Abstract:The pretreatment technique of microwave-assisted extraction coupled to headspace solid-phase microextraction (MAE–HS-SPME) was investigated on the extraction of aroma components from Cinnamon. The extracted volatiles were analyzed by gas chromatography-mass spectrometry(GC-MS) method, and the determination results were compared with that of simultaneous distillation and extraction (SDE) and HS-SPME methods. The results showed that the optimal extraction conditions of MAE–HS-SPME were extracting 4.5min at 120W microwave power from 10 g sample in 100mL deionized water using a 100 ?m polyacrylate (PA) fiber, and then desorbing for 20 s at 250 ℃. The GC-MS analysis results showed that 62 components were identified and accounted for 95.60% of the total peak areas. The main volatiles were the same as that separated from HS-SPME fiber and SDE method. The main volatiles were 3-phenyl-2-propenal, ?-cubebene, 1-methoxy-4-[1-propenyl]-benzene, 4,7-dimethyl-1-[1-methylethyl]-1,2,4a,5,6,8a- hexahydro-naphthalene, etc. The components extracted by MAE–HS-SPME covered almost all the components extracted by HS-SPME and SDE. The total number of the components extracted by MAE–HS-SPME was 18 more than that extracted by HS-SPME and 26 more than that extracted by SDE. The results indicated that MAE–HS-SPME is a high performance pretreatment method for the analysis of aroma components in Cinnamon.