Shah Hiten J, Kundlik Mohan L, Pandya Ankit, Prajapati Shivkumar, Subbaiah Gunta, Patel Chhagan N, Patel Dasharath M, Suhagia Bhanu N
Bioanalytical Laboratory, Torrent Research Centre, Bhat, Gandhinagar-382428, Gujarat, India.
Biomed Chromatogr. 2009 Feb;23(2):141-51. doi: 10.1002/bmc.1095.
A selective, rapid and simple liquid chromatography-tandem mass spectrometry (LC-MS/MS) method is described for assay of donepezil in human plasma using escitalopram as an internal standard. Chromatographic separation was achieved on a Betabasic-C(8), 5 microm, 100 x 4.6 mm column using methanol:water:formic acid (90:9.97:0.03, v/v/v) as mobile phase. Detection of donepezil and internal standard was achieved by ESI MS/MS in positive ion mode using 380.20/91.10 and 325.13/262.00 transitions, respectively. The linearity over the concentration range of 0.15-50 ng/mL for donepezil was obtained and the lower limit of quantification was 0.15 ng/mL. For each level of quality control samples, inter-day and intra-day precisions (RSD) were < or =8.92 and 10.35% and accuracy (%RE) were < or =7.33% and 9.33%, respectively. The recovery was more than 88.50% for both donepezil and internal standard by solid-phase extraction, eliminating evaporation and reconstitution steps.
本文描述了一种选择性、快速且简单的液相色谱-串联质谱法（LC-MS/MS），以艾司西酞普兰作为内标物，用于测定人血浆中的多奈哌齐。采用甲醇:水:甲酸（90:9.97:0.03，v/v/v）作为流动相，在一根粒径为5微米、规格为100×4.6毫米的Betabasic-C(8)柱上实现色谱分离。多奈哌齐和内标物分别通过电喷雾串联质谱（ESI MS/MS）在正离子模式下，采用380.20/91.10和325.13/262.00的跃迁进行检测。多奈哌齐在0.15 - 50 ng/mL浓度范围内呈线性，定量下限为0.15 ng/mL。对于每个质量控制样品水平，日间和日内精密度（相对标准偏差，RSD）分别≤8.92%和10.35%，准确度（相对误差，%RE）分别≤7.33%和9.33%。通过固相萃取，多奈哌齐和内标物的回收率均超过88.50%，无需蒸发和复溶步骤。
