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

Determination of Sulfonamides and Quinolones in Feeds by Ultra Performance Liquid Chromatography- Tandem Mass Spectrometry

关键词:  超高效液相色谱-串联质谱  饲料  磺胺类药物  喹诺酮类药物

Key words:  UPLC-MS/MS  feeds  sulfonamides  quinolones

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0.1～100mg/kg,其平均回收率为60.6～118.6%,相对标准偏差在1.9～15.2%之间。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。

Abstract:

A method based on ultraperformance 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 60.6～118.6% at the spiked level of 0.1～100mg/kg in feeds. The relative standard deviation was from1.9～15.2%. With the advantages of good anti-interference ability, rapidness and sensitivity, the method adapts to the determination of sulfonamides and quinolones in feeds.