QuEChERS HPLC-MS/MS法测定禽肉中9种喹诺酮类兽药残留量

摘要

A method was developed for simultaneous determination of 9-quinolones(danofloxacinmesylate,en-rofloxacin, sarafloxacin,ciprofloxacin,ofloxacin,norfloxacin,enoxacin, pefloxacin, difloxacin) in poultry byQuEChERS-high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The chicken muscle was extracted with acetonitrile, EDTA-Mcllvaine and acetic acid,dehydrated with Na2SO4, purified with C18 sorbent and separated by C18 column using methanol and water (containing 0.1%formic acid) as mobile phase. The mass spectrometric acquisitions were carried out by means of multiple reaction mon-itoring(MRS) in positive ionization mode. The linear relation of 9 quinolones was good and the correlation coef-ficient(r2)was more than 0.993. The limit of detection(LOD) of 9 quinolones was 0.07μg/kg-0.20μg/kg and the limit of quantification (LOQ) was 0.23μg/kg-0.67μg/kg. The recovery rates of the target analyte were be-tween 70.8%-93.0%. The relative standard deviations (RSD) were less than 8.9%. The method was reliable for the determination of quinolones inpoultry.%建立QuEChERS-液相色谱串联质谱法同时检测禽肉中的丹诺沙星、恩诺沙星、沙拉沙星、环丙沙星、氧氟沙星、诺氟沙星、依诺沙星、培氧沙星、双氟沙星9种喹诺酮类兽药残留量方法.样品以乙腈、EDTA-Mcllvaine和乙酸为提取试剂,无水硫酸钠为脱水剂,C18为吸附剂进行净化,以甲醇-0.1%甲酸水为流动相,反相C18色谱柱分离,正离子多反应监测模式进行质谱分析.9种喹诺酮在1.0μg/kg~200μg/kg范围内具有良好的线性关系,相关系数(r2)均在0.993以上.检出限范围为0.07μg/kg~0.20μg/kg,定量限范围在0.23μg/kg~0.67μg/kg之间.平均回收率介于70.8%~93.0%之间,相对标准偏(RSD)低于8.9%.该方法适合于检测禽肉中的喹诺酮类药物残留量的测定.