液相色谱-电喷雾串联质谱法测定人血浆中的艾芬地尔

建立了测定人血浆中艾芬地尔的液相色谱-串联质谱方法。血浆样品用乙酸乙酯液-液提取后,以甲醇-6 mmol/L乙酸铵溶液(pH 7.40)(体积比为90∶10)为流动相进行分离。在Q TRAPTM串联质谱仪上,以选择性反应离子监测(SRM)方式进行定量分析,用于监测的离子为m/z 326.1→308.2 (艾芬地尔)和m/z 531.0→82.1 (酮康唑,内标)。在6 min内完成了艾芬地尔的检测,工作曲线的线性范围为0.25～50 μg/L,日内、日间精密度分别小于2.7%和6.5%,平均回收率为101.3%～105.0%,检测限为0.08 μg/L。本方法灵敏度高,特异性好,可以用于临床试验的血浆样品的检测。

Determination of ifenprodil in human plasma using liquid chromatography with electrospray tandem mass pectrometry

A method for the determination of ifenprodil levels in human plasma was established. Ifenprodil and the internal standard (IS), ketoconazole, were extracted from the plasma with ethyl acetate using liquid-liquid extraction. The extracts were separated by high performance liquid chromatography (HPLC) using methanol-6 mmol/L ammonium acetate (pH value was adjusted to 7.40) (90 : 10, v/v) as the mobile phase, and were then detected using mass spectrometry (MS). Electrospray source was applied and operated in positive ion mode. Selected reaction monitoring (SRM) mode with the transition of m/z 326.1 --> 308.2 was used to quantify ifenprodil, and m/z 531.0 --> 82.1 for IS. The excellent sensitivity and selectivity of the HPLC-MS/MS method allowed quantitation and identification of ifenprodil at low levels with a run time of 6.0 min. The assay was linear over the range from 0.25 to 50 microg/L. The intra-day and inter-day precisions measured as relative standard deviations (RSDs) were less than 2.7% and less than 6.5%, respectively. The average recoveries varied between 101.3% and 105.0%, and the detection limit was 0.08 microg/L. Due to its simplicity and accuracy, the established method is suitable for the application in a pharmaceutical study of the intervenous drop infusion of ifenprodil tartrate.