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| 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 |
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| DOI： |
| 中文关键词: 食用油脂 3-氯丙醇酯 缩水甘油酯 气相色谱-串联质谱法 |
| 英文关键词:edible oil 3-chloropropanol esters glycidyl esters GC-MS |
| 基金项目: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） |
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| 中文摘要: |
| 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8870%~92.42%，相对标准偏差（RSD）为2.80%~6.17%，3-MCPDE和GEs分别在40~15 000 μg/kg和 200~15 000 μg/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1 077.7 μg/kg， GEs的检出率为79.17%，平均含量为1 074.8 μg/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。 |
| 英文摘要: |
| 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 (40-15 000 μg/kg for 3-MCPDE and 200 -15 000 μg/kg for GEs) with a correlation coefficient (R2) of 0.996 0 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 1 077.7 μg/kg, and the detection rate of GEs was 79.17% with an average content of 1 074.8 μg/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. |
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