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建立了一种超高效液相色谱-串联质谱法(UPLC-MS/MS)测定多种基质(鸡肉、鱼肉、鸡肝、鸡蛋和牛奶)中三甲氧苄氨嘧啶的分析方法。样品用甲酸-乙腈(1:9,V/V)溶液提取,正己烷除脂净化,Acquity UPLC BEH C18柱(1.7μm,2.1 mm×50 mm)分离,以甲醇和体积分数0.1%甲酸5 mmol乙酸铵(V/V)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)模式检测。结果表明:三甲氧苄氨嘧啶质量浓度在1.25~15.0μg/L范围内线性关系良好(r≥0.99)。方法的定量限(信噪比为10)为5.0μg/kg,在5.0,10.0μg/kg添加浓度的回收率为61.2%~108.5%,相对标准偏差(n=6)在1.4%~9.8%之间。方法适合于多种基质中三甲氧苄氨嘧啶的测定。
A high performance liquid chromatography-tandem mass spectrometry (UPLC-MS / MS) method was developed for the determination of trimethoprim in various substrates (chicken, fish, chicken liver, egg and milk). The sample was extracted with formic acid-acetonitrile (1: 9, V / V) solution and hexane was degreased. The sample was separated on an Acquity UPLC BEH C18 column (1.7 μm, 2.1 mm × 50 mm) Ammonium acetate (V / V) was used as the mobile phase for gradient elution, electrospray positive ion (ESI +) mode ionization, and multi-reaction monitoring (MRM) mode. The results showed that the concentration of trimethoprim was linear in the range of 1.25 ~ 15.0 μg / L (r ≥ 0.99). The limit of quantification (S / N ratio 10) was 5.0 μg / kg. The recoveries were 61.2% -108.5% at 5.0 and 10.0 μg / kg, and the relative standard deviations (n = 6) between. The method is suitable for the determination of trimethoprim in various matrices.