大黄碳酸氢钠片中大黄及薄荷油的质量控制研究
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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,5μm)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。
Objective: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.
Objective: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.
引文
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[11]毛春芳,施忠,罗琳,等.HPLC法同时测定大黄中芦荟大黄素等11种成分的量[J].中草药,2014,45(16):2400-240.
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[14]国家药典委员会.中华人民共和国药典(四部)[S].北京:中国医药科技出版社,2015:375-376.
[2]周立文,杜改焕.大黄碳酸氢钠片联合莫沙必利治疗2型糖尿病便秘50例临床观察[J].中医临床研究,2014,6(15):59-60.
[3]谭成波,胡永才,周海洋,等.大黄碳酸氢钠片预防成人重度烧伤便秘的疗效观察[J].现代医药卫生,2012,28(15):2356-2357.
[4]许邑匡,候伟俊.大黄碳酸氢钠片对血液透析不充分患者的疗效观察[J].中国社区医师·医学专业,2012,19(14):208-209.
[5]张彦平,马东梅.大黄碳酸氢钠片治疗急性黄疸型肝炎的疗效观察[J].医学信息,2009,1(5):224.
[6]金鹏.不同厂家大黄碳酸氢钠片中大黄素、大黄酚的含量考察[J].今日药学,2012,22(10):615-618.
[7]Wang J,Zhao Y,Xiao X,et al.Assessment of the renal protection and hepatotoxicity of rhubarb extract in rats[J].J Ethnopharmacol,2009,124(1):18-25.
[8]Hawryl M,Swieboda R,Hawryl A,et al.Micro Two-Dimensional Thin-Layer Chromatography and chemometric analysis of essential oils from selected Mentha species and its application in herbal fingerprinting[J].Journal of Liquid Chromatography&Related Technologies,2015,38(20):1794-1801.
[9]国家药典委员会.中华人民共和国药典(四部)[S].北京:中国医药科技出版社,2015:57.
[10]国家药典委员会.中华人民共和国药典(一部)[S].北京:中国医药科技出版社,2015:24.
[11]毛春芳,施忠,罗琳,等.HPLC法同时测定大黄中芦荟大黄素等11种成分的量[J].中草药,2014,45(16):2400-240.
[12]国家药典委员会.中华人民共和国药典(一部)[S].北京:中国医药科技出版社,2015:945.
[13]国家药典委员会.中华人民共和国药典(一部)[S].北京:中国医药科技出版社,2015:1168.
[14]国家药典委员会.中华人民共和国药典(四部)[S].北京:中国医药科技出版社,2015:375-376.