摘要
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)测定大米粉中硒代胱氨酸(SeCys2)、甲基-硒代半胱氨酸(MeSeCys)、亚硒酸根(Se(Ⅳ))、硒代蛋氨酸(SeMet)、硒酸根(Se(Ⅵ))等5种硒形态的分析方法.采用Hamilton PRP-X100分析柱,以pH 4和pH 6的20 mmol·L-1的柠檬酸溶液辅以少量甲醇为流动相,在梯度洗脱条件下,9 min内可实现5种硒形态完全分离.SeCys2、MeSeCys、Se(Ⅳ)、SeMet、Se(Ⅵ)的检出限分别为0.88、0.69、1.00、0.90、0.82μg·L-1.利用富硒小麦粉标准物质RM8436探讨了不同提取方式的提取效果.最终确定75 mmol·L-1 Tris-HCl(pH 7.5)添加XIV蛋白酶和Driselase酶作为提取剂,在37℃振荡提取3 h为大米样品前处理方法.利用该方法分析了富硒地区大米粉中的硒形态,结果表明,大米粉中的硒主要以有机硒形态为主,其中SeMet是最主要的硒形态,占总硒的90%左右.
An analytical method for the determination of five selenium species in rice flour samples was developed using high performance liquid chromatography combined with inductively coupled plasma mass spectrometry(HPLC-ICP-MS).Seleno-Cystine(SeCys2),(Methyl)Seleno-Cysteine(MeSeCys),Selenite(Se(Ⅳ)),Selenoate(Se(Ⅵ))and Selenomethionine(SeMet)were completely separated on a Hamilton PRP-X100 anion exchange column using 20 mmol·L-1 citric acid solution(pH 4.0),20 mmol·L-1 citric acid solution(pH 6.0)and methyl alcohol as the mobile phase under gradient elution within 9 minutes.The detection limits of SeCys2,MeSeCys,Se(Ⅳ),SeMet and Se(Ⅵ)were 0.88,0.69,1.00,0.90,0.82μg·L-1,respectively.75 mmol·L-1 Tris-HCl(pH 7.5)with XIV protease and Driselase was eventually selected as extractant.Different sample preparation methods had been compared and oscillation method with 3 h at 37℃was chosen finally.This method was applied to measure selenium species in rice flour samples from selenium-enriched areas.The results indicated that SeMet was the main species in rice flour,accounting for about 90%of the total amount of selenium.
作者
邵鹏威
路国慧
郑宇
胡俊栋
赵全升
杨永亮
刘崴
SHAO Pengwei;LU Guohui;ZHENG Yu;HU Jundong;ZHAO Quansheng;YANG Yongliang;LIU Wei(College of Environmental Sciences and Engineering,Qingdao University,Qingdao,266071,China;National Research Center for Geo-Analysis(NRCGA),Beijing,100037,China)
出处
《环境化学》
CAS
CSCD
北大核心
2020年第5期1434-1441,共8页
Environmental Chemistry
基金
中国地质科学院基本科研业务费项目(YYWF201620)
中国地质大调查项目(DD20190589)资助
关键词
硒
形态分析
大米粉
高效液相色谱-电感耦合等离子体质谱
selenium
speciation analysis
rice flour
high performance liquid chromatography-inductively coupled plasma mass spectrometry(HPLC-ICP-MS)
