AOAC-RI ERP Book - FAOM METHOD.pdf

7DEOH

( $QDO\WH FRQFHQWUDWLRQV LQ WKH PL[HG VWRFN

2SWLPXP HOXWLRQ YROXPH

VWDQGDUG VROXWLRQ Analyte

Concentration, μg/mL

Anthracene

10 10 10 10 10 10 25 10 25 10 10 50 25 25 25 25 25 10 25

Benz[ a ]anthracene

Benzo[ a ]pyrene

Benzo[ b @ÀXRUDQWKHQH Benzo[ g,h,i ]perylene Benzo[ k @ÀXRUDQWKHQH

Chrysene

Dibenz[ a,h ]anthracene

Fluoranthene

)LJXUH % $Q H[DPSOH RI HOXWLRQ SUR¿OHV RI 3$+V RQ D VLOLFD JHO 63( FDUWULGJH DQG GHWHUPLQDWLRQ RI WKH RSWLPXP HOXWLRQ YROXPH

Fluorene

Indeno[1,2,3- cd ]pyrene

Naphthalene Phenanthrene

G. GC/MS Analysis a GC conditions. —Table 2014.08G provides GC conditions WKDW ZHUH XVHG E\ WKH FROODERUDWLYH VWXG\ SDUWLFLSDQWV 2WKHU FRQGLWLRQV H J FROXPQ WHPSHUDWXUH DQG ÀRZ SURJUDP DQG LQMHFWLRQ WHFKQLTXH DQG YROXPH FDQ EH XVHG DV ORQJ DV WKH ODERUDWRU\ TXDOL¿FDWLRQ FULWHULD IRU VHSDUDWLRQ VHQVLWLYLW\ DQG OLQHDULW\ DUH PHW 7KH LQMHFWLRQ WHPSHUDWXUH RU SURJUDP QHHGV WR be optimized to enable quantitative transfer of less volatile PAHs. ,I SURJUDPPDEOH WHPSHUDWXUH YDSRUL]HU 379 VROYHQW YHQW PRGH LV XVHG VROYHQW YHQWLQJ SDUDPHWHUV WHPSHUDWXUH WLPH ÀRZ SUHVVXUH QHHG WR EH FDUHIXOO\ RSWLPL]HG WR SUHYHQW ORVVHV RI WKH volatile PAHs, especially naphthalene. The separation criteria GHPRQVWUDWHG LQ )LJXUH 2014.08C LQFOXGH 1 D EDVHOLQH VHSDUDWLRQ of benzo[ a ]pyrene and benzo[ e @S\UHQH FRQFHQWUDWLRQ UDWLR RI 2 DW OHDVW YDOOH\ VHSDUDWLRQ RI DQWKUDFHQH DQG SKHQDQWKUHQH FRQFHQWUDWLRQ UDWLR HYDOXDWHG IRU WKH DQWKUDFHQH SHDN DQG 3 DW OHDVW YDOOH\ VHSDUDWLRQ IRU EHQ]R> b @ÀXRUDQWKHQH benzo[ j @ÀXRUDQWKHQH DQG EHQ]R> k @ÀXRUDQWKHQH FRQFHQWUDWLRQ UDWLR RI Note : Criteria for separation of chrysene and WULSKHQ\OHQH DQRWKHU 3$+ FULWLFDO SDLU ZHUH QRW VHW IRU WKH collaborative study. For accurate quantitation of chrysene, at least YDOOH\ VHSDUDWLRQ LV UHFRPPHQGHG ZKLFK FDQ EH DFKLHYHG using selective stationary phases. The maximum oven temperature program may not exceed the PD[LPXP WHPSHUDWXUH OLPLW IRU D JLYHQ FROXPQ %DFNERQH PRGL¿HG FROXPQV VXFK DV 5[L 6LO 06 RU '% 06 DUH UHFRPPHQGHG for their better temperature stability and also good selectivity for FULWLFDO 3$+ SDLUV RU JURXSV LQFOXGLQJ WKH DQWKUDFHQH SKHQDQWKUHQH SDLU RU EHQ]RÀXRUDQWKHQHV &RQGXFW SURSHU LQOHW DQG FROXPQ maintenance to ensure adequate operation of the GC instrument. Perform system checks. b MS conditions. ²$Q\*& 06 LQVWUXPHQW VLQJOH TXDGUXSROH WULSOH TXDGUXSROH 72) RU LRQ WUDS ZLWK (, PD\ EH XVHG DV ORQJ DV LW SURYLGHV UHVXOWV PHHWLQJ WKH ODERUDWRU\ TXDOL¿FDWLRQ UHTXLUHPHQWV 7KH VWXG\ SDUWLFLSDQWV XVHG WKH IROORZLQJ LQVWUXPHQWV VLQJOH TXDGUXSROH $JLOHQW ±/DERUDWRU\ $JLOHQW % ;/ ,QHUW± /DERUDWRULHV DQG ± $JLOHQW &±/DERUDWRULHV DQG WULSOH TXDGUXSROH $JLOHQW %±/DERUDWRU\ 7KHUPR 764± /DERUDWRU\ DQG WLPH RI ÀLJKW /HFR 3HJDVXV '±/DERUDWRU\ 3D\ VSHFLDO DWWHQWLRQ WR WKH RSWLPL]DWLRQ RI WKH 06 WUDQVIHU OLQH DQG 06 VRXUFH WHPSHUDWXUH +LJKHU 06 VRXUFH WHPSHUDWXUHV

