This preliminary study presents first data on organochlorine pesticides (OCPs) and polychlorinated biphenyls (PCBs) concentrations in water and sediment samples of Devolli River. It is located in Southeast Albania, in Korca field, which is the second agricultural area in Albania. Sampling stations water of Devolli River were selected in eight different stations, starting from its stream (Gramozi Mountain) to the end of Korca field, near Banja hydropower (Gramshi region). Sampling of water and sediments were done in the same stations, in December 2018. Pesticides were used in the past in this area for many years mainly for agricultural purposes. Also, basin of Devolli River is affected from industrial activity and urban pollution, too. Water irrigation and rainfall contribute on their transport from soil to underground and surface waters. Organochlorine pesticides and PCB are very stable compounds that can be found in the environment for many years after their application. Liquid-liquid extraction was used for isolation of OCPs and PCBs in water samples while ultrasonic extraction was used for their extraction in sediment samples. The simultaneous analysis of organochlorine pollutants in water samples was performed by gas chromatography technique using electron capture detector (GC/ECD). Rtx-5 capillary column (30 m x 0.33 mm x 0.25 um) was used for separation of 17 organochlorine pesticides according EPA 8081A and 7 PCB markers. Relatively high concentrations of organochlorine pesticides were detected in water and sediment samples of Devolli River compare with other rivers of Albania. Their presence can be due to their previous use in Korca field. Volatile PCBs were found in higher concentration in water samples because of atmospheric deposition. Levels of some individual pesticides in surface water samples of Devolli River were found to be higher than permitted levels according to Albania and EU norms. Responsible authorities should be done continues monitoring in water samples of this river.