In this work, we demonstrate a simplistic, substrate-free hydrothermal synthesis of the nickel-cobalt-based bimetallic oxide compound (NiCo2O4) as a highly sensitive and selective platform for the detection of flutamide in biological fluids. The NCO/GCE sensor shows a low detection limit (LOD) of 4 nM (LOD = 3s/m). The sensor shows two linear ranges of detection, namely nanomolar (10-500 nM) and micromolar (1-400 μM) with a sensitivity of 120.17 μA μM−1 cm−2 and 23.18 μA μM−1 cm−2, respectively. The enhanced sensing performance of the sensor is attributed to the electro-catalytic active sites of the NOC micro flowers facilitated with the Ni2+/Ni3+ and Co2+/Co3+ redox couple. The sensor is efficacious in the detection of flutamide in simulated blood serum with a decent range of recovery percentages from ∼106.45 to ∼97.60%. The efficacy of the NCO/GCE sensor using a facile, low-cost method prompts its versatile use as a promising platform for bioanalytical applications. This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique