高效液相色谱-电感耦合等离子体质谱法测定人尿中硒形态  

Determination of Selenium Speciations in Human Urine by High Performance Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry

作　　者：刘源 陈绍占 陈镇 姚晓慧 周天慧[2,3] 刘丽萍 LIU Yuan;CHEN Shao-zhan;CHEN Zhen;YAO Xiao-hui;ZHOU Tian-hui;LIU Li-ping(School of Public Health,Capital Medical University,Beijing 100069,China;Beijing Key Laboratory of Diagnostic and Traceability Technologies for Food Poisoning,Beijing Center for Disease Prevention and Control,Beijing 100013,China;Center for Preventive Medicine Research,Beijing 100013,China)

机构地区：[1]首都医科大学公共卫生学院,北京100069 [2]北京市疾病预防控制中心食物中毒诊断溯源技术北京市重点实验室,北京100013 [3]北京市预防医学研究中心,北京100013

出　　处：《分析测试学报》2020年第2期273-277,共5页Journal of Instrumental Analysis

基　　金：上海市科技创新行动计划(17142202600)。

摘　　要：采用高效液相色谱-电感耦合等离子体质谱法(HPLC-ICP/MS)测定人尿中硒代胱氨酸(SeCys 2)、甲基硒代半胱氨酸(MeSeCys)、亚硒酸盐[Se(Ⅳ)]、硒代蛋氨酸(SeMet)、硒酸盐[Se(Ⅵ)]5种硒形态。样品经超纯水稀释后,采用Hamilton PRP-X100色谱柱(250 mm×4 mm,10μm)分离,以40 mmol/L磷酸氢二铵(含1%甲醇,pH 5)为流动相进行等度洗脱,13 min内可将5种硒形态分离。5种硒形态的线性范围为0~300.0μg/L,相关系数(r)均大于0.999,检出限为0.2~0.5μg/L。除SeCys 2的加标回收率为37.7%~70.4%外,MeSeCys、Se(Ⅳ)、SeMet、Se(Ⅵ)的加标回收率为80.0%~123%;5种硒形态的相对标准偏差(RSD)均不大于7.8%。应用该方法测定实际样品,结果显示人尿中硒形态主要以SeCys 2为主,同时含有少量MeSeCys、SeMet、无机硒及未知含硒化合物。A high performance liquid chromatography-inductively coupled plasma mass spectrometry(HPLC-ICP/MS)was developed for the determination of five speciations of selenium,i.e.selenocystine(SeCys 2),methylselenocysteine(MeSeCys),selenite[Se(Ⅳ)],selenomethionine(SeMet)and selenate[Se(Ⅵ)]in human urine.The samples were diluted with ultra-pure water,and separated on a Hamilton PRP-X100 column(250 mm×4 mm,10μm)by isocratic elution using 40 mmol/L diammonium hydrogen phosphate containing 1%methanol(pH 5)as mobile phase.Five selenium speciations could be separated within 13 min.There were linear relationships for five selenium speciations in the range of 0-300.0μg/L with correlation coefficients(r)larger than 0.999.The detection limits of the method were 0.2-0.5μg/L.Recoveries for MeSeCys,Se(Ⅳ),SeMet and Se(Ⅵ)were in the range of 80.0%-123%,except that the recovery for SeCys 2 was 37.7%-70.4%.The relative standard deviations(RSD)were not more than 7.8%.Results showed that SeCys 2 was the main selenium speciation in human urine,and a small amount of MeSeCys,SeMet,inorganic selenium and some unknown selenium compounds were also found.

关 键 词：人尿 硒形态 高效液相色谱-电感耦合等离子体质谱法 

分 类 号：O657.63[理学—分析化学] Q581[理学—化学]