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分析研究洛哌丁胺盐酸盐和曲美布汀药物的电荷转移配合物。CT 配合物的光谱和热特性。

Analytical studies on the charge transfer complexes of loperamide hydrochloride and trimebutine drugs. Spectroscopic and thermal characterization of CT complexes.

机构信息

National Organization for Drug Control and Research (NODCAR), Pyramid Ave., P.O. 29, Cairo, Egypt.

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

出版信息

Spectrochim Acta A Mol Biomol Spectrosc. 2014 Aug 14;129:84-95. doi: 10.1016/j.saa.2014.02.110. Epub 2014 Mar 17.

Abstract

Charge transfer complexes of loperamide hydrochloride (LOP.HCl) and trimebutine (TB) drugs as electron donor with 2,3-dichloro-5,6-dicyano-p-benzoquinone (DDQ), tetracyanoethylene (TCNE) and 7,7,8,8-tetracyanoquinodimethane (TCNQ) as π-acceptors in acetonitrile were investigated spectrophotometrically to determine the cited drugs in pure and dosage forms. The reaction gives highly coloured complex species which are measured spectrophotometrically at 460, 415 and 842nm in case of LOP.HCl and at 455, 414 and 842nm in case of TB using DDQ, TCNE and TCNQ reagents, respectively. The optimum experimental conditions have been studied carefully and optimized. Beer's law was obeyed over the concentration ranges of 47.70-381.6, 21.50-150.5 and 10.00-100.0μgmL(-1) for LOP.HCl and 37.85-264.9, 38.75-310.0 and 7.75-155.0μgmL(-1) for TB using DDQ, TCNE and TCNQ reagents, respectively. Sandell sensitivity, standard deviation, relative standard deviation, limit of detection and quantification were calculated. The obtained data refer to high accuracy and precision of the proposed method. These results are also confirmed by inter and intra-day precision with percent recovery of 99.18-101.1% and 99.32-101.4% in case of LOP.HCl and 98.00-102.0% and 97.50-101.4% in case of TB using DDQ, TCNE and TCNQ reagents for intra- and inter-day, respectively. These data were compared with those obtained using official methods for the determination of the cited drugs. The stability constants of the CT complexes were determined. The final products of the reaction were isolated and characterized using FT-IR, (1)H NMR, elemental analysis and thermogravimetric analysis (TG). The stoichiometry and apparent formation constant of the complexes formed were determined by applying the conventional spectrophotometric molar ratio method.

摘要

洛哌丁胺盐酸盐 (LOP.HCl) 和曲美布汀 (TB) 药物与 2,3-二氯-5,6-二氰对苯醌 (DDQ)、四氰乙烯 (TCNE) 和 7,7,8,8-四氰基对醌二甲烷 (TCNQ) 的荷转移络合物作为电子供体在乙腈中进行了光谱研究,以确定纯品和制剂中的这些药物。反应生成高色络合物,分别使用 DDQ、TCNE 和 TCNQ 试剂,在 460、415 和 842nm 处测定 LOP.HCl 的光谱,在 455、414 和 842nm 处测定 TB 的光谱。仔细研究并优化了最佳实验条件。LOP.HCl 在 47.70-381.6、21.50-150.5 和 10.00-100.0μgmL(-1)范围内,TB 在 37.85-264.9、38.75-310.0 和 7.75-155.0μgmL(-1)范围内,DDQ、TCNE 和 TCNQ 试剂的浓度范围内均符合比尔定律。计算了桑德尔灵敏度、标准偏差、相对标准偏差、检出限和定量限。所得到的数据表明该方法具有高精度和高重现性。这些结果也通过日内和日间精密度得到证实,LOP.HCl 的回收率为 99.18-101.1%和 99.32-101.4%,TB 的回收率为 98.00-102.0%和 97.50-101.4%,分别使用 DDQ、TCNE 和 TCNQ 试剂进行日内和日间。这些数据与用于测定这些药物的官方方法获得的数据进行了比较。测定了 CT 络合物的稳定常数。反应的最终产物使用傅里叶变换红外光谱 (FT-IR)、(1)H NMR、元素分析和热重分析 (TG) 进行了分离和表征。通过应用常规分光光度摩尔比法确定了形成的络合物的化学计量和表观形成常数。

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