毛细管气相色谱法测定生物样品中痕量甲基汞  

GC DETERMINATION OF TRACE AMOUNTS OF METHYL-MERCURY IN BIOLOGICAL SAMPLES WITH CAPILLARY CHROMATOGRAPHIC COLUMN

作　　者：朱霞萍[1] 张勇[1] 汪模辉[1] 苏茜[1] 倪师军[1] 何秋玲[1] 

机构地区：[1]成都理工大学 材料与化学化工学院,成都610059

出　　处：《理化检验（化学分册）》2006年第5期344-346,共3页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：教育部高校博士学科点专项科研基金(No.20050616009);国家地质调查项目(No.200314200015)

摘　　要：建立了以5 g·L-1L-半胱氨酸为萃取溶剂,采用改装的家用微波炉微波辅助加热提取分离,所得溶液用盐酸酸化后用苯反萃取后用毛细管气相色谱(电子捕获器)测定甲基汞的新方法测定甲基汞的线性范围为0．1～1．0 ng,检出限为0．064 ng对0．80 ng甲基汞进行7次测定,其RSD为4．58%,应用于实际样品中甲基汞的测定,回收率在95．5％-102．3％之间。A gas chromatographic method using capillary chromatographic column （OV-17） and electron capture detection was proposed for the determination of methylmercury in biological samples. The sample was pretreated with 5 g·L^-1 aqueous solution of L-cysteine assisted by microwave heating, to extract methylmercury and make it dissolved in aqueous solution, which was back-extracted with benzene after acidifying the solution with HC1, to separate methylmercury from fat and protein co-existing in the sample. The range of linearity for the method was from 0. 1-1.0 ng, with a detection limit of 0. 064 ng. Precision test at the concentration level of 0. 80 ng gave a value of RSD （n=7） of 4.58%. In its application to the analysis of several aquatic products recoveries in the range of 95. 5%-102, 3% were obtained.

关 键 词：气相色谱 微波辅助提取 甲基汞 

分 类 号：O657.8[理学—分析化学]