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建立了微波辅助萃取、高效液相色谱-电感耦合等离子体质谱联用(HPLC-ICP/MS)测定生物样品中汞形态的方法.采用醋酸铵/L-半胱氨酸缓冲盐及甲醇体系组成的流动相按一定比例进行梯度洗脱,并结合了ICP/MS的时间分辨采集优化程序分析二价汞、甲基汞、乙基汞、苯基汞等4种汞形态.根据所建立的HPLCICP/MS方法分析了鱼肉及人发标准参考物质中的汞形态,样品前处理采用盐酸-半胱氨酸体系作为萃取剂、微波辅助萃取法.对于鱼肉和人发标准参考物质,6次平行样测定结果的相对标准偏差(RSD%)均小于5%,且测定值与标准值较吻合.该方法前处理简单、样品提取效率高、分析时间短、精密度及重现性理想,极适用于生物样品中汞形态的快速萃取与分析.
A method for the determination of mercury speciation in biological samples by microwave-assisted extraction and high performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICP / MS) was established.The ammonium acetate / L-cysteine buffer salt and methanol system The mobile phase was eluted with a certain percentage of gradient and combined with ICP / MS time-resolved collection and optimization program to analyze the four mercury species such as mercury, methylmercury, ethylmercury and phenylmercury.According to HPLCICP / MS method was used to analyze the mercury speciation in standard reference materials for fish and human hair.The samples were pretreated with hydrochloric acid-cysteine as extraction solvent and microwave-assisted extraction method.For fish and human hair reference materials, six parallel samples The results showed that the relative standard deviations (RSD%) were less than 5%, and the measured values were in good agreement with the standard values.The method was simple in pretreatment, high in sample extraction efficiency, short in analysis time, good in precision and reproducibility, Rapid Extraction and Analysis of Mercury Speciation in Biological Samples.