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中国精品科技期刊2020

顶空固相微萃取-全二维气相色谱/飞行时间质谱测定三种芒果香气成分

黄豆 曹烙文 岑延相 区梓峰 胡韩 谭国斌 麦泽彬 黄正旭 李雪 吴曼曼

黄豆,曹烙文,岑延相,等. 顶空固相微萃取-全二维气相色谱/飞行时间质谱测定三种芒果香气成分[J]. 食品工业科技,2021,42(15):218−226. doi:  10.13386/j.issn1002-0306.2020070275
引用本文: 黄豆,曹烙文,岑延相,等. 顶空固相微萃取-全二维气相色谱/飞行时间质谱测定三种芒果香气成分[J]. 食品工业科技,2021,42(15):218−226. doi:  10.13386/j.issn1002-0306.2020070275
HUANG Dou, CAO Luowen, CEN Yanxiang, et al. Detection of Aroma Components in Three Cultivars of Mango with Headspace Solid Phase Microextraction-Comprehensive Two-dimensional Gas Chromatograph/Time of Flight Mass Spectrometer[J]. Science and Technology of Food Industry, 2021, 42(15): 218−226. (in Chinese with English abstract). doi:  10.13386/j.issn1002-0306.2020070275
Citation: HUANG Dou, CAO Luowen, CEN Yanxiang, et al. Detection of Aroma Components in Three Cultivars of Mango with Headspace Solid Phase Microextraction-Comprehensive Two-dimensional Gas Chromatograph/Time of Flight Mass Spectrometer[J]. Science and Technology of Food Industry, 2021, 42(15): 218−226. (in Chinese with English abstract). doi:  10.13386/j.issn1002-0306.2020070275

顶空固相微萃取-全二维气相色谱/飞行时间质谱测定三种芒果香气成分

doi: 10.13386/j.issn1002-0306.2020070275
基金项目: 2017年国家重点研发计划(2017YFB1103903);广东省协同创新与平台环境建设(2019B121205004);2019年度广东省国际科技合作项目国际合作项目(2018A050506020)。
详细信息
    作者简介:

    黄豆(1994−),男,本科,助理工程师,研究方向:全二维气相色谱-飞行时间质谱仪应用方法开发,E-mail: huangdou1224@163.com

    通讯作者:

    吴曼曼(1989−),女,硕士,中级工程师,研究方向:从事飞行时间质谱仪的研发和应用,Email:mm.wu@hxmass.com

  • 中图分类号: TS207.3

Detection of Aroma Components in Three Cultivars of Mango with Headspace Solid Phase Microextraction-Comprehensive Two-dimensional Gas Chromatograph/Time of Flight Mass Spectrometer

  • 摘要: 本文采用顶空固相微萃取(Headspace Solid Phase Microextraction,HS-SPME)与全二维气相色谱/飞行时间质谱联用仪(Comprehensive Two-dimensional Gas Chromatograph/Time of Flight Mass Spectrometer,GC×GC-TOFMS)比较了不同萃取头、萃取温度、萃取时间、解吸温度等因素对萃取效果的影响,对三个品种的芒果香气成分进行了分析鉴定。结果表明,最适萃取条件为:萃取头50/30 μm DVB/CAR /PDMS(Divinylbenzene/Carboxen/Polydimethylsiloxane),萃取温度60 ℃,萃取时间60 min,解吸温度250 ℃。凭借全二维气相色谱/飞行时间质谱联用仪强大的分离及定性能力,可以获得比常规一维气相色谱/质谱联用仪更多的香气成分信息。3种芒果共检测出170种香气成分,金煌芒、小台芒、青皮芒中分别测到96、90、68种香气成分,峰面积含量占各自挥发性成分总量的74.04%、90.75%、78.91%。170种香气成分中醇类25种、芳香烃4种、醛类15种、酸类6种、酮类18种、烯烃56种、酯类46种,7类化合物中烯烃类化合物在三种芒果中含量占比最高,金煌芒中含有相比其他两种芒果具有更多的酯类、醛类和醇类等香气成分,相应的青皮芒独有的香味成分则相对较少,这也是金煌芒香气浓郁,而青皮芒香气较寡淡的原因。3种芒果共有的香气成分有26种,比如萜品油烯、3-蒈烯、β-月桂烯、石竹烯、珂巴烯和γ-依兰油烯等烯烃组成芒果基本的香气,但共有成分在不同品种芒果中的含量存在明显差异。比如,金煌芒中3-蒈烯明显更高,含量为10.783%,小台芒中萜品油烯明显更高,含量为17.545%。
  • 图  1  GC×GC和GC分离效果对比图

