中国农业科学 ›› 2019, Vol. 52 ›› Issue (19): 3448-3459.doi: 10.3864/j.issn.0578-1752.2019.19.014
李晓颍1,王海静1,徐宁伟1,曹翠玲2,刘建珍1,武春成1,张立彬1()
收稿日期:
2019-03-27
接受日期:
2019-08-21
出版日期:
2019-10-01
发布日期:
2019-10-11
通讯作者:
张立彬
作者简介:
李晓颍,E-mail:xiaoyingli_run@163.com。
基金资助:
LI XiaoYing1,WANG HaiJing1,XU NingWei1,CAO CuiLing2,LIU JianZhen1,WU ChunCheng1,ZHANG LiBin1()
Received:
2019-03-27
Accepted:
2019-08-21
Online:
2019-10-01
Published:
2019-10-11
Contact:
LiBin ZHANG
摘要:
【目的】 优化前处理影响因素,分析欧李果实挥发性成分,明确挥发性成分特点并对果实特征性香气成分进行评价。【方法】 以欧李果实为试材,采用顶空固相微萃取-气相色谱-质谱联用法(HS-SPME-GC-MS)测定其挥发物成分,通过优化前处理影响因素,确定最佳试验条件。利用解卷积系统(AMDIS)与NIST11质谱数据库以及保留指数(RI)对其挥发性成分进行鉴定,内标法确定挥发物含量,并计算香气强度值(OAVs),评价欧李果实香气品质与特征。【结果】 在欧李果实中累计鉴定出63种挥发物,含量范围为0.01—3.25 μg·kg -1。挥发物以酯类、烷类为主,并有少数醇类、芳香类、醛类、萜类、酸类、酮类,其中苯甲酸乙酯含量最高。通过参考相关挥发物香气阈值并计算部分挥发物OAVs可知,己酸乙酯、乙酸苯乙酯、β-芳樟醇、乙酸己酯、壬醛等物质对欧李果实香气成分构成具有重要作用,而烷烃不具有特征性香气。欧李果实香气主要为青香、花香、果香、脂蜡香和其他少数香型(木香型、芳香油香型等),并以青香、花香、果香型物质为主,三者总含量达到挥发物总量的80%。【结论】 优化确立的试验条件为:果肉去核切碎处理,取样量5 g,萃取温度50℃,萃取时间与平衡时间均为30 min。SPME前处理条件对果实挥发性成分检测到的种类与含量有较大影响,通过优化试验条件可以获得最佳检测结果。欧李果实挥发物组成复杂,除烃类物质香气品质较弱外,多数具有特征香气,且香气强度属中高级,酯类物质是欧李果实的重要挥发物组成,清香型、花香型和果香型是欧李果实香气成分的主要特点。
李晓颍,王海静,徐宁伟,曹翠玲,刘建珍,武春成,张立彬. 顶空固相微萃取-气相色谱-质谱联用法分析 欧李果实挥发性成分[J]. 中国农业科学, 2019, 52(19): 3448-3459.
LI XiaoYing,WANG HaiJing,XU NingWei,CAO CuiLing,LIU JianZhen,WU ChunCheng,ZHANG LiBin. Analysis of Volatile Components in Cerasus Humilis (Bge.) Sok by Headspace Solid Phase Microextraction-Gas Chromatography-Mass Spectrometry[J]. Scientia Agricultura Sinica, 2019, 52(19): 3448-3459.
