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中国精品科技期刊2020
曾桥,唐文洁,温谨瑞,等. 顶空固相微萃取-气相色谱-质谱法分析杜仲叶茯砖茶加工过程中挥发性成分[J]. 食品工业科技,2023,44(1):96−108. doi: 10.13386/j.issn1002-0306.2022030409.
引用本文: 曾桥,唐文洁,温谨瑞,等. 顶空固相微萃取-气相色谱-质谱法分析杜仲叶茯砖茶加工过程中挥发性成分[J]. 食品工业科技,2023,44(1):96−108. doi: 10.13386/j.issn1002-0306.2022030409.
ZENG Qiao, TANG Wenjie, WEN Jinrui, et al. Analysis of Volatile Components in the Manufacturing Process of Eucommia ulmoides Leaves Fuzhuan Tea Based on Headspace Solid Phase Microextraction/Gas Chromatography-Mass Spectrometry Method[J]. Science and Technology of Food Industry, 2023, 44(1): 96−108. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2022030409.
Citation: ZENG Qiao, TANG Wenjie, WEN Jinrui, et al. Analysis of Volatile Components in the Manufacturing Process of Eucommia ulmoides Leaves Fuzhuan Tea Based on Headspace Solid Phase Microextraction/Gas Chromatography-Mass Spectrometry Method[J]. Science and Technology of Food Industry, 2023, 44(1): 96−108. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2022030409.

顶空固相微萃取-气相色谱-质谱法分析杜仲叶茯砖茶加工过程中挥发性成分

Analysis of Volatile Components in the Manufacturing Process of Eucommia ulmoides Leaves Fuzhuan Tea Based on Headspace Solid Phase Microextraction/Gas Chromatography-Mass Spectrometry Method

  • 摘要: 为了解杜仲叶茯砖茶加工过程中挥发性成分变化,应用顶空固相微萃取(headspace solid phase microextraction, HS-SPME)结合气相色谱-质谱(gas chromatography-mass spec trometry, GC-MS)联用技术对杜仲叶茯砖茶加工过程中挥发性成分变化规律进行分析。结果表明,杜仲叶茯砖茶中共鉴定出152种挥发性成分,酸类、酯类、酮类和醇类为相对含量较高的挥发性成分,主成分分析、分层聚类分析及偏最小二乘判别分析均可直观地对杜仲叶茯砖茶不同加工阶段进行有效的区分。此外,在杜仲叶茯砖茶加工过程中,酸类、醇类、酮类和酯类等挥发性成分组成和结构发生了明显的变化,如丙酸、乙酸、2-己烯醛等具有刺激性、青辛气等不良气味的挥发性成分含量呈下降趋势,而芳樟醇、月桂酸、肉豆蔻酸、棕榈酸乙酯、菊苣酮、乙醛等具有菌花香、木香、花果香、乳香特性的挥发性成分相对含量呈上升趋势。基于VIP值筛选出64种标志差异性挥发性成分,其中,5-甲基吲哚、正三十二烷和十二醇等成分在原料中,3-氨基苯酚、环十五内酯、5-羟基-3-甲基-1-茚酮等成分在渥堆样本中,苯甲酸、4-乙烯基-2-甲氧基苯酚、1-己烯-3-醇等成分在气蒸样本中,植酮、2-吡咯甲醛和2-羟基环十五酮等成分在发花8 d的样本中以及乙琥胺、对丙基茴香醚等成分在发花25 d的样本中相对含量远高于其在其它阶段样本中的含量,这些成分可以作为杜仲叶茯砖茶对应加工阶段的候选标记物。在最终产品S5茶样中,棕榈酸甲酯、二氢猕猴桃内酯、月桂酸、植酮、β-紫罗兰酮等为相对含量较高的呈香挥发性成分,可能是构成杜仲叶茯砖茶风味特征的主要物质,这为识别杜仲叶茯砖茶的香气特征以及加工过程中香气成分的定向调控提供了基础。

     

    Abstract: In order to examine the variation of volatile components of Eucommia ulmoides leaves Fuzhuan tea during the production process, the combination of headspace solid phase microextraction (HS-SPME) with gas chromatography-mass spectrometry (GC-MS) was applied to explore the changes of volatile components of tea products during the production process. The results showed that 152 volatile components were identified in the production process of Eucommia ulmoides leaves Fuzhuan tea. Among these volatile components, the relative contents of acids, esters, ketones, alcohols were high and may be the main volatile components of Eucommia ulmoides leaves Fuzhuan tea during the production process. Principal components analysis (PCA), hierarchical cluster analysis (HCA) and partial least squares discriminant analysis (PLS-DA) were used to effectively distinguish the different processing stages of Eucommia ulmoides leaves Fuzhuan tea. The composition and structure of volatile components, such as acids, alcohols, ketones and esters, altered significantly during the production process of Eucommia ulmoides leaves Fuzhuan tea, whereas the contents of the volatile components with irritant, green, spicy and bad smell volatile components such as propanoic acid, acetic acid and 2-hexenal showed a decreased trend. Moreover, linalool, dodecanoic acid, tetradecanoic acid, hexadecanoic acid ethyl ester, 4-hydroxy-5-methyl-3(2H)-furanone, acetaldehyde and other volatile components with fungus fragrance, woody fragrance, flower fruit fragrance and frankincense presented a increased trend. Based on VIP value, 64 markers of differential volatile components during the production process were identified. For instance, the relative contents of 5-methyl-1H-Indole, dotriacontane and 1-dodecanol in the raw material samples, 3-amino-phenol, oxacyclohexadecan-2-one and 5-hydroxy-3-methyl-1-indanone in the piling fermentation samples, benzoic acid, 2-methoxy-4-vinylphenol and 1-hexen-3-ol in the steam and forming stage samples, 6,10,14-trimethyl-2-penta- decanone, 1H-pyrrole-2-carboxaldehyde and 2-hydroxy-cyclopentadecanone in the 8th day of flowering stage samples, and ethosuximide, 1-methoxy-4-propyl-benzene in the 25th day of flowering stage samples were relatively higher compared with other stages. Therefore, these compounds might be the potential indicators for the assessment of the raw material screening, piling fermentation, steam and forming, different stages of flowering of Eucommia ulmoides leaves Fuzhuan tea. In the finished product, hexadecanoic acid methyl ester, (R)-5,6,7,7a- tetrahydro-4,4,7a-trimethyl-2(4H)-Benzo-furanone, dodecanoic acid, 6,10,14-trimethyl-2-Penta-decanone, β-ionone and other volatile components were relatively higher compared with the content of aromatic volatile components, which might be the main material basis of fragrance of Eucommia ulmoides leaves Fuzhuan tea. The results can provide the material basis for identifying the aroma characteristics and regulating the formation of aroma of Eucommia ulmoides leaves Fuzhuan tea during processing.

     

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