The widespread usage of antibiotics in human and animal medication has brought global concerns over environmental contamination of antibiotic residues. In this study, 16 kinds of antibiotics in different environmental media of water, sediments, and soils in Anqing city, Anhui province were determined by ultra-performance liquid chromatography tandem mass spectrometry. A total of fourteen kinds of antibiotics were detected in surface water, with a total concentration up to 479 ng·L−1, while six kinds of antibiotics were detected in sediment and soil with concentrations ranging from 15.1 to 108 μg·kg−1. Ciprofloxacin (12.8–99.5 ng·L−1) and tetracycline (17.2–225μg·kg−1) antibiotics exhibited the highest concentration in water and soil, respectively. In spatial distribution, the total concentration of antibiotics in surface water from the highest to the lowest followed the order of urban area, mainstream of Wan River, suburbs, tributaries of Wan River, indicating that the level of antibiotic concentration in surface water is positively associated with the frequency of human activities. In addition, the antibiotic mass fraction in agriculture land and fishpond were found higher than that in other sampling sites. Moreover, the environmental risk assessment results showed that ciprofloxacin, erythromycin, ofloxacin, enrofloxacin and tetracycline might pose medium to high risks to algae and bacteria in aquatic ecosystem.