SPME-GC-MS技术结合rOAV分析不同加工工艺紫娟白茶的关键香气物质

李沅达; 吴婷; 黄刚骅; 任玲; 马晨阳; 周小慧; 李亚莉; 周红杰

doi:10.13386/j.issn1002-0306.2022060240

SPME-GC-MS技术结合rOAV分析不同加工工艺紫娟白茶的关键香气物质

doi: 10.13386/j.issn1002-0306.2022060240

云南农业大学茶学院，云南昆明 650000

基金项目: 云岭技术领军人才（发改委〔2014〕1782）；国家自然科学基金项目（31260197）；国家自然科学基金项目（31460215）。

详细信息

作者简介:
李沅达（1998−），男，硕士研究生，研究方向：茶叶加工与质量控制，E-mail：1772955439@qq.com

通讯作者:
周红杰（1962−），男，硕士，教授，研究方向：茶叶加工与品质鉴定，E-mail：1051195348@qq.com

中图分类号: TS272.4
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出版历程
- 收稿日期: 2022-06-27
- 刊出日期: 2023-05-01

SPME-GC-MS Technique Combined with rOAV for the Analysis of Key Aroma Substances of Zijuan White Tea with Different Processing Processes

College of Tea, Yunnan Agricultural University, Kunming 650000, China

摘要

摘要: 为研究不同加工工艺紫娟白茶的关键香气化合物，采用顶空固相微萃取-气相色谱-质谱联用技术（Head-space solid-phase micro extraction and gas chromatography mass spectrometry，HS-SPME-GC-MS），结合感官审评、PCA验证、OPLS-DA分析以及相对香气活度值（Relative odor activity value，rOAV），分析筛选紫娟白茶的关键香气化合物。结果表明：共检测出82种主要香气组分，以醇类、酯类、杂环及芳香族化合物为主，芳樟醇、水杨酸甲酯、苯甲醇、β-紫罗兰酮等相对含量较高，rOAV法分析结果显示：1-辛烯-3-醇、α-紫罗兰酮、苯乙醛、水杨酸甲酯等9种挥发性有机化合物对自然萎凋的紫娟白茶（TZW）花果香馥郁且带毫香、辛香、药香的香气形成具有较大贡献，1-辛烯-3-醇、α-紫罗兰酮、β-紫罗兰酮、苯甲醛等9种挥发性有机化合物对复式萎凋紫娟白茶（CZW）果香浓郁且带花香、辛香的香气形成具有较大贡献。OPLS-DA分析结合rOAV发现1-辛烯-3-醇和水杨酸甲酯是TZW与CZW香气差异的关键化合物。综上所述，自然萎凋方式加工的紫娟白茶花果香更加浓郁，可以有效提高紫娟白茶的香气品质。
- 紫娟 /
- 白茶 /
- 关键香气物质 /
- 顶空固相微萃取-气相色谱-质谱联用(HS-SPME-GC-MS)
Abstract: In order to study the key aroma compounds of Zijuan white tea with different processing technologies, headspace solid-phase micro extraction and gas chromatography mass spectrometry (HS-SPME-GC-MS), combined with sensory evaluation, PCA validation, OPLS-DA analysis and relative odor activity value (rOAV), was used to analyze and screen the key aroma compounds of Zijuan white tea. The results showed that 82 major aroma components were detected, mainly alcohols, esters, heterocyclic and aromatic compounds, with relatively high contents of linalool, methyl salicylate, benzyl alcohol and β-Ionone. The results of rOAV analysis showed that 9 volatile organic compounds including 1-octen-3-ol, α-Ionone, phenylacetaldehyde and methyl salicylate contributed to the aroma formation of natural withering Zijuan white tea (TZW) with floral and fruity aroma and spicy medicinal aroma, and 9 volatile organic compounds including 1-octen-3-ol, α-Ionone, β-Ionone and benzaldehyde contributed to the aroma formation of compound withering Zijuan white tea (CZW) with floral and fruity aroma and spicy aroma. OPLS-DA analysis combined with rOAV showed that 1-octene-3-ol and methyl salicylate were the key compounds for aroma difference between TZW and CZW. In summary, the flower and fruit aroma of Zijuan white tea processed by natural wilting was more abundant, which could effectively improve the aroma quality of Zijuan white tea.
- Zijuan /
- white tea /
- key aroma substances /
- headspace solid-phase microextraction coupled with gas chromatography-mass spectrometry(HS-SPME-GC-MS)

