Titre
Direct detection and quantification of 19-norandrosterone sulfate in human urine by liquid chromatography-linear ion trap mass spectrometry.
Type
article
Institution
Externe
Périodique
Auteur(s)
Strahm, E.
Auteure/Auteur
Saudan, C.
Auteure/Auteur
Sottas, P.E.
Auteure/Auteur
Mangin, P.
Auteure/Auteur
Saugy, M.
Auteure/Auteur
Liens vers les personnes
ISSN
1570-0232
Statut éditorial
Publié
Date de publication
2007
Volume
852
Numéro
1-2
Première page
491
Dernière page/numéro d’article
496
Peer-reviewed
Oui
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.
PID Serval
serval:BIB_C409EDAA168B
PMID
Date de création
2008-05-19T10:00:54.740Z
Date de création dans IRIS
2025-05-21T02:56:38Z