The volatiles of mature (180 days after full bloom) Korla Pear fruit were extracted with methyl tert-butyl ether (MTBE) and headspace solid phase microextraction (HS-SPME),respectively. Qualitative and quantitative analyses of volatiles were performed in combination with gas chromatography-mass spectrometry (GC-MS). The composition of volatiles in different tissues was compared with the basis of screening suitable volatiles extraction methods. The results showed that the effect of extracting volatiles from Korla Pear with HS-SPME was better than that of MTBE. 15 compounds were detected with MTBE-GC-MS,while no esters,aromatic hydrocarbons nor ketones were detected. 98 compounds mainly including aldehydes,esters,alcohols and terpenes were detected with HS-SPME-GC-MS. (E)-2-hexenal,hexanal,α-farnesene,1-nonanol,hexyl acetate were the main volatiles. Volatiles in the peel were more than that in the pulp. 32 compounds were unique in the peel. The results of the primary metabolites analyzed with GC-MS showed that 17 sugars including fructose,glucose and sorbitol,and 8 organic acids such as malic acid were detected in the pulp. The sugar/acid ratio was 71.49.