A solid phase extraction (SPE) method has been developed for the analysis of 4 rodenticides: warfarin, couatetralyl, bromadiolone and brodifacoum, using reverse phase high performance liquid chromatograph (HPLC) as determination system. The recovery is 62.6-90.0% (RSD5.1-7.8%) and 37.5-67.7% (RSD5.4%-12.8%) in whole blood and liver sample respectively. The procedure is simple and stable. And the method was confirmed to be effective in the animal experiment.