Nowadays, Furosemide (FUR) is of the diuretic drugs that most has been used for various purposes such as treatment of chronic diseases and chemical adulterant in slimming health foods. Thus, a approach rapid, facile and low-cost for detection of FUR in real samples is crucial for accurate monitoring of the state of human health. In this work, Co 3 [Co(CN)6]2/Fe3O4/β-cyclodextrin(CD)-modified spent Zn-C batteries graphite electrodes (Co3[Co(CN)6]2/Fe3O4-CD/GrCE) was developed by the the first time for electrochemical detection of FUR. The Co 3 [Co(CN)6]2/Fe3O4-CD hybrid nanocomposite was prepared by chemical precipitation reactions followed by a sonochemical step, in where the self-assembly process was governed by magnetic interactions between nanoparticles. Transmission electron microscopy revealed a nanostructure consisting of aggregates of ultra-small Fe 3 O 4 nanoparticles covering the surface of the Co 3 [Co(CN) 6 ] 2 nanoparticles, this structure was coated by a shell of β-CD polymer. The composition and structural properties were investigated by Fourier transform infrared spectroscopy (FTIR) and X-ray diffraction. As results, hybrid nanocomposite exhibited good crystallinity and main chemical groups referents to the Co 3 [Co(CN) 6 ] 2 , Fe 3 O 4 and β-CD. While the voltammetric characterization of the modified GrCE in the alkaline supporting electrolyte promoted the formation of CoOOH/Fe 3 O 4 -CD casting films with high electrical conductivity, stability and a large electrochemical response. In the presence of FUR was observed a significant reduction in the current density of the oxidation of CoOOH to CoO 2 , this behavior is possibly associated the limitation of the OH - ions difusion in the interlayer space of CoOOH. The anodic current density inhibition mechanism was employed to detect FUR by linear scanning voltammetry (LSV). The LSV response Co 3 [Co(CN) 6 ] 2 /Fe 3 O 4 -CD/GrCE in presence of FUR was linear working range from 0.05 to 4.2 μM, with excellent sensibility of 4012.1 A mol -1 L cm -2 and low detection limit (LOD) of 7.65 nmol L -1 . The facile detection method also exhibits high selectivity, stability, and good reproducibility, which suggests practical feasibility of large-scale manufacturing. Therefore, the high ultrasensitive, time-saving and low-cost approach electrochemcial sensor reported here present a great potentials for detection and monitoring of FUR in drug, human urine samples and dietary food supplements.