不同产地红茶香气品质的SPMEGC-MS分析
目的：红茶由于其原料产地、茶树品种以及加工工艺的不同，制成的红茶品质也有所差异，致使红茶的风味有着明显的地域特性。香气是茶叶品质优劣的重要评判因子，对茶叶香气活性成分进行提取分析，不仅对评价茶叶品质具有重要的意义，还能给消费者的选择提供参考。总结前人的研究，人们对于红茶香气的研究大都集中于同一品种不同等级，不同加工工艺之间的对比；而对于不同产地工夫红茶香气物质之间差异的研究还鲜少。本研究对云南、湖北、福建三个地域红茶的香气物质进行了鉴定和分析，揭示了滇红、闽红、宜红等不同产地工夫红茶香气品质形成的化学物质基础，对中国红茶香气品质的系统性分析具有积极作用，也可为今后开发风格多样的红茶新产品提供科学依据。
方法：本试验采用感官审评方法及顶空固相微萃取（HS-SPME）结合气相色谱-质谱联用技术（GC-MS），对云南、福建、宜昌三地红茶香气的物质基础及其主要呈香特征进行了比较综合分析。
结果：①从感官审评得分综合来看，特级滇红>一级滇红>二级滇红>福鼎红茶>宜昌红茶>三级滇红，其中云南大叶种所制红茶感官品质表现为：外形肥壮紧结，匀整显毫，汤色红艳明亮，香气以甜香为主，滋味鲜爽醇厚，感官品质优异；福鼎红茶外形紧结，有金毫，汤色红明亮，带花香，滋味甜醇尚鲜；宜昌红茶条索紧细有毫，色泽乌润，汤色红艳，香气甜纯滋味鲜醇。②在6种红茶中共分离鉴定出67种香气化合物，主要以醇类物质为主，其次是醛类、酮类和酯类。其中特级滇红中共有34种香气物质，含量较高的香气化合物分别为芳樟醇（61.13%）、a -松油醇（0.93%）、顺-α,α-5-三甲基-5-乙烯基四氢化呋喃-2-甲醇（5.24%）、苯乙醛（2.15%）等；一级滇红中共有22种香气组分，含量较高的化合物分别为芳樟醇（37.26%）、顺-氧化芳樟醇（5.40%）、、橙花醇（6.93%）、2,2,6-三甲基-6-乙烯基四氢-2H-呋喃-3-醇（2.18%）、α-松油醇（1.55%）、β-环柠檬醛（1.12%）、水杨酸甲酯（5.06%）、长叶烯（3.59%）等；二级滇红中共有33种香气化合物，含量较高的香气化合物分别为芳樟醇（10.09%）、顺-α,α-5-三甲基-5-乙烯基四氢化呋喃-2-甲醇（7.27%）、2,2,6-三甲基-6-乙烯基四氢-2H-呋喃-3-醇（1.95%）、橙花醇（1.31%）、柠檬醛（1.82%）、茉莉酮（2.19%）、β-紫罗酮（1.12%）、水杨酸甲酯（4.28%）、月桂烯（3.53%）；三级滇红含量较高的香气化合物分别为芳樟醇（19.92%）、顺-α,α-5-三甲基-5-乙烯基四氢化呋喃-2-甲醇（8.63%）、2,2,6-三甲基-6-乙烯基四氢-2H-呋喃-3-醇（3.20%）、α-松油醇（1.20%）、香叶醇（1.01%）、苯乙醛（3.95%）、臧红花醛（3.94%）、β-环柠檬醛（1.44%）、β-紫罗酮（3.14%）、二氢猕猴桃内酯（1.06%）；福鼎红茶中共有32种挥发性组分，含量较高的香气化合物分别为芳樟醇（14.04%）、藏红花醛（4.08%）、β-环柠檬醛（2.44%）、β-紫罗酮（2.05%）、香叶基丙酮（1.94%）、二氢猕猴桃内酯（2.12%）、月桂烯（2.76%）、β-柏木烯（1.19%）；宜昌红茶共有29种香气组分，含量较高的香气化合物分别为香叶醇（28.14%）、芳樟醇（2.77%）、雪松醇（3.63%）、β-紫罗酮（3.00%）、棕榈酸（1.62%）。③对6种红茶茶样挥发性物质的呈香特征进行分析，结果发现3个产地的工夫红茶挥发性香气组分种类和含量基本一致，但仍存在一定差异，如滇红工夫中有26种特有成分，主要为反-α,α-5-三甲基-5-乙烯基四氢化呋喃-2-甲醇、顺-氧化芳樟醇、α-松油醇、(E)- 反式-橙花叔醇等，滇红工夫产于云南省昌宁县，作为滇红的核心产区，昌宁由于其特殊的地理气候条件，所产茶叶品质优异，整体表现出较高的香气和锐度，香精油特征明显；宜红工夫中有4种特有成分，主要为香叶醇、β-柏木烯、棕榈酸等，产自湖北宜昌的宜红茶属于我国的三大传统工夫红茶之一，香叶醇作为相对质量分数最高的单萜烯醇物质，与茶叶感官审评呈现出花果甜香表现出高度相关性；闽红工夫中有6种特有成分，主要包括β-紫罗兰酮、β-二氢紫罗兰酮、1,5,5-三甲基-6-亚甲基-环己烯、氯代二十七烷等，产自于福建福鼎的工夫红茶除醇类物质之外含量最高的则是酮类物质，占了总挥发性物质的16.8%，且羰基类化合物中β-紫罗兰酮及其氧化物是其红茶香气的主要贡献物质。
