离子色谱-电感耦合等离子体质谱法测定奶粉中的硒形态  

Determination of Selenium Species in Milk Powder by IC-ICP-MS

作　　者：林立[1,2] 孙海波[2] 孙继红[1] 

机构地区：[1]北京工业大学,北京100022 [2]国家食品质量安全监督检验中心,北京100094

出　　处：《理化检验（化学分册）》2015年第9期1227-1231,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：国家质检总局科技计划项目(2012QK013)

摘　　要：采用离子色谱-电感耦合等离子体质谱法测定奶粉中的硒形态。奶粉样品经乙酸沉淀蛋白,流动相提取。选用Hamilton PRP X-100阴离子柱（250mm×4.6mm,5μm）,以5mmol·L^-1柠檬酸、10mmol·L^-1乙酸铵和0.1%（体积分数）三氟乙酸为流动相（pH 5.2）,8min内实现了硒酸盐[Se（Ⅵ）]、亚硒酸盐[Se（Ⅳ）]、硒代蛋氨酸（SeMet）和硒代胱氨酸[（SeCys）2]等4种硒形态的基线分离。方法的检出限在0.03~0.10μg·L^-1之间。加标回收率在25.0%~105%之间,测定值的相对标准偏差（n=6）在1.8%~7.8%之间。IC combined with ICP-MS was applied to the determination of selenium species in milk powder.The milk powder sample was precipitated with acetic acid and extracted with mobile phase.The Hamilton PRP X-100 anion column（250mm×4.6 mm,5μm）along with 5 mmol·L^-1 citric acid,10 mmol·L^-1 ammonium acetate and 0.1%（φ）trifluoro acetic acid as mobile phase（pH 5.2）was used for separation.The 4selenium species,i.e.selenate[Se（Ⅵ）],selenite[Se（Ⅳ）],selenomethionine（SeMet）and selenocystine[（SeCys）2]were completely separated within 8min.The detection limits of the method found ranged from 0.03,0.10μg·L^-1.Recovery rates measured by standard addition method were in the range of 25.0%-105%,with RSD（n=6）in the range of 1.8%-7.8%.

关 键 词：离子色谱 电感耦合等离子体质谱法 奶粉 硒 

分 类 号：O657.63[理学—分析化学]