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顺序注射色谱法测定药物制剂中盐酸氨溴索和多西环素的含量

Sequential injection chromatographic determination of ambroxol hydrochloride and doxycycline in pharmaceutical preparations.

作者信息

Satínský Dalibor, Santos Lucia M L Dos, Sklenárová Hana, Solich Petr, Montenegro M Conceição B S M, Araújo Alberto N

机构信息

Department of Analytical Chemistry, Faculty of Pharmacy, Charles University, Heyrovského 1203, Hradec Králové 500 05, Czech Republic.

出版信息

Talanta. 2005 Dec 15;68(2):214-8. doi: 10.1016/j.talanta.2005.06.059. Epub 2005 Aug 9.

Abstract

A new separation method based on a novel reversed-phase sequential injection chromatography (SIC) technique was used for simultaneous determination of ambroxol hydrochloride and doxycycline in pharmaceutical preparations in this contribution. The coupling of short monolith with SIA system results in an implementation of separation step to until no-separation low-pressure method. A Chromolith((R)) Flash RP-18e, 25-4.6mm column (Merck, Germany) and a FIAlab((R)) 3000 system (USA) with a six-port selection valve and 5ml syringe were used for sequential injection chromatographic separations in our study. The mobile phase used was acetonitrile-water (20:90, v/v), pH 2.5 adjusted with 98% phosphoric acid, flow rate 0.48mlmin(-1), UV detection was at 213nm. The validation parameters have shown good results: linearity of determination for both compounds including internal standard (ethylparaben) >0.999; repeatability of determination (R.S.D.) in the range 0.5-5.4% at three different concentration levels, detection limits in the range 0.5-2.0mugml(-1), and recovery from the pharmaceutical preparation in the range 99.3-99.9%. The chromatographic resolution between peak compounds was >5.0 and analysis time was <9min under the optimal conditions. The method was found to be applicable for routine analysis of the active compounds ambroxol hydrochloride and doxycycline in various pharmaceutical preparations.

摘要

本文采用一种基于新型反相顺序注射色谱(SIC)技术的新分离方法,用于同时测定药物制剂中的盐酸氨溴索和多西环素。短整体柱与顺序注射分析(SIA)系统的联用实现了从不分离的低压方法到分离步骤的转变。本研究采用德国默克公司的Chromolith((R)) Flash RP-18e,25-4.6mm色谱柱和美国的FIAlab((R)) 3000系统,该系统带有一个六通选择阀和5ml注射器用于顺序注射色谱分离。所用流动相为乙腈-水(20:90,v/v),用98%磷酸调节pH至2.5,流速为0.48mlmin(-1),紫外检测波长为213nm。验证参数显示出良好的结果:两种化合物(包括内标对羟基苯甲酸乙酯)的测定线性>0.999;在三个不同浓度水平下测定的重复性(相对标准偏差)在0.5-5.4%范围内,检测限在0.5-2.0mugml(-1)范围内,从药物制剂中的回收率在99.3-99.9%范围内。在最佳条件下,峰化合物之间的色谱分辨率>5.0,分析时间<9分钟。该方法适用于各种药物制剂中活性成分盐酸氨溴索和多西环素的常规分析。

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