      Used for maintaining the
   temperature of the overlay
   medium.
     See Section 2.2.5. Step (c).
Table  10-1.  Guide for Virus Inoculation, Suspended Cell Concentration and Overlay
            Volume of Agar Medium
Vessel Type
1 -oz* glass
bottle
25 -cm' plastic
flask
6-oz glass
bottle
75 -cm2 plastic
flask
Volume of Virus
Inoculum (mLJ
0.1
0. 1 -0.5
0.5-1.0
1.0-2.0
Volume of Agar
Overlay Medium (mL)
5
10
20
30
Total Numbers
of Cells
1 X 107
2X107
4X107
6X107
'Size is given in oz only when it is commercially designated in that unit.

               10-3

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December 1987
 (g) Waterbath set at 50° ± 1 °C.
       Used for maintaining the agar
     temperature.
       See Section 2.2.6, Step (d).

 (h) Incubator capable of maintaining
     the temperatures of cell cultures
     at 36.5° ± 1 °C.

 (i)  Sterilizing filter—0.22-um pore
     size with a 142-mm diameter to
     sterilize Medium 199 from Sec-
     tion 2.2.3 and reagents in excess
     of 1 liter volumes (Millipore Corp.,
     GS series, or equivalent).
       Where the volumes of media
     prepared are for large-scale viral
     analyses (20 liters or morel, the
     use of a 293-mm diameter steril-
     izing filter may be more appro-
     priate. Use a 47-mm diameter fil-
     ter (or sterilizing volumes of less
     than 1 liter.

 (j)  Fiberglass prefilters for use with
     sterilizing filters {Millipore Corp.,
    AP15 and AP20, or equivalent).
      Stack AP20 andAP15 prefilters
     and 0.22-fjm membrane filter into
     disc filter holder with AP20 prefli-
     ter on top and 0.22-um membrane
     filler on bottom.

 {k)  Disc filter holders—47-mm, 142-
     mm or 293-mm diameter (Milli-
     pore Corp., or equivalent).
       Use only pressure type filter
     holders. Place membrane filter
     and prefilters in holder as
     instructed in Section 2.2.1. Step
     in.

 (I) Positively-charged cartridge fil-
     ter—10-inch (Zeta plus TSM,
     product no. 45134-01-600P, AMF
     Cuno Division, or equivalent).

 (m) Holder for cartridge filter with
     adaptor for 10-inch cartridge (type
     PL-1), product no. YY1601200,
     Millipore Corp., or equivalent).

 (n) Culture capsule filter (product no.
     12140, Gelman Sciences, Inc., or
     equivalent).

 (o) Petri dish—50-mm diameter (Fal-
     con Labware Division, or
     equivalent).

 2.2.2  Media and reagents.

 (a) Medium 199 prepared at a 2X con-
     centration with Earle's salts,
     0,05% lactalbumin and L-
     glutamine and without phenol red
     and NaHC03 (Grand Island Biolog-
     ical Co., product no. 400-1100, or
     equivalent).

 (b) HEPES—1 M (Sigma Chemical Co.,
     product no. H3375, or equivalent).
       Prepare SO mL of a 1 M solution
     of HEPES.

 (c) GG-free newborn calf serum—
     heat inactivated at 56°C for 30
     min, certified free of viruses, bac-
     teriophage and mycoplasma
     (Grand Island Biological Co., prod-
     uct no. 210-6400, or equivalent).
       Procure at least one 100-mL
     size bottle.

 (d) Sodium bicarbonate (NaHCO3)—
     7.5% solution.
       Prepare 50 mL of a 7.5% solu-
     tion of sodium bicarbonate. Steril-
     ized by filtration through 0.22-um
     filter.

 (e) Magnesium chloride (MgCI2-
     6H20)—1.0% solution.
       Prepare 50 mL of a 1.0% solu-
     tion of magnesium chloride.

 (f) Sodium chloride (NaCI).

 (g) Sodium phosphate dibasic
    (Na2H PCv7H20).

 (h) Sodium phosphate monobasic
    (NaH2P04-H2O).

 (i) Water,  deionized, distilled.
      See Chapter 4.

 (j) Hydrochloric acid (HCI)—1 M.
      Prepare 100 mL of a 1M solu-
    tion of  hydrochloric acid.

 (k) Sodium hydroxide (NaOH)—1  M.
      Prepare 100 mL of a 1M solu-
    tion of  sodium hydroxide.

 (I) Pancreatin 1X powder (ICN Nutri-
    tional Biochemicals, product no.
    102557, or equivalent).

im) Neutral red solution—0.1%, 100
    mL volume (Grand Island Biologi-
    cal Co., product no. 630-5330, or
    equivalent).
      Procure one 100-mL bottle.

 (n) Bacto skim milk (Difco Laborato-
    ries, product no. 0032-01, or
    equivalent).
      Prepare 1OO mL of Bacto skim
    milk in  accordance with directions
    given by manufacturer.

 (o) GIBCO  bacteriological agar (Grand
    Island Biological Co., product no.
    M00010B, or equivalent).
 (p) Antibiotics—penicillin G, dihydros-
    treptomycin sulfate, tetracycline
    and amphotericin B (Sigma Chem-
    ical Co., or equivalent).
      Use stock antibiotic solutions
    previously prepared in Section
    2.1.3.

 (q) Thioglycollate medium (Bacto de-
    hydrated fluid thioglycollate
    medium, Difco Laboratories, or
    equivalent).
      Prepare 100 mL of thioglycol-
    late medium in accordance with
    directions given by manufacturer.

