Solid-phase extraction (SPE), gas chromatography electron capture detector (GC-ECD) and gas chromatography nitrogen-phosphorous detector (GC-NPD) and gas chromatography–mass spectroscopy (GC-MS) were applied for trace-level de-termination of 20 pesticides in river nile water. Samples were collected from March to October 2003 from different sites located in Greater Cairo, Egypt. First, extrac-tion by on-site solid-phase extraction of 1 liter from field and laboratory spiked and unspiked (raw river water) samples using poly-divinyl benzene-N-vinyl pyrolidine cartridge based sorbent. Next, water extracts were subject of analysis by GC-ECD and GC-NPD. Next, selected samples that were positive to GC-ECD or GC-NPD were analyzed by GC-MS in order to improve the determination of detected pesti-cides. Recoveries from laboratoy spiked samples were > 85% for 16 of the 20 com-pounds with % relative standard deviation (% RSD) in the 5 to 10 % range. The lowest recoveries were for aldrin, 52 % and prothiofos, 48 %. A similar trend was observed with p,p-DDE and p,p-DDT values. Field spike results also indicated high % recovery for most of the target compounds. Values were > 85% for 12 of the 20 analytes, as was the case in laboratory spikes, Aldrin, 54 % and prothiofos, 55 % yielded the lowest values. Overall field spike recovery reproducibility was lower since % RSDs were higher, 15-40 %. Overall results indicated a relatively high de-gree of accuracy and precision could be achieved for most of the target compounds by methods applied in present study.