同位素稀释/液相色谱-串联质谱测定婴幼儿配方奶粉中脂溶性维生素  

Determination of Fat Vitamins in Infant Formula Milk by Isotope Dilution / High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：赵孔祥[1] 娄婷婷[1] 何佳[1] 陈其勇[1] 葛宝坤[1] 郑文杰[1] 

机构地区：[1]天津出入境检验检疫局,天津300461

出　　处：《分析测试学报》2015年第12期1372-1376,共5页Journal of Instrumental Analysis

基　　金：天津出入境检验检疫局科研资助项目(TK081-2013)

摘　　要：采用液相色谱-串联质谱（LC-MS/MS）结合同位素稀释定量方法,建立了婴幼儿配方奶粉中维生素A、维生素D_2、维生素D_3、维生素E和维生素K15种脂溶性维生素同时测定的分析方法。样品经脂肪酶酶解,氢氧化钾-乙醇皂化,石油醚提取,乙醇定容,经BEH C18色谱柱（100 mm×2.1 mm,1.7μm）分离后,以甲醇（甲酸0.02%）-0.1%甲酸溶液为流动相,0.4 m L/min梯度洗脱,采用大气压化学电离,正离子多反应监测模式测定。5种脂溶性维生素在一定浓度范围内具有良好的线性关系,相关系数（r2）大于0.99,加标回收率为83.8%～113.7%,相对标准偏差（RSD,n=6）为1.2%～10.1%,定量下限（LOQ）为0.5～10μg/100g。该方法简便、快速、灵敏、准确,可满足配方奶粉中脂溶性维生素的检测要求。A liquid chromatography-tandem mass spectrometric method（ LC-MS / MS） was developed for the determination of content of vitamin A,vitamin D_2,vitamin D_3,vitamin E and vitamin K1 in infant formula milk. The fat vitamins were extracted with petroleum ether after enzymatic hydrolysis and saponification. The chromatographic separation was completed with the column of BEH C18（ 100 mm × 2. 1 mm,1. 7 μm） using methanol（ 0. 02% formic acid）-0. 1% formic acid solution as mobile phase. Ionization mode was positive atmospheric pressure chemical ionization（ APCI）.Mass spectrometry data was acquired by multiple reaction monitoring（ MRM） mode. The quantification analysis was carried out by isotope dilution method（ each vitamin had its isotope internal standard）. The calibration curves of 5 fat vitamins were linear in the certain concentration ranges with correlation coefficients（ r～2） above 0. 99. The recoveries at three spiked levels（ low,middle and high）ranged from 83. 8% to 113. 7% with relative standard deviations（ RSD,n = 6） of 1. 2%-10. 1%.The quantitation limits were in the range of 0. 5-10 μg /100 g. The method was rapid,easy,accurate and sensitive,and could be used to detect fat vitamins in infant formula milk.

关 键 词：同位素稀释 液相色谱-串联质谱(LC-MS/MS) 脂溶性维生素 维生素A 维生素D 维生素E 维生素K1 测定 

分 类 号：O657.63[理学—分析化学] O629.4[理学—化学]