高效液相色谱-原子荧光光谱联用技术测定富硒鸡蛋中的硒形态  

Determination of Selenium Species in Se-enriched Eggs by High Performance Liquid Chromatography-Atomic Fluorescence Spectrometry

作　　者：周晓华 王铁良[1,2] 魏亮亮 钟红舰[1] 魏红[1,2] 张迪[1] 刘进玺 郭洁[1,2] 吴绪金[1] 段然 ZHOU Xiaohua;WANG Tieliang;WEI Liangliang;ZHONG Hongjian;WEI Hong;ZHANG Di;LIU Jinxi;GUO Jie;WU Xujin;DUAN Ran(Institute of Agricultural Product Quality and Safety,Henan Academy of Agricultural Sciences,Zhengzhou,Henan 450002,China;Laboratory of Quality&Safety Risk Assessment for Agro-products(Zhengzhou),Ministry of Agriculture,Zhengzhou,Henan 450002,China)

机构地区：[1]河南省农业科学院农产品质量安全研究所,郑州450002 [2]农业农村部农产品质量安全风险评估实验室(郑州),郑州450002

出　　处：《中国无机分析化学》2023年第12期1451-1458,共8页Chinese Journal of Inorganic Analytical Chemistry

基　　金：河南省科技攻关项目(232102110165);中原科技创新领军人才项目(234200510012);河南省农业科学院自主创新基金资助项目(2023ZC074,2023ZC129)。

摘　　要：为监测市场上富硒鸡蛋中蛋清及蛋黄中硒形态的种类及分布规律,优化建立了一种高效液相色谱-氢化物发生-原子荧光光谱联用技术测定富硒鸡蛋蛋清及蛋黄粉中硒形态的方法。随机选取富硒鸡蛋样品,进行蛋清蛋黄分离、冷冻干燥及蛋黄脱脂处理,处理后样品经Tris-HCl缓冲液(5 mmol/L,pH=7.5) 55℃恒温振荡、酶解提取,高速离心机(10 000 r/min)离心10 min,上清液过0.22μm有机滤膜后采用高效液相色谱-氢化物发生-原子荧光光谱联用技术进行测定,外标法定量。结果表明,能在11 min内实现5种硒形态的基线分离,且各种硒形态的线性相关系数(r)均大于0.999 4,其检出限在0.5~3.0μg/L,回收率在81.6%~110%,可以满足检测需求,按照实验方法测定市场上富硒鸡蛋中的硒形态,方法灵敏度高、准确性好,且测得的富硒鸡蛋蛋清样品中硒形态主要成分为硒代蛋氨酸,而蛋黄样品主要成分为硒代半胱氨酸,还有少量的硒代蛋氨酸,同时,一些鸡蛋还含有极少量的亚硒酸根,但蛋清及蛋黄中硒代氨基酸的含量总和占总硒含量的83.3%~98.4%,适用于富硒鸡蛋中的硒形态提取。由此可见,市场上富硒鸡蛋中的硒主要以硒代氨基酸的形式存在,比较适合日常补硒,建立的方法可以对市场上富硒食品起到一定监测作用。In order to monitor the types and distribution of selenium species in egg whites and egg yolks of selenium-rich eggs in the market,a method for determination of selenium species in egg whites and egg yolk powder of selenium-rich eggs by high performance liquid chromatogram-hydride generation-atomic fluorescence spectrometry was optimized and established.Se-rich egg samples were randomly selected for egg white and yolk separation,freeze-drying and yolk degreasing treatment,and then,the samples were extracted by Tris-HCl buffer solution(5 mmol/L,pH=7.5)at 55℃under constant temperature oscillation and enzymatic hydrolysis,and centrifuged by high-speed centrifuge(10000 r/min)for 10 min.After passing through 0.22μm organic filter membrane,the supernatant was determined by high performance liquid chromatography,hydride generation and atomic fluorescence spectrometry,and quantified by external standard method.The results showed that the method achieved baseline separation of five selenium species within 11 minutes,the linear correlation coefficients(r)of all selenium forms were greater than 0.9994,the detection limits were between 0.5—3.0μg/L,and the recoveries were between 81.6%and 110%,which could meet the detection requirements.The selenium species in selenium-rich eggs on the market was determined by this method with high sensitivity and accuracy.The main component of selenium form in the egg white sample of selenium-rich eggs was selenomethionine,while the main component of the egg yolk sample was selenocysteine and a small amount of selenomethionine.At the same time,some eggs also contained a very small amount of selenite.However,seleno-amino acids in egg white and egg yolk accounted for 83.3%—98.4%of the total selenium content,which was suitable for the extraction of selenium form in selenium-rich eggs.It can be seen that selenium in selenium-rich eggs on the market mainly exists in the form of seleno-amino acids,which is suitable for daily selenium supplementation,and this method can play a certain role

关 键 词：高效液相色谱-原子荧光光谱联用技术 富硒鸡蛋 硒形态 硒代氨基酸 分布规律 

分 类 号：O657.31[理学—分析化学]