多种油脂性食品中氯丙醇酯的检测及暴露危险分析

Determination and exposure risk analysis of chloropropanols esters in a variety of fat-rich foods

中文关键词:  氯丙醇酯  油脂性食品  气相色谱质谱法  暴露危险

英文关键词:chloropropanols esters  fat-rich food  gas chromatography-mass spectrometry  exposure risk

中文摘要:

      目的 建立同时测定2-氯-1,3-丙二醇酯(2-chloropane-1,3-diol esters, 2-MCPD酯)和3-氯-1,2-丙二醇酯(3-chloropane-1,2-diol esters, 3-MCPD酯)的气相色谱-质谱联用(gas chromatography-mass spectrometry, GC-MS)检测方法, 对云南省内的油脂性食品进行检测和评估。方法 提取样品中的脂肪后, 依次使用甲醇钠水解和硅藻土小柱净化, 洗脱液挥干后用正己烷溶解, 七氟丁酰基咪唑衍生化, 气相色谱-质谱法测定, 内标法定量。结果 该方法的线性范围为20~600 ng, 相关性较好(r≥0.9994), 检出限为27.0 μg/kg, 回收率为79.4%~95.6%, 精密度相对标准偏差RSD≤5.5%。154份油脂性食品的检出率为30%, 含量范围在27.7~1850.0 μg/kg内。结论 该方法操作简单, 稳定可靠, 灵敏度高, 能满足日常检测的需要。云南省内的油脂性食品中2-MCPD酯和3-MCPD酯的总体暴露水平不高。

英文摘要:

      Objective To establish a method for simultaneous determination of 2-chloropane-1,3-diol esters (2-MCPD esters) and 3-chloropane-1,2-diol esters (3-MCPD esters) by gas chromatography-mass spectrometry (GC-MS), and investigate 2-MCPD esters and 3-MCPD esters residues in rich-fat foods from Yunnan province. Methods Fat was extracted from samples and hydrolyzed with sodium methylate. Following purification using diatomaceous earth columns and derivation with heptafluorobutyrylimidazole (HFBI), analytes were determined by GC-MS and quantified by internal standard method. Results The linearity was good in the range of 20~600 ng (r≥0.9994), limits of detection were 27.0 μg/kg, the recoveries were 79.4%~95.6%, with RSD≤5.5%. Among 154 fat-rich food, the detection rate of 2-MCPD esters and 3-MCPD esters was 30%, and the content ranged from 27.7~1850.0 μg/kg. Conclusion The method is simple, stable and reliable with high sensitivity, and is suitable for the determination of 2-MCPD esters and 3-MCPD esters. The exposure levels of 2-MCPD esters and 3-MCPD esters in fat-rich foods are low.