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This study describes titanium and zirconium incorporations into a FAU zeolite and subsequent modification with nickel hexacyanoferrate.The obtained materials (ZTiNiH and ZZrNiH) were characterized by Fourier Transform Infrared Spectroscopy (FTIR), Scanning Electron Microscopy (SEM), X-ray Dispersive Energy Spectroscopy (EDS), Porosity and Surface Area and Cyclic Voltammetry (CV). The cyclic voltammograms applied to the modifed ZTiNiH and ZZrNiH graphite pastes indicate sensitivity to isoniazid (IZN). The modifed ZTiNiH graphite paste electrode displayed a linear analytical curve response from 4.0× 10–5 to 7.0× 10–4 mol L− 1 and limit of detection of 4.9×10− 5 mol L− 1, while the modified ZZrNiH electrode presented a linear analytical curve response from 1.0×10− 5 a 3.0×10− 4 mol L− 1 and limit of detection of 2.0×10− 5 mol L− 1. After catalytic IZN electro-oxidation, a study concerning the main IZN interferents was performed and its recovery from a synthetic urine sample was assessed. The obtained ZTiNiH and ZZrNiH materials are noteworthy for their good limit of detection and recovery eficiency when applied to real samples, thus comprising potential candidates for the development of electrochemical sensors aiming at IZN detection.