Firstly, poly[phenyl thiadiazole methacrylamide-co-divinylbenzene-co-2-acrylamido-2-methylpropane sulfonic acid] (PTMAAm-co-DVB-co-AMPS), a new polymer resin was synthesized. This polymer resin was characterized by elemental analyzer, X-ray diffractometer, scanning electron microscope (SEM) and IR spectrometer. The glass column packed with the synthesized polymer resin was used for solid phase extraction (SPE). At the same time, the analytes were separated and preconcentrated from various water, dried vegetables samples and standard reference material (CRM) with SPE and determined by flame atomic absorption spectrometer (FAAS). The experimental conditions of this method such as pH, flow rates of sample, flow rates of eluent, type / concentration / volume of eluent, sample volume and matrix ions were examined. The limits of detection (mu g L-1) were calculated (3s) 0.9 for Mn(II), 1.4 for Cd(II), Co(II) and Zn(II), 1.5 for Cr(III), 2.2. for Cu(II), 1.9 for Pb(II),1.5 for Ni(II) and 1.9 for Fe(III) (n = 21). The low relative standard deviation, 2% (n = 11) and preconcentration factor as 75 for analytes were obtained.