响应面法优化野菊花蒙花苷的提取工艺及大悟县不同区域野菊花中蒙花苷含量的测定

喻书诚 王思龙 张林 王有宁 李长春 汤亚芳 斯琴朝克图 刘牛 郑操 姚国新

喻书诚,王思龙,张林,等. 响应面法优化野菊花蒙花苷的提取工艺及大悟县不同区域野菊花中蒙花苷含量的测定[J]. 食品工业科技,2021,42(18):235−243. doi:  10.13386/j.issn1002-0306.2021040265
引用本文: 喻书诚,王思龙,张林,等. 响应面法优化野菊花蒙花苷的提取工艺及大悟县不同区域野菊花中蒙花苷含量的测定[J]. 食品工业科技,2021,42(18):235−243. doi:  10.13386/j.issn1002-0306.2021040265
YU Shucheng, WANG Silong, ZHANG Lin, et al. Optimization of Extraction Process of Buddleoside in Chrysanthemum indicum L. by Response Surface Methodology and Determination of Buddleoside Content in C. indicum L. from Different Regions in Dawu County[J]. Science and Technology of Food Industry, 2021, 42(18): 235−243. (in Chinese with English abstract). doi:  10.13386/j.issn1002-0306.2021040265
Citation: YU Shucheng, WANG Silong, ZHANG Lin, et al. Optimization of Extraction Process of Buddleoside in Chrysanthemum indicum L. by Response Surface Methodology and Determination of Buddleoside Content in C. indicum L. from Different Regions in Dawu County[J]. Science and Technology of Food Industry, 2021, 42(18): 235−243. (in Chinese with English abstract). doi:  10.13386/j.issn1002-0306.2021040265

响应面法优化野菊花蒙花苷的提取工艺及大悟县不同区域野菊花中蒙花苷含量的测定

doi: 10.13386/j.issn1002-0306.2021040265
基金项目: 国家自然科学基金(31900062,31700069,41401348);湖北省教育厅科学研究计划资助项目(Q20192702)
详细信息
    作者简介:

    喻书诚(1999−),男,本科,研究方向:植物资源开发利用,E-mail:yucamellia@163.com

    通讯作者:

    郑操(1988−),男,博士,讲师,研究方向:植物资源开发利用,E-mail:zhengc1314@163.com

    姚国新(1977−),男,博士,教授,研究方向:特色农业资源利用,E-mail:guoxiny2010@foxmail.com

  • 中图分类号: R284.2

Optimization of Extraction Process of Buddleoside in Chrysanthemum indicum L. by Response Surface Methodology and Determination of Buddleoside Content in C. indicum L. from Different Regions in Dawu County

  • 摘要: 为了探究湖北省大悟县不同地区分布的野菊花中蒙花苷的含量,本研究在单因素实验的基础上,采用Box-Behnken法设计了4因素3水平的响应面试验,对影响蒙花苷得率的主要因素进行了优化,并以最优工艺测定了湖北省孝感市大悟县不同区域野菊花样品中的蒙花苷含量。工艺优化结果表明,溶质质量分数、液料比、提取温度、提取时间是影响蒙花苷得率的四个主要因素。其中,提取温度对蒙花苷得率的影响最大,随后依次是提取时间、液料比和溶质质量分数。蒙花苷最优提取工艺为:乙醇质量分数54%、液料比150:1 (mL/g)、提取温度80 ℃、提取时间60 min,蒙花苷对应得率为2.75%±0.03%,与模型预测值2.80%无显著性差异。且该工艺条件还展现出稳定性好(RSD<5%)、精密度高(RSD<5%)、加标回收率优良(>80%)等特点,适用于实际野菊花样本中蒙花苷含量的测定。含量结果表明,大悟县不同地区野菊花样品中蒙花苷含量差异较大,介于0~2.75%之间,其中第027、037、060、094号取样地蒙花苷含量较高,均超过2.5%。本研究可为野菊花食材或药材的质量评价提供可靠方法,也可为高蒙花苷含量野菊花优良品种的种植和选育提供重要依据。
  • 图  1  孝感市大悟县野菊花样品采样分布图

    Figure  1.  Sampling and distribution map of C. indicum L. in Dawu County, Xiaogan City

