液相色谱-串联质谱法测定蜂产品中20种喹诺酮类药物的残留量

Determination of 20 Quinolones Residues in Bee Products by Ultra Performance Liquid Chromatography- Tandem Mass Spectrometry

关键词:  超高效液相色谱-串联质谱  蜂蜜  蜂王浆  喹诺酮类药物  残留

Key words:  UPLC-MS/MS  honey  royal jelly  quinolones  residues

摘要:

建立了同时测定蜂蜜和蜂王浆中20种喹诺酮类药物的超高效液相色谱-串联质谱方法。以磷酸盐缓冲液(pH 3.0)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0.5 μg/kg,定量限为1.0 μg/kg,在蜂蜜和蜂王浆中添加浓度范围为1.0～5.0 μg/kg,其平均回收率为64.9～112.1%,相对标准偏差在0.6～14.7%之间。方法抗干扰能力强、分析速度快、灵敏度高,适用于蜂产品中喹诺酮类药物残留量的测定。

Abstract:

A method based on ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) has been developed for the determination of 20 quinolones residues in bee products. The analyte was extracted with phosphate buffer solution(pH3.0), 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 0.5 μg/kg and 1.0 μg/kg . The average recoveries ranged from 64.9～112.1% at the spiked level of 1.0～5.0 μg/kg in honey and royal jelly. The relative standard deviation was from0.6～15.7%. With the advantages of good anti-interference ability, rapidness and sensitivity, the method adapts to the determination of 20 quinolones in bee products.