表1
欧李果实挥发性成分及其含量"
序号 No. | 挥发性成分 Volatile | 分子式 Formula | 分子量 Mass | 保留时间 Retention time (min) | 含量 Content (μg·kg-1) | 保留指数 RI | 鉴定依据 Identification | |
---|---|---|---|---|---|---|---|---|
Cal. | Ref. | |||||||
醇类 Alcohol | ||||||||
1 | 2-乙基-己醇 2-Ethyl-hexanol | C8H18O | 130 | 20.30 | 0.02 | 1034 | 1035 | MS, RI |
2 | 辛醇 Octanol | C8H18O | 130 | 23.64 | 0.03 | 1083 | 1087 | MS, RI |
3 | 壬醇 Nonanol | C9H20O | 144 | 29.12 | 0.28 | 1172 | 1171 | MS, RI |
4 | (Z)-3-己烯-1-醇 (Z)-3-Hexen-1-ol | C6H12O | 100 | 8.87 | 0.01 | 855 | 855 | MS, RI |
5 | 苯乙醇 Phenylethyl alcohol | C8H10O | 122 | 26.05 | 0.15 | 1126 | 1121 | MS, RI |
芳香类 Arenes | ||||||||
6 | 邻二甲苯 o-Xylene | C8H10 | 106 | 9.60 | 0.06 | 870 | 879 | MS, RI |
7 | 萘 Naphthalene | C10H8 | 128 | 29.23 | 0.02 | 1174 | 1170 | MS, RI |
8 | 2-甲基萘 2-Methylnaphthalene | C11H10 | 142 | 33.81 | 0.03 | 1289 | 1289 | MS, RI |
酸类 Acids | ||||||||
9 | 苯甲醛 Benzaldehyde | C7H6O | 106 | 14.96 | 0.12 | 956 | 961 | MS, RI |
10 | 壬醛 Nonanal | C9H18O | 142 | 25.62 | 0.16 | 1117 | 1107 | MS, RI |
11 | (E)-3-甲基-4-癸烯酸 (E)-3-Methyl-4-decenoic acid | C11H20O2 | 184 | 37.59 | 0.06 | 1413 | 1415 | MS, RI |
萜类 Terpenoids | ||||||||
12 | β-芳樟醇 β-Linalool | C10H18O | 154 | 25.35 | 0.24 | 1111 | 1103 | MS, RI |
13 | α-法呢烯 α-Farnesene | C15H24 | 204 | 39.63 | 0.1 | 1512 | 1512 | MS, RI |
烷类 Alkyls | ||||||||
14 | 2-壬酮 2-Nonanone | C9H18O | 142 | 24.93 | 0.05 | 1102 | 1104 | MS, RI |
15 | 十二烷 Dodecane | C12H26 | 170 | 30.25 | 0.48 | 1200 | 1200 | MS, RI |
16 | 十三烷 Tridecane | C13H28 | 184 | 34.24 | 0.61 | 1300 | 1300 | MS, RI |
17 | 2-甲基-十三烷 2-Methyl-tridecane | C14H30 | 198 | 36.36 | 0.04 | 1369 | 1362 | MS, RI |
18 | 法呢烷 Farnesane | C15H32 | 212 | 36.72 | 0.08 | 1381 | 1378 | MS, RI |
19 | 十四烷 Tetradecane | C14H30 | 198 | 37.33 | 0.32 | 1400 | 1400 | MS, RI |
20 | 正辛基环己烷 Octylcyclohexane | C14H28 | 196 | 38.39 | 0.10 | 1451 | 1451 | MS, RI |
21 | 5-甲基-十四烷 5-Methyl-tetradecane | C15H32 | 212 | 38.51 | 0.07 | 1456 | 1454 | MS, RI |
22 | 4-甲基-十四烷 4-Methyl-tetradecane | C15H32 | 212 | 38.62 | 0.11 | 1462 | 1460 | MS, RI |
23 | 4,11-二甲基-十四烷 4,11-Dimethyl-tetradecane | C16H34 | 226 | 38.70 | 0.85 | 1465 | 1464 | MS, RI |
24 | 3-甲基-十四烷 3-Methyl-tetradecane | C15H32 | 212 | 38.87 | 0.14 | 1473 | 1470 | MS, RI |
25 | 十五烷 Pentadecane | C15H32 | 212 | 39.44 | 1.31 | 1500 | 1500 | MS, RI |