 (r) Nutrient agar (Difco Laboratories,
    or equivalent).
      Prepare 100  mL of nutrient agar
    and pour 5 mL  aliquots into petri
    dishes for use in Section 2.4.2.
2.2.3  Preparation of Medium 199.

 (a) Sources of cell culture media.
      Commercially-prepared liquid
    cell culture media and medium
    components are available from
    several sources. Cell culture
    media can also be purchased in
    powder form that requires only
    dissolution in deionized distilled
    water and sterilization.
      Media from commerical sources
    are quality controlled. However.
    media can also be prepared in the
    laboratory from chemicals. Such
    preparations are labor intensive
    and may be expensive but allow
    quality control oLthe process by
    the preparing laboratory.
      The procedure described is for
    preparation of 500 mL of Medium
    199 at a 2X concentration. This
    procedure will prepare sufficient
    medium for at least fifty 6-oz glass
    bottles or eighty 25-cm2 plastic
    flasks.
 (b) Place a three-inch stir bar into a
    one-liter flask.

 (c) Add contents of a 1 -liter packet of
    Medium 199 into flask.

 (d) Add 355 mL of deionized distilled
    water to medium in flask.

 (e) Rinse medium packet with three
    washeS'Of 20 mL each of deion-
    ized distilled water and add to
    flask.
      Note measure of deionized dis-
    tilled water is 5% less than
    desired final volume of medium.
                                                      10-4

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                                                                                                    December 1987
 (f)  Mix on magnetic stirrer until
    medium is completely dissolved.

(g)  Filter reagent under pressure
    through a disc filter stack.
      This sterilizing step requires the
    use of pref liters in line before the
    final sterilizing filter. Prepare filter
    stack according to instructions in
    Section 2.2.1. Step (j).
      As an alternative, use cartridge
    pref liter described in Section
    2.2.1, Step II) and the capsule
    sterilizing filter in Section 2.2.1,
    Step (n).

(h)  Sterility testing.
      Test each lot of medium to con-
    firm sterility before the lot is used
    for plaque assay procedure (see
    Section 2.4).

 (i)  Store sterilized medium in tightly
    stoppered or capped container at
    4°C.
      Medium may be stored for per-
    iods of up to two months.


2.2.4   Preparation of pancreatin
solution for use in detecting reovirus.

 (a) Add 0.03 g of NaH2 PCvH2O to a
    250-mL flask.

 (b)  Add 100 mL of deionized distilled
    water to the flask.

 (c)  Mix contents of flask on magnetic
    stirrer until reagent is dissolved.

 (d)  Add 0.05 g of Na2H PCv7H2O to a
    250-mL flask.

 (e)  Add 100 ml of deionized distilled
    water to the flask.

 (f)  Mix contents of flask until  reagent
    is dissolved.

(g)  Sterilize NaH2PO4 and Na2H PO4
    stock solutions in accordance with
    instructions given in Chapter 3,
    Section 2.1.

(h)  Cool to room temperature (22°-
    25°C).

 (i)  Prepare phosphate buffer from the
    stock solutions by mixing 16 mL of
    NaH2 PO4 with 84 mL of Na2H POi
    in a 250-mL flask.

 (j)  Place three-inch stir bar into a
    2000-mL flask.

(k)  Add 984 mL of deionized distilled
    water to flask.
 (I) Place flask on magnetic stirrer and
    stir at a speed sufficient to
    develop vortex.

(m) Add 16 mL of phosphate buffer
    from Step (i) to the water.
      Remaining phosphate buffer
    solution may be stored at 4°C
    until needed.

 (n) Add 10 g of pancreatin from Sec-
    tion 2.2.2, Step (I) and 8.5 g of
    NaCI to the phosphate buffered
    water.

 (o) Continue mixing contents of flask
    on magnetic stirrer until reagents
    are dissolved.

 (p) Check  pH  of pancreatin solution
    and adjust to pH 7.5 if necessary.

 (q) Filter solution under pressure
    through a disc filter stack.
      This sterilizing step requires the
    use ofpref liters in line before the
    final sterilizing filter. Prepare filter
    stack according to instructions in
    Section 2.2.1, Step (j).
      As an alternative, use the car-
    tridge pref liter described in Sec-
    tion 2.2.1, Step (I) and the capsule
    sterilizing filter in Section 2.2.1,
    Step In).

 (r) Sterility testing.
      Test each lot to confirm sterility
    before the lot is used for reovirus
    recovery (see Section 2.4).

 (s) Store sterilized pancreatin solution
    in tightly stoppered or capped  con-
    tainer  at-20°C.
      Recommend solution be divided
    into 50-mL aliquots. Quantities
    prepared in Steps (a) through (s)
    are sufficient for at least fifty 6-oz
    glass bottles or eighty 25-cm2
    plastic flasks.
      Solution may be stored for peri-
    ods of up  to six months.
2.2.5   Preparation of overlay medium
for plaque assay.
   The procedure described is for prep-
aration of 100 mL of over/ay medium
and will prepare sufficient media for at
least ten 6-oz glass bottles or twenty
25-oz plastic flasks when mixed with
the agar prepared in Section 2.2.6.


 (a) Add 79 mL of Medium 199 (2X con-
    centration from Section 2.2.3,
    Step (i) and 4 mL of GG-free new-
    born calf serum from Section
    2.2.2, Step (c) to a 250-mL flask.
 (b) Add the stock solutions listed in
    Steps (b.1) through (b.7) to flask.
      Start with Step (b. 1) and add in
    the order listed, swirling to mix
    after each addition.

