大孔树脂纯化小鱼仙草总黄酮的工艺研究及成分分析

    Macroporous Resin Purifies Total Flavonoids of Mosla Dianthera with Process Research and Component Analysis

    • 摘要:
      目的 采用大孔树脂富集纯化法联合超高效液相色谱-四级杆-飞行时间串联质谱法(UPLC-Q-TOF-MS)对小鱼仙草的黄酮类化学成分进行提取、纯化和分析鉴定。
      方法 以总黄酮提取率为评价指标,考察9种大孔树脂最大上样量、吸附时间、吸附温度、乙醇浓度和流速的最佳水平,筛选出大孔树脂的最佳型号,得到最佳工艺条件。采用UPLC-Q-TOF-MS法鉴定分析最佳工艺条件下所得总黄酮中的化学成分。
      结果 大孔树脂富集纯化小鱼仙草总黄酮最佳工艺条件:HPD-300大孔树脂,最大上样量72 mg·g−1,吸附时间100 min,吸附温度25 ℃,60%乙醇解吸,流速4 BV·h−1,总黄酮纯度为89.2%。经UPLC-Q-TOF-MS法鉴定分析可知,小鱼仙草总黄酮类物质主要包括木犀草素等11种化学成分。
      结论 本研究可为小鱼仙草质量控制、药效物质基础研究及资源开发利用提供科学依据。

       

      Abstract:
      OBJECTIVE The macroporous resin enrichment and purification method combined with ultra-high performance liquid chromatography-quadrupole-time of flight mass spectrometry (UPLC-Q-TOF-MS) was used to extract, purify and analyze the flavonoids of Mosla dianthera.
      METHODS  Based on the extraction rate of total flavonoids, the maximum loading amount, adsorption time, adsorption temperature, ethanol concentration and flow rate of 9 kinds of macroporous resins were investigated, and the best macroporous resins for enrichment and purification of total flavonoids were selected. Then the best technological conditions were obtained. Next, the chemical constituents of the total flavonoids obtained under optimal process conditions were identified by UPLC-Q-TOF-MS method.
      RESULTS The optimal process conditions for macroporous resin enrichment and purification of total flavonoids of Mosla dianthera were as follows: HPD-300 macroporous resin was selected, the maximum loading amount was 72 mg·g−1, the adsorption time was 100 min, the adsorption temperature was 25 ℃, 60% ethanol was used, and the flow rate was 4 BV·h−1. The purity of total flavonoids obtained after enrichment and purification was 89.2%. From the identification and analysis of UPLC-Q-TOF-MS method, the total flavonoids of Mosla dianthera. mainly included 11 chemical components such as luteolin.
      CONCLUSION This study can provide a scientific basis for the quality control, basic research on pharmacodynamic substances and resources development and utilization of Mosla dianthera.

       

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