血液与尿液中铅形态化合物的HPLC-ICP-MS分析  

Analysis of Lead Compounds in Blood and Urine by HPLC-ICP-MS

作　　者：吴书凡 骆如欣 张素静 马安德 马栋 WU Shu-fan;LUO Ru-xin;ZHANG Su-jing;MA An-de;MA Dong(School of Public Health,Southern Medical University,Guangzhou 510515,China;Shanghai Forensic Service Platform,Shanghai Key Laboratory of Forensic Medicine,Academy of Forensic Science,Shanghai 200063,China)

机构地区：[1]南方医科大学公共卫生学院,广东广州510515 [2]司法鉴定科学研究院上海市法医学重点实验室上海市司法鉴定专业技术服务平台,上海200063

出　　处：《分析测试学报》2020年第6期800-803,共4页Journal of Instrumental Analysis

基　　金：国家自然科学基金面上项目(81671868);上海市法医学重点实验室资助项目(17DZ2273200);国家重点专项研究项目(2016YFC0503607);国家重点专项研究项目(2016YFC0800704);上海市司法鉴定专业技术服务平台资助项目(16DZ2290900)。

摘　　要：建立了血液和尿液中2种铅形态化合物(三甲基铅、三乙基铅)的高效液相色谱-电感耦合等离子体质谱(HPLC-ICP-MS)分析方法。利用苯溶液萃取铅形态化合物,超声离心后以硫代硫酸钠溶液进行反萃取。以0.1 mol/L乙酸铵-0.1 mol/L乙酸与甲醇为流动相进行等度洗脱,Agilent Zorbax Plus C18(4.6 mm×100 mm,3.5μm)对提取物进行分离,ICP-MS分析样品中铅形态化合物。结果表明,血液和尿液中2种铅形态化合物的线性范围分别为3~200 ng/mL和5~400 ng/mL,检出限为0.85~1.31 ng/mL,定量下限为3.00~5.00 ng/mL,日内及日间相对标准偏差(RSD)为1.8%~10%,提取回收率为85.3%~104%,基质效应为88.3%~117%。该方法样品前处理简单,检出限低,准确度高,适用于人体血液和尿液中三甲基铅、三乙基铅的测定。A high-performance liquid chromatography-inductively coupled plasma-mass spectrometric(HPLC-ICP-MS) method was established for the detection of two lead compounds,i.e.trimethyllead and triethyllead in blood and urine.The samples were extracted with benzene as solvent,followed by baci-extraction with sodium thiosulfate after sonication and centrifugation.The extracts were separated by HPLC using an Agilent Zorbax Plus C18 column(4.6 mm×100 mm,3.5 μm),with 0.1 mol/L ammonium acetate-0.1 mol/L acetic acid and methanol as mobile phases by isocratic elution,and then detected by ICP-MS.Results showed that there were good linear relationships for two lead compounds in blood and urine samples in the ranges of 3-200 ng/mL and 5-400 ng/mL,with their limits of detection and limits of quantitation of 0.85-1.31 ng/mL and 3.00-5.00 ng/mL,respectively.The recoveries ranged from 85.3% to 104% with intra-day and inter-day relative standard deviations(RSD) of 1.8%-10%,and the matrix effects of 88.3%-117%.The developed method was simple,sensitive and accurate,and it was suitable for the determination of trimethyllead and triethyllead in human blood and urine.

关 键 词：高效液相色谱-电感耦合等离子体质谱(HPLC-ICP-MS) 三甲基铅 三乙基铅 血液 尿液 

分 类 号：O657.63[理学—分析化学] S859.81[理学—化学]