非正常食用油鉴别新方法(二):特征奇数碳脂肪酸的多维气相色谱-质谱检测

A novel method for the identification of illegal cooking oil(2):determination of special odd-chain fatty acids by multidimensional gas chromatography-mass spectrometry

通过对脂肪酸的非靶标/靶标筛查,确立了非正常食用油(俗称地沟油)的内源性特征指示物:两种奇数碳脂肪酸,包括源自动物油的13-甲基十四烷酸和源自加热植物油的十一烷酸。并借助多维气相色谱-质谱技术,依据不同极性气相色谱柱的保留作用,不仅实现了不同碳数烷酸以及同碳数烷酸异构体之间的有效分离,达到了对13-甲基十四烷酸和十一烷酸准确定量的目的;而且实现了对目标化合物的在线净化、富集。凭借该项检测方法,参加了国家食品安全风险评估中心组织的第四、五批地沟油盲样考核。经过不断完善,该方法阴性样品的正确率提高到100%,阳性样品的正确率分别达到71%和75%。再结合辣椒碱指标,从内、外源指示物两方面全面、准确地对食用油样品进行判定,使得阳性样品的正确率分别提高至89%和100%。目前,该方法已经入选国家卫生部公布的四大地沟油鉴定仪器分析方法,正等待权威部门的协同性验证。

Endogenesis referents from illegal cooking oil（ICO）,namely,13-methyl-tetradecanoic acid and undecanoic acid have been confirmed via non-target and target screening of fatty acids.The former is mainly originated from animal oil,and the later from heated vegetable oil.Based on the retention interactions between gas chromatographic columns with different polarities and alkyl acids,the alkyl acids with various carbon chain or their isomers with the same carbon chains can be separated effectively using multidimensional gas chromatography-mass spectrometry.And the accurate quantification of 13-methyl-tetradecanoic acid and undecanoic acid was obtained.The target compounds can be cleaned up online and enriched with the developed method.Subsequently,the fourth and fifth assessments organized by China National Center for Food Safety Risk Assessment were performed in our laboratory.After continuous improvement,the precision of the method was increased.In detail,100% vegetable oils,71% ICO（the 4th batch） and 75% ICO（the 5th batch） have been identified.In combination with the capsaicinoid contents,edible oils can be identified in a comprehensive way,and the precision for ICO samples was increased to 89% and 100% for the 4th batch and the 5th batch samples,respectively.Owing to the aforementioned advantages,the developed method has been chosen as one of the four instrumental methods for the identification of ICO by China Ministry of Public Health,waiting for the validation from authoritative departments.