液相色谱串联质谱检测食品中的黄曲霉毒素

为提高黄曲霉毒素的检测灵敏度，建立快速液相色谱串联质谱(LC-MS/MS)法对食品中的4 种黄曲霉毒素B1、B2、G1、G2 进行定性定量分析。样品粉碎后用体积比为84:16 的乙腈- 水混合液提取，过滤后通过真菌毒素净化柱进样，采用C18 柱分离，0.1% 甲酸溶液和甲醇做流动相，以60:40 比例等度洗脱，质谱在多反应监测(MRM)的正离子模式下进行分析。4 种组分在5min 内完全分离，而且此方法线性关系良好，黄曲霉毒素B1、B2、G1、G2 的检出限分别是0.012、0.009、0.013、0.007μg/kg，平均加标回收率在80%～95% 之间，相对标准偏差小于5%。该方法快速灵敏、准确可靠，其检出限可满足欧盟地区严格的黄曲霉毒素限量标准。

Determination of Aflatoxins in Food by Liquid Chromatography-Tandem Mass Spectrometry

In order to improve detection sensitivity of aflatoxions, a liquid chromatography-tandem mass spectrometry method was established for the simultaneously qualitative and quantitative analysis of aflatoxins B1, B2, G1 and G2. Samples were sequentially extracted by acetonitrile-water at a ratio of 84:16 (V/V), cleaned up with multifunctional cleaning column. After injection, the chromatographic separation was achieved on a C18 column using a mobile phase composed of a mixture of 0.1% formic acid and methanol through gradient elution. The analysis was realized by multiple reaction-monitoring modes. Under above conditions, aflatoxins B1, B2, G1 and G2 could be completely separated in 5 min with an excellent linear relationship. The determination limits for 4 kinds of aflatoxins were 0.012, 0.009, 0.013μg/kg and 0.007μg/kg, respectively. The recovery rate of spiked samples was in the range of 80%－95% with a relative standard deviation less than 5%. This method can provide a rapid, sensitive, accurate and reproducible detection for aflatoxins and its detection limit is sensitive enough to meet the European regulation for aflatoxins.