超高效液相色谱-串联质谱法测定鸡肉中的利巴韦林和金刚烷胺

摘要

A method for the determination of ribavirin and amantadine in chicken has been developed by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS).After extracted by 1％ (volume percentage) trichloroacetic acid solution-acetonitrile (1:1,v/v) and purified by a Supelco LC-SCX cartridge,the samples were loaded onto an Acquity UPLC BEH Hillic column (150 mm × 2.1 mm,1.7 μm)and separated with gradient elution.The electrospray was operated in the positive mode and the samples were monitored by the multiple reaction monitoring (MRM) mode.The limits of quantification (LOQs,S/N=10)of ribavirin and amantadine were 4.0 μg/kg.The calibration curves showed good linearity in the range of 10.0-100.0 μg/L,and the correlation coefficients (r2) were not lower than 0.99.When the spiked levels were 4.0,8.0 and 20.0 μg/kg,the recoveries of ribavirin and amantadine in chicken ranged from 78％ to 102.5％,with the relative standard deviations (RSDs) of 2.2％-7.6％.The results indicate that the method is simple,rapid,sensitive and suitable for the qualitative and quantitative analyses of ribavirin and amantadine in chicken samples.%建立了超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定鸡肉中利巴韦林和金刚烷胺的分析方法.样品用1％(体积分数)三氯乙酸溶液-乙腈(1∶1,v/v)溶液提取,经Supelco LC-SCX固相萃取柱净化后用Acquity UPLC BEH HiUic柱(150mm×2.1 mm,1.7 μm)分离,以甲醇和0.1％(体积分数)甲酸作为流动相进行梯度洗脱,电喷雾正离子(ESI+)模式电离,多反应监测(MRM)模式进行检测.结果表明,利巴韦林和金刚烷胺在10.0～100.0 μg/L范围内线性关系良好(r2≥0.99).方法的定量限(信噪比为10)为4.0 pg/kg,在4.0、8.0、20.0 μg/kg添加水平的回收率为78％ ～ 102.5％,相对标准偏差(n=6)在2.2％～7.6％之间.该方法快速、灵敏、准确,适合于鸡肉中利巴韦林和金刚烷胺的同时、快速、高灵敏度的分析检测.