气相色谱-质谱法测定婴幼儿配方乳粉中3-氯-1,2-丙二醇酯和缩水甘油酯  

Determination of 3-Monochloropropane-1,2-Diol Esters and Glycidyl Esters in Infant Formula Milk Powder by Gas Chromatography-Mass Spectrometry

作　　者：王胜杰 梁琳 WANG Shengjie;LIANG Lin(Shanghai Institute of Quality Inspection and Technical Research,Shanghai 200233,China)

机构地区：[1]上海市质量监督检验技术研究院,上海200233

出　　处：《乳业科学与技术》2024年第6期31-36,共6页JOURNAL OF DAIRY SCIENCE AND TECHNOLOGY

基　　金：国家市场监督管理总局项目(2022MK033)。

摘　　要：建立气相色谱-质谱法测定婴幼儿配方乳粉中3-氯-1,2-丙二醇酯和缩水甘油酯的分析方法。通过优化脂肪提取和衍生条件,考察方法的加标回收率、线性关系、精密度、检出限和定量限,内标法定量。结果表明,本实验方法在绝对含量5~500 ng范围内具有良好的线性关系(r>0.999),检出限0.006 mg/kg,定量限0.015 mg/kg。10、100、500 ng 3个水平下的加标回收率在95.6%~100.9%之间,相对标准偏差均小于5.03%。通过批量比较气相色谱-质谱法与气相色谱-串联质谱法的检测数据,样品中3-氯-1,2-丙二醇酯和缩水甘油酯含量没有因仪器不同而出现明显差异。相比之下,气相色谱-质谱法仪器简单易操作,成本较低,便于在不同等级实验室推广,适用于婴幼儿配方乳粉中3-氯-1,2-丙二醇酯和缩水甘油酯的含量测定。An analytical method for the determination of 3-monochloropropane-1,2-diol esters(3-MCPDEs)and glycidyl esters(GEs)in infant formula milk powder was established using gas chromatography-mass spectrometry(GC-MS).Based on optimized lipid extraction and derivatization conditions,the method was evaluated for spiked recovery,linear relationship,precision,limit of detection(LOD)and limit of quantification(LOQ).Quantification was carried out using the internal standard method.The proposed method showed good linearity in the range of 5–500 ng(r>0.999),with an LOD of 0.006 mg/kg and an LOQ of 0.015 mg/kg.The recovery rates at three spiked concentration levels of 10,100 and 500 ng ranged from 95.6%to 100.9%,with relative standard deviations(RSDs)less than 5.03%.The results of GC-MS and gas chromatography-tandem mass spectrometry(GC-MS/MS)for 3-MCPDEs and GEs in several batches of infant formula samples did not significantly differ.In addition,compared with GC-MS/MS,the GC-MS method was simpler and easier to operate with lower cost and could be promoted in different levels of laboratories.Therefore,this method is suitable for determining the content of 3-MCPDEs and GEs in infant formula milk powder.

关 键 词：婴幼儿配方乳粉 3-氯-1 2-丙二醇酯 缩水甘油酯 气相色谱-质谱法 酸水解 

分 类 号：TS252.7[轻工技术与工程—农产品加工及贮藏工程]