Pesticide residues in surface water and sediments are extremely important because of their potential impacts on aquatic ecosystems and their implications on drinking water sources. Pesticide contamination of fresh water is causing concern with respect to long-term and low-dose effects of pesticides on public health, as well as their impact on no target species. Thus, intensive research on the fate and transport of pesticides in the environment is needed. Gas chromatography (GC) with electron-capture detection (ECD) and nitrogen-phosphorous detection (NPD) were employed for the identification of different pesticides in water and sediment samples. For this purpose, extraction procedure with dichloromethane and ethyl acetate were used. The aim of our work was the quantitative determination of pesticides from several compound classes in water and sediment from Golcuk National Park (Turkey). In GC-NPD/ECD, the detection limits were between 2.75-135 ng/L for the studied pesticides, recoveries ranged from 90 to 102% in samples and the relative standard deviations were in the range 1 to 10%. The correlation coefficients obtained from calibration curves of the pesticides standards were found to be 0.999. No pesticides residue was detected in the samples analyzed. This result is highly significant because of its impacts on public health and animals living in the Golcuk National Park.