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Mercury speciation in Cuban commercial edible fish by HPLC-ICP-MS using the double spike isotope dilution analysis strategy

A sensitive and accurate quantitative method for the speciation of inorganic Hg2+ and methyl-mercury by ID-HPLC–ICP-MS has been optimised and implemented for marine fish samples. Quantitative extraction of Hg species was achieved using a 0.1% (v/v) 2-mercaptoethanol, 0.05% (w/v) L-cysteine and 0.10% (v/v) HCl solution by sonication for 30 min. Chromatographic separation of mercury species was carried out on a C8 reverse phase column with 0.05% (v/v) 2-mercaptoethanol, 0.075% (w/v) L-cysteine and 0.06 mol L−1 ammonium acetate as the mobile phase. A species specific isotope dilution analysis approach, using 201CH3Hg+ and 200Hg2+ was employed for the quantification of both species. Two biological Certified Reference Materials (DOLT-2, DORM-2) were analysed to assess the analytical performance. No significant differences were found between the obtained concentrations and the certified reference values for total Hg and CH3Hg+. The results indicate that no species interconversion reactions occurred during the used extraction and chromatographic separation procedures. The detection limits for CH3Hg+ and Hg2+ species were 7.7 and 5.2 ng g−1, respectively. The method recovery (expressed as the sum of both species contents in relation to total Hg concentration analysed by ICP-MS) was about 97 ± 5%. The procedure was applied to speciation of mercury in 12 species of the most commonly consumed commercial fish in Cuba.