液相色谱-电喷雾串联质谱法测定人血浆中的艾芬地尔  

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

作　　者：杨波[1] 陈勇川[1] 向荣凤[1] 杨丹[1] 夏培元[1] 刘松青[1] 

机构地区：[1]第三军医大学西南医院药剂科,重庆400038

出　　处：《色谱》2008年第3期322-326,共5页Chinese Journal of Chromatography

摘　　要：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-6mmol/L乙酸铵溶液（pH7.40）（体积比为90∶10）为流动相进行分离。在QTRAP^TM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/z326.1→308.2（艾芬地尔）和m/z531.0→82.1（酮康唑,内标）。在6min内完成了艾芬地尔的检测,工作曲线的线性范围为0.25～50μg/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0.08μg/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。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 μg/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 μg/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.

关 键 词：液相色谱 串联质谱 艾芬地尔 血浆 

分 类 号：O658[理学—分析化学]