液质联用法结合自动固相萃取同时测定药食同源杂粮中14种真菌毒素

Simultaneous determination of 14 mycotoxins in medicine and food homologous coarse cereals by liquid chromatography tandem mass spectrometry combined with automatic solid phase extraction

建立液相色谱-串联质谱法结合自动固相萃取同时测定药食同源杂粮中14种真菌毒素的方法。样品经乙腈-水溶液(体积比6:4)提取,再利用一步法快速净化柱(QMyco-Multi)在自动固相萃取仪上完成快速净化,最后通过液相色谱分离,在电喷雾离子源(ESI)正负离子模式下同时进行多重反应离子监测(MRM)。结果表明:14种真菌毒素在不同质量浓度范围内线性关系良好(相关系数>0.99),定量限为0.2~10.0μg/kg,加标回收率为81%~117%,相对标准偏差(RSD)为2.0%~7.2%(n=6)。制备的方法简单快速、灵敏准确,可用于药食同源杂粮中14种真菌毒素的同时测定。

A method for the simultaneous determination of 14 mycotoxins in medicine and food homologous coarse cereals by liquid chromatography tandem mass spectrometry(LC-MS/MS)combined with automatic solid phase extraction technology was established.Samples were extracted with acetonitrile-water solution(volume ratio 6:4),and then quickly purified by one-step rapid purification column(QMyco Multi)on the automatic solid phase extractor.Finally,it was separated by liquid chromatography,and multiple reaction ion monitoring(MRM)was carried out simultaneously under the positive and negative ion mode of electric spray ion source(ESI).The results showed that the linear relationship of 14 mycotoxins was good within different mass concentration ranges(correlation cofficient>0.99).The quantification limit was 0.2-10.0μg/kg,the recovery rate of spiked samples was 81%-117%,and the relative standard deviation(RSD)was 2.0%-7.2%(n=6).The preparation method was simple,fast,sensitive,and accurate,and could be used for the simultaneous determination of 14 mycotoxins in medicine and food homologous coarse cereals.