This report focuses on evaluating the influence of structural and physical properties of MoS2 material on electrochemical behaviors as well as sensing performance toward the detection of targeted chloramphenicol (CAP) molecules. The various MoS2 samples were fabricated via a simple ultrasonication route at different experimental times. Through using X-ray diffraction (XRD), Raman, and scanning electron microscopy (SEM), structural and chemophysical characterizations were analyzed and discussed. Furthermore, from electrochemical measurements such as CV, EIS, DPV, and CA, the recorded results exhibited strong differences in the current response and the kinetic parameters of redox reactions among the proposed electrodes. It is also interesting to note that the proposed possible hypotheses and suitable mechanisms are particularly necessary to explain in more detail the important changes in kinetic parameters and sensing performance at MoS2-modified electrodes. Among them, the MoS2-3 sample with good crystallinity, high purity, low intrinsic thickness, and particularly, a defect-rich structure offered remarkable advances compared with that of other materials. As a result, this electrode exhibited an extended linear range (0.5 - 50 μM), a lower detection limit (0.1 μM), good repeatability, and high selectivity.