The current study investigated the levels of multi pesticide residues in the highly consumed types of Nile fish in Egypt;tilapia and cat fish. Total of 50 Nile tilapia (Oreochromis niloticus) and 50 African catfish (Clarias gariepinus) collected from two areas in Assiut city, where most industries are situated beside the agricultural activities and raising farm animals are the main activities. The first area; Elwasta, there is a facility of electrical power station, and the second area; Mankbad in which the cement factory is there. Fish samples were analyzed by High Resolution Gas Chromatography/ Mass Spectrometry. Average pesticide residues concentrations ± SE in muscle of tilapia and catfish (n = 10 pooled samples with five fish each) was determined. The results indicated the presence of different types of organophosphorous (OPs), organochlorine (OCs), polychlorinated biphenyles (PCBs), hexachlorobenzene (HCB) and trifluralin pesticides in Elwasta and Mankbad in varying degrees. Diazenon was the only OP pesticide exceeded the permissible limit in both investigated areas in two types of fish. On the other hand, OCs, PCBs, HCB and trifluralin pesticide residue levels were not exceeded the maximum allowable concentration limit. As general, an increase in pesticides residue level was obtained in Mankbad than Elwasta. In addition, higher values are realized for the detected pesticide residues in cat fish than tilapia. The results of the study have shown that the extensive and recent use of these types of pesticides in the present time in Egypt