In this study, heterostructures containing hydrothermally derived ZnO and combustion derived NiFe2O4 were co-deposited on nickel foam (NF) substrate. The modification of NF based substrate with the synthesised electrocatalysts is capable of increasing the electrochemically active surface area (ECSA) due to its porous network. The fabricated ZnO@NF, NiFe2O4@NF and ZnO/NiFe2O4@NF electrodes were tested in phosphate buffer saline (PBS) (pH = 7.4 ± 0.2) to understand their chemical kinetics which reveals a diffusion-controlled process. A comparative study reveals that the presence of surface charges on ZnO/NiFe2O4@NF electrode, influences the selectivity by enhancing the sensitivity towards UA which is attributed to the low charge transfer resistance and its higher ECSA of 1.487 cm2. The linear response current was observed between 0.52 mM and 1.48 mM with a detection limit (LOD) of 8.22 μM and limit of quantification (LOQ) of 27.4 μM. The sensitivity was found to be 2.31 mA.mM−1cm−2. The main advantages of ZnO/NiFe2O4@NF electrode is its simple fabrication technique which is inexpensive, stability over a period of 13 days with current loss of ∼19.2 %. The proposed ZnO/NiFe2O4 based non-enzymatic UA sensor is capable of selectively detecting UA in the presence of various interferents. UA acts as a biomarker for the diagnosis of different stages of chronic kidney disease (CKD). Hence, the validity of the developed heterostructure was investigated for real time UA sensing using spot urine samples. The recovery percentage was found to be between 95.7 % and 103.5 % further paving way for the use of this electrode for diagnosis of CKD.