Electrochemical oxidation of edoxaban and its determination in pharmaceutical samples and human serum

• Published in: Microchemical journal 2024-09, Vol.204, p.110926, Article 110926
• Main Authors: Rocha, Manoelly Oliveira, Dallegrave, Alexsandro, Klein, Thágor Moreira, Lavayen, Vladimir, Steppe, Martin, Da Silva, Jacqueline Arguello
• Format: Article
• Language: English
• Subjects: Carbon paste electrode; Edoxaban; Electrochemical sensor
• ISSN: 0026-265X; 1095-9149
• DOI: 10.1016/j.microc.2024.110926

[Display omitted] •Novel and sensitive voltammetric method for EDX sensing using a CPE.•A pH-dependent and irreversible oxidation peak resulted from the oxidation of EDX.•The developed sensor is suitable for pharmaceutical and biological sample analysis. Edoxaban (EDX) electrooxidation was investigated at a carbon paste electrode using cyclic voltammetry (CV), differential pulse voltammetry (DPV), and chronoamperometry (CA). Several experimental conditions were evaluated, including buffer solution, pH, concentration, and scan rate. The results indicated that the redox process was irreversible over the pH and scan range studied and exhibited a diffusion-controlled behaviour. Furthermore, the drug was subjected to bulk electrolysis followed by UHPLC-QTOF/MS to elucidate the mechanism behind its electrooxidation. The present study also demonstrated the electroanalytical method’s ability to successfully determine EDX in pharmaceutical formulations and human serum without interference from the leading excipients and biological constituents. The obtained analytical curves exhibited two linear ranges, from 1.2 × 10−6 to 1.2 × 10−5 mol/L and from 1.4 × 10−5 to 7.4 × 10−5 mol/L, with a sensitivity of 0.068 μA (μmol/L)−1 and a limit of detection (LOD) of 2.6 × 10−7 mol/L, at a relative standard deviation (RSD) of 2.96 %.