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分光光度法测定药物制剂中的β-肾上腺素能阻滞剂

Spectrophotometric determination of beta-adrenergic blocking agents in pharmaceutical formulations.

作者信息

Salem Hesham

机构信息

Analytical Chemistry Department, Faculty of Pharmacy, Minia University, Minia, Egypt.

出版信息

J Pharm Biomed Anal. 2002 Jul 1;29(3):527-38. doi: 10.1016/s0731-7085(02)00100-0.

Abstract

Simple, rapid and sensitive spectrophotometric procedures were developed for the analysis of atenolol, timolol maleate, propranolol hydrochloride, metoprolol tartarate, betaxolol hydrochloride, levobunolol hydrochloride and bisprolol fumarate in pure form as well as in their pharmaceutical formulations. The methods are based on the reaction of these drugs as n-electron donors with the sigma-acceptor iodine, and the pi-acceptors: 7,7,8,8-tetracyanoquinodimethane, 2,3-dichloro-5,6-dicyano-1,4-benzoquinone, tetracyanoethylene, 2,3,5,6-tetrabromo-1,4-benzoquinone (bromanil) and 2,3,5,6-tetrachloro-1,4-benzoquinone (chloranil). The obtained charge-transfer complexes were measured at 365 nm for iodine (in 1,2-dichloroethane), at 840, 420, and 470 nm for 7,7,8,8-tetracyan-oquinodimethane, tetracyanoethylene and 2,3-di-chloro-5,6-dicyano-1,4-benzoquinone (in acetonitrile), respectively, and at 450 and 440 nm for bromanil and chloranil (in ethanol), respectively. Due to the rapid development of colors at ambient temperature, the obtained results were used on thin-layer chromatograms for the detection of the investigated drugs. Beer's plots were obeyed in a general concentration range of 4-120 microg ml(-1) with correlation coefficients not less than 0.9991. The proposed procedures could be applied successfully to the determination of the investigated drugs in tablets and ophthalmic solutions with good recovery; percent ranged from 98.03+/-0.98 to 100.30+/-0.90. The association constants and standard free energy changes using Benesi-Hildebrand plots were studied.

摘要

开发了简单、快速且灵敏的分光光度法,用于分析阿替洛尔、马来酸噻吗洛尔、盐酸普萘洛尔、酒石酸美托洛尔、盐酸倍他洛尔、盐酸左布诺洛尔和富马酸比索洛尔的纯品及其药物制剂。这些方法基于这些药物作为n电子供体与σ受体碘以及π受体:7,7,8,8-四氰基对苯二醌、2,3-二氯-5,6-二氰基-1,4-苯醌、四氰基乙烯、2,3,5,6-四溴-1,4-苯醌(四溴苯醌)和2,3,5,6-四氯-1,4-苯醌(四氯苯醌)的反应。所形成的电荷转移络合物在365nm处测定碘(在1,2-二氯乙烷中),在840、420和470nm处分别测定7,7,8,8-四氰基对苯二醌、四氰基乙烯和2,3-二氯-5,6-二氰基-1,4-苯醌(在乙腈中),在450和440nm处分别测定四溴苯醌和四氯苯醌(在乙醇中)。由于在室温下颜色迅速形成,所得结果用于薄层色谱图上以检测所研究的药物。在4 - 120μg ml⁻¹的一般浓度范围内符合比尔定律,相关系数不小于0.9991。所提出的方法可成功应用于片剂和眼用溶液中所研究药物的测定,回收率良好;百分比范围为98.03±0.98至100.30±0.90。使用贝内西 - 希尔德布兰德图研究了缔合常数和标准自由能变化。

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