Attributed to high stability and reproducibility, nonenzymatic electrochemical sensors have been extensively utilized in the detection of various chemical substances. In this study, multiwalled carbon nanotube (MWCNT)/Ti‐doped ZnO composite was prepared for fabrication of working electrode used in the detection of glutamate and ascorbic acid. Ti‐doped ZnO particles with the average size of 44.47 ± 4.05 nm were synthesized by the solution combustion technique. Hydrothermal impregnation was employed in preparation of the MWCNT/Ti‐doped ZnO composite. Electrocatalytic activities of the MWCNT/Ti‐doped ZnO composite were examined using the cyclic voltammetry technique. The cyclic voltammograms revealed the reduction reaction of glutamate close to −.5 V, whereas the oxidation reaction of ascorbic acid close to .5 V. Fair electrocatalytic performance, with acceptable sensitivity, limit of detection, and selectivity suggested potential utilization of MWCNT/Ti‐doped ZnO nanocomposite in the detection of ascorbic acid and glutamate.