超高效液相色谱串联质谱法测定豆芽中15种喹诺酮类药物

Determination of 15 Quinolone Antibiotics in Soy Bean Sprout by Ultra Performance Liquid Chromatograhpy-Tandem Mass Spectrometry

采用超高效液相色谱串联质谱同时测定绿豆芽和黄豆芽中15种喹诺酮类药物的含量。样品经0.1 mol/L的EDTA-Mcllvaine缓冲溶液提取后,经Waters Oasis HLB固相萃取小柱净化,氮吹复溶后,采用Agilent Eclipse Plus C18柱(150 mm×3.0 mm,1.8μm)分离,以0.2%甲酸乙腈和0.2%甲酸水为流动相梯度洗脱,采用电喷雾离子源正离子动态多反应监测模式测定,外标法定量。2种豆芽基质中15种喹诺酮类药物的线性范围为5~120μg/kg,相关系数大于0.9996,方法检出限均为5μg/kg。15种喹诺酮在3个加标水平下平均回收率为64%~120%,相对标准偏差(n=6)0.13%~3.96%。采用该方法对400批豆芽进行检测分析,喹诺酮类药物残留检出率达到21.3%。结果表明该方法简单、灵敏、准确,实用性强,可用于豆芽中15种喹诺酮类药物残留的测定。

A high-performance liquid chromatography-tandem mass spectorometric(HPLC-MS/MS)method was developed for the simultaneous determination of 15 quinolone residues in mung bean sprouts and soybean sprouts.The sample was extracted with 0.1 mol/L EDTA-Mcllvaine buffer solution and cleaned by Waters Oasis HLB SPE.After evaporated to dryness under a stream of nitrogen,the analytes were then separated by the Agilent Eclipse Plus C18 column(150 mm×3.0 mm,1.8μm),using binary mobile phase gradient with water containing 0.2%formic acid and acetonitrile containing 0.2%formic acid.The compounds were detected under the Dynamic multiple reaction monitoring(DMRM)mode and quantified by the external standard method.The linearity of 15 quinolone in the range from 5~120μg/kg exhibited correlation coefficients greater than 0.9996.The limits of detection(LOD)were 5μg/kg.The average recoveries of 15 quinolones at three level spiked concentrations ranged from 64%to 120%,with the relative standard deviations(n=6)between 0.13%and 3.96%.The method was applied to detect 400 soy bean sprouts,the 23.1%of samples were detected the quinolones.The method was simple,rapid,sensitive and reliable,it could be applied to determine 15 quinolones in soy bean sprout.