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A Method for Methylmercury and Inorganic Mercury in Biological Samples Using High Performance Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry.

A new determination method was developed for the measurement of methylmercury (Me-Hg) and inorganic mercury (i-Hg) in biological samples using high-performance liquid chromatography-inductively coupled plasma-mass spectrometry (HPLC-ICP-MS) following alkaline extraction. Mercury species in biological samples were extracted with 10% (w/w) tetramethylammonium hydroxide (TMAH) solution at 80°C for 2 h. Methylmercury was completely separated from i-Hg by adamantyl type and octadecylsilyl type columns within 6 and 4 min using isocratic elution, respectively. The detection limits (3σ) of adamantyl and octadecylsilyl columns using the proposed system were 0.08 and 0.13 ng g-1 (as Hg), respectively. Inorganic Hg completely separates from Me-Hg without tailing. The proposed determination methods were applied to several biological certified reference materials (CRMs). The measurement results of Me-Hg obtained by the present method were in good agreement within the expanded uncertainties (k = 2) with the certified values. The analytical precision (n = 3) of Me-Hg was less than 2%, and the recoveries of Me-Hg and i-Hg were 101 ± 1 and 103 ± 3%, respectively. In addition, this method enables the determination of Me-Hg and i-Hg for 20 samples in 1 h.