Abstract: A method of capillary column gas chromatography-MS with separation by SPE was proposed for the determination of triadimenfon in soil and vegetables.Triadimenfon in the sample was extracted with acetonitrile and the extract was evaporated to near dryness by N2-blowing at 80 ℃.The residue was taken up with 2 mL of n-hexane and purified further by passing through a SPE micro-column packed with acidic aluminum oxide and rinsing with a mixed solvent of n-hexane and acetone (2+1) to remove sulfur which is usually existed in soil samples.Triadimenfon on the column was then eluted with n-hexane-acetone (1+3) mixture and the eluate was concentrated and made up to 5.0 mL with n-hexane which was ready for GC-MS analysis under the prescribed conditions.Standard curve was prepared with triadimenfon solution in the concentration range of 0.006-1.44 mg·L-1.Limit of detection (3S/N) of the method was found to be 0.001 mg·kg-1.Results of tests for recovery and precision at 3 concentration levels were found in the ranges of 84%-92% and (RSD) 1.93%-4.04% respectively.