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大黄碳酸氢钠片中大黄及薄荷油的质量控制研究

曾玉梅   

  1. 梅州市食品药品监督检验所
  • 收稿日期:2018-12-19 修回日期:2019-02-20 出版日期:2019-02-25 发布日期:2019-02-25
  • 基金资助:
    2018年梅州市社会发展科技计划项目(项目编号:2018B078)

Quality Control of Rhubarb and Peppermint Oil in Rhubarb Bicarbonate Tablets

zengyumei   

  1. Mei Zhou Institute for food and Drug Control
  • Received:2018-12-19 Revised:2019-02-20 Online:2019-02-25 Published:2019-02-25

摘要: ]目的:应用现代色谱方法对大黄碳酸氢钠片中大黄及薄荷油的质量控制进行研究,为补充完善现有质量控制标准提供参考。方法:采用高效液相色谱(HPLC)法,以Agilent XDB C18(4.6 mm×250 mm,5 μm)为色谱柱,甲醇-0.1%磷酸水(85∶15)为流动相,在254 nm的波长下测定大黄中4种游离型蒽醌(大黄酸、大黄素、大黄酚和大黄素甲醚)的含量。采用薄层色谱法,对薄荷油进行定性鉴别。结果:应用HPLC含量测定方法操作简单,精密度、稳定性、重复性实验结果良好,大黄酸、大黄素、大黄酚和大黄素甲醚值线性关系良好(r>0.999 5),平均加样回收率好,测得3个不同厂家大黄碳酸氢钠片中大黄的含量有显著性差异;薄层色谱的定性鉴别方法操作简便,结果准确。结论:大黄碳酸氢钠片的现行质量控制标准应进行修订,建议增补关于大黄的定量考察项目,且应更新优化其项下薄荷油的定性鉴别方法,以增加鉴别实验结果的可靠性。

Abstract: Use modern chromatographic methods to study the quality control of rhubarb and peppermint oil in rhubarb sodium bicarbonate tablets, provide reference for supplementing and improve the existing quality control standards. Methods:Used Agilent XDB C18(250 mm × 4.6 mm, 5 μm) column and the mobile phase was methanol-0.1% phosphoric acid water (85∶15). The content of four kinds rhubarb(Rhein, emodin, chrysophanol and emodin methyl ether) were determined at 254 nm by HPLC. Peppermint oil was qualitatively identified by TLC. Results: The method for determination by HPLC was simple, and the precision, stability and repeatability were good. The linear relationship between rhein, emodin, chrysophanol and emodin methyl ether were good (r>0.999 5). The recovery rates also good, and the content of rhubarb in the rhubarb sodium bicarbonate tablets in three different manufacturers was significantly different. The qualitative identification method by TLC was simple and accurate. Conclusion: The current quality control standards should be revised. It is recommended to add quantitative research items on rhubarb, and the qualitative identification method for peppermint oil should be updated and optimized to increase the reliability of the identification results.