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In this study, a SnO2/CeO2 nanostructured oxide was prepared by a sonication-based approach. The prepared SnO2/CeO2 nanostructured oxide was examined for its structural and morphological characteristics using powder X-ray diffraction, Fourier transform infrared spectroscopy, transmission electron microscopy, X-ray electron microscopy, and Brunauer–Emmett–Teller analysis. An electrochemical sensor was fabricated by deposition of the SnO2/CeO2 nanostructured oxide on a glassy carbon electrode (GCE) using a binder (SnO2/CeO2/GCE). The fabricated SnO2/CeO2/GCE, as an efficient electrochemical sensor, was employed for detection of hydrazine using the electrochemical technique viz. linear sweep voltammetry (LSV). The voltammetric detection of hydrazine at the SnO2/CeO2/GCE sensor exhibits a rapid increase in the oxidation peak current upon addition of hydrazine. The electrochemical response of the SnO2/CeO2/GCE shows excellent sensitivity for hydrazine. The sensitivity, limit of detection (LOD), and limit of quantification (LOQ) of the sensor using LSV technique are estimated to be 81 μA μM−1 cm−2, 0.179 μM, and 0.52 μM, respectively. The SnO2/CeO2/GCE as a sensor shows a mostly linear relationship between current and concentration of hydrazine over the concentration range of 3–26 μM (R2 = 0.975). Overall, our proposed SnO2/CeO2/GCE sensor shows significant stability, selectivity, sensitivity, repeatability, and reproducibility.