Varin F, The Minh T u, Benoît F, Villeneuve J P, Théorêt Y
Faculté de Pharmacie, Université de Montréal, Canada.
J Chromatogr. 1992 Feb 7;574(1):57-64. doi: 10.1016/0378-4347(92)80097-a.
A simple and sensitive high-performance liquid chromatographic procedure to determine spironolactone and its three major metabolites in biological specimens is described. The assay involves sequential extraction on C18 and CN solid phases, and subsequent separation on a reversed-phase column. In plasma samples, spironolactone and its metabolites were completely separated within 8 min using an isocratic mobile phase, while in urine samples a methanol gradient was necessary to achieve a good separation within 14 min. Recoveries for all analytes were greater than 80% in plasma and 72% in urine. Linear responses were observed for all compounds in the range 6.25-400 ng/ml for plasma and 31.25-2000 ng/ml for urine. The plasma and urine methods were precise (coefficient of variation from 0.8 to 12.5%) and accurate (-12.1% to 7.4% of the nominal values) for all compounds. The assay proved to be suitable for the pharmacokinetic study of spironolactone in healthy human subjects.
本文描述了一种用于测定生物样品中螺内酯及其三种主要代谢物的简单、灵敏的高效液相色谱方法。该测定方法包括在C18和CN固相上进行顺序萃取，随后在反相柱上进行分离。在血浆样品中，使用等度流动相，螺内酯及其代谢物在8分钟内完全分离，而在尿液样品中，需要甲醇梯度才能在14分钟内实现良好分离。所有分析物在血浆中的回收率大于80%，在尿液中的回收率为72%。血浆中所有化合物在6.25-400 ng/ml范围内、尿液中在31.25-2000 ng/ml范围内均观察到线性响应。血浆和尿液方法对所有化合物均具有精密度（变异系数为0.8至12.5%）和准确度（为标称值的-12.1%至7.4%）。该测定方法被证明适用于健康人体受试者中螺内酯的药代动力学研究。
