Article (Scientific journals)
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
Christiaens, B.; Fillet, Marianne; Chiap, Patrice et al.
2004In Journal of Chromatography. A, 1056 (1-2), p. 105-110
Peer Reviewed verified by ORBi
 

Files


Full Text
articleJChromA1056_2004.pdf
Publisher postprint (127.5 kB)
Request a copy

All documents in ORBi are protected by a user license.

Send to



Details



Keywords :
validation; mass spectrometry; cyproterone acetate
Abstract :
[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).
Disciplines :
Chemistry
Biochemistry, biophysics & molecular biology
Author, co-author :
Christiaens, B.
Fillet, Marianne ;  Université de Liège - ULiège > Département de pharmacie > Analyse des médicaments
Chiap, Patrice ;  Université de Liège - ULiège > Département de pharmacie > Analyse des médicaments
Rbeida, O.
Ceccato, Attilio ;  Université de Liège - ULiège > Département de pharmacie
Streel, B.
De Graeve, Jean ;  Université de Liège - ULiège > Services généraux (Faculté de médecine) > Relations académiques et scientifiques (Médecine)
Crommen, Jacques ;  Université de Liège - ULiège > Département de pharmacie > Analyse des médicaments
Hubert, Philippe  ;  Université de Liège - ULiège > Chimie analytique
Language :
English
Title :
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
Publication date :
12 November 2004
Journal title :
Journal of Chromatography. A
ISSN :
0021-9673
eISSN :
1873-3778
Publisher :
Elsevier Science Bv, Amsterdam, Netherlands
Volume :
1056
Issue :
1-2
Pages :
105-110
Peer reviewed :
Peer Reviewed verified by ORBi
Available on ORBi :
since 03 May 2010

Statistics


Number of views
47 (3 by ULiège)
Number of downloads
0 (0 by ULiège)

Scopus citations®
 
34
Scopus citations®
without self-citations
31
OpenCitations
 
6

Bibliography


Similar publications



Contact ORBi