气相色谱/质谱法分析内蒙古蜂胶挥发性成分

Analysis of Volatile Components from Inner Mongolia Propolis by Gas Chromatography-Mass Spectrometry

以内蒙古蜂胶为实验材料,采用传统水蒸气蒸馏法(HD)、同时蒸馏萃取法(SDE)和动态顶空进样(DHS)提取制备挥发性成分,以气相色谱-质谱(GC-MS)法检测。对获得的蜂胶挥发性成分进行了分析,从HD所得样品中检测出了12种化合物,主要是3-甲基-2-丁烯-1-醇(26.81%)、苯乙醇(17.16%)、1,2,3,4,4a,5,6,7-八氢-α,α,4a,8-四甲基-2-萘甲醇(14.53%)、2-甲氧基-4-乙烯基苯酚(9.47%)、α-没药醇(4.29%)等。从SDE法所得样品中检测出了40种化合物,主要是α-没药醇(20.19%)、2-甲基-3-丁烯-2-醇(10.76%)、3-甲基-2-丁烯-1-醇(8.28%)、薁(5.21%)等。从DHS法所得样品中检测出了70种化合物,主要是十七烷(6.96%)、菲(3.99%)、芳姜黄酮(3.80%)、1-(1,5-二甲基-4-己烯基)-4-甲基-苯(3.41%)、十八烷(3.23%)、1-甲氧基-4-(1-丙烯基)-苯(2.59%)、十六烷(2.47%)等。研究表明:内蒙古蜂胶挥发物与北京蜂胶及唐山蜂胶的组分相近,原因可能是它们具有相似的胶源植物。DHS得到的挥发性物质种类最多,SDE次之,HD最少。如需获得生物活性检测样品,SDE是一个更好的方法。

To study the volatile components in propolis collected in Inner Mongolia, the volatile components were extracted by three methods, traditional hydrodistillation（ HD）, simultaneous distillation extraction（SDE） and dynamic headspace sampling（DHS）, and analyzed the components by GC/MS. By searching the database, we selected high similarity from the results, combining with the reported compounds. The relative content of the components was calculated by peak area normalization method. The major components were 3-methyl-2-buten-1-ol（26.81% ）, phenylethyl alcohol（ 17.06% ）, 1,2,3,4,4a,5,6,7- octahydro-α ,α ,4α,8-tetramethyl-2-naphthalenemethanol （ 14. 53% ）, 2-methoxy-4- vinylphenol （ 9. 47% ）, α-bisabolol （ 4. 29% ）. 40 kinds of volatile components were identified by SDE-GC/MS. The main components were α-bisabolol （20. 19% ）, 2-methyl-3-buten-2-ol（ 10.76% ）, 3-methyl-2-buten-l-ol（ 8. 28% ）, azulene （5.21）. 70 kinds of volatile components were identified by DHS-GC/MS. The main of them are hcptadecane （6.96%）, phennathrene （ 3. 99% ） , ar-tumerone （ 3. 80% ） , 1-（ 1,5-dimethyl-4-hexenyl ）-4-methyl-benzene （ 3. 14% ） , octadecane（3.23% ） , 1-（ 1,5-dimethyl-4-hexenyl）-4-methyl-benzene（3.14% ） , hexadecane（2.47% ）. The volatile components in propolis of Inner Mongolia were similar to the proplis of Beijing and Tangshan. The possible cause is that there are similar plant sources of propolis. Among the three methods, the most volatile components can be detected by DHS. It may be the best analytical way, but the volatile components can not be obtained by this way for further biological activity experiment. For that purpose, SDE is the best way.