A novel inorganic flocculent composite of Al(III)-Mg(II) poly-magnesium-aluminum-sulfate (PMAS) is used to remove organic matter from biologically treated leachate in some landfills in Beijing, China. Jar-test experiments are employed to determine the optimum conditions for the removal of organic matter, which is represented as UV(254). Under optimum conditions, the removal of COD, BOD(5), and color is also determined. Moreover, gas chromatography coupled with mass spectrometry (GC-MS) is used to analyze the organic matter in the biologically treated leachate before and after treatment by the coagulant. The experimental results indicate that the removal of COD, BOD(5), UV(254), and color by coagulation with PMAS can reach above 65%, 60%, 85%, and 85%, respectively, under optimal conditions. This greatly weakens its pollution extent and improves its visual appeal. Forty-one kinds of organic pollutants in the biologically treated leachate were determined. Some of them belong to the Black List of water environmental preferred controlled pollutants, as judged by the United States and China. The species of alkyl, alkene, acyclic alcohol, and acyclic acyl amines are about 85% removed, some of them are removed completely, while the species of acids, esters, and ketones are removed at about 65%. Those contaminants with benzene rings, such as aromatic hydrocarbons, hydroxybenzene, aromatic alcohol, and aromatic acyl amine, are about 50% partially removed.