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梯度洗脱LC-ICP/MS法测定5种硒形态

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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.
Determination of 5 Selenium Species by Gradient Elution LC-ICP/MS
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.

selenium speciesliquid chromatography-inductively coupled plasma-mass spectrometrygradient elution

陈思伊、唐琼、黄丽、施向东、范云燕

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南宁市疾病预防控制中心,广西南宁 530023

硒形态 液相色谱-电感耦合等离子体质谱法 梯度洗脱

广西卫生健康委自筹经费科研课题广西卫生健康委自筹经费科研课题广西卫生应急技能培训中心开放课题(2022)南宁市科学研究与技术开发计划

Z20200530Z20200394HESTCG20225ZC20223240

2024

食品安全导刊
商业科技质量中心 北京肉类食品协会

食品安全导刊

影响因子:0.065
ISSN:1674-0270
年,卷(期):2024.(13)
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