结论：6种红茶分别检测出32、22、33、35、32和29种香气成分，明确了3个不同地域红茶的香气物质基础，为红茶品质特征的进一步研究提供了较为充分的数据。香气成分按化合物的结构类型分析，3个产地的香气物质包括醇、醛、酮、酯、杂环等化合物，相对总含量分别为88.25%、85.03%、44.64%、77.28%、68.92%和68.2%。主要香气化学成分依次为芳樟醇及芳樟醇氧化物、2,2,6-三甲基-6-乙烯基四氢-2H-呋喃-3-醇、β-环柠檬醛、β-紫罗酮、香叶基丙酮、水杨酸甲酯等，这些成分的共同作用构成了红茶的香气基调。
图片来源于图司机
Objectives: The quality of black tea is different because of the difference of raw material origin, tea tree varieties and processing technology, which makes the flavor of black tea has obvious regional characteristics. Aroma is an important factor to evaluate the quality of tea. Extracting and analyzing the active components of tea aroma is not only of great significance to evaluate the quality of tea, but also provides reference for consumers' choices. Summarizing the previous studies, most of the research on the aroma of black tea focuses on the comparison between different grades of the same variety and different processing technology.However, there are few researches on the difference of aroma substances of congou black tea from different regions. This study identified and analyzed the aroma compounds of black tea from Yunnan, Hubei, and Fujian,revealing the chemical basis of aroma quality formation of Gongfu black tea from different regions such as Yunnan, Fujian and Yichang,it can also provide scientific basis for developing new black tea products with various styles in the future.
Methods:The material basis of black tea aroma and the characteristics of main aromatic components in Yunnan, Fujian and Yichang were analyzed by using sensory evaluation method and headspace solid phase microextraction (HS-SPME) combined with gas chromatography-mass spectrometry (GC-MS).
