DLLME-LC/MS/MS法快速检测食用油中黄曲霉毒素

Rapid Analysis of Aflatoxins in Edible Oils with Dispersive Liquid-Liquid Microextraction Prior to Highperformance Liquid Chromatography-Tandem Mass Spectrometry

试验建立了分散液相微萃取技术和高效液相色谱-串联质谱联用快速分析食用油中5种黄曲霉毒素的新方法。食用油样品先用正己烷溶解分散,再用一定比例的乙腈和水萃取,振荡漩涡离心后LC-MS/MS测定。试验对影响萃取效果的因素进行了优化,在优化试验条件下,方法的线性范围为0.06~10μg/kg,检出限为0.02~0.03μg/kg,相关系数为0.993 3~0.999 0,样品加标回收率为70.2%~86.8%,相对标准偏差为2.4%~7.3%。该方法已成功应用于食用油中黄曲霉毒素的分析测定。

A novel, simple and highly sensitive method was developed for the rapid analysis of Aflatoxins at trace level in edible oils. It was based on dispersive liquid-liquid microextraction（DLLME） and High performance liquid chromatographymass/mass spectrometry（LC-MS/MS）. Edible oil samples were dissolved and dispersed in hexane, then extracted with a certain proportion of acetonitrile and water. The LC-MS/MS was determined by oscillating vortex and centrifugation. The experiment has optimized the factors that affect the extraction. Under the optimal conditions, the linearity（0.06-10 μg/kg）, limits of detection（0.02-0.03 μg/kg） and the correlation coefficients were in the range of 0.993 3-0.999 0, the recoveries of spiked samples were in the range of 70.2%-86.8% and relative standard deviation（2.4%-7.3%） was obtained. The method had been successfully applied to the analysis and determination of aflatoxins in edible oils.