Reference : Fully automated method for the liquid chromatographic-tandem mass spectrometric determin...
Scientific journals : Article
Human health sciences : Pharmacy, pharmacology & toxicology
http://hdl.handle.net/2268/22562
Fully automated method for the liquid chromatographic-tandem mass spectrometric determination of cyproterone acetate in human plasma using restricted access material for on-line sample clean-up.
English
Christians, Benoit [Université de Liège - ULG > Analyse des Médicaments > > >]
Fillet, Marianne mailto [Université de Liège - ULg > Département de pharmacie > Analyse des médicaments >]
Chiap, Patrice [Centre Hospitalier Universitaire de Liège - CHU > > Pharmacologie clinique >]
Rbeida, Omar [Université de Liège - ULG > Analyse des médicaments > > >]
Ceccato, Attilio mailto [Université de Liège - ULg > Département de pharmacie > Analyse des médicaments >]
Streel, Bruno [SMB > > > > > >]
De Graeve, Jean mailto [Université de Liège - ULg > Services généraux (Faculté de médecine) > Relations académiques et scientifiques (Médecine) >]
Crommen, Jacques mailto [Université de Liège - ULg > Département de pharmacie > Analyse des médicaments >]
Hubert, Philippe mailto [Université de Liège - ULg > Département de pharmacie > Analyse des médicaments > >]
2004
Journal of Chromatography. A
Elsevier Science
1056
1-2
105-10
Yes (verified by ORBi)
International
0021-9673
Amsterdam
The Netherlands
[en] Automation ; Chromatography, Liquid/methods ; Cyproterone Acetate/blood ; Humans ; Reference Standards ; Reproducibility of Results ; Sensitivity and Specificity ; Spectrometry, Mass, Electrospray Ionization/methods
[en] A new automated method for the quantitative analysis of cyproterone acetate (CPA) in human plasma has been developed using on-line solid phase extraction (SPE) prior to the LC-MS/MS determination. The method was based on the use of a pre-column packed with internal-surface reversed-phase material (LiChrospher RP-4 ADS, 25 mm x 2 mm) for sample clean-up coupled to LC separation on an octadecyl silica stationary phase by means of a column switching system. A 30 microl plasma sample volume was injected directly onto the pre-column using a mixture of water, acetonitrile and formic acid (90:10:0.1 (v/v/v)) adjusted to pH 4.0 with diluted ammonia as washing liquid. The analyte was then eluted in the back-flush mode with the LC mobile phase consisting of water, methanol and formic acid (10:90:0.1 (v/v/v)). The dispensing flow rates of the washing liquid and the LC mobile phase were 300 microl min(-1). Medroxyprogesterone acetate (MPA) was used as internal standard. The MS ionization of the analytes was achieved using electrospray (ESI) in the positive ion mode. The pseudomolecular ionic species of CPA and MPA (417.4 and 387.5) were selected to generate daughter ions at 357.4 and 327.5, respectively. Finally, the developed method was validated according to a new approach using accuracy profiles as a decision tool. Very good results with respect to accuracy, detectability, repeatability, intermediate precision and selectivity were obtained. The LOQ of cyproterone acetate was 300 pg ml(-1).
FNRS
Researchers ; Professionals ; Students
http://hdl.handle.net/2268/22562

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