Electropolymerized neutral red, thionine, and aniline were used as part of hybrid nanocomposite conductive polymers, to create an amperometric reagent-less biosensor for glucose determination. The structure of the obtained polymers was studied using infrared (IR) spectroscopy and scanning electron microscopy. Electrochemical characteristics were studied by cyclic voltammetry and impedance spectroscopy. It was shown that, from the point of view of both the rate of electron transfer to the electrode, and the rate of interaction with the active center of glucose oxidase (GOx), the most promising is a new nanocomposite based on poly(neutral red) (pNR) and thermally expanded graphite (TEG). The sensor based on the created nanocomposite material is characterized by a sensitivity of 1000 ± 200 nA × dm³/mmol; the lower limit of the determined glucose concentrations is 0.006 mmol/L. The glucose biosensor based on this nanocomposite was characterized by a high correlation (R² = 0.9828) with the results of determining the glucose content in human blood using the standard method. Statistical analysis did not reveal any deviations of the results obtained using this biosensor and the reference method. Therefore, the developed biosensor can be used as an alternative to the standard analysis method and as a prototype for creating sensitive and accurate glucometers, as well as biosensors to assess other metabolites.

Biomembranes based on an organosilica sol–gel matrix were used to immobilize bacteria Paracoccus yeei VKM B-3302 as part of a biochemical oxygen demand (BOD) biosensor. Diethoxydimethylsilane (DEDMS) and tetraethoxysilane (TEOS) were used as precursors to create the matrix in a 1:1 volume ratio. The use of scanning electron microscopy (SEM) and the low-temperature nitrogen adsorption method (BET) showed that the sol–gel matrix forms a capsule around microorganisms that does not prevent the exchange of substrates and waste products of bacteria to the cells. The use of DEDMS as part of the matrix made it possible to increase the sensitivity coefficient of the biosensor for determining BOD by two orders of magnitude compared to a biosensor based on methyltriethoxysilane (MTES). Additionally, the long-term stability of the bioreceptor increased to 68 days. The use of such a matrix neutralized the effect of heavy metal ions on the microorganisms’ catalytic activity in the biosensor. The developed biosensor was used to analyze water samples from water sources in the Tula region (Russia).