Abstract: Simultaneous purification and separation of 28 polychlorinated biphenyls (PCBs), 16 polycyclic aromatic hydrocarbons (PAHs) and 21 organochlorine pesticides (OCPs) in marine sediment extracts by using solid-phase extraction (SPE) column of alumina-silica gel is presented in this paper. The results indicate that using 4 cm 3% deactivated alumina and 6 cm 3% deactivated silica gel and cutting off PCBs collection after loading 10 mL C₆H₁₄ eluting solvent through the 8 mm i.d.×15 cm column can yield satisfactory separation of PCBs, PAHs and OCPs, especially between PCBs and higher cyclic PAHs and higher polarity OCPs. All 65 kinds of PCBs, PAHs and OCPs can be completely recovered with being continuously eluted by 20 mL C₆H₁₄/CH₂Cl₂ (V/V, 1∶1). All of 65 kinds of PCBs, PAHs and OCPs can be effectively recoveried, and the recoveries are ranged from 75% to 110%,76% to 115% and 75% to 130%, respectively. Using marine sediment standard reference materials, the method provides the advantages of being practical, reliable, easy to operate, having low reagent consumption, low cost, etc., and is very suitable for the quantification of marine sediment samples with complicated matrices during marine environmental geology surveys.