Analytical Chemistry Department, Faculty of Pharmacy, Cairo University, Cairo, Egypt.
Pharmaceutical Analytical Chemistry Department, College of Pharmaceutical Sciences and Drug Manufacturing, Misr University for Science & Technology, Giza, Egypt.
Biomed Chromatogr. 2021 Sep;35(9):e5132. doi: 10.1002/bmc.5132. Epub 2021 May 5.
Two selective, sensitive and environmentally safe LC methods were developed and validated for determination of paracetamol, caffeine, ergotamine tartrate and metoclopramide in coformulated antimigraine tablets along with p-aminophenol, p-nitrophenol and theophylline as officially specified impurities. The first is based on high-performance thin-layer chromatography (HPTLC) coupled with densitometric quantitation. Separation was achieved on HPTLC silica gel 60 F plates as stationary phase using ethyl acetate:aqueous ammonium hydroxide solution:glacial acetic acid (10.0:0.4:0.1, by volume) as a developing system followed by scanning of the separated bands at 210.0 nm. The subsequent method depends on HPLC with diode array detection. The LC separation was accomplished on a Scharlau C (250 × 4.6 mm, 5 μm) column using a mixture of 20.0 mm sodium dihydrogen phosphate, pH 3.0, adjusted with o-phosphoric acid and methanol, at a flow rate of 1.3 mL/min in a gradient elution program. The separated peaks were detected at 210.0 nm. The proposed methods have been validated and proven to meet the requirements outlined in the International Council for Harmonisation (ICH) guidelines. The greenness profile evaluation was carried out using three tools, namely, the National Environmental Method Index, the Analytical EcoScale and the Green Analytical Procedure Index tool, and a comparative study was then conducted. Successful application of the developed methods for determination of the cited quaternary mixture in Metograine tablets confirms their suitability regarding the analytical performance and ecological impact in quality control assay and impurity profiling purposes.
建立并验证了两种选择性强、灵敏度高且环境友好的 LC 方法，用于同时测定复方偏头痛片中的对乙酰氨基酚、咖啡因、酒石酸麦角胺和甲氧氯普胺，以及作为官方指定杂质的对氨基酚、对硝基苯酚和茶碱。第一种方法基于高效薄层色谱（HPTLC）结合密度定量法。以 HPTLC 硅胶 60F 板为固定相，采用乙酸乙酯：氨水：冰醋酸（10.0：0.4：0.1，体积比）作为展开系统，分离后在 210.0nm 处扫描分离带。随后的方法依赖于二极管阵列检测的 HPLC。LC 分离在 Scharlau C（250×4.6mm，5μm）柱上完成，使用 20.0mm 磷酸二氢钠、pH3.0，用邻磷酸调，与甲醇以 1.3mL/min 的流速在梯度洗脱程序中进行。分离峰在 210.0nm 处检测。所提出的方法已经过验证，证明符合国际协调理事会（ICH）指南中概述的要求。使用三种工具，即国家环境方法指数、分析生态规模和绿色分析程序指数工具，对绿色度进行了评估，并进行了比较研究。所开发方法成功应用于 Metograine 片剂中所述季铵混合物的测定，证实了它们在质量控制分析和杂质分析目的中分析性能和生态影响方面的适用性。
