尿液和粪便中的地高辛及其代谢物：一种荧光衍生化——高效液相色谱技术。

Digoxin and metabolites in urine and feces: a fluorescence derivatization--high-performance liquid chromatographic technique.

作者信息

Shepard T A, Hui J, Chandrasekaran A, Sams R A, Reuning R H, Robertson L W, Caldwell J H, Donnerberg R L

出版信息

J Chromatogr. 1986 Jul 11;380(1):89-98. doi: 10.1016/s0378-4347(00)83627-0.

Abstract

A high-performance liquid chromatography method is described for the determination of digoxin and its metabolites digoxigenin, digoxigenin monodigitoxoside, digoxigenin bis-digitoxoside and dihydrodigoxin (20S and 20R) excreted in urine and feces. The urine sample or fecal supernatant is extracted with methylene chloride in the presence of digitoxigenin or digitoxin as internal standard. Pre-column derivatization is achieved using 1-naphthoyl chloride with subsequent separation of the derivatized compounds on either a normal- or reversed-phase system with fluorescence detection. Recoveries for digoxin and all metabolites from fecal samples were in the range 60-74%, which is comparable to that previously determined for urine samples. Standard curve data revealed linearity over a wide range of concentrations. Coefficients of variation for the analysis were less than 10% for all compounds over a range of 5-125 ng per ml urine and 10-250 ng per 200 mg feces. Peaks for digoxin and metabolites in urine and feces were obtained when human excreta were analyzed.

摘要

描述了一种高效液相色谱法，用于测定尿液和粪便中排泄的地高辛及其代谢物洋地黄毒苷、洋地黄毒苷单洋地黄毒糖苷、洋地黄毒苷双洋地黄毒糖苷和二氢地高辛（20S和20R）。以洋地黄毒苷或洋地黄毒苷作为内标，用二氯甲烷萃取尿液样品或粪便上清液。使用1-萘甲酰氯进行柱前衍生化，随后在正相或反相系统上对衍生化化合物进行分离，并进行荧光检测。粪便样品中地高辛和所有代谢物的回收率在60%-74%之间，与之前测定的尿液样品回收率相当。标准曲线数据显示在很宽的浓度范围内呈线性。在每毫升尿液5-125纳克和每200毫克粪便10-250纳克的范围内，所有化合物分析的变异系数均小于10%。分析人体排泄物时，获得了尿液和粪便中地高辛及其代谢物的峰。