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M
ASTOVSKA
ET AL
.:
J
OURNAL OF
AOAC I
NTERNATIONAL
V
OL
.
98, N
O
. 2, 2015
477
Received December 16, 2014.
The method was approved by the Expert Review Panel for
Polycyclic Aromatic Hydrocarbons (PAHs) as First Action.
The Expert Review Panel for Polycyclic Aromatic Hydrocarbons
(PAHs) invites method users to provide feedback on the First
Action methods. Feedback from method users will help verify that
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RESIDUES AND TRACE ELEMENTS
A collaborative study was conducted to determine
selected polycyclic aromatic hydrocarbons (PAHs)
and their relevant alkyl homologs in seafood
matrixes using a fast sample preparation method
followed by analysis with GC/MS. The sample
preparation method involves addition of
13
C-PAH
surrogate mixture to homogenized samples and
extraction by shaking with a water–ethyl acetate
mixture. After phase separation induced by addition
of anhydrous magnesium sulfate–sodium chloride
(2 + 1, w/w) and centrifugation, an aliquot of the
ethyl acetate layer is evaporated, reconstituted in
hexane, and cleaned up using silica gel SPE. The
analytes are eluted with hexane–dichloromethane
(3 + 1, v/v
),
the clean extract is carefully evaporated,
reconstituted in isooctane, and analyzed by GC/MS.
To allow for the use of various GC/MS instruments,
GC columns, silica SPE cartridges, and evaporation
techniques and equipment, performance-based
criteria were developed and implemented in the
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These criteria helped laboratories optimize their
GC/MS, SPE cleanup, and evaporation conditions;
check and eliminate potential PAH contamination
in their reagent blanks; and become familiar with
WKH PHWKRG SURFHGXUH 7HQ ODERUDWRULHV IURP ¿YH
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study, which was conducted on three seafood
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benzo[
a
]pyrene (BaP) ranging from 2 to 50 μg/kg.
Each matrix had a varying mixture of three different
BaP levels. The other studied PAHs were at varying
levels from 2 to 250 μg/kg to mimic typical PAH
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analyzed as blind duplicates at each level of BaP and
corresponding other PAH levels. In addition, a blank
with no added PAHs for each matrix was analyzed
singly. Eight to 10 valid results were obtained for
the majority of determinations. Mean recoveries of
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levels were all in the range of 70–120%: 83.8–115%
in shrimp, 77.3–107% in mussel, and 71.6–94.6% in
oyster, except for a slightly lower mean recovery
of 68.6% for benzo[
a
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25 μg/kg in oyster (RSD
r
: 5.84%, RSD
R
: 21.1%) and
lower mean recoveries for anthracene (Ant) and BaP
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and 48.2–49.7%, respectively). The lower mean
recoveries of Ant and BaP were linked to degradation
of these analytes in oyster samples stored at –20°C,
which also resulted in lower reproducibility (RSD
R
values in the range of 44.5–64.7% for Ant and
40.6–43.5% for BaP). However, the repeatability was
good (RSD
r
of 8.78–9.96% for Ant and 6.43–11.9%
for BaP), and the HorRat values were acceptable
(1.56–1.94 for Ant and 1.10–1.45 for BaP). In all other
cases, repeatability, reproducibility, and HorRat
values were as follows: shrimp: RSD
r
1.40–26.9%,
RSD
R
5.41–29.4%, HorRat: 0.22–1.34; mussel: RSD
r
2.52–17.1%, RSD
R
4.19–32.5%, HorRat: 0.17–1.13;
and oyster: RSD
r
3.12–22.7%, RSD
R
8.41–31.8%,
HorRat: 0.34–1.39. The results demonstrate that
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and their alkyl homologs in seafood samples. The
method was approved by the Expert Review Panel
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2014.08.
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s a response to the 2010 oil spill in the Gulf of Mexico,
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issued a call for methods for determination of polycyclic
Determination of Polycyclic Aromatic Hydrocarbons (PAHs)
in Seafood Using Gas Chromatography-Mass Spectrometry:
Collaborative Study
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