Goto N, Sato T, Shigetoshi M, Ikegami K
Research Laboratories, Yoshitomi Pharmaceutical Industries, Ltd., Saitama, Japan.
J Chromatogr. 1992 Jul 24;578(2):203-6. doi: 10.1016/0378-4347(92)80417-o.
The dioxopiperazine metabolites of quinapril in plasma and urine were extracted with hexane-dichloroethane (1:1) under acidic conditions. Following derivatization with pentafluorobenzyl bromide and purification of the desired reaction products using a column packed with silica gel, the metabolites were analysed separately by capillary column gas chromatography-electron-impact mass spectrometry with selected-ion monitoring. The limits of quantitation for the metabolites were 0.2 ng/ml in plasma and 1 ng/ml in urine. The limits of detection were 0.1 ng/ml in plasma and 0.5 ng/ml in urine, at a single-to-noise ratio of greater than 3 and greater than 5, respectively. The proposed method is applicable to pharmacokinetic studies.
喹那普利在血浆和尿液中的二氧哌嗪代谢物在酸性条件下用己烷 - 二氯乙烷(1:1)萃取。用五氟苄基溴衍生化后,使用硅胶填充柱对所需反应产物进行纯化,然后通过毛细管柱气相色谱 - 电子轰击质谱联用选择离子监测分别分析代谢物。代谢物的定量限在血浆中为0.2 ng/ml,在尿液中为1 ng/ml。检测限在血浆中为0.1 ng/ml,在尿液中为0.5 ng/ml,信噪比分别大于3和大于5。所提出的方法适用于药代动力学研究。