<p>An electrochemical sensor based on a MoS₂-Ti₃C₂T_x nanocomposite-modified screen-printed carbon electrode (SPCE) was developed for the separate and simultaneous determination of nitrite and caffeine. The morphological and structural characterization of the MoS₂-Ti₃C₂T_x nanocomposite was performed using scanning electron microscopy (SEM), X-ray diffraction (XRD) techniques, and Fourier transform infrared spectroscopy (FTIR). The electrochemical performance was studied using Cyclic Voltammetry (CV), and Differential Pulse Voltammetry (DPV) techniques. The integration of MoS₂ and Ti₃C₂ enhanced the electrocatalytic activity and electron transfer efficiency of the sensor, resulting in distinct and well-defined oxidation peaks for both analytes. The electrochemical reaction revealed a diffusion-controlled and reversible redox process, as confirmed by the linear relationship between the anodic peak potential and the logarithm of the scan rate. The sensor exhibited optimal performance at physiological pH, with excellent sensitivity and selectivity. The developed MoS₂-Ti₃C₂T_x /SPCE sensor demonstrated high sensitivity, measured at 11.63 µA µM⁻¹ cm⁻² for nitrite and 13.65 µA µM⁻¹ cm⁻² for caffeine. The corresponding limits of detection (LOD) were estimated to be 0.04 µM and 0.07 µM, with linear range 9.6–332 µM for nitrite and 12.6–225 µM for caffeine, respectively. Additionally, the modified electrode exhibited remarkable stability and reproducibility at MoS₂-Ti₃C₂T_x /SPCE. The practical applicability was demonstrated through real sample analysis in sausage, spinach, Coca-Cola, and coffee, achieving high recovery rates (95.5-106.2%) and low relative standard deviations (≤ 2.8%). This study demonstrates that the MoS₂-Ti₃C₂T_x nanocomposite can be effectively utilized for detecting harmful substances in the food industry.</p>