Direct detection and quantification of 19-norandrosterone sulfate in human urine by liquid chromatography-linear ion trap mass spectrometry.

Détails

ID Serval
serval:BIB_C409EDAA168B
Type
Article: article d'un périodique ou d'un magazine.
Collection
Publications
Titre
Direct detection and quantification of 19-norandrosterone sulfate in human urine by liquid chromatography-linear ion trap mass spectrometry.
Périodique
Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences
Auteur(s)
Strahm E., Saudan C., Sottas P.E., Mangin P., Saugy M.
ISSN
1570-0232
Statut éditorial
Publié
Date de publication
2007
Peer-reviewed
Oui
Volume
852
Numéro
1-2
Pages
491-496
Langue
anglais
Résumé
19-Norandrosterone sulfate (19-NAS) is the sulfoconjugated form of 19-norandrosterone (19-NA), the major metabolite of the steroid nandrolone. A sensitive and accurate liquid chromatography/tandem mass spectrometry (LC-MS/MS) assay was developed for the direct measurement of 19-NAS in human urine samples. The method involved a quaternary amine SPE protocol and subsequently injection of the extract onto an analytical column (Uptisphere ODB, 150 mm x 3.0 mm, 5 microm) for chromatographic separation and mass spectrometry detection in negative electrospray ionisation mode. The sulfoconjugate of 19-NA was identified in urine by comparison of mass spectra and retention time with a reference substance. The limit of detection (LOD) and lowest limit of quantification (LLOQ) of 19-NAS were of 40 pg/mL and 200 pg/mL, respectively. For a nominal concentration of 2 ng/mL, recovery (94%), intra-day precision (2.7%), intra-assay precision (6.6%) and inter-assay precision (14.3%) were determined. Finally, this analytical method was applied for quantifying the concentration of 19-NAS in doping samples, using calibration curves (0.2-20 ng/mL) and the standard-addition method. The results show the feasibility of applying this LC-MS/MS assay as a complementary tool to detect misuse of nandrolone or nandrolone precursors.
Mots-clé
Chromatography, Liquid/methods, Estranes/urine, Humans, Reference Standards, Reproducibility of Results, Sensitivity and Specificity, Spectrometry, Mass, Electrospray Ionization/methods, Tandem Mass Spectrometry/methods
Pubmed
Web of science
Création de la notice
19/05/2008 12:00
Dernière modification de la notice
03/03/2018 21:12
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