高效液相色谱-电感耦合等离子体质谱法测定谷类食品中的4种硒形态  

Determination of Selenium Species in Cereals by High Performance Liquid Chromatography-Inductively Coupled Plasma-Mass Spectrometry

作　　者：孟莉 许亚丽 夏曾润 贺博 祁蒙 杜小平 卜贤盼 唐德剑 MENG Li;XU Yali;XIA Zengrun;HE Bo;QI Meng;DU Xiaoping;BU Xianpan;TANG Dejian(Ankang R&D Center for Se-enriched Products,Ankang 725000;Key Laboratory of Se-enriched Products Development and Quality Control,Ministry of Agriculture and Rural Affairs,Ankang 725000)

机构地区：[1]安康市富硒产品研发中心,陕西安康725000 [2]农业农村部富硒产品开发与质量控制重点实验室,陕西安康725000

出　　处：《分析科学学报》2021年第6期843-846,共4页Journal of Analytical Science

基　　金：陕西省创新能力支撑计划(No.2018TD-021)。

摘　　要：本文建立了高效液相色谱-电感耦合等离子体质谱(HPLC-ICP-MS)联用技术测定谷类食品中硒代胱氨酸(SeCys_(2))、亚硒酸根(Se(Ⅳ))、硒代蛋氨酸(SeMet)和硒酸根(Se(Ⅵ)) 4种硒形态的方法。采用Hamilton PRP-X100阴离子交换柱,在流动相为40 mmol/L (NH_(4))_(2)HPO_(4),pH=6.0条件下,16 min内可以完全分离以上4种硒形态。在1~200μg/L范围内,各硒形态线性关系良好,相关系数r均>0.999;SeCys_(2)、Se(Ⅳ)、SeMet、Se(Ⅵ)的方法检出限分别为4.8μg/kg、4.5μg/kg、7.0μg/kg和5.2μg/kg。将该方法应用于谷类食品中硒形态的分析,Se(Ⅳ)、SeMet、Se(Ⅵ)的加标回收率为89.7%~99.3%,且主要形态为SeMet。建立的方法具有操作简单、快速高效、灵敏度高等优点,可满足谷类食品中硒形态定量分析。In this work,selenocystine(SeCys_(2)),selenite(Se(Ⅳ)),selenomethionine(SeMet),and selenate(Se(Ⅵ)) in cereals were determined by high performance liquid chromatography-inductively coupled plasma-mass spectrometry.0.2 g of the pulverized sample was placed in a centrifuge tube,and sonicated for 3 h at 37 ℃ in water bath.After standing for 10 min,the sample solution was then centrifuged for 10 min at 4 ℃ with 9 000 r/min and the supernatant was filtered through a 0.22 μm membrane for testing.The selenium species were separated completely within 16 min by Hamilton PRP-X100 anion exchange column under the condition of mobile phase 40 mmol/L diammonium hydrogen phosphate(pH=6.0).The linear coefficients of four selenium species were above 0.999,and the detection limits of SeCys_(2),Se(Ⅳ),SeMet,Se(Ⅵ) were 4.8,4.5,7.0 and 5.2 μg/kg,respectively.The developed method was applied to the speciation of selenium in cereals,and it was found that the main selenium form in cereals is SeMet.The method has the advantages of convenient operation,rapidity,efficiency and high sensitivity,which can meet the requirements of the quantitative analysis of selenium species in cereals.

关 键 词：高效液相色谱-电感耦合等离子体质谱 谷类食品 硒形态 

分 类 号：O657.63[理学—分析化学]