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化学计量学辅助同时测定合成二元混合物及药物剂型中的阿替洛尔和氯噻酮

Chemometrics-assisted simultaneous determination of atenolol and chlorthalidone in synthetic binary mixtures and pharmaceutical dosage forms.

作者信息

Ferraro Mónica C F, Castellano Patricia M, Kaufman Teodoro S

机构信息

Area Análisis de Medicamentos, Facultad de Ciencias Bioquímicas y Farmacéuticas, Universidad Nacional de Rosario, Suipacha 531, S2002LRK Rosario, Argentina.

出版信息

Anal Bioanal Chem. 2003 Dec;377(7-8):1159-64. doi: 10.1007/s00216-003-2185-6. Epub 2003 Sep 3.

Abstract

Resolution of binary mixtures of atenolol (ATE) and chlorthalidone (CTD) with minimum sample pre-treatment and without analyte separation has been successfully achieved, using a new and rapid method based on partial least squares (PLS1) analysis of UV spectral data. The simultaneous determination of both analytes was possible by PLS1 processing of sample absorbances between 255 and 300 nm for ATE and evaluation of absorbances in the 253-268 nm region for CTD. The mean recoveries for synthetic samples were 100.3 +/- 1.0% and 100.7 +/- 0.7% for ATE and CTD, respectively. Application of the proposed method to two commercial tablet preparations in the content uniformity test showed them to contain 103.5 +/- 0.8% and 104.9 +/- 1.8% ATE respectively, as well as 103.4 +/- 1.2% and 104.5 +/- 2.2% CTD. Use of this method also allowed the elaboration of dissolution profiles of the drugs in two commercial combined formulation products, through the simultaneous determination of both drugs during the dissolution test. At the dissolution time of 45 min specified by USP XXIV, both pharmaceutical formulations complied with the test.

摘要

使用一种基于紫外光谱数据偏最小二乘法(PLS1)分析的新型快速方法,成功实现了在最小化样品预处理且不进行分析物分离的情况下,对阿替洛尔(ATE)和氯噻酮(CTD)二元混合物的拆分。通过对255至300nm波长范围内样品吸光度进行PLS1处理来测定ATE,对253 - 268nm波长区域内的吸光度进行评估来测定CTD,从而实现了两种分析物的同时测定。合成样品中ATE和CTD的平均回收率分别为100.3±1.0%和100.7±0.7%。将该方法应用于两种市售片剂制剂的含量均匀度测试,结果显示它们分别含有103.5±0.8%和104.9±1.8%的ATE,以及103.4±1.2%和104.5±2.2%的CTD。使用该方法还能够通过在溶出度测试期间同时测定两种药物,来绘制两种市售复方制剂产品中药物的溶出曲线。在USP XXIV规定的45分钟溶出时间时,两种药物制剂均符合测试要求。

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