郭倩池, 王康宇, 张龄月, 郭云龙, 贡济宇, 高文义. 基于UHPLC-Q-Orbitrap/MS鉴定当归四逆颗粒化学成分[J]. 质谱学报, 2024, 45(3): 432-446. DOI: 10.7538/zpxb.2023.0114
引用本文: 郭倩池, 王康宇, 张龄月, 郭云龙, 贡济宇, 高文义. 基于UHPLC-Q-Orbitrap/MS鉴定当归四逆颗粒化学成分[J]. 质谱学报, 2024, 45(3): 432-446. DOI: 10.7538/zpxb.2023.0114
GUO Qian-chi, WANG Kang-yu, ZHANG Ling-yue, GUO Yun-long, GONG Ji-yu, GAO Wen-yi. Identification of Chemical Components of Danggui Sini Granules by UHPLC-Q-Orbitrap/MS[J]. Journal of Chinese Mass Spectrometry Society, 2024, 45(3): 432-446. DOI: 10.7538/zpxb.2023.0114
Citation: GUO Qian-chi, WANG Kang-yu, ZHANG Ling-yue, GUO Yun-long, GONG Ji-yu, GAO Wen-yi. Identification of Chemical Components of Danggui Sini Granules by UHPLC-Q-Orbitrap/MS[J]. Journal of Chinese Mass Spectrometry Society, 2024, 45(3): 432-446. DOI: 10.7538/zpxb.2023.0114

基于UHPLC-Q-Orbitrap/MS鉴定当归四逆颗粒化学成分

Identification of Chemical Components of Danggui Sini Granules by UHPLC-Q-Orbitrap/MS

  • 摘要: 本研究运用超高效液相色谱-四极杆-静电场轨道阱质谱(UHPLC-Q-Orbitrap/MS)技术快速鉴定当归四逆颗粒的化学成分。采用SUPELCO C18色谱柱(100 mm×4.6 mm×2.7 μm),以0.1%甲酸水溶液-乙腈为流动相进行梯度洗脱,正、负离子模式下采集数据。根据精确质荷比和二级质谱碎片离子信息,结合相关文献快速鉴定当归四逆颗粒的成分,并对化合物的药味来源进行归属。结果表明,在正、负离子模式下,分别从当归四逆颗粒鉴定出34、38种化合物,其中包括20种黄酮类、15种有机酸类、11种皂苷类、9种萜类、5种苯酞类、1种苯丙素类、1种醛类、1种核苷类、1种木脂素类及8种其他类化合物。本研究可为阐释当归四逆颗粒的药效物质基础提供依据。

     

    Abstract: Due to the complexity and diversity of the chemical composition of traditional Chinese medicines (TCMs), the identification of components of TCMs can effectively guarantee the quality of TCMs and be of great significance for the development and utilization of TCMs. In this study, the ultra-high performance liquid chromatography-quadrupole-electrostatic field Orbitrap mass spectrometry (UHPLC-Q-Orbitrap/MS) was used to comprehensively analyze the chemical composition of Danggui Sini Granules. The UHPLC separation was performed on a SUPELCO C18 column (100 mm×4.6 mm×2.7 μm), and the column temperature was 30 ℃, the injection volume was 5 μL. The mobile phase was consisted of 0.1% formic acid aqueous solution (A) and acetonitrile (B) with the flow rate of 0.5 mL/min. MS data was collected under positive and negative ion modes. A self-constructed database of organic acids, flavonoids, phthalides, triterpenoids, saponins and other compounds was established by searching online databases. Rapid identification of the constituents of Danggui Sini Granules based on precise m/z and secondary fragment ion information in combination with literature data was achieved, and the herbal sources of the compounds were attributed. Seventy-two compounds are identified from Danggui Sini Granules, including 20 flavonoids, 15 organic acids, 11 saponins, 9 terpenoids, 5 phthalides, 1 phenylpropanoid, 1 aldehyde, 1 nucleoside, 1 lignan and 8 other compounds. Among them, the organic acids and phthalides are mainly from Angelicae Sinensis Radix, the flavonoids are mainly from Glycyrrhizae Radix et Rhizoma, the saponins are mainly from Akebiae Caulis, the terpenoids are mainly from Paeoniae Radix Rubra, the nucleosides are mainly from Jujubae Fructus, and other compounds are mainly from Asari Radix et Rhizoma and Cinnamomi Cortex. The results showed that the chemical composition of this compound preparation is rich and structurally diverse, which not only provides data support for comprehensive understanding of its chemical composition, but also a preliminary research basis for clarifying the material basis of its pharmacological action. However, there are still some unknown species whose specific structures have not been clarified. The structural identification and differentiation of these compounds are somewhat limited in the absence of sufficient controls, and can be followed up with deeper separation and identification by techniques such as nuclear magnetic resonance mass spectrometry (NMR-MS).

     

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