Soil contamination is regarded as one of the most serious issues to humanity all over the world. It is statistically believed that over one-fifth of the farmland, that is 20 million ha, is found to be contaminated by heavy metals in China. And the related issues, caused by soil contamination, of food safety, human health and eco-environmental quality attract much attention by public with more serious contamination than before. The technological approach for soil remediation is widely investigated. The technology of soil washing is effective for contaminants removal, while the treatment procedure might lead to component leaching from soil system, harmful for soil fertility, physicochemical properties and ecological functions. The study of spectral characteristics on leaching component is significant for decision-making of contaminated sites remediation and ecological function recovery, while the related investigation seems weaker nowadays. The paper mainly revealed the leaching characteristics of component from Pb/Cd contaminated loess in the washing process with Ethylene Diamine Tetraacetic Acid (EDTA) in reaction column, and the research objectives included base cations, loess nutrients, clay minerals and organic matter. The variation of clay minerals was analyzed by X-ray diffraction (XRD) and scanning electron microscope (SEM), and 3D-EEM fluorescence spectrum was used for the identification of dissolved organic matter (DOM). The experimental results showed: the leaching component from loess is detected in the washing reaction. The final removal efficiency (240 min) of Pb and Cd from loess are 49.86% and 62.25%, respectively. The sodium ions and nitrate nitrogen are the most easily leaching component, and little difference of clay minerals is identified before and after washing reaction. The fulvic acid-like (FA-like) material was firstly (10 min) detected around Eex/em=240~250/320~340 and Eex/em=260~290/450~470 in 3D-EEM fluorescence spectrum, and the humin acid-like (HA-like, Eex/em=290~320/430~490) appeared at 60 min with weaker fluorescence intensity of FA-like (Eex/em=240/320). The decreased fluorescence intensity of FA-like and HA-like, shown after 120 min and 240 min, indicated the component variation of DOM in the leaching solution. The spectroscopy approach is appropriate for characteristics identification of leaching component from co-contaminated loess.