基于QuEChERS法-超高效液相色谱-串联质谱同位素标记内标法测定动物源性食品中11种喹诺酮类药物残留

The simultaneous determination of eleven quinolone drug residues in animal-sourced foods by the UPLC-MS/MS with isotope-labeled internal standards coupled with the QuEChERS method

目的建立同时测定动物源性食品中11种喹诺酮类药物残留的超高效液相色谱-串联质谱(UPLC-MS/MS)检测方法。方法结合QuEChERS技术,优化样品前处理方法,采用同位素标记内标法,以甲醇-乙腈(2∶3,V/V)与0.2%甲酸水溶液为流动相梯度洗脱,质谱分析采用电喷雾电离,正离子多反应监测(MRM)模式。结果 11种喹诺酮类药物在2.5~100.0μg/L范围内具有良好的线性关系,检测限范围为0.21~1.16μg/kg,平均回收率在82.7%~118.6%之间,相对标准差<15%。结论本法操作简便,精密度和准确度好,适用于动物源性食品中喹诺酮类药物残留的大批量样品快速检测。

Objective To establish an UPLC-MS/MS method for the simultaneous determination of eleven quinolone drug residues in animal-sourced foods. Methods The procedure for the pretreatment of samples was optimized by the QuEChERS method,and the isotope-labeled standards were used in UPLC-MS/MS. In the UPLC-MS/MS,the ultra performance liquid chromatography was performed using a gradient methanol-acetonitrile(2∶3,V/V)and 0.2% formic acid solution as mobile phase,and the detector of the electrospray ionization-tandem mass spectrometry was set in the positive and multiple reaction monitoring(MRM)mode. Results The calibration curves of the eleven quinolones showed a good linearity in the range of 2.5-100.0 μg/L. The limits of detection ranged from 0.21 to 1.16 μg/kg,the average recoveries were in the range of 82.7% to 118.6%,and the relative standard deviations were less than 15.0%. Conclusion The method could be simply put into operation,with a good precision and accuracy,which is suitable for rapid detection of quinolone drug residues in a large number of animal-sourced food samples.