高效液相色谱串联傅里叶变换离子回旋共振质谱法鉴定二丁颗粒的化学成分

Characterization of Chemical Constituents of Erding Granules by Using HPLC-FT-ICR-MS

    摘要
  • 摘要:
      目的  采用高效液相色谱串联傅里叶变换离子回旋共振质谱(HPLC-FT-ICR-MS)法鉴定二丁颗粒(紫花地丁、半边莲、蒲公英、板蓝根)的化学成分。
      方法  采用Kinetex C18色谱柱(150 mm×4.6 mm, 2.6 μm), 流动相A: 乙腈, 流动相B: 0.1%甲酸水溶液, 梯度洗脱, 流速: 1.0 mL · min-1, 柱温: 30 ℃, 进样量: 10 μL。电喷雾电离源正、负离子模式检测, 根据高分辨质谱信息结合对照品数据及相关文献对二丁颗粒化学成分进行快速鉴定。
      结果  在二丁颗粒中共检测到106个化合物, 准确鉴定出22个化合物, 推测了84个化合物的结构, 其主要化学成分为黄酮及其苷类、生物碱、有机酸、香豆素及其衍生物、倍半萜类、木质素类等。
      结论  实验初步阐释了二丁颗粒的化学成分组成, 为其质量控制和药效物质基础研究提供了依据。

     

    Abstract:
      OBJECTIVE  To characterize the chemical constituents of Erding Granules by high performance liquid chromatography tandem Fourier transform ion cyclotron resonance mass spectrometry (HPLC-FT-ICR-MS) method.
      METHODS  The Kinetex-C18 column (150 mm×4.6 mm, 2.6 μm) was used, the optimum column temperature was 30 ℃, the mobile phase composed of acetonitrile and 0.1% formic acid solution for gradient elution at the flow rate of 1.0 mL·min-1. Electrospray ionization source (ESI) with negative and positive ion modes were applied for HPLC-FT-ICR-MS analysis. The chemical components were identified by combining the high resolution data, the MS/MS information and previous literatures.
      RESULTS  A total of 106 compounds were detected and characterized in Erding Granules. Among them, 22 compounds were accurately identified by comparing with standards and 84 compounds were tentatively predicted.
      CONCLUSION  The chemical compositions of Erding Granules are preliminarily characterized, which provides the basis for further research of pharmacodynamic substance.

     

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