Polycyclic aromatic hydrocarbons (PAHs) and organochlorine pesticides (OCPs) were measured in suspended particles and dissolved phase from the Baiertang water column and the Macao water column samples as collected from the Guangzhou channel of the Pearl River and the Macao harbor, where the sediments were heavily contaminated with organic pollutants. Total OCPs concentration varies from 23.4 to 61.7 ng/l in Baiertang water column and from 25.2 to 67.8 ng/l in Macao column, while total PAHs concentration varies from 987.1 to 2878.5 ng/l in the Baiertang water column and from 944.0 to 6654.6 ng/l in the Macao column. The vertical distribution profiles of pollutants and the partition of pollutants between particles and dissolved phases indicate that the sediments in Baiertang act as an important source of selected pollutants, and the pollutants in water of this region were mainly originated from the release and re-suspension of contaminants residing in the sediments. The sediments in Macao harbor act as a reservoir for organochlorine pesticides, such as DDTs mainly introduced by river inflow from Xijiang and PAHs input by brackish water from the Lingdingyang estuary. Combustion of fossil fuels and petroleum input are the main sources of PAHs in the Macao water column, while combustion of fossil fuels and coal is responsible for the PAHs in the Baiertang water column. The ratios of DDT/(DDD + DDE) for the Macao water column samples demonstrate that such chemicals were input into this region in recent times.