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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。
A series of pre-treatment techniques of dispersive solid phase extraction (SPE) and high performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS) were established to detect nine quinolones (danofloxacin, enrofloxacin, sarafloxacin, ciprofloxacin, Norfloxacin, enoxacin, peoxifloxacin, bifloxacin) veterinary drug residues analysis. The samples were extracted with acetonitrile, EDTA-Mcllvaine and acetic acid, anhydrous sodium chloride as dehydrating agent, C18 as adsorbent, methanol-0.1% formic acid as mobile phase, reversed-phase C18 column, Reaction monitoring mode for mass spectrometry. Results: Nine quinolones showed a good linear relationship in the range of 1.0 ~ 200 μg / kg with the correlation coefficients (r ~ 2) above 0.991. The limits of detection ranged from 0.07 to 0.20 μg / kg. The limits of quantification ranged from 0.22 to 0.67 μg / kg. The average recoveries ranged from 73.5% to 92.9% with relative standard deviations (RSDs) below 11.8%. The results show that this method is suitable for the determination of quinolones residues in eggs.