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Cationic iron (III) tetrakis-5, 10, 15, 20-( N-methyl-4-pyridyl) porphyrin (Fe IIITMPyP) was intercalated into layered semiconductor KNb 3O 8 by ion-exchange method. The target product was characterized by XRD, Fourier transform infrared, UV–vis, and TGA. Fe IIITMPyP forms an inclined monolayer between Nb 3O 8− nanosheets and endues the nanocomposite with excellent electrochemical catalytic activities. The target nanocomposite modified glass carbon electrode shows good electrocatalytic activities for the oxidation of ascorbic acid (AA); the catalytic mechanism was proposed. Differential pulse voltammetric technique was used for detection of AA in neutral aqueous solution; a detection limit of 4.2 × 10 −5 M was obtained, and the modified electrode showed good reproducibility in electrochemical detection. [ABSTRACT FROM AUTHOR]