Universität zu Köln

de Oliveira, Fabio Azamor, Casilli, Alessandro, Piper, Thomas, da Silva, Thais Reis, da Silva, Cristiane Abrantes, Santana da Silva, Raquel Vieira, Dal Sasso, Marco Aurelio, dos Santos Goncalves Salgueiro, Gutierri Ricardo, Padilha, Monica Costa, Gualberto Pereira, Henrique Marcelo, Thevis, Mario and de Aquino Neto, Francisco Radler (2019). Implementation and Performance of the Gas Chromatography/Combustion/Isotope Ratio Mass Spectrometry-Based Method for the Confirmatory Analysis of Endogenous Anabolic Steroids during the Rio de Janeiro Olympic and Paralympic Games 2016. Anal. Chem., 91 (18). S. 11747 - 11757. WASHINGTON: AMER CHEMICAL SOC. ISSN 1520-6882

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Abstract

Carbon isotope ratio (CIR) confirmation is one of the most complex and delicate analyses in the doping control field, due to the nature of the molecules to be confirmed, normally present in urinary samples as a consequence of an endogenous production. The requirements for method validation established by the World Anti-Doping Agency (WADA) have been pushing the accredited laboratories to improve their methods. The choice of the method is always a cost benefit ratio involving a hard-working and time-consuming analysis and the guarantee of reporting of reliable results. This work presents the method fully validated by the Brazilian Doping Control Laboratory as part of the preparation for the Rio de Janeiro Summer Olympic and Paralympic Games 2016. Sample preparation encompassed solid-phase extraction, liquid-liquid extraction, enzymatic hydrolysis, acetylation, and purification by preparative high-performance liquid chromatography, and analyses were performed by gas chromatography/combustion/isotope ratio mass spectrometry. This proved to be a robust method to CIR confirmation in a big event, as demonstrated by the analysis of 179 samples during the Games 2016, from clearly negative results and adverse findings for testosterone (T) and related substances, boldenone and its metabolite, 19-norandrosterone and formestane. Two atypical findings were also reported for T and metabolites.

Item Type:	Journal Article
Creators:	Creators Email ORCID ORCID Put Code de Oliveira, Fabio Azamor UNSPECIFIED UNSPECIFIED UNSPECIFIED Casilli, Alessandro UNSPECIFIED UNSPECIFIED UNSPECIFIED Piper, Thomas UNSPECIFIED UNSPECIFIED UNSPECIFIED da Silva, Thais Reis UNSPECIFIED UNSPECIFIED UNSPECIFIED da Silva, Cristiane Abrantes UNSPECIFIED UNSPECIFIED UNSPECIFIED Santana da Silva, Raquel Vieira UNSPECIFIED UNSPECIFIED UNSPECIFIED Dal Sasso, Marco Aurelio UNSPECIFIED UNSPECIFIED UNSPECIFIED dos Santos Goncalves Salgueiro, Gutierri Ricardo UNSPECIFIED UNSPECIFIED UNSPECIFIED Padilha, Monica Costa UNSPECIFIED UNSPECIFIED UNSPECIFIED Gualberto Pereira, Henrique Marcelo UNSPECIFIED UNSPECIFIED UNSPECIFIED Thevis, Mario UNSPECIFIED UNSPECIFIED UNSPECIFIED de Aquino Neto, Francisco Radler UNSPECIFIED UNSPECIFIED UNSPECIFIED
URN:	urn:nbn:de:hbz:38-141230
DOI:	10.1021/acs.analchem.9b02341
Journal or Publication Title:	Anal. Chem.
Volume:	91
Number:	18
Page Range:	S. 11747 - 11757
Date:	2019
Publisher:	AMER CHEMICAL SOC
Place of Publication:	WASHINGTON
ISSN:	1520-6882
Language:	English
Faculty:	Unspecified
Divisions:	Unspecified
Subjects:	no entry
Uncontrolled Keywords:	Keywords Language CARBON-ISOTOPE RATIO; DRUG-TESTING DATA; GC-C-IRMS; URINARY STEROIDS; C-13/C-12 RATIOS; REFERENCE-POPULATION; SPORTS; FORMESTANE; BOLDENONE; ABUSE Multiple languages Chemistry, Analytical Multiple languages
Refereed:	Yes
URI:	http://kups.ub.uni-koeln.de/id/eprint/14123