![Show Menu](styles/mobile-menu.png)
![Page Background](./../common/page-substrates/page0038.jpg)
© 2015 AOAC INTERNATIONAL
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
( $QDO\WH FRQFHQWUDWLRQV LQ WKH PL[HG VWRFN
VWDQGDUG VROXWLRQ
Analyte
Concentration, μg/mL
Anthracene
10
Benz[
a
]anthracene
10
Benzo[
a
]pyrene
10
Benzo[
b
@ÀXRUDQWKHQH
10
Benzo[
g,h,i
]perylene
10
Benzo[
k
@ÀXRUDQWKHQH
10
Chrysene
25
Dibenz[
a,h
]anthracene
10
Fluoranthene
25
Fluorene
10
Indeno[1,2,3-
cd
]pyrene
10
Naphthalene
50
Phenanthrene
25
Pyrene
25
1-Methylnaphthalene
25
2,6-Dimethylnaphthalene
25
1-Methylphenanthrene
25
1,7-Dimethylphenanthrene
10
3-Methylchrysene
25
7DEOH
) 'LOXWLRQ VFKHPH IRU SUHSDUDWLRQ RI WKH
FDOLEUDWLRQ VWDQGDUG VROXWLRQV
Calibration
level
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
Final
vol.
a
, μL
1
—
—
50
50
1000
2
—
—
100
50
1000
3
—
—
200
50
1000
4
—
—
500
50
1000
5
—
100
—
50
1000
6
—
200
—
50
1000
7
—
500
—
50
1000
8
100
—
—
50
1000
a
Bring to volume using isooctane.
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
2SWLPXP HOXWLRQ YROXPH
)LJXUH
% $Q H[DPSOH RI HOXWLRQ SUR¿OHV RI 3$+V
RQ D VLOLFD JHO 63( FDUWULGJH DQG GHWHUPLQDWLRQ RI WKH
RSWLPXP HOXWLRQ YROXPH