The electrochemical sensor is receiving much attention because of the evolving on-time sensing technology. It is crucial to develop new catalysts for electrochemical sensor applications with favorable physicochemical, electrocatalytic properties and good conductivity to meet the demands of on-time monitoring applications. The excellence of this research work is the preparation of Ti3C2TX@MCO nanocomposite by ultra-sonication method for the sensing of p-Nitrotoluene (p-NT). The prepared electrode material exhibits excellent electrocatalytic properties towards the sensing of p-NT compared with other electrodes. The p-NT was quantified by Differential Pulse Voltammetry (DPV) and Amperometric (i-t) techniques. The good linear range was observed by DPV (3–1860 μM) and i-t method (0.18 – 4170 μM). The calculated limit of detection (LOD) from DPV and i-t methods are 93.5 and 35.1 nM, respectively. The sensitivity values calculated from DPV, and i-t methods are 1.68 µA/µM. cm2 and 1.71 µA/µM. cm2, respectively. The proposed sensor system exhibits better selectivity, reproducibility, repeatability and stability for sensing of p-NT. A real time p-NT detection study was conducted using environmental water samples.