doi:10.16597/j.cnki.issn.1002-154x.2022.07.002
金樱子配方颗粒质量控制研究
李蕊∗ 张志强 高扬
(北京康仁堂药业有限公司,中药配方颗粒关键技术国家地方联合工程研究中心, 北京市中药配方颗粒工程技术研究中心,北京 101301)
Study on Quality Control of Rosa Laevigata Dispensing Granules
Li Rui∗; Zhang Zhiqiang; Gao Yang;
(Beijing Tcmages Pharmaceutical Co. , Ltd. ,Traditional Chinