In this study, CuAlO2/Al2O3 micro-sphere was prepared by sol-gel techniques and annealed under N2-atmosphere. The microsphere composite materials physio-chemical properties were studied using various analytical techniques. The surface morphology prepared materials were observed from the field-emission scanning electron microscopy with spherical structure. The surface area and the surface morphology were explored using the Brunnauer-Emmmett-Teller method. In this research, we studied a CuAlO2/Al2O3 microspheres decorated screen printed carbon electrode (SPCE) utilized to detected the furaltadone (FLT). The electrochemical active surface area has determined using ferric cyanide system and randles-sevick equations. The CuAlO2/Al2O3 microspheres electrochemical ability was analysed using cyclic voltammetry and differential pulse voltammetry towards detection of FLT. These CuAlO2/Al2O3 microspheres decorated electrodes exhibited excellent electrochemical sensor with a limit of detection and sensitivity is 20 nM and 12.7845 μA μM-1 cm-2, respectively. Moreover, the CuAlO2/Al2O3 microspheres/SPCE electrodes exhibit excellent stability, repeatability, reproducibility, and higher sensitivity. The decorated sensor electrode real time applications were successfully studied to analyzing FLT in river and bond water with excellent recovery results.