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建立了液相色谱-电感耦合等离子体质谱法(HPLC-ICP-MS)测定水产品中甲基汞的快速分析方法,实验以甲醇/水/巯基乙醇(V/V/V=5/95/0.5)的混合液为甲基汞提取液,以微波辅助提取为手段,整个前处理过程不到半小时,以甲醇/水/巯基乙醇(V/V/V=5/95/0.1)为流动相,采用C8柱(30 mm×3 mm,3μm),在1.0 mL/min流速下,甲基汞和汞离子在6 min内实现完全分离,两者检出限分别为0.20μg/L和0.50μg/L,相关系数分别为0.9999和0.9993,相对标准偏差RSD≤5.6%,在鱼样中分别添加低(0.20μg/L)、中(1.0μg/L)、高(2.0μg/L)三个浓度的甲基汞标准溶液,回收率为88.0%～99.5%,满足分析测试要求。采用建立的方法研究了鲫鱼对甲基汞的吸收规律,结果表明,随着饲养水域中甲基汞含量的升高以及饲养时间的增加,鲫鱼体内甲基汞的富集越来越显著。
A rapid method for the determination of methylmercury in aquatic products by liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICP-MS) was established. The experiment was carried out with methanol / water / mercaptoethanol (V / V / V = 0.5) was a methylmercury extract, and microwave assisted extraction was used as a means. The whole pretreatment process was less than half an hour with methanol / water / mercaptoethanol (V / V / V = 5/95 / 0.1) The chromatographic separation was performed on a C8 column (30 mm × 3 mm, 3 μm) with a flow rate of 1.0 mL / min. The detection limits were 0.20 μg / L and 0.50 μg / L, and the relative standard deviations were 0.9999 and 0.9993, respectively. The relative standard deviations (RSDs) were less than or equal to 5.6% A concentration of methylmercury standard solution, the recovery rate of 88.0% to 99.5%, to meet the analytical test requirements. The established method was used to study the absorption of methylmercury by crucian carp. The results showed that the accumulation of methylmercury in crucian carp was more and more obvious with the increase of methylmercury in feeding waters and the increase of feeding time.