Mercury speciation in thawed out and refrozen fish samples by gas chromatography coupled to inductively coupled plasma mass spectrometry and atomic fluorescence spectroscopy.
Different sub-sampling procedures were applied for the determination of mercury species (as total mercury Hg, methylmercury MeHg+ and inorganic mercury Hg2+) in frozen fish meat. Analyses were carried out by two different techniques. After the sample material was pre-treated by microwave digestion, atomic fluorescence spectroscopy (AFS) was used for the determination of total Hg. Speciation analysis was performed according to the following procedure: dissolution of sample material in tetramethylammonium hydroxide (TMAH), derivatisation with sodium tetraethylborate (NaBEt4), extraction into isooctane and measurement with gas chromatography inductively coupled plasma mass spectrometry (GC-ICPMS) for the identification and quantification of methylmercury (MeHg+) and inorganic mercury (Hg2+). The concentration range of total Hg measured in the shark fillets is between 0.9 and 3.6 microg g(-1) thawed out shark fillet. Speciation analysis leads to > or =94% Hg present as MeHg+. Homogeneity, storage conditions and stability of analytical species and sample materials have great influence on analytical results. Sub-sampling of half-frozen/partly thawed out fish and analysis lead to significantly different concentrations, which are on average a factor of two lower.
Krystek
Petra
P
Laboratory for Analytical Chemistry, National Institute for Public Health and the Environment (RIVM), P.O. Box 1, 3720, BA, Bilthoven, The Netherlands. petra.krystek@rivm.nl
Ritsema
Rob
R
D000818:Animals; D005399:Fishes; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D008628:Mercury / Q000032:analysis / Q000145:classification*; D011786:Quality Control; D012015:Reference Standards; D013050:Spectrometry, Fluorescence / Q000379:methods*
D008628:Mercury