高效液相色谱-氢化物发生-原子荧光光谱联用技术测定高脂作物中的硒形态

Determination of Selenium Species in Se-Enriched High-Fat Crops by High Performance Liquid Chromatography-Hydride Generation-Atomic Fluorescence Spectrometry

优化建立一种富硒高脂作物中硒形态的提取方法,进一步了解市场上芝麻、花生、核桃等富硒高脂作物中存在的硒形态。高脂样品需先进行脱脂处理,称取一定量脱脂后样品加入一定量的三(羟甲基)氨基甲烷缓冲液,超声酶提取,离心,过膜,最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,5种硒形态标液保留时间定性,外标法定量,以此确定市场上高脂样品中硒的赋存形态及含量。该方法能在10 min内实现5种硒形态的基线分离,且线性良好,各种硒形态的线性相关系数(r)均不小于0.9992,其检出限在1.0~3.0μg/L之间,回收率在89.8%~100.6%之间。利用该方法测定了市售的富硒芝麻、花生、核桃等高脂作物中的硒形态,结果发现高脂作物中的硒赋存形态为硒代蛋氨酸,且含量占总硒含量的88.0%~96.9%,该方法简单、快速,适用于富硒高脂作物中的硒形态提取。

An optimized extraction method for selenium form in selenium-rich high-fat crops was established to understand the selenium forms in sesame,peanut,walnut and other selenium-rich high-fat crops in the market.After defatted,the sample was added with a certain amount of Tris-HCl buffer solution,centrifuged after ultrasound,and then passed through the film.The samples were determined by high performance liquid chromatography-hydride generation-atomic fluorescence spectrometry,and quantified by external standard method.The method could achieve baseline separation of five selenium forms within 10 min with good linearity.The linear correlation coefficients(r)of all selenium forms were greater than 0.9992.The detection limits were between 1.0 and 3.0μg/L,and the recoveries were ranged from 89.8%to 100.6%.The selenium forms in high fat crops,such as sesame,peanut and walnut,were determined by this method.The results indicated that the selenium forms in high fat crops were selenomethionine,and the content of selenomethionine accounted for 88.0%~96.9%of the total selenium content.This method is simple,rapid and suitable for the extraction of selenium forms in high fat crops.