Document Detail


Doping control analysis of trimetazidine and characterization of major metabolites using mass spectrometric approaches.
MedLine Citation:
PMID:  24913825     Owner:  NLM     Status:  Publisher    
Abstract/OtherAbstract:
Since January 2014, the anti-anginal drug trimetazidine [1-(2,3,4-trimethoxybenzyl)-piperazine] has been classified as prohibited substance by the World Anti-Doping Agency (WADA), necessitating specific and robust detection methods in sports drug testing laboratories. In the present study, the implementation of the intact therapeutic agent into two different initial testing procedures based on gas chromatography-mass spectrometry (GC-MS) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) is reported, along with the characterization of urinary metabolites by electrospray ionization-high resolution/high accuracy (tandem) mass spectrometry. For GC-MS analyses, urine samples were subjected to liquid-liquid extraction sample preparation, while LC-MS/MS analyses were conducted by established 'dilute-and-inject' approaches. Both screening methods were validated for trimetazidine concerning specificity, limits of detection (0.5-50 ng/mL), intra-day and inter-day imprecision (<20%), and recovery (41%) in case of the GC-MS-based method. In addition, major metabolites such as the desmethylated trimetazidine and the corresponding sulfoconjugate, oxo-trimetazidine, and trimetazidine-N-oxide as identified in doping control samples were used to complement the LC-MS/MS-based assay, although intact trimetazidine was found at highest abundance of the relevant trimetazidine-related analytes in all tested sports drug testing samples. Retrospective data mining regarding doping control analyses conducted between 1999 and 2013 at the Cologne Doping Control Laboratory concerning trimetazidine revealed a considerable prevalence of the drug particularly in endurance and strength sports accounting for up to 39 findings per year. Copyright © 2014 John Wiley & Sons, Ltd.
Authors:
Gerd Sigmund; Anja Koch; Anne-Katrin Orlovius; Sven Guddat; Andreas Thomas; Wilhelm Schänzer; Mario Thevis
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Publication Detail:
Type:  JOURNAL ARTICLE     Date:  2014-6-9
Journal Detail:
Title:  Drug testing and analysis     Volume:  -     ISSN:  1942-7611     ISO Abbreviation:  Drug Test Anal     Publication Date:  2014 Jun 
Date Detail:
Created Date:  2014-6-10     Completed Date:  -     Revised Date:  -    
Medline Journal Info:
Nlm Unique ID:  101483449     Medline TA:  Drug Test Anal     Country:  -    
Other Details:
Languages:  ENG     Pagination:  -     Citation Subset:  -    
Copyright Information:
Copyright © 2014 John Wiley & Sons, Ltd.
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