Oxymetazoline, a nasal decongestant drug was investigated by a sensitive, simple and reproducible electrochemical method using Titania (TiO2) nanoparticles and carboxyl group functionalized multi-walled carbon nanotubes fabricated on glassy carbon electrode using cyclic voltammetry and differential pulse voltammetry. The possible electro-oxidation mechanism of this drug was also studied in detail. The performance of designed method was determined by electrochemical impedance spectroscopy, cyclic voltammetry and anodic stripping differential pulse voltammetry. The obtained results revealed enhanced electrochemical behavior of oxymetazoline as compared to bare glassy carbon electrode. Under optimum conditions i.e. buffer pH; pH 7.0 phosphate buffer solution, accumulation potential; 0 V, and accumulation time; 180 s, the differential pulse voltammetric response of oxymetazoline was probed between the linear concentration range of 0.12 mu M to 1.5 mu M in aqueous medium containing pH 7.0 PBS and 20% methanol. The limit of detection of oxymetazoline was evaluated as 4.40 nM. Moreover, the developed sensing method was validated for its practical application in nasal spray with excellent recovery.