Abstract: The concentration of organic elements (C, H, N, S and O) in agricultural, non-agricultural soils and sediments were investigated from upstream of the Pearl River, China. The results showed that total C, N and S concentrations were closely correlated in agricultural soils and were significantly higher than those in non-agricultural soils. The differences of H and O contents in 2 kinds of soil were not significant. Agricultural soil would not be deficient in S due to high total S concentration and low ratios of C/N and N/S. For most sample sites, organic indexes of sediment have reached the grade Ⅳ (> 0.50), where were organic pollution. Total C concentration of sediment were positively correlated with that of agricultural or non-agricultural soils, and total N concentration of sediment was significantly positively correlated with that of agricultural soil. There were significant differences for the source of organic matter between sediment and non-agricultural soil.