超高效液相色谱串联-质谱法同时测定香辛料中7种真菌毒素

Determination of 7 Mycotoxin Contaminants in Spices by Ultra-high Performance Liquid Chromatography-tandem Mass Spectrometry

建立了同时测定香辛料中7种真菌毒素的超高效液相色谱-串联质谱分析方法(UPLC-MS/MS)。选用香辛料中的辣椒、花椒和八角为研究对象,粉碎后的样品用70%甲醇水溶液提取,6合1免疫亲和柱净化,ACQUITYUPLCHSST3色谱柱分离,超高效液相色谱-串联质谱测定,电喷雾正离子(ESI+)多反应离子监测方式监测,外标法定量。结果表明,7种真菌毒素在各自的线性响应范围内线性关系良好,相关系数均不低于0.995,7种真菌毒素的定量限为0.5~20μg/kg。低、中、高3个加标水平平均回收率(n=6)为67.25%~113.47%,相对标准偏差(RSD)为1.07%~10.20%。该方法具有前处理简单、净化效果好、灵敏度高和高通量检测的优点,适用于香辛料中多组分真菌毒素残留的分离和检测。

A method was developed for the determination of 7 mycotoxins in spices by ultra - high performance liquid chromatography-tendem mass spectrometry( UPLC-MS /MS).Selection of spices in chili,pepper and star anise for the study, smashed samples were extracted with 70% methanol water solution,purified by multifunction immunological affinity column, isolated by ACQUITY UPLC HSS T3 chromatographic column,determined by ultra - efficient liquid chromatography - mass spectrometry.The mass spectrometry was conducted by using positive ( ESI +) electrospray ionization and multi - reactions monitoring( MRM) models,with external standard method.The results indicated that 7 mycotoxins had good linear relationship, correlation coefficient were not less than 0.995,and the limit of quantitation( LOQ) for the range from 0.5 to 20 μg /kg.The average recovery rates at three levels of adding external standard were from 67.25% to 113.47%,with a relative standard deviation( RSD) varying from 1.07% to 10.20%.The method had simple process,good purification effect and the advantages of high sensitivity and high throughput detection,suitable for spices in multicomponent separation and detection of mycotoxin residues.