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| Simultaneous determination of 3-chloropropanol esters and glycidyl esters in edible oils by gas chromatography-mass spectrometry |
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| DOI： |
| KeyWord:edible oil 3-chloropropanol esters glycidyl esters GC-MS |
| FundProject: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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| Abstract: |
| 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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