Research Center for Drug Metabolism, College of Life Science, Jilin University, Changchun 130021, PR China.
J Pharm Biomed Anal. 2010 Feb 5;51(3):716-22. doi: 10.1016/j.jpba.2009.10.009. Epub 2009 Oct 14.
A rapid and sensitive method based on liquid chromatography-tandem mass spectrometry (LC-MS/MS) for the simultaneous quantitation of paracetamol, caffeine, pseudoephedrine, chlorpheniramine and cloperastine in human plasma has been developed and validated. After sample preparation by liquid-liquid extraction, the analytes and internal standard (diphenhydramine) were analyzed by reversed-phase HPLC on a Venusil Mp-C(18) column (50mmx4.6mm, 5microm) using formic acid:10mM ammonium acetate:methanol (1:40:60, v/v/v) as mobile phase in a run time of 2.6min. Detection was carried out by electrospray positive ionization mass spectrometry in the multiple-reaction monitoring mode. The method was linear for all analytes over the following concentration (ng/ml) ranges: paracetamol 5.0-2000; caffeine 10-4000; pseudoephedrine 0.25-100; chlorpheniramine 0.05-20; cloperastine 0.10-40. Intra- and inter-day precisions (as relative standard deviation) were all < or =11.3% with accuracy (as relative error) of +/-5.0%. The method was successfully applied to a study of the pharmacokinetics of the five analytes after administration of a combination oral dose to healthy Chinese volunteers.
建立并验证了一种基于液相色谱-串联质谱(LC-MS/MS)的快速、灵敏的方法,用于同时定量测定人血浆中的扑热息痛、咖啡因、伪麻黄碱、氯苯那敏和克仑特罗。经过液液萃取样品制备后,采用反相 HPLC 法,在 Venusil Mp-C(18)柱(50mmx4.6mm,5μm)上,以甲酸:10mM 乙酸铵:甲醇(1:40:60,v/v/v)为流动相,运行时间为 2.6min,以内标(苯海拉明)为内标,对分析物和内标(苯海拉明)进行分析。采用电喷雾正离子化质谱,在多重反应监测模式下进行检测。该方法在以下浓度(ng/ml)范围内对所有分析物均呈线性:扑热息痛 5.0-2000;咖啡因 10-4000;伪麻黄碱 0.25-100;氯苯那敏 0.05-20;克仑特罗 0.10-40。日内和日间精密度(以相对标准偏差表示)均<或=11.3%,准确度(以相对误差表示)为+/-5.0%。该方法成功地应用于研究健康中国志愿者口服联合剂量后 5 种分析物的药代动力学。