This work described the sonohydrolysis of Bi(NO3)3 into Bi2O3 and simultaneous sonochemical exfoliation of graphite into graphene sheets in the alkaline environment and its electocatalytic performance towards the detection of anti-depression drug imipramine (IMPR). The ultrasound (37/80 kHz; 60 W) effectively hydrolyzed the Bi(NO3)3 into a single crystalline monoclinic phase of Bi2O3 nanotiles in the alkaline condition. And also, the sonochemical reaction condition can trigger the lamellar particles on the graphite bulk surface and allowed to exfoliated the graphite (EG) into graphene nanosheets as well. The material characterizations are done by XRD, Raman, FESEM, and HRTEM. It shows the α-Bi2O3 nanotiles along with EG nanosheets with high crystallinity and low defects. The (0 0 2) plane in XRD confirms the high crystalline nature of EG. The monoclinic stretching vibrations (90-600 cm-1) confirms the Raman modes of Bi2O3. The prepared Bi2O3-EG composites are subjected to the electrochemical determination of IMPR which revealed appreciable analytical performances. The results showed that the Bi2O3-EG exhibits better results in the 3 h sonication process. Bi2O3-EG-3 exhibited a good linear range (0.02-82.3 µM) and an acceptable limit of detection (6 nM). And also Bi2O3-EG-3 exhibits the significant tolerance limit when compared to other potential interfering compounds.