    {b.1) 6 mL-of NaHC03 from Sec-
         tion 2.2.2, Step (d).

    (b.2) 2 mL of MgCI2 from Section
         2.2.2, Step (e).

    (b.3) 3 mL of neutral solution
         from Section 2.2.2, Step (m).

    (b.4) 4 mL of 1  M HEPES from
         Section 2.2.2, Step(b).

    (b.5) 0.2 mL of penicillin-
         streptomycin stock from Sec-
         tion 2.1.3, Step (a).

    (b.6) 0.1 mL of tetracycline stock
         from Section 2.1.3, Step (b).

    (b.7) 0.04 mL of fungizone stock
         from Section 2.1.3, Step (c).
           For preparation of overlay
         medium for reovirus recov-
         ery, the serum and the skim
         milk from Section 2.2.7,
         Step (a) are replaced with
         2.8 mL of pancreatin solu-
         tion and 3.2 mL  of deionized
         distilled water.

 (c) Place flask with overlay medium in
    waterbath set at 36° ± 1 °C.
2.2.6  Preparation of overlay agar for
plaque assay.

 (a) Add 3 g of agar from Section 2.2.2,
    Step (o) to a 250-mL flask.

 (b) Add 100 mL of deionized distilled
    water to flask.

 (c) Sterilize agar in accordance with
    instructions given in Chapter 3,
    Section 2,1.

 (d) Hold agar in waterbath set at 50° ±
2.2.7   Preparation of agar overlay
medium.

 (a) Add 2 mL of skim milk from Section
    2.2.2, Step (n) to overlay medium
    prepared in Section 2.2.5.

 (b) Mix equal portions of overlay
    medium and agar by adding the
    medium to the agar flask.
                                                      10-5

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December 1987
      To prevent solidification of the
    liquified agar, limit the portion of
    agar overlay medium mixed to
    that volume which can be
    dispensed in 10 min.
2.2.8  Addition of overlay agar to cell
culture test vessels.

 (a) To each cell culture test vessel, add
    the volume of warm (42-46°C)
    agar overlay medium appropriate
    for the cell surface area of the
    vessels used.
      The volume of agar overlay
    medium that is appropriate for a
    particular virus assay culture ves-
    sel is listed in Table 10-1.
      To prevent disturbing cells with
    the force of the liquid against the
    cell monolayer, add agar overlay
    medium to the side of the cell cul-
    ture test vessel opposite the cell
    monolayer.

 (b) Place cell  culture test vessel, mon-
    olayer side down, on a level sta-
    tionary surface at room tempera-
    ture (22-25°C) so that the agar
    will remain distributed evenly
    before it solidifies.
      Care must be taken to ensure
    that all caps on bottles and flasks
    are tight; otherwise, the gas seal
    will not be complete and an
    erroneous virus assay will result.

 (c) Cover cell culture test vessels with
    a sheet of aluminum foil, a tightly
    woven cloth, or some other suita-
    ble cover to reduce light intensity
    and thus,  prevent damage to the
    cell monolayer.
      Agar is  fully solidified within 30
    min,

 (d) After 30 min invert cell culture test
    vessels and incubate in the dark
    at 36.5° ± 1 °C.
2.3   Counting Viral Plaques

2.3.1   Counting technique.

 (a) Count, mark and record plaques in
    cell culture test vessels on days
    two, three, four, six, eight and
    twelve after adding the agar over-
    lay medium.
      Depending on the virus density
    and virus types present in the
    inoculated sample, rescheduling
    of virus counts at plus or minus
    one day may be deemed prefera-
    ble. Virus titers are calculated
    from total count.
 (b) Examine cell culture test vessels on
    day sixteen.
      If no new plaques appear at 16
    days, discard vessels; otherwise
    continue to count, mark and
    record plaques every two days
    until no new plaques appear
    between counts.
      Note that most plaques will
    appear within 1 week.
2.3.2  Calculation of virus liter.

 (a) Calculate virus liter in plaque form-
    ing units (PFU) for each virus-
    conlaining sample concenlrale.
      To determine the numbers of
    PFU per mL in water, sewage
    sludge, soil, or dredge spoil sam-
    ple concentrate, multiply the
    number of PFU by the reciprocal
    of the inoculum volume.
      If the inoculum volume was di-
    luted, also multiply the number of
    PFU by the reciprocal of the dilu-
    tion made.

 (b) Calculate virus content of original
    sample.
      To  obtain virus content of the
    original sample in terms of PFU
    per mL, multiply the product from
    Section 2.3.2. Step (a) by the con-
    centration factor which is calcu-
    lated by dividing the volume of the
    original sample by the volume of
    the sample concentrate. For soil.
    digested dewatered sludge and
    dredge spoil samples, correct for
    water content and report in PFU
    per gram of dry weight.
      Dry weight is determined by
    evaporating a given sample in a
    weighed dish, drying in an  oven at
    104 ± 1°C to a constant weight
    and then determining the increase
    in weight over that of the empty
    dish.
2.4   Procedure for Verifying Sterilily
of Liquids
   There are many techniques availa-
ble for verifying the sterility of liquids
such as cell culture media and
medium components. Three tech-
niques, described below, are standard
in many laboratories. The capabilities
of these techniques, however, are
limited to detecting microorganisms
that grow unaided in the test medium
utilized. Viruses, mycoplasma, and
microorganisms that possess fastid-
ious  growth requirements or that
require living host systems will not be
detected. Nonetheless,  with the
 exception of a few special contamina-
 tion problems, the test procedures and
 microbiological media listed below
 should prove adequate. Do not add
 antibiotics to media or medium com-
 ponents until after sterility of the rea-
 gents, media and medium components
 has been demonstrated.
 2.4.1   Procedure for verifying sterility
 of small volumes of liquids.

