固相支撑液液萃取-苯硼酸衍生化法测定婴幼儿配方乳粉中氯丙二醇酯及缩水甘油酯  

Determination of chloropropanols esters and glycidyl esters in infant formula milk powder by phenylboronic acid derivatization and solid-phase supported liquid-liquid extraction

作　　者：梁秀清 王艳丽 李芳芳 陈倩倩 李海霞 高喜凤 张红霞 张喜琦 张卉 刘艳明 LIANG Xiuqing;WANG Yanli;LI Fangfang;CHEN Qianqian;LI Haixia;GAO Xifeng;ZHANG Hongxia;ZHANG Xiqi;ZHANG Hui;LIU Yanming(Shandong Institute for Food and Drug Control,Shandong Research Center of Engineering and Technology for Safety Inspection of Food and Drug Control,Shandong Research Center of Engineering and Technology for Quality Control of Food for Special Medical Purposes,Jinan 250101,China)

机构地区：[1]山东省食品药品检验研究院,山东省食品药品安全检测工程技术研究中心,山东省特殊医学用途配方食品质量控制工程技术研究中心,济南250101

出　　处：《分析试验室》2023年第6期784-790,共7页Chinese Journal of Analysis Laboratory

基　　金：山东省食品药品检验研究院发展类课题(SDIFDC-KY-4-2022002)资助。

摘　　要：建立了一种基于固相支撑液液萃取技术与苯硼酸衍生化法相结合测定婴幼儿配方乳粉中氯丙二醇酯(MCPDE)及缩水甘油酯(GE)含量的气相色谱-质谱法。样品经乙酸乙酯提取,甲醇钠-甲醇溶液水解,苯硼酸衍生化,硅藻土柱固相支撑液液萃取净化,气相色谱-质谱法选择离子监测分析,内标法定量。结果表明,氯丙二醇酯及缩水甘油酯质量浓度在4~400 ng/mL范围内线性关系良好,线性相关系数均大于0.999,定量限为0.010 mg/kg;在婴幼儿配方乳粉中进行0.010, 0.025, 0.10和0.25 mg/kg加标回收实验,回收率在81.6%~109.3%之间,相对标准偏差(RSD)为3.8%~6.3%。该方法能够满足婴幼儿配方乳粉中氯丙二醇酯及缩水甘油酯的检测要求。A method was established for the determination of chloropropanols ester(MCPDE)and glycidyl esters(GE)in infant formula milk powder by GC-MS based on phenylboronic acid derivatization and solid-phase supported liquid-liquid extraction.The infant formula milk powder samples were extracted with ethyl acetate,hydrolyzed with sodium methoxide in methanol,derivatized with phenylboronic acid,and purified by solid-phase supported liquid-liquid extraction.The analytes were detected by GC-MS in selected ion monitoring(SIM)mode and quantified by internal standard method.The results showed that the linear concentration range was 4-400 ng/mL with the correlation coefficients(R~2)greater than 0.999.The limits of quantitation(LOQs)were 0.010 mg/kg.The spiked recoveries of the analytes from blank infant formula samples at four levels of 0.010,0.025,0.10,0.25 mg/kg ranged from 81.6%to 109.3%with the relative standard deviations(RSDs)of 3.8%-6.3%.The established method could be applied to determine MCPDE and GE in infant formula milk powder.

关 键 词：固相支撑液液萃取 苯硼酸衍生化法 氯丙二醇酯 缩水甘油酯 

分 类 号：TS252[轻工技术与工程—农产品加工及贮藏工程]