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© 2015 AOAC INTERNATIONAL
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[Applicable for the determination of the following PAHs
in mussel, oyster, and shrimp: 1,7-dimethylphenanthrene,
1-methylnaphthalene,
1-methylphenanthrene,
2,6-dimethyl-
naphthalene, 3-methylchrysene, anthracene, benz[
a
]anthracene,
benzo[
a
]pyrene, benzo[
b
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g,h,i
]perylene,
benzo[
k
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GLEHQ]>
a,h
]anthracene,
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cd
]pyrene, naphthalene,
phenanthrene, and pyrene. These were representative PAH analytes
selected for the collaborative study. The method has been single-
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therefore, is expected to be applicable to other GC-amenable PAHs
and seafood matrices. The concentration ranges evaluated within
the collaborative study are given in Table
2014.08A
.]
Caution
:
See
Appendix B: Laboratory Safety
. Use appropriate
personal protective equipment such as laboratory
coat, safety glasses or goggles, appropriate chemical-
resistant gloves, and a fume hood. Dispose of solvents
and solutions according to federal, state, and local
regulations. Always handle open containers of solvents
inside the fume hood, including the pouring, mixing,
evaporating, and preparing standard solution. Keep
containers covered or closed when not in use.
Hexane and isooctane
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irritants. Harmful if inhaled, swallowed, or absorbed
through the skin. May also cause skin and eye irritation.
Ethyl acetate
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Harmful if swallowed in quantity. Vapors may cause
drowsiness.
Toluene
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inhaled, swallowed, or absorbed through the skin. May
also cause skin and eye irritation. May cause drowsiness.
Possible teratogen.
Dichloromethane
.—Noncombustible, liquid irritant.
Harmful if inhaled, swallowed, or absorbed through the
skin. May also cause skin and eye irritation. Asphyxiant.
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Possible carcinogen and mutagen.
PAHs
.—Carcinogens, respiratory sensitizers, teratogens,
reproductive hazard, mutagens. Harmful if inhaled,
swallowed, or absorbed through the skin. May also cause
skin and eye irritation.
See
Tables
2014.08B
–
D
for results of the interlaboratory study
supporting acceptance of the method.
A. Principle
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addition of
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LQ D P/ SRO\SURS\OHQH FHQWULIXJH WXEH IRU PLQ 6XEVHTXHQWO\
4 g anhydrous magnesium sulfate and 2 g sodium chloride are
added to the mixture to induce phase separation and force the
analytes into the ethyl acetate layer. The tube is again shaken by
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in hexane. The analytes are eluted with hexane–dichloromethane
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which are dependent on the silica deactivation. The clean extract
LV FDUHIXOO\ HYDSRUDWHG UHFRQVWLWXWHG LQ P/ LVRRFWDQH DQG
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See
Figure
2014.08A
IRU WKH PHWKRG ÀRZ
chart.
B. Apparatus
a
Homogenizer
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b
Solvent evaporator
.—Any suitable solvent evaporator,
such as a rotary vacuum evaporator, Kuderna-Danish evaporator,
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Concentration, μg/L
Equivalent concentration, μg/kg
Calibration level
BaP and others
a
Chr and others
b
Naph
c
13
C-PAHs
BaP and others Chr and others
Naph
13
C-PAHs
1
5
12.5
25
50
0.5
1.25
2.5
5
2
10
25
50
50
1
2.5
5
5
3
20
50
100
50
2
5
10
5
4
50
125
250
50
5
12.5
25
5
5
100
250
500
50
10
25
50
5
6
200
500
1000
50
20
50
100
5
7
500
1250
2500
50
50
125
250
5
8
1000
2500
5000
50
100
250
500
5
a
Analytes at 10 μg/mL in the mixed stock standard solution.
b
Analytes at 25 μg/mL in the mixed stock standard solution.
c
Analytes at 50 μg/mL in the mixed stock standard solution.