Hybrid xerogel (H5) crafted from guar gum−gelatin dual-templated polymerization of tetramethoxysilane (TMOS) behaved as an effective carrier support for glucose oxidase (GOX). H5 has been characterized using Fourier transform spectroscopy (FTIR), X-ray diffraction (XRD), Field emission scanning electron microscopy (FESEM), BET surface area studies, and Zeta potential and particle size distribution analysis. Under optimized conditions, H5−GOX showed a much higher bioactivity (20.73 U mg −1 ) than free GOX (9.26 U mg −1 ). The kinetic parameters of free GOX (K M = 13.988 mg mL −1 , V max = 1.785 μmole mL −1 min −1 ) and H5−GOX (K M = 5.403 mg mL −1 , V max = 1.75 μmole mL −1 min −1 ) revealed that immobilization could enhance the substrate affinity of GOX, although it did not alter the enzymatic reaction rate. H5−GOX retained ∼96% of its initial bioactivity with 15 days of storage as a dry solid at room temperature. Recycling of H5−GOX showed only marginal loss in bioactivity up to six cycles.