The fluorescence properties of dissolved organic matter (DOM) in Fu River in Baoding were investigated by three-dimensional fluorescence spectrometry. The type, distribution and origin of the DOM were estimated on basis of the position, number and intensity of fluorescence peaks in the spectra. Two types of fluorescence peaks were detected from Fu River. There are protein-like fluorescence peaks A with Ex/Em=225～230/340 nm and soluble microbial metabolites peaks B with Ex/Em=275/340～350 nm. The protein-like fluorescence peaks and soluble microbial metabolites peaks were founded in different times and stations in Fu River. Certain correlation was observed between the fluorescence intensity of DOM and the water quality parameters of Fu River. Good correlation of different fluorescence peaks showed the same of source. The fluorescence intensity of the two types had a significant positive relationship with COD, TN, TP and NH3-N concentration, this phenomenon indicating that the fluorescence peaks can speculate the level of pollution of Fu River. These results provided a reference for the pollution control in Fu River.