Electrochemical Determination of the Steroid Tibolone and Its Metabolites in Saliva Samples. Issue 21 (12th November 2020)

• Record Type: Journal Article
• Authors: Silva, Weberson P.; Rocha, Raquel G.; Felisbino, John K. R. P.; Sousa, Raquel M. F.; Munoz, Rodrigo A. A.; Richter, Eduardo M.
• Is Part Of: ChemElectroChem. Volume 7:Issue 21(2020)
• Page Start: 4469
• Page End: 4476
• Publication Date: 2020-11-12
• Subjects: boron-doped diamond -- electrochemical mechanisms -- forensic chemistry -- rapid analysis -- synthetic steroids; Electrochemistry -- Periodicals; 541.37
• DOI: 10.1002/celc.202001248
• Languages: English
• ISSNs: 2196-0216

Abstract

Abstract: 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). Abstract : Anti‐doping : The steroid tibolone is a synthetic steroid banned by the World Anti‐Doping Agency (WADA). In this work, a simple and low‐cost electrochemical method is reported for the first time for fast screening analysis of TIB and its metabolites (3‐α hydroxytibolone and 3‐β hydroxytibolone) in authentic human saliva samples using a boron‐doped diamond electrode and square‐wave voltammetry. The method has great potential to be used in anti‐doping analysis.