| 徐爱军1，王念念2，陈嘉祎3，钱美霞3，梁伟1，张鸿1.13 C同位素-碱水解-气相色谱-质谱法结合全自动前处理平台测定食用油中氯丙醇酯及缩水甘油酯[J].中国油脂,2026,51(7):.[XU Aijun1, WANG Niannian2, CHEN Jiayi3, QIAN Meixia3, LIANG Wei1, ZHANG Hong1.Determination of chloropropanediol esters and glycidyl ester in edible oils by 13C isotope- alkaline hydrolysis- GC-MS coupled with a fully automatic pretreatment platform[J].China Oils and Fats,2026,51(7):.] |
| 13 C同位素-碱水解-气相色谱-质谱法结合全自动前处理平台测定食用油中氯丙醇酯及缩水甘油酯 |
| Determination of chloropropanediol esters and glycidyl ester in edible oils by 13C isotope- alkaline hydrolysis- GC-MS coupled with a fully automatic pretreatment platform |
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投稿时间：2025-04-06 修订日期：2026-03-17 录用日期：2025-05-21
出版日期：2026-07-20
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| DOI：10.19902/j.cnki.zgyz.1003-7969.250172 |
| 中文关键词: 同位素法 氯丙醇酯 缩水甘油酯 碱水解法 |
| 英文关键词:isotope method chloropropanediol esters glycidyl ester alkaline hydrolysis method |
| 基金项目: |
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| Author Name | Affiliation | | XU Aijun1, WANG Niannian2, CHEN Jiayi3, QIAN Meixia3, LIANG Wei1, ZHANG Hong1 | 1.Shanghai Esensing Analytical Technology Co. , Ltd. , Shanghai 200233, China
2.Jiangsu Goldland Grain,
Oil and Foodstuff Co. , Ltd. , Nantong 226602, Jiangsu, China
3.Bunge (Nanjing) Grain and
Oil Co. , Ltd. , Nanjing 210046, China |
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| 中文摘要: |
| 为了满足中小型油脂企业生产的实际需求，建立了13C同位素-碱水解-气相色谱-质谱法同时测定食用油中3-氯丙醇酯（3-MCPDE）、2-氯丙醇酯（2-MCPDE）和缩水甘油酯（GE）的方法。采用全自动前处理平台并按照GB 5009.191—2024第二篇第一法中的碱水解法对样品进行前处理后进行气相色谱-质谱法检测，内标法定量。结果表明：该方法中3-MCPDE、2-MCPDE和GE在0.2~2 mg/kg范围内呈现良好线性关系（R2>0.997），定量限为0.2 mg/kg，检出限为0.06 mg/kg；在0.2、1.0 mg/kg和16 mg/kg加标水平下，3种污染物的平均加标回收率为90.0%~104.5%；在6次重复实验下，该方法测定3种污染物的变异系数为3.01%~4.15%，重现性良好；该方法准确可靠，与GB 5009.191—2024第二篇第一法的检测结果无显著差异。综上，该方法可用于食用油中3-MCPDE、2-MCPDE和GE的同时测定。 |
| 英文摘要: |
| To meet the practical demands of small and medium-sized edible oil processing plants, a method was established for the simultaneous determination of 3-monochloropropanediol ester (3-MCPDE), 2-monochloropropanediol ester (2-MCPDE), and glycidyl ester (GE) in edible oils using 13C isotope-alkaline hydrolysis-gas chromatography-mass spectrometry (GC-MS). A fully automatic pretreatment platform was used to prepare the samples according to the alkaline hydrolysis method described in Method 1 of Part 2 of GB 5009.191-2024, then was detected by GC-MS, and quantification was performed using the internal standard method. The results showed that for 3-MCPDE, 2-MCPDE, and GE, the method exhibited good linearity (R2 > 0.997) in the range of 0.2-2 mg/kg, with a limit of quantification of 0.2 mg/kg and a limit of detection of 0.06 mg/kg. At spiked levels of 02, 1.0 mg/kg, and 1.6 mg/kg, the average recovery rates for the three contaminants ranged from 900% to 1045%. In six replicate experiments, the coefficient of variation for the determination of the three contaminants using the established method ranged from 3.01% to 4.15%, indicating good reproducibility. The established method was accurate and reliable, with no significant difference in results compared to those obtained using Method 1 of Part 2 of GB 5009.191-2024. In conclusion, the established method is suitable for the simultaneous determination of 3-MCPDE, 2-MCPDE and GE in edible oils. |
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