Gross A S, Phillips A C, Boutagy J, Shenfield G M
Department of Clinical Pharmacology, Royal North Shore Hospital, St Leonards, N.S.W., Australia.
J Chromatogr. 1993 Nov 17;621(1):115-20. doi: 10.1016/0378-4347(93)80085-i.
A method to determine the concentration of dexfenfluramine and its active metabolite nordexfenfluramine in human urine from healthy volunteers is described utilising a high-performance liquid chromatographic procedure with liquid-liquid extraction and ultraviolet detection. Analytes are measured after extraction of alkalinised urine with diethyl ether and subsequent back extraction with 0.5 M H2SO4 and with chromatography performed on a reversed-phase C18 column, using a mobile phase of acetonitrile-50 mM K2HPO4 (25:75, v/v) (flow-rate 1.3 ml/min) and ultraviolet detection at 210 nm. The sensitivity of the technique (10 ng/ml) is appropriate to measure both parent drug and metabolite in urine in humans for up to 5 days after a single 30-mg dose. The method is selective, reproducible (within- and between-day coefficient of variation ranged from 4.2 to 15%) and accurate (bias less than 8%) and thus suitable for dexfenfluramine pharmacokinetic investigations.
描述了一种利用高效液相色谱法结合液液萃取和紫外检测来测定健康志愿者尿液中右芬氟拉明及其活性代谢物去甲右芬氟拉明浓度的方法。在用乙醚萃取碱化尿液并随后用0.5 M硫酸反萃取后，对分析物进行测量，并在反相C18柱上进行色谱分析，使用乙腈 - 50 mM磷酸氢二钾（25:75，v/v）的流动相（流速1.3 ml/min），并在210 nm处进行紫外检测。该技术的灵敏度（10 ng/ml）适合于在单次30 mg剂量后长达5天内测量人体尿液中的母体药物和代谢物。该方法具有选择性、可重现性（日内和日间变异系数范围为4.2%至15%）和准确性（偏差小于8%），因此适用于右芬氟拉明的药代动力学研究。
