摘要
目的建立液相色谱-电感耦合等离子质谱法(liquid chromatography-inductively coupled plasma mass spectrometry,LC-ICP-MS)测定谷物类大豆样品中5种硒形态[硒代胱氨酸(SeCys2)、甲基硒代L-半胱氨酸(MeSeCys)、亚硒酸根(SeⅣ)、硒代蛋氨酸(SeMet)和硒酸根(SeVI)]的分析方法。方法样品采用超声水解,加入链酶蛋白酶E提取,经C18反向色谱柱(4.6 mm×150 mm,5μm,100Å)分离,以30 mmol/L磷酸氢二铵、0.5 mmol/L四丁基溴化铵、2%甲醇为流动相,流动相的pH用甲酸调节至5.8~6.0,通过ICP-MS测定5种硒形态。结果经方法优化后,LC-ICP-MS方法可以在8 min内将5种硒形态完全分离,且各个硒形态标准曲线的线性关系良好(r 2≥0.995),方法检出限为0.5~1.0μg/L,定量限为1.5~3.0μg/L,加标回收率为97.34%~100.33%,相对标准偏差为0.46%~1.2%。结论本方法具有前处理简单、快捷,灵敏度高,分析速度快等优点,适用于大豆食品中硒的形态分析。
Objective To establish a method for determination of 5 different forms of selenium[selenium cystine(SeCys2),methyl selenium generation L-cysteine(MeSeCys),and selenium acid radical(SeⅣ),selenomethionine(SeMet)and selenium acid group(SeVI)]in grain soybean samples by liquid chromatography with inductively coupled plasma mass spectrometry(LC-ICP-MS).Methods The samples were hydrolyzed by ultrasound and extracted by adding pronase E,and separated by C18 chromatographic column(4.6 mm×150 mm,5μm,100Å)using 30 mmol/L diammonium phosphate,0.5 mmol/L tetrbutyl ammonium bromide,and 2%methanol as mobile phase.The pH of the mobile phase was adjusted to 5.8~6.0 by formic acid,then 5 selenium forms were determined by ICP-MS.Results After the optimization of the method,5 selenium forms could be separated completely in 8 minutes by LC-ICP-MS,and the linear relationship of the standard curves of selenium forms was good(r^2≥0.995).The limits of detection the method were 0.5–1.0μg/L,the limits of quantitation were 1.5–3.0μg/L,the recovery rates were 97.34%–100.33%,and the relative standard deviations were 0.46%–1.2%.Conclusion This method has the advantages of simple,fast pretreatment,high sensitivity and fast analytical speed,and is suitable for speciation analysis of selenium species in soybean food.
作者
魏琴芳
贾彦博
胡文彬
洪春来
韦燕燕
WEI Qin-Fang;JIA Yan-Bo;HU Wen-Bin;HONG Chun-Lai;WEI Yan-Yan(Hangzhou Institute for Food and Drug Control,Hangzhou 310022,China;Institute of Environment,Resource Soil and Fertilizer,Zhejiang Academy of Agricultural Sciences,Hangzhou 310021,China;College of Agriculture,Guangxi University,Nanning 530004,China)
出处
《食品安全质量检测学报》
CAS
2020年第8期2456-2461,共6页
Journal of Food Safety and Quality
关键词
液相色谱法
电感耦合等离子质谱法
大豆
硒形态
liquid chromatography
inductively coupled plasma mass spectrometry
soybean
selenium species