Smoked bamboo has been put into mass production. However, many heat release volatiles would produce air pollution during thermoplasticization process. Therefore, the heat release behavior of smoked bamboo biomass was studied by TD-GC/MS to make full use of and prevent the pollution of the volatile materials. The main constituents were acetic acid(43.95%), cyclotrisiloxane, hexamethyl-(15.89%), octasiloxane, 1,1,3,3,5,5,7,7,9,9, 11,11,13,13,15,15-hexadecamethyl-(8.22%), 1,3-benzodioxole, 5-(2-propenyl)- (4.8%), cyclodecasiloxane, eicosamethyl-(4.51%), etc at 100°С. And the main constituents were acetic acid(42.05%), 1-phenanthrenecarboxaldehyde,7-ethenyl- 1,2,3,4,4a, 4b,5,6,7,9,10,10a-dodecahydro-1,4a,7-trimethyl-(8.42%), bicyclo[2.2.1]heptan-2-one, 1,7,7-trimethyl-,(1r)- (8.12%), cyclotrisiloxane, hexamethyl-(6.17%), 1,3-benzodioxole, 5-(2- propenyl)-(5.26%), 4-nitro-4'-chlorodiphenylsulfoxide(3.13%), etc at 115°С. The heat release volatiles of smoked bamboo biomass might be used as biomedicines. Particularly, the volatiles had good application prospects and popularized value in purification of cedrol and acetic acid.