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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
引用本文:乔宇,谢笔钧,张妍,张韵,潘思轶.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[J].色谱,2008,26(4):509-514.
作者姓名:乔宇  谢笔钧  张妍  张韵  潘思轶
作者单位:College of Food Science &Technology, Huazhong Agricultural University, Wuhan 430070, China
基金项目:农业部农业结构调整重大技术研究专项 , 湖北省重大科技攻关项目
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40 min。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%。

关 键 词:保留指数  固相微萃取  气相色谱-质谱法  香气活性化合物  嗅觉检测法  血橙  
收稿时间:2007-10-18
修稿时间:2008-7-30

Characterization of aroma active compounds in blood orange juice by solid phase microextraction and gas chromatography-mass spectrometry-olfactometry
QIAO Yu,XIE Bijun,ZHANG Yan,ZHANG Yun,PAN Siyi.Characterization of aroma active compounds in blood orange juice by solid phase microextraction and gas chromatography-mass spectrometry-olfactometry[J].Chinese Journal of Chromatography,2008,26(4):509-514.
Authors:QIAO Yu  XIE Bijun  ZHANG Yan  ZHANG Yun  PAN Siyi
Institution:College of Food Science &Technology, Huazhong Agricultural University, Wuhan 430070, China
Abstract: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=1020, 1143, 1169, separately) are also the major contributors to the overall aroma.
Keywords:solid phase microextraction (SPME)  gas chromatography-mass spectrometry (GC-MS)  olfactometry  retention index  aroma active compounds  blood orange
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