| Summary: | This research revealed the effect of carboxyl-functionalization on the mesoporous carbon (MC)-fixed glucose oxidase (GOx) for promoting the properties of bioelectrodes. It showed that the oxidation time, temperature and concentration, can significantly affect MC carboxylation. The condition of 2 M ammonium persulfate, 50 °C and 24 h was applied in the study for the successful addition of carboxyl groups to MC, analyzed by FTIR. The nitrogen adsorption isotherms, and X-ray diffraction analysis showed that the carboxylation process slightly changed the physical properties of MC and that the specific surface area and pore size were all well-maintained in MC-COOH. Electrochemical characteristics analysis showed that Nafion/GOx/MC-COOH presented better electrocatalytic activity with greater peak current intensity (1.13-fold of oxidation peak current and 4.98-fold of reduction peak current) compared to Nafion/GOx/MC. Anodic charge-transfer coefficients (α) of GOx/MC-COOH increased to 0.77, implying the favored anodic reaction. Furthermore, the GOx immobilization and enzyme activity in MC-COOH increased 140.72% and 252.74%, leading to the enhanced electroactive GOx surface coverage of Nafion/GOx/MC-COOH electrode (22.92% higher, 1.29 × 10<sup>−8</sup> mol cm<sup>−2</sup>) than the control electrode. Results showed that carboxyl functionalization could increase the amount and activity of immobilized GOx, thereby improving the electrode properties.
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