This study is focused on optimization of preconcentration procedure of trace amounts of platinum group metals (PGMs) by solid phase extraction. Amberlite polystyrene-divinylbezene based sorbent was used for this purpose. Under the optimizing process were optimize number of parameters such as pH value of sorption; type and concentration of complexing agent; concentration and type of cationic surfactant; type, pH, and volume of eluent mixture; acidity of final solution and various interfering influences (presence of various ions, matrix effects). Ammonium-pyrrolidindithiocarbamate, thiourea, 4-(2-pyridylazo) resorcinol and 8-hydroxyquinoline-5-sulfonic acid were used as complexing agents for PGMs. Sorbent was conditioned using cationic surfactant solution. Benzyldimethyltetradecyl ammonium chloride, N-(alpha-carbethoxypentadecyl)trimethyl ammonium bromide and benzyldimethyldodecyl ammonium bromide were tested. Mixture of acetonitrile and HCl was proved as eluent. The influences of various concentrations of hydrochloric acid during the complexation, elution and partial evaporation of the eluent prior the determination were tested. Effects of various elements and ions were studied during the sorption and retention on the above mentioned sorbent. Simultaneous determination of PGMs was performed by ICP-MS spectrometer using helium collision cell and internal standard. Detection limits for individual elements at discussed conditions were evaluated. The optimized method of solid phase extraction was applied to spiked real water samples and lichens for testing influences of matrix and efficient of sorption process. It was discovered that recovery ratio of sorption process is diverse for individual studied elements. Acceptable results was achieved for Platinum and Palladium which showed recovery ratio about 100 % and 95 % for Osmium.