气相色谱-串联质谱法测定婴幼儿配方奶粉中氯丙醇酯和缩水甘油酯  

Gas Chromatography-Mass Spectrometry Method for Determination of Chloropropanol Esters and Glycidyl Esters in Infant Formula

作　　者：林丽珊 傅武胜 张一可[3] 高博 蓝丽华[1,5] 庞杰 LIN Lishan;FU Wusheng;ZHANG Yike;GAO Bo;LAN Lihua;PANG Jie(College of Food Science,Fujian Agriculture and Forestry University,Fuzhou 350000,China;Fujian Key Laboratory of Zoonoses,Fujian Provincial Center for Disease Control and Prevention,Fuzhou 350001,China;School of Public Health,Fujian Medical University,Fuzhou 350122,China;Fujian International Travel Health Care Center,Fuzhou 350003,China;College of Pharmacy,Fujian University of Traditional Chinese Medicine,Fuzhou 350122,China)

机构地区：[1]福建农林大学食品科学学院,福建福州350000 [2]福建省人兽共患病研究重点实验室,福建省疾病预防控制中心,福建福州350001 [3]福建医科大学公共卫生学院,福建福州350122 [4]福建国际旅行卫生保健中心,福建福州350003 [5]福建中医药大学药学院,福建福州350122

出　　处：《食品科学》2020年第22期295-300,共6页Food Science

基　　金：国家自然科学基金面上项目(81172671);福建省卫生系统中青年骨干人才培养项目(2013-ZQN-ZD-9);福建省杰出青年基金项目(2011J06011)。

摘　　要：采用气相色谱-串联质谱法成功建立婴幼儿配方奶粉(以下简称婴配)中氯丙醇酯(chloropropanols esters,MCPDE)和缩水甘油酯(glycidyl esters,GE)的测定方法。对提取条件进行优化,单因素试验结果表明,婴配称取量为1.50 g、氨水用量为3.0 mL,脂肪在105℃条件下干燥1h时,测定结果较为可靠。在此条件下,MCPDE、GE的检出限分别为5、10μg/kg(以脂肪计),在100~2000μg/kg内与峰面积比值呈线性关系,相关系数R为0.999。以婴配样品YL-34中提取的脂肪为基质,在含量为100、400、1000μg/kg下进行加标实验,以奶粉计对应含量分别为20.5、82.0、205μg/kg,回收率为81.5%~114%,相对标准偏差在2.6%~10%(n=6)之间。采用此法参加FAPAS国际能力验证,结果满意。结果表明,建立的方法较好地满足了婴配样品中MCPDE和GE的定量,因此被指定为国家食品安全风险监测工作手册方法。A novel gas chromatography-mass spectrometry(GC-MS)method was developed to determinate the contents of chloropropanol esters(MCPDE)and glycidyl esters(GE)in infant formula.The extraction conditions were optimized as follows:milk powder 1.50 g,ammonia solution 3.0 mL,drying temperature 105℃,and drying time 1 h.Under these conditions,satisfactory results were obtained.The limits of detection(LODs)were 5 and 10μg/kg for MCPDE and GE(calculated as fat),respectively.A good linear range was obtained in the concentration range of 100-2000μg/kg with a correlation coefficient of 0.999.When a mixed standard was spiked to the fat extracted from infant formula YL-34 at levels of 100,400,and 1000μg/kg,which were calculated on the basis of milk powder as 20.5,82.0,and 205μg/kg,respectively,the recoveries varied from 81.5%to 114%with relative standard derivations(RSDs)of 2.6%-10%(n=6).When this method was applied in FAPAS international proficiency test,satisfactory results were obtained.Our results showed that the novel method had good accuracy and repeatability,and was suitable for quantification of both MCPDE and GE in infant formula.Therefore,the procedure has been included in the Chinese national food safety risk monitoring manual.

关 键 词：氯丙醇酯 缩水甘油酯 婴幼儿配方奶粉 测定方法 

分 类 号：TS201.6[轻工技术与工程—食品科学]