Abstract: A method was developed to analysis residue of fipronil in cereal and soil. After acetonitrile was added, the samples were sonicated in an ultrasonic water bath and then centrifuged, filtered, and cleaned up by a column containing neutral alumina and active carbon, successive eluted by ethyl acetate /n-hexane (3:5，V/V). The pesticide residues were determined by gas chromatography with electron-capture detection. Recoveries at spiked concentrations between 0.01 to 0.5mg/kg were 80.60%~99.66% with RSDs less than 9%.The limit of detection was 0.01mg/kg. The sensitivity and accuracy of the proposed method were fit for analysis of pesticide residue in cereal and soil.