微波无溶剂萃取法提取野菊花精油工艺及成分分析

滕云 杨丽

滕云,杨丽. 微波无溶剂萃取法提取野菊花精油工艺及成分分析[J]. 食品工业科技,2021,42(18):226−234. doi:  10.13386/j.issn1002-0306.2021020185
引用本文: 滕云,杨丽. 微波无溶剂萃取法提取野菊花精油工艺及成分分析[J]. 食品工业科技,2021,42(18):226−234. doi:  10.13386/j.issn1002-0306.2021020185
TENG Yun, YANG Li. Extracting Process of Essential Oil from Chrysanthemum indicum by Solvent-free Microwave Extraction and Its Components Analysis[J]. Science and Technology of Food Industry, 2021, 42(18): 226−234. (in Chinese with English abstract). doi:  10.13386/j.issn1002-0306.2021020185
Citation: TENG Yun, YANG Li. Extracting Process of Essential Oil from Chrysanthemum indicum by Solvent-free Microwave Extraction and Its Components Analysis[J]. Science and Technology of Food Industry, 2021, 42(18): 226−234. (in Chinese with English abstract). doi:  10.13386/j.issn1002-0306.2021020185

微波无溶剂萃取法提取野菊花精油工艺及成分分析

doi: 10.13386/j.issn1002-0306.2021020185
基金项目: 国家自然科学基金青年科学基金项目(32002083);河南省科技攻关项目(172102110248)
详细信息
    作者简介:

    滕云(1974−),女,硕士,讲师,研究方向:植物资源开发与应用,E-mail:tengyun1224@163.com

    通讯作者:

    杨丽(1981−),女,硕士,讲师,研究方向:观赏植物应用,E-mail:sunnylily000@126.com

  • 中图分类号: TS255.1+9

Extracting Process of Essential Oil from Chrysanthemum indicum by Solvent-free Microwave Extraction and Its Components Analysis

  • 摘要: 采用微波无溶剂萃取法(Solvent-free microwave extraction, SFME)分别提取野菊花鲜花精油和干花精油,对提取工艺进行了优化;并通过气相色谱-质谱联用技术(chromatograpy-mass spectrometry, GC-MS)分析两种精油化学成分,用峰面积归一法计算各组分相对含量。结果表明:野菊花鲜花精油的最佳提取条件为提取时间50 min,微波功率540 W,精油得率为鲜花重的0.1129%;干花精油的最佳提取条件为料液比1:5 g/mL,浸泡时间3 h,提取时间60 min,微波功率540 W,精油得率为干花重的0.1926%;经GC-MS分析,SFME提取野菊花鲜花精油的主要化学成分是单萜及单萜类含氧化合物,相对含量较多的化合物是乙酸桧酯(13.20%)、甲位侧柏酮(11.10%)、桧醇(9.70%)、菊醇(5.06%)、甲位水芹烯(3.87%)、荜澄茄油烯(3.78%)、桉叶油素(3.61%)、崖柏醇(3.37%)、2-侧柏烯(3.36%)。干花精油的主要化学成分是单萜含氧化合物及倍半萜,相对含量较多的化合物是菊醇(8.59%)、反式石竹烯(7.63%)、大根香叶烯(7.06%)、Α-合金欢烯(5.86%)、甲位侧柏酮(4.85%)、乙酸桧酯(4.34%)、乙酸菊醇酯(3.45%)、右旋樟脑(3.35%)。野菊花鲜花精油的含量比干花更高,单萜含氧化合物相对含量高于干花精油,更具有应用价值。
  • 图  1  微波无溶剂萃取装置

    Figure  1.  Solvent-free microwave extraction device

    图  2  提取时间对鲜花精油得率的影响

    Figure  2.  Effect of extraction time on the yield of essential oil from fresh flowers

    图  3  微波功率对鲜花精油得率的影响

    Figure  3.  Effect of microwave power on yield of essential oil from fresh flowers

    图  4  料液比对干花精油得率的影响

    Figure  4.  Effect of material-liquid ratio on yield of essential oil from dried flowers

    图  5  浸泡时间对干花精油得率的影响

    Figure  5.  Effect of soaking time on yield of essential oil from dried flowers

    图  6  提取时间对干花精油得率的影响

    Figure  6.  Effect of extraction time on yield of essential oil from dried flowers

    图  7  微波功率对干花精油得率的影响

    Figure  7.  Effect of microwave power on the yield of essential oil from dried flowers

    表  1  鲜花精油提取因素水平设计

    Table  1.   Factors and levels of essential oil extraction from fresh flowers

    水平因素
    A提取时间(min)B微波功率(W)
    140450
    250540
    360630
    下载: 导出CSV

    表  2  干花精油提取正交试验因素水平设计

    Table  2.   Factors and levels of orthogonal test for extraction of essential oil from dried flowers

    水平因素
    A料液比(g/mL)B浸泡时间(h)C提取时间(min)D微波功率(W)
    11:4240450
    21:5350540
    31:6460630
    下载: 导出CSV

    表  3  鲜花精油提取试验结果

    Table  3.   Test results of essential oil extraction from fresh flowers

    试验号因素精油得率(%)
    AB
    11(40)1(450)0.0723
    21(40)2(540)0.0926
    31(40)3(630)0.0951
    42(50)1(450)0.0819
    52(50)2(540)0.1129
    62(50)3(630)0.1125
    73(60)1(450)0.0889
    83(60)2(540)0.1126
    93(60)3(630)0.1049
    k10.08670.0810
    k20.10240.1060
    k30.10210.1042
    R0.01570.0250
    下载: 导出CSV

