This work addresses the electrocatalytic activity of a binary metal oxide catalyst of NiMn₂O₄ for electroxidation of sarcosine, the well-known prostate cancer biomarker. The nanocatalyst described was prepared via hydrothermal synthesis route, followed by calcination at 800 °C. Field emission scanning electron microscopy and X-ray diffraction were applied to obtain information about the material morphology and structure. A carbon paste electrode modified with nano-NiMn₂O₄ showed unique catalytic activity in sarcosine electroxidation which led to a significant rise in oxidation current (about four times) in comparison with the blank electrode. However, the carbon paste electrodes containing single oxides of NiO and Mn₂O₃ exhibited no considerable enhancement in sarcosine signal. The cyclic voltammetry results indicated that the Mn³⁺/Mn⁴⁺ couple was responsible for sarcosine oxidation, and NiO may enhance the content of Mn⁴⁺species in NiMn₂O₄ material. The carbon paste-based NiMn₂O₄ electrode was applied in the sensitive determination of sarcosine in the concentration range of 0.01–5.0 μM with the relative standard deviation of 3.49% (n = 5). The detection limit and quantification limit of the probe were determined to be 3.8 and 12 nM, respectively. The remarkable sensitivity and high selectivity of the method approved the sensor applicability in measurement of sarcosine content in urine samples.