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An electrochemical sensor based on polyaniline‐ZnO−NiO (PANI‐ZnO−NiO) nanocomposite was developed for the non‐enzymatic detection of malathion. The structure, surface morphology, and optical properties of the as‐prepared nanocomposite were studied by XRD, FTIR, SEM, and UV‐Vis spectroscopy. The electrochemical behavior of the nanocomposite based sensor was first evaluated through cyclic voltammetry (CV). Under optimum conditions, differential pulse voltammetry (DPV) was further utilized for malathion detection, which proved the PANI‐ZnO−NiO/GCE electrode as an effective electrochemical sensor. The developed electrochemical sensor showed a low detection limit of 1.0×10−8 M with a wider linear range of 10 to 70 nM for malathion. [ABSTRACT FROM AUTHOR]