基于化学计量学的枸杞多糖部分酸水解产物PMP-HPLC指纹图谱

席璟睿 张懿琳 吴梦琪 张文清 徐志珍 夏玮

席璟睿,张懿琳,吴梦琪,等. 基于化学计量学的枸杞多糖部分酸水解产物PMP-HPLC指纹图谱[J]. 食品工业科技,2021,42(18):268−275. doi:  10.13386/j.issn1002-0306.2020110002
引用本文: 席璟睿,张懿琳,吴梦琪,等. 基于化学计量学的枸杞多糖部分酸水解产物PMP-HPLC指纹图谱[J]. 食品工业科技,2021,42(18):268−275. doi:  10.13386/j.issn1002-0306.2020110002
XI Jingrui, ZHANG Yilin, WU Mengqi, et al. PMP-HPLC Fingerprint of Partial Acid Hydrolysate of Lycium barbarum Polysaccharides Based on the Chemometric Methods[J]. Science and Technology of Food Industry, 2021, 42(18): 268−275. (in Chinese with English abstract). doi:  10.13386/j.issn1002-0306.2020110002
Citation: XI Jingrui, ZHANG Yilin, WU Mengqi, et al. PMP-HPLC Fingerprint of Partial Acid Hydrolysate of Lycium barbarum Polysaccharides Based on the Chemometric Methods[J]. Science and Technology of Food Industry, 2021, 42(18): 268−275. (in Chinese with English abstract). doi:  10.13386/j.issn1002-0306.2020110002

基于化学计量学的枸杞多糖部分酸水解产物PMP-HPLC指纹图谱

doi: 10.13386/j.issn1002-0306.2020110002
详细信息
    作者简介:

    席璟睿(1995−),女,硕士研究生,研究方向:天然产物的分离分析,E-mail:m15900937319_1@163.com

    通讯作者:

    夏玮(1976−),女,博士,副教授,研究方向:天然产物的分离分析,E-mail:xiawei1999@ecust.edu.cn

  • 中图分类号: O657.7+2

PMP-HPLC Fingerprint of Partial Acid Hydrolysate of Lycium barbarum Polysaccharides Based on the Chemometric Methods

  • 摘要: 本文通过构建枸杞多糖的部分酸水解产物指纹图谱,结合多种化学计量学方法评价不同产地枸杞多糖的差异并用于市售样品的真伪鉴别。采用水提醇沉法提取16批不同产地的枸杞多糖,采用三氟乙酸部分水解,将水解产物中的单糖和寡糖采用1-苯基-3-甲基-5-吡唑啉酮(PMP)柱前衍生化HPLC分析,通过中药色谱指纹图谱软件评估不同产地样品的相似性,采用聚类分析(HCA)、主成分分析(PCA)和偏最小二乘判别分析(PLS-DA)对指纹图谱进行综合评价。结果表明,不同产地枸杞多糖部分酸水解产物中均含有7种单糖、聚合度(DP 2~4)的半乳糖醛酸聚糖和3种其他类型的二糖。16批产地的枸杞多糖相似度在0.911~0.997,HCA、PCA和PLS-DA将不同产地的枸杞多糖分为3类,分类结果与产地有一定的相关性,并且筛选出3个影响产地间差异的标志性成分,分别为葡萄糖(Glc)、阿拉伯糖(Ara)和半乳糖(Gal)。本文建立的指纹图谱可用于枸杞多糖的质量控制。
  • 图  1  枸杞多糖部分酸水解产物的PMP-HPLC色谱图

