分光光度法定量测定药物纯制剂和片剂中胡萝卜碱的研究与应用

Asad Raza, Tariq Mahmood Ansari
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引用次数: 3

摘要

本文介绍了两种简便、新颖的分光光度法测定制剂中解痉药卡罗弗碱的方法。第一种(A)是直接法,纯药物在乙醇溶剂中在λmax 304 nm处进行分析。该方法在0.5 ~ 18 μg/ml范围内呈线性关系,相关系数为0.999,摩尔吸光度为5.55 × 104 L mol−1 cm−1。检测限和定量限分别为0.44和1.47 μg/ml。而第二种方法(B)是基于胡萝卜碱作为n电子供体与7,7,8,8-四氰喹诺二甲烷(TCNQ)作为pi受体之间的电荷转移反应,得到高度着色的稳定配合物,该配合物在波长525 nm处显示出最大吸收带。热力学参数计算为缔合常数KCT为7.53 × 104 mol−1,吉布斯自由能ΔG°为- 6.72 kJ mol−1。对影响电荷转移反应的各种因素进行了仔细的研究和优化。在最佳反应条件下,溶液浓度在1 ~ 35 μ ml−1范围内符合比尔定律,摩尔吸光度为1.17 × 104 L mol−1 cm−1,相关系数为0.9999。根据ICH指南对建议的方法进行了验证。
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Development and applications of spectrophotometric methods for quantitative determination of caroverine in pharmaceutical pure and tablet formulations

This paper describes two simple and novel analytical methods by using spectrophotometric technique for the determination of caroverine a spasmolytic drug in pharmaceutical formulations. The first (A) is a direct method in which analysis of the pure drug was carried out at its λmax 304 nm in ethanol solvent. The method was linear from 0.5 to 18 μg/ml with correlation coefficient of 0.999 and molar absorptivity of 5.55 × 104 L mole−1 cm−1. Limit of detection and limit of quantification were 0.44 and 1.47 μg/ml. While the second method (B) is based on the charge transfer reaction between caroverine as n-electron donor and 7,7,8,8-tetracyanoquinodimethane (TCNQ) as pi-acceptor resulting in highly colored stable complex, which showed maximum absorption band at wavelength of 525 nm. The thermodynamic parameters were calculated as association constant KCT of 7.53 × 104 mol−1 and Gibbs free energy ΔG° of −6.72 kJ mol−1. Different variables affecting the charge transfer reaction were carefully studied and optimized. At the optimum reaction conditions, Beer’s law was obeyed in a concentration range of 1–35 μg ml−1 with molar absorptivity of 1.17 × 104 L mole−1 cm−1 and correlation coefficient of 0.9999. The proposed methods were validated according to ICH guidelines.

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