A sample cleanup procedure for the simultaneous determination of PCDD/Fs,PBDD/Fs,PCBs and PBDEs in soil was developed.Firstly,four series of halogenated organic contaminants were separated into chlorinated(PCBs and PCDD/Fs) and brominated(PBDEs and PBDD/Fs) groups,with multi-layer gel column containing silver nitrate silica.Florisil column was subsequently used to separate PCBs from PCDD/Fs and PBDEs from PBDD/Fs,respectively.The results indicated that the four series contaminants could be completely separated.Recoveries and relative standard deviations(RSDs) of standard-spiked samples were as follows:PCDD/Fs:61%-83%,1.4%-14.2%;PBDD/Fs:71%-110%,2.8%-14.9%;PCBs:68%-92%,3.6%-15.2%;PBDEs:81%-87%,10.9%-17.4%.This method was applied in the simultaneous detection of four series of compounds in soil samples,and the results were no obvious difference with that of the reported method(the deviation of two methods was not more than 12.5% )，which implys that the developed method has good accuracy and reliability.