AOAC RI Chemical Cont. Methods-2018 Awards

478  M astovska et al . : J ournal of AOAC I nternational V ol . 98, N o . 2, 2015

aromatic hydrocarbons (PAHs) in seafood. The primary goal was to significantly reduce the time-to-signal (including sample preparation and extraction) in comparison with currently accepted analytical methods requiring 96–120 hours to complete. In addition, acceptable methods had to demonstrate an LOQ of 1 µg/kg for benzo[ a ]pyrene (BaP) in seafood. The SPSC PAH Working Group on Quantitative Methods evaluated about 30 methods that were submitted as a response to the call or found in the literature. The evaluation criteria included: fitness-for-purpose requirements (LOQ, speed, and scope), identification and quantification (compatibility with MS), quality of data to meet AOAC INTERNATIONAL single-laboratory validation requirements (e.g., accuracy, precision, and analysis of reference materials), and practical considerations, such as availability of equipment. The Working Group selected a method developed for the determination of PAHs, polychlorinated biphenyls (PCBs), and polybrominated diphenyl ethers (PBDEs) in fish and seafood by Jana Hajslova’s group at the Institute of Chemical Technology (ICT) in Prague, Czech Republic (1) within a European integrated project CONffIDENCE (Contaminants in Food and Feed: Inexpensive Detection for Control of Exposure; 2). This method was studied within the presented collaborative study, for which the analytes were narrowed down to include only PAHs and some of the relevant PAH alkyl homologs ( see Table 1 for the list of 19 studied analytes and their abbreviations).

Table 1. PAHs included in the collaborative study Name

Abbreviation

1,7-Dimethylphenanthrene 1-Methylnaphthalene 1-Methylphenanthrene 2,6-Dimethylnaphthalene

1,7-DMP

1-MN 1-MP

2,6-DMN

3-Methylchrysene

3-MC

Anthracene

Ant

Benz[ a ]anthracene Benzo[ a ] pyrene Benzo[ b ]fluoranthene Benzo[ g,h,i ]perylene Benzo[ k ]fluoranthene

BaA BaP BbF

BghiP

BkF Chr

Chrysene

Dibenz[ a,h ]anthracene

DBahA

Fluoranthene

Flt

Fluorene

Fln

Indeno[1,2,3- cd ]pyrene

IcdP Naph

Naphthalene Phenanthrene

Phe Pyr

Pyrene

Table 2. PAH fortification levels (in µg/kg) in the shrimp, mussel, and oyster test samples Shrimp Mussel

Oyster

Low

Mid

High

Low

Mid

High

Low

Mid

High

PAH

Level 1

Level 2

Level 4

Level 1

Level 3

Level 4

Level 2

Level 3

Level 5

1,7-DMP a

20 20 10 15 10

20 75 25 40 30 10 15

20

40 20 10 15 10

40

40

80 75 25 40 30 10 15

80

80

1-MN 1-MP

200 125 175 145

100

200 125 175 145

100

250 200 225 225

50 75 90 15 25 10 30 10 20 10 25 50 10

50 75 90 15 25 10 30 10 20 10 25 50 10

2,6-DMN

3-MC

Ant

5 5 2 5 2 2

40 60 25 75 20 40

5 5 2 5 2 2

40 60 25 75 20 40

60

BaA BaP BbF

100

5

5

50

10

10

100

BghiP

5 8

5 8

25 75

BkF Chr

15

50

175

15

100

175

50

100

250

DBahA

2 5

5

15 50

2 5

15 50

5

20 75

Fln

15 25

15 25

Flt

10

100

10

100

150

IcdP Naph

2

5

20

2

20

5

25

25 15 15

80 50 40

160 175 125

25 15 15

125 100

160 175 125

80 50 40

125 100

225 250

Phe Pyr

75 200 a  1,7-DMP served as a homogenization check, which was added to the blank mussel and oyster matrix during the homogenization step (prior to fortification). 75