Results:①From the perspective of sensory evaluation scores, special-class Yunnan black tea>first-class Yunnan black tea>second-class Yunnan black tea>Fujian black tea>Yichang black tea>third-class Yunnan black tea,and the sensory quality of black tea produced by Yunnan large-leaf tea (Camellia sinensis var.assamica) is as follows: the appearance of black tea is plump and tight, the color of the soup is red and bright, the aroma is mainly sweet, the taste is fresh and mellow, and the sensory quality is excellent; the appearance of Fuding black tea is tight knot with golden hair, a bright red color in the soup with flowers, sweet and fresh in taste; Yichang black tea is tight and thin with a dark and moist color , the soup color is red, the aroma is sweet and pure, and the taste is fresh and mellow.②A total of 67 aroma compounds were isolated and identified in 6 types of black tea, mainly consisting of alcohols, followed by aldehydes, ketones, and esters. There were 34 kinds of aroma substances in special-class Yunnan black tea, and the aroma compounds with higher content were 1,6-Octadien-3-ol,3,7-dimethyl-(61.13%),3-Cyclohexene-1-methanol, .alpha.,.alpha.,4-trimethyl-,(0.93%),2-Furanmethanol,5-ethenyltetrahydro-.alpha.,.alpha.,5-trimethyl-,cis-(5.24%),Benzeneacetaldehyde(2.15%), etc.There are a total of 22 aroma components in the first-class Yunnan black tea, and the compounds with higher content are 1,6-Octadien-3-ol,3,7-dimethyl-(37.26%),cis-Linalool Oxide(5.40%),2,6-Octadien-1-ol,3,7-dimethyl-(6.93%),2H-Pyran-3-ol,6-ethenyltetrahydro-2,2,6-trimethyl-(2.18%),3-Cyclohexene-1-methanol, .alpha.,.alpha.,4-trimethyl-,(1.55%),1-Cyclohexene-1-carboxaldehyde,2,6,6-trimethyl-(1.12%),Methyl Salicylate(5.06%),1,4-Methanoazulene, decahydro-4,8,8-trimethyl-9-methylene-, (1S,3aR,4S,8aS)-(+)-(3.59%),etc.There are a total of 33 aroma compounds in second-class Yunnan black tea, with the higher content being 1,6-Octadien-3-ol,3,7-dimethyl-(10.09%),2-Furanmethanol,5-ethenyltetrahydro-.alpha.,.alpha.,5-trimethyl-,cis-(7.27%),2H-Pyran-3-ol,6-ethenyltetrahydro-2,2,6-trimethyl-(1.95%),2,6-Octadien-1-ol,3,7-dimethyl-(1.31%),2,6-Octadienal,3,7-dimethyl-(1.82%),3-Methyl-2-pent-2-enyl-cyclopent-2-enone(2.19%),3-Buten-2-one,4-(2,6,6-trimethyl-2-cyclohexen-1-yl)-,(E)(1.12%),and Methyl Salicylate(4.28%),etc.The aroma compounds with higher content of third-class Yunnan black tea are1,6-Octadien-3-ol,3,7-dimethyl-(19.92%),2-Furanmethanol,5-ethenyltetrahydro-.alpha.,.alpha.,5-trimethyl-,cis-(8.63%),2H-Pyran-3-ol,6-ethenyltetrahydro-2,2,6-trimethyl-(3.20%),3-Cyclohexene-1-methanol, .alpha.,.alpha.,4-trimethyl-,(1.20%),Benzeneacetaldehyde(3.98%),1,3-Cyclohexadiene-1-carboxaldehyde,2,6,6-trimethyl-(3.94%),1-Cyclohexene-1-carboxaldehyde,2,6,6-trimethyl-(1.44%),3-Buten-2-one,4-(2,6,6-trimethyl-2-cyclohexen-1-yl)-,(E)-(3.14%),2(4H)-Benzofuranone,5,6,7,7a-tetrahydro-4,4,7a-trimethyl-,(R)(1.06%),etc.There are a total of 32 volatile components in Fuding black tea, with the highest content of aromatic compounds being 1,6-Octadien-3-ol, 3,7-dimethyl-(14.04%),1,3-Cyclohexadiene-1-carboxaldehyde,2,6,6-trimethyl-(4.08%),1-Cyclohexene-1-carboxaldehyde,2,6,6-trimethyl-(2.44%),3-Buten-2-one,4-(2,6,6-trimethyl-2-cyclohexen-1-yl)-,(E)-(2.05%),5,9-Undecadien-2-one,6,10-dimethyl-,(E)-(1.94%),2(4H)-Benzofuranone,5,6,7,7a-tetrahydro-4,4,7a-trimethyl-,(R)-(2.12%),1H-3a,7-Methanoazulene,octahydro-3,8,8-trimethyl-6-methylene-,[3R-(3.alpha.,3a.beta.,7.beta.,8a.alpha.)]