Separation and purification were done by column chromatographic fractionation; HPLC and 13C-NMR were used to determine the chemical structure of polysaccharide from Atractylodes macrocephala Koidz;, The molecular weight of the polysaccharide was estimated to be 1.36 x 10(5) (PSAM-1) and 1.04 x 10(5) (PSAM-2).