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液相色谱法测定药物制剂中的萘啶酸

Liquid chromatographic determination of nalidixic acid in pharmaceutical preparations.

作者信息

Walker S T

机构信息

Northeast Regional Laboratory, U.S. Food and Drug Administration, Brooklyn, NY 11232, USA.

出版信息

J AOAC Int. 1996 Mar-Apr;79(2):431-3.

PMID:8920129
Abstract

A simple, rapid, and environmentally safe liquid chromatographic (LC) method was developed for the qualitative and quantitative determination of pharmaceutical preparations of nalidixic acid. The new method was applied to commercial preparations of tablets and a suspension of nalidixic acid and found to be satisfactory for both quantitative and qualitative determinations. Previous LC methods either used chloroform to extract, which we were trying to eliminate, or used a mobile phase of about pH 2.5, which will destroy the column coating. The LC system for the new method uses sulfanilic acid as internal standard, a mu-Bondapak C18 column, and a mobile phase of methanol, 0.0045M dibasic potassium phosphate, and 0.0072M hexadecyltrimethylammonium bromide. The detection wavelength is 254 nm. The sample is dissolved in methanol, and an aliquot is injected through a 20 microL injection loop. Average recoveries ranged from 99.4 to 101.3%.

摘要

开发了一种简单、快速且环境安全的液相色谱(LC)方法,用于定性和定量测定萘啶酸药物制剂。该新方法应用于萘啶酸片剂和混悬液的市售制剂,结果表明其在定量和定性测定方面均令人满意。以往的液相色谱方法要么使用氯仿进行萃取(我们试图避免这种情况),要么使用pH约为2.5的流动相(这会破坏柱涂层)。新方法的液相色谱系统使用磺胺酸作为内标、μ-Bondapak C18柱以及由甲醇、0.0045M磷酸氢二钾和0.0072M十六烷基三甲基溴化铵组成的流动相。检测波长为254nm。样品溶解于甲醇中,取一份等分试样通过20微升进样环进样。平均回收率在99.4%至101.3%之间。

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