Different metal oxide (MO) nanomaterials, such as ZnO, SnO2, and nanocomposites of ZnO:SnO2 with various ratios of (1:9), (2:8), and (3:7) were prepared and coated on glassy carbon electrode (GCE). These MOs were tested as sensing material for organophosphate (OP) pesticides detection. Among all MOs, ZnO:SnO2 (1:9) coated GCE increases redox peak current at different buffer solutions with varying pH compared to bare GCE. Moreover, among these pH values, ZnO:SnO2 (1:9) coated GCE significantly enhanced the redox peak at pH 6.2, emphasizing optimal electrochemical conditions for the given pesticides. The morphological, elemental composition, metal ions-functional group interation, and crystallinity of different MO nanocomposites were examined using field-emission scanning electron microscopy (FESEM), fourier transform infrared spectroscopy (FTIR), energy dispersive X-ray spectrum (EDX), and X-ray diffraction (XRD), respectively. The modified GCE with ZnO:SnO2 (1:9) showed an excellent performance during the electrochemial sensing of the diazinon (DiZn) pesticide. Therefore, detailed study was carried out for the sensing of DiZn. Furthermore, the electrochemical behavior of the ZnO:SnO2 (1:9) coated GCE was evaluated using cyclic voltammetry (CV) with 0.5 mL (5 mM) potassium ferrocyanide, resulting in a pronounced increase in anodic and cathodic peak potentials (Epa = 0.423 V, Epc = 0.1945 V) and currents (Ipa = 9.867 × 10-5 mA, Ipc = -7.993 × 10-5 mA). In addition, electrochemical impedance spectroscopy (EIS) demonstrated a reduction in charge transfer resistance for the coated ZnO:SnO2 (1:9) GCE. Differential pulse voltammetry (DPV) further showed a linear relationship between current and pesticide concentration, with a high correlation coefficient (R2 = 0.996), low limit of detection (LOD = 0.0133 mM) and low limit of quantification (LOQ = 0.0405 mM). Real samples, including tap and seawater, were analyzed to validate the method’s applicability. Additionally, chronoamperometry with a step potential of 1.2 V indicated high sensitivity for DiZn detection, with a sensitivity of 0.23 mA mM−1 cm−2. Finally, the stability of the ZnO:SnO2 (1:9) coated GCE was confirmed through recyclability tests over three cycles using CV and DPV techniques, ensuring its robustness for practical applications in pesticide detection.
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