A silicagel fractionation procedure for environmental sample extracts, which separates chlorinatedhydrocarbons(CHCs) and organophosphorus, pyrethroid pesticides into two groups for subsequent instrumentalanalysis, was developed in this study. This method was achieved by optimizing the fraction cut-off volume of elutionand different solvents. Using fully activated silica gel and cut-off CHCs collection after 10 mi 10% dichloromethane(DCM) in n-hexane passing through the column resulted in satisfactory separation of CHCs and organophosphorus,pyrethroid pesticides. This procedure had a higher reliability for CHCs than for organophosphorus, pyrethroidpesticides, because there is a relatively reliable recovery for CHCs. This approach is less expensive due to reducingsample pre-treatment time and solvent consumption.