NiCo2O4 and NiFe2O4 were synthesized by the hydrothermal route using the molar composition, 2.2 CoCl2·6H2O:1.0 NiCl2·6H2O:9 urea:832 H2O and 2.2 FeCl2·4H2O:1.0 NiCl2·6H2O:9 urea:832 H2O, respectively. For the comparative study, NiO, Co3O4, and Fe3O4 were also prepared. Materials were characterized by a complementary combination of X-ray diffraction, nitrogen sorption, and Scanning electron microscopy. Non-enzymatic electrochemical sensors (using above-mentioned metal oxides) were constructed for the detection of lindane in the aqueous-methanol medium. Electrochemical techniques such as cyclic voltammetry, differential pulse voltammetry, and amperometry were used for the detection of lindane. Reproducibility, stability, and interference studies were performed to obtain the suitable non-enzymatic sensor. The analytical performance of the sensor was demonstrated for the detection of lindane in tap water samples.