Elagawany Mohamed, Farid Nehal F, Elgendy Bahaa, Abdelmomen Esraa H, Abdelwahab Nada S
Pharmaceutical Chemistry, Faculty of Pharmacy, Damanhour University, Damanhour, Egypt.
Center for Clinical Pharmacology, Washington University School of Medicine and St. Louis College of Pharmacy, St Louis, MO, USA.
Biomed Chromatogr. 2019 Sep;33(9):e4579. doi: 10.1002/bmc.4579. Epub 2019 Jun 2.
An efficient, economic and high yielding method was described for the synthesis of baclofen (BAC) pharmacopoeial impurities (impurity A and impurity B) which can be used for gram-scale synthesis. Furthermore, a novel ecofriendly thin-layer chromatographic TLC-densitometric method was established and validated for the determination of BAC and its synthesized impurities. The developed TLC-densitometric method is based on the chromatographic separation using TLC plates (60 F ) using a green mobile phase of ethyl acetate-methanol-ammonia solution, 33% (8:2:0.1, by volume) with UV scanning at 220 nm. The proposed method was validated with respect to International Conference on Harmonization guidelines. The validated method was successfully applied for determination of BAC in pure form and in its commercial dosage form. Additionally, the greenness profile of the developed method was evaluated and compared with those of the reported chromatographic methods. The developed method was found to be superior to the published methods, being environmentally benign.
描述了一种高效、经济且高产的合成巴氯芬（BAC）药典杂质（杂质A和杂质B）的方法，该方法可用于克级规模的合成。此外，还建立并验证了一种新型环保的薄层色谱-密度测定法，用于测定BAC及其合成杂质。所开发的薄层色谱-密度测定法基于使用TLC板（60F）进行色谱分离，采用乙酸乙酯-甲醇-氨溶液（33%，体积比为8:2:0.1）的绿色流动相，并在220nm处进行紫外扫描。该方法根据国际协调会议指南进行了验证。验证后的方法成功应用于纯形式和商业剂型中BAC的测定。此外，还评估了所开发方法的绿色度概况，并与报道的色谱方法进行了比较。结果发现，所开发的方法优于已发表的方法，对环境无害。
