液相色谱-四极杆/静电场轨道阱质谱同时测定粮油中77种真菌毒素

Determination of Seventy-Seven Kinds of Mycotoxins in Grain and Oil by Liquid Chromatography-Quadrupole-Exactive Orbitrap Mass Spectrometry

建立了直接提取/稀释-超高效液相色谱-四极杆/静电场轨道阱高分辨质谱技术同时测定粮油中77种真菌毒素的方法。样品经过乙腈-水-乙酸(70∶29∶1)提取,稀释,CORTECSTM■UPLC■C18柱(1.6μm,2.1 mm×100 mm)分离,在一级母离子全扫描加数据依赖的二级子离子扫描模式(Full MS/dd MS^(2))下进行快速筛查、定量。77种化合物在各自浓度范围内线性良好(R^(2)≥0.99),定量限为0.6~48.0μg/kg,在3个不同浓度水平进行加标回收实验,回收率在70%~120%范围内的占95%以上,相对标准偏差为0.1%~8.7%。采用建立的方法对236批来自全区各地市的食用植物油进行检测,部分产品检出了不同含量的真菌毒素。该方法简便、准确,可满足粮油中真菌毒素的检测工作需要。

A rapid method based on ultra performance liquid chromatography-quadrupole-exactive orbitrap mass spectrometry(UPLC-Q-Exactive Orbitrap)was developed for the determination of 77 mycotoxins in grain and oil.The samples were extracted with acetonile-water-acetic acid(70∶29∶1),and dilute by water.The analytes were separated on a CORTECS■UPLC■C18(1.6μm,2.1 mm×100 mm)column,then,rapidly screened and quantified in Full MS/dd MS^(2) mode by UPLC-Q-Exactive Orbitrap.There were good linear relationships for the 77 analytes in their respective concentration ranges with correlation coefficients(R^(2))not less than 0.99.The method showed the limit of quantitation(LOQ)ranged from 0.6 to 48.0μg/kg.The recoveries for the 77 compounds at three spiked levels mainly ranged from 70%to 120%,with the relative standard deviations from 0.1%to 8.7%.The method was successfully applied to the determination of 236 batches of plant oil from different regions of the whole autonomous region,and different levels of mycotoxins was detected in part of the samples.The method was convenient and accurate,thus,it is suitable for the determination of the 77 mycotoxins in grain and oil.