Department of Pharmaceutics, Faculty of Pharmacy, Umm Al-Qura University, Makkah, Saudi Arabia; Department of Pharmaceutics and Industrial Pharmacy, Faculty of Pharmacy, Minia University, Minia, Egypt.
Department of Pharmaceutics, Faculty of Pharmacy, Ain Shams University, Cairo, Egypt.
Ann Pharm Fr. 2021 Nov;79(6):652-663. doi: 10.1016/j.pharma.2021.02.008. Epub 2021 Mar 3.
Three simple, sensitive, precise, reproducible and validated spectrophotometric methods have been developed for the quantification of pipazethate HCl as antitussive drug in pure and dosage forms.
The methods are based on utilization of N-bromosuccinimide as an oxidant and three dyes, amaranth, methylene blue, and indigo carmine, as auxiliary reagents. The proposed methods are based on oxidation reaction of pipazethate HCl with a known excess of N-bromosuccinimide in acid medium, followed by determination of unreacted N-bromosuccinimide by the reaction with a fixed amount of dyes, amaranth, methylene blue, and indigo carmine followed by the measurement of the absorbance at 520, 663 and 610nm, respectively. The optimization of the reaction conditions was investigated.
Under the optimum conditions, linear relationships with good correlation coefficients (0.9998-0.9999) were found over the concentration ranges of 0.3-9.0, 0.5-12 and 0.5-10μgmL with a limit of detection (LOD) of 0.1, 0.15 and 0.15μgmL using amaranth, methylene blue, and indigo carmine methods, respectively. Intra-day and inter-day accuracy and precision of the methods have been evaluated. No interference was observed from the common tablet excipients.
The developed methods were validated in accordance with ICH guidelines and successfully applied to the analysis of pipazethate HCl in dosage forms with good accuracy and precision. The reliability of the methods was further ascertained by performing recovery studies via the standard addition method. Statistical comparison of the results obtained by applying the proposed methods with those of the reported method by applying Student's t-test and variance ratio F-test at the 95% confidence level revealed good agreement and indicates no significant difference in accuracy and precision.
开发了三种简单、灵敏、精确、重现和验证的分光光度法，用于定量测定盐酸哌嗪作为镇咳药的纯品和制剂。
这些方法基于利用 N-溴代丁二酰亚胺作为氧化剂和三种染料，苋菜红、亚甲蓝和靛蓝胭脂红，作为辅助试剂。所提出的方法基于盐酸哌嗪在酸性介质中与已知过量的 N-溴代丁二酰亚胺的氧化反应，然后通过与固定量的染料苋菜红、亚甲蓝和靛蓝胭脂红的反应来测定未反应的 N-溴代丁二酰亚胺，然后分别在 520nm、663nm 和 610nm 处测定吸光度。研究了反应条件的优化。
在最佳条件下，在 0.3-9.0、0.5-12 和 0.5-10μgmL 的浓度范围内，与苋菜红、亚甲蓝和靛蓝胭脂红方法的相关系数（0.9998-0.9999）呈良好的线性关系，检测限（LOD）分别为 0.1、0.15 和 0.15μgmL。方法的日内和日间准确性和精密度已得到评估。未观察到常见片剂赋形剂的干扰。
所开发的方法符合 ICH 指南进行了验证，并成功应用于制剂中盐酸哌嗪的分析，具有良好的准确性和精密度。通过标准加入法进行回收研究进一步证实了方法的可靠性。应用所提出的方法获得的结果与应用已报道的方法获得的结果进行统计学比较通过学生 t 检验和方差比 F 检验在 95%置信水平下，表明准确性和精密度没有显著差异。
