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Possibilities of column coupling electrophoresis provided with a fiber-based diode array detection in enantioselective analysis of drugs in pharmaceutical and clinical samples.
J Chromatogr A. 2008 Jan 25; 1179(1):9-16.JC

Abstract

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. Isotachophoresis (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.

Authors+Show Affiliations

Department of Pharmaceutical Analysis and Nuclear Pharmacy, Faculty of Pharmacy, Comenius University, Odbojárov 10, Bratislava, Slovak Republic. mikus@fpharm.uniba.skNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article
Research Support, Non-U.S. Gov't

Language

eng

PubMed ID

17905259

Citation

Mikus, Peter, et al. "Possibilities of Column Coupling Electrophoresis Provided With a Fiber-based Diode Array Detection in Enantioselective Analysis of Drugs in Pharmaceutical and Clinical Samples." Journal of Chromatography. A, vol. 1179, no. 1, 2008, pp. 9-16.
Mikus P, Maráková K, Marák J, et al. Possibilities of column coupling electrophoresis provided with a fiber-based diode array detection in enantioselective analysis of drugs in pharmaceutical and clinical samples. J Chromatogr A. 2008;1179(1):9-16.
Mikus, P., Maráková, K., Marák, J., Kaniansky, D., Valásková, I., & Havránek, E. (2008). Possibilities of column coupling electrophoresis provided with a fiber-based diode array detection in enantioselective analysis of drugs in pharmaceutical and clinical samples. Journal of Chromatography. A, 1179(1), 9-16.
Mikus P, et al. Possibilities of Column Coupling Electrophoresis Provided With a Fiber-based Diode Array Detection in Enantioselective Analysis of Drugs in Pharmaceutical and Clinical Samples. J Chromatogr A. 2008 Jan 25;1179(1):9-16. PubMed PMID: 17905259.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Possibilities of column coupling electrophoresis provided with a fiber-based diode array detection in enantioselective analysis of drugs in pharmaceutical and clinical samples. AU - Mikus,Peter, AU - Maráková,Katarína, AU - Marák,Jozef, AU - Kaniansky,Dusan, AU - Valásková,Iva, AU - Havránek,Emil, Y1 - 2007/09/14/ PY - 2007/07/04/received PY - 2007/08/30/revised PY - 2007/09/03/accepted PY - 2007/10/2/pubmed PY - 2008/4/5/medline PY - 2007/10/2/entrez SP - 9 EP - 16 JF - Journal of chromatography. A JO - J Chromatogr A VL - 1179 IS - 1 N2 - 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. Isotachophoresis (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. SN - 0021-9673 UR - https://www.unboundmedicine.com/medline/citation/17905259/Possibilities_of_column_coupling_electrophoresis_provided_with_a_fiber_based_diode_array_detection_in_enantioselective_analysis_of_drugs_in_pharmaceutical_and_clinical_samples_ DB - PRIME DP - Unbound Medicine ER -