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图 1 不同加工工艺紫娟白茶挥发性化合物热图

Figure 1. Heat map of volatile chemical compounds of Zijuan white tea with different processing processes

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图 2 不同加工工艺紫娟白茶挥发性化合物PCA模型得分散点图

Figure 2. Scatter plot of PCA model scores of volatile compounds of Zijuan white tea with different processing processes

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图 3 不同加工工艺紫娟白茶挥发性化合物OPLS-DA模型得分图（A）和散点图（B）

Figure 3. OPLS-DA model score (A) and scatter plot (B) of volatile compounds of Zijuan white tea with different processing processes

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表 1 不同加工方式紫娟白茶感官审评结果

Table 1. Sensory evaluation results of Zijuan white tea with different processing methods

样品名称	外型（25%）		香气（25%）		汤色（10%）		滋味（30%）		叶底（10%）		总分
样品名称	评语	得分	评语	得分	评语	得分	评语	得分	评语	得分	总分
TZW	靛青带毫，匀整	91	花果香馥郁、带毫香、辛香、药香	94	靛黄、较明亮	91	甜醇	90	黄绿、较软	90	91.35
CZW	芽叶连枝，靛青	90.5	果香浓郁、带花香、辛香	91	靛黄、较明亮	91	甜、较醇	90.5	靛青、明亮	91	90.73

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表 2 不同加工方式紫娟白茶的挥发性成分与相对含量

Table 2. Volatile components and relative contents of Zijuan white tea in different processing methods

