Abstract: The major nutritional components,the aggregation state of water molecules and composition of volatile compounds were systematically analyzed in two cereals from Tibet by LF- NMR and HS- SPME- GC / MS. The results showed that the protein( 24.2%),dietary fiber( 15.20%),and β- glucan( 7.61%) contents of Tibet highland barley were significantly higher than that of Tibet jizhuagu,although the fat content( 1.01%) of the former was lower than that of the latter.The contents of combined water distribution were 88.4% and 87.7% in Tibet highland barley and jizhuagu,respectively. 72 volatile compounds were identified mainly in barley including hydrocarbons( 44.37%),alcohols( 18.06%) and aldehydes( 14.03%).70 volatile compounds were identified mainly in jizhuagu including alcohols( 34.81%),hydrocarbon( 34.65%) and ketones( 9.78%). In short,the barley from Tibet had a higher nutritional quality,a higher percentage of combined water and better flavor quality than jizhuagu.This study provided a useful basis for further development and reasonable diet of barley and jizhuagu from Tibet.