Triolein-containing semipermeable membrane devices (triolein-SPMD) were deployed 1 m above the sediments at two sampling sites in the Huaihe River, China, for a period of 28 d. Sediment and fish samples were simultaneously collected from the same sampling sites. Concentrations of substituted benzenes, selected pesticides, polycyclic aromatic hydrocarbon (PAH), and polychlorinated biphenyls (PCBs) were measured in triolein-SPMDs, sediments, and fishes. The concentrations of these hydrophobic organic contaminants (HOCs) in fish and in sediment organic carbon were correlated with HOCs accumulation in triolein-SPMDs. Our results showed reasonably good correlations between the log concentrations of contaminants in fish lipid and in triolein-SPMDs. Good correlations were also found between the log concentrations of contaminants in sediment organic carbon and in triolein- SPMDs (except for PAHs). The results were discussed in terms of the partitioning of hydrophobic organic contaminants among different compartments in the aquatic environment and the suitability of using triolein-SPMDs to predict bioconcentration factor (BCF) and sediment-water partitioning coefficient (Koc).