Water pollution is a global concern. Inorganic and organic pollutants constitute primary pollutants in water resources. Therefore, it is of great concern to develop advanced sorbent materials for effective and efficient removal of metals and oil from water. In this study, synthesis of new LDH composites which would be used for sorption of heavy metals and oils from polluted water. For this purpose, MgAlOH- ɣ-Fe2O3-MoS2 composite was prepared and characterized were made via FT-IR and XRD. The XRD powder pattern of the composite showed that it contained g-Fe2O3 (PDF card no:00-002-1047), MgAl(OH)14.XH2O (PDF card no:00-043-0072) and MoS2 (PDF card no:00-037-4492). Thermal stability of the composite was investigated via DTA/TG technique. MgAlOH-ɣ-Fe2O3-MoS2 composite was shows highly efficient sorption for vegetable oil up to 418% times its own weight. The ablity of MgAlOH- ɣ-Fe2O3-MoS2 composite for removing Pb2+ ions from aqueous solution. Pb2+ analysis was made by ICP-OES. The effect of Pb2+ amounts, PH, sorbent amounts and solvent flow rate on the adsorption capacity of MgAlOH- ɣ-Fe2O3-MoS2 composite were also ivestigated.