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
Institution
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
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
20/08/2019 16:39