经典名方羌活胜湿汤基准样品的特征图谱分析

    Analysis of Specific Chromatogram of Classical Formula Qianghuo Shengshi Tang Reference Samples

    • 摘要:
      目的  建立羌活胜湿汤基准样品特征图谱,阐明羌活胜湿汤关键质量属性,为经典名方羌活胜湿汤基准样品的质量评价提供参考。
      方法 采用SilGreen C18色谱柱(4.6 mm×250 mm,5 μm),流动相为乙腈-0.2%甲酸水溶液,检测波长328 nm,建立羌活胜湿汤基准样品的HPLC特征图谱分析方法。采用多种色谱柱及仪器进行系统适应性考察。采用HPLC-LTQ-Orbitrap MS技术,在正离子模式下对羌活胜湿汤基准样品的特征峰进行鉴别。
      结果 特征图谱共标定14个特征峰,分别归属羌活、独活、藁本、川芎、蔓荆子,以阿魏酸(3号峰)为基准峰。通过质谱分析,共鉴定了22个化合物,包括香豆素及黄酮类成分。
      结论 所建立的羌活胜湿汤特征图谱简便稳定、重复性好,通过质谱指认及来源归属,基本明确了羌活胜湿汤基准样品的物质基础,为羌活胜湿汤的开发和质量控制提供参考依据。

       

      Abstract:
      OBJECTIVE  To establish the specific chromatogram of Qianghuo Shengshi Tang(QHSS) reference sample, clarify the key quality attributes of QHSS, providing reference for the quality evaluation of QHSS reference sample.
      METHODS  The SilGreen C18 column(4.6 mm×250 mm, 5 μm) was used. The mobile phase consisted acetonitrile and 0.2% formic acid aqueous solution. The detection wavelength was 328 nm. Established an HPLC characteristic spectrum analysis method for the reference sample of QHSS. A variety of chromatographic columns and different instruments were applied to investigate the adaptability of the system. HPLC-LTQ-Orbitrap MS was used to identify the specific peaks of the QHSS reference samples in positive ion mode.
      RESULTS  There were 14 peaks in the specific chromatogram, which belonged to Notopterygii Rhizoma Et Radix, Angelicae Pubescentis Radix, Ligustici Rhizoma Et Radix, Chuanxiong Rhizome, Viticis Fructus, respectively. Ferulic acid(peak 3) was reference peak. A total of 22 compounds were identified by mass spectrometry, including coumarin and flavonoids.
      CONCLUSION  The established specific chromatogram method of QHSS is simple, stable and reproducible. The material basis of QHSS reference sample is basically determined, providing a reference for the development and quality control of QHSS.

       

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