Lan Jing, Wang Jian, Wu Dan, Wang Yingwu, Fawcett J Paul, Gu Jingkai
Research Center for Drug Metabolism, College of Life Science, Jilin University, Changchun 130021, PR China.
Rapid Commun Mass Spectrom. 2006;20(22):3309-12. doi: 10.1002/rcm.2741.
An analytical method for the determination of tranilast in human plasma using tramadol as the internal standard has been developed based on liquid chromatography/tandem mass spectrometry. Sample preparation involved protein precipitation with methanol. Separation by reversed-phase high-performance liquid chromatography using methanol/10 mM ammonium acetate (70: 30, v/v) as mobile phase was complete in a run time of 2.4 min. Detection on a Q TRAP system used multiple reaction monitoring. The method was linear in the range 0.06-20 microg/mL with intra- and inter-day precisions (as relative standard deviation) of 2.2-2.6% and 2.3-2.9%, respectively. Accuracy (as relative error) was <-2.5%. The method was applied in a pharmacokinetic study in healthy volunteers treated with a single 80 mg oral dose of tranilast.
基于液相色谱/串联质谱法，建立了一种以曲马多为内标测定人血浆中曲尼司特的分析方法。样品制备采用甲醇沉淀蛋白。以甲醇/10 mM醋酸铵（70:30，v/v）为流动相，通过反相高效液相色谱在2.4分钟内完成分离。在Q TRAP系统上进行检测，采用多反应监测。该方法在0.06 - 20 μg/mL范围内呈线性，日内和日间精密度（相对标准偏差）分别为2.2 - 2.6%和2.3 - 2.9%。准确度（相对误差）< -2.5%。该方法应用于健康志愿者单次口服80 mg曲尼司特的药代动力学研究。