 (a)  Inoculate 5 mL of the material to be
     tested for sterility into 5 mL of thi-
     oglycollate broth.

 (b)  Shake the mixture and incubate at
     36.5° ±1°C,

 (c)  Examine the inoculated broth daily
    for seven days to determine
     whether growth of contaminating
     organisms has occurred.
       Vessels that contain thioglycol-
     late medium must be tightly
     sealed before and after medium is
     inoculated. A clouded condition
     that develops in the media indi-
     cates the occurrence of contami-
    nating organisms.
2.4.2   Procedure for verifying sterility
of large volumes of liquids.

 (a) Filter 50-100 mL of the liquid '
    tested for sterility through a 47-
    mm diameter, 0.22-jUrri pore size
    membrane filter.

 (b) Remove filter from  its holder, and
    place filter on surface of solidified
    nutrient agar in a Petri dish.
      Place filter face up on agar.

 (c) Incubate Petri dish  at 36.5° ± 1 °C
    and examine filter surface daily
    for seven days to determine
    whether growth of  contaminating
    organisms has occurred.
                i

2.4.3  Visual evaluation of media for
microbial contaminants.

 (a) Incubate cell culture media that
    contain NaHC03 at  36.5° ± 1 °C
    for at least one week prior to use.

 (b) Visually examine the clarity of the
    culture media.
     A clouded condition that devel-
    ops in the media indicates the
    occurrence of contaminating
    organisms.

 (c) Discard any media that lose clarity.
                                                     10-6

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                                                                                                 December T987
3.   Suspended Cell
     Procedure

  The suspended cell technique for
enumeration of viruses from environ-
mental samples has the advantage of
detecting more viruses at a lower con-
centration than the cell monolayer
procedure.  The suspended cell tech-
nique also requires less time because
plaque assay involves no prior planting
of the cells or medium changes.
Plaques are easier to pick because the
cells are suspended within the agar
layer and not on the surface of the
bottle or flask where they must be
scraped off, and the system is inde-
pendent of the surface area of the
plaque assay vessel.  On the other
hand, the suspended cell technique
requires ten times more cells initially
than the cell monolayer procedure.
Suspended cells last only about one
week in the agar overlay as compared
to three weeks for cells used in the
monolayer technique. Moreover,
plaques in the suspended cell proce-
dure are not as well defined and thus
more difficult to count and because
the addition of pancreatin in the over-
lay would inhibit or retard cell growth
in this procedure, it cannot be used for
reovirus detection.
  Where low numbers of indigenous
viruses are anticipated in a test sam-
ple (5 PFU or less per mL), the sus-
pended cell procedure should be used
by itself or together with the cell mon-
olayer procedure. For assaying sam-
ples with high viral concentrations,
the recommended method would be
the cell monolayer procedure.
  If there is a likelihood that a test
sample will be toxic to cell cultures or
may be so darkly colored as to result in
inaccurate plaque counts, then only
the cell monolayer procedure should
be used and only  after the cell mono-
layer is treated in accordance with the
method described in Chapter 8 (April,
1986 revision).
3.1   Sample Inoculation of Sus-
pended Cells for Virus Assay

3.1.1   Apparatus and materials.

(a) Glassware, Pyrex glass, clear
   (Corning Glass Works, or
   equivalent).
     Storage vessel must be
   equipped with airtight closures.

(b) Culture tubes, disposable, borosili-
   cate glass—18 x 150 mm (Curtin
   Matheson Scientific, product no.
   339-333, or equivalent).
(c) Culture tube caps, slip-on-type—
   18 mm diameter (VWR Scientific,
   product no. 60879-162; or
   equivalent).

(d) Test tube rack for culture tubes.

(e) Cornwall syringe, or equivalent
   with cannula or syringe needle.
     A pipetting device will expedite
   virus assay when large volumes of
   cells, media or reagents must be
   handled.

 (f) Magnetic stirrer and stir bars.

(g) Shaker, rocker platform style (Bel-
   Ico Glass, Inc., product no. 7740-
   20020, or equivalent).

(h) Incubator capable of maintaining
   temperature of cells at 36.5° ±
3.1.2  Procedure for inoculating test
sample.

 (a) Arrange culture tubes in series.
      Number of culture tubes
    required will be equal to the mL of
    sample to be tested.

 (b) Place stir bar in flask.

 (c) Add  cell suspension from Chapter
    9, Section 6.1.8 to flask.

 (d) Dilute cell suspension to the
    appropriate cell concentration,
    while mixing on  magnetic stirrer.
      See Table 10-1 for cell concen-
    tration parameters. Dilute cell
    suspension with growth medium
    prepared in Chapter 9, Section
    3.3.3.
      Base cell dilution on results of
    cell counts performed in Chapter
    9, Section 6.2

(e) Add 1 mL of diluted cell suspension
   to each tube.
     A pipetting device will expedite
   processing when large cell
   volumes must be dispensed.

 (f) Add into each tube a 1 -mL volume
   of test sample concentrate.

(g) Swirl each tube gently to achieve a
   uniform mixture.

(h) Place inoculated tubes in rack.

