Abstract: GC-MS with dispersive solid phase extraction was applied to the determination of 3 pyrethroids in surface water. The water sample was treated by passing a SPE column packed with HC-C18 as extractant. Dichloromethane was used as eluant. The eluate was separated on HP-5MS quartz capillary column. EI and SIM were adopted in MS. Under optimal conditions. Linearity ranges of the 3 pyrethroids were same between 0.05-10.0 μg·L-1, with detection limits (3S/N) in the range of 0.001-0.005 μg·L-1. The proposed method was used for analysis of surface water samples, and recovery was tested by standard addition method, giving results in the range of 95.0%-99.8%, and RSDs (n=6) found were in the range of 4.3%-11%.