Abstract: Residual amounts of S-triazine herbicides in samples of agricultural products and the soil of their producing area were extracted by dispersive solid phase extraction (DSPE) with acetonitrile (saturated with glacial acetic acid and n-hexane) as extraction solvent and PSA, C18, Carb as adsorbent. The eluate was determined by GC-MS. Under the selection ion monitoring mode, linearity ranges for 13 S-triazine herbicides were between 0.05-5.0 mg·L-1, with lower limits of determination (10S/N) of 0.01 mg·kg-1 for simazine and cyanazine, and 0.005 mg·kg-1 for the others. Tests for recovery and precision were made by addition of 0.01 mg·kg-1 and 0.1 mg·kg-1 of standard solutions, and analyzed by the proposed method, values of recovery in the range of 75.0%-111.8% and values of RSD′s (n=6) in the range of 3.2%-9.2% were obtained.