 (i) Place test tube rack on,rocker  plat-
   form shaker housed in a 36° ±
    1 °C incubator.
 (j) Rock tubes at a rate of 16 oscilla-
    tions per min for 60 min to permit
    viruses to adsorb onto and infect
    cells.
      Complete preparation for agar
    overlay procedure during 60 min '
    incubation period.

 (k) Before cell culture test vessels are
    inoculated, identify vessels by
    coding them with  an indelible
    marker.

3.2  Agar Overlay Procedure for
Plaque Assay

3.2.1  Apparatus and materials.

 (a) Glassware, Pyrex  glass, clear
    (Corning Glass Works, or
    equivalent).

 (b) Magnetic stirrer and stir bars.

 (c) Autoclavable inner-braided tubing
    with metal quick-disconnect con-
    nectors  or with thumbscrew-drive
    clamps for connecting tubing to
    equipment to be used under
    pressure.
      Quick-disconnect disconnectors
    can be used only after equipment
    has been properly adapted.

 (d) Positive pressure air or nitrogen
    source equipped with pressure
    gauge.
      Pressure source, if laboratory
    air line or pump,-must be
    equipped with oil filter. Deliver to
    pressure vessel and filter holder
    no more pressure  than recom-
    mended by manufacturer.

(e) Dispensing pressure vessel—5- or
    20-liter capacity (Millipore Corp.,
    or equivalent).

 (f) Waterbath set at 36° ±1°C.
      Used for maintaining the
    temperature of the overlay
    medium.
     See Section 3.2.5. Step (c).

(g) Wat.erbath set at 50° ±1°C.
     Used for maintaining agar
    temperature.    '.:;'-
     See Section 3.2.6, Step (d).

(h) Incubator capable  of maintaining
    the temperatures of cell cultures
    at36.5°±1°C.

 (i) Sterilizing filter—0.22-pm pore
    size with a 47-mm diameter to
    sterilize  stock antibiotic solutions
    from Section 3.2.3 (Millipore
                                                      10-7

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 December 1987
     Corp,, GS series, or equivalent).
       The 47-mm sterilizing filter may
     also be used for the verification of
     medium and reagent sterility in
     Section 3.4.

  (j)  Sterilizing filter—0.22-pm pore
     size with a 142-mm diameter to
     sterilize Medium 199 from Sec-
     tion 3.2.4 (Millipore Corp., GS ser-
     ies, or equivalent).
       Where the volumes of media
    prepared are for large-scale viral
    analyses, the use of a 293-mm
    diameter sterilizing filter may be
    mora appropriate.

 (k) Fiberglass prefilters for use with
    sterilizing filters (Millipore Corp.,
    APIS and AP20, or equivalent).
      Stack AP20 and AP15 prefilters
    and 0.22-nm membrane filter into
    disc filter holder with AP20 prefil-
    ter on top and0.22-um membrane
    filter on bottom.

 (I) Membrane filter apparatus for ste-
    rilization—47-mm diameter filter
    holder and 50-mL slip tip syringe
    (Millipore Corp., Swinnex filter,
    product no. SX0047000, or equiv-
    alent for filter holder only).
       Disassemble Swinnex filter
     holder. Place membrane filter and
    prefilters in holder as instructed in
    Section 3.2.1. Step (k).

(m)  Disc filter holders—142-mm or
    293-mm diameter (Millipore
     Corp., or equivalent).
       Use only pressure type filter
    holders. Place membrane filter
    and prefilters in holder as
    instructed in Section 3.2.1, Step
    M.

 (n) Positively-charged cartridge fil-
    ter—1 0-inch (Zeta plus TSM,
    product no. 45134-01-600P, AMF
    Cuno Division, or equivalent).

 (o) Holder for cartridge filter with
    adaptor for 10-inch cartridge (type
    PL-1. product no. YY1601200,
    Millipore Corp., or equivalent).

 (p) Culture capsule filter (product no.
    12140, Gelman Sciences, Inc., or
    equivalent).

 (q) Petri dish—50-rnm diameter (Fal-
    con Labware Division, or
    equivalent)

3.2.2  Media and reagents.

 (a) Medium 199 prepared at a 2X con-
    centration with Garle's salts.
    0.05% lactalbumin and L-
    glutamine and without phenol red
    and NaHCOa (Grand Island Biolog-
    ical Co., product no. 400-1 1 00, or
    equivalent).

 (b) HEPES — 1 M (Sigma Chemical Co.,
    product no. H-3375, or
    equivalent).
      Prepare 50 mL of a 1 M solution
    of HEPES.

 (c) GG-free newborn calf serum —
    heat inactivated at 56°C for 30
    min, certified free of viruses, bac-
    teriophage and mycoplasma
    (Grand Island Biological Co., prod-
    uct no. 210-6400, or equivalent).
      Procure at least one 100-mL
    size bottle.

 (d) Sodium bicarbonate (NaHCOs) —
    7.5% solution.
      Prepare 5O mL of a 7.5% solu-
    tion of sodium bicarbonate. Steril-
    ized by filtration through 0.22 -/urn
    filter.
 (e) Magnesium chloride (
    6HZO)—1 .0% solution.
      Prepare 50 mL of a 1.0% solu-
    tion of magnesium chloride.

 (f) Water, deionized distilled.
      See Chapter 4.
(g)  Hydrochloric acid (HCI)—1 M.
     Prepare 100 mL of a 1M solu-
    tion of hydrochloric acid.

