Journal
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
Volume 877, Issue 27, Pages 3003-3011Publisher
ELSEVIER SCIENCE BV
DOI: 10.1016/j.jchromb.2009.07.013
Keywords
Doping; Sibutramine; GC-MS; WADA; MSTFA/MBTFA
Funding
- Fundacao Universitario Jose Bonifacio-FUJB
- CNPq
- FAPERJ
- CBF
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A method for identifying the metabolites of sibutramine 1-(4(chlorophenyl)-N,N-dimethyl-alpha-(2-methylpropyl))cyclobutanemethanamine) in urine, utilizing a double derivatization strategy, with N-methyl-N-(trimethylsilyl)-trifluoroacetamide and N-methyl-bis-(trifluoroacetamide), in gas chromatography/mass spectrometry is proposed. This methodology results in mass spectra with at least three fragments in abundance superior to 20%, attending the World Anti-Doping Agency identification criteria for qualitative assays. The characterization of the derivatives was obtained through two ionization modes: Chemical Ionization and Electron Impact ionization, both in full scan mode. Sibutramine was administered to 5 (five) volunteers and the excretion profile followed for 92 h. Routine analytical, hydroxy-cyclobutane-bis-nor-sibutramine which becomes the more abundant metabolite in the first 10 h and hydroxy-isopropyl-bis-nor-sibutramine which becomes the most abundant after 40 h, were proposed for doping monitoring. (C) 2009 Elsevier B.V. All rights reserved.
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