Abstract An analytical procedure for detecting residues of a new herbicide, flufenacet, in soil, wheat grain and straw by gas chromatographic method using various solvents and extraction methods was standardized. The best results were obtained when samples fortified with flufenacet and were extracted with acetone–0.2 M HCl (95:5) using a horizontal shaker for soil and Soxhlet extractor for plant samples. The clean up was done by partitioning with dichloromethane. The GC equipped with an electron-capture detector and a column packing of HP-1 as stationary phase and nitrogen as a carrier gas at a flow-rate of 15 ml min −1 was used. Temperatures of oven, injector and detector were adjusted at 190, 210 and 270°C, respectively. The retention time of flufenacet was 2.07 min. The herbicide recoveries ranged between 81 to 100% from the three matrices.