Abstract: Matrix solid-phase dispersion and high performance liquid chromatography(MSPD-HPLC)was ultilized to determine 2,4-dichlorophenol(2,4-DCP) and 4-chloro-2-methylphenol(4-C-2-MP) residues in three different types of soil. Soil sample and silica gel were manually blended together, followed by addition of 2.0 mL distilled water. Samples were introduced into glass column, and eluted with dichloromethane. Then 0.5 mL ethylene glycol was added into the extract. The solution was concentrated and diluted to 1.0 mL. Samples were analyzed by HPLC-DAD. The recoveries of two analytes in three different soils ranged from 90% to 118%, with relative standard deviation(RSD) from 0.1% to 8.5% at spiked level ranged from 0.01 to 2.5 mg/kg. Limits of quantifications(LOQs) of this method were 0.01 mg/kg. Limits of detections(LODs) reached 2-3 μg/kg. The recovery tests of MSPD method and classical SLE method showed that with MSPD high recovery could be achieved. This MSPD-HPLC-DAD method was also applied to analytes recoveries of soils at different aging times. In conslusion, this method is characterized by simple, analysis time saving, less solvent consumption and is suitable for residues analysis of 2,4-DCP and 4-C-2-MP in soils.