Nitrogen‐doped mesoporous carbons (N‐MCs) are promising materials for electrochemical sensors or biosensors. However, facile and effective methods for the preparation of N‐MCs for electrochemical detection of dopamine (DA) are required. A molten‐glucose‐assisted hard‐template approach has been developed to synthesize N‐MC materials by in situ introduction of nitrogen precursors, including ethylenediaminetetraacetic acid disodium salt (EDTA), dicyandiamide, and melamine. The combined characterization of X‐ray diffraction (XRD), N2 sorption, scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X‐ray photoelectron spectroscopy (XPS) indicate the successful preparation of N‐MC materials. Most importantly, after detailed examination by cyclic voltammetry (CV) and differential pulse voltammetry (DPV), N‐MC obtained by using melamine as precursor (designated as N‐MC‐MA) displays good catalytic activity for electrochemical oxidation of DA. The N‐MC‐MA‐based DA sensor shows a linear range from 0.2–8 μm with a detection limit of 0.05 μm in the presence of ascorbic acid (AA) and uric acid (UA), thus showing excellent sensitivity and selectivity for electrochemical DA detection.
