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建立了复合预混饲料中29种兽药同时检测的超高效液相色谱-串联质谱分析方法。样品经甲醇-乙腈(1:1,V/V)混合溶液提取,提取液经Oasis HLB固相萃取柱净化,29种兽药经Waters Acquity UPLC BEH C18色谱柱分离,以甲醇和0.1%甲酸水溶液为流动相进行梯度洗脱。电喷雾正离子(ESI+)模式电离,多反应监测模式检测,内标法定量。结果表明:29种兽药在0.01~5.0μg/mL范围内呈良好的线性关系,相关系数(r)均大于0.993;复合预混饲料中3个浓度添加水平平均回收率为65.5%~92.2%;相对标准偏差为3.8%~15%。
A method for simultaneous determination of 29 veterinary drugs in compound premix feed by ultra performance liquid chromatography-tandem mass spectrometry was established. The samples were extracted with a mixture of methanol and acetonitrile (1: 1, V / V). The extracts were purified by Oasis HLB solid phase extraction column. 29 kinds of veterinary drugs were separated by Waters Acquity UPLC BEH C18 column. The methanol and 0.1% Mobile phase gradient elution. Electrospray positive ion (ESI +) mode ionization, multi-reaction monitoring mode detection, internal standard method. The results showed that 29 kinds of veterinary drugs showed a good linear relationship in the range of 0.01-5.0 μg / mL, the correlation coefficients (r) were all greater than 0.993. The average recoveries of three concentrations in composite premix feed ranged from 65.5% to 92.2%. The relative standard deviation was 3.8% ~ 15%.