Table of Contents Table of Contents
Previous Page  35 / 311 Next Page
Information
Show Menu
Previous Page 35 / 311 Next Page
Page Background

© 2015 AOAC INTERNATIONAL

&RQWDLQLQJ $FHQDSKWKHQH

13

C

6

DFHQDSKWK\OHQH

13

C

6

,

DQWKUDFHQH

13

C

6

EHQ]>

a

@DQWKUDFHQH

13

C

6

benzo[

b

@ÀXRUDQWKHQH

13

C

6

EHQ]R>

k

@ÀXRUDQWKHQH

13

C

6

,

EHQ]R>

g,h,i

@SHU\OHQH

13

C

12

EHQ]R>

a

@S\UHQH

13

C

4

,

FKU\VHQH

13

C

6

GLEHQ]>

a,h

@DQWKUDFHQH

13

C

6

ÀXRUDQWKHQH

13

C

6

ÀXRUHQH

13

C

6

LQGHQR>

cd

]

S\UHQH

13

C

6

QDSKWKDOHQH

13

C

6

SKHQDQWKUHQH

13

C

6

,

DQG S\UHQH

13

C

6

( 3UHSDUDWLRQ RI 6WDQGDUG 6ROXWLRQV

a

Individual stock solutions.—

Prepare individual PAH stock

VROXWLRQV DW DSSUR[LPDWHO\

RU

—J P/ LQ WROXHQH

b

Mixed stock standard solution.—

Use analyte individual

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 DQG

dilute to volume with isooctane.

d

Working PAH Solution B.—

$FFXUDWHO\ WUDQVIHU P/ RI WKH

:RUNLQJ 3$+ 6ROXWLRQ $ LQWR D P/ YROXPHWULF ÀDVN DQG GLOXWH WR

volume with isooctane.

e

Internal standard solution.—

3UHSDUH —J P/ VROXWLRQ RI

13

& 3$+V LQ LVRRFWDQH E\ IROG GLOXWLRQ RI WKH —J P/ (3$

13

C-PAHs cocktail with isooctane.

