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Screening for anabolic steroids in sports: analytical strategy based on the detection of phase I and phase II intact urinary metabolites by liquid chromatography tandem mass spectrometry

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dc.contributor.author Balcells Aribau, Georgina, 1987-
dc.contributor.author Pozo Mendoza, Óscar J., 1975-
dc.contributor.author Esquivel López, Argitxu, 1989-
dc.contributor.author Kotronoulas, Aristotelis
dc.contributor.author Joglar Tamargo, Jesús
dc.contributor.author Segura Noguera, Jordi
dc.contributor.author Ventura Alemany, Rosa
dc.date.accessioned 2015-06-05T08:33:58Z
dc.date.issued 2015
dc.identifier.citation Balcells G, Pozo OJ, Esquivel A, Kotronoulas A, Joglar J, Segura J. et al. Screening for anabolic steroids in sports: analytical strategy based on the detection of phase I and phase II intact urinary metabolites by liquid chromatography tandem mass spectrometry. J Chromatogr A. 2015 Apr 10;1389:65-75. DOI: 10.1016/j.chroma.2015.02.022.
dc.identifier.issn 0021-9673
dc.identifier.uri http://hdl.handle.net/10230/23745
dc.description.abstract In order to improve the detection capabilities of anabolic androgenic steroids (AAS) in sports, a liquid chromatography-tandem mass spectrometry (LC-MS/MS) screening method for the simultaneous detection of AAS phase I and phase II intact urinary metabolites (glucuronides and sulfates) was developed. A total of 36 metabolites (7 unconjugated; 19 glucuronides and 10 sulfates) corresponding to 15 of the most reported AAS were included. Analytes were extracted from urine using C18 cartridges. LC and MS conditions were studied in-depth to determine the most sensitive and selective conditions for each analyte. A selected reaction monitoring method was set up. The optimization of the experimental parameters for 13 metabolites not available as standards was performed using excretion study urines. Extraction recoveries were above 77% for all 23 validated analytes. Intra-day precision was lower than 21%, and LODs were in the range 0.25-4ng/mL for 18 of the 23 analytes. Matrix effect was evaluated using post column infusion and ranged from 92 to 147%. The method was successfully applied to excretion study urines of different exogenous AAS. The suitability of the strategy was demonstrated with methyltestosterone and stanozolol excretion study urines by achieving detection times of 22 and 21 days, respectively. The method is compliant with the World Antidoping Agency requirements for most of the studied compounds. It represents a cost-effective approach that improves the detection capabilities of AAS by increasing the sensitivity for some metabolites and by including recently described phase II long-term metabolites not detectable using the current screening strategy.
dc.description.sponsorship Grants by Ministerio de Economía y Competividad (Gobierno de Espana) ˜ (Project number DEP2012-35612) and Generalitat de Catalunya (Consell Català de l’Esport and DIUE 2014 SGR 692) are gratefully acknowledged
dc.format.mimetype application/pdf
dc.language.iso eng
dc.publisher Elsevier
dc.relation.ispartof Journal of Chromatography A. 2015 Apr 10;1389:65-75
dc.rights © 2015 Elsevier. Licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 International http://creativecommons.org/licenses/by-nc-nd/4.0/ http://dx.doi.org/10.1016/j.chroma.2015.02.022.
dc.rights.uri http://creativecommons.org/licenses/by-nc-nd/4.0/
dc.subject.other Anabolitzants
dc.subject.other Dopatge en els esports
dc.title Screening for anabolic steroids in sports: analytical strategy based on the detection of phase I and phase II intact urinary metabolites by liquid chromatography tandem mass spectrometry
dc.type info:eu-repo/semantics/article
dc.identifier.doi http://dx.doi.org/10.1016/j.chroma.2015.02.022
dc.relation.projectID info:eu-repo/grantAgreement/ES/3PN/DEP2012-35612
dc.rights.accessRights info:eu-repo/semantics/openAccess
dc.type.version info:eu-repo/semantics/acceptedVersion

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