The pollution level and source of perfluoroalkyl substances (PFASs) in mainstream and tributary of Daling River in northeast China were investigated in present study. Concentrations of PFASs in surface water and sediment ranged from 4.6 to 3,410 ng/L and from 0.08 to 2.6 ng/g dry weight, respectively. The lowest levels of PFASs were found in vicinity of a drinking water source located in upstream of Daling River. Xihe tributary, which is adjacent to two local fluorine industrial parks, contained the highest level of PFASs. Short-chain PFASs, including perfluorobutanoic acid and perfluorobutane sulfonate, were of higher levels due to their emerging as alternative products for perfluorooctane sulfonate. High level of perfluorooctanoic acid was also found in Daling River. Based on these results, it can be concluded that the relatively severe pollutions of Xihe tributary were caused by long-term development of the two local fluorine industry parks.