    Figure  1.  Separation effect comparison of GC×GC and GC

    图  2  反向和正向柱系统测试金煌芒的二维色谱轮廓图

    Figure  2.  Chromatogram of JinHuang mango tested by reverse and forward column systems

    注:a:反向柱系统;b:正向柱系统。

    图  3  四种香气成分的质谱匹配图

    Figure  3.  Mass spectrum matching map of four kinds of aroma components

    注:a:3-蒈烯;b:萜品油烯;c:邻伞花烃;d:αα,4-三甲基苯甲醇。

    图  4  三种芒果的二维色谱轮廓图

    Figure  4.  Chromatogram of three kinds of mangos

    注:a:金煌芒;b:小台芒;c:青皮芒。

    表  1  不同萃取头的萃取效果

    Table  1.   Extraction effect of different fiber

    萃取头类型PDMSDVB/CAR/PDMS
    总峰面积795360945479
    检出有效化合物总数(个)88114
    下载: 导出CSV

    表  2  不同萃取温度下的萃取效果

    Table  2.   Extraction effect of different extraction temperature

    萃取头温度(℃)506070
    总峰面积902356945479923432
    检出有效化合物总数(个)98114110
    下载: 导出CSV

    表  3  不同萃取时间下的萃取效果

    Table  3.   Extraction effect of different extraction time

    萃取头时间(min)506070
    总峰面积894556945479933227
    检出有效化合物总数(个)93114110
    下载: 导出CSV

    表  4  不同解吸温度下的萃取效果

    Table  4.   Extraction effect of different desorption temperature

    解吸温度(℃)240250260
    总峰面积927956945479944678
    检出有效化合物总数(个)101114110
    下载: 导出CSV

