Abstract: A new sensor based on the grafting of 4-tert-butylcatechol on the surface of a glassy carbon electrode (GC) was developed for the catalytic oxidation of homocysteine (Hcy). The GC-modified electrode exhibited a reversible redox response at neutral pH. Under the optimum conditions cyclic voltammetric results indicated the excellent electrocatalytic activity of modified electrode toward the oxidation of Hcy at reduced over-potential about 350 mV. A linear dynamic range of 0.01–3.0 mM and a detection limit of 1.0 mM were obtained for Hcy. The modified electrode was used as an electrochemical sensor for selective determination of Hcy in human blood.