26 | 5-丙基-十三烷 5-Propyl-tridecane | C16H34 | 226 | 39.69 | 0.16 | 1515 | 1516 | MS, RI |
27 | 6-甲基-十五烷 6-Methyl-pentadecane | C16H34 | 226 | 40.29 | 0.06 | 1551 | 1551 | MS, RI |
28 | 壬基环已烷 n-Nonylcyclohexane | C15H30 | 210 | 40.37 | 0.22 | 1556 | 1556 | MS, RI |
29 | 4-甲基-十五烷 4-Methyl-pentadecane | C16H34 | 226 | 40.45 | 0.04 | 1560 | 1557 | MS, RI |
30 | 2-甲基-十五烷 2-Methyl-pentadecane | C16H34 | 226 | 40.53 | 0.15 | 1566 | 1564 | MS, RI |
序号 No. | 挥发性成分 Volatile | 分子式 Formula | 分子量 Mass | 保留时间 Retention time (min) | 含量 Content (μg·kg-1) | 保留指数 RI | 鉴定依据 Identification | |
Cal. | Ref. | |||||||
31 | 3-甲基-十五烷 3-Methyl-pentadecane | C16H34 | 226 | 40.65 | 0.12 | 1573 | 1571 | MS, RI |
32 | 十六烷 Hexadecane | C16H34 | 226 | 41.11 | 0.36 | 1600 | 1600 | MS, RI |
33 | 2,6,10-三甲基-十五烷 2,6,10-Trimethyl-pentadecane | C18H38 | 254 | 41.84 | 0.17 | 1643 | 1649 | MS, RI |
酯类 Esters | ||||||||
34 | 乙酸乙酯 Ethyl acetate | C4H8O2 | 88 | 2.95 | 0.32 | 659 | 634 | MS |
35 | 己酸乙酯 Ethyl hexanoate | C8H16O2 | 144 | 18.14 | 0.11 | 1003 | 1001 | MS, RI |
36 | 乙酸叶醇酯 (Z)-3-Hexenyl acetate | C8H14O2 | 142 | 18.63 | 0.25 | 1010 | 1007 | MS, RI |
37 | 乙酸己酯 Hexyl acetate | C8H16O2 | 144 | 19.15 | 0.66 | 1017 | 1017 | MS, RI |
38 | 苯甲酸甲酯 Methyl benzoate | C8H8O2 | 136 | 24.87 | 0.05 | 1101 | 1093 | MS, RI |
39 | 异丁酸叶醇酯 (Z)-3-Hexenyl isobutyrate | C10H18O2 | 170 | 27.79 | 0.21 | 1138 | 1145 | MS, RI |
40 | 丁酸己酯 Hexyl butanoate | C10H20O2 | 172 | 28.05 | 0.10 | 1145 | 1148 | MS, RI |
41 | 己酸异丁酯 Isobutyl hexanoate | C10H20O2 | 172 | 28.16 | 0.07 | 1147 | 1148 | MS, RI |
42 | 乙酸苯甲酯 Benzyl acetate | C9H10O2 | 150 | 28.69 | 0.14 | 1161 | 1161 | MS, RI |
43 | 苯甲酸乙酯 Ethyl benzoate | C9H10O2 | 150 | 28.92 | 3.25 | 1167 | 1170 | MS, RI |
44 | 4-辛烯酸乙酯 Ethyl 4-octenoate | C10H18O2 | 170 | 29.87 | 0.04 | 1190 | 1191 | MS, RI |
45 | 辛酸乙酯 Ethyl octanoate | C10H20O2 | 172 | 30.22 | 0.20 | 1199 | 1201 | MS, RI |
46 | 乙酸辛酯 Octyl acetate | C10H20O2 | 172 | 30.80 | 0.04 | 1214 | 1213 | MS, RI |
47 | 异戊酸叶醇酯 cis-3-Hexenyl isovalerate | C11H20O2 | 184 | 31.56 | 0.42 | 1233 | 1235 | MS, RI |
48 | 异戊酸己酯 Hexyl 2-methylbutyrate | C11H22O2 | 186 | 31.74 | 0.24 | 1237 | 1239 | MS, RI |
49 | 2-辛烯酸乙酯 Ethyl (E)-2-octenoate | C10H18O2 | 170 | 32.12 | 0.04 | 1247 | 1246 | MS, RI |
50 | 己酸异戊酯 Isoamyl hexanoate | C11H22O2 | 186 | 32.23 | 0.05 | 1250 | 1251 | MS, RI |
