Abstract: GC with SPE was applied to the determination of endosulfan in fish-pond in a poisoning case.The water sample taken from the fish-pond was separated by SPE on CNWBOND LC-C18 SPE column at pH 4,and CHCl3 was used as eluant.The eluate was separated on CP-SIL 8 capillary column and detected by ECD.Linear relationships between values of peak area and mass concentration of α-endosulfan and β-endosulfan were kept in the same range of 0.05-5 μg·L-1,with same detection limits (3S/N) of 0.01 μg·L-1 .Values of recovery found by standard addition method were in the range of 91.1%-95.8%,and values of RSD′s (n=6) were less than 1%.