A novel cobalt-doped two-dimensional molybdenum diselenide/polypyrrole hybrid-based carbon nanofiber (Co/MoSe2/PPy@CNF) was prepared using the hydrothermal method followed by electrospinning technique. The structural and morphological properties of the 2D-TMD@CNF-based hybrids were characterized through X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), energy-dispersive spectrometry (EDS), and transmission electron microscopy (TEM). The Co-MoSe2/PPy@CNF exhibited large surface area, porous structure, and improved active sites due to the synergistic effect of the components. The electrochemical and electrocatalytic characteristics of the 2D-TMD@CNF-modified electrodes were also investigated using cyclic voltammetry (CV) and differential pulse voltammetry (DPV) techniques. The Co/MoSe2/PPy@CNF electrode was used as an electrochemical sensor for simultaneous detection of ascorbic acid (AA), dopamine (DA), and uric acid (UA) and showed enhanced catalytic activity and sensitivity. Using DPV measurements, the Co/MoSe2/PPy@CNF demonstrated wide linear ranges of 30–3212 μM for AA, 1.2–536 μM for DA, and 10–1071 μM for UA with low detection limits of 6.32, 0.45, and 0.81 μM, respectively. The developed sensor with the Co/MoSe2/PPy@CNF-modified electrode was also applied to a human urine sample and gave recoveries ranging from 94.0 to 105.5% (n = 3) for AA, DA, and UA. Furthermore, the Co/MoSe2/PPy@CNF-based sensor exhibited good selectivity and reproducibility for the detection of AA, DA, and UA.
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