51 | 乙酸苯乙酯 Phenethyl acetate | C10H12O2 | 164 | 32.47 | 1.16 | 1256 | 1256 | MS, RI |
52 | 辛酸丙酯 Propyl octanoate | C11H22O2 | 186 | 33.96 | 0.05 | 1293 | 1292 | MS, RI |
53 | 壬酸乙酯 Ethyl nonanoate | C11H22O2 | 186 | 34.15 | 0.05 | 1298 | 1298 | MS, RI |
54 | 乙酸壬酯 Nonyl acetate | C11H22O2 | 186 | 34.73 | 0.08 | 1316 | 1314 | MS, RI |
55 | 乙酸橙花酯 Neryl Acetate | C12H20O2 | 196 | 36.95 | 0.03 | 1388 | 1372 | MS, RI |
56 | (E)-己酸-2-己烯酯 (E)-2-Hexenyl hexanoate | C12H22O2 | 198 | 37.10 | 0.14 | 1393 | 1391 | MS, RI |
57 | 癸酸乙酯 Ethyl caprate | C12H24O2 | 200 | 37.25 | 0.21 | 1398 | 1398 | MS, RI |
58 | (Z)-庚酸-3-己烯酯 (Z)-3-Hexenyl heptanoate | C13H24O2 | 212 | 39.08 | 0.13 | 1483 | 1489 | MS, RI |
59 | 庚酸丁酯 Butyl heptanoate | C11H22O2 | 186 | 39.17 | 0.07 | 1488 | 1490 | MS, RI |
60 | (Z)-3-辛酸己烯酯 (Z)-3-Hexenyl octanoate | C14H26O2 | 226 | 40.80 | 0.78 | 1582 | 1588 | MS, RI |
61 | 辛酸己酯 Hexyl octanoate | C14H28O2 | 228 | 40.86 | 0.54 | 1585 | 1582 | MS, RI |
62 | 月桂酸乙酯 Ethyl laurate | C14H28O2 | 228 | 41.05 | 0.17 | 1596 | 1597 | MS, RI |
63 | 软脂酸乙酯 Ethyl palmitate | C18H36O2 | 284 | 46.14 | 0.09 | 1900 | 1914 | MS, RI |
表2
欧李果实挥发性成分香气强度与品质"
化合物 Compound | 香气阈值 Odor threshold (μg·kg-1) | 香气强 度值 OAVs | 香气品质 Aroma quality[ | 香气类型 Odor type[ | 香气强度 Odor strength[ |
---|---|---|---|---|---|
苯甲醛 Benzaldehyde | 350[ | <0.001 | 苦杏仁味 Bitter almond-like | 芳香型 Aromatic | 高 High |
邻二甲苯 o-Xylene | 天竺葵香气 Geranium-like | 芳香型 Aromatic | 中 Medium | ||
苯甲酸甲酯 Methyl benzoate | 0.52[ | 0.096 | 杏仁味 Almond-like | 酚香型 Phenolic | 高 High |
己酸乙酯 Ethyl hexanoate | 0.01[ | 10.873 | 凤梨果香 Pineapple-like | 果香型 Fruity | 高 High |
异丁酸叶醇酯 (Z)-3-Hexenyl isobutyrate | 苹果香 Apple-like | 果香型 Fruity | 高 High | ||
乙酸己酯 Hexyl acetate | 2[ | 0.33 | 梨子香 Pear-like | 果香型 Fruity | 中 Medium |
2-壬酮 2-Nonanone | 5[ | 0.01 | 似草香、泥土气息 Weedy and earthy-like | 果香型 Fruity | 中 Medium |
4-辛烯酸乙酯 Ethyl 4-octenoate | 柑橘气味 Citrus-like | 果香型 Fruity | 中 Medium | ||
2-辛烯酸乙酯 Ethyl (E)-2-octenoate | 凤梨果香 Pineapple-like | 果香型 Fruity | 中 Medium | ||
己酸异戊酯 Isoamyl hexanoate | 苹果香 Apple-like | 果香型 Fruity | 中 Medium | ||
2-乙基-己醇 2-Ethyl-hexanol | 香草味 Herbaceou-like | 花香型 Floral | 中 Medium | ||
β-芳樟醇 β-Linalool | 0.5[ | 0.476 | 铃兰香气 Keiskei-like | 花香型 Floral | 中 Medium |
苯乙醇 Phenylethyl alcohol | 750[ | <0.001 | 玫瑰花香 Rose-like | 花香型 Floral | 中 Medium |
