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NRC Publications Archive Archives des publications du CNRCThis publication could be one of several versions: author's original, accepted manuscript or the publisher's version. / La version de cette publication peut être l'une des suivantes : la version prépublication de l'auteur, la version acceptée du manuscrit ou la version de l'éditeur. For the publisher's version, please access the DOI link below./ Pour consulter la version de l'éditeur, utilisez le lien DOI ci-dessous.http://doi.org/10.1039/b301299aJournal of Analytical Atomic Spectrometry, 18, 5, pp. 431-436, 2003 Determination of methylmercury in fish tissues by isotope dilution SPME-GC-ICP-MS{ A method is described for the accurate and precise determination of monomethylmercury (MMHg) by species specific isotope dilution (ID) calibration using solid phase microextraction (SPME) in combination with gas chromatographic (GC) separation and inductively coupled plasma mass spectrometric (ICP-MS) detection. Samples were digested with methanolic potassium hydroxide, derivatized in aqueous solution with sodium tetrapropylborate and headspace sampled with a polydimethylsiloxane coated SPME fused silica fiber. The analyte was then directly transferred from the fiber to the head of the GC column for desorption by insertion of the fiber through the heated injection port. Reverse spike ID analysis was performed to determine the accurate concentration of an in-house synthesized 198 Hg-enriched monomethylmercury (MM 198 Hg) spike [candidate Certified Reference Material (CRM) EOM-1] using two natural abundance MMHg standards. Concentrations of 0.719 ¡ 0.015 and 4.484 ¡ 0.029 mgg 21 (one standard de...