    表  5  三种芒果的香气成分及相对含量

    Table  5.   Aroma components and relative contents of three kinds of mangos

    序号类别化合物名称 化学式 一维时间(min)二维时间(s)金煌芒(%)小台芒(%)青皮芒(%)
    1醇类乙醇C2H6O4.280.610.7071.0400.088
    2异戊醇C5H12O10.950.830.007
    31-己醇C6H14O14.950.900.010
    43-己烯-1-醇C6H12O15.780.860.3210.0010.003
    5环己基甲醇C7H14O20.452.230.004
    64-萜烯醇C10H18O21.031.600.002
    73-环戊基-1-丙醇C8H16O22.532.630.009
    8顺式-3-壬烯-1-醇C9H18O23.121.080.013
    9α-松油醇C10H18O23.281.320.053
    10(6Z)-壬烯-1-醇C9H18O23.781.060.005
    11对薄荷-1,5-二烯-8-醇C10H1624.031.200.010
    12(E,Z)-3,6-亚壬基-1-醇C9H16O24.531.010.853
    13(E,Z)-3,6-壬二烯-1-醇C9H16O24.621.000.313
    14反式,顺式-2,6-壬二烯-1-醇C9H16O24.950.980.0100.005
    15(E)-2-癸烯-1-醇C10H20O25.782.440.025
    164-丙基-1,6-庚二烯-4-醇C10H18O26.032.430.088
    17异香芹醇C10H16O26.281.290.0630.010
    18αα,4-三甲基苯甲醇C10H14O26.701.040.3840.5510.239
    19醇类苯甲醇C7H8O27.280.730.1260.0600.005
    20苯乙醇C8H10O27.950.840.0060.004
    211-十二醇C12H26O29.031.340.010
    22二-表-1,10-库贝醇C15H26O30.702.280.029
    23蓝桉醇C15H26O33.371.920.217
    24α-杜松醇C15H26O33.871.730.046
    251-十六醇C16H34O36.531.702.366
    26芳香烃类对伞花烃C10H1412.282.652.776
    27邻伞花烃C10H1412.482.691.9830.4403.784
    284-异丙烯基甲苯C10H1216.952.010.042
    29去氢白菖烯C15H2225.953.270.3960.6000.007
    30醛类2-己烯醛C6H10O11.031.490.015
    31苯甲醛C7H6O19.121.180.0480.301
    32(E)-2-壬醛C9H16O19.371.760.1640.013
    33(E,Z)-2,6-壬醛C9H14O20.701.570.194
    34苯乙醛C8H8O22.121.180.156
    35十四醛C14H28O28.032.494.534
    364-甲氧基苯甲醛C8H8O230.121.110.504
    37十五醛C15H30O30.122.510.031
    38(4,6,6-三甲基双环[3.1.1]庚-3-烯-2-基)乙醛C12H18O30.622.510.243
    39(Z)-13-十八碳烯醛C18H34O30.702.420.178
    40十六醛C16H32O32.122.610.444
    41胡椒醛C15H2433.951.021.017
    422-异丙基-5-甲基己基-4-烯醛C10H16O34.370.890.008
    43顺式,顺式,顺式-7,10,13-十六碳三醛C16H26O36.622.180.022
    44香兰素C8H8O339.780.770.3100.006
    45酸类丁酸C4H8O222.370.510.123
    46己酸C6H12O227.030.550.0070.115
    47辛酸C8H16O231.620.560.003
    48壬酸C9H18O233.620.590.055
    49十四烷酸C14H28O241.950.830.2970.0800.007
    50正十六酸C16H32O245.371.030.004
    51酮类2,2,4-三甲基-3-戊酮C8H14O616.030.520.007
    524-羟基-2-戊酮C5H10O217.700.770.001
    533,5-辛二烯-2-酮C8H12O19.121.450.053
    545-乙基二氢-2(3H)-呋喃酮C6H10O223.371.150.007
    554,6,6-三甲基-(1S)-双环[3.1.1] -3-庚烯-2-酮C10H14O24.371.840.148
    561-(4-甲基苯基)-乙酮C9H10O24.871.360.098
    571-(3-甲基苯基)-乙酮C9H10O24.871.360.037
    58(Z)-6,10-二甲基-5,9-十二烯-2-酮C13H22O26.622.080.033
    59(E)-6,10-二甲基-5,9-十一碳二烯-2-酮C13H22O26.702.080.3300.1760.013
