An amorphous and mesoporous silica/titania (SiTi) material was synthesized by sol-gel method and its surface was modified with gold nanoparticles (AuNP) previously stabilized in a chitosan solution. The presence of small AuNP, with diameter lower than 10 nm was confirmed by transmission electron microscopy (TEM) and UV–Vis spectroscopy. Carbon paste electrodes were prepared to test the electrochemical properties by using cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) in [Fe(CN)6]3−/4− solution probe whereby the material silica-titania/gold nanoparticles (SiTi/AuNP) showed a huge improvement in the redox peak current and low charge transfer resistance. This electrode presented a good response for both norepinephrine and dopamine by means of square wave voltammetry (SWV) measurements; great sensitivity for both analytes, in an extensive linear range, was obtained. The limits of detection were 0.35 μmol L−1 and 0.57 μmol L−1 for norepinephrine and dopamine, respectively. Additionally, this electrode showed high selectivity for both analytes and it was applied in the simultaneous determination of norepinephrine and dopamine. The sensor was also tested in simulated biological fluids presenting a good recovery. The SWV electrochemical response of norepinephrine was also investigated in the presence of possible interferers such as uric acid, ascorbic acid and glucose and there was no significant interference. The prepared electrode also exhibits good reproducibility for norepinephrine detection, with relative standard deviation of 5.19%.