高效液相色谱-电感耦合等离子体质谱(HPLC-ICP-MS)联用测定富硒小麦中硒代氨基酸  

Determination of Seleno-amino Acids in Selenium-rich Wheat by HPLC-ICP-MS

作　　者：卢鑫[1] 张琳[1] 王铁良 成东梅 周晓华 LU Xin;ZHANG Lin;WANG Tieliang;CHENG Dongmei;ZHOU Xiaohua(Jiyuan Vocational and Technical College,Jiyuan,Henan 459000,China;Institute of Agricultural Quality Standards and Testing Technology,Henan Academy of Agricultural Sciences,Zhengzhou,Henan 450023,China;Jiyuan Academy of Agricultural Sciences,Jiyuan,Henan 459000,China)

机构地区：[1]济源职业技术学院,河南济源459000 [2]河南省农业科学院农业质量标准与检测技术研究所,郑州450023 [3]济源市农业科学院,河南济源459000

出　　处：《中国无机分析化学》2023年第12期1466-1472,共7页Chinese Journal of Inorganic Analytical Chemistry

基　　金：河南省高等学校重点科研计划项目(21B150014);河南省农科院“四优四化”科技支撑行动计划项目(SYSH20200107007)。

摘　　要：为科学补硒和促进富硒小麦的种植推广,用蛋白酶XIV辅助微波振荡提取富硒小麦中硒代氨基酸,采用C18分离柱分离,以磷酸氢二铵(30.0 mmol/L)+甲醇(1.0%)+四丁基溴化铵溶液(2.0 mmol/L,pH=6.5)为流动相,能在10 min内实现5种硒代氨基酸的分离。在高能氦气模式(HEHe)下,用^(78)Se的色谱峰面积积分作为定量依据,建立了高效液相色谱-电感耦合等离子体质谱联用技术(HPLC-ICP-MS)检测富硒小麦中硒代氨基酸的方法。5种硒代氨基酸在1.0~200.0μg/L线性相关性良好,检出限在0.11~0.29μg/L。以富硒小麦为基体进行加标回收,除硒代胱氨酸(SeCys_(2))可能不稳定,易分解造成回收率偏低外,其他4种硒代氨基酸的加标回收率在92.3%~102%,相对标准偏差为1.6%~4.2%(n=7)。用所建立的方法测定农业科技工作者种植推广的富硒小麦,结果发现小麦中的硒赋存形态多为硒代蛋氨酸(SeMet),此外,小麦中还含有少量硒代胱氨酸(SeCys_(2))、硒代半胱氨酸(SeCys)、甲基硒代半胱氨酸(MeSeCys)和硒代乙硫氨酸(SeEt)。方法具有良好的精密度和准确度,适用于富硒小麦中硒代氨基酸的形态分析。In order to supplement selenium scientifically and promote the planting and popularization of Se-enriched wheat,the selenoamino acids were extracted from selenium-rich wheat by microwave ultrasonic protease,and separated by C18 column,using murl diammonium hydrogen phosphate(30.0 mmol/L),methanol(1.0%),and tetrabutylammonium bromide(2.0 mmol/L,pH=6.5)as mobile phase.Five selenoamino acids could be separated in 10 min.In the high energy helium mode(HEHe),using the chromatographic peak integral area of 78 Se as the quantitative basis,a method for the rapid determination of seleno-amino acids in selenium-rich wheat by high performance liquid chromatography-inductively coupled plasma mass spectrometry(HPLC-ICP-MS)was established.The linear correlation of the five selenoamino acids was in the range of 1.0—200.0μg/L,and the detection limit was 0.11—0.29μg/L.The recovery test with selenium-rich wheat as matrix showed that except that SeCys_(2) may be unstable and easy to decompose,the recovery rate of the other four selenoamino acids was between 92.34%and 102.46%,and the relative standard deviation was 1.6%—4.2%(n=7).This method was used to determine the selenium-rich wheat planted and popularized by agricultural scientists and technicians.The results showed that most of the selenium in wheat was selenomethionine.In addition,wheat also contained a small amount of selenocysteine,selenocysteine and methyl selenocysteine.The method is simple,rapid,precise and accurate,which is suitable for the speciation analysis of selenoamino acids in selenium-rich wheat.

关 键 词：高效液相-电感耦合等离子体质谱(HPLC-ICP-MS) 微波振荡提取 富硒小麦 硒代氨基酸 

分 类 号：O657.63[理学—分析化学]