Lukkari P, Nyman T, Riekkola M L
Department of Chemistry, University of Helsinki, Finland.
J Chromatogr A. 1994 Jul 15;674(1-2):241-6. doi: 10.1016/0021-9673(94)85229-4.
beta-Adrenergic blocking agents are used for the treatment of angina pectoris, cardiac arrhythmia, hypertension, anxiety attacks, thyrotoxicosis, migraine and glaucoma. Owing to their sedative effect, they are also used as doping agents in sport. All beta-blockers have an alkanol amine side chain terminating in a secondary amino group in their structure. 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 in serum. The phosphate buffer 0.08 M (pH 6.7) solution contained 15 mM N-cetyl-N,N,N-trimethylammonium bromide. Nine parent beta-blockers could be separated in a single run and the concentrations determined by internal standard (ephedrine) method. The simple clean-up procedure consisted of enzyme hydrolysis (Helix pomatia), protein precipitation, and filtration through 0.5-microns PTFE membranes. The MECC method exhibited good repeatability and a linear range of 75-300 micrograms/ml. The method was successfully applied after concentration to the determination of propranolol in real samples.
β-肾上腺素能阻滞剂用于治疗心绞痛、心律失常、高血压、焦虑症发作、甲状腺毒症、偏头痛和青光眼。由于其镇静作用，它们还被用作体育运动中的兴奋剂。所有β-阻滞剂在其结构中都有一个以仲氨基结尾的链烷醇胺侧链。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，用于血清中β-阻滞剂的分离和测定。0.08 M（pH 6.7）的磷酸盐缓冲溶液含有15 mM N-十六烷基-N，N，N-三甲基溴化铵。九种母体β-阻滞剂可以在一次运行中分离出来，并通过内标（麻黄碱）法测定浓度。简单的净化程序包括酶水解（海螺酶）、蛋白质沉淀和通过0.5微米聚四氟乙烯膜过滤。MECC方法具有良好的重复性，线性范围为75-300微克/毫升。该方法在浓缩后成功应用于实际样品中普萘洛尔的测定。