    表  4  方差分析表

    Table  4.   Variance analysis table

    方差来源III型平方和df均方FP
    校正模型0.00240.00041322.3410.005
    截距0.08510.0854589.3810.000
    A0.00048820.00024431.4820.017*
    B0.00116420.00058213.2000.004**
    误差0.00007440.000018
    总计0.0879
    校正的总计0.0028
    注:**P<0.01,表示差异极显著;*P<0.05,表示差异显著。表6同。
    下载: 导出CSV

    表  5  干花精油正交试验结果

    Table  5.   Results of orthogonal test for essential oil of dried flower

    试验号因素精油得率(%)
    ABCD
    11(1:4)1(2)1(40)1(450)0.0751
    21(1:4)2(3)2(50)2(540)0.1543
    31(1:4)3(4)3(60)3(630)0.1509
    42(1:5)1(2)2(50)3(630)0.1913
    52(1:5)2(3)3(60)1(450)0.1678
    62(1:5)3(4)1(40)2(540)0.1499
    73(1:6)1(2)3(60)2(540)0.1910
    83(1:6)2(3)1(40)3(630)0.1493
    93(1:6)3(4)2(50)1(450)0.1600
    k10.12680.15250.12480.1343
    k20.16970.15710.16850.1651
    k30.16680.15360.16990.1638
    R0.04290.00460.04510.0308
    下载: 导出CSV

    表  6  方差分析结果

    Table  6.   Variance analysis table

    方差来源III型平方和df均方FP
    校正模型0.009a60.00286.4920.011
    截距0.21510.21512071.690.000083
    A0.00320.00297.0220.010*
    C0.00420.002111.2450.009**
    D0.00220.00151.2090.019*
    误差0.00003620.000018
    总计0.2249
    校正的总计0.0098
    下载: 导出CSV

    表  7  野菊花精油的主要化学组分

    Table  7.   The main chemical constituents of essential oil from chrysanthemum indicum

    编号
    (No.)
    保留指数(RI)化合物名称
    (compound name)
    化学式相对含量(relative content)(%)
    鲜花干花
    I单萜
    19323-桧烯C10H161.18
    2945α-蒎烯C10H162.771.49
    39504-亚甲基-1-(1-甲基乙基)双环[3.1.0]2-己烯C10H140.70
    4953莰烯C10H160.951.06
    59692-侧柏烯C10H163.36
    6985乙位蒎烯C10H161.600.86
    7998月桂烯C10H160.87
    81008甲位水芹烯C10H163.870.55
    91027乙位水芹烯C10H160.74
    101031对伞花烃C10H142.271.25
    111038柠檬烯C10H160.75
    121060γ-松油烯C10H160.830.62
    II单萜含氧化合物
    131048桉叶油素C10H18O3.611.24
    141104FilifoloneC10H14O0.63
    151108(9ci)-2,6,6-三甲基-1,4-环己二烯-1-羧醛C10H14O0.51
    161110甲位侧柏酮C10H16O11.104.85
    171115乙位侧柏酮C10H16O2.090.99
    181124蒎烯酮C10H14O1.952.02
    191131桧醇C10H16O9.70
    211133反式-1-甲基-4-(1-甲基乙烯基)环己-2-烯-1-醇C10H16O0.93
    2011393-ThujanolC10H18O0.52
    221148右旋樟脑C10H16O0.813.35
    231155冰片C10H18O0.781.49
    241165菊醇C10H18O5.068.60
    251158崖柏醇C10H18O3.37
    261170龙脑C10H18O2.72
    2711804-松油烯醇C10H18O1.050.60
    281191甲位松油醇C10H18O0.600.67
    291220香芹醇C10H16O1.70
    301326桃金娘烯醇C10H16O0.51
    III倍半萜
    311380alpha-copaeneC15H240.63
    321395B-榄香烯C15H242.112.83
    331397荜澄茄油烯C15H243.78
    341430反式石竹烯C15H242.177.63
    351438(E)-β-金合欢烯C15H240.722.45
    361440香柑油烯C15H241.130.67
    371450α-律草烯C15H240.51
    381493大根香叶烯C15H247.06
    391501(+)-bicyclogermacreneC15H240.80
    401509α-金合欢烯C15H246.39
    411524Β-倍半水芹烯C15H240.71
    IV倍半萜含氧化合物
    421526桉油烯醇C15H24O0.56
    431575(+)-maaliolC15H26O0.84
    441580氧化石竹烯C15H24O3.52
    451646T-杜松醇C15H26O0.64
    461670(1S,8aα)-十氢-1,4aβ-二甲基-7β-异丙烯基-1-萘酚C15H26O1.79
    471779(-)-a-CostolC15H24O0.72
    V酯类
    481240乙酸菊醇酯C10H16O.C2H4O21.463.45
    491249乙酸芳樟酯C12H20O20.67
    501280L-乙酸冰片酯C12H20O22.08
    511302乙酸桧酯C12H18O213.204.34
    VI其他
    52正二十三烷C23H480.64
    小计
    单萜含量19.156.57
    单萜含氧化合物含量41.5629.89
    倍半萜含量9.9129.68
    倍半萜含氧化合物含量08.07
    酯类含量15.339.87
    其他含量00.64
    合计85.9584.72
    注:− 表示不含该化合物,↓表示含该化合物,但相对含量低于 0.5%。
    下载: 导出CSV
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出版历程
  • 收稿日期:  2021-02-24
  • 网络出版日期:  2021-08-05
  • 刊出日期:  2021-09-14

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