    60反式-β-紫罗兰酮C13H20O28.282.140.0480.174
    61四氢-6-丙基-2H-吡喃-2-酮C8H14O228.871.350.238
    62二氢-5-戊基-2(3H)-呋喃酮C9H16O230.201.320.1680.272
    63环辛酮C8H14O31.450.700.004
    645-己基二氢-2(3H)-呋喃酮C10H18O232.281.390.018
    65四氢-6-戊基- 2H-吡喃-2-酮C10H18O233.281.450.0060.010
    66四氢-6-(2-戊烯基)-(Z)-2H-吡喃-2-酮C10H16O234.451.370.071
    675,6,7,7a-四氢-4,4,7a-三甲基-(R)-2(4H)-苯并呋喃酮C11H16O235.701.430.044
    685,6,7,7a-四氢-4,4,7a-三甲基-2(4H)-苯并呋喃酮C11H16O235.781.430.004
    69烯烃/环烷烃α-蒎烯C10H165.623.5610.418
    703,6,6-三甲基 -双环[3.1.1]-2-庚烯C10H165.623.730.030
    711-甲基-2,4-环二烯C7H105.951.720.003
    72莰烯C10H166.623.600.013
    734-甲基-3-(1-甲基亚乙基)-环己烯C10H168.123.970.009
    74烯烃/环烷烃2-蒈烯C10H168.123.970.495
    75β-蒎烯C10H168.123.980.1530.560
    763-蒈烯C10H168.623.6810.7839.5698.905
    77α-水芹烯C10H169.123.510.3661.2971.504
    78β-月桂烯C10H169.283.011.1812.1732.417
    79(+)-2-蒈烯C10H169.533.521.4806.0215.216
    801-甲基-4-(1-甲基乙基)-1,3-环己二烯C10H169.783.320.308
    81柠檬烯C10H1610.123.341.4873.3053.623
    82β-水芹烯C10H1610.373.380.5552.2352.172
    83(Z)-3,7-二甲基-1,3,6-辛二烯C10H1611.372.880.0200.014
    84γ-松油烯C10H1611.533.350.0070.3760.850
    85Β-罗勒烯C10H1611.782.830.2120.140
    86萜品油烯C10H1612.623.1512.85117.54512.975
    874,5-二甲基-2,6-辛二烯C10H1813.122.370.104
    881,3,8-对薄荷三烯C12H22O215.702.550.8891.4901.518
    891,5,8-对薄荷三烯C15H2416.452.650.5421.1501.076
    90E,E-2,6-二甲基-1,3,5,7-辛四烯C10H1416.872.390.183
    912,4-二甲基苯乙烯C10H1216.872.051.6273.7910.590
    92α-毕澄茄烯C15H2417.204.730.356
    933-乙基-1,4-己二烯C8H1417.701.290.108
    94(E,E)-2,4-庚二烯C7H10O17.701.300.0700.134
    95依兰烯C15H2417.874.770.010
    96珂巴烯C15H2418.034.801.2187.7912.587
    97(-)-α-古芸烯C15H2419.035.000.002
    98(E)2,5-二甲基-1,6-辛二烯C10H1819.532.172.5320.726
    99β-珂巴烯C15H2420.454.300.738
    100α-愈创木烯C15H2420.534.310.260
    101β-榄香烯C15H2420.533.492.065
    102石竹烯C15H2420.624.180.1800.608
    103顺式-穆罗拉-3,5-二烯C15H2421.454.231.4892.171 0.759
    1042-亚甲基-5-(1-甲基乙烯基)-8-甲基-
    双环[5.3.0]癸烷
    C15H2421.783.880.0150.131
    105(+)-香橙烯C15H2421.784.230.114
    1061R,3Z,787-9-4,11,11三甲基-8-亚甲基
    双环[7.2.0]-3-十一碳烯
    C15H2421.783.950.0980.4140.708
    107葎草烯C15H2422.283.741.362
    1081,2,3,3a,4,5,6,7-八氢-1,4-二甲基-7-(1-甲基乙烯基)-
    [1R-(1α,3,4α,7β)]-天蓝烯
    C15H2422.454.121.2990.184
    109顺式-β-金合欢烯C15H2422.453.211.543
    110马兜铃烯C15H2422.533.800.010
    111(+)-喇叭烯C15H2422.954.021.629
    1123,7-二甲基-(Z)-2,6-辛二烯C10H16O23.031.330.6730.4870.060
    113大根香叶烯C15H2423.203.670.031
    114异长叶烯C15H2423.373.892.018
