开发和验证测定盐酸莫西沙星的分光光度法、原子吸收法和动力学法。

Analytical Chemistry Insights Pub Date : 2011-01-01 Epub Date: 2011-11-07 DOI:10.4137/ACI.S8090
Lobna M Abdellaziz, Mervat M Hosny
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引用次数: 0

摘要

本研究开发并验证了三种简单的分光光度法和原子吸收光谱法,用于测定纯品和药物制剂中的盐酸莫西沙星。方法 (A) 是一种动力学方法,基于 Fe(3+) 离子在 1,10 邻菲罗啉(邻苯)存在下对盐酸莫西沙星的氧化作用。方法(B)描述了测定盐酸莫西沙星的分光光度法程序,该程序基于盐酸莫西沙星将铁(III)还原为铁(II)的能力,而铁(II)在与 2,2'联吡啶(bipy)反应后迅速转化为相应的稳定有色络合物。我们仔细研究了方法(A)和方法(B)中形成的三络合物,并分别在 510 纳米和 520 纳米处测量了它们的吸光度。方法(C)是基于药物和四碘化铋(III)在酸性介质中形成离子对结合体,形成橙红色的离子对结合体。可通过三种不同的程序对这种关联物进行定量测定。将形成的沉淀过滤掉,溶解在丙酮中,在 462 纳米波长下用分光光度法定量(步骤 1);或者用盐酸分解,直接用原子吸收光谱法测定铋的含量(步骤 2)。此外,滤液中残留的未反应金属复合物也是通过间接原子吸收光谱技术测定其金属含量(步骤 3)。所有建议的方法都根据国际协调会议(ICH)指南进行了验证,建议的三种方法都可以测定盐酸莫西沙星,方法 A 和方法 B 的检测范围为(0.8-6,0.8-4),方法 C 中的程序 1-3 的检测范围为(16-96,16-96 和 16-72)。所提出的方法成功地用于测定药物制剂中的药物,不受常见辅料的干扰。所提议的方法得到的结果与参考方法得到的结果相当。
本文章由计算机程序翻译,如有差异,请以英文原文为准。

Development and validation of spectrophotometric, atomic absorption and kinetic methods for determination of moxifloxacin hydrochloride.

Development and validation of spectrophotometric, atomic absorption and kinetic methods for determination of moxifloxacin hydrochloride.

Development and validation of spectrophotometric, atomic absorption and kinetic methods for determination of moxifloxacin hydrochloride.

Development and validation of spectrophotometric, atomic absorption and kinetic methods for determination of moxifloxacin hydrochloride.

Three simple spectrophotometric and atomic absorption spectrometric methods are developed and validated for the determination of moxifloxacin HCl in pure form and in pharmaceutical formulations. Method (A) is a kinetic method based on the oxidation of moxifloxacin HCl by Fe(3+) ion in the presence of 1,10 o-phenanthroline (o-phen). Method (B) describes spectrophotometric procedures for determination of moxifloxacin HCl based on its ability to reduce Fe (III) to Fe (II), which was rapidly converted to the corresponding stable coloured complex after reacting with 2,2' bipyridyl (bipy). The formation of the tris-complex formed in both methods (A) and (B) were carefully studied and their absorbance were measured at 510 and 520 nm respectively. Method (C) is based on the formation of ion- pair associated between the drug and bismuth (III) tetraiodide in acidic medium to form orange-red ion-pair associates. This associate can be quantitatively determined by three different procedures. The formed precipitate is either filtered off, dissolved in acetone and quantified spectrophotometrically at 462 nm (Procedure 1), or decomposed by hydrochloric acid, and the bismuth content is determined by direct atomic absorption spectrometric (Procedure 2). Also the residual unreacted metal complex in the filtrate is determined through its metal content using indirect atomic absorption spectrometric technique (procedure 3). All the proposed methods were validated according to the International Conference on Harmonization (ICH) guidelines, the three proposed methods permit the determination of moxifloxacin HCl in the range of (0.8-6, 0.8-4) for methods A and B, (16-96, 16-96 and 16-72) for procedures 1-3 in method C. The limits of detection and quantitation were calculated, the precision of the methods were satisfactory; the values of relative standard deviations did not exceed 2%. The proposed methods were successfully applied to determine the drug in its pharmaceutical formulations without interference from the common excipients. The results obtained by the proposed methods were comparable with those obtained by the reference method.

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