Reference : Determination of enantiomeric purity of S-amlodipine by chiral LC with emphasis on re...
Scientific journals : Article
Human health sciences : Pharmacy, pharmacology & toxicology
http://hdl.handle.net/2268/105128
Determination of enantiomeric purity of S-amlodipine by chiral LC with emphasis on reversal of enantiomer elution order.
English
Dossou, Katina Sourou Sylvestre [Université de Liège - ULg > Département de pharmacie > Analyse des médicaments]
Edorh, P. A. [> > > >]
Chiap, Patrice mailto [Université de Liège - ULg > Département de pharmacie > Département de pharmacie]
Chankvetadze, B. [> > > >]
Servais, Anne-Catherine mailto [Université de Liège - ULg > Département de pharmacie > Analyse des médicaments]
Fillet, Marianne mailto [Université de Liège - ULg > Département de pharmacie > Analyse des médicaments]
Crommen, Jacques mailto [Université de Liège - ULg > Département de pharmacie > Département de pharmacie]
2011
Journal of Separation Science
Wiley-VCH Verlag Gmbh
34
1772-1780
Yes (verified by ORBi)
International
1615-9306
1615-9314
Weinheim
Germany
[en] An LC method was developed and prevalidated for the enantiomeric purity determination of S-amlodipine in polar organic solvent chromatography using a chlorine-containing cellulose-based chiral stationary phase (CSP). The concentration of formic acid (FA) (0.01-0.2%) in the mobile phase containing acetonitrile as the main solvent was found to influence the elution order of amlodipine enantiomers as well as the enantioresolution. A reversal of the enantiomer elution order of amlodipine was only observed with chiral stationary phases with both electron-withdrawing (chloro) and electron-donating groups (methyl) on the phenyl moieties of the chiral selector, namely cellulose tris(3-chloro-4-methylphenylcarbamate) and cellulose tris(4-chloro-3-methylphenylcarbamate). The highest enantioresolution (R(s) : 4.1) value was obtained at the lowest FA concentration (0.01%) using cellulose tris(4-chloro-3-methylphenylcarbamate) as the chiral selector and the enantiomeric impurity, R-amlodipine, eluted first under these conditions. Therefore, the mobile phase selected for the prevalidation of the method consisted of ACN/0.1% DEA/0.01% FA and the temperature was set at 25 degrees C. The method was prevalidated by means of the strategy based on the total measurement error and the accuracy profile. The method was found to be selective and the limit of quantification was found to be about 0.05% for R-amlodipine, while the limit of detection was close to 0.02%.
http://hdl.handle.net/2268/105128
10.1002/jssc.201100339
Copyright (c) 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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