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Optimization of the Separation of Ephedrine, Pseudoephedrine, Phenylephrine, and Synephrine by Hydrophilic Interaction Liquid Chromatography Employing Experimental Design Methodology

Authorized Users Only
2015
Authors
Jovanović, Marko
Rakić, Tijana
Ivanović, Darko
Jančić-Stojanović, Biljana
Article (Published version)
Metadata
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Abstract
Hydrophilic interaction liquid chromatography (HILIC) has emerged as an alternative separation technique for small polar compounds. Design of Experiments (DoE) methodology in the analysis of the retention behavior and method development have been shown to be successful. This article addresses the retention behavior and optimization of chromatographic separation of a model mixture consisting of four sympathomimetic drugs (ephedrine, pseudoephedrine, phenylephrine, synephrine), on a bare silica column by HILIC. The acetonitrile content, pH of the aqueous phase, and concentration of ammonium acetate in aqueous phase were optimized according to the matrix of Box-Behnken design, and retention data were fitted to second-order polynomial models. The obtained coefficients of determination R-2 were higher than 0.990 and adjusted R-2 exceeded 0.972, while the lowest value for Predicted R-2 was 0.845. Beside of statistical analysis, graphical estimation of retention behavior was performed. In ord...er to optimize the separation, indirect modeling of selectivity factors of critical peak pairs (the diastereoisomers ephedrine/pseudoephedrine and the positional isomers phenylephrine/synephrine) and grid point search approach were employed. After the development of the grids, optimal chromatographic conditions were selected (acetonitrile content 91%, pH of the aqueous phase 4.5 and ammonium acetate concetration 35mmolL(-1)), providing a total analysis time of 14min.

Keywords:
method optimization / sympathomimetic drugs / hydrophilic interaction liquid chromatography / design of experiments
Source:
Instrumentation Science & Technology, 2015, 43, 2, 156-169
Publisher:
  • Taylor & Francis Inc, Philadelphia
Projects:
  • Modelling of different chromatographic systems with chemometrical approach in pharmaceutical analysis (RS-172052)

DOI: 10.1080/10739149.2014.910670

ISSN: 1073-9149

WoS: 000348320100003

Scopus: 2-s2.0-84921520297
[ Google Scholar ]
5
3
URI
http://farfar.pharmacy.bg.ac.rs/handle/123456789/2400
Collections
  • Radovi istraživača / Researchers’ publications
Institution
Pharmacy
TY  - JOUR
AU  - Jovanović, Marko
AU  - Rakić, Tijana
AU  - Ivanović, Darko
AU  - Jančić-Stojanović, Biljana
PY  - 2015
UR  - http://farfar.pharmacy.bg.ac.rs/handle/123456789/2400
AB  - Hydrophilic interaction liquid chromatography (HILIC) has emerged as an alternative separation technique for small polar compounds. Design of Experiments (DoE) methodology in the analysis of the retention behavior and method development have been shown to be successful. This article addresses the retention behavior and optimization of chromatographic separation of a model mixture consisting of four sympathomimetic drugs (ephedrine, pseudoephedrine, phenylephrine, synephrine), on a bare silica column by HILIC. The acetonitrile content, pH of the aqueous phase, and concentration of ammonium acetate in aqueous phase were optimized according to the matrix of Box-Behnken design, and retention data were fitted to second-order polynomial models. The obtained coefficients of determination R-2 were higher than 0.990 and adjusted R-2 exceeded 0.972, while the lowest value for Predicted R-2 was 0.845. Beside of statistical analysis, graphical estimation of retention behavior was performed. In order to optimize the separation, indirect modeling of selectivity factors of critical peak pairs (the diastereoisomers ephedrine/pseudoephedrine and the positional isomers phenylephrine/synephrine) and grid point search approach were employed. After the development of the grids, optimal chromatographic conditions were selected (acetonitrile content 91%, pH of the aqueous phase 4.5 and ammonium acetate concetration 35mmolL(-1)), providing a total analysis time of 14min.
PB  - Taylor & Francis Inc, Philadelphia
T2  - Instrumentation Science & Technology
T1  - Optimization of the Separation of Ephedrine, Pseudoephedrine, Phenylephrine, and Synephrine by Hydrophilic Interaction Liquid Chromatography Employing Experimental Design Methodology
VL  - 43
IS  - 2
SP  - 156
EP  - 169
DO  - 10.1080/10739149.2014.910670
ER  - 
@article{
author = "Jovanović, Marko and Rakić, Tijana and Ivanović, Darko and Jančić-Stojanović, Biljana",
year = "2015",
url = "http://farfar.pharmacy.bg.ac.rs/handle/123456789/2400",
abstract = "Hydrophilic interaction liquid chromatography (HILIC) has emerged as an alternative separation technique for small polar compounds. Design of Experiments (DoE) methodology in the analysis of the retention behavior and method development have been shown to be successful. This article addresses the retention behavior and optimization of chromatographic separation of a model mixture consisting of four sympathomimetic drugs (ephedrine, pseudoephedrine, phenylephrine, synephrine), on a bare silica column by HILIC. The acetonitrile content, pH of the aqueous phase, and concentration of ammonium acetate in aqueous phase were optimized according to the matrix of Box-Behnken design, and retention data were fitted to second-order polynomial models. The obtained coefficients of determination R-2 were higher than 0.990 and adjusted R-2 exceeded 0.972, while the lowest value for Predicted R-2 was 0.845. Beside of statistical analysis, graphical estimation of retention behavior was performed. In order to optimize the separation, indirect modeling of selectivity factors of critical peak pairs (the diastereoisomers ephedrine/pseudoephedrine and the positional isomers phenylephrine/synephrine) and grid point search approach were employed. After the development of the grids, optimal chromatographic conditions were selected (acetonitrile content 91%, pH of the aqueous phase 4.5 and ammonium acetate concetration 35mmolL(-1)), providing a total analysis time of 14min.",
publisher = "Taylor & Francis Inc, Philadelphia",
journal = "Instrumentation Science & Technology",
title = "Optimization of the Separation of Ephedrine, Pseudoephedrine, Phenylephrine, and Synephrine by Hydrophilic Interaction Liquid Chromatography Employing Experimental Design Methodology",
volume = "43",
number = "2",
pages = "156-169",
doi = "10.1080/10739149.2014.910670"
}
Jovanović M, Rakić T, Ivanović D, Jančić-Stojanović B. Optimization of the Separation of Ephedrine, Pseudoephedrine, Phenylephrine, and Synephrine by Hydrophilic Interaction Liquid Chromatography Employing Experimental Design Methodology. Instrumentation Science & Technology. 2015;43(2):156-169
Jovanović, M., Rakić, T., Ivanović, D.,& Jančić-Stojanović, B. (2015). Optimization of the Separation of Ephedrine, Pseudoephedrine, Phenylephrine, and Synephrine by Hydrophilic Interaction Liquid Chromatography Employing Experimental Design Methodology.
Instrumentation Science & TechnologyTaylor & Francis Inc, Philadelphia., 43(2), 156-169.
https://doi.org/10.1080/10739149.2014.910670
Jovanović Marko, Rakić Tijana, Ivanović Darko, Jančić-Stojanović Biljana, "Optimization of the Separation of Ephedrine, Pseudoephedrine, Phenylephrine, and Synephrine by Hydrophilic Interaction Liquid Chromatography Employing Experimental Design Methodology" 43, no. 2 (2015):156-169,
https://doi.org/10.1080/10739149.2014.910670 .

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