Bottom sediments and a 210Pb dated sedimentary core in Macao Estuary were quantitatively analyzed with GC-MS for coprostanol and other sterols. Higher coprostanol concentrations were detected at Port Interior and Lower Qianshan River, indicative of serious sewage pollution from densely populated Macao Island and Zhuhai City. However, very low concentrations of coprostanol were detected around Coloane Island as well as Port Exterior and Maliuzhou River except sites adjacent sewage outlets. Coprostanol pollution in Macao Estuary originates mainly from locally direct discharge of untreated wastewater. The concentrations of coprostanol in ZJ-9 were mainly in range of 150-280 ng/g with an average of 210 ng/g for more than 20 years from early 1970s to early 1990s. However, it increased obviously since 1993, and reached the highest in 1995-1996. However, a sharp decrease of coprostanol concentration from 470 to 31 ng/g after 1996 was observed corresponding to the first wastewater treatment plant in Taipa Island going into action.