| Summary: | A simple photoelectrochemical (PEC) sensor based on non-modified nanostructured anodic TiO<sub>2</sub> was fabricated and used for a rapid and sensitive detection of glucose. The anodic TiO<sub>2</sub> layers were synthesized in an ethylene glycol-based solution containing NH<sub>4</sub>F (0.38 wt.%) and H<sub>2</sub>O (1.79 wt.%) via a three-step procedure carried out at the constant voltage of 40 V at 20 °C. At the applied potentials of 0.2, 0.5, and 1 V vs. saturated calomel electrode (SCE), the developed sensor exhibited a photoelectochemical response toward the oxidation of glucose, and two linear ranges in calibration plots were observed. The highest sensitivity of 0.237 µA µmol<sup>−1</sup> cm<sup>−2</sup> was estimated for the applied bias of 1 V. The lowest limit of detection (LOD) was obtained for the potential of 0.5 V vs. SCE (7.8 mM) with the fastest response at ~3 s. Moreover, the proposed PEC sensor exhibited relatively high sensibility, good reproducibility, and due to its self-cleaning properties, a good long-term stability. Interfering tests showed the selective response of the sensor in the presence of urea and uric acid. Real-life sample analyses were performed using an intravenous glucose solution, which confirmed the possibility of determining the concentration of analyte in such types of samples.
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