梯度洗脱LC-ICP/MS法测定5种硒形态
Determination of 5 Selenium Species by Gradient Elution LC-ICP/MS
陈思伊 1唐琼 1黄丽 1施向东 1范云燕1
作者信息
- 1. 南宁市疾病预防控制中心,广西南宁 530023
- 折叠
摘要
建立一种梯度洗脱液相色谱-电感耦合等离子体质谱法(Liquid Chromatography-Inductively Coupled Plasma-Mass Spectrometry,LC-ICP/MS)分析硒代胱氨酸、甲基硒代半胱氨酸、亚硒酸根、硒代蛋氨酸、硒酸根5种硒形态.样品通过Hamilton PRP-X100阴离子色谱柱,分别以流动相A 40 mmol·L-1 磷酸氢二铵+5 mmol·L-1 柠檬酸(pH=4.6)和流动相B 60 mmol·L-1 磷酸氢二铵+5 mmol·L-1 柠檬酸(pH=4.6)梯度洗脱5 种硒形态,流速为 1.0 mL·min-1,切换时间分别为 3.0 min和 6.4 min,ICP/MS检测,外标法定量.5 种硒形态在8.5 min内检测完毕;0.5～200.0 μg·L-1 相关系数r＞0.999,最低检测质量浓度为0.10～0.39 μg·L-1.相较于《生活饮用水标准检验方法 第 6 部分:金属和类金属指标》(GB/T 5750.6-2023)硒形态分析法,该方法将分析时间缩短了 46.8%,5种形态峰分离度更好、灵敏度更高.
Abstract
A gradient elution liquid chromatography coupled with inductively coupled plasma-mass spectrometry(ICP/MS)method was established for determination of SeCys2,MeSeCys,Se(Ⅳ),SeMet and Se(Ⅵ).5 selenium species samples were separated using a Hamilton PRP-X100 anion exchange column,with mobile phase A 40 mmol·L-1(NH4)2HPO4+5 mmol·L-1 C6H8O7·H2O(pH=4.6)and mobile phase B 60 mmol·L-1(NH4)2HPO4+5 mmol·L-1 C6H8O7·H2O(pH=4.6)at flow rate of 1.0 mL·min-1,and the mobile phase switching times were 3.0 min and 6.4 min,respectively,they were determined by ICP/MS and quantified with external standard calibration method.5 selenium species were detected within 8.5 min.In the concentration range of 0.5～200.0 μg·L-1,the correlation coefficients(r)of the 5 selenium species were greater than 0.999.The limits of detection of the method were 0.10～0.39 μg·L-1.Compared with the method in GB/T 5750.6-2023,the analysis time of this method was shortened by 46.8%,and the resolutions and sensitivities of 5 selenium species were better.
关键词
硒形态/液相色谱-电感耦合等离子体质谱法/梯度洗脱Key words
selenium species/liquid chromatography-inductively coupled plasma-mass spectrometry/gradient elution引用本文复制引用
基金项目
广西卫生健康委自筹经费科研课题(Z20200530)
广西卫生健康委自筹经费科研课题(Z20200394)
广西卫生应急技能培训中心开放课题(2022)(HESTCG20225)
南宁市科学研究与技术开发计划(ZC20223240)
出版年
2024
NETL
NSTL
万方数据