QuEChERS EMR-Lipid技术结合LC/MS/MS快速筛查与确证猪肉中55种兽药残留

Rapid Screening and Confirmation of 55 Kinds of Veterinary Drug Residues in Pork by QuEChERS EMR-Lipid Technology and LC/MS/MS

运用QuEChERS Enhanced Matrix Removal(EMR)-Lipid技术作为前处理方法,通过高效液相-三重四极杆质谱联用技术建立猪肉中55种兽药残留的快速检测方法。样品采用5%甲酸乙腈进行提取,经QuEChERS EMR-Lipid净化,氮吹浓缩后的溶液通过Agilent Eclipse Plus C18(150 mm×3.0 mm,1.8μm)进行分离,在三重四极杆正离子动态多反应监测模式下进行检测,通过保留时间及离子对丰度比进行快速筛查和确证,并采用基质标准曲线定量。结果表明,55种化合物在30 min内完成分离,在1.25~250 ng/mL范围内线性关系良好,相关系数r≥0.998,定量限均为1μg/kg,在1~100μg/kg加标回收中,回收率在60.5%~139.5%,RSD在1.0%~20.1%(n=6)。本方法简单、快捷、高效,适用于猪肉中多兽药残留的快速筛查与确证。

To establish a method for rapid screening and confirmation of 55 kinds of veterinary drug resides in pork,QuEChERS EMR-Lipid technology was used as a pre-processing method,and HPLC-triple quadrupole mass spectrometer was used as a method of detecting. The sample was extracted with acetonitrile(containing 5% formic acid),purified by QuEChERS EMR-Lipid,concentrated by nitrogen,separated by Agilent Eclipse Plus C18(150 mm×3.0 mm,1.8 μm),detected by triple quadrupole mass spectrometer(ESI+)and dynamic multiple reaction monitoring(dMRM)mode,rapid screening and validation were performed by retention time and ion abandance ratio. Results showed that 55 kinds of compounds were separated in 30 min. The calibration curves had good linearity between 1.25~250 ng/mL with the correlation coefficient r≥0.998.The limits of quantification were 1 μg/kg. The recoveries ranged from 60.5%~139.5% at the concentrations of 1~100 μg/kg with the relative standard deviations between 1.0%~20.1%(n=6). This method was simple,fast and efficient,which could be used for rapid screening and confirmation of the veterinary drug residues in pork.