Micke Gustavo Amadeu, Costa Ana Carolina O, Heller Melina, Barcellos Michelle, Piovezan Marcel, Caon Thiago, de Oliveira Marcone Augusto Leal
Department of Chemistry, Federal University of Santa Catarina, 88040-900 Florianopolis, SC, Brazil.
J Chromatogr A. 2009 Nov 6;1216(45):7957-61. doi: 10.1016/j.chroma.2009.08.083. Epub 2009 Sep 6.
The aim of this study was to develop a fast capillary electrophoresis method for the determination of propranolol in pharmaceutical preparations. In the method development the pH and constituents of the background electrolyte were selected using the effective mobility versus pH curves. Benzylamine was used as the internal standard. The background electrolyte was composed of 60mmolL(-1) tris(hydroxymethyl)aminomethane and 30mmolL(-1) 2-hydroxyisobutyric acid, at pH 8.1. Separation was conducted in a fused-silica capillary (32cm total length and 8.5cm effective length, 50microm I.D.) with a short-end injection configuration and direct UV detection at 214nm. The run time was only 14s. Three different strategies were studied in order to develop a fast CE method with low total analysis time for propranolol analysis: low flush time (Lflush) 35runs/h, without flush (Wflush) 52runs/h, and Invert (switched polarity) 45runs/h. Since the three strategies developed are statistically equivalent, Wflush was selected due to the higher analytical frequency in comparison with the other methods. A few figures of merit of the proposed method include: good linearity (R(2)>0.9999); limit of detection of 0.5mgL(-1); inter-day precision better than 1.03% (n=9) and recovery in the range of 95.1-104.5%.
本研究的目的是开发一种快速毛细管电泳法,用于测定药物制剂中的普萘洛尔。在方法开发过程中,利用有效迁移率与pH曲线选择背景电解质的pH值和成分。使用苄胺作为内标。背景电解质由60mmolL(-1)三(羟甲基)氨基甲烷和30mmolL(-1)2-羟基异丁酸组成,pH为8.1。在熔融石英毛细管(总长32cm,有效长度8.5cm,内径50μm)中进行分离,采用短端进样配置,并在214nm处进行直接紫外检测。运行时间仅为14秒。为了开发一种用于普萘洛尔分析的总分析时间短的快速毛细管电泳方法,研究了三种不同的策略:低冲洗时间(Lflush)35次/小时、无冲洗(Wflush)52次/小时和反向(切换极性)45次/小时。由于所开发的三种策略在统计学上等效,与其他方法相比,Wflush因分析频率更高而被选中。该方法的一些性能指标包括:良好的线性(R(2)>0.9999);检测限为0.5mgL(-1);日间精密度优于1.03%(n=9),回收率在95.1-104.5%范围内。