title: A method for the routine determination of methylmercury in marine tissue by GC isotope dilution-ICP-MS.
abstract: Currently, there is no legal limit for methyl mercury (MeHg) in food; thus, no standardized method for the determination of MeHg in seafood exists within the European jurisdiction. In anticipation of a future legislative limit an inductively coupled plasma isotope dilution mass spectrometry (GC-ICP-ID-MS) method was developed in collaboration with the European Standardization Organization (CEN). The method comprises spiking the tissue sample with Me201Hg, followed by decomposition with tetramethylammonium hydroxide, pH adjustment and derivatization with sodium tetraethylborate, and finally organic extraction of the derivatized MeHg in a hexane phase. Subsequently, the sample is analyzed via GC-ICP-MS and the result calculated using the ID equation. The working range of the method was 0.0005-1.321 mg/kg MeHg in marine tissue, with an internal reproducibility (RSD) of 12-1%. The method was validated based on statistical measures, such as the z-scores, using the commercially available reference materials from National Institute of Standards and Technology Standard Reference Material (NIST SRM) 1566b, NIST SRM 2977 and National Research Council of Canada (NRCC) TORT 2, NRCC, DORM 3, NRCC DOLT 4, and European Reference Material (ERM) CE 464. Z-scores for all standard reference materials, except for NIST SRM 1566b, were better than 11.51. The wide range of marine tissues used during the validation ensures that the method will be applicable for measuring of MeHg in seafood matrixes of all kinds.
authors.affiliation: National Institute of Nutrition and Seafood Research, P.O. Box 2029 Nordnes, 5817 Bergen, Norway. sva@nifes.no
authors.forename: Stig
authors.initials: S
authors.lastname: Valdersnes
authors.forename: Amund
authors.initials: A
authors.lastname: Maage
authors.forename: Daniel
authors.initials: D
authors.lastname: Fliegel
authors.forename: Kåre
authors.initials: K
authors.lastname: Julshamn
mesh_terms: D001881:Borates / Q000737:chemistry; D002623:Chemistry Techniques, Analytical / Q000379:methods* / Q000592:standards; D002845:Chromatography / Q000379:methods; D005060:Europe; D005504:Food Analysis / Q000379:methods*; D005506:Food Contamination / Q000032:analysis*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006586:Hexanes / Q000737:chemistry; D006863:Hydrogen-Ion Concentration; D007201:Indicator Dilution Techniques; D007554:Isotopes / Q000737:chemistry; D013058:Mass Spectrometry / Q000379:methods* / Q000592:standards; D008767:Methylmercury Compounds / Q000032:analysis*; D012015:Reference Standards; D015203:Reproducibility of Results; D017747:Seafood / Q000032:analysis*; D014481:United States
chemical_list: D001881:Borates; D006586:Hexanes; D007554:Isotopes; D008767:Methylmercury Compounds; C080440:sodium tetraethylborate; C073972:dimethyl mercury