摘要
目的对清热除湿颗粒主要成分进行薄层鉴别,并采用超高效液相色谱(ultra performance liquid chromatography, UPLC)测定其主要指标性成分含量,为其质量控制提供参考。方法以3批清热除湿颗粒中试样品为研究对象,对方中龙胆、黄芩、车前草、生地黄、白茅根、茯苓及甘草7种药材进行薄层色谱鉴别,并应用UPLC法对君药龙胆、臣药黄芩的指标性成分龙胆苦苷、黄芩苷进行含量测定,采用Acquity UPLC HSS T3C18色谱柱(2.1 mm×100 mm,1.7 μm),以乙腈-0.01%甲酸水为流动相,梯度洗脱。结果薄层鉴别专属性强,可有效鉴别龙胆、黄芩、车前草、生地黄、白茅根、茯苓及甘草。UPLC含量测定方法学考察结果表明,龙胆苦苷在0.014~0.028 μg、黄芩苷在0.015~0.449 μg范围线性关系良好,加样回收率合格。结论采用薄层色谱法对清热除湿颗粒7种药材进行定性鉴别,UPLC法对龙胆苦苷、黄芩苷进行含量测定,可较为全面控制清热除湿颗粒的质量。
Objective To study the quality standard of Qingre-Chushi granules, including TLC identification of main components and ultra performance liquid chromatography determination of main components, so as to lay a foundation for further development of new drugs. Methods Seven constituents, including Gentianae Radix et Razoma, Scutellaria Radix, Plantaginis Herba, Rehmanniae Radix, Imperarae Rhizoma, Poria and Glycyrrhiza Radix et Rhizoma, were determined by TLC. The content of gentiopicroside and Baicalin in Gentiana officinalis and Scutellaria baicalensis was determined by UPLC on Acquity UPLC HSS T3C18 column (2.1 mm×100 mm, 1.7 μm) with acetonitrile-0.01% formic acid water as mobile phase and gradient elution. Results TLC was highly specific and could effectively identify Gentian, Scutellaria baicalensis, Plantain, Rehmannia glutinosa, Rhizoma cocos, and licorice. The results of UPLC assay showed that there was a good linear relationship between gentiopicroside and Baicalin in the range of 0.014-0.028 μg and 0.015-0.449 μg, and the recovery of the three concentrations were all up to standard. Conclusions TLC can be used to identify the seven components of Qingre-Chushi granules, and UPLC can be used to determine the contents of three indicators, which can control the quality of Qingre-Chushi granules.
作者
韩旭阳
朱建新
王宏
李萍
曾祖平
Han Xuyang;Zhu Jianxin;Wang Hong;Li Ping;Zeng Zuping(Beijing Hospital of Traditional Chinese Medicine, Capital Medical University, Beijing Institute of Traditional Chinese Medicine, Beijing Key Laboratory of Clinic and Basic Research with Traditional Chinese Medicine on Psoriasis, Beijing 100010, China)
出处
《国际中医中药杂志》
2018年第12期1181-1186,共6页
International Journal of Traditional Chinese Medicine
基金
北京市中医药科技发展资金项目(JJ2010-23、JJ2013-22).
关键词
质量控制
色谱法
薄层
超高效液相色谱
清热除湿颗粒
Quality control
Chromatography,thin layer
Ultra performance liquid chromatography
Qingre-Chushi granules