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Elucidation of urinary metabolites of fluoxymesterone by liquid chromatography-tandem mass spectrometry and gas chromatography-mass spectrometry

Oscar Juan Pozo Mendoza (UGent) , Wim Van Thuyne (UGent) , Koen Deventer (UGent) , Peter Van Eenoo (UGent) and Frans Delbeke (UGent)
(2008) JOURNAL OF MASS SPECTROMETRY. 43(3). p.394-408
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Abstract
The suitability of liquid chromatography tandem mass spectrometry (LC-MS/MS) and gas chromatography mass spectrometry (GC-MS) for the elucidation of fluoxymesterone metabolism has been evaluated. Electrospray ionization (ESI) and collision induced dissociation (CID) fragmentation in LC-MS/MS and electron impact spectra (EI) in GC-MS have been studied for fluoxymesterone and two commercially available metabolites. MSn experiments and accurate mass measurements performed by an ion-trap analyser and a QTOF instrument respectively have been used for the elucidation of the fragmentation pathway. The neutral loss scan of 20 Da (loss of HF) in LC-MS/MS has been applied for the selective detection of fluoxymesterone metabolites. In a positive fluoxymesterone doping control sample, 9 different analytes have been detected including the parent compound. Seven of these metabolites were also confirmed by GC-MS including 5 previously unreported metabolites. On the basis of the ionization, the CID fragmentation, the accurate mass of the product ions and the EI spectra of these analytes, a tentative elucidation as well as a proposal for the metabolic pathway of fluoxymesterone has been suggested. The presence of these compounds has also been confirmed by the analysis of five other positive fluoxymesterone urine samples.

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Chicago
Pozo Mendoza, Oscar Juan, Wim Van Thuyne, Koen Deventer, Peter Van Eenoo, and Frans Delbeke. 2008. “Elucidation of Urinary Metabolites of Fluoxymesterone by Liquid Chromatography-tandem Mass Spectrometry and Gas Chromatography-mass Spectrometry.” Journal of Mass Spectrometry 43 (3): 394–408.
APA
Pozo Mendoza, O. J., Van Thuyne, W., Deventer, K., Van Eenoo, P., & Delbeke, F. (2008). Elucidation of urinary metabolites of fluoxymesterone by liquid chromatography-tandem mass spectrometry and gas chromatography-mass spectrometry. JOURNAL OF MASS SPECTROMETRY, 43(3), 394–408.
Vancouver
1.
Pozo Mendoza OJ, Van Thuyne W, Deventer K, Van Eenoo P, Delbeke F. Elucidation of urinary metabolites of fluoxymesterone by liquid chromatography-tandem mass spectrometry and gas chromatography-mass spectrometry. JOURNAL OF MASS SPECTROMETRY. 2008;43(3):394–408.
MLA
Pozo Mendoza, Oscar Juan, Wim Van Thuyne, Koen Deventer, et al. “Elucidation of Urinary Metabolites of Fluoxymesterone by Liquid Chromatography-tandem Mass Spectrometry and Gas Chromatography-mass Spectrometry.” JOURNAL OF MASS SPECTROMETRY 43.3 (2008): 394–408. Print.
@article{424637,
  abstract     = {The suitability of liquid chromatography tandem mass spectrometry (LC-MS/MS) and gas chromatography mass spectrometry (GC-MS) for the elucidation of fluoxymesterone metabolism has been evaluated. Electrospray ionization (ESI) and collision induced dissociation (CID) fragmentation in LC-MS/MS and electron impact spectra (EI) in GC-MS have been studied for fluoxymesterone and two commercially available metabolites. MSn experiments and accurate mass measurements performed by an ion-trap analyser and a QTOF instrument respectively have been used for the elucidation of the fragmentation pathway. The neutral loss scan of 20 Da (loss of HF) in LC-MS/MS has been applied for the selective detection of fluoxymesterone metabolites. In a positive fluoxymesterone doping control sample, 9 different analytes have been detected including the parent compound. Seven of these metabolites were also confirmed by GC-MS including 5 previously unreported metabolites. On the basis of the ionization, the CID fragmentation, the accurate mass of the product ions and the EI spectra of these analytes, a tentative elucidation as well as a proposal for the metabolic pathway of fluoxymesterone has been suggested. The presence of these compounds has also been confirmed by the analysis of five other positive fluoxymesterone urine samples.},
  author       = {Pozo Mendoza, Oscar Juan and Van Thuyne, Wim and Deventer, Koen and Van Eenoo, Peter and Delbeke, Frans},
  issn         = {1076-5174},
  journal      = {JOURNAL OF MASS SPECTROMETRY},
  language     = {eng},
  number       = {3},
  pages        = {394--408},
  title        = {Elucidation of urinary metabolites of fluoxymesterone by liquid chromatography-tandem mass spectrometry and gas chromatography-mass spectrometry},
  url          = {http://dx.doi.org/10.1002/jms.1343},
  volume       = {43},
  year         = {2008},
}

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