Abstract

A novel approach was presented to synthesize Pd nanoparticles supported on the surface of porous silicon (PSi) powder by a simple in-situ redox reaction between Pd+2 and PSi in hydrofluoric acid solution. Ionic liquid and Pd/PSi nanocomposite doped carbon-ceramic electrode was prepared by mixing them with electrode matrix before gelation. Pd/PSi nanocomposite in carbon-ceramic ionic liquid electrode (CCILE) was utilized as a novel electrocatalyst and exhibited a synergetic impact on the oxidation of codeine (COD) and acetaminophen (ACT). The chemical, electrochemical, and morphological, features of the provided nanostructure were characterized by means of X-ray diffraction spectroscopy, energy dispersive X-ray spectroscopy (EDX), Fourier-transform infrared spectroscopy (FT-IR), as well as cyclic voltammetry (CV). The peak currents of oxidation were raised, and the oxidation peak potentials of ACT and COD were declined on the proposed sensor surface by the high electrochemical activity, high surface area, fast electron transfer rate, as well as proper antifouling features of this nanostructure. ACT and COD were determined simultaneously via differential pulse voltammetry (DPV). Using the proposed electrochemical sensor, ACT and COD could be measured in the range of 0.3–15 µmol L−1 with detection limits of 24 nM and 32 nM, respectively. As a final point, the provided electrochemical sensor was utilized to determine ACT and COD in the real samples, including pharmaceutical compounds and blood serum with satisfactory results.

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