固相微萃取/动态顶空-气相色谱-质谱联用法对蜂胶与杨树胶挥发性成分的分析

Analysis of volatile compounds of propolis and poplar tree gum by SPME/DHS-GC-MS

目的分析、鉴定蜂胶和杨树树胶的挥发性成分。方法分别采用固相微萃取法(SPME)、动态顶空(DHS)对蜂胶和杨树树胶挥发性成分进行提取,经气相色谱-质谱联用(GC-MS)法结合计算机检索对其挥发性成分进行分析和鉴定。结果采用SPME法鉴定出37种挥发性化合物,占整个峰面积的97.71%;DHS法鉴定出52种化合物,占整个峰面积的92.46%。蜂胶中的酯类物质(乙酸-3-甲基-3-丁烯-1-醇酯、3-甲基-2-丁烯-1-醇甲酸酯、乙酸-3-甲基-3-丁烯-1-醇酯、3-甲基-2-丁烯酸-2-苯乙酯、壬酸乙酯、月桂酸乙酯、棕榈酸乙酯)、醇类物质(3-戊烯-2-醇、3-甲基-2-丁烯-1-醇、?--桉叶醇)、萜烯类物质(?-葎草烯、雪松烯)烯烃类物质八氢二甲基-2-(1-亚异丙基)萘在杨树胶中未检测到。而杨树胶中醇类物质(?/?)-?--红没药醇、烯烃类物质?-姜黄烯2,6,6,9-四甲基-三环[5.4.0.0(2,8)]-9-十一烯也未在蜂胶中检测到。结论通过GC-MS方法对蜂胶和杨树胶的挥发性成分进行分析比较,鉴定出蜂胶与杨树胶各自特有的成分,获得蜂胶与杨树胶的异同,从而为真假蜂胶的鉴别提供理论依据并可将其应用到蜂胶的标准制定及真假鉴别中去。

Objective To analyze and identify the volatile components of propolis and poplar tree gum.Methods The major volatile compounds of propolis and poplar tree gum were extracted by solid phase micro-extraction(SPME),dynamic headspace(DHS).And then the volatile components were analyzed and identified by gas chromatography-mass spectrometry(GC-MS) combined with computer,Results Totally 37 compounds were identified using SPME method,accounting for 97.71 % of the total peak area.Totally 52 compounds were identified by DHS method,accounting for 92.46 % peak area for propolis.And several compounds were identified using SPME or DHS method in propolis but not in poplar tree gum,such as 3-Methyl-3-buten-1-ol,acetate;2-Buten-1-ol,3-methyl-,formate;3-Methyl-3-buten-1-ol,acetate;2-Buten-1-ol,3-methyl-,acetate;2-Butenoic acid,3-methyl-,2-phenylethyl ester;Nonanoic acid,ethyl ester;Dodecanoic acid,ethyl ester;Hexadecanoic acid,ethyl ester;3-Penten-2-ol;2-Buten-1-ol,3-methyl-;Naphthalene,1,2,3,4,4a,5,6,8a-octa hydro4a,8-dimethyl-2-(1-methylethenyl)-,[2R-(2.alpha.,4a.alpha.,8a.beta.)]-;10s,11s-Himachala-3(12),4diene andβ-Humulene.Meanwhile,some other compounds were identified using SPME or DHS method in poplar tree gum but not in propolis,such as Tricyclo[5.4.0.0(2,8)]undec-9-ene,2,6,6,9-tetramethyl-;α-Bisabolol and α-Curcumene.Conclusion The aim of this work was to develop a reliable and sensitive GC-MS method for determining volatile components in propolis and poplar buds with a simple sample pretreatment method.Subsequently,the method was applied to distinguish poplar tree gum from propolis.