The Xijiang River is the major tributary of the Pearl River, South China, and is the major source water system for more than 4.5 million of urban population and 28.7 million of rural population. We initiated a systematic study on detection and quantification of organic pollutants in both water and suspended particulate matter (SPM) for samples collected in a span of 12 months. Our results showed that total concentrations of 15 polycyclic aromatic hydrocarbons (PAHs) varied from 21.7 to 138 ng l(-1) in water and from 40.9 to 665 microg kg(-1) in SPM. The organic carbon normalized distribution coefficients (K(OC)) computed for the PAHs were correlated well with their octanol-water partition coefficient (K(OW)). The estimated annual loadings of Ant, BaA, and BghiP and the total PAHs in the Xijiang River were 1620, 330, 177 and 19,400 kg, respectively. Further analysis of the data showed that combustion may be the major source of PAHs and that direct leakage of petroleum products may be insignificant.