High performance liquid chromatography was used to analysis pymetrozine residues in rice and apple.Residues of pymetrozine were extracted from rice with acetonitrile:ammonia(10:1,V:V) and apple with acetonitrile,cleaned up by SPE column,and determined by HPLC equipped with VWD.The average recoveries and coefficient of variations of the method were 75.99%～96.03%, 1.64%～4.74% for rice sample and 74.84%～86.28%, 1.67%～5.43% for apple sample.The minium detectable amount and concentration of pymetrozine were 6×10-10g and 0.02 mg•kg-1.The method of pymetrozine in rice and apple accords with demands of residue analysis of pesticide.