In this manuscript, a self-assembled electrochemical sensor was prepared by coating with carbon nanotube (CNT) decorated hydrogel (HG) combining with electrodeposition of methylene blue (MB), and then used for the detection of ascorbic acid (AA). The three-dimensional network of HG has the advantages of large electroactive surface area, rapid diffusion and electron transfer rate, strong adhesive ability and stabilization the polymerized MB. The MB provides high electrocatalytic activity and works as an electron transfer mediator to facilitate the oxidation of AA. The successful synthesis of the hydrogel and the preparation of the sensor are confirmed by scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), atomic force microscopy (AFM) and X-ray photoelectron spectroscopy (XPS). The layer-by-layer assembly was identified by AFM with the heights of 22.1 nm and 186.8 nm for hydrogel and MB layers, respectively. Under the optimal conditions, the sensor has a linear range of 0.1 mM to 10 mM and a detection limit of 0.05 mM. What’s more, the prepared sensor also exhibits good stability (current retention of 91.22% after 100 cycles for testing 0.25 mM AA), excellent anti-interference ability, good reproducibility (RSD of 4.26% for five independent experiments), excellent opertional stability (RSD of 1.66% for 30 consecutive AA additions), fast response time (< 4 s) and has satisfied results in the detection for AA in vitamin C tablets.

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