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In this work, an n-octadecylamine functionalized mesoporous carbon nanocomposite (ODA-MPC) was synthesized, and its novel application was demonstrated by utilizing it as a sorbent in matrix solid-phase dispersion (MSPD) of nine pesticide residues identified by gas chromatography-mass spectrometer. Here, the protection of the sorbent by the mesoporous fiber membrane enabled it to process complex aqueous matrices and made it advantageous to be used in MSPD. The results confirmed the excellent ability of ODA-MPC to remove matrix interferences and reduce matrix effects compared to the traditional solid phase extraction. In particular, the recoveries were 85.0–95.8% (n = 3) with relative standard deviations less than 5%. Additionally, nine pesticide residues in vegetables and fruit were satisfactorily extracted and detected.