The two-dimensional metal chalcogenides (TMC) have been fascinated more interest in a wide range of electrochemical applications owing to their high conductivity and excellent catalytic performance. Herein, we report the electrochemical sensor based on the urchin-like structured bimetallic strontium sulfide and bismuth sulfide (SrS/Bi2S3) nanocomposites prepared by a simple hydrothermal method. For the first time, the prepared SrS/Bi2S3 nanocomposites were used to sense the carcinogenic herbicide maleic hydrazide (MHZ) in food and water samples. Moreover, the analytical performance of SrS/Bi2S3 modified screen-printed carbon electrode (SrS/Bi2S3/SPC electrode) shows excellent results with a wide range of (0.01–104 µM and 104–814 µM), and the detection limit of 1.8 nM towards the MHZ detection. Furthermore, the developed sensor expressed good selectivity, repeatability, stability, and reproducibility. Finally, the real sample analysis of the developed sensor was tested in the potatoes and river water samples, which shows the recoveries of 97.8–98.9% and 97.2–98.2%.