Analytical challenges in doping control: Comprehensive two-dimensional gas chromatography with time of flight mass spectrometry,a promising option |
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Authors: | AI Silva Jr HMG Pereira A Casilli FC Conceição FR Aquino Neto |
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Institution: | 1. LAB DOP LADETEC/Instituto de Química, Universidade Federal do Rio de Janeiro, Ilha do Fundão, Avenida Athos da Silveira Ramos, 149-Centro de Tecnologia-Bloco A, Sala 603 - Cidade Universitária, Rio de Janeiro, CEP 21941-909, RJ, Brazil;2. Cefet Química, Rio de Janeiro, Brazil;3. Dipartimento Farmaco-chimico, Facoltà di Farmacia, Università di Messina, Messina, Italy |
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Abstract: | Doping control screening based on the enhanced resolution of comprehensive two-dimensional (2D) gas chromatography hyphenated to time of flight mass spectrometer was investigated. The identification of anabolic agents (clenbuterol, norandrosterone, epimetendiol, two methyltestosterone metabolites and 3′-hydroxystanozolol) contained in a spiked urine sample (2 ng/ml) was demonstrated. Special emphasis was given to 3′-hydroxystanozolol, mainly considering the difficulty in its detection. In contrast to conventional GC–MS approaches that must use single-ion monitoring, the GC × GC–TOFMS method enabled the identification of that metabolite through the deconvolution of the full mass spectrum and also resolved the co-eluted peaks of 3′-hydroxystanozolol and an endogenous component. |
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Keywords: | Comprehensive two-dimensional gas chromatography Time of flight mass spectrometry Doping control Anabolic agents 3&prime -Hydroxystanozolol |
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