AOAC-RI ERP Book - FAOM METHOD.pdf

Dichloromethane .—Noncombustible, liquid irritant. Harmful if inhaled, swallowed, or absorbed through the skin. May also cause skin and eye irritation. Asphyxiant. &DXVHV FHQWUDO QHUYRXV V\VWHP &16 GHSUHVVLRQ 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 +RPRJHQL]HG VHDIRRG VDPSOHV J VDPSOH ZLWK D —J NJ addition of 13 & 3$+ VXUURJDWH PL[WXUH DUH PL[HG ZLWK P/ ZDWHU RU P/ ZDWHU LQ WKH FDVH RI VKULPS DQG RWKHU PRUH YLVFRXV VDPSOHV DQG VKDNHQ YLJRURXVO\ E\ KDQG ZLWK P/ HWK\O DFHWDWH 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 KDQG IRU PLQ DQG WKHQ FHQWULIXJHG IRU PLQ DW ! UFI $ P/ DOLTXRW RI WKH HWK\O DFHWDWH OD\HU LV HYDSRUDWHG UHFRQVWLWXWHG LQ P/ KH[DQH DQG FOHDQHG RQ DQ 63( FROXPQ ZLWK J VLOLFD JHO DQG DSSUR[LPDWHO\ J DQK\GURXV VRGLXP VXOIDWH RQ WKH WRS 7KH FROXPQ LV FRQGLWLRQHG ZLWK P/ KH[DQH±GLFKORURPHWKDQH Y Y DQG P/ KH[DQH IROORZHG E\ DSSOLFDWLRQ RI WKH P/ H[WUDFW in hexane. The analytes are eluted with hexane–dichloromethane Y Y XVLQJ YROXPH GHWHUPLQHG IRU WKH JLYHQ VLOLFD JHO 63( FDUWULGJHV IURP WKH HOXWLRQ SUR¿OHV RI WDUJHW DQDO\WHV DQG IDW which are dependent on the silica deactivation. The clean extract LV FDUHIXOO\ HYDSRUDWHG UHFRQVWLWXWHG LQ P/ LVRRFWDQH DQG DQDO\]HG E\ *& 06 See Figure 2014.08A IRU WKH PHWKRG ÀRZ chart. B. Apparatus a Homogenizer ²:$5,1* EOHQGHU 0RGHO %/ &RQDLU &RUS 6WDPIRUG &7 RU HTXLYDOHQW b Solvent evaporator .—Any suitable solvent evaporator, such as a rotary vacuum evaporator, Kuderna-Danish evaporator,

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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 @ÀXRUDQWKHQH EHQ]R> g,h,i ]perylene, benzo[ k @ÀXRUDQWKHQH FKU\VHQH GLEHQ]> a,h ]anthracene, ÀXRUDQWKHQH ÀXRUHQH LQGHQR> cd ]pyrene, naphthalene, phenanthrene, and pyrene. These were representative PAH analytes selected for the collaborative study. The method has been single- ODERUDWRU\ YDOLGDWHG IRU 3$+V LQ ¿VK DQG VKULPS DQG 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 ²+LJKO\ ÀDPPDEOH OLTXLG irritants. Harmful if inhaled, swallowed, or absorbed through the skin. May also cause skin and eye irritation. Ethyl acetate ²+LJKO\ ÀDPPDEOH OLTXLG LUULWDQWV Harmful if swallowed in quantity. Vapors may cause drowsiness. Toluene ²+LJKO\ ÀDPPDEOH OLTXLG LUULWDQW +DUPIXO LI inhaled, swallowed, or absorbed through the skin. May also cause skin and eye irritation. May cause drowsiness. Possible teratogen.

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$ 3$+ DQG & 3$+ FRQFHQWUDWLRQV LQ WKH FDOLEUDWLRQ VWDQGDUG VROXWLRQV 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 2 3 4 5 6 7 8

5

12.5

25 50

50 50 50 50 50 50 50 50

0.5

1.25

2.5

5 5 5 5 5 5 5 5

10 20 50

25 50

1 2 5

2.5

5

100 250 500

5

10 25 50

125 250 500

12.5

100 200 500

10 20 50

25 50

1000 2500 5000

100 250 500

1250 2500

125 250

1000

100

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.

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