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Linear alkylbenzene sulfonates (LAS) in the surface sediment and the river water of the Tama River were determined by combined gas liquid chromatography and mass spectrometry.The composition of LAS homologues in the river sediment was remarkably different from that in the river water; the proportions of C12 and C13 LAS in the sediment were higher than those in the water, while those of C10 and C11 LAS were lower. The ratio of the concentration of the LAS homologues in the sediment to that in the water increased exponentially with increasing the carbon number of the alkyl group.