(h)  Sodium hydroxide (NaOH)—I'M."
     Prepare JOO mL of a 1M solu-
    tion of sodium hydroxide.

 (i)  Neutral red solution—0.1% (Grand
    Island Biological Co., product no.
    630-5330, or equivalent).
     Procure one 100-mL bottle.
     Sterilize by filtration through
    0.22-/jm filter.


 (j)  Bacto skim milk (Difco Laborato-
    ries, product  no. 0032-01, or
    equivalent).
     Prepare 100 mL of Bacto skim
    milk in accordance with directions
    given by manufacturer.

(k)  GIBCO bacteriological agar (Grand
    Island Biological Co., product no.
    MOOO10B, or equivalent).

 (I) Antibiotics—penicillin G, dihydro-
   streptomycin sulfate, tetracycline
   and amphotericin B (Sigma Chem-
    ical Co., or equivalent).
      Use antibiotics of at least tissue
    culture grade. See Section 3.2.3
    for preparation of stock antibiotic
    solutions.

 (m) Ascorbic acid.

 (n) Thioglycollate medium (Bacto de-
    hydrated fluid thioglycollate
    medium, Difco Laboratories, or
    equivalent).
      Prepare 100 mL of thioglycol-
    late medium in accordance with
    directions given by manufacturer.

 (o) Nutrient agar (Difco Laboratories,
    or equivalent).
      Prepare 100 mL of nutrient agar
    and pour 5 mL aliquots into petri
    dishes for use in Section 3.4.2.
3.2.3   Procedure for preparaton of
stock antibiotic solutions.
  If not purchased in sterile form,
stock antibiotic solutions must be
filter-sterilized by the use of0.22-fjm
membrane filters.
  Antibiotic stock solutions should be
placed in screw-capped containers
and stored at -20°C until needed.
Once thawed they may be refrozen;
however, to avoid repeated freezing
and thawing of these stock solutions
distribute them in quantities that are
sufficient to support no more than a
week's virus assay work. Stock solu-
tions can be stored for up to 4 months.
Quantities prepared in Steps (a), (b)
and(c) are sufficient for at least 100
liters of media.

(a) Preparation of penicillin-
    streptomycin stock solution.
      The procedure described is 'for
    preparation of ten 10-mL volume
    penicillin-streptomycin stock solu-
    tions at concentrations of
    1,000,000 units of penicillin and
    1,000 mg of streptomycin per 10-
    mL unit. The antibiotic concentra-
    tions listed in Step (a. 1) may not
    correspond to the concentrations
    obtained from other lots or from  a
    different source.

    (a.1) Add appropriate amounts
        (within 5%) of penicillin G
        and  dihydrostreptomycin sul-
        fate  to a 250-mL flask con-
        taining 100 mL of deionized
        distilled water.
          For penicillin supplied at
        1435 units per mg, add 7 g
        of the antibiotic.
          For streptomycin supplied
        at 740 mg per g, add 14 g of
        the antibiotic.
                                                      10-8

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                                                                                                     December 1987
     (a.2) Mix contents of flask on
          magnetic stirrer until antibi-
          otics are dissolved.

     (a.3) Sterilize antibiotics by filtra-
          tion through 0.22-//m
          membrane filter.

    (a.4) Dispense the penicillin-
         streptomycin stock in 10-mL
         volumes into screw-capped
         containers.

 (b) Preparation of tetracycline stock
     solution.
       The procedure described is for
     preparation of ten 5-mL tetracy-
     cline stock solutions at concentra-
     tions of 0.125 g per 5 mL unit.

     (b.1) Add 1.25 g of tetracycline
         hydrochloride powder and
         3.75 g of ascorbic acid to a
         125-mL flask containing 50
         mL of deionized distilled
         water.

     (b.2) Mix contents of flask on
         magnetic stirrer until antibi-
         otic is dissolved.

    (b.3) Sterilize antibiotic by filtra-
         tion through 0.22-//m mem-
         brane filter.

    (b.4) Dispense the tetracycline
         stock in 5-mL volumes into
         screw-capped containers.

 (c) Preparation of amphotericin Bffun-
    gizone) stock solution.
      The procedure described is for
    preparation of ten 2.5-mL fungi-
    zone stock solutions at concentra-
    tions of O.0125 g per 2.5 mL unit.

    (c.1) Add 0.125 g of fungizone to
        a 50-mL flask containing 25
        mL of deionized distilled
        water.

    (c.2) Mix contents of flask on
        magnetic stirrer until antibi-
        otic  is dissolved.

    (c.3) Sterilize antibiotic by filtra-
        tion through  0.22-^m mem-
        brane filter.

    (c.4) Dispense the fungizone stock
        in 2.5-mL volumes into
        screw-capped containers.

3.2.4  Preparation of Medium 199.

 (a) Sources of cell culture media.
      Commercially-prepared liquid
    cell culture media and medium
     components are available from
     several sources. Cell culture
     media can also be purchased in
     powder form that requires only
     dissolution in deionized distilled
     water and sterilization.
      Media from commercial sources
     are quality controlled. However,
     media can also be prepared in the
     laboratory from chemicals. Such
     preparations are labor intensive
     and may be expensive but allow
     quality control of the process at
     the level of the preparing labora-
     tory. The procedure described is
     for preparation of 500 mL of
     Medium 199 at a 2X concentra-
     tion. This procedure will prepare
     sufficient medium for at least fifty
     6-oz glass bottles or eighty 25-
     cm2 plastic flasks.
 (b) Place a three-inch stir bar into a
    one-liter flask.

