论文部分内容阅读
目的建立人胎盘灌流液中奥司他韦和羧酸奥司他韦的高效液相色谱-串联质谱(HPLC-MS/MS)测定方法。方法以甲硝唑为内标,胎盘灌流液样品经沉淀蛋白处理,色谱柱为Shim-pack XR-ODSⅡ柱(2.0 mm×75 mm,2.2μm);0.1%甲酸-0.1%甲酸乙腈溶液为流动相,梯度洗脱,流速为0.3 m L·min-1;电喷雾电离源,正离子多离子反应监测,奥司他韦和羧酸奥司他韦定量离子对分别为m/z 313.0→166.1和m/z 285.1→197.1。结果奥司他韦和羧酸奥司他韦分别在0.41~100 ng·m L-1、4.1~1 000 ng·m L-1范围内线性关系良好,平均方法回收率89.3%~104.7%,日内及日间RSD均小于15%,稳定性考察结果良好。结论本方法可用于人胎盘灌流液中奥司他韦和羧酸奥司他韦浓度的检测。
Objective To establish a method for the determination of oseltamivir and oseltamivir carboxylate in human placental perfusate by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS). Methods Metronidazole was used as an internal standard. The sample of placental perfusate was precipitated and the column was Shim-pack XR-ODSⅡ (2.0 mm × 75 mm, 2.2 μm). 0.1% formic acid-0.1% formic acid in acetonitrile Phase and gradient elution at a flow rate of 0.3 m L · min-1. The electrospray ionization source, positive ion detection of multi-ion reaction, oseltamivir and oseltamivir carboxylate were m / z 313.0 → 166.1 And m / z 285.1 → 197.1. The results showed that oseltamivir and oseltamivir carboxylate had good linearity in the range of 0.41-100 ng · m L-1, 4.1-1000 ng · m L-1, and the average recovery was 89.3% -104.7% The RSDs were less than 15% during the day and during the day, and the stability was good. Conclusion This method can be used for the determination of oseltamivir and oseltamivir carboxylate in human placental perfusate.