气相色谱-串联质谱法同时测定食用油脂中3-氯丙醇酯和缩水甘油酯  

Simultaneous determination of 3-chloropropanol esters and glycidyl esters in edible oils by gas chromatography-mass spectrometry

作　　者：刘瑶 高彤 张浩[1] 孙尚德[1] 陈小威[1] LIU Yao;GAO Tong;ZHANG Hao;SUN Shangde;CHEN Xiaowei(College of Food Science and Engineering,Henan University of Technology,Zhengzhou 450001,China)

机构地区：[1]河南工业大学粮油食品学院,郑州450001

出　　处：《中国油脂》2025年第2期87-94,共8页China Oils and Fats

基　　金：国家“十四五”重点研发项目(2021YFD2100302);河南省自然科学基金面上项目(232300420017);河南工业大学自科创新基金(2021ZKCJ02)。

摘　　要：旨在为减控3-氯丙醇酯(3-MCPDE)和缩水甘油酯(GEs)的污染程度和监测其含量变化奠定基础,建立了一种简便、快捷且能同时对食用油脂中3-MCPDE和GEs定性定量分析的检测方法。采用甲醇钠-甲醇溶液对样品进行碱水解反应12 min,用正己烷脱脂后,再用苯基硼酸(PBA)溶液衍生化20 min,采用乙酸乙酯提取3次,提取液氮吹至干,用少量乙酸乙酯复溶后,作为待测样液,设置质谱电离能量60 eV,进行GC-MS分析。结果表明:建立的方法的平均加标回收率为88.70%~92.42%,相对标准偏差(RSD)为2.80%~6.17%,3-MCPDE和GEs分别在40~15 000μg/kg和200~15 000μg/kg较宽的范围内呈现良好线性关系(R2≥0.996 0);该方法准确可靠,与进出口标准(SN/T 5220-2019)的检测结果无显著差异;采用该方法对24份常见市售食用油脂的3-MCPDE和GEs污染情况进行分析发现,3-MCPDE的检出率高达95.83%,平均含量为1 077.7μg/kg, GEs的检出率为79.17%,平均含量为1 074.8μg/kg,且棕榈油和米糠油的3-MCPDE含量和GEs含量远高于其他植物油。该方法具有简便、灵敏度和准确度高等优点,可用于食用油脂中3-MCPDE和GEs的同时测定,另外,急需改善棕榈油和米糠油中3-MCPDE和GEs的污染情况。To lay the foundation for reducing and controlling the pollution levels of 3-chloropropanol esters(3-MCPDE)and glycidyl esters(GEs),and monitoring their content changes,a simple,rapid method for the simultaneous qualitative and quantitative analysis of 3-MCPDE and GEs in edible oils was established.The samples were subjected to alkaline hydrolysis reaction using sodium methanol-methanol solution for 12 min,defatted with n-hexane,then derivatized with phenylboronic acid(PBA)solution for 20 min,and extracted with ethyl acetate for three times.The extract was nitrogen-blown to dryness,and re-solubilized with a small amount of ethyl acetate as the sample solution to be measured.The mass spectrometry was set to ionization energy of 60 eV,and then GC-MS was carried out to analyze the samples.The results showed that the established method had an average spiked recovery rate of 88.70%-92.42%and a relative standard deviation(RSD)of 2.80%-6.17%.3-MCPDE and GEs showed a good linear relationship over a wide range(40-15000μg/kg for 3-MCPDE and 200-15000μg/kg for GEs)with a correlation coefficient(R2)of 0.9960 or higher.The method was accurate and reliable,with no significant difference from the results of import and export standards(SN/T 5220-2019).When the method was applied to analyze 24 common commercial edible oils,it was found that the detection rate of 3-MCPDE was as high as 95.83% with an average content of 1077.7μg/kg,and the detection rate of GEs was 79.17% with an average content of 1074.8μg/kg.Palm oil and rice bran oil had significantly higher levels of 3-MCPDE and GEs compared to other vegetable oils.This method is characterized by its simplicity,high sensitivity,and high accuracy,and it can be used for the simultaneous determination of 3-MCPDE and GEs in edible oils.Additionally,there is an urgent need to improve the pollution situation of palm oil and rice bran oil.

关 键 词：食用油脂 3-氯丙醇酯 缩水甘油酯 气相色谱-串联质谱法 

分 类 号：TS225.1[轻工技术与工程—粮食、油脂及植物蛋白工程] TQ646[轻工技术与工程—食品科学与工程]