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The Paraiba do Sul River, in the State of Rio de Janeiro, was studied for its water quality, by determining the levels of selected polycyclic aromatic hydrocarbons (PAHs) and pesticides from six sites in two cities, Resende and Campos dos Goytacazes, as they have industrial and agricultural activities. This study was carried out between July 2001 and March 2002. The method involved 200 mL samples taken by off-line, solid phase extraction by OASIS polymeric cartridges followed by gas chromatography-mass spectrometry (GC-MS). Recoveries and standard deviation of pesticides in non polluted real water sample spiked with a standard mixture were 82-119% and less then 20%. For PAH, recoveries and standard deviation were 56-78% and less then 18%, respectively, with exception to acenaphthylene, 23% and 2.7%. Atrazine was detected in the average concentration of 0.231 mug L-1 in two sites in Campos dos Goytacazes, near the sugar-cane power plants and plantations area, while no detection was observed in Resende. Irgarol was observed in Campos dos Goytacazes downtown at 0.138 mug L-1, an area of small boating activities. Benzo[a] pyrene was detected at 0.255 mug L-1 in Resende, near the Presidente Dutra highway. PAHs were not detected in the water samples from Campos dos Goytacazes.