使用高效液相色谱法和放射免疫分析法同时分析洋地黄毒苷及其临床相关代谢物。

Simultaneous analysis of digitoxin and its clinically relevant metabolites using high-performance liquid chromatography and radioimmunoassay.

作者信息

Santos S R, Kirch W, Ohnhaus E E

机构信息

I. Medizinische Klinik, Christian-Albrechts-Universität, Kiel, F.R.G.

出版信息

J Chromatogr. 1987 Aug 7;419:155-64. doi: 10.1016/0378-4347(87)80274-8.

DOI:10.1016/0378-4347(87)80274-8

PMID:3667774

Abstract

A specific assay for determining the urinary excretion of unchanged digitoxin and its metabolites is described. The procedure includes solvent extraction of urine at pH 8.5, reversed-phase high-performance liquid chromatography (HPLC) and radioimmunoassay (RIA) of equivalent fractions. Confidence limits showed good linearity and precision of recovery and high sensitivity, accuracy and specificity. Cross-reactivities were high for digitoxigenin (DGTN) and digitoxigenin bisdigitoxoside (Bis-DGTN), they were low for digitoxigenin monodigitoxoside (Mono-DGTN) or digoxin when [125I]digitoxin RIA was used. The interference of endogenous compounds in urine in the RIA was overcome by using HPLC. Compared with results reported in the literature, the urinary recovery of unchanged digitoxin was lower, being only 8.11 +/- 1.51% of the dose administered. Amounts of 6.52 +/- 1.31% were excreted hydrolysed as Bis-DGTN, Mono-DGTN, DGTN or C12-hydroxylated as digoxin.

摘要

本文描述了一种用于测定地高辛原形及其代谢产物尿排泄量的特定分析方法。该方法包括在pH 8.5条件下对尿液进行溶剂萃取、反相高效液相色谱（HPLC）以及对等量馏分进行放射免疫分析（RIA）。置信限显示回收率具有良好的线性和精密度，且灵敏度、准确度和特异性高。当使用[125I]地高辛RIA时，洋地黄毒苷元（DGTN）和洋地黄毒苷元双洋地黄毒糖苷（双-DGTN）的交叉反应性较高，而洋地黄毒苷元单洋地黄毒糖苷（单-DGTN）或地高辛的交叉反应性较低。通过使用HPLC克服了尿液中内源性化合物对RIA的干扰。与文献报道的结果相比，地高辛原形的尿回收率较低，仅为给药剂量的8.11±1.51%。以双-DGTN、单-DGTN、DGTN形式水解或以地高辛形式C12-羟基化排泄的量为6.52±1.31%。