Thiocyanate (SCN) is a hazardous byproduct of the detoxification of cyanide. Even in minute quantity, the SCN has a negative impact on health. Although there are several ways for SCN analysis, an efficient electrochemical procedure has hardly ever been attempted. Here, the author reports the development of a highly selective and sensitive electrochemical sensor for SCN utilizing Poly (3, 4-Ethylenedioxythiophene) incorporated MXene (PEDOT/MXene) modified screen-printed electrode (SPE). The Raman, X-ray photoelectron (XPS), and X-ray diffraction (XRD) analyses support the effective integration of PEDOT on the MXene surface. Further, scanning electron microscopy (SEM) is employed to demonstrate the formation of MXene and PEDOT/MXene hybrid film. In order to specifically detect SCN in phosphate buffer media (pH 7.4), the PEDOT/MXene hybrid film is grown on the SPE surface via the electrochemical deposition method. Under the optimized condition, the PEDOT/MXene/SPE-based sensor provides a linear response against SCN from 10 to 100 µM and 0.1 μM to 1000 μM with the lowest limit of detections (LOD) of 1.44 μM and 0.0325 μM by differential pulse voltammetry (DPV) and amperometry, respectively. For accurate detection of SCN, our newly created PEDOT/MXene hybrid film-coated SPE demonstrates excellent sensitivity, selectivity, and repeatability. Ultimately, this novel sensor can be used to detect SCN precisely in environmental and biological samples.