Universität zu Köln

Sigmund, Gerd, Koch, Anja, Orlovius, Anne-Katrin, Guddat, Sven, Thomas, Andreas ORCID: 0000-0003-1199-0743, Schaenzer, Wilhelm and Thevis, Mario (2014). Doping control analysis of trimetazidine and characterization of major metabolites using mass spectrometric approaches. Drug Test. Anal., 6 (11-12). S. 1197 - 1206. HOBOKEN: WILEY. ISSN 1942-7611

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Abstract

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 (0.5-50ng/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 (c) 2014 John Wiley & Sons, Ltd.

Item Type:	Journal Article
Creators:	Creators Email ORCID ORCID Put Code Sigmund, Gerd UNSPECIFIED UNSPECIFIED UNSPECIFIED Koch, Anja UNSPECIFIED UNSPECIFIED UNSPECIFIED Orlovius, Anne-Katrin UNSPECIFIED UNSPECIFIED UNSPECIFIED Guddat, Sven UNSPECIFIED UNSPECIFIED UNSPECIFIED Thomas, Andreas UNSPECIFIED orcid.org/0000-0003-1199-0743 UNSPECIFIED Schaenzer, Wilhelm UNSPECIFIED UNSPECIFIED UNSPECIFIED Thevis, Mario UNSPECIFIED UNSPECIFIED UNSPECIFIED
URN:	urn:nbn:de:hbz:38-423978
DOI:	10.1002/dta.1680
Journal or Publication Title:	Drug Test. Anal.
Volume:	6
Number:	11-12
Page Range:	S. 1197 - 1206
Date:	2014
Publisher:	WILEY
Place of Publication:	HOBOKEN
ISSN:	1942-7611
Language:	English
Faculty:	Unspecified
Divisions:	Unspecified
Subjects:	no entry
Uncontrolled Keywords:	Keywords Language HUMAN PLASMA; HUMAN URINE; MS METHOD; DRUGS; QUANTIFICATION; PARKINSONISM Multiple languages Biochemical Research Methods; Chemistry, Analytical; Pharmacology & Pharmacy Multiple languages
URI:	http://kups.ub.uni-koeln.de/id/eprint/42397