Implementation of a mixed-mode solid-phase extraction is discussed as a promising approach for matrix clean-up in multiresidue/multimatrix methods. Sorbents characterized by different mechanisms of sorption such as reversed-phase (graphitized carbon), weak anion exchange (primary-secondary amine) and strong anion exchange (quaternary amine) were studied for their effectiveness in the removal of the matrix co-extractives in grains, fruits and vegetables for trace pesticide residues analysis. The pesticide residues were determined by gas chromatography with electron capture and mass spectrometric detection. Recoveries data of 25 pesticides from different groups at 0.01 mg/kg level ranged between 73 and 117% and with standard deviation below 15%. The limits of quantification were below or at 0.01 mg/kg.