Abstract: A high performance liquid chromatography as well as gas chromatographic electron-capture detective method for thed etermination of trace deltamethrin in sheep tissues was presented. A batch of twelve sheeps were bathed with large volume of diluted deltamethrin solution (50mg/L) in common bathing pool; then sheeps divided into four groups and put to executed in differental time limit, for example 3,7,15, and 30 days. The analytical samples were from differental sheep's tissue, such as liver, kidney、musele and adipose tissue etc. The detection limit (s/n=2) was 0.05ng, and the mean recoveries was higher than 93%.