Resumo

MORALES HERRERA, Ana María et al. Qualitative determination of metabolites in urine of six glucocorticoids by high performance liquid chromatography coupled to mass-sprectrometry. Rev. colomb. cienc. quim. farm. [online]. 2014, vol.43, n.1, pp.137-152. ISSN 0034-7418.  https://doi.org/10.15446/rcciquifa.v43n1.45469.

Glucocorticoids use is prohibited on the sport during competitions when they are administered by systemic routes for which WADA defined a reporting level of 30ng/ml for parent compounds and their metabolites. In this paper has been developed an analytical methodology for the qualitative determination of the main metabolites of some synthetic glucocorticoids: Betamethasone, Budesonide, Dexamethasone, Methylprednisolone, Prednisolone and Triamcinolone Acetonide, present in urine samples preserved by the Laboratory of Doping Control of COLDEPORTES. The methodology included a comparison between the extraction of free and conjugated with glucuronide analytes (to determine which of the two fractions was more useful in the analysis of these substances), their separation by high performance liquid chromatography with positive ionization and detection using ion trap (HPLC -MS- MS). Major metabolites were selected by their retention times, later fragmented to obtain its spectra and through their abundance determine the amount present in each fraction (free and conjugated). There were identified the six glucocorticoids and twelve metabolites, that will allow to make a more extended screening of the consumption of these substances. Also it was confirmed that the amounts for most of the compounds of interest, were higher in the free fraction of the urine samples, but it is not possible to eliminate the hydrolysis process because some metabolites are excreted as conjugates.

Palavras-chave : Glucocorticoids; HPLC; ESI Mass spectrometry; Anti-doping analysis; Urine samples.

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