![Show Menu](styles/mobile-menu.png)
![Page Background](./../common/page-substrates/page0085.png)
M
ASTOVSKA
ET AL
.:
J
OURNAL OF
AOAC I
NTERNATIONAL
V
OL
.
98, N
O
. 2, 2015
485
HYDSRUDWLRQ WHFKQLTXH H J VPDOO URXQG ERWWRP ÀDVNV VXLWDEOH
WXEHV RU JODVVZDUH IRU .XGHUQD 'DQLVK HYDSRUDWLRQ ,W LV
UHFRPPHQGHG WR KHDW WKH JODVVZDUH IRU DW OHDVW K DW
& WR
remove potential contamination.
D. Reference Standards
(
a
)
PAH standards.—
+LJK SXULW\ UHIHUHQFH VWDQGDUGV RI WKH
3$+DQDO\WHV
GLPHWK\OSKHQDQWKUHQH PHWK\OQDSKWKDOHQH
PHWK\OSKHQDQWKUHQH
GLPHWK\OQDSKWKDOHQH PHWK\O
FKU\VHQH DQWKUDFHQH EHQ]>
a
@DQWKUDFHQH EHQ]R>
a
]pyrene,
EHQ]R>
b
@ÀXRUDQWKHQH
EHQ]R>
g,h,i
@SHU\OHQH
EHQ]R>
k
]
ÀXRUDQWKHQH FKU\VHQH GLEHQ]>
a,h
@DQWKUDFHQH ÀXRUDQWKHQH
ÀXRUHQH LQGHQR>
cd
]pyrene, naphthalene, phenanthrene,
and pyrene).
(
b
)
U.S. Environmental Protection Agency (EPA) 16 PAH
cocktail.—
( & 3URGXFW 1R (6
J P/ P/
LQ QRQDQH &DPEULGJH ,VRWRSH /DEV
7HZNVEXU\ 0$ 86$
)
or equivalent.
&RQWDLQLQJ $FHQDSKWKHQH &
6
DFHQDSKWK\OHQH
( &
6
DQWKUDFHQH &
6
EHQ]>
a
]anthracene ( &
6
,
EHQ]R>
b
@ÀXRUDQWKHQH &
6
EHQ]R>
k
@ÀXRUDQWKHQH
( &
6
EHQ]R>
g,h,i
]perylene ( &
12
EHQ]R>
a
]pyrene
( &
4
FKU\VHQH &
6
GLEHQ]>
a,h
]anthracene
( &
6
ÀXRUDQWKHQH &
6
ÀXRUHQH &
6
LQGHQR>
cd
]pyrene ( &
6
QDSKWKDOHQH &
6
phenanthrene ( &
6
DQG S\UHQH &
6
E. Preparation of Standard Solutions
(
a
)
Individual stock solutions.—
Prepare individual PAH
VWRFN VROXWLRQV DW DSSUR[LPDWHO\ RU
J P/ LQ WROXHQH
(
b
)
Mixed stock standard solution.—
8VH DQDO\WH LQGLYLGXDO
stock solutions to obtain a mixed solution of each PAH at
J P/ IRU EHQ]R>
a
@S\UHQH DQG RWKHU ORZ OHYHO 3$+V
RU
J P/ IRU FKU\VHQH DQG RWKHU KLJKHU OHYHO 3$+V RU
J P/ IRU QDSKWKDOHQH LQ LVRRFWDQH
See
Table
2014.08E
for analyte concentrations in the mixed stock standard solution.
(
c
)
Working PAH Solution A.—
$FFXUDWHO\ WUDQVIHU
P/ RI
WKH PL[HG VWRFN VWDQGDUG VROXWLRQ LQWR D P/ YROXPHWULF ÀDVN
and dilute to volume with isooctane.
(
d
)
Working PAH Solution B.—
$FFXUDWHO\ WUDQVIHU
P/ RI
WKH :RUNLQJ 3$+ 6ROXWLRQ $ LQWR D P/ YROXPHWULF ÀDVN DQG
dilute to volume with isooctane.
