A sensitive method for the high-performance liquid chromatographic determination of five organophosphorus pesticides (paraoxon, methyl-parathion, ethyl-parathion, guthion and fenitrothion) in fruits and tap and river water samples is described. For the determination of pesticides in fruits a simple and rapid sample preparation procedure was developed that allowed pesticides to be determined at 50–100 μg/kg levels with recoveries ranging from 83 to 118% and relative standard deviations below 6%. The determination of pesticide residues in surface water samples was also successfully accomplished. Concentrations at sub-ppb levels can be measured by using a solid-phase concentration step, the recoveries being over 80%. In analyses of both fruits and surface waters, the sensitivity levels achieved were 2–10 times lower than legal limits admitted in the European Economic Community.