【摘要】 试验建立了一种分散固相萃取前处理技术结合高效液相色谱-串联质谱法检测禽蛋中9种喹诺酮类(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)兽药残留的分析方法。样品以乙腈、EDTA-Mcllvaine和乙酸为提取试剂、无水氯化钠为脱水剂、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。结果:9种喹诺酮在1.0~200μg/kg范围内具有良好的线性关系,相关系数(r~2)均在0.991以上;检出限范围为0.07~0.20μg/kg,定量限范围为0.22~0.67μg/kg;平均回收率介于73.5%~92.9%之间,相对标准偏差(RSD)低于11.8%。结果表明,该方法适合于检测禽蛋中喹诺酮类药物残留量。更多还原

【Abstract】 A method for the determination of 9 quinolones(danofloxacin mesylate,enrofloxacin,sarafloxacin,ciprofloxacin,ofloxacin,norfloxacin,enoxacin,pefloxacin,difloxacin)in eggs by dispersive solid phase extraction and high performance liquid chromatography- tandem mass spectrometry(HPLC- MS/MS)had been developed. The egg was extracted with acetonitrile,EDTA-Mcllvaine and acetic acid,dehydrated with Na Cl,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 monitoring(MRM)in positive ionization mode. The linear relation of9 quinolones was good and the correlation coefficient(r~2)was more than 0.991. The limit of detection(LOD)of 9 quinolones was 0.07 to 0.20 μg/kg and the limit of quantification(LOQ)was 0.22 to 0.67 μg/kg. The recovery rates analyte were between 73.5% to 92.9%. The relative standard deviations(RSD)were less than 8.9%. The method was reliable for the determination of quinolones in eggs.更多还原