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The SiO2/TiO2/Nb2O5 material was set by the sol–gel method and was characterized by several techniques through thermogravimetric, spectroscopic, and textural analyzes. For the two synthesized materials, the specific surface area was 350.0 and 494.0 m2 g−1 (SiTiNb-A and SiTiNb-B, respectively). An enhance of the crystalline order with the temperature increase of the thermal treatment was observed. Through X-ray Photoelectron Spectroscopy analysis, the binding energy values for the Ti 2p and Nb 3d levels showed the insertion of Ti and Nb atoms in the silica matrix. The Electron Dispersive Spectroscopy analyses also confirmed the high dispersion of the metals presented on the materials surface. The Thermogravimetric Analysis showed weight loss for the of 37.6% (SiTiNb-A) and 29.7% (SiTiNb-B). The presence of the crystalline phases TiO2-anatase and monoclinic-Nb2O5 in the materials was confirmed through the data obtained by association of powder X-ray Diffraction and FT-Raman. Values obtained from optical band-gap aimed the dependence of the oxides concentration and the calcination temperature. Finally, the pyridine adsorption studies have indicated the presence of Lewis and Brønsted acid sites.

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(designated as SiAlNb and SiAlTi, respectively), obtained using the sol-gel method were used to immobilize chloroperoxidase. Hydrogen peroxide was quantified using potassium hexacyanoferrate(II) as a redoxmediator and amperometric measurements at 0.0 V vs. Ag/AgCl/Cl À (3 M). The SiAlTi biosensor presented higher sensitivity than the SiAlNb biosensor, however, the first one did not present a good response regarding time. The developed biosensor using the SiAlNb mixed oxide provided good signal levels, good linearity, good stability (retaining approximately 70% of its original response after 6 weeks of usage), a low detection limit (3 mM), good sensitivity, a suitable working range (from 4 to 19 mM), fast response and good repeatability. The recovery of the amperometric method for the detection of hydrogen peroxide in synthetic samples was approximately 100 AE 2%, and for Listerine® Whitening PreBrush Rinse samples fortified with 1, 2 and 3% (v/v) of hydrogen peroxide, it was 100 AE 3%.