The design and development of inexpensive, and extremely sensitive sensors for Hydroxylamine (HYA) are imperative due to its toxicity to animals, plants, and aquatic life. This work proposes a high-performance enzyme-free electrochemical sensor for HYA based on its oxidation on Nickel cobaltite (NCO) spinel-modified fluorine doped tin oxide (FTO) electrode. Hydrothermally grown irregularly shaped NCO nanoparticles (NPs) of size around 10 nm are characterized by XRD, XPS, UV–visible, BET, and TEM to evaluate the structural and morphological characteristics. NCO-modified FTO (NCO@FTO) electro-oxidizes HYA at a potential of 0.66 V vs. Ag/AgCl, delivering 1.7 times the current response than bare FTO. The rich catalytically active redox couples of Ni and Co, high conductivity, and high surface area of the NCO NPs contribute to the superior electrochemical response of NCO@FTO. As an amperometric sensor, NCO@FTO detects HYA in a wide range of 10 to 4000 µM concentration with a high sensitivity of 408 μA mM−1 cm−2. The sensor has a detection limit of 0.47 μM (S/N = 3), faster response of less than 3 s, excellent selectivity, and good stability. The practical feasibility of the proposed sensor is investigated by employing it in the monitoring of real samples. This study demonstrates NCO@FTO as an efficient low-cost sensor for HYA and extends the use of spinel metal oxides in bioanalysis. © 2023 Elsevier Ltd