This research combined m-XRF and m-XAFS technology to determination quantity, distribution and chemical state of zinc into duodenal wall using different zinc sources. Tsuji et al. (2005) reported that elemental distributions in biological materials, such as wheat and rice grains were investigated by the micro-XRF method. This research demonstrates zinc elemental distributions and quantity can be detected in the duodenal wall by the m-XRF method, and determine the intestinal absorption maximum quantity area of zinc for measuring m-XAFS spectra to prepare.