UPLC-MS/MS法测定阿胶糕中6种黄曲霉毒素的方法

The Methods of Simultaneous Determination of 6 Kinds of Aflatoxins in Gelatin Cake by UPLC-MS/MS

研究利用超高效液相色谱-串联质谱仪建立保健食品阿胶糕中6种黄曲霉毒素的快速检测方法。采用84%的乙腈作为提取剂,免疫亲和柱净化,色谱条件:Hypersil Gold C8色谱柱(150 mm×2.1 mm, 3μm);流动相为0.1%甲酸水溶液和乙腈,梯度洗脱,流速0.2 mL/min,柱温30℃,正离子模式扫描。结果表明:6种黄曲霉毒素在0.15~40.0ng/m L范围内具有良好的线性关系(线性相关系数均大于0.999),各组分的检出限在0.07~0.03μg/kg之间,定量限在0.02~0.15μg/kg之间。当加标浓度为1.0~10.0μg/kg时,回收率为69.2%%~106.7%,精密度为0.9%~4.1%。该方法快速、简便、可靠,应用于实际样品检测重现性良好,可为阿胶糕及其它保健食品中黄曲霉毒素的快速检测提供参考依据。

To establish a rapid detection method for six aflatoxins in health food gelatin cake by ultra performance liquid chromatography-tandem mass spectrometry,84%acetonitrile was used as extractant for purification by immunoaffinity column.Chromatographic conditions were Hypersil Gold C8 column(150 mm×2.1 mm,3μm).Mobile phase was 0.1%formic acid aqueous solution(5 mmol/L)and acetonitrile by gradient elution,flow rate was 0.2 mL/min,column temperature was 30℃,positive ion mode scanning.The results showed that the six aflatoxins had good linearity in the range of 0.15-40.0 ng/mL(linear correlation coefficient was greater than 0.999),and the detection limits of each component ranged from 0.07μg/kg to 0.03μg/kg.The limit of quantification was between 0.02μg/kg and 0.15μg/kg.When the spiked concentration is 1.0-10.0μg/kg,the recovery is 69.2%%-106.7%,and the precision is 0.9%-4.1%.The method was rapid,simple and reliable,it could be applied to the actual sample detection with good reproducibility,and could provide a reference for the rapid detection of aflatoxin in the gelatin cake and other health foods.