顶空固相微萃取-气相色谱质谱法分析红富士葡萄果实香气

李凯; 商佳胤; 苏宏; 田淑芬; 黄建全; 张娜; 王丹; 王超霞

doi:10.19303/j.issn.1008-0384.2021.04.007

顶空固相微萃取-气相色谱质谱法分析红富士葡萄果实香气

doi: 10.19303/j.issn.1008-0384.2021.04.007

李凯^1,,
商佳胤¹,
苏宏¹,
田淑芬^2, ,,
黄建全¹,
张娜¹,
王丹¹,
王超霞²

1.
天津市农业科学院果树研究所，天津　300384
2.
天津农学院园艺园林学院，天津　300384

基金项目: 中国农学会青年人才托举工程第四届（2018-2020年度）项目（2018QNRC001）；天津市林果现代农业产业技术体系（ITTFPRS2018005）；国家现代农业（葡萄）产业技术体系建设专项（CARS-29-zp-1）；青年科研人员创新研究与实验项目（201914）

详细信息

作者简介:
李凯（1987−），男，硕士，助理研究员，研究方向：葡萄栽培与酿酒（E-mail：kaiwine@126.com）

通讯作者:
田淑芬（1966−），女，教授，研究方向：葡萄次生代谢（E-mail：tianshufen@263.net）

中图分类号: S 663.1
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出版历程
- 收稿日期: 2020-07-25
- 修回日期: 2020-11-26
- 网络出版日期: 2021-03-27
- 刊出日期: 2021-04-30

Composition and Characteristics of Benifuji Grape Aroma

1.
Pomology Institute, Tianjin Academy of Agricultural Sciences, Tianjin　300384, China
2.
College of Horticulture and Landscape Architecture, Tianjin Agricultural College, Tianjin　300384, China

摘要

摘要: 目的检测分析天津产区红富士葡萄果实香气，研究其葡萄果实的活性呈香成分及香气特征。方法采用顶空固相微萃取（HS-SPME）及气相色谱-质谱技术（GC-MS）提取检测果实香气，内标-标准曲线法定量，结合气味活性值及果实香气轮廓，分析葡萄果实活性呈香成分及香气特征。结果天津产区红富士葡萄果实中共定性定量39种香气化合物（总浓度9737.05 μg·L⁻¹），酯类浓度最高，醇类次之；乙酸乙酯、1-己醇、反式-2-己烯-1-醇、丁酸乙酯和反式-2-己烯-1-醛是5种主要香气成分，它们的浓度之和（9461.79 μg·L⁻¹）与检出化合物总浓度的比值高达97.17%，其中乙酸乙酯浓度（9036.53 μg·L⁻¹）最为突出，分别占酯类浓度、总浓度的98.53%和92.81%；气味活性值结果显示，其果实香气主要由丁酸乙酯、2-甲基丁酸乙酯、己酸乙酯和异丁酸乙酯等12种活性呈香成分贡献；香气轮廓直观地显示，其果实香气主要由花卉类、水果类、植物类、脂肪类、化学类和香料类气味构成，其中水果类气味最为突出。结论天津产区红富士葡萄果实香气主要由酯类、醇类和醛类成分构成，含量最为丰富的酯类化合物贡献了突出的水果类气味。
- 红富士葡萄 /
- 顶空固相微萃取 /
- 香气成分 /
- 气味活性值 /
- 香气轮廓
Abstract: Objective Aromatic compounds and characteristics of Benifuji grapes grown in Tianjin were analyzed. Method Headspace solid phase microextraction (HS-SPME) and gas chromatography-mass spectrometry (GC-MS) were used to extract, determine, and quantify by internal standards and standard curves on the aromatics in Benifuji grapes. Olfactory property of the grapes was characterized according to the odor activity value (OAV) and aroma profiling. Result Thirty-nine aromatic compounds in a combined concentration of 9 737.05 μg·L⁻¹ were identified. Esters were the dominant substances followed by alcohols. Ethyl acetate, 1-hexanol, trans-2-hexene-1-ol, ethyl butyrate, and trans-2-hexene-1-al were the 5 major aromatics, totaling 9 461.79 μg·L⁻¹ in concentration and accounting for 97.17% of the total relevant volatiles. Ethyl acetate concentration, which constituted 9 036.53 μg·L⁻¹, was by far the greatest amount among all. It accounted for 98.53% of all esters and 92.81% of total aromatics. The OAV of the grapes was contributed mainly by 12 compounds, such as ethyl butyrate, ethyl-2-methylbutyrate, ethyl hexanoate, and ethyl isobutyrate. A visualized aroma profiling for the grapes showed characteristics of flowers, fruits, plants, fats, chemicals, and spices, with the fruity note the most predominant. Conclusion The aroma of Benifuji grapes grown in Tianjin was made of volatiles including esters, alcohols, and aldehydes, with the esters being the most predominant components in quantity.
- Benifuji grape /
- headspace solid phase microextraction (HS-SPME) /
- aroma component /
- odor activity value /
- aroma profile

