高效液相色谱-串联质谱法测定多种食品和饲料中的胶霉毒素

摘要

建立了加压溶剂萃取结合全自动固相萃取技术-高效液相色谱-串联质谱法(high performance liquid chromatography-mass spectrometry,HPLC-MS/MS)测定玉米和小麦等禾谷食品、猪的肌肉和肝脏等动物源食品及猪和鸡的饲料中胶霉毒素的液相色谱串联质谱法.前处理时依次采用加压溶剂萃取(pressurized liquid extraction,PLE)和全自动固相萃取(automated solid phase extraction,ASPE)技术,乙腈/水(50/50,V/V)为玉米、小麦及饲料样品的加压溶剂萃取液,乙腈/正己烷(60/40,V/V)为猪的肌肉和肝脏样品的加压溶剂萃取液,甲醇/水(85/15,V/V)为所有样品的全自动固相萃取洗脱液.HPLC-MS/MS检测,基质匹配工作曲线外标法定量.结果表明,不同样品中胶霉毒素在0.2～100 μg/L范围内具有良好的线性关系,相关系数R2≥0.995 8;不同样品中的胶霉毒素最低检出限在0.09 ～0.15 μg/kg,最低定量限在0.23 ～0.31 μg/kg;添加不同浓度水平的胶霉毒素,平均回收率为81.8％ ～95.4％,变异系数≤13.2％.%A method was developed for the determination of gliotoxin in food and feed by HPLC-MS/MS with pressurized liquid extraction (PLE) and auto-solid phase extraction (ASPE).The extracting solution were:acetonitrile/water (50/50,v/v) in plant samples,and acetonitrile/hexane (10/90,v/v) in animal samples.The elution solution was methanol-water (15/85,v/v) (ASPE).Qualitative analysis was performed with electrospray ionization in positive mode (ESI +) under multiple reaction monitoring (MRM) modes.The matrix-matched calibrations were used to quantify the residue concentrations.The calibration curves showed good linearity in the certain concentration for gliotoxin,with correlation coefficients (R2) more than 0.995 8.The average recoveries of gliotoxin were in the range of 81.8％-95.4％ at three spiked concentration levels,and relative standard deviations were less than 13.2％.The limits of quantitation (LOQ) were in the range of 0.23-0.31 μg/kg.Conclusion:A simple and automated method has been successfully developed for rapid determination of gliotoxin in food and feed.