[关键词]
[摘要]
建立了一种气相色谱-串联质谱仪(GC-MS/MS)同时测定多种油脂类食品中3-氯丙醇酯(3-MCPDE),2-氯丙醇酯(2-MCPDE)和缩水甘油酯(GE)的检测方法。通过试验对样品提取、酯交换、衍生化,以及GC-MS/MS检测条件进行了优化,采用建立的GC-MS/MS方法对植物油、焙烤类食品、油炸膨化类食品以及奶粉四类食品中3-MCPDE,2-MCPDE和GE进行检测,方法的定量限在四类食品中分别为10、20、50和100 μg/kg。方法的总体平均回收率范围为68.9%~116.5%,相对标准偏差(RSDn=6)为2.11%~13.90%,结果表明样品在较宽的线性范围内,呈良好线性相关,相关系数(R)大于0.99。本方法提取效率高,净化效果好,检测灵敏度和准确度高,能够满足日常工作中植物油类、奶粉类、油炸膨化食品类和焙烤食品类等基质中3-MCPDE、GE和2-MCPDE的定性定量检测。
[Key word]
[Abstract]
A gas chromatography-tandem mass spectrometry (GC-MS/MS) method was established for the simultaneous determination of 3-chloropropanol ester (3-MCPDE), 2-chloropropanol ester (2-MCPDE) and gycidyl ester (GE) in various fatty foods in this study. The 3-MCPDE, 2-MCPDE and GE in vegetable oils, bakery foods, fried- puffed foods and milk powder were determined by GC-MS/MS after the optimization of extraction, transesterification and derivatization of samples and conditions of GC-MS/MS. The limits of quantitation (LOQs) of the four types of food products were 10, 20, 50 and 100 μg/kg, respectively, and the total mean recoveries were in the range of 68.9% ~116.5% with the relative standard deviation (RSD n=6) of 2.11%~13.90%. The results showed that the samples had good linear correlation within a wide linear range, and the correlation coefficients (R) were higher than 0.99. The proposed method had the advantages of high extraction efficiency, good purification effect, high detection sensitivity and accuracy, which could be used for qualitative and quantitative determination of 3-MCPDE, 2-MCPDE and GE in vegetable oils, milk powder, fried- puffed foods and bakery foods.
[中图分类号]
[基金项目]
国家质检总局科技计划项目(2015IK061)