挥发性化合物	保留时间（min）	保留指数	相对含量（%）		VIP值	FC值
挥发性化合物	保留时间（min）	保留指数	TZW	CZW	VIP值	FC值
酯类
水杨酸甲酯	13.46	1195	11.34±0.20	16.95±0.71	1.21	0.02
二氢猕猴桃内酯	19.57	1532	0.88±0.06	0.90±0.06	1.09	0.02
磷酸三乙酯	12.03	1118	0.53±0.02	0.80±0.02	1.21	0.02
3-己烯-1-醇苯甲酸酯	20.23	1571	0.37±0.01	0.03±0.00	1.09	0.02
苯甲酸己酯	20.36	1579	0.30±0.02	0.05±0.01	1.13	0.01
邻苯二甲酸丁庚酯-4-丁基酯	23.97	1957	0.15±0.02	0.21±0.01	1.13	0.01
棕榈酸甲酯	23.77	1923	0.14±0.01	0.17±0.02	1.16	0.01
（E,Z）-2-己烯酸-3-己烯酯	17.79	1430	0.13±0.01	0.13±0.01	1.15	0.01
乙酸叶醇酯	13.24	1184	0.09±0.00	0.09±0.00	1.18	0.01
己酸叶醇酯	16.84	1377	0.06±0.01	0.04±0.00	1.19	0.01
棕榈酸异丙酯	24.31	2020	0.02±0.00	0.02±0.00	1.20	0.01
亚油酸甲酯	24.67	2092	0.01±0.00	0.01±0.00	1.22	0.01
杂环及芳香族化合物
2-（5-甲基-5-乙烯基四氢呋喃-2-基）丙-2-基乙酯-碳酸	11.45	1088	6.93±0.03	4.68±0.04	1.20	0.03
环氧-β-紫罗兰酮	18.72	1483	3.93±0.17	2.93±0.17	1.20	0.03
（3R，6S）-2,2,6-三甲基-6-乙烯基四氢-2H-吡喃-3-醇	13.1	1176	3.81±0.08	1.38±0.03	1.18	0.03
顺-α,α-5-三甲基-5-乙烯基四氢化呋喃-2-甲醇	11.14	1072	1.74±0.03	1.66±0.04	1.18	0.03
3,5-二羟基戊苯	19.31	1517	1.65±0.07	2.10±0.12	1.19	0.03
2,4-二叔丁基苯酚	19.09	1504	0.74±0.05	1.37±0.06	1.16	0.03
3-（1-甲基乙基）-氧杂环丁烷	5	762	0.39±0.03	0.30±0.01	1.20	0.02
间伞花烃	10.28	1026	0.11±0.01	0.10±0.01	1.06	0.03
间氨基苯乙炔	15.3	1293	0.09±0.01	0.10±0.00	1.20	0.03
1,3,4-噁二唑	4.36	728	0.08±0.00	0.05±0.00	1.20	0.02
3-苯基呋喃	14.01	1224	0.07±0.01	0.10±0.01	1.19	0.02
酮类
β-紫罗兰酮	18.67	1480	5.06±0.18	5.06±0.12	1.17	0.06
3,5-辛-3,5-二烯-2-酮	11.07	1068	1.04±0.01	1.10±0.01	1.17	0.06
橙化基丙酮	18.06	1446	0.67±0.03	0.85±0.06	1.13	0.04
1-乙基-2,5-吡咯烷二酮	12.24	1130	0.47±0.05	1.07±0.10	1.19	0.04
Z-四氢-6-（2-戊烯基）-2H-吡喃-2-酮	18.82	1489	0.44±0.04	0.30±0.03	1.19	0.04
α-紫罗兰酮	17.66	1423	0.38±0.01	0.51±0.01	1.18	0.04
5-乙基-6-甲基庚-3-烯-2-酮	12.43	1140	0.35±0.03	0.28±0.01	1.18	0.04
植酮	23.25	1844	0.25±0.02	0.20±0.02	1.12	0.04
2-羟基-5-甲基苯乙酮	15.61	1310	0.16±0.02	0.17±0.02	1.18	0.04
法尼基丙酮	23.7	1910	0.13±0.01	0.14±0.01	1.19	0.03
茉莉酮	17.13	1393	0.09±0.01	0.03±0.00	1.20	0.03
烃类
β-蒎烯	9.6	990	2.09±0.14	2.16±0.14	0.89	0.10
十四烷	17.23	1399	0.33±0.02	0.54±0.03	0.94	0.10
十六烷	20.68	1599	0.24±0.02	0.44±0.04	1.05	0.09
3-甲基十五烷	20.19	1569	0.16±0.02	0.28±0.02	1.08	0.09
3,4-二甲基-2,4,6-辛三烯	12.19	1128	0.15±0.01	0.16±0.01	1.14	0.06
十二烷	13.54	1199	0.13±0.02	0.21±0.01	0.98	0.08
5-丙基十三烷	16.7	1369	0.13±0.02	0.22±0.01	1.13	0.08
4,4-二甲基-十一烷	16.37	1351	0.09±0.02	0.14±0.01	1.11	0.08
3-甲基十七烷	22.7	1772	0.09±0.01	0.14±0.01	1.06	0.08
6-甲基十二烷	12.18	1127	0.09±0.01	0.08±0.02	1.11	0.08
植烷	22.94	1799	0.08±0.01	0.13±0.01	1.14	0.07
