色谱

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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

乔宇,谢笔钧,张妍,张韵,潘思轶   

  1. College of Food Science &Technology, Huazhong Agricultural University, Wuhan 430070, China
  • 收稿日期:2007-10-18 修回日期:2008-07-30 出版日期:2008-07-30 发布日期:1983-12-25
  • 通讯作者: 潘思轶
  • 基金资助:
    农业部农业结构调整重大技术研究专项(04-09-03B)和湖北省重大科技攻关项目(2005AA201C68).

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   

  1. College of Food Science &Technology, Huazhong Agricultural University, Wuhan 430070, China
  • Received:2007-10-18 Revised:2008-07-30 Online:2008-07-30 Published:1983-12-25
  • Contact: PAN Siyi

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

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.

Key words: aroma active compounds, blood orange , gas chromatography-mass spectrometry (GC-MS), olfactometry, retention index, solid phase microextraction (SPME)