ORBi: Chiap Patrice - Automated determination of pirlindole enantiomers in plasma by on-line coupling of a pre-column packed with restricted access material to a chiral liquid chromatographic column

Reference : Automated determination of pirlindole enantiomers in plasma by on-line coupling of a pre...


	Document type :	Scientific journals : Article
	Discipline(s) :	Human health sciences : Pharmacy, pharmacology & toxicology Physical, chemical, mathematical & earth Sciences : Chemistry
	To cite this reference:	http://hdl.handle.net/2268/4190

Title :	Automated determination of pirlindole enantiomers in plasma by on-line coupling of a pre-column packed with restricted access material to a chiral liquid chromatographic column
Language :	English
Author, co-author :	Chiap, Patrice [Université de Liège - ULg > Département de pharmacie > Analyse des médicaments >]
	Ceccato, Attilio [Université de Liège - ULg > Département de pharmacie > Analyse des médicaments >]
	Gora, R. [> > > >]
	Hubert, Philippe [Université de Liège - ULg > > Chimie analytique >]
	Geczy, J. [> > > >]
	Crommen, Jacques [Université de Liège - ULg > Département de pharmacie > Analyse des médicaments >]
Publication date :	15-Jan-2002
Journal title :	Journal of Pharmaceutical & Biomedical Analysis
Publisher :	Pergamon-Elsevier Science Ltd
Volume :	27
Issue/season :	3-4
Pages :	447-455
Audience :	International
ISSN :	0731-7085
City :	Oxford
Keywords :	[en] pirlindole enantiomers ; chiral liquid chromatography ; plasma ; sample preparation ; column-switching ; restricted access material
Abstract :	[en] A fully automated liquid chromatographic method has been developed for the determination of the enantiomers of pirlindole, an antidepressant drug, in human plasma. The method is based on the use of a pre-column packed with restricted access material (RAM) (LiChrospher ADS RP-4) for sample clean-up coupled to a column containing a cellulose tris-(3,5-dimethylphenylcarbamate) based chiral stationary phase (Chiralcel OD-R) for the separation and quantitative analysis of pirlindole enantiomers. A 50-microl plasma volume was injected directly onto the pre-column using a mixture of phosphate buffer (pH 5.0) and methanol (97:3; v/v) as washing liquid. By rotation of a switching valve, the analytes were then eluted in the back-flush mode with the LC mobile phase. A complete separation of pirlindole enantiomers was obtained in 22 min on the Chiralcel OD-R column, using a mobile phase made of a mixture of phosphate buffer (pH 5.0) containing 50 mM sodium perchlorate and acetonitrile (65:35; v/v). The flow-rate was 0.6 ml/min and the analytes were detected fluorometrically using 295 and 340 nm as excitation and emission wavelengths, respectively. The method was then validated and was found to be linear in the 2.5-200 ng/ml range. The limit of detection was lower than 1 ng/ml. Repeatability and intermediate precision at a concentration of 50 ng/ml were about 1.5 and 3.5%, respectively.
Permalink :	http://hdl.handle.net/2268/4190

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