Synthesis of nanoflakes-covered microparticles of nickel-Application for electrocatalytic oxidation and quantitation of nitrofurazone

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Nickel microparticles covered with nanoflakes (NMCN) were hydrothermally synthesized in an alkaline solution of acrylamide dissolved in ethylene glycol/ethylenediamine at 200 °C. Structure and morphology of NMCN were characterized by field-emission scanning electron microscopy and X-ray powder diffraction, respectively. NMCN was applied, as an electrode modifier, with a surface concentration of 5.1 × 10−8 mol cm−2, and a detailed study was performed for the kinetics of charge transfer across the modified electrode/electrolyte interface using cyclic voltammetry. For the redox transition of NMCN in an alkaline solution, electron transfer coefficient and apparent charge-transfer rate constant were acquired as 0.65 and 0.6 s−1, respectively. The modified electrode was then applied for a study on the electrocatalytic oxidation of nitrofurazone (NF) on the NMCN surface through an electrochemical-catalytic (EC') mechanism. The oxidation process was followed by a NF diffusion coefficient of 2.9 × 10−6 cm2 s−1 and a catalytic rate constant of 3.0 × 104 cm3 mol−1 s−1. Also, an electron transfer coefficient of 0.40 was attained. The modified electrode was employed as a novel, time-saving, sensitive and simple amperometric sensor for NF, and quantified the drug with a linear range of 30–570 μmol L−1 and a sensitivity of 0.694 ± 0.002 A L mol−1 cm−2. Also, a detection limit of 4.3 μmol L−1 was attained. The sensor was employed for direct assay of NF in the human serum and ointments.