Article (Scientific journals)
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
Rousseau, Anne; Florence, Xavier; Pirotte, Bernard et al.
2010In Journal of Chromatography. A, 1217 (51), p. 7949-55
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Keywords :
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.
Disciplines :
Pharmacy, pharmacology & toxicology
Author, co-author :
Rousseau, Anne ;  Université de Liège - ULiège > Département de pharmacie > Analyse des médicaments
Florence, Xavier ;  Université de Liège - ULiège > Doct. sc. bioméd. & pharma. (Bologne)
Pirotte, Bernard ;  Université de Liège - ULiège > Département de pharmacie > Chimie pharmaceutique
Varenne, Anne
Gareil, Pierre
Villemin, Didier
Chiap, Patrice ;  Université de Liège - ULiège > Pharmacologie clinique
Crommen, Jacques ;  Université de Liège - ULiège > Département de pharmacie > Analyse des médicaments
Fillet, Marianne ;  Université de Liège - ULiège > Département de pharmacie > Analyse des médicaments
Servais, Anne-Catherine  ;  Université de Liège - ULiège > Département de pharmacie > Analyse des médicaments
Language :
English
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
Publication date :
2010
Journal title :
Journal of Chromatography. A
ISSN :
0021-9673
eISSN :
1873-3778
Publisher :
Elsevier Science, Amsterdam, Netherlands
Volume :
1217
Issue :
51
Pages :
7949-55
Peer reviewed :
Peer Reviewed verified by ORBi
Funders :
F.R.S.-FNRS - Fonds de la Recherche Scientifique [BE]
Fonds Léon Fredericq [BE]
Available on ORBi :
since 09 August 2010

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