The increasing use of fipronil, a phenylpyrazole insecticide with known toxicity and endocrine-disrupting effects, poses significant environmental and health risks due to its persistence in agricultural products and ecosystems. This study presents the development of a novel TiO2-ZnO/graphene (GTZ) hybrid nanocomposite electrode for ultra-sensitive electrochemical detection of fipronil. The GTZ nanocomposite was synthesized using a microwave-assisted technique and characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), and Fourier-transform infrared spectroscopy (FTIR). SEM results showed that TiO2 and ZnO nanoparticles were well dispersed in the graphene layer. XRD diffractograms confirmed the presence of the anatase TiO2 phase and Wurtzite ZnO phase in GTZ nanocomposites. FTIR analysis revealed the presence of oxygen-containing functional groups, Ti-O and Zn-O bonds, indicating successful modification of graphene. Cyclic voltammetry was employed to evaluate the sensing capabilities of the GTZ electrode, demonstrating a linear response to fipronil concentrations as low as 0.0023 µg/L, with a high reproducibility (RSD 1.77 %). The electrode’s enhanced sensitivity can be attributed to the synergistic interaction between TiO2-ZnO nanoparticles and graphene, providing a large electroactive surface area and improved electron transfer kinetics. This study confirms the potential of GTZ nanocomposite electrodes as a cost-effective and portable platform for real-time monitoring of fipronil residues in environmental and agricultural samples.
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