| 郝宇1,2，马艺荧3，于力涛3.气相色谱-质谱法同时检测植物油中2-氯丙醇酯、
3-氯丙醇酯和缩水甘油酯及其风险评估[J].中国油脂,2025,50(7):.[HAO Yu1,2, MA Yiying3, YU Litao3.Simultaneous determination of 2-chloropropanol ester, 3-chloropropanol ester and glycidyl esters in vegetable oils by gas chromatography- mass spectrometry and its risk assessment[J].China Oils and Fats,2025,50(7):.] |
| 气相色谱-质谱法同时检测植物油中2-氯丙醇酯、
3-氯丙醇酯和缩水甘油酯及其风险评估 |
| Simultaneous determination of 2-chloropropanol ester, 3-chloropropanol ester and glycidyl esters in vegetable oils by gas chromatography- mass spectrometry and its risk assessment |
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| DOI：10.19902/j.cnki.zgyz.1003-7969.240143 |
| 中文关键词: 气相色谱-质谱法 植物油 2-氯丙醇酯 3-氯丙醇酯 缩水甘油酯 |
| 英文关键词:gas chromatography-mass spectrometry vegetable oil 2-chloropropanol ester 3-chloropropanol ester glycidyl esters |
| 基金项目:2023年度哈尔滨商业大学“青年科研创新人才”培育计划(2023-KYYWF-0995)；烹饪科学四川省高等学校重点实验室2022年度资助项目(PRKX2022Z06)；2022年大学生创新创业计划项目(S202210240088) |
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| Author Name | Affiliation | | HAO Yu1,2, MA Yiying3, YU Litao3 | 1.College of Toursim and Cuisine, Harbin University of Commerce, Harbin 150028, China
2.Cuisine Science Key Laboratory of Sichuan Province, Sichuan Tourism University, Chengdu
610100, China
3.Heilongjiang Academy of Green Food Science, Harbin 150028, China |
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| 中文摘要: |
| 旨在为监控植物油中氯丙醇酯和缩水甘油酯（GEs）水平提供技术参考，通过对样品前处理条件进行优化，建立一种同时测定植物油中2-氯丙醇酯（2-MCPDE）、3-氯丙醇酯（3-MCPDE）和GEs的气相色谱-质谱法（GC-MS），采用该方法测定50份市售植物油中的2-MCPDE、3-MCPDE和GEs含量，并进行暴露风险水平分析。结果表明：建立的方法为样品（0.2 g）经叔丁基甲醚-乙酸乙酯溶液和甲醇钠-甲醇溶液水解，正己烷脱脂，大孔硅藻土柱净化，20 mL乙酸乙酯洗脱，N-七氟丁酰基咪唑（HFBI）衍生后进行GC-MS检测，内标法定量；该方法2-MCPDE和3-MCPDE含量在5~800 ng/mL范围内线性良好，3-MCPDE和GEs总量在10~1 600 ng/mL范围内线性良好，检出限均为10.0 μg/kg，定量限均为25.0 μg/kg，决定系数均大于0.998，灵敏度高；在7次重复实验下，该方法测定3种污染物含量的相对标准偏差（RSD）均小于8%，重复性和精密度良好；在25、125 μg/kg和250 μg/kg加标水平下，3种污染物的回收率在81.40%~91.69%之间；市售植物油中的2-MCPDE、3-MCPDE、GEs含量分别为ND~380 μg/kg、ND~59.4 μg/kg、ND~65.3 μg/kg，检出率分别为48%、42%、38%，18岁及以上人群氯丙醇酯的平均暴露水平远低于欧盟规定的每日耐受摄入量〔2 μg/（kg·d）〕，对人体造成危害的可能性小。综上，建立的同时测定植物油中2-MCPDE、3-MCPDE和GEs含量的方法灵敏度高、精确度良好，植物油中氯丙醇酯和GEs暴露风险较小但其污染问题仍值得关注。 |
| 英文摘要: |
| To provide technical reference for monitoring the levels of chloropropanol esters(MCPDE) and glycidyl esters(GEs) in vegetable oils, a gas chromatography-mass spectrometry (GC-MS)method for simultaneous determination of 2-MCPDE, 3-MCPDE and GEs in vegetable oils was established through optimization of sample pretreatment conditions. The method was applied to analyze 50 commercially available vegetable oils, followed by exposure risk assessment. The results showed that the established method for samples (0.2 g) hydrolyzed with tert-butyl methyl ether-ethyl acetate solution and sodium methoxide-methanol solution, defatted with n-hexane, purified using a macroporous diatomaceous earth column with 20 mL ethyl acetate elution, and derivatized with HFBI to GC-MS analysis with internal standard quantification. The method showed good linearity for 2-MCPDE and 3-MCPDE in 5-800 ng/mL range, and total 3-MCPDE and GEs in 10-1 600 ng/mL range, with detection limits of 10.0 μg/kg, quantification limits of 25.0 μg/kg, determination coefficients more than 0.998, and high sensitivity. The method demonstrated good precision with RSD less than 8% across seven replicates. Average recoveries ranged 81.40%-91.69% at three spiked levels (25, 125 μg/kg and 250 μg/kg). In commercially available vegetable oils, 2-MCPDE, 3-MCPDE and GEs levels were ND (not detected) -380 μg/kg, ND-59.4 μg/kg and ND-65.3 μg/kg, respectively, with detection rates of 48%, 42% and 38%. The average MCPDE exposure level for adults (≥18 years) remained significantly below the tolerable daily intake regulated by European Union (2 μg/(kg·d)), indicating low health risks. In conclusion, the established method for the simultaneous determination of 2-MCPDE, 3-MCPDE and GEs in vegetable oils exhibits high sensitivity and precision, and the exposure risk of MCPDE and GEs is low, while their contamination in vegetable oils still warrants attention. |
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