1,1'-氧双-辛烷	21.6	1667	0.05±0.00	0.08±0.01	1.12	0.07
4-乙基十四烷	22.52	1752	0.03±0.00	0.05±0.00	1.13	0.07
4-甲基十八烷	22.64	1766	0.03±0.00	0.04±0.00	1.15	0.07
2,6,10-三甲基十三烷	18.3	1459	0.03±0.01	0.03±0.01	1.15	0.06
α-二去氢菖蒲烯	19.79	1546	0.01±0.00	0.01±0.00	1.05	0.10
酸类
己酸	9.77	998	4.73±0.48	5.24±0.45	0.97	0.12
香叶酸	16.27	1346	1.28±0.15	0.47±0.08	1.03	0.11
壬酸	14.79	1266	0.62±0.12	0.67±0.08	1.05	0.11
庚酸	11.26	1078	0.20±0.02	0.16±0.00	1.05	0.10
醛类
苯乙醛	10.61	1043	3.15±0.08	2.76±0.14	0.95	0.15
苯甲醛	9.06	962	1.97±0.03	1.68±0.01	0.86	0.15
己醛	5.67	796	0.57±0.04	0.71±0.02	0.96	0.15
β-环柠檬醛	13.96	1221	0.24±0.01	0.27±0.01	1.02	0.13
2,4-二羟基-6-甲基苯甲醛	17.18	1396	0.21±0.02	0.44±0.08	0.98	0.14
癸醛	13.64	1205	0.06±0.00	0.03±0.00	0.98	0.14
醇类
芳樟醇	11.73	1103	14.62±0.44	18.62±0.27	0.10	0.98
苯甲醇	10.44	1034	5.33±0.17	1.22±0.04	0.05	0.97
苯乙醇	11.94	1115	4.82±0.09	4.00±0.21	0.03	0.94
2-庚醇	7.86	900	3.64±0.38	3.58±0.29	0.01	0.92
叶绿醇	23.38	1861	3.30±0.52	4.69±0.55	0.14	0.92
香叶醇	14.47	1249	3.02±0.14	1.37±0.10	0.30	0.63
Z-3-己烯-1-醇	6.89	854	2.53±0.12	1.31±0.08	0.37	0.62
1-辛烯-3-醇	9.4	980	0.85±0.06	1.53±0.06	0.30	0.60
4-甲基-5-己烯-2-醇	7.58	886	0.81±0.09	0.75±0.05	0.42	0.50
橙花醇	14.02	1225	0.48±0.01	0.33±0.02	0.51	0.42
α-松油醇	13.5	1197	0.34±0.01	0.54±0.03	0.53	0.41
Z-橙花叔醇	20.03	1560	0.16±0.01	0.27±0.03	0.59	0.38
4-甲基己醇	4.38	729	0.14±0.01	0.09±0.01	0.59	0.35
植物醇	24.75	2112	0.13±0.01	0.11±0.03	0.71	0.29
鲸蜡醇	20.55	1591	0.09±0.01	0.17±0.01	0.75	0.27
异植醇	23.91	1947	0.09±0.00	0.08±0.01	0.73	0.26
2-己基-1-癸醇	21.71	1675	0.06±0.01	0.05±0.01	0.76	0.25
正十五醇	22.88	1793	0.05±0.00	0.09±0.01	0.75	0.25
（E）-6-壬烯-1-醇	12.68	1154	0.04±0.00	0.05±0.00	0.87	0.18
3,7,11,15-四甲基-1-十六烷基-3-醇	24.89	2142	0.04±0.00	0.02±0.00	0.87	0.17
癸醇	17.09	1391	0.03±0.00	0.06±0.00	0.95	0.16
月桂醇	17.09	1391	0.03±0.00	0.06±0.00	0.94	0.16

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表 3 不同加工方式紫娟白茶的挥发性成分香气贡献度

Table 3. Aroma contribution of volatile components of Zijuan white tea by different processing methods

挥发性化合物	rOAV		香气类型^[33]
挥发性化合物	TZW	CZW	香气类型^[33]
1-辛烯-3-醇	100	100	清香、蘑菇香、脂香
α-紫罗兰酮	11.12	8.34	果香
苯乙醛	9.25	4.52	花香、清香
β-紫罗兰酮	8.49	4.73	花香、果香
苯甲醛	7.71	3.66	苦杏仁香、果香
环氧-β-紫罗兰酮	6.59	2.74	花香
水杨酸甲酯	3.33	2.77	杏仁香、果香
Z-橙花叔醇	1.93	1.78	花香
己醛	1.48	1.03	果香、清香
β-环柠檬醛	0.57	0.35	果香
芳樟醇	0.54	0.38	花香
香叶醇	0.47	0.12	花香
Z-3-己烯-1-醇	0.42	0.12	清香、药香
橙花醇	0.14	0.05	花香、果香
乙酸叶醇酯	0.14	0.07	果香、药香
2-庚醇	0.10	0.06	果香、药香

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