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投稿时间:2018-04-07
投稿时间:2018-04-07
中文摘要: 建立高效液相色谱-电感耦合等离子体质谱联用(high performance liquid chromatography-inductively coupled plasma mass spectrometry,HPLC-ICP-MS)检测富硒小麦中4种硒形态分析方法。使用微波辅助酶萃取富硒小麦中亚硒酸盐(SeIV)、硒酸盐(SeVI)、硒代蛋氨酸(SeMet)和硒代胱氨酸(SeCys2),采用 Hamilton PRP X-100色谱柱,以6 mmol/L柠檬酸为流动相,pH=5.0,在9 min内可完全分离4种硒形态。SeCys2、SeIV、SeMet、SeVI的检出限分别为0.23、0.15、0.30、0.16 μg/L,线性相关系数(r2)均大于 0.999。以富硒小麦为基体进行加标回收试验,SeCys2、SeIV、SeMet、SeVI的回收率在93.7%~105.2%之间,相对标准偏差为2.2%~6.6%(n=6)。方法简单快速,具有良好的精密度和准确度,适用于富硒小麦中硒形态分析。
中文关键词: 微波辅助萃取 高效液相色谱 电感耦合等离子体质谱 富硒小麦 硒形态
Abstract:An analytical method for determination of four selenium species in selenium-enriched wheat by high performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICP-MS)was established.Selenite(SeIV),selenate(SeVI),selenomethionine(SeMet)and selenocystine(SeCys2)were quantitatively extracted with Protease XIV in a microwave field.The results showed that four selenium species could be separated within 9 min by using a Hamilton PRP X-100 reversed-phase anion exchange column with 6 mmol/L citric acid as mobile phase under pH 5.0.The detection limits of SeCys2,SeIV,SeMet,SeVI were 0.23,0.15,0.30,0.16 μg/L with correlation coefficient(r2)of more than 0.999,the recoveries were in the range of 93.7%-105.2%,and the relative standard deviations(RSD)were 2.2%-6.6%(n=6).The proposed method has some advantages including good accuracy,high precision,fast and simple operation,which can meet the requirements for analyzing of selenium species in selenium-enriched wheat.
keywords: microwave-assisted extraction high performance liquid chromatography inductively coupled plasma mass spectrometry selenium-enriched wheat selenium species
文章编号:201902026 中图分类号: 文献标志码:
基金项目:河北省地质矿产勘查开发局科技项目(201827)
Author Name | Affiliation |
QIN Chong,SHI Chang,WAN Qiu-yue,WANG Lei,LIU Ai-qin,AN Cai-xiu | Hebei Research Center for Geoanalysis,Baoding 071051,Hebei,China |
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