    图  2  溶剂种类对蒙花苷得率的影响

    Figure  2.  Effect of solvent type on the yield of buddleoside

    图  3  溶质质量分数对蒙花苷得率的影响

    Figure  3.  Effect of solute mass fraction on the yield of buddleoside

    图  4  提取时间对蒙花苷得率的影响

    Figure  4.  Effect of extraction time on the yield of buddleoside

    图  5  液料比对蒙花苷得率的影响

    Figure  5.  Effect of liquid-solid ratio on the yield of buddleoside

    图  6  提取温度对蒙花苷得率的影响

    Figure  6.  Effect of extraction temperature on the yield of buddleoside

    图  7  各因素之间交互作用对蒙花苷得率的影响

    Figure  7.  Response surface graphs showing the effect of extraction conditions on the yield of buddleoside

    图  8  蒙花苷的高效液相色谱图

    Figure  8.  Liquid chromatograms of buddleoside

    注:A为蒙花苷标准品;B为33号野菊花样品回流提取液。

    表  1  响应面试验因素水平设计

    Table  1.   Factors and levels of response surface experiment

    因素水平
    −101
    A溶质质量分数(%)405060
    B提取时间(min)304560
    C液料比(mL/g)150:1200:1250:1
    D提取温度(℃)607080
    下载: 导出CSV

    表  2  响应面实验设计和结果

    Table  2.   Experimental design and results of the response surface experiment

    实验号ABCDY蒙花苷得率(%)
    101101.75
    20−1101.94
    3−10−101.81
    410−101.86
    501012.38
    6001−11.69
    700−112.35
    80−1011.91
    9010−11.70
    100−1−101.79
    11−10011.76
    1200002.01
    13100−11.20
    1411001.79
    1500001.96
    16−10101.80
    1701−102.50
    1800002.10
    19−1−1001.69
    2010−101.61
    21−100−11.74
    221−1001.60
    23−11001.84
    2410012.00
    2500001.99
    2600002.00
    270−10−11.68
    2800−1−11.82
    2900112.06
    下载: 导出CSV

    表  3  响应面回归方程方差分析

    Table  3.   Variance analysis of response surface regression equation

    方差来源平方和自由度均方FP显著性
    模型1.80140.1348.06<0.0001**
    A0.02810.02810.350.0062**
    B0.1510.1555.72<0.0001**
    C0.1410.1450.44<0.0001**
    D0.5710.57213.00<0.0001**
    AB0.000306210.0030630.110.7404
    AC0.01410.0145.280.0375*
    AD0.1510.1557.31<0.0001**
    BC0.210.275.01<0.0001**
    BD0.0510.0518.630.0007**
    CD0.00664210.0066422.480.1378
    A20.4510.45169.09<0.0001**
    B20.00589310.0058932.200.1604
    C20.00342610.0034261.280.2773
    D20.02710.0279.910.0071**
    残差0.038140.002682
    失拟项0.026100.0026140.920.5875
    误差0.01140.002849
    总变异1.8428
    决定系数0.9796调整决定系数0.9592
    注:**表示差异达到极显著水平(P<0.01),*表示差异达到显著水平(P<0.05)。
    下载: 导出CSV

    表  4  蒙花苷的加标回收结果

    Table  4.   Results of standard recoveries of buddleoside

    水平加标量(mg)回收量(mg)回收率(%)
    143.4887
    221.7186
    310.8181
    下载: 导出CSV

    表  5  大悟县不同区域野菊花样品中的蒙花苷含量结果

    Table  5.   Content of buddleoside in C. indicum L. from different regions of Dawu County

    编号含量(%)编号含量(%)编号含量(%)编号含量(%)
    0011.940320.550631.730942.51
    0021.860331.860640.020951.09
    0031.770340.670650.000960.00
    0041.870351.230661.430970.62
    0050.010362.120672.030981.85
    0060.000372.540682.090990.02
    0071.460382.320692.181001.45
    0080.370391.370701.751011.90
    0090.000402.190710.001020.37
    0100.940412.060720.001031.39
    0110.190422.060732.001041.49
    0120.020430.000741.751051.44
    0130.630440.050751.201060.01
    0140.010450.110761.451070.91
    0152.090460.000771.471080.00
    0161.780471.960781.341090.00
    0171.840480.020791.531101.43
    0180.960492.210800.071112.32
    0190.250501.230810.331121.66
    0201.790511.370821.721131.70
    0211.830520.400830.001140.00
    0220.000530.010841.641150.00
    0231.530541.730850.011160.02
    0240.000550.950861.221170.69
    0250.000560.610871.911180.16
    0260.710570.000880.001191.36
    0272.750580.020890.161200.12
    0281.600590.010900.001211.93
    0290.000602.520910.01
    0300.630612.010920.00
    0311.090621.870931.64
    下载: 导出CSV
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    《食品工业科技》编辑部携手万方数据开通学术不端专属检测通道,具体信息参见本刊动态。