In this work a new sensor in nano size containing Mn-nanoparticles decorated organo-functionalized nanosized SiO 2 -Al 2 O 3 mixed-oxide support was developed as a new electrocatalysis for oxidation of organic compounds such as captopril. SiO 2 -Al 2 O 3 mixed-oxide were functionalized with Schiff base ligand and thereatfer, in the next step, Mn-nanoparticles were prepared over the organofunctionalized SiO 2 -Al 2 O 3 mixed-oxide. The synthesized materials were characterized with different methods such as FT-IR spectroscopy, UV-vis, CHN elemental analysis, TEM, ICP-OES, cyclic voltammetry, and electrochemical impedance spectroscopy. Under the optimum conditions (pH 7.0) in cyclic voltammetry, the oxidation of the captopril was occurred at a potential about 650 mV at a surface of the modified electrode. Linear sweep voltammetry exhibited two wide linear dynamic ranges of 0.30-5.0 and 5.0-340 mmol L À1 captopril. The detection limit was found to be 0.095 mmol L À1 captopril. The kinetic parameters such as electron transfer coefficient and catalytic reaction rate constant were also determined. Finally, the modified electrode used as a novel electrochemical sensor for the determination of captopril in real samples such as pharmaceutical, patient and safe human urine.