液相色谱-串联质谱法测定饲料中磺胺类和喹诺酮类药物的含量

摘要

建立了同时测定饲料中21种磺胺类药物和13种喹诺酮类药物的超高效液相色谱-串联质谱方法。以2％氨水乙腈和0．1 mol／L 氢氧化钠溶液提取样品中的待测物，HLB固相萃取柱净化，液相色谱-串联质谱法测定，外标法定量。药物在1～50 ng／mL浓度范围内线性关系良好，相关系数均大于0．99。方法的检出限为0．05 mg／kg，定量限为0．10 mg／kg，在不同饲料中添加浓度范围为0．1～100 mg／kg，平均回收率为60．6％～118．6％，相对标准偏差在1．9％～15．2％之间。本方法抗干扰能力强、分析速度快、灵敏度高，适用于饲料中磺胺类和喹诺酮类药物的测定。%A method based on ultra performance liquid chromatography-tandem mass spectrometry ( UPLC-MS/MS) has been developed for the determination of sulfonamides and quinolones in feeds. The analyte was extracted with acetonitrile containing 2% ammonia and 0. 1 mol/L sodium hydroxide solution, and cleaned by HLB solid phase extraction cartridge. Quantification of the analyte was achieved by UPLC-MS/MS with multiple reaction monitoring ( MRM ) using external standard method. The calibration curves of the drugs were linear in the concentration ranges of 1 ~ 50 ng/mL with correlation coefficients more than 0. 99. Detection limits and quantification limits of the method for the analyte were 0. 05 mg/kg and 0. 1 mg/kg in feeds. The average recoveries ranged from 60.6% to 118.6% at the spiked level of 0.1~100 mg/kg in feeds. The relative standard deviation was from 1. 9% to 15. 2%. With the advantages of good anti-interference ability, rapidness and sensitivity, the method adapted to the determination of sulfonamides and quinolones in feeds.