| Summary: | The preparation and characterization of a hybrid composite, based on carbon cloth (CC) matrix functionalized with two-dimensional (2D) MoS<sub>2</sub> flakes and MoO<sub>3</sub>, and its use for developing an electrochemical sensor for the determination of riboflavin (RF) is here reported. The 2D-MoS<sub>2</sub>-MoO<sub>3</sub>CC composite was prepared by depositing 2D-MoS<sub>2</sub> nanosheets, obtained by liquid phase exfoliation (LPE), on the surface of a carbon cloth fiber network, previously functionalized with a layer of molybdenum oxide (α-MoO<sub>3</sub>) by radio-frequency magnetron reactive sputtering technique. The 2D-MoS<sub>2</sub>-MoO<sub>3</sub>CC composite was characterized by scanning electron microscopy and energy dispersive X-ray analysis (SEM-EDX), and Raman spectroscopy. An electrochemical sensor has been then fabricated by fixing a slice of the 2D-MoS<sub>2</sub>-MoO<sub>3</sub>CC composite on the working electrode of a screen-printed carbon electrode (SPCE). The 2D-MoS<sub>2</sub>-MoO<sub>3</sub>-CC/SPCE sensor display good electrochemical characteristics which have been exploited, for the first time, in the electroanalytical determination of riboflavin (RF). The sensitivity to RF, equal to 0.67 µA mM<sup>−1</sup> in the linear range from 2 to 40 µM, and a limit of detection (LOD) of 1.5 µM at S/N = 3, demonstrate the promising characteristics of the proposed 2D-MoS<sub>2</sub>-MoO<sub>3</sub>-CC/SPCE electrochemical sensor for the determination of riboflavin.
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