f

Calibration standard solutions.—

Prepare eight levels of

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

.—Accurately transfer

—/ RI WKH :RUNLQJ 3$+ 6ROXWLRQ % LQWR WKH YLDO DQG DGG —/

RI WKH —J P/

13

& 3$+V VROXWLRQ DQG —/ LVRRFWDQH &DS WKH

YLDO DQG YRUWH[ PL[ EULHÀ\

2 For level 2 calibration standard

.—Accurately transfer

—/ RI WKH :RUNLQJ 3$+ 6ROXWLRQ % LQWR WKH YLDO DQG DGG —/

RI WKH —J P/

13

& 3$+V VROXWLRQ DQG —/ LVRRFWDQH &DS WKH

YLDO DQG YRUWH[ PL[ EULHÀ\

3 For level 3 calibration standard

.—Accurately transfer

—/ RI WKH :RUNLQJ 3$+ 6ROXWLRQ % LQWR WKH YLDO DQG DGG —/

RI WKH —J P/

13

& 3$+V VROXWLRQ DQG —/ LVRRFWDQH &DS WKH

YLDO DQG YRUWH[ PL[ EULHÀ\

4 For level 4 calibration standard

.—Accurately transfer

—/ RI WKH :RUNLQJ 3$+ 6ROXWLRQ % LQWR WKH YLDO DQG DGG —/

RI WKH —J P/

13

& 3$+V VROXWLRQ DQG —/ LVRRFWDQH &DS WKH

YLDO DQG YRUWH[ PL[ EULHÀ\

5 For level 5 calibration standard

.—Accurately transfer

—/ RI WKH :RUNLQJ 3$+ 6ROXWLRQ $ LQWR WKH YLDO DQG DGG —/

RI WKH —J P/

13

& 3$+V VROXWLRQ DQG —/ LVRRFWDQH &DS WKH

YLDO DQG YRUWH[ PL[ EULHÀ\

6 For level 6 calibration standard

.—Accurately transfer

—/ RI WKH :RUNLQJ 3$+ 6ROXWLRQ $ LQWR WKH YLDO DQG DGG —/

RI WKH —J P/

13

& 3$+V VROXWLRQ DQG —/ LVRRFWDQH &DS WKH

YLDO DQG YRUWH[ PL[ EULHÀ\

7 For level 7 calibration standard

.—Accurately transfer

—/ RI WKH :RUNLQJ 3$+ 6ROXWLRQ $ LQWR WKH YLDO DQG DGG —/

RI WKH —J P/

13

& 3$+V VROXWLRQ DQG —/ LVRRFWDQH &DS WKH

YLDO DQG YRUWH[ PL[ EULHÀ\

8 For level 8 calibration standard

.—Accurately transfer

—/ RI WKH PL[HG VWRFN VWDQGDUG VROXWLRQ LQWR WKH YLDO DQG DGG

—/ RI WKH —J P/

13

& 3$+V VROXWLRQ DQG —/ LVRRFWDQH &DS

WKH YLDO DQG YRUWH[ PL[ EULHÀ\

F. Extraction and Cleanup Procedure

1

$GG —/ RI WKH —J P/

13

& 3$+V VROXWLRQ WR “ J RI

WKRURXJKO\ KRPRJHQL]HG VHDIRRG VDPSOH LQ D P/ SRO\SURS\OHQH

centrifuge tube.

2

9RUWH[ VDPSOH IRU V DQG OHW HTXLOLEUDWH IRU PLQ

3

$GG P/ P/ LQ WKH FDVH RI VKULPS RI SXUL¿HG ZDWHU

DQG P/ HWK\O DFHWDWH

4

6KDNH WXEH YLJRURXVO\ E\ KDQG IRU PLQ

5

$GG J RI PXIÀHG DQK\GURXV PDJQHVLXP VXOIDWH DQG J

VRGLXP FKORULGH DQG VHDO WKH WXEH ZHOO HQVXUH WKDW SRZGHU GRHV

QRW JHW LQWR WKH VFUHZ WKUHDGV RU ULP RI WKH WXEH

6

6KDNH WXEH YLJRURXVO\ E\ KDQG IRU PLQ HQVXULQJ WKDW

FU\VWDOOLQH DJJORPHUDWHV DUH EURNHQ XS VXI¿FLHQWO\ GXULQJ VKDNLQJ

7

&HQWULIXJH WXEH DW ! UFI IRU PLQ

8

7DNH D P/ DOLTXRW RI WKH XSSHU HWK\O DFHWDWH OD\HU DGG

—/ LVRRFWDQH DV D NHHSHU DQG JHQWO\ HYDSRUDWH DOO HWK\O DFHWDWH

until only isooctane and co-extracted sample fat are left.

9

5HFRQVWLWXWH LQ P/ KH[DQH

7DEOH

&

continued

PAH

No. of

laboratories

No. of

replicates

Mean

concn, μg/kg

Mean

recovery, % s

r

, μg/kg

s

R

, μg/kg RSD

r

, % RSD

R

, % HorRat

10

20

17.9

89.3

0.9

1.6

4.9

8.8

0.30

Naph

9

18

23.7

94.6

1.9

4.0

8.1

17.1

0.61

10

20

105.9

84.7

10.1

26.7

9.5

25.2

1.12

8

16

146.7

91.7

7.2

19.2

4.9

13.1

0.61

Phe

8

16

14.5

96.8

0.8

0.9

5.3

6.1

0.20

8

16

93.1

93.1

3.9

8.5

4.1

9.2

0.40

8

16

160.8

91.9

5.8

13.0

3.6

8.1

0.38

Pyr

10

20

14.2

94.6

0.7

1.3

5.0

9.3

0.31

10

20

71.5

95.4

2.9

7.0

4.0

9.8

0.41

10

20

116.5

93.2

4.5

9.6

3.8

8.3

0.37