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胶束电动毛细管色谱法测定尿液中的十种β受体阻滞剂

Determination of ten beta-blockers in urine by micellar electrokinetic capillary chromatography.

作者信息

Lukkari P, Sirén H, Pantsar M, Riekkola M L

机构信息

Department of Chemistry, University of Helsinki, Finland.

出版信息

J Chromatogr. 1993 Feb 19;632(1-2):143-8. doi: 10.1016/0021-9673(93)80037-9.

DOI:10.1016/0021-9673(93)80037-9
PMID:8095937
Abstract

beta-Adrenergic blocking agents are of therapeutic value in the treatment of migraine and various cardiovascular disorders (angina pectoris, cardiac arrhythmia, hypertension). Owing to their sedative effect, they are also used as doping agents in sport. A characteristic feature of beta-blockers is the alkanolamine side-chain terminating in a secondary amino group. The pKa values vary from 9.2 to 9.8. Because some beta-blockers are hydrophilic and some lipophilic, simultaneous determination is difficult. In this work, a method based on micellar electrokinetic capillary chromatography (MECC) was developed for the separation and determination of beta-blockers. The 0.08 M phosphate buffer (pH 7.0) solution contained 10 mM N-cetyl-N,N,N-trimethylammonium bromide (CTAB). Ten parent beta-blockers in human urine could be separated in a single run and determined quantitatively by the internal standard (2,6-dimethylphenol) method. Neither endogenous compounds in urine nor caffeine and its metabolites interfered with the analysis. The clean-up procedure for urine consisted of a simple filtration through 0.5-microns PTFE membranes. The MECC method exhibited good repeatability and a linear range of 25-150 micrograms/ml. The method was applied to determination of oxprenolol in real samples.

摘要

β-肾上腺素能阻滞剂在偏头痛和各种心血管疾病(心绞痛、心律失常、高血压)的治疗中具有治疗价值。由于其镇静作用,它们也被用作体育运动中的兴奋剂。β-阻滞剂的一个特征是其链烷醇胺侧链以仲氨基结尾。其pKa值在9.2至9.8之间变化。由于一些β-阻滞剂是亲水性的,一些是亲脂性的,因此同时测定很困难。在这项工作中,开发了一种基于胶束电动毛细管色谱法(MECC)的方法用于β-阻滞剂的分离和测定。0.08M磷酸盐缓冲液(pH7.0)溶液含有10mM十六烷基三甲基溴化铵(CTAB)。人尿中的十种母体β-阻滞剂可以一次运行分离,并通过内标(2,6-二甲基苯酚)法定量测定。尿中的内源性化合物以及咖啡因及其代谢物均不干扰分析。尿液的净化程序包括通过0.5微米的聚四氟乙烯膜进行简单过滤。MECC方法具有良好的重复性,线性范围为25-150微克/毫升。该方法应用于实际样品中氧烯洛尔的测定。

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