    115α-布藜烯C15H2423.373.991.396
    116β-布藜烯C15H2423.373.731.883
    117γ-依兰油烯C15H2423.453.834.575
    118α-依兰烯C15H2423.623.633.3691.9541.396
    119紫苏烯C15H2423.623.682.5910.066
    120毕澄茄烯C15H2424.783.592.3580.448
    121螺环[4.4]-1-壬烯C10H16O25.622.460.1850.408
    122双环[5.2.0]-1-壬烯C9H1425.622.410.199
    123α-白菖考烯C15H2027.702.833.097
    1242-甲基-1-烯-3-壬炔C10H1627.031.230.2070.067
    125酯类乙酸乙酯C4H8O23.451.080.0960.580
    126丙酸乙酯C5H10O24.531.500.039
    127酯类丁酸乙酯C6H12O26.201.960.002
    1282-丁烯酸-(Z)-甲酯C5H8O26.531.441.884
    129环丙基羧酸乙酯C6H10O27.871.830.003
    130丁酸丙酯C7H14O28.282.440.0320.472
    1312-丁烯酸-(Z)-乙酯C6H10O29.451.740.017
    132丁酸丁酯C8H16O210.952.670.0350.008
    133己酸乙酯C8H16O211.452.510.010
    1342-丙烯酸-2-甲基-环氧乙烷基甲酯C7H10O312.531.710.048
    135乙酸己酯C8H16O212.532.230.004
    136(Z)-3-己烯-1-醇乙酯C8H14O213.621.960.014
    137(E)-3-己烯-1-醇乙酯C8H14O213.781.950.002
    138(E)-2-己烯-1-醇乙酯C8H14O214.281.911.2900.617
    139丁酸-(Z)-2-戊烯酯−C9H16O215.122.410.007
    140(Z)-丙酸-3-己烯酯C9H16O215.622.280.014
    141辛酸乙酯C10H20O216.872.680.6180.136
    142顺-3-己烯基丁酯C10H18O217.372.510.463
    143环丙烷羧酸-2-戊酯C9H16O217.452.190.0110.2140.508
    144戊二酸戊酯C7H14O317.453.030.003
    145丁酸-4-己烯-1-酯C10H18O217.532.500.002
    146丁酸-(E)- 2-己烯酯C10H18O217.952.462.306
    147(E)-2-甲基-2-丁烯-1-甲基丙烯酸甲酯C9H14O218.781.960.008
    1482-丁烯酸-2-甲基丙酯C8H14O219.952.280.107
    1491,2-丙二醇-1-乙酸酯C5H10O320.700.690.028
    1502-丁烯酸-3-(E,Z)-己烯酯C10H16O221.032.040.015
    151丁酸辛酯C12H24O221.372.911.5170.937
    1524-甲基丙烯酸戊酯C11H20O221.452.530.004
    1531,2-丙二醇-2-乙酸酯C5H10O321.700.680.002
    154丁内酯C4H6O221.780.950.005
    155癸酸乙酯C12H24O221.872.780.002
    156(E)-六角-3-烯基(E)-2-甲基-2-丁烯酸酯C11H18O222.532.320.805
    1574Z-己烯基苯甲酸酯C11H18O222.532.290.394
    1584Z-己烯酸己烯酯C11H18O222.532.280.012
    159丁酸壬酯C13H26O223.703.021.059
    160丁酸-1-乙烯己酯C12H22O224.282.780.027
    161乙酸-顺式- -3-壬烯酯C11H20O224.282.740.006
    162烟酸乙酯C8H9NO225.781.350.213
    163十二酸乙酯C14H28O226.372.880.035
    164丙位辛内酯C8H14O227.951.280.741
    165丁酸-(E)-3,7-二甲基-2,6-辛二烯基酯C14H24O227.452.630.2390.028
    166三醋酸甘油酯C9H14O631.281.010.592
    1671,2,3-丙三醇-1-乙酸酯C5H10O434.370.660.447
    168三氟-3,7-二甲基辛基乙酸酯C12H21F3O234.781.590.003
    169δ-十二内酯C12H22O237.281.580.002
    170苯甲酸苄酯C14H12O240.531.580.168
    注:“−”为未检出。
    下载: 导出CSV
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出版历程
  • 收稿日期:  2020-07-23
  • 网络出版日期:  2021-06-25
  • 刊出日期:  2021-08-01

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