The contents of various elements in rhizoma dioscoreae were analyzed and compared with those of shishou D. opposita Thunb on the whole jointly by XRF and PXRD. The results showed that the element Cu, Al and Mn could not be detected in rhizoma dioscoreae, but the element Mg, Zn and Cr were found, and other elements contents changed to different degrees; there are starch and whewellite in both groups, the crystal type of starches separated from rhizoma dioscoreae cultivars was a typical B-type pattern, but as C-type and V-type in shishou D. opposita Thunb, which is a mixture of A-type, B-type and V-type. The combination of two testing techniques could be applied to the mensuration and analysis of the elements and micro-structural of Dioscorea opposita Thunb which could be from different producing areas.