We have successfully prepared the titanium dioxide (TiO 2 ) nanoparticles (NPs) and sulfur-incorporated graphitic carbon nitride (S-GCN)-modified carbon paste electrode (CPE). The CPEs modified with TiO 2 NPs and S-GCN were employed for detecting and quantifying the skeletal muscle relaxant cyclobenzaprine hydrochloride (CBP) using cyclic voltammetry and square wave voltammetry (SWV) techniques. Optimal electrochemical conditions were indicated by the pH study results, with the highest peak current observed at a physiological pH of 7.4. The electrochemical process was determined to involve an equivalent number of protons (H + ) and electrons (e − ). The concentration variation of CBP (ranging from 0.06 to 10 × 10 −7 mol L −1 ) was explored using SWV. The limits of detection and quantification were determined as 6.4 × 10 −9 and 2.1 × 10 −8 M, respectively. The proposed electrode configuration was applied to analyze real samples, including water, biomedical, and pharmaceutical specimens.