An on-line combination of gel permeation chromatography and gas chromatography has been designed using either a laboratory-built or a commercially available LC-GC apparatus to determine organophosphorus pesticides in olive oil. Gel permeation chromatography was used for sample pretreatment, viz. to separate the low-molecular-mass pesticides from the higher-molecular-mass fat constituents of the oil. A mixture of n-decane and the azeotropic mixture of ethyl acetate and cyclohexane was found to give an adequate separation between the fat and the organophosphorus pesticides. The pesticide-containing fraction, monitored by a UV detector, was transferred on-line to the gas chromatograph using a loop-type interface. n-Decane (6%, v/v) was added to the eluent in order to widen the application range of the transfer technique towards more volatile pesticides. After solvent evaporation through the solvent vapour exit and subsequent GC separation, the compounds were selectively detected with a thermionic or a flame photometric detector. The set-up allowed the direct analysis of oil samples after dilution in the gel permeation chromatography eluent without further sample clean-up. Detection limits were about 5 and 10 μg/kg with the thermionic and the flame photometric detector, respectively, when using an injection volume of only 30 μl of the 20-fold diluted oil. The total procedure was linear in the 0.01-10 mg/kg range for both detectors. For twenty organophosphorus pesticides, the relative standard deviations were 3-13% at the 20-60 μg/kg level.