顶空-固相微萃取法并气相色谱-质谱法测定八角茴香挥发性成分

Determination of volatile components from Illicium verum Hook. F. by HS-SPME and GC-MS

采用顶空-固相微萃取法(HS-SPME)分离富集八角茴香中挥发性成分,再利用气相色谱-质谱法(GC-MS)分析八角茴香中的挥发性成分,然后与传统的同时蒸馏萃取(SDE)并GC-MS法测定结果进行对比.结果表明,以萃取量作为考察指标时,最佳萃取条件为:称取1.0 g样品,选用100μmPA萃取头,温度50℃,萃取40 min,250℃下解吸10 s,GC-MS分析得到102种成分,定性确认其中69种成分,占总峰面积的85.46%.此时测出的八角茴香中主要挥发性成分为反式茴香脑(58.75%)、1-[3-甲基-2-丁烯基]-4丙烯基苯(12.68%)、茴香脑(7.50%)、3,7-二甲基-1,6-辛二烯-3-醇(2.22%)等.SDE法提取出93种成分,定性确认其中61种,占总峰面积的92.62%.此时测出的八角茴香主要挥发性成分与HS-SPME法测得的相同,其中58种为2种方法所共有.HS-SPME法可以代替SDE法对八角茴香中挥发性成分进行分离富集.

The head space-solid phase microextraction （HS -SPME） method was used to extract the volatile components from lllicium velum Hook. F.. The extracted volatile components were analyzed by gas chromatography -mass spectrometry（ GC -MS） method, and the determination results were compared with that of simultaneous distillation and extraction （SDE） - GC - MS. The results showed that the optimal extraction conditions were extracting 40 min at 50℃ from 1.0 g sample using a 100 μm polyacrylate （PA） fiber, and then desorbing for 10 s at 250 ℃. The GC - MS analysis results showed that 102 compositions were separated, and of which 69 components were identified and accounted for 85.46% of the total peak areas. The main volatile components were 1 - methoxy -4 - [ 1 - propenyl] - benzene（58. 75% ）, 1 - [3 - methyl - 2 - butenoxy ] - 4 - [ 1 - propenyl ] benzene （ 12. 68% ）, 1 - methoxy - 4 - [ 2 - propenyl ] - benzene （7.50%） and 3,7 - dimethy - 1,6 - octadien - 3 - ol （2. 22% ）. 93 components were separated from the SDE extraetant, of which 61 components were identified,which accounted for 92. 62% of the total peak areas. The main volatile components were the same as that separated from HS-SPME fiber and 58 components were common. The HS - SPME method can replace the SPE method for separation and enrichment of volatile components from lllicium verum Hook. F.