Source:http://linkedlifedata.com/resource/pubmed/id/18395062
Switch to
Predicate | Object |
---|---|
rdf:type | |
lifeskim:mentions | |
pubmed:issue |
2
|
pubmed:dateCreated |
2008-4-8
|
pubmed:abstractText |
19-Nortestosterone (nandrolone) major metabolites in human urine are excreted as sulfoconjugated and glucuroconjugated forms. A sensitive and selective liquid chromatography/tandem mass spectrometry (LC/MS/MS) method in negative ESI mode was developed for direct quantification of 19-norandrosterone sulfate (19-NAS) and 19-noretiocholanolone sulfate (19-NES). For both sulfoconjugates, the [M-H](-) ion at m/z 355 and the fragment ion at m/z 97 were used as the precursor and product ions, respectively. The purification method involved a complete and rapid separation of sulfates and glucuronides in two extracts after loading the sample on a weak anion exchange solid phase extraction support (SPE Oasis WAX). Then, sulfates were separated by LC (Uptisphere ODB, 150 mm x 3.0 mm, 5 microm) and analyzed on a linear trap and a triple quadrupole mass spectrometer. The lower limit of detection (LLOD) and lowest limit of quantification (LLOQ) were of 100 pg mL(-1) and 1 ng mL(-1), respectively. Assay validation demonstrated good performances in terms of trueness (92.0-104.9%), repeatability (0.6-7.2%) and intermediate precision (1.3-10.8%) over the range of 1-2500 ng mL(-1). Finally, 19-NAS and 19-NES in urine samples collected after intake of 19-norandrostenedione (nandrolone precursor) were quantified. This assay may be easily implemented to separate glucuronide and sulfate steroids from urine specimens prior to quantification by LC/MS/MS.
|
pubmed:language |
eng
|
pubmed:journal | |
pubmed:citationSubset |
IM
|
pubmed:chemical | |
pubmed:status |
MEDLINE
|
pubmed:month |
Apr
|
pubmed:issn |
1873-4324
|
pubmed:author | |
pubmed:issnType |
Electronic
|
pubmed:day |
21
|
pubmed:volume |
613
|
pubmed:owner |
NLM
|
pubmed:authorsComplete |
Y
|
pubmed:pagination |
228-37
|
pubmed:meshHeading |
pubmed-meshheading:18395062-Chromatography, Liquid,
pubmed-meshheading:18395062-Humans,
pubmed-meshheading:18395062-Reproducibility of Results,
pubmed-meshheading:18395062-Sensitivity and Specificity,
pubmed-meshheading:18395062-Spectrometry, Mass, Electrospray Ionization,
pubmed-meshheading:18395062-Steroids,
pubmed-meshheading:18395062-Tandem Mass Spectrometry
|
pubmed:year |
2008
|
pubmed:articleTitle |
Profiling of 19-norsteroid sulfoconjugates in human urine by liquid chromatography mass spectrometry.
|
pubmed:affiliation |
Laboratoire Suisse d'Analyse du Dopage, Institut Universitaire de Médecine Légale, Chemin des Croisettes 22, 1066 Epalinges, Switzerland.
|
pubmed:publicationType |
Journal Article,
Research Support, Non-U.S. Gov't,
Validation Studies
|