Nanosized cobalt aluminate (CoAl2O4) was prepared by thermolysis of heteronuclear coordination compound, namely [Al2Co(C2O4)4(OH2)6]. The synthesized precursor was characterized by chemical analysis, vibrational spectra and thermal analysis. The cobalt aluminate obtained after a heating treatment of the precursor at 700C was characterized by IR, XRD, TEM coupled with SAED measurements. Two types of carbon-based electrodes, glassy carbon and boron-doped diamond electrodes were decorated with the obtained cobalt aluminate in order to enhance the electroanalytical performance for the tetracycline (TC) detection in the aqueous solutions. Cyclic voltammetry technique was used to determine the effect of the nanosized CoAl2O4 on the electrochemical oxidation of C and as consequence, for TC detection at both carbon-based electrodes. The obtained cobalt aluminate exhibited the electrocatalytic activity toward TC detection in direct relation with the type of the carbon substrate, which allowed enhancing the electroanalytical parameters of TC detection in the aqueous solution.