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Electrochemical Determination of the Steroid Tibolone and Its Metabolites in Saliva Samples
Author(s) -
Silva Weberson P.,
Rocha Raquel G.,
Felisbino John K. R. P.,
Sousa Raquel M. F.,
Munoz Rodrigo A. A.,
Richter Eduardo M.
Publication year - 2020
Publication title -
chemelectrochem
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.182
H-Index - 59
ISSN - 2196-0216
DOI - 10.1002/celc.202001248
Subject(s) - tibolone , repeatability , chromatography , supporting electrolyte , detection limit , chemistry , saliva , electrolyte , high performance liquid chromatography , electrochemistry , analyte , reagent , electrode , analytical chemistry (journal) , estrogen , medicine , biochemistry , endocrinology
Tibolone (TIB) is a synthetic steroid banned by the World Anti‐Doping Agency (WADA) due to its similar properties to estrogen and progesterone. In this work, a simple and low‐cost electrochemical method for the determination of TIB and its metabolites (3‐α hydroxytibolone and 3‐β hydroxytibolone) in authentic human saliva is reported. Square‐wave voltammetry (SWV) with an unmodified boron‐doped diamond (BDD) electrode and phosphate buffer 0.1 mol L −1 were selected as the electrochemical technique, working electrode, and supporting electrolyte, respectively. Analytical characteristics of the proposed method include good repeatability (RSD <2.4 %), wide linear range (1 to 110 μmol L −1 ; r=0.999) and low detection limit (0.3 μmol L −1 ). Average recovery values (104±3 % for TIB and 98±5 % for the metabolites) for direct analysis of spiked saliva samples (only diluted in supporting electrolyte) indicate that no significant matrix interference was observed. The proposed method was also efficient for the determination of TIB in pharmaceutical samples (statistically similar results to those obtained by HPLC).