 (c) Add contents of a 1 -liter packet of
    Medium  199 into flask.

 (d) Add 355  mL of deionized distilled
    water to medium  in flask.
      Note measure of deionized dis-
    tilled water is 5% less than
    desired total volume of medium.

 (e) Rinse medium packet with three
    washes of 20 mL each of deion-
    ized distilled water and add to
    flask.

 (f) Mix on magnetic stirrer until
    medium is completely  dissolved.

(g) Filter reagent under pressure
    through a disc filter stack.
      This sterilizing step requires the
    use of prefliters in line before the
    final sterilizing filter. Prepare filter
    stack according to instructions in
    Section 3.2.1, Step (k).
     As an alternative, use the car-
    tridge pref liter described in Sec-
    tion 3.2.1, Step (n) and the cap-
    sule sterilizing filter in Section
    3.2.1, Step Ip).

(h) Sterility testing.
      Test each lot of medium to con-
    firm sterility before the lot is used
    for plaque assay procedure (see  •
    Section 3.4).

 (i)  Store sterilized medium in tightly
    stoppered or capped container at.
    4°C.
     Medium may be stored for peri-
    ods of up to two months.
 3.2.5  Preparation of overlay medium
 for plaque assay.
    The procedure described is for prep-
 aration of 100 mL of overlay medium
 and will provide sufficient medium for
 at least ten 6-oz glass bottles or
 twenty 25-cm2 plastic flasks when
 mixed with the agar prepared in Sec-
 tion 3.2.6.

  (a) Add 79 mL of Medium 199 (2X con-
     centration) from Section 3.2.4,
     Step (i) and 4 mL of GG-free new-
     born calf serum from Section
     3.2.2, Step {c} to a 250-mL flask.

  (b) Add the stock solutions listed in
     Steps (b.1) through (b.7) to flask.
       Start with Step (b. 1) and add in
     the order listed, swirling to mix
     after each addition.

     (b.1) 6 mL of NaHCOs from Sec-
          tion 3.2.2, Step (d).

     (b.2) 2 mL of.MgCI;, from  Section
          3.2.2, Step (e).

     (b.3) 3 mL of neutral red solution
          from Section 3.2.2, Step (i).

     (b.4) 4 mL of 1 M HEPES  from
         'Section 3.2.2., Step(b).

     (b.5) 0.2 mL of penicillin-
          streptomycin stock from Sec-
          tion 3.2.3, Step (a).

     (b.6) 0.1 mL of tetracycline stock
          from Section 3.2.3, Step (b).

     (b.7) 0.04 mL of fungizone stock
          from Section 3:2.3, Step (c).

 (c)  Place flask with overlay medium in
     waterbath set at 36° ± 1 °C,
3.2.6  Preparation of overlay agar for
plaque assay.

 (a) Add 3 g of agar from Section 3.2.2,
    Step (k) to a 250-mL flask.

 (b) Add 100 mL of deionized distilled
    water to flask.

 (c) Sterilize agar in accordance with
    instructions given in Chapter 3,
    Section 2.1.

 (d) Hold agar in waterbath set at 50° ±
3.2.7   Preparation of agar overlay
medium.
                                                       10-9

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 December 1987
  (a) Add 2 mL of skim milk from Section
     3,2.2, Step (j) to overlay medium
     prepared in Section 3.2.5.

  (b) Mix equal portions of overlay
     medium and agar by adding the
     medium to the agar flask.
       To prevent solidification of the
     liquified agar. limit the portion of
     agar overlay medium mixed to
     that volume which can be
     dispensed in 10 min.
 3.2.8  Procedure.

  (a) Following incubation of test tubes
     in Section 3,1.2, Step (j), add to
     one tube at a time the volume of
     warm (42-44°C) agar overlay
     medium appropriate for the cell
     surface area of the cell culture
     test vessels to be used.
       The volume of agar overlay
     medium that is appropriate for a
     particular virus assay culture ves-
     sel is listed in Table 10-1.

  (b) Immediately after adding agar to
     tube, pour contents into cell cul-
     ture test vessel.

  (c) Tightly cap vessel.

  (d) Swirl to mix contents of vessel.

  (e) Place cell culture test vessel on a
     level stationary surface at room
     temperature (22-25°C) so that the
     contents will distribute evenly
     before it solidifies.
      Care must be taken to ensure
     that all caps on bottles and flasks
     are tight; otherwise, the gas seal
     will not be complete and an
     erroneous virus assay will result.

  (f) Cover cell culture test vessels with
     a sheet of aluminum foil, a tightly
     woven cloth, or some other suita-
     ble cover to reduce light intensity
     and thus, prevent damage to the
     cell monolayer.
      Agar is fully solidified within 30
     min.

 (g) Invert cell culture test vessels and
     incubate in the dark at 36.5° ±
3.3  Counting Viral Plaques

3.3.1  Technique.

 (a) Mark and record plaque numbers at
    each counting period.
       Virus titers are calculated from
     total count.

  (b) Count on days two, three, four, five
     and seven after adding the agar
     overlay medium.
       Cells that are suspended in the
     agar over/ay degenerate more
     rapidly that those from'an over-
     lay ed monolayer culture. Thus,
     scheduling plaque counts for
     longer than seven days is not
     recommended.
       Depending on the virus density
     and virus types present in the
     inoculate sample, a rescheduling
     of viral counts at plus or minus
     one day may be deemed prefera-
     ble within the seven-day counting
     period.
 3.3.2  Virus enumeration.

