碱消解-高效液相色谱-电感耦合等离子体质谱法测定生物样品中的甲基汞和乙基汞

Determination of Methylmercury and Ethylmercury in Biological Samples by Alkaline Digestion-High Performance Liquid Chromatography-Inductively Coupled Plamas Mass Spectrometry

摘要: 建立了碱消解-高效液相色谱-电感耦合等离子体质谱联用系统测定生物样品中甲基汞(MeHg)与乙基汞(EtHg)的分析方法.为提高灵敏度,选用微流量的PFA雾化器,在优化的检测条件下,MeHg及EtHg检出限可达到0.036μg/L和0.03μg/L;线性范围达到4个数量级,两条工作曲线线性相关系数为1.对1.78μg/L MeHg、1.65μg/L EtHg的混合标准溶液重复测定7次,色谱峰面积的相对标准偏差(RSD)分别为1.79%和1.44%.对标准物质BCR 464(金枪鱼)的分析结果表明,测定值与标准值基本吻合,但略低于标准值;甲基汞和乙基汞的加标回收率分别为85.9%和84.5%.高效液相色谱与质谱联用技术的高灵敏度和低检出限能够满足生物样品中汞形态定量分析的要求.

Abstract: A method for the determination of methylmercury and ethylmercury in biological samples by HPLC-ICP-MS with alkaline digestion was established. Micro-flow nebulizer was used to improve intensity. In optimized conditions, the detection limits for methylmercury and ethylmercury were 0.036 μg/L and 0.03 μg/L respectively. The linear range was up to 4 order of magnitude from 0.03x μg/L to 3x μg/L and the relative standard deviation was 1.79％ and 1.44％. The method was validated by analyzing the BCR 464 (tunny) and spiked experiment. The recovery was 85.9% for methylmercury and 84.5% for ethylmercury.