A simple, highly sensitive, accurate, and low-cost electrochemical sensor was developed for the determination of over-the-counter painkiller, paracetamol (PC). The enhanced sensing capabilities of the developed sensor were fabricated by the single-step modification of disposable pencil graphite electrodes (PGEs) with the simultaneous electrochemical reduction in graphene oxide and antimony (II) salts. For this purpose, an electrochemically reduced graphene oxide–antimony nanoparticle (ERGO-SbNP) nanocomposite material was prepared by trapping metallic nanoparticles between individual graphene sheets in the modification of PGEs. Structural characterization by FTIR and Raman spectroscopy was employed to confirm the presence of oxygen functional groups and defects in the conjugated carbon-based structure of GO. Morphological differences between the modified PGEs were confirmed by HRTEM and HRSEM for the presence of nanoparticles. The modified electrodes were further electrochemically characterized using CV and EIS. The electrooxidation of PC on an ERGO-SbNPs-PGE was achieved by adsorptive stripping differential pulse voltametric analysis in 0.1 mol·L−1 phosphate buffer solution at pH = 7.0. The optimum current response was used to record a detection limit of 0.057 µmol·L−1 for PC. The electrochemical sensor was further used in real sample analysis for a commercially available pharmaceutical tablet (500 mg PC), for which the percentage recovery was between 99.4% and 100.8%.
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