Possibilities of column coupling electrophoresis provided with a fiber-based diode array detection in enantio selective analysis of drugs in pharmaceutical and clinical samples

作     者：Mikus, Peter Marakova, Katarina Marak, Jozef Kaniansky, Dusan Valagkova, Iva Havranek, Emil 

作者机构：Comenius Univ Fac Pharm Dept Pharmaceut Anal & Nucl Pharm SK-83232 Bratislava Slovakia Comenius Univ Fac Nat Sci Dept Analyt Chem SK-84215 Bratislava Slovakia 

出 版 物：《JOURNAL OF CHROMATOGRAPHY A》 (色谱法杂志Ａ辑)

年 卷 期：2008年第1179卷第1期

页      面：9-16页

核心收录：

学科分类：0710[理学-生物学] 081704[工学-应用化学] 07[理学] 08[工学] 0817[工学-化学工程与技术] 070302[理学-分析化学] 0703[理学-化学] 

基　　金：Slovak Grant Agency for Science  (1/0003/08  1/2310/05  1/3558/06  1/4299/07  FaF UK/12/2006  FaF UK/19/2007) 

主　　题：isotachophoresis capillary zone electrophoresis column-coupling diode array detection drug charged cyclodextrin enantiomer purity pharmaceuticals clinical analysis multicomponent mixture 

摘      要：The present work illustrated possibilities of column coupling electrophoresis combined with ionizable chiral selector and diode array detection (DAD) for the enantioselective analysis of trace drugs (pheniramine and its analogs) in pharmaceutical and clinical samples. lsotachophoresis (ITP), on-line coupled with capillary zone electrophoresis (CZE), served as an ideal injection technique (high sample load capacity, narrow and sharp drugs zones) of on-line pretreated samples (preseparation, purification and preconcentration of drugs) for the CZE stage. Enhanced (enantio)separation selectivity of CZE with ionizable chiral selector (carboxyethyl-beta-cyclodextrin recognized between drugs enantiomers on one hand as well as between drugs and sample matrix constituents on the other hand) enabled to obtain pure zones of the drugs enantiomers, suitable for their detection and quantitation. DAD in comparison with single wavelength UV detection enhanced value of analytical information verifying purity of drugs enantiomers zones (indicating interferents with different spectra to those of drugs). Obtained results indicated pure zones of interest confirming effective ITP-CZE (enantio)separation process. Distinguishing the trace analytes signals superposed on the baseline noise was provided with sufficient reliability (for this purpose the background correction and smoothing procedure had to be applied to the raw DAD spectra). The proposed ITP-CZE-DAD methods were characterized by favorable performance parameters (sensitivity, linearity, precision, recovery, accuracy, robustness, selectivity) and successfully applied for (i) enantiomeric purity testing of dexbrompheniramine in commercial pharmaceutical tablets and (ii) enantioselective metabolic study of pheniramine in human urine. (c) 2007 Elsevier B.V. All rights reserved.