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建立和验证盐酸异克舒令制剂的含量测定的定时法。

Development and validation of fixed-time method for the determination of isoxsuprine hydrochloride in commercial dosages forms.

机构信息

Department of Chemistry, Aligarh Muslim University, UP, India.

出版信息

Drug Test Anal. 2010 Sep;2(9):442-6. doi: 10.1002/dta.153.

DOI:10.1002/dta.153
PMID:20812296
Abstract

The main aim of this work was to develop a kinetic spectrophotometric method for the quantitative analysis of isoxsuprine hydrochloride in commercial tablets. The method is based on the reaction of isoxsuprine hydrochloride (ISx) with hydroxylamine hydrochloride and ammonium cerium (IV) nitrate in sulphuric acid medium at room temperature which resulted in the formation of yellow-coloured product peaking at 380 nm. The reaction is followed spectrophotometrically by measuring the absorbance as a function of time. Fixed time method (ΔA = A₄-A₂, where A₂ and A₄ refer to absorbance measurements taken at 2 and 4 min, respectively) was adopted for constructing the calibration curve which was found to be linear over the concentration range of 30-80 µgmL⁻¹ with molar absorptivity of 5.95 × 10³ L mol⁻¹ cm⁻¹. The method has been applied successfully to the determination of isoxsuprine hydrochloride in tablets. Statistical comparison (point and interval hypothesis tests) of the results showed that there is no significant difference between the proposed method and reference method.

摘要

本工作的主要目的是开发一种动力学分光光度法,用于定量分析市售片剂中的盐酸异克舒林。该方法基于盐酸异克舒林(ISx)与盐酸羟胺和硫酸介质中的硝酸铈(IV)铵在室温下的反应,反应生成的黄色产物在 380nm 处有最大吸收。通过测量吸光度随时间的变化来进行分光光度法跟踪反应。采用固定时间法(ΔA = A₄-A₂,其中 A₂ 和 A₄ 分别指在 2 分钟和 4 分钟时的吸光度测量值)构建校准曲线,发现其在 30-80μgmL⁻¹浓度范围内呈线性,摩尔吸光系数为 5.95×10³ L mol⁻¹ cm⁻¹。该方法已成功应用于片剂中盐酸异克舒林的测定。结果的统计比较(点和区间假设检验)表明,该方法与参考方法之间无显著性差异。

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