    Figure  1.  PMP-HPLC fingerprints of LBPs partial acid hydrolyzate

    图  2  枸杞多糖部分酸水解产物的PMP-HPLC对照指纹图谱

    Figure  2.  PMP-HPLC control fingerprint of LBPs partial acid hydrolysate

    图  3  混合单糖标准品的PMP-HPLC色谱图

    Figure  3.  PMP- HPLC chromatogram of the mixed standards

    图  4  LBPs部分酸水解产物在负离子模式下的总离子流图

    Figure  4.  Total ion chromatogram of LBPs in negative mod

    图  5  LBPs部分酸水解产物的PMP-UHPLC-DAD色谱图

    Figure  5.  PMP-HPLC-DAD fingerprints of LBPs partial acid hydrolyzate

    图  6  LBPs部分酸水解产物中寡糖的二级质谱图

    Figure  6.  MS / MS spectrums of LBPs partial acid hydrolysate

    注:(a)~(e)为质荷比m/z 671.2581,673.2687,687.2448,701.2947,87.76261和1053.2797离子的MS2

    图  7  5批市售枸杞多糖样品部分酸水解产物的PMP-HPLC色谱图

    Figure  7.  PMP-HPLC spectrum of 5 commercially available samples partial acid hydrolysate

    图  8  LBPs的聚类分析树状图

    Figure  8.  Cluster analysis of LBPs

    图  9  LBPs主成分分析图

    Figure  9.  PCA results of LBPs

    图  10  LBPs偏最小二乘判别分析图

    Figure  10.  PLS-DA results of LBPs

    图  11  LBPs偏最小二乘判别分析的VIP值

    Figure  11.  VIP of PLS-DA of LBPs

    表  1  原材料批次与产地

    Table  1.   16 batches of LBPs sample source

    批次产地批次产地
    S1宁夏中宁S9宁夏银川
    S2宁夏银川S10宁夏中宁
    S3甘肃景泰S11宁夏银川
    S4宁夏中宁S12宁夏银川
    S5河北巨鹿S13青海柴达木
    S6青海格尔木S14宁夏银川
    S7宁夏银川S15新疆楼兰
    S8内蒙古S16云南
    下载: 导出CSV

    表  2  枸杞多糖部分酸水解产物的PMP-HPLC色谱图的相似度评价结果

    Table  2.   Similarity of PMP-HPLC-DAD fingerprint of LBPs partial acid hydrolyzate

    样品.相似度样品相似度
    S10.981S90.996
    S20.995S100.987
    S30.996S110.991
    S40.988S120.994
    S50.978S130.911
    S60.995S140.982
    S70.997S150.994
    S80.994S160.972
    下载: 导出CSV

    表  3  枸杞多糖部分酸水解物中单糖和寡糖的鉴定

    Table  3.   Identification of monosaccharides and oligosaccharides of LBPs partial acid hydrolyzate

    峰号[M+H]+
    11053.2797DP4的半乳糖醛酸聚糖
    2877.2561DP 3的半乳糖醛酸聚糖
    3701.2947DP 2的半乳糖醛酸聚糖
    4687.2448六碳糖+GalA
    5511.2167Man
    6673.2687DP 2的六碳糖
    7495.2220Rha
    8671.2581GalA+Rha
    9525.1963GalA
    10511.2184Glc
    11511.2179Gal
    12481.2067Xyl
    13481.2073Ara
    下载: 导出CSV

    表  4  特征值和方差贡献率

    Table  4.   Characteristic value and variance contribution rate

    峰号初始特征值 提取载荷平方和
    总计方差贡献率(%)累积贡献率(%)总计方差贡献率(%)累积贡献率(%)
    14.40733.89733.8974.40733.89733.897
    23.00423.11057.0073.00423.11057.007
    32.89322.25779.2642.89322.25779.264
    40.9997.68886.952
    50.6865.27792.229
    60.4033.10295.331
    70.2561.97397.304
    80.2091.60698.910
    90.0960.73999.650
    100.0330.25799.907
    110.0110.08299.989
    120.0010.011100.000
    131.930E-50.000100.000
    下载: 导出CSV
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出版历程
  • 收稿日期:  2020-11-03
  • 网络出版日期:  2021-08-09
  • 刊出日期:  2021-09-14

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