lectrochemical detection of nitrite was achieved via electrodeposition of gold nanoparticles (AuNPs) onto glassy carbon electrodes, followed by 3‐mercaptopropionic acid (MPA) self‐assembly, enabling attachment of an iron(III) monoamino‐phthalocyanine (FeMAPc) catalyst via amide bond formation. The use of scanning electron microscopy, energy dispersive X‐ray spectroscopy and ultraviolet‐visible spectroscopy realised surface characterisation while cyclic voltammetry and electrochemical impedance spectroscopy techniques were applied for electrochemical interrogation. The electrochemical behaviour of nitrite at the bare (GCE), AuNPs/GCE, FeMAPc/GCE and FeMAPc‐MPA/AuNPs/GCE was further scrutinised using differential pulse voltammetry in phosphate buffer solution (0.1 M PBS, pH 5.8). Overall the FeMAPc‐MPA/AuNPs/GCE resulted in sensitivity 14.5 nA/µM, which was double that of AuNPs/GCE, 2.4 times FeMAPc/GCE and 3.5 times the response at a bare GCE, with linear range 1.9 µM–2.04 mM (PBS, pH 5.8) and LOD 0.21 µM. An interference study revealed that the proposed sensor (FeMAPc‐MPA/AuNPs/GCE) exhibited a selective response in the presence of interfering anions and the analytical capability of the sensor was demonstrated via nitrite ion determination in real water samples.