乙酸苯甲酯 Benzyl acetate | 茉莉花香 Jasmin fresh | 花香型 Floral | 中 Medium | ||
壬醇 Nonanol | 50[ | 0.006 | 玫瑰花、甜橙气息 Rose-and orange-like | 花香型 Floral | 中 Medium |
乙酸辛酯 Octyl acetate | 12[ | 0.003 | 花香、草香 Floral and herbal-like | 花香型 Floral | 中 Medium |
乙酸苯乙酯 Phenethyl acetate | 0.25[ | 4.629 | 甜蜜香味 Sweet honey-like | 花香型 Floral | 中 Medium |
2-甲基萘 2-Methylnaphthalene | 甜香 Sweety | 花香型 Floral | 中 Medium | ||
乙酸橙花酯 Neryl Acetate | 甜香 Sweet floral | 花香型 Floral | 中 Medium | ||
乙酸乙酯 Ethyl acetate | 5[ | 0.064 | 略带水果的酒香气味 Slightly fruity and winey-like | 醚香型 Ethereal | 高 High |
α-法呢烯 α-Farnesene | 草香 Herbal-like | 木香型 Woody | 中 Medium | ||
(Z)-3-己烯-1-醇 (Z)-3-Hexen-1-ol | 香草味 Herbaceous-like | 青香型 Green | 高 High | ||
乙酸叶醇酯 (Z)-3-Hexenyl acetate | 香蕉味 Banana-like | 青香型 Green | 高 High | ||
丁酸己酯 Hexyl butanoate | 250[ | <0.001 | 蔬菜气息 Vegetables-like | 青香型 Green | 中 Medium |
己酸异丁酯 Isobutyl hexanoate | 可可香气 Cocoa-like | 青香型 Green | 中 Medium | ||
苯甲酸乙酯 Ethyl benzoate | 60[ | 0.054 | 焦油味 Tar-like | 青香型 Green | 中 Medium |
异戊酸叶醇酯 cis-3-Hexenyl isovalerate | 青苹果气息 Green apple-like | 青香型 Green | 中 Medium | ||
异戊酸己酯 Hexyl 2-methylbutyrate | 生果实味 Raw fruit-like | 青香型 Green | 中 Medium | ||
(E)-己酸-2-己烯酯 (E)-2-Hexenyl hexanoate | 青香 Green | 青香型 Green | 中 Medium | ||
庚酸丁酯 Butyl heptanoate | 甘草味 Licorice-like | 青香型 Green | 中 Medium | ||
(Z)-3-辛酸己烯酯 (Z)-3-Hexenyl octanoate | 弱的青香 Faint Green-like | 青香型 Green | 中 Medium | ||
辛酸己酯 Hexyl octanoate | 新鲜蔬菜气息 Fresh Vegetables-like | 青香型 Green | 中 Medium | ||
壬醛 Nonanal | 1[ | 0.156 | 柑橘香 Citrus-like | 醛香型 Aldehydic | 高 High |
萘 Naphthalene | 21[ | 0.001 | 干树脂气味 Dry resinous | 辛香型 Spicy | 高 High |
辛酸丙酯 Propyl octanoate | 椰子气味 Coconut-like | 椰子香型 Coconut | 中 Medium | ||
软脂酸乙酯 Ethyl palmitate | 2000[ | <0.001 | 微弱蜡香 Soft waxy-like | 脂蜡香型 Waxy | 低 Low |
辛醇 Octanol | 110[ | <0.001 | 脂蜡香气、柑橘气息 Waxy and orange-like | 脂蜡香型 Waxy | 中 Medium |
辛酸乙酯 Ethyl octanoate | 5[ | 0.04 | 白兰地香气 Brandy-like | 脂蜡香型 Waxy | 中 Medium |
壬酸乙酯 Ethyl nonanoate | 略带脂肪-油脂气味 Slightly fatty-oily-like | 脂蜡香型 Waxy | 中 Medium | ||
乙酸壬酯 Nonyl acetate | 果香和栀子花香气 Fruity and gardenia-like | 脂蜡香型 Waxy | 中 Medium | ||
癸酸乙酯 Ethyl caprate | 23[ | <0.001 | 油脂、酒香气味 Oily and winey-like | 脂蜡香型 Waxy | 中 Medium |
月桂酸乙酯 Ethyl laurate | 花生香气 Peanut-like | 脂蜡香型 Waxy | 中 Medium |
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