 (a) Calculate virus titer in plaque form-
     ing units (PFU) for each virus-
     containing sample concentrate.
       To determine the numbers of
     PFU per mL in water, sewage
     sludge, soil, or dredge spoil sam-
     ple concentrate, multiply the
     number of PFU by the reciprocal
     of the inoculum volume.
       If the inoculum volume was di-
     luted, also multiply the number of
     PFU by the reciprocal of the dilu-
     tion made.

 (b) Calculate virus content of original
     sample.
       To obtain virus content of the
     original sample in terms of PFU
     per mL, multiply the product from
     Section 2.3.2, Step fa) by the con-
     centration factor which is calcu-
     lated by dividing the volume of the
     original sample by the volume of
     the sample concentrate. For soil,
     digested de watered sludge and
     dredge spoil samples, correct for
     water content and report in PFU
    per gram of dry weight.
3.4  Procedure for Verifying Sterility
of Liquids

  There are many techniques availa-
ble for verifying the sterility of liquids
such as cell culture media and'
medium components. Three tech-
niques, described below, are standard
in many laboratories. The capabilities
of these techniques, however, are
limited to detecting microorganisms
that grow unaided on the test medium
utilized. Viruses,  mycoplasma, and
 microorganisms that possess fastid-
 ious growth requirements or that
 require living host systems will not be
 detected. Nonetheless, with the
 exception of a few special contamina-
 tion problems, the test procedures and
 microbiological media listed below
 should prove adequate. Do not add
 antibiotics to media or medium com-
 ponents until after sterility of the rea-
 gents, media and medium components
 has been demonstrated.
3.4.1   Procedure for verifying sterility
of small volumes of liquids.

 (a) Inoculate 5 mL of the material to be
    tested for sterility into 5 mL of thi-
    oglycollate broth.

 (b) Shake the mixture and incubate at
    36.5°±1°C.

 (c) Examine the inoculated broth daily
    for seven days to determine
    whether growth of contaminating
    organisms  has occurred.
      Vessels that contain thioglycol-
    late medium must be tightly
    sealed before and after medium is
    inoculated. A  clouded condition
    that develops in the media indi-
    cates the occurrence of contami-
    nating organisms.
3.4.2  Procedure for verifying sterility
of large volumes of liquids.

 (a) Filter 50-100 mL of the liquid
    tested for sterility through a 47-
    mm diameter, 0:22-/urn pore size
    membrane filter.

 (b) Remove filter from its holder, arid
    place filter on ssurface of solidified
    nutrient agar in a Petri dish.
      Place filter face up on agar.

 (c) Incubate Petri dish at 36.5° ± 1 °C
    and examine filter surface daily
    for seven days to determine
    whether growth of contaminating
    organisms has occurred.
3.4.3  Visual evaluation of media for
microbial contaminants.

(a) Incubate cell culture media that
    contain NaHCO3 at 36.5° ± 1 °C
    for at least one week prior to use.

(b) Visually examine the clarity of the
    culture media.
     A clouded condition that devel-
    ops in the media indicates the
                                                     10-10

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    occurrence of contaminating
    organisms.

 (c) Discard any media that lose clarity.
 4.   Bibliography

 Cooper, P. D. 1967. The Plaque Assay
   of Animal Viruses, p. 243-311./n K.
   Maramorosch and H. Koprowski
   (eds.). Methods in Virology, Vol. 3.
   Academic Press, New York, NY.
 Dahling, D. R., G. Berg, and D. Ber-
   man. 1974. BGM, A Continuous Cell
   Line More Sensitive than Primary
   Rhesus and African Green Kidney
   Cells for the Recovery of Viruses
   from Water. Health Lab. Sci.
   11:275-282.
 Dahling, D. R. and B. A. Wright. 1986.
   Optimization of the BGM Cell Line
   Culture and Viral Assay Procedures
   for Monitoring Viruses in the Envi-
   ronment. Appl. Environ. Microbiol.
   51:790-812.
 Dahling, D. R. and B. A. Wright.
   Optimization of Suspended Cell
   Method and Comparison with Cell
   Monolayer Technique for Virus
   Assays. In Preparation.
 Dulbecco, R. 1952. Production  of
   Plaques in Monolayer Tissue Cul-
   tures  by Single Particles of an
   Animal Virus. Proc. Natl. Acad. Sci
   U.S. 38:747-752.
 Dulbecco, R. and M. Vogt. 1954.
   Plaque Formation and Isolation of
   Pure Lines with Poliomyelitis Vi-
   ruses. J.  Exp. Med. 99:167-182.
 Hsiung, G.  D. and J. L. Melnick. 1955.
   Plaque Formation with  Poliomyelitis,
   Coxsackie and Orphan (Echo) Vi-
   ruses in Bottle Cultures of Monkey
   Epithelial Cells.  Virology. 1:533-535.
 Lennette, E. H. and N. J. Schmidt
  (eds.). 1979. Diagnostic Procedures
  for Viral, Rickettsial and Chlamydial
  Infections. 5th ed. American Public
  Health Association, Inc., Washing-
  ton, DC. 1138 pp.
Laboratory Manual in Virology.  1974.
  Edition Two. Ontario Ministry of
  Health, Toronto, Ontapo, Canada.
  375 pp.             5
Rovozzo, G. C. andC. N. Burke.  1973.
  A Manual of Basic Virological Tech-
  niques. Prentice-Hall, Inc., Engle-
  wood Cliffs, NJ.  287 pp.
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