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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

ƒ& 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