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
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(250 mm×4.6 mm,5 μm),以5 mmol·L-1柠檬酸、10 mmol·L-1乙酸铵和0.1%(体积分数)三氟乙酸为流动相(pH 5.2),8 min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0.03~0.10 μg·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。
电感耦合等离子体质谱法
奶粉
硒
IC
ICP-MS
Milk powder
Selenium
Abstract
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 (250 mm×4.6 mm, 5 μm) 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 4 selenium species, i.e. selenate ［Se(Ⅵ)］, selenite ［Se(Ⅳ)］, selenomethionine (SeMet) and selenocystine ［(SeCys)2］ were completely separated within 8 min. The detection limits of the method found ranged from 0.03, 0.10 μg·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%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201509004
所属栏目 试验与研究
基金项目 国家质检总局科技计划项目(2012QK013)
收稿日期 2014/8/12
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备注林立(1977-),女,四川宜宾人,高级工程师,博士 研究生,主要从事分析化学的研究。
引用该论文: LIN Li,SUN Hai-bo,SUN Ji-hong. Determination of Selenium Species in Milk Powder by IC-ICP-MS[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2015, 51(9): 1227～1231
林立,孙海波,孙继红. 离子色谱-电感耦合等离子体质谱法测定奶粉中的硒形态[J]. 理化检验－化学分册, 2015, 51(9): 1227～1231
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【3】ANNALISA B, ISABELLA M, LAURA R, et al.Seleniuminteractions with essential and toxic elements in egg yolk from commercial and fortified eggs［J］.J Trace Elem Med Biol, 2008,22:234-241.
【4】STIBILJ V, VADNJAL R, KOVAC M, et al. The effect of dietary arsenic additions on the distribution of selenium and iodine in eggs and tissues of laying hens［J］.Arch Environ Contam Toxicol, 2004,46:275-280.
【5】MICHALKE B, SCHRAME O, KETTRUP A. Capillary electrophoresis coupled to inductively coupled pjasma mass spectrometry (EE/ICP-MS) and to electro speayionization mass spectrometry (CE/ESI-MS): An approach for maximum species information in speciation of selenium［J］ . Fresenius Anal Chem, 1999,363:456-459.
【6】GOMEZ-ARIZA J L, BERNA-LDAZA V, VILLEGAS-PORTERO M J. Comparative study of the instrumental couplings of high performance liquid chromatography with microwave-assisted digestion hydride generation atomic fluorescence spectrometry and inductively coupled plasma mass spectrometry for chiral speciation of selenomethionine in breast and formula milk［J］. Analytica Chimica Acta, 2004,520:229-235.
【7】BENDAHL L, GAMMELGAARD B, JONS O, et al. Interfacing capillary electrophoresis with in-ductively coupled plasma mass spectrometry by direct injection nebulization for selenium specia-tion［J］. J Anal At Spectrom, 2001,16(1):38-42.
【8】赵少华,宇万太,张璐,等.环境介质中硒的检测方法研究进展［J］.干旱环境监测, 2005,19(2):107-110.
【9】方建军,祝华明,方芳,等.富硒大米中硒形态分析［J］.食品研究与开发, 2012,33(9):146-150.
【10】张美琴,季华曼,杨洪生,等.氢化物发生原子荧光光谱法测定水产品中有机硒和无机硒［J］.中国水产科学, 2012,19(5):900-905.
【11】王振华,何滨,史建波,等.液相色谱-双通道原子荧光检测联用法同时测定砷和硒的形态［J］.色谱, 2009,27(5):711-716.
【12】李晶,孔维恒,高峰,等.HPLC-ICP-MS法分析测定富硒保健品中的硒形态［J］.现代仪器, 2012,18(3):37-39.
【13】王丙涛,谢丽琪,林燕奎,等.高效液相色谱-电感耦合等离子体质谱联用检测食品中的五种硒形态［J］.色谱, 2011,29(3):223-227.
【14】喻宏伟,陈春英,高愈希,等.高效液相色谱-电感耦合等离子体质谱法分析生物样品中硒的化学形态［J］.分析化学, 2006,34(6):749-753.
【15】荆淼,余振花,李文龙,等.应用HPLC-ICP-MS技术分析硒的不同形态方法初探［J］.质谱学报, 2006,27(7):46-47.
【16】倪张林,汤富彬,张玮,等.HPLC-DRC-ICP-MS测定富硒蔬菜中的硒形态［J］.分析试验室, 2006,32(2):39-43.
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