By using the ultraviolet absorption spectrum,the fluorescence spectrum and three dimensional fluorescence spectra,the composition of dissolved organic matter(DOM) and the humification degree,etc.in the sediment of hydro-fluctuation belt(Yunyang part) were analyzed.The relationship between the test parameters and the pollution degree in the region was discussed.The research results of UV spectrum data E3/E4 showed that in 4 sampling sites which included Huangshi Town,Gaoyang Town,Shuangjiang Town and Quma Town,the humification degree in the sediment of hydro-fluctuation belt in Shuangjiang Town sampling site was lower,and the aromaticity was smaller.Moreover,the effect of human factor was comparatively smaller.The fluorescence index value which represented the source of humus in DOM was 1.62-1.88.It showed that the biological and terrestrial source both existed.Three dimensional spectra results showed that the pollution degrees in 4 sampling sites were all smaller,and some prevention measures should be taken early.