AOAC-RI ERP Book - FAOM METHOD.pdf

M ASTOVSKA ET AL .: J OURNAL OF AOAC I NTERNATIONAL V OL . 98, N O . 2, 2015 479

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Collaborative Study

Purpose

7KH SXUSRVH RI WKLV VWXG\ ZDV WR HYDOXDWH WKH PHWKRG¶V intralaboratory and interlaboratory performance and submit the UHVXOWV WR $2$& ,17(51$7,21$/ IRU DGRSWLRQ DV DQ 2I¿FLDO Method for the determination of PAHs in seafood.

Study Design

This study evaluated the method performance for GHWHUPLQDWLRQ RI VHOHFWHG 3$+V LQFOXGLQJ DON\O KRPRORJV relevant to an oil spill contamination ( see Table 1), in three VHDIRRG PDWUL[HV VKULPS R\VWHUV DQG PXVVHOV ZLWK ¿YH GLIIHUHQW OHYHOV RI %D3 UDQJLQJ IURP WR —J NJ (DFK PDWUL[ KDG D YDU\LQJ PL[WXUH RI WKUHH GLIIHUHQW %D3 OHYHOV ³ORZ ´ ³PLG ´ DQG ³KLJK´ 7KH RWKHU VWXGLHG 3$+V ZHUH DGGHG DW YDU\LQJ OHYHOV IURP WR —J NJ WR PLPLF W\SLFDO 3$+ SDWWHUQV 7DEOH 7KH IRUWL¿HG DQDO\WHV LQ WKH WKUHH PDWUL[HV ZHUH DQDO\]HG DV EOLQG GXSOLFDWHV DW HDFK OHYHO RI %D3 DQG FRUUHVSRQGLQJ RWKHU 3$+ OHYHOV ,Q DGGLWLRQ D EODQN ZLWK QR DGGHG 3$+V IRU HDFK PDWUL[ ZDV DQDO\]HG VLQJO\ 7KH $2$& RI¿FLDO PHWKRG JXLGHOLQHV IRU FROODERUDWLYH VWXG\ SURFHGXUHV were followed for the preparation of the study and data analysis. %ODQN PXVVHO DQG R\VWHU VDPSOHV ZHUH KRPRJHQL]HG ZLWK OLTXLG QLWURJHQ DQG WHVWHG LQ GXSOLFDWH E\ DQ LQGHSHQGHQW ODERUDWRU\ IRU SRWHQWLDO FRQWDPLQDWLRQ ZLWK WKH WDUJHW 3$+V 'XULQJ KRPRJHQL]DWLRQ SRUWLRQV RI WKH EODQN PDWUL[HV ZHUH VSLNHG ZLWK GLPHWK\OSKHQDQWKUHQH '03 DW DQG —J NJ LQ WKH FDVH RI PXVVHO DQG R\VWHU UHVSHFWLYHO\ 7KHVH ZHUH XWLOL]HG DV D KRPRJHQL]DWLRQ FKHFN WKURXJKRXW WKH FRXUVH RI WKH VWXG\ 7KH FROODERUDWRUV GHWHUPLQHG '03 DORQJ ZLWK WKH RWKHU DQDO\WHV ZKLFK ZHUH VSLNHG LQWR J VDPSOH SRUWLRQV SODFHG LQ SRO\SURS\OHQH FHQWULIXJH WXEHV E\ WKH VWXG\ GLUHFWLRQ WHDP )LYH GLIIHUHQW VSLNLQJ OHYHOV ZHUH PDGH DW YDU\LQJ 3$+ FRQFHQWUDWLRQV 7DEOH UHVXOWLQJ LQ WKUHH GLIIHUHQW GXSOLFDWH VSLNHG VDPSOHV PDWUL[ LQ DGGLWLRQ WR a blank. Participants were supplied with the test samples ready IRU DQDO\VLV ODEHOHG ZLWK XQLTXH LGHQWL¿FDWLRQ QXPEHUV $OO WHVW VDPSOHV ZHUH VKLSSHG IUR]HQ RQ GU\ LFH ZLWK D PDWHULDO UHFHLSW GRFXPHQW WR EH UHWXUQHG WR WKH 6WXG\ 'LUHFWRUV 7KH WHVW VDPSOHV KDG WR EH VWRUHG LQ D IUHH]HU VHW WR PDLQWDLQ DW OHDVW ± “ ƒ& 7HVW VDPSOHV ZHUH WR EH DQDO\]HG DIWHU FRPSOHWLRQ RI ODERUDWRU\ TXDOL¿FDWLRQ DQG SUDFWLFH VDPSOH DQDO\VLV %ODQN VKULPS PDWUL[ SHHOHG ZLWKRXW KHDG DQG WDLO DQG XQFRRNHG ZDV KRPRJHQL]HG ZLWKRXW WKH XVH RI OLTXLG QLWURJHQ XVLQJ D EOHQGHU $IWHU WHVWLQJ IRU SRWHQWLDO FRQWDPLQDWLRQ ZLWK WKH WDUJHW 3$+V J EODQN VDPSOH SRUWLRQV ZHUH SODFHG LQ SRO\SURS\OHQH FHQWULIXJH WXEHV ZKLFK ZHUH VHQW WR VWXG\ SDUWLFLSDQWV WRJHWKHU ZLWK VSLNLQJ VROXWLRQV ODEHOHG ZLWK XQLTXH LGHQWL¿FDWLRQ QXPEHUV 8VLQJ LQVWUXFWLRQV SURYLGHG E\ WKH 6WXG\ 'LUHFWRUV SDUWLFLSDQWV IRUWL¿HG WKH EODQN VKULPS VDPSOHV themselves on the day of the analysis. 7KUHH GLIIHUHQW VSLNLQJ OHYHOV ZHUH XVHG DW YDU\LQJ 3$+ FRQFHQWUDWLRQV 7DEOH UHVXOWLQJ LQ WKUHH GLIIHUHQW GXSOLFDWH VSLNHG VDPSOHV LQ DGGLWLRQ WR D EODQN VHYHQ VDPSOHV DOWRJHWKHU Test Sample Preparation

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