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

作　　者：陈思伊 唐琼[1] 黄丽[1] 施向东[1] 范云燕[1] CHEN Siyi;TANG Qiong;HUANG Li;SHI Xiangdong;FAN Yunyan(Nanning Center for Disease Control and Prevention,Nanning 530023,China)

机构地区：[1]南宁市疾病预防控制中心,广西南宁530023

出　　处：《食品安全导刊》2024年第13期100-103,共4页China Food Safety Magazine

基　　金：广西壮族自治区卫生健康委员会自筹经费科研课题(Z20200530,Z20200394);广西卫生应急技能培训中心2022年度开放课题项目(HESTCG20225);南宁市科学研究与技术开发计划项目(ZC20223240)。

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;0.5~200.0μg·L^(-1)相关系数r>0.999,最低检测质量浓度为0.10~0.39μg·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。A gradient elution liquid chromatography coupled with inductively coupled plasma-mass spectrometry(ICP/MS)method was established for determination of SeCys_(2),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)(NH_(4))_(2)HPO_(4)+5 mmol·L^(-1)C_(6)H_(8)O_(7)·H_(2)O(pH=4.6)and mobile phase B 60 mmol·L^(-1)(NH4)2HPO_(4)+5 mmol·L^(-1)C_(6)H_(8)O_(7)·H_(2)O(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 0.5~200.0μg·L^(-1),the correlation coefficients(r)of the 5 selenium species were greater than 0.999.The limits of detection of the method were 0.10~0.39μg·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 

分 类 号：O657.63[理学—分析化学] TS207.3[理学—化学]