Reference : Development and validation of a nonaqueous capillary electrophoretic method for the e...
Scientific journals : Article
Human health sciences : Pharmacy, pharmacology & toxicology
http://hdl.handle.net/2268/67945
Development and validation of a nonaqueous capillary electrophoretic method for the enantiomeric purity determination of a synthetic intermediate of new 3,4-dihydro-2,2-dimethyl-2H-1-benzopyrans using a single-isomer anionic cyclodextrin derivative and an ionic liquid
English
Rousseau, Anne mailto [Université de Liège - ULg > Département de pharmacie > Analyse des médicaments >]
Florence, Xavier mailto [Université de Liège - ULg > > > Doct. sc. bioméd. & pharma. (Bologne)]
Pirotte, Bernard mailto [Université de Liège - ULg > Département de pharmacie > Chimie pharmaceutique >]
Varenne, Anne [> >]
Gareil, Pierre [> >]
Villemin, Didier [> >]
Chiap, Patrice mailto [Université de Liège - ULg > > Pharmacologie clinique >]
Crommen, Jacques mailto [Université de Liège - ULg > Département de pharmacie > Analyse des médicaments >]
Fillet, Marianne mailto [Université de Liège - ULg > Département de pharmacie > Analyse des médicaments >]
Servais, Anne-Catherine mailto [Université de Liège - ULg > Département de pharmacie > Analyse des médicaments >]
2010
Journal of Chromatography. A
Elsevier Science
1217
51
7949-55
Yes (verified by ORBi)
International
0021-9673
Amsterdam
The Netherlands
[en] Nonaqueous capillary electrophoresis ; Single-isomer anionic cyclodextrins ; Ionic liquid ; Benzopyran derivatives ; Enantiomeric purity
[en] The enantiomeric purity determination of a synthetic intermediate of new 3,4-dihydro-2,2-dimethyl-2H-1-benzopyrans, i.e. 4-amino-2,2-dimethyl-6-ethoxycarbonylamino-3,4-dihydro-2H-1-benzopyran, was successfully carried out using an anionic cyclodextrin (CD) derivative combined with a chiral ionic liquid (IL). In order to obtain high resolution and efficiency values, the addition of a chiral IL, i.e. ethylcholine bis(trifluoromethylsulfonyl)imide (EtChol NTf2), to the background electrolyte containing heptakis(2,3-di-O-methyl-6-O-sulfo)-β-CD (HDMS-β-CD) was found to be essential. A simultaneous increase in separation selectivity and enantioresolution seems to indicate a synergistic effect of HDMS-β-CD and EtChol NTf2. The best enantioseparation of the key intermediate was achieved using a methanolic solution of 0.75 M formic acid, 10 mM ammonium formate, 1.5 mM HDMS-β-CD and 5 mM EtChol NTf2. Levamisole was selected as internal standard. The optimized conditions allowed the determination of 0.1 % of each enantiomer in the presence of its stereoisomer using the method of standard additions. The NACE method was then fully validated with respect to selectivity, response function, trueness, precision, accuracy, linearity and limits of detection and quantification.
Fonds de la Recherche Scientifique (Communauté française de Belgique) - F.R.S.-FNRS ; Fonds Léon Fredericq
http://hdl.handle.net/2268/67945

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