固相微萃取-气相色谱-质谱联用结合嗅觉检测法鉴定血橙汁中的香气活性化合物  

Characterization of aroma active compounds in blood orange juice by solid phase microextraction and gas chromatography-mass spectrometry-olfactometry

作　　者：乔宇[1] 谢笔钧[1] 张妍[1] 张韵[1] 潘思轶[1] 

机构地区：[1]华中农业大学食品科技学院,湖北武汉430070

出　　处：《色谱》2008年第4期509-514,共6页Chinese Journal of Chromatography

基　　金：农业部农业结构调整重大技术研究专项项目(04-09-03B);湖北省重大科技攻关项目(2005AA201C68)

摘　　要：采用固相微萃取-气相色谱-质谱法(SPME-GC-MS)和嗅觉检测法对血橙汁中的挥发性物质进行分析,确定了血橙汁中的香气活性化合物。采用二乙烯基苯/碳分子筛/聚二甲基硅氧烷共聚物(DVB/CAR/PDMS)萃取头在40℃条件下顶空萃取40min。通过气相色谱-质谱联用结合保留指数,在所萃取的血橙汁的挥发性化合物中共鉴定出46种化合物。通过嗅觉检测法检测出34种具有气味的化合物,其中23种被定性。结果表明,对血橙汁香气起主要贡献的化合物是丁酸乙酯、辛醛、γ-松油烯、芳樟醇、4-乙酰基-1-甲基环己烯、癸醛、(-)-香芹酮、乙酸香叶酯、巴伦西亚桔烯以及保留指数分别为1020,1143,1169和小于800的4个未知化合物,这些香气强度较高的化合物的总相对含量为7.22%。Volatile compounds of fresh blood orange juice were analyzed by solid phase microextraction and gas chromatography-mass spectrometry （ SPME-GC-MS ） and the aroma active compounds were identified by olfactometry. The volatile compounds were extracted by headspace solid phase microextraction （HS-SPME） using a divinylbenzene/carboxen/polydimethylsiloxane （DVB/CAR/PDMS） fiber for 40 min at 40 ℃. The analysis was carried out using an HP 6890N GC equipped with an HP-5 column （30 m × 0. 25 mm × 0.25 μm ） directly connected to an HP 5975 series mass selective detector and a sniffing port （ODP2, Gerstel） using helium as carrier gas. Compound identifications were made by the comparison of the mass spectra, retention times, retention indices （IR ） and odor of the volatile components in the extracts with those of the corresponding reference standards. Forty-six compounds were identified by GC-MS and IR. The major components of the juice were limonene （ 86.36% ）, linalool （ 3.69% ）, β- myrcene （ 1.79%）, octanal （ 1. 32%） and valencene （1.27%）. GC-MS-olfactometry analysis was performed to determine 34 compounds with aroma activity, of which 23 compounds were identified. The major contributors to orange juice aroma activity are ethyl butanoate, octanal, γ-terpinene, 4-acetyl-1-methylcyclohexene, decanal, （ - ）-carvone, geranyl acetate, valencene. These compounds of strong aroma intensity represent 7.22% of the total volatile compounds. Other four unknown compounds （IR 〈 800; IR = 1 020, 1 143, 1 169, separately） are also the major contributors to the overall aroma.

关 键 词：固相微萃取 气相色谱-质谱法 嗅觉检测法 保留指数 香气活性化合物 血橙 

分 类 号：O658[理学—分析化学]