ORBi: Rousseau Anne - 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

Reference : Development and validation of a nonaqueous capillary electrophoretic method for the enan...


	Document type :	Scientific journals : Article
	Discipline(s) :	Human health sciences : Pharmacy, pharmacology & toxicology
	To cite this reference:	http://hdl.handle.net/2268/67945

Title :	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
Language :	English
Author, co-author :	Rousseau, Anne [Université de Liège - ULg > Département de pharmacie > Analyse des médicaments >]
	Florence, Xavier [Université de Liège - ULg > > > Doct. sc. bioméd. & pharma. (Bologne)]
	Pirotte, Bernard [Université de Liège - ULg > Département de pharmacie > Chimie pharmaceutique >]
	Varenne, Anne [ > > ]
	Gareil, Pierre [ > > ]
	Villemin, Didier [ > > ]
	Chiap, Patrice [Université de Liège - ULg > > Pharmacologie clinique >]
	Crommen, Jacques [Université de Liège - ULg > Département de pharmacie > Analyse des médicaments >]
	Fillet, Marianne [Université de Liège - ULg > Département de pharmacie > Analyse des médicaments >]
	Servais, Anne-Catherine [Université de Liège - ULg > Département de pharmacie > Analyse des médicaments >]
Publication date :	2010
Journal title :	Journal of Chromatography. A
Publisher :	Elsevier Science
Audience :	International
ISSN :	0021-9673
City :	Amsterdam
Country :	The Netherlands
Keywords :	[en] Nonaqueous capillary electrophoresis ; Single-isomer anionic cyclodextrins ; Ionic liquid ; Benzopyran derivatives ; Enantiomeric purity
Abstract :	[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.
Funders :	Fonds de la Recherche Scientifique (Communauté française de Belgique) - F.R.S.-FNRS ; Fonds Léon Fredericq
Permalink :	http://hdl.handle.net/2268/67945

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