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通络生骨胶囊原粉化学成分鉴定及牡荆苷含量测定

Identification of chemical components and determination of vitexin in the raw powder of Tongluo Shenggu capsule

  • 摘要: 采用UPLC-MS/MS对通络生骨胶囊原粉中的化合物进行分析鉴定,并建立牡荆苷HPLC含量测定方法。通过采用Acquity UPLC® BEH C18(2.1 mm×100 mm,1.7 μm)色谱柱,以0.2%甲酸-甲醇为流动相进行梯度洗脱,柱温30 ℃,流速0.3 mL/min,进样量1 μL;通过ESI质谱源,在正、负离子模式下分别采集数据,成功鉴定出通络生骨胶囊原粉中的12个黄酮类和3个芪类化合物。同时,采用XBridge C18(4.6 mm×250 mm,5 µm)色谱柱,以0.05%冰醋酸-甲醇为流动相进行梯度洗脱,柱温30 ℃,流速1.0 mL/min,进样量20 µL,建立了牡荆苷的HPLC含量测定方法。该方法在10~40 µg/mL范围内线性关系良好(R=1.000),平均回收率为96.7%。这些方法的建立为通络生骨胶囊原粉的质量控制和开发利用提供了科学依据。

     

    Abstract: The present study employed UPLC-MS/MS to analyze and identify compounds in the raw powder of Tongluo Shenggu capsules. An HPLC method for the determination of vitexin content was established. The analysis of this drug was performed on a 30 ℃ thermostatic Acquity UPLC® BEH C18 (2.1 mm×100 mm,1.7 μm) column, with the mobile phase comprising 0.2% formic acid-methanol flowing at 0.3 mL /min in a gradient elution manner. Mass spectrometry was detected by ESI sources in both positive and negative ion modes for qualitative identification of chemical constituents. 12 flavonoid and 3 stilbenes compounds in the raw powder of Tongluo Shenggu capsules were successfully identified. Additionally, an HPLC method for the determination of vitexin content was established using a XBridge C18 column (4.6 mm × 250 mm, 5 µm) with a mobile phase of 0.05% glacial acetic acid in methanol for gradient elution, at a column temperature of 30 °C, a flow rate of 1.0 mL/min, and an injection volume of 20 μL. The method demonstrated good linearity in the concentration range of 10 µg/mL to 40 µg/mL (R=1.000) with an average recovery rate of 96.7%. The establishment of these methods provides a scientific basis for the quality control and development of the raw powder of Tongluo Shenggu capsules.

     

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