Addison R S, Duffy S L, Mathers S R
Department of Medicine, University of Queensland, Royal Brisbane Hospital, Australia.
J Chromatogr Sci. 1999 Mar;37(3):61-4. doi: 10.1093/chromsci/37.3.61.
A simple high-performance liquid chromatography assay using fluorescence detection for the major metabolite of the gastric prokinetic drug cisapride, norcisapride, is presented. Analysis is performed using an Alltech Platinum EPS C8 column with a mobile phase made up of methanol and 0.02M sodium dihygrogen phosphate (45:55, v/v) containing triethylamine (1 g/L). Complete resolution is achieved among norcisapride, the internal standard (metoclopramide), and endogenous urinary components. The assay is linear over the range 50-2000 ng/mL with a mean recovery of 71.2% across the analytical range following solvent extraction with toluene-isoamyl alcohol (95:5, v/v). Intraday coefficients of variation (precision) determined at 200 and 1000 ng/mL are 6.0 and 9.8%, respectively, and interday coefficients of variation are 8.8 and 6.6%, respectively. Intra- and interassay accuracy (as mean relative error) determined at the same concentrations is within 10% in all cases. An analysis of urine samples from a healthy volunteer following the administration of a single 10-mg oral dose of cisapride is shown.
本文介绍了一种简单的高效液相色谱法，用于检测胃动力药物西沙必利的主要代谢产物去甲西沙必利，采用荧光检测。分析使用Alltech Platinum EPS C8柱，流动相由甲醇和含三乙胺（1 g/L）的0.02M磷酸二氢钠（45:55，v/v）组成。去甲西沙必利、内标（甲氧氯普胺）和内源性尿液成分之间实现了完全分离。该检测方法在50 - 2000 ng/mL范围内呈线性，在用甲苯 - 异戊醇（95:5，v/v）进行溶剂萃取后，整个分析范围内的平均回收率为71.2%。在200和1000 ng/mL处测定的日内变异系数（精密度）分别为6.0%和9.8%，日间变异系数分别为8.8%和6.6%。在相同浓度下测定的批内和批间准确度（作为平均相对误差）在所有情况下均在10%以内。展示了一名健康志愿者口服单剂量10 mg西沙必利后尿液样本的分析结果。