(
e
)
Internal standard solution.—
3UHSDUH J P/ VROXWLRQ RI
& 3$+V LQ LVRRFWDQH E\ IROG GLOXWLRQ RI WKH J P/ (3$
& 3$+V FRFNWDLO ZLWK LVRRFWDQH
(
f
)
Calibration standard solutions—
3UHSDUH HLJKW OHYHOV
RI FDOLEUDWLRQ VWDQGDUG VROXWLRQV P/ HDFK LQ P/ DPEHU
VFUHZ FDS YLDOV ,W LV UHFRPPHQGHG WR GLVWULEXWH VPDOO SRUWLRQV
HQRXJK IRU D VLQJOH LQMHFWLRQ RI WKH FDOLEUDWLRQ VWDQGDUG
VROXWLRQV LQWR PXOWLSOH FULPS WRS YLDOV ZLWK / GHDFWLYDWHG
JODVV LQVHUWV
See
Table
2014.08A
for analyte concentrations in
the calibration standards and Table
2014.08F
for the dilution
scheme.
(
1
)
For level 1 calibration standard
±$FFXUDWHO\ WUDQVIHU
/ RI WKH :RUNLQJ 3$+ 6ROXWLRQ % LQWR WKH YLDO DQG DGG
/ RI WKH J P/ & 3$+V VROXWLRQ DQG / LVRRFWDQH
&DS WKH YLDO DQG YRUWH[ PL[ EULHÀ\
(
2
)
For level 2 calibration standard
±$FFXUDWHO\ WUDQVIHU
/ RI WKH :RUNLQJ 3$+ 6ROXWLRQ % LQWR WKH YLDO DQG DGG
/ RI WKH J P/ & 3$+V VROXWLRQ DQG / LVRRFWDQH
&DS WKH YLDO DQG YRUWH[ PL[ EULHÀ\
(
3
)
For level 3 calibration standard
±$FFXUDWHO\ WUDQVIHU
/ RI WKH :RUNLQJ 3$+ 6ROXWLRQ % LQWR WKH YLDO DQG DGG
/ RI WKH J P/ & 3$+V VROXWLRQ DQG / LVRRFWDQH
&DS WKH YLDO DQG YRUWH[ PL[ EULHÀ\
(
4
)
For level 4 calibration standard
±$FFXUDWHO\ WUDQVIHU
/ RI WKH :RUNLQJ 3$+ 6ROXWLRQ % LQWR WKH YLDO DQG DGG
/ RI WKH J P/ & 3$+V VROXWLRQ DQG / LVRRFWDQH
&DS WKH YLDO DQG YRUWH[ PL[ EULHÀ\
(
5
)
For level 5 calibration standard
±$FFXUDWHO\ WUDQVIHU
/ RI WKH :RUNLQJ 3$+ 6ROXWLRQ $ LQWR WKH YLDO DQG DGG
/ RI WKH J P/ & 3$+V VROXWLRQ DQG / LVRRFWDQH
&DS WKH YLDO DQG YRUWH[ PL[ EULHÀ\
(
6
)
For level 6 calibration standard
±$FFXUDWHO\ WUDQVIHU
/ RI WKH :RUNLQJ 3$+ 6ROXWLRQ $ LQWR WKH YLDO DQG DGG
/ RI WKH J P/ & 3$+V VROXWLRQ DQG / LVRRFWDQH
&DS WKH YLDO DQG YRUWH[ PL[ EULHÀ\
(
7
)
For level 7 calibration standard
±$FFXUDWHO\ WUDQVIHU
/ RI WKH :RUNLQJ 3$+ 6ROXWLRQ $ LQWR WKH YLDO DQG DGG
/ RI WKH J P/ & 3$+V VROXWLRQ DQG / LVRRFWDQH
&DS WKH YLDO DQG YRUWH[ PL[ EULHÀ\
(
8
)
For level 8 calibration standard
±$FFXUDWHO\ WUDQVIHU
/ RI WKH PL[HG VWRFN VWDQGDUG VROXWLRQ LQWR WKH YLDO DQG
Table 2014.08C. (
continued
)
PAH
1R RI
laboratories
1R RI
replicates
Mean
concn, μg/kg
Mean
recovery, % s
r
, μg/kg s
R
, μg/kg RSD
r
, % RSD
R
, % HorRat
10
20
Naph
9
18
10
20
8
16
Phe
8
16
8
16
8
16
Pyr
10
20
10
20
10
20