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In this study, a new organic–inorganic material, based on an alpha-metatungstate [H 2 W 12 O 40 ] 6 − cluster, was synthesized via the hydrothermal method by using aminopyridinium (APy) + cations as the hybrid material, and characterized by FT-IR and UV spectra analysis. The hybrid composite was immobilized on a gold electrode decorated with gold nanoparticles (AuNPs) and the modified electrode exhibited excellent electrocatalytic activities towards the reduction of H 2 O 2 at neutral pH with a response time of < 10 s. The H 2 O 2 response at the modified electrode displays a linear response ranging from 40 μM to 10 mM. Based on the H 2 O 2 reduction activity, the (APy) 6 [H 2 W 12 O 40 ] composite was successfully used for the fabrication of a novel enzymatic glucose biosensor. The glucose oxidase enzyme (GOx) was immobilized onto the hybrid composite on AuNPs/gold electrodes; the (APy) 6 [H 2 W 12 O 40 ] composites were used as both mediation and bridging molecules. A multilayer architecture was constructed from hybrid POM alternating with (GOx), using glutaraldehyde as a covalent attachment cross-linker. Cyclic voltammetry (CV), SWV and chronoamperometry were used to determine the electrochemical properties of the mediator and characterize its reaction with (GOx). The resulting glucose biosensor exhibits a wide linear response for glucose from 40 μM to 10 mM with a sensitivity of 15.0 μA mM − 1 . [ABSTRACT FROM AUTHOR]