A method developed for study of metribuzin degradation in soil is presented. LC-MS-MS and electrospray ionisation was used for analysis of metribuzin and the metabolites deaminometribuzin (DA), diketometribuzin (DK) and deaminodiketometribuzin (DADK). Soil samples were extracted by pressurized liquid extraction using methanol-water (75:25) at 60 o C. In general, recoveries were about 75% for metribuzin, DA and DADK and their detection limit in soil was 1.25 μg/kg. Lower sensitivity was observed for DK, with detection limit at 12.5 μg/kg and recovery about 50%.