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盐酸提取-液相色谱-原子荧光联用技术检测水产品中甲基汞等汞化合物
引用本文:吕超,刘丽萍,董慧茹,李筱薇. 盐酸提取-液相色谱-原子荧光联用技术检测水产品中甲基汞等汞化合物[J]. 分析试验室, 2010, 29(2)
作者姓名:吕超  刘丽萍  董慧茹  李筱薇
作者单位:1. 北京化工大学,北京,100029;北京市疾病预防控制中心,北京,100013
2. 北京市疾病预防控制中心,北京,100013
3. 北京化工大学,北京,100029
4. 中国疾病预防控制中心营养与食品安全所,北京,100050
基金项目:北京市优秀人才培养(20051D0302640)项目资助
摘    要:建立了HCl提取,高效液相色谱与原子荧光联用技术测定水产中无机汞、甲基汞、乙基汞形态的分析方法。对前处理方法和液相色谱的最佳参数进行优化,实验表明,3种汞化合物的线性范围为0~100μg/L,相关系数(r)均优于0.9990,检出限在0.3~0.6μg/L之间,汞化合物各形态的RSD均小于5%,加标回收率在78.8%~116.8%之间,标准物质(GBW10029),(GBW09101B)中汞形态的测定值均在标准值范围内,参加甲基汞FAPAS国际比对,测定结果的Z比分数为1.0,故本方法适用于水产品中汞化合物形态的分析测定。

关 键 词:盐酸提取  液相色谱-原子荧光联用技术    形态分析  水产品  

Hydrochloric acid extract-mercury speciation analysis by high performance liquid chromatography coupled atomic fluorescence spectrometry
Lv Chao,LIU Li-ping,DONG Hui-ru,LI Xiao-wei. Hydrochloric acid extract-mercury speciation analysis by high performance liquid chromatography coupled atomic fluorescence spectrometry[J]. Chinese Journal of Analysis Laboratory, 2010, 29(2)
Authors:Lv Chao  LIU Li-ping  DONG Hui-ru  LI Xiao-wei
Affiliation:Beijing University of Chemical Technology;Beijing 100029;2.Beijing Center for Disease Prevention and Control;Beijing 100013;3.Institute for Nutrition and Food Safety;Chinese Center for Disease Control and Prevention;Beijing 100050
Abstract:Hydrochloric acid extract, interface technique coupled high performance liquid chromatography with atomic fluorescence spectrometry for methyl-, ethyl- and inorganic mercury analysis is established in this article. Pre-treatment and liquid chromatography methods were optimized in order to obtain the best conditions. The experimental results show that the linear range for three mercury species are all between 0 and 100 μg/L, the linear coefficient (r) are all more than 0.9990, the detection limits are between 0.3~0.6 (μg/L). The relative standard deviations (RSD) for the determination of three species are all less than 5%. The recoveries are all between 78.8%~116.8%, and the determination of mercury speciation of fish reference material (GBW10029) and human hair reference material (GBW09101B) are all in the scope of standard values. Compared to the international standard value of methylmercury FAPAS, the result of the Z score is 1.0. The proposed method has been applied to the determination of mercury speciation in aquatic product.
Keywords:Hydrochloric acid extract  Liquid chromatography-atomic fluorescence spectrometry technique  Mercury  Speciation analysis  Aquatic product  
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