title: Simultaneous determination of pirlindole enantiomers and dehydropirlindole by chiral liquid chromatography.
abstract: Liquid chromatography was employed for the determination of pirlindole enantiomers and its oxidation product dehydropirlindole (DHP). The direct separation of pirlindole enantiomers and DHP was achieved on a cellulose tris-(3,5-dimethylphenylcarbamate) chiral stationary phase (Chiralcel OD-R). Acetonitrile was used as the organic modifier and sodium perchlorate was used as an ionic additive in the mobile phase. The influence of acetonitrile and sodium perchlorate concentrations on enantioselectivity and achiral selectivity towards DHP was investigated in order to find suitable conditions for the determination of low amounts of each analyte. The mobile phase selected consisted of a mixture of acetonitrile and phosphate buffer (pH 5.0) containing sodium perchlorate (0.05 M) (35:65, v/v) and the UV detector was set at 220 nm. The method developed was validated and was found to be linear in the 0.1-5 microg ml(-1) range (r2 = 0.999 for the three compounds). Repeatability and the intermediate precision for the three analytes at a concentration of 0.1 microg ml(-1) were about 3 and 4%, respectively. This concentration corresponds to the quantification of 0.1% for the minor enantiomer. Actual determinations of enantiomeric purity for single enantiomers of pirlindole were performed.
authors.affiliation: Laboratory of Drug Analysis, Institute of Pharmacy, University of Liège, CHU B-36, Belgium.
authors.forename: A
authors.initials: A
authors.lastname: Ceccato
authors.forename: P
authors.initials: P
authors.lastname: Hubert
authors.forename: P
authors.initials: P
authors.lastname: de Tullio
authors.forename: J F
authors.initials: JF
authors.lastname: Liégeois
authors.forename: M
authors.initials: M
authors.lastname: Stachow
authors.forename: J
authors.initials: J
authors.lastname: Géczy
authors.forename: J
authors.initials: J
authors.lastname: Crommen
mesh_terms: D000097:Acetonitriles / Q000737:chemistry; D002227:Carbazoles / Q000032:analysis*; D002623:Chemistry Techniques, Analytical / Q000379:methods*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004340:Drug Contamination; D015394:Molecular Structure; D010472:Perchlorates / Q000737:chemistry; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D017670:Sodium Compounds / Q000737:chemistry; D013237:Stereoisomerism
chemical_list: D000097:Acetonitriles; D002227:Carbazoles; D010472:Perchlorates; D017670:Sodium Compounds; C067315:3,3a-dehydropyrazidol; C031068:sodium perchlorate; C009830:pirlindole; C032159:acetonitrile