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

刘源; 陈绍占; 陈镇; 姚晓慧; 周天慧; 刘丽萍

doi:doi：10.3969/j.issn.1004-4957.2020.02.017

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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

更新时间：2023-05-25

- 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
- 分析测试学报 2020年39卷第2期页码：273-277
- 作者机构：
  
  1. 首都医科大学公共卫生学院
  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
  3. 北京市预防医学研究中心
- 作者简介：
- 基金信息：
- DOI：doi：10.3969/j.issn.1004-4957.2020.02.017
  中图分类号：
- 纸质出版：2020
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刘源, 陈绍占, 陈镇, 姚晓慧, 周天慧, 刘丽萍. 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[J]. 分析测试学报, 2020,39(2):273-277.

刘源, 陈绍占, 陈镇, 姚晓慧, 周天慧, 刘丽萍. Determination of Selenium Speciations in Human Urine by High Performance Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry[J]. 2020, 39(2): 273-277.
刘源, 陈绍占, 陈镇, 姚晓慧, 周天慧, 刘丽萍. 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[J]. 分析测试学报, 2020,39(2):273-277. DOI： doi：10.3969/j.issn.1004-4957.2020.02.017.

刘源, 陈绍占, 陈镇, 姚晓慧, 周天慧, 刘丽萍. Determination of Selenium Speciations in Human Urine by High Performance Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry[J]. 2020, 39(2): 273-277. DOI： doi：10.3969/j.issn.1004-4957.2020.02.017.

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(SeCys2)、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，10 μm)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0~300.0 μg/L，相关系数(r)均大于0.999，检出限为0.2~0.5 μg/L。除SeCys2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SeCys2为主，同时含有少量MeSeCys、SeMet、无机硒及未知含硒化合物。

Abstract

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(SeCys2)

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，10 μm) 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 0-300.0 μg/L with correlation coefficients(r) larger than 0.999.The detection limits of the method were 0.2-0.5 μg/L.Recoveries for MeSeCys

Se(Ⅳ)

SeMet and Se(Ⅵ) were in the range of 80.0%-123%

except that the recovery for SeCys2 was 37.7%-70.4%.The relative standard deviations(RSD) were not more than 7.8%.Results showed that SeCys2 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.

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