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图 1 红富士葡萄果实香气轮廓

Figure 1. Aroma profile of Benifuji grapes

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表 1 红富士葡萄果实香气成分种类、数量及浓度

Table 1. Category, number, and concentration of aromatics in Benifuji grapes

化合物 Compounds	数量 Number	浓度 Concentration/ （μg·L⁻¹）	占总质量浓度比值 Ratio of subtotal to total/%
醇类 Alcohols	12	433.33±14.23	4.45±0.15
酯类 Esters	12	9170.95±58.55	94.19±0.60
萜烯类 Terpenes	4	16.90±0.68	0.17±0.00
醛类 Aldehydes	7	103.25±6.28	1.06±0.06
其他类 Others	4	12.62±0.46	0.13±0.00
总计 Total	39	9737.05±80.20	100.00
注：数据为平均值±标准差，下同。 Note: The data were mean ± standard deviation, the same below.

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表 2 红富士葡萄果实香气成分浓度

Table 2. Concentrations of aromatics in Benifuji grapes

编号 Code	化合物 Compounds	保留时间 Retention time/min	匹配因子 Match factor	标准品质量浓度范围 Standard concentration range/（μg·L⁻¹）	水中阈值 Odour threshold in water/（μg·L⁻¹）	果实中质量浓度 Concentration in grape/（μg·L⁻¹）
	醇类 Alcohols
V1	正丁醇 1-Butanol	2.878	82.50	3.12-50.00	500^[17-19]	8.17±0.42
V2	3-甲基-1-丁醇 3-Methyl-1-butanol	4.041	99.24	12.50-200.00	300^[17,19]	9.87±0.36
V3	2-甲基-1-丁醇 2-Methyl-1-butanol	4.136	99.36	3.12-50.00	300^[18]	4.93±0.19
V4	正戊醇 1-Pentanol	4.836	96.30	12.50-200.00	4000^[17,19]	36.70±1.13
V5	反式-2-己烯-1-醇 trans-2-Hexen-1-ol	7.774	91.20	125.00-2000.00	100^[20]	144.54±4.55
V6	1-己醇 1-Hexanol	7.862	96.77	125.00-2000.00	500^[17-18]	167.13±5.17
V7	1-庚醇 1-Heptanol	11.637	95.52	3.12-50.00	425^[17]	5.29±0.61
V8	1-辛烯-3-醇 1-Octen-3-ol	11.911	97.80	3.12-50.00	1^[19,21]	7.78±0.55
V9	2-乙基己醇 2-Ethyl-hexanol	13.785	98.50	3.12-50.00	270^[22]	0.04±0.00
V10	苯甲醇 Benzyl alcohol	14.006	95.40	12.50-200.00	10000^[4,19]	41.72±0.92
V11	1-辛醇 1-Octanol	15.428	95.20	3.12-50.00	110^[19]	4.10±0.15
V12	2-苯乙醇 2-Phenylethyl alcohol	16.926	99.00	62.50-1000.00	1100^[4,19]	3.07±0.18
	酯类 Esters
V13	乙酸乙酯 Ethyl acetate	2.254	98.20	1875.00-30000.00	5000^[17]	9036.53±53.85
V14	丙酸乙酯 Ethyl propionate	3.604	97.56	3.12-50.00	10^[17]	15.88±0.76
V15	乙酸丙酯 Propyl acetate	3.657	96.63	3.12-50.00	4700^[23]	5.98±0.46
V16	异丁酸乙酯 Ethyl isobutyrate	4.649	92.70	1.25-20.00	0.1^[17]	1.36±0.08
V17	丁酸乙酯 Ethyl butyrate	5.737	98.98	7.50-120.00	1^[17]	62.31±1.23
V18	乙酸丁酯 Butyl acetate	6.140	99.30	1.25-20.00	66^[17]	0.52±0.02
V19	2-甲基丁酸乙酯 Ethyl-2-methylbutyrate	7.250	98.62	1.25-20.00	0.1^[24]	4.35±0.17
V20	己酸乙酯 Ethyl hexanoate	12.702	91.85	1.25-20.00	1^[17]	15.46±0.69
V21	乙酸己酯 Hexyl acetate	13.223	95.52	1.25-20.00	670^[23,25]	6.07±0.30
V22	辛酸乙酯 Ethyl octanoate	20.055	98.09	1.25-20.00	194^[17]	9.94±0.41
V23	乙酸苯乙酯 Phenylethyl acetate	22.108	98.55	1.25-20.00	480^[17]	6.21±0.27
V24	壬酸乙酯 Ethyl nonanoate	23.488	96.99	1.25-20.00	377^[17]	6.34±0.31
	萜烯类Terpenes
V25	β-蒎烯 β-pinene	12.318	90.42	12.50-200.00	140^[17]	1.36±0.02
V26	柠檬烯 Limonene	13.679	97.68	3.12-50.00	10^[4,19]	6.16±0.24
V27	异松油烯 Terpinolene	15.956	97.85	1.25-20.00	200^[17]	5.08±0.24
V28	里哪醇 Linalool	16.432	98.93	62.50-1000.00	6^[4,18]	4.30±0.18
	醛类 Aldehydes
V29	正戊醛 Pentanal	3.292	93.70	3.12-50.00	12^[19]	2.90±0.10
V30	正己醛 Hexanal	5.592	96.80	31.25-500.00	4.5^[17,18]	10.19±0.49
V31	反式-2-己烯-1-醛 trans-2-Hexen-1-al	7.265	94.90	125.00-2000.00	17^[19]	51.28±3.65
V32	正庚醛 Heptanal	8.987	98.80	3.12-50.00	3^[19]	5.12±0.26
V33	苯甲醛 Benzaldehyde	11.082	99.00	3.12-50.00	350^[17,18]	7.26±0.32
V34	苯乙醛 Phenylacetaldehyde	14.291	94.30	3.12-50.00	4^[17,18]	26.48±1.46
V35	壬醛 Nonanal	16.610	99.60	1.25-20.00	1^[17]	0.02±0.00
	其他 Others
V36	6-甲基-5-庚烯-2-酮 6-Methyl-5-heptene 2-one	12.230	83.90	3.12-50.00	50^[19]	9.30±0.33
V37	2-辛酮 2-Octanone	12.352	89.70	3.12-50.00	5^[17]	2.64±0.12
V38	苯乙烯 Styrene	8.508	98.49	0.62-10.00	37^[26]	0.11±0.00
V39	辛酸 Octanoic acid	20.085	93.67	0.62-10.00	3000^[17]	0.57±0.01

