The use of supercritical fluid extraction and pressurized fluid extraction for the determination of total petroleum hydrocarbons (TPH), the phthalate content and polycyclic aromatic hydrocarbons (PAH) in soil and river sediment samples is described. Quantification of TPH was performed by FTIR spectrometry and that of phthalates and PAH by GC/MS. Using the above methods gave the same results as the Soxhlet extraction, in addition to time saving and a lower solvent consumption.