An efficient method was developed for the determination of diniconazole in grape by gas chromatography. The diniconazole residue in the sample was extracted by acetone. The extract was cleaned-up by liquid-liquid extraction and then solid phase extraction. The diniconazole residue was separated completely from other impurities in the sample through SPB -1701 capillary column (30 m x 0.53 mm i.d. x 1.0 micron) and determined by an electron capture detector. The recoveries ranged from 85.8% to 94.7% when the added levels were from 0.01 mg/kg to 1.00 mg/kg. The RSD was within 5% and the limit of detection was 0.01 mg/kg.