Sediments from inland areas and open bays along the Korean coast were analyzed to examine the distribution of dioxin-like and estrogenic compounds. Concentrations of target chemicals varied considerably among locations (Lake Shihwa, Masan Bay, and Kwangyang Bay) and between inland and coastal areas. Principal component analysis (PCA) of contaminants measured in sediments showed that all of the inland locations from Lake Shihwa were highly contaminated, and the variations among locations were explained predominantly by the distribution of alkylphenols and polycyclic aromatic hydrocarbons (PAHs). PCA of PAH congener profiles among locations indicated that automobiles were a major source of PAH contamination. Dioxin-like and estrogenic activities associated with sediment from inland sites were approximately three- and six-fold, respectively, greater than those associated with open bay locations. The target dioxin-like and estrogenic compounds measured in raw extracts of sediments accounted for approximately 20% and 40% of the activities measured in the sediment extracts. The results suggest that a combination of instrumental and bioanalytical measurements of dioxin-like and estrogenic compounds is a valuable approach to screen, identify, and prioritize the risks posed by contaminants in complex environmental matrices.