Pyrene

1-Methylnaphthalene 2,6-Dimethylnaphthalene 1-Methylphenanthrene 1,7-Dimethylphenanthrene

3-Methylchrysene

XVLQJ DQ DQDO\WLFDO EDODQFH (OXWH WKH FDUWULGJH ZLWK DGGLWLRQDO î P/ KH[DQH±GLFKORURPHWKDQH Y Y DQG FROOHFW LQ WKUHH HYDSRUDWLRQ WXEHV ÀDVNV RI NQRZQ HPSW\ ZHLJKW e (YDSRUDWH WKH IRXU HOXWLRQ IUDFWLRQV WR GU\QHVV DQG gravimetrically determine the amount of fat eluting in each fraction by subtracting the empty weights from newly recorded weights after solvent evaporation. There should be no fat eluting in the RSWLPXP HOXWLRQ IUDFWLRQ IRU 3$+V WKLV FDQ DOVR EH REVHUYHG YLVXDOO\ LQ WKH WXEHV f ,I WKHUH LV IDW FRHOXWLQJ ZLWK 3$+V WKHQ WKH 3$+ DQG IDW HOXWLRQ SUR¿OHV KDYH WR EH UHH[DPLQHG WR GHWHUPLQH RSWLPXP HOXWLRQ YROXPH IRU 3$+ DQG IDW VHSDUDWLRQ SRWHQWLDOO\ VDFUL¿FLQJ XS WR RI ODWH HOXWLQJ 3$+ DPRXQWV LI QHFHVVDU\ RU D GLIIHUHQW silica gel cartridge has to be used.

7DEOH

) 'LOXWLRQ VFKHPH IRU SUHSDUDWLRQ RI WKH

FDOLEUDWLRQ VWDQGDUG VROXWLRQV

Vol. of mixed stock standard solution, μL

Vol. of working PAH solution a , μL

Vol. of working PAH solution B, μL

Vol. of 13 C-PAH 1 μg/mL solution, μL

Calibration level

Final vol. a , μL

1

—

—

50

50

1000

—

—

100

1000

2

50

—

—

200

1000

3

50

—

—

500

1000

4

50

—

100

—

1000

5

50

—

200

—

1000

6

50

—

500

—

1000

7

50

8

100

—

—

50

1000

Bring to volume using isooctane.

a

© 2015 AOAC INTERNATIONAL