-(1.19%), etc.Yichang black tea has a total of 29 aroma components, with the highest content of aroma compounds being 2,6-Octadien-1-ol,3,7-dimethyl-,(E)-(28.14%),1,6-Octadien-3-ol,3,7-dimethyl-(2.77%),Cedrol(3.63%),3-Buten-2-one,4-(2,6,6-trimethyl-2-cyclohexen-1-yl)-,(E)-(3.00%),n-Hexadecanoic acid(1.62%), etc.③Analysising the aroma characteristics of volatile compounds in six types of black tea samples revealed that the types and contents of volatile aroma components in Gongfu black tea from three producing areas were basically the same, but there were still some differences.For example, there were 26 kinds of unique components in Yunnan black tea.Mainly 2-Furanmethanol,5-ethenyltetrahydro-.alpha.,.alpha.,5-trimethyl-,trans-,cis-Linalool Oxide,3-Cyclohexene-1-methanol,.alpha.,.alpha.,4-trimethyl-,1,6,10-Dodecatrien-3-ol,3,7,11-trimethyl-, etc.Yunnan black tea is produced in Changning County, Yunnan Province. As the core producing area of Yunnan black tea, it has excellent quality due to its special geographical and climatic conditions, showing high aroma and sharpness as a whole.The characteristic of essential oil is obvious.There are four special components in Yichang Congou, mainly 2,6-Octadien-1-ol,3,7-dimethyl-,(E)-,1H-3a,7-Methanoazulene,octahydro-3,8,8-trimethyl-6-methylene-,[3R-(3.alpha.,3a.beta.,7.beta.,8a.alpha.)]-,n-Hexadecanoic acid, etc. Yihong black tea, produced in Yichang, Hubei Province, is one of the three traditional gongfu black teas in our country.As the monoterpene with the highest relative mass fraction, geraniol shows a high correlation with the tea's sensory evaluation showing a sweet floral and fruity aroma.There are 6 unique components in Fujian black tea, mainly including 3-Buten-2-one, 4-(2,6,6-trimethyl-1-cyclohexen-1-yl)-,(E)-,2-Butanone,4-(2,6,6-trimethyl-1-cyclohexen-1-yl)-,1,5,5-Trimethyl-6-methylene-cyclohexene,Heptacosane, 1-chloro-,etc.In addition to alcohol substances,the highest content of Gongfu black tea produced in Fuding,Fujian Province,is ketones,accounting for 16.8% of the total volatile substances,and 3-Buten-2-one, 4-(2,6,6-trimethyl-1-cyclohexen-1-yl)-,(E)- and its oxides in carbonyl compounds are the main contributing substances to the aroma of the black tea.
Conclusion:Six types of black tea were detected with 32, 22, 33, 35, 32, and 29 aroma components, clarifying the aroma substance basis of black tea from three different regions, providing sufficient data for further research on the quality characteristics of black tea.According to the structure type of the compounds, the aroma substances of the three producing areas include alcohols, aldehydes, ketones, esters, heterocyclic compounds and other compounds, with a relative total content of 88.25%, 85.03%, 44.64%, 77.28%, 68.92%, and 68.2%, respectively.The main aroma chemical components are linalool and linalool oxide,2H-Pyran-3-ol,6-ethenyltetrahydro-2,2,6-trimethyl-,1-Cyclohexene-1-carboxaldehyde,2,6,6-trimethyl-,3-Buten-2-one,4-(2,6,6-trimethyl-2-cyclohexen-1-yl)-,(E)-,5,9-Undecadien-2-one,6,10-dimethyl-,(E)-,Methyl Salicylate, etc. The aroma base of black tea is formed by the combined action of these components.
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