【摘要】 建立了快速测定鳗鱼肌肉中氧氟沙星、诺氟沙星、恩诺沙星、环丙沙星、氟甲喹和恶喹酸6种喹诺酮类(QNs)药物残留的超高效液相色谱-串联质谱(UPLC-MS/MS)方法。样品经0.2mol/L磷酸盐缓冲液(PBS,pH=7.0)匀浆后,采用酸性乙腈(含0.2%甲酸)提取,正己烷脱脂,用ACQUITY UPLC BHE C18柱(100×2.1 mm,1.7μm),以乙腈-5mmol/L乙酸铵溶液(含0.2%甲酸)为流动相,用多反应监测(MRM)正离子扫描方式进行质谱检测,内标法定量。结果表明,该方法对以上6种喹诺酮类药物的线性范围为0.1~50μg/kg,相关系数(r)均大于0.9976;检出限为0.03~0.25μg/kg,定量限为0.1~0.8μg/kg,在1.0、2.0、10μg/kg 3个添加水平的回收率为84.8%~97.8%,相对标准偏差为4.5%~11.3%。该法简单、灵敏、特异性强,适用于鳗鱼肌肉中喹诺酮类药物多残留的检测。更多还原

【Abstract】 A ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method for the determination of six quinolone(QN)residues in eel muscle has been developed.The sample was extracted with acetonitrile(containing 0.2% formic acid)after homogenized by phosphate solution(0.2mol/L,pH=7.0),and then cleaned-up with hexane.The LC separation was performed on a column of ACQUITY UPLC BHE C18(100×2.1 mm,1.7μm)with acetonitrile and 5 mmol/L ammonium acetate solution(containing 0.2%formic acid)as the mobile phase.The analyte was detected by positive electrospray ionization(ESI)mode and multiple reaction monitoring(MRM)mode.The calibration curve showed good linearity within the concentrations of 0.1-50 μg/kg.The limits of detection were 0.03-0.25 μg/kg,and the limits of quantification were 0.1-0.8μg/kg.Average recoveries of six QNs(spiked at the levels of 1.0,2.0and 10.0μg/kg)ranged from 84.8% to 97.8%,with relative standard deviations between 4.5% and 11.3%.The results demonstrate that the method is simple,accurate and suitable for the simultaneous determination of multi-residues of quinolones in eel muscle.更多还原