超高效液相色谱-四极杆-飞行时间质谱技术非靶向定性筛查猪肉中79种药物残留

Qualitative Non-targeted Screening of 79 Drug Residues in Pork by Ultra-performance Liquid Chromatography Quadrupole Time-of-flight Mass Spectrometry

利用超高效液相色谱-四极杆-飞行时间质谱(UPLC-Q-TOF MS)建立了猪肉中79种药物残留的非靶向定性筛查方法。猪肉样本采用0.5%(体积分数)甲酸-乙腈溶液先提取,甲醇后提取的组合提取方式,离心后上清液通过FAVEX-NM50兽药残留快速柱净化。以Acquity UPLC BEH HSS-C_(18)色谱柱(2.1 mm×150 mm,1.7μm)进行分离,UPLC-Q-TOF MS电喷雾正离子模式电离,全信息串联质谱(MSE)模式检测。79种物质在相应范围内的线性关系良好,相关系数(r~2)均不小于0.99,方法的检出限和定量下限分别为0.05~10μg/kg和0.10~20μg/kg。基于实验室自建质谱数据库,对模拟阳性样本以及市售猪肉样本进行筛查,同时使用高灵敏度Xevo TQ-S串联四极杆质谱多反应监测模式(MRM)对市售猪肉样本进行验证。结果表明,所建立的方法高效、快速、通量高,适用于猪肉中药物残留的筛查和鉴定。

An analytical method was developed for qualitative non-targeted screening of 79 drug residues in pork by ultra-performance liquid chromatography quadrupole time-of-flight mass spectrometry(UPLC-Q-TOF MS).The samples were firstly extracted with 0.5%(by volume)formic acid-acetonitrile,then extracted with methanol.After centrifugation, the supernatant was cleaned up with FAVEX-NM50 rapid column of veterinary drug residues,then separated on an Acquity UPLC BEH HSS-C_(18)column(2.1 mm × 150 mm,1.7 μm),ionized in ESImode,and detected in MSEmode.The calibration curves for 79 drugs had good linearity in the linear range with correlation coefficients(r~2)not less than0.99.The limits of detection and the limits of quantitation were in the ranges of 0.05-10 μg/kg and 0.10-20 μg/kg, respectively.The simulated positive samples and commercial pork samples were screened using the self-built mass spectrometry database.Meanwhile, the commercial pork samples were detected by high sensitivity Xevo TQ-S tandem quadrupole mass spectrometry in multiple reaction monitoring(MRM)mode.Method validation showed that the established method was efficient, rapid and high throughput,which is suitable for the screening and identification of drug residues in pork.