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分光光度法测定纯品和制剂中芬布芬钙药物。电荷转移固体制剂的光谱特性。

Spectrophotometric determination of fenoprofen calcium drug in pure and pharmaceutical preparations. Spectroscopic characterization of the charge transfer solid complexes.

机构信息

Chemistry Department, Faculty of Science, Cairo University, 12613 Giza, Egypt.

Chemistry Department, Faculty of Science, Cairo University, 12613 Giza, Egypt.

出版信息

Spectrochim Acta A Mol Biomol Spectrosc. 2018 Jan 15;189:357-365. doi: 10.1016/j.saa.2017.08.027. Epub 2017 Aug 10.

DOI:10.1016/j.saa.2017.08.027
PMID:28830039
Abstract

Simple, accurate and robust spectrophotometric method was developed for determination of fenoprofen calcium drug (FPC). The proposed method was based on the charge transfer (CT) reaction of FPC drug (as n-electron donor) with 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ), 2,4,6-trinitrophenol (picric acid, PA) or 1,2,5,8-tetrahydroxyanthraquinone (Quinalizarin, QZ) (as π-acceptors) to give highly colored charge transfer complexes. Different variables affecting the reaction such as reagent concentration, temperature and time have been carefully optimized to achieve the highest sensitivity. Beer's law was obeyed over the concentration ranges of 2-60, 0.6-90 and 4-30μgmL using DDQ, PA and QZ CT reagents, respectively, with correlation coefficients of 0.9986, 0.9989 and 0.997 and detection limits of 1.78, 0.48 and 2.6μgmL for the CT reagents in the same order. Elucidation of the chemical structure of the solid CT complexes formed via reaction between the drug under study and π-acceptors was done using elemental, thermal analyses, IR, H NMR and mass spectrometry. X-ray diffraction was used to estimate the crystallinity of the CT complexes. Their biological activities were screened against different bacterial and fungal organisms. The method was applied successfully with satisfactory results for the determination of FPC drug in fenoprofen capsules. The method was validated with respect to linearity, limit of detection and quantification, inter- and intra-days precision and accuracy. The proposed method gave comparable results with the official method.

摘要

建立了一种简单、准确、稳定的分光光度法用于测定非诺洛芬钙药物(FPC)。该方法基于 FPC 药物(作为 n-电子供体)与 2,3-二氯-5,6-二氰基-1,4-苯醌(DDQ)、2,4,6-三硝基苯酚(苦味酸,PA)或 1,2,5,8-四羟基蒽醌(Quinalizarin,QZ)(作为 π-受体)的电荷转移(CT)反应,生成高色的电荷转移络合物。仔细优化了影响反应的不同变量,如试剂浓度、温度和时间,以获得最高的灵敏度。使用 DDQ、PA 和 QZ CT 试剂,在 2-60、0.6-90 和 4-30μgmL 的浓度范围内,比尔定律均得到遵守,相关系数分别为 0.9986、0.9989 和 0.997,检测限分别为 1.78、0.48 和 2.6μgmL,按相同顺序为 CT 试剂。通过研究药物与 π-受体之间的反应形成的固体 CT 络合物的化学结构通过元素、热分析、IR、H NMR 和质谱法进行了阐明。X 射线衍射用于估计 CT 络合物的结晶度。它们的生物活性被筛选用于不同的细菌和真菌生物体。该方法成功地应用于非诺洛芬胶囊中 FPC 药物的测定,结果令人满意。该方法在线性、检测限和定量限、日内和日间精密度和准确度方面进行了验证。所提出的方法与官方方法具有可比性的结果。

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