液相色谱-氢化物发生原子荧光光谱法测定富硒酵母中硒的形态  

Quantitative Determination of Selenium Species in Se-enriched Yeast Using Liquid Chromatography-Hydride Generation Atomic Fluorescence Spectrometry

作　　者：肖志明[1] 宋荣[1] 贾铮[1] 李阳[1] 樊霞[1] 

机构地区：[1]中国农业科学院农业质量标准与检测技术研究所国家饲料质量监督检验中心(北京),北京100081

出　　处：《分析化学》2014年第9期1314-1319,共6页Chinese Journal of Analytical Chemistry

摘　　要：建立了富硒酵母中硒酸Se（Ⅵ）、亚硒酸Se（Ⅵ）、硒代蛋氨酸（SeMet）和硒甲基硒代半胱氨酸（SeMeCys）4种硒形态的高效液相色谱-氢化物发生原子荧光光谱（HPLC-HG-AFS）分析方法。样品采用蛋白酶和胰蛋白酶酶解提取,20 mmol/L（NH4）2HPO4为流动相,经PRP-X100阴离子交换色谱柱分离后HG-AFS测定。结果显示,4种硒形态标准曲线的线性关系良好（R^2≥0.9995）,方法检出限为0.5~5.0μg/kg,平均回收率为82.5%~101.2%,日内相对标准偏差≤8.6%,日间相对标准偏差≤14.5%。本方法前处理简单、灵敏度高、设备便宜、运行费用低廉,适用于富硒饲料产品中硒的形态分析。A rapid and sensitive method has been developed for the simultaneous determination of four selenium species Se（Ⅵ）, Se（Ⅳ）, selenomethionine, and Se-methylselenocysteine in Se-enriched yeast by liquid chromatography-hydride generation atomic fluorescence spectrometry （HPLC-HG-AFS）. The isolation of the analytes from yeast samples was accomplished by protease ）Ⅻ and trypsin enzymatic digestion. The target compounds were separated on a PRP-X100 anion exchange column and analyzed by HG-AFS. The mobile phase was 20 mmol/L （NH4 ）2HPO4. Good linearity was obtained for all the selenium species, with linear correlation coefficients higher than 0. 9996. The LODs of the four species were between 0.5 and 5.0 μg/kg. Average recoveries for the four analytes were in the ranges of 82.5% -101.2%, with intra- and inter-day RSD lower than 8.6% and 14.5, respectively. The proposed analytical method is simple, sensitive, with low operation cost, making it applicable for the determination of the selenium species in Se-enriched feeds.

关 键 词：液相色谱 氢化物发生原子荧光光谱 富硒酵母 硒形态 

分 类 号：S816.17[农业科学—饲料科学] O657[农业科学—畜牧学]