Abstract: New method for analysis of nitrofene in rice was reported in this paper.Rice samples were extracted with dichoromethane. The extracted solution was purified by neutral aluminum oxide arid Florisil mix-up column.The prepared samples was tested with gas chromatography equipped with NPD and 3% OV-17 gas chrom Q 80 -100 mech column. This method was applicable to the determination of nitrofene residue in rice with satisfactory recovery rate ( 87.33-91.47%, variant coefficient from 3.36% to 6.31% )and fine detection limit 0.0212ppm.