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使用溶剂改性剂改善传统反相柱中β-受体阻滞剂的峰形和分离性能。

Improvement of peak shape and separation performance of beta-blockers in conventional reversed-phase columns using solvent modifiers.

作者信息

Ruiz-Angel M J, Torres-Lapasió J R, Carda-Broch S, García-Alvarez-Coque M C

机构信息

Departament de Química Analítica, Facultat de Química, Universitat de València, Dr. Moliner 50, 46100 Burjassot (València), Spain.

出版信息

J Chromatogr Sci. 2003 Aug;41(7):350-8. doi: 10.1093/chromsci/41.7.350.

Abstract

A comparative study of peak shape, elution behavior, and resolution of 16 beta-blockers (acebutolol, alprenolol, atenolol, bisoprolol, carteolol, celiprolol, esmolol, labetalol, metoprolol, nadolol, oxprenolol, pindolol, practolol, propranolol, sotalol, and timolol) chromatographed with hybrid mobile phases of triethylamine (TEA)-acetonitrile and sodium dodecyl sulfate (SDS)-propanol is performed using conventional reversed-phase columns and isocratic elution. Both solvent modifiers (TEA and SDS) prevent the interaction of the basic drugs with the alkyl-bonded phase. However, the protection mechanisms of silanols on the packing are different. Whereas TEA associates with the silanol sites (blocking ion-exchange processes or repelling the solutes), the long hydrophobic chain of SDS is inserted in the bonded organic layer with the sulfate group protruding outside, which makes the stationary phase negatively charged. The effects of TEA, acetonitrile, SDS, and propanol on the elution strength, efficiency, peak asymmetry, and resolution are examined under an experimental design basis that is assisted by computer simulation to reach more general conclusions. The combination of improved peak shapes, larger selectivity, and a smaller range in retention among compounds of extreme polarity leads to the observation that a greater number of beta-blockers can be resolved with a hybrid micellar system.

摘要

使用常规反相柱和等度洗脱,对16种β受体阻滞剂(醋丁洛尔、阿普洛尔、阿替洛尔、比索洛尔、卡替洛尔、塞利洛尔、艾司洛尔、拉贝洛尔、美托洛尔、纳多洛尔、氧烯洛尔、吲哚洛尔、普拉洛尔、普萘洛尔、索他洛尔和噻吗洛尔)在三乙胺(TEA)-乙腈和十二烷基硫酸钠(SDS)-丙醇混合流动相下的色谱峰形状、洗脱行为和分离度进行了比较研究。两种溶剂改性剂(TEA和SDS)都能防止碱性药物与烷基键合相相互作用。然而,硅醇对填料的保护机制不同。TEA与硅醇位点结合(阻断离子交换过程或排斥溶质),而SDS的长疏水链插入键合有机层,硫酸根基团突出在外,使固定相带负电。在计算机模拟辅助的实验设计基础上,研究了TEA、乙腈、SDS和丙醇对洗脱强度、效率、峰不对称性和分离度的影响,以得出更普遍的结论。改进的峰形、更大的选择性以及极性极端的化合物之间保留时间范围更小,这些因素共同导致了这样的观察结果:使用混合胶束系统可以分离出更多的β受体阻滞剂。

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