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表 3 活性呈香成分的气味活性值（OAV）

Table 3. OAVs of active aromatic components

化合物 Compounds	香气描述 Odour descriptor	香系 Odourseries	OAV
反式-2-己烯-1-醇 trans-2-Hexen-1-ol	草本绿植^[20,25,27]，树叶、胡桃木^[28] Herbaceous green, leaf, walnut	3	1.45±0.05
1-辛烯-3-醇 1-Octen-3-ol	蘑菇^[21,28,29]，青草、鱼腥味^[30] Mushroom,fishy, grassy	3, 4	7.78±0.55
乙酸乙酯 Ethyl acetate	菠萝^{[25,28,31,32]}，溶剂^[25,33]，香料^[31]，大茴香^[32]Pineapple, solvent, balsamic, anise	2, 5, 6	1.81±0.01
丙酸乙酯 Ethyl propionate	水果^[18]，香蕉、苹果^[31] Fruit, banana, apple	2	1.59±0.08
异丁酸乙酯 Ethyl isobutyrate	香蕉^[30]，甜香^[28,34]，橡胶^[28]，水果^[30,31,34] Banana, sweet, rubber, fruity	2, 5	13.64±0.80
丁酸乙酯 Ethyl butyrate	苹果^[28,30,34]，菠萝、香蕉^[34] Apple, pineapple, banana	2	62.31±1.23
2-甲基丁酸乙酯 Ethyl-2-methylbutyrate	苹果^[28] Apple	2	43.54±1.70
己酸乙酯 Ethyl hexanoate	水果^[28,34]，青苹果、香蕉、类似红酒^[23,31] Fruity, green apple banana, wine-like	2	15.46±0.69
正己醛 Hexanal	鱼腥味^[30]，青草^[28,30]，动物脂油、脂肪^[28] Fishy, grass, tallow, fat	3, 4	2.27±0.11
反式-2-己烯-1-醛 trans-2-Hexen-1-al	青草^[27]，绿叶^[28] Grass herbaceous, green leaf,	3	3.03±0.21
正庚醛 Heptanal	柑橘类植物、脂肪、不新鲜的^[28]，鱼干^[30] Citrus, fat, rancid, dry fish	3, 4	1.71±0.09
苯乙醛 Phenylacetaldehyde	山楂花、蜂蜜、甜香^[28]，玫瑰^[35] Hawthorn, honey, sweet, rose	1, 2	6.62±0.37
注：气味系列：1：花卉类，2：水果类，3：植物类，4：脂肪类，5：化学类，6：香料类，7：烘焙类，8：矿物类。 Note: Odour series: 1: Floral, 2: Fruity, 3: Vegetal, 4: Fatty, 5: Chemical, 6: Spicy, 7: Roast, 8: Mineral.

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