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采用在线柱后光化学衍生化和荧光检测的高效液相色谱法简单快速地测定人血浆中氯米芬顺式和反式异构体。

Simple and rapid determination of clomiphene cis and trans isomers in human plasma by high-performance liquid chromatography using on-line post-column photochemical derivatization and fluorescence detection.

作者信息

Urmös I, Benkö S M, Klebovich I

机构信息

Department of Pharmacokinetics, EGIS Pharmaceuticals Ltd., Budapest, Hungary.

出版信息

J Chromatogr. 1993 Jul 23;617(1):168-72. doi: 10.1016/0378-4347(93)80438-a.

Abstract

A validated, sensitive and rapid high-performance high-performance liquid chromatographic method has been developed for the analysis of both cis and trans isomers of clomiphene in human plasma. The method involves a new off-line pre-column solid-phase extraction for sample preparation of clomiphene from human plasma in the presence of an internal standard. Analysis was performed by isocratic elution on a LiChrospher 100 RP-18 5-microns column using on-line post-column photochemical derivatization, with fluorescence detection at 247 nm (excitation) and 378 nm (emission). The limit of quantitation was 0.75 ng/ml for the cis isomer and 1.25 ng/ml for the trans isomer. The precision and accuracy of method were between good laboratory practice (GLP) required limits.

摘要

已开发出一种经过验证的、灵敏且快速的高效液相色谱法,用于分析人血浆中克罗米酚的顺式和反式异构体。该方法涉及一种新的离线柱前固相萃取,用于在存在内标的情况下从人血浆中制备克罗米酚样品。采用等度洗脱,在LiChrospher 100 RP - 18 5微米柱上进行分析,使用在线柱后光化学衍生化,在247 nm(激发)和378 nm(发射)处进行荧光检测。顺式异构体的定量限为0.75 ng/ml,反式异构体的定量限为1.25 ng/ml。该方法的精密度和准确度在良好实验室规范(GLP)要求的限度范围内。

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