The control of glucose concentration is a crucial factor in clinical diagnosis and the food industry. Electrochemical biosensors based on reduced graphene oxide (rGO) and conducting polymers have a high potential for practical application. A novel thermal reduction protocol of graphene oxide (GO) in the presence of malonic acid was applied for the synthesis of rGO. The rGO was characterized by scanning electron microscopy, X-ray diffraction analysis, Fourier-transform infrared spectroscopy, and Raman spectroscopy. rGO in combination with polyaniline (PANI), Nafion, and glucose oxidase (GOx) was used to develop an amperometric glucose biosensor. A graphite rod (GR) electrode premodified with a dispersion of PANI nanostructures and rGO, Nafion, and GOx was proposed as the working electrode of the biosensor. The optimal ratio of PANI and rGO in the dispersion used as a matrix for GOx immobilization was equal to 1:10. The developed glucose biosensor was characterized by a wide linear range (from 0.5 to 50 mM), low limit of detection (0.089 mM), good selectivity, reproducibility, and stability. Therefore, the developed biosensor is suitable for glucose determination in human serum. The PANI nanostructure and rGO dispersion is a promising material for the construction of electrochemical glucose biosensors.

We present a detailed study of the structural and electrical changes occurring in two graphene oxide (GO) samples during thermal reduction in the presence of malonic acid (MA) (5 and 10 wt%) and P₂O₅ additives. The morphology and de-oxidation efficiency of reduced GO (rGO) samples are characterized by Fourier transform infrared, X-ray photoelectron, energy-dispersive X-ray, Raman spectroscopies, transmission electron and scanning electron microscopies, X-ray diffraction (XRD), and electrical conductivity measurements. Results show that MA and P₂O₅ additives are responsible for the recovery of π-conjugation in rGO as the XRD pattern presents peaks corresponding to (002) graphitic-lattice planes, suggesting the formation of the sp²-like carbon structure. Raman spectra show disorders in graphene sheets. Elemental analysis shows that the proposed reduction method in the presence of additives also suggests the simultaneous insertion of phosphorus with a relatively high content (0.3–2.3 at%) in rGO. Electrical conductivity measurements show that higher amounts of additives used in the GO reduction more effectively improve electron mobility in rGO samples, as they possess the highest electrical conductivity. Moreover, the relatively high conductivity at low bulk density indicates that prepared rGO samples could be applied as metal-free and non-expensive carbon-based electrodes for supercapacitors and (bio)sensors.

Graphene-based derivatives, such as graphene oxide (GO) and reduced graphene oxide (rGO), have gained significant attention in the field of electrochemical sensors