Three-dimensional synchronous fluorescence of each component of Liuwei dihuang pills (Prepared rehmannia root, cornel, yam, alisma, poria cocos, and cortex moutan) is measured by using FLS920P fluorescence spectrometer. Feature parameters were extracted. It can be found that each component is fluorescent material and the lines are all different. Furthermore, Three-dimensional synchronous fluorescence of Liuwei dihuang pills boiling with standard water and non-standard water are all measured and there are significant differences between them. It can be applied in distinguishing different formula of Chinese medicine decoction. Experimental and Theoretical conclusion show that: the three-dimensional fluorescence spectrometry method and the combination of synchronous fluorescence spectroscopy method can further improve the sensitivity and selectivity of fluorescence spectroscopy, have a distinct advantage in a complex multi-component mixture of fluorescence spectroscopic analysis. The study can provide a convenient and reliable method for establishing a complete fingerprint of Chinese traditional medicine. It also can help identifying the component and the quality of Chinese patent medicine.