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• Fabrication and characterization of a novel MnTMPyP/TaMoO 6 nanocomposite were performed for the first time. • The simultaneous determination of DA and AA at MnTMPyP/TaMoO 6 was performed, and it has a low detection limit. • MnTMPyP/TaMoO 6 nanocomposite has satisfactory stability, good reproducibility and strong anti-interference property. • The performance of MnTMPyP/TaMoO 6 nanocomposite for AA and DA in actual samples was evaluated. [Display omitted] A novel highly selective nanocomposite MnTMPyP/TaMoO 6 was successfully synthesized and developed for simultaneous detection of Ascorbic acid (AA) and dopamine (DA). Firstly, the host material LiTaMoO 6 was synthesized by the high temperature solid phase method. After the exfoliation/restacking process of the host material, the nanocomposite was formed through electrostatic self-assembly. The structure and morphology were characterized using X-ray diffraction (XRD), scanning electron microscope (SEM), transmission electron microscope (TEM), energy dispersive spectrometer analysis (EDS), ultraviolet-visible (UV–vis) and Fourier transform infrared spectrometer (FTIR). And the electrochemical behaviors of the modified electrode were further explored by cyclic voltammetry (CV), electrochemical impedance analysis (EIS), and differential pulse voltammetry (DPV). Under the optimal conditions, the MnTMPyP/TaMoO 6 provides a high sensitivity and selectivity in detecting AA and DA with linear response ranges of 12–674 μM. The resulting detection limit is also calculated as 0.97 and 0.54 μM, respectively. In addition, the MnTMPyP/TaMoO 6 nanocomposite exhibits excellent stability, reproducibility, and good anti-interference. [ABSTRACT FROM AUTHOR]