292 / 471
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
1,7-DMP
1-Methylnaphthalene
1-MN
1-Methylphenanthrene
1-MP
2,6-Dimethylnaphthalene
2,6-DMN
3-Methylchrysene
3-MC
Anthracene
Ant
Benz[
a
]anthracene
BaA
Benzo[
a
] pyrene
BaP
Benzo[
b
]fluoranthene
BbF
Benzo[
g,h,i
]perylene
BghiP
Benzo[
k
]fluoranthene
BkF
Chrysene
Chr
Dibenz[
a,h
]anthracene
DBahA
Fluoranthene
Flt
Fluorene
Fln
Indeno[1,2,3-
cd
]pyrene
IcdP
Naphthalene
Naph
Phenanthrene
Phe
Pyrene
Pyr
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
20
40
40
40
80
80
80
1-MN
20
75
200
20
100
200
75
100
250
1-MP
10
25
125
10
50
125
25
50
200
2,6-DMN
15
40
175
15
75
175
40
75
225
3-MC
10
30
145
10
90
145
30
90
225
Ant
5
10
40
5
15
40
10
15
60
BaA
5
15
60
5
25
60
15
25
100
BaP
2
5
25
2
10
25
5
10
50
BbF
5
10
75
5
30
75
10
30
100
BghiP
2
5
20
2
10
20
5
10
25
BkF
2
8
40
2
20
40
8
20
75
Chr
15
50
175
15
100
175
50
100
250
DBahA
2
5
15
2
10
15
5
10
20
Fln
5
15
50
5
25
50
15
25
75
Flt
10
25
100
10
50
100
25
50
150
IcdP
2
5
20
2
10
20
5
10
25
Naph
25
80
160
25
125
160
80
125
225
Phe
15
50
175
15
100
175
50
100
250
Pyr
15
40
125
15
75
125
40
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).
Candidates for 2016 Method of the Year
233