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薄层色谱法与紫外测定法联用用于尿液中萘普生及其主要代谢物的定量分析。

Coupling of TLC and UV-measurement for quantification of naproxen and its main metabolite in urine.

作者信息

Abdel-Moety E M, Al-Obaid A M, Jado A I, Lotfi E A

机构信息

Department of Pharmaceutical Chemistry, College of Pharmacy, King Saud University, Riyadh, Saudi Arabia.

出版信息

Eur J Drug Metab Pharmacokinet. 1988 Oct-Dec;13(4):267-71. doi: 10.1007/BF03190090.

Abstract

A simple sensitive method of high specificity and selectivity for quantitative determination of the non-steroidal anti-inflammatory drug naproxen and its main metabolite, 6-demethylated derivative, in biological specimens is described. Like naproxen, its metabolite absorbs maximally at 232 nm; this makes their simultaneous quantification, via direct UV-measurements at lambda max, in biological fluids quite impossible. Simple TLC-separation on silica gel F254 using chloroform + methanol (85:15, v/v) achieved the best fractionation of the unchanged drug and its metabolite from the matrix-contents of urine. UV-quantification of fractionated components could reach concentration levels of 0.2-3.0 micrograms ml-1 (ppm) in worked up urine samples. Varying levels of unchanged antiinflammatory drug and the phenolic metabolite could be accurately traced in urine samples following a 2.9 mg/kg oral dose after different time-intervals. Synthetic preparation of the metabolite by demethylation of naproxen is briefly mentioned.

摘要

本文描述了一种简单、灵敏、高特异性和高选择性的方法,用于定量测定生物样本中的非甾体抗炎药萘普生及其主要代谢物6-去甲基衍生物。与萘普生一样,其代谢物在232nm处有最大吸收;这使得通过在最大吸收波长处直接进行紫外测量来同时定量生物流体中的它们变得完全不可能。使用氯仿+甲醇(85:15,v/v)在硅胶F254上进行简单的薄层色谱分离,能从尿液的基质成分中实现对未变化药物及其代谢物的最佳分离。对分离后的组分进行紫外定量,在处理后的尿液样本中可达到0.2 - 3.0微克/毫升(ppm)的浓度水平。口服2.9毫克/千克剂量后,在不同时间间隔的尿液样本中,可以准确追踪到不同水平的未变化抗炎药和酚类代谢物。文中简要提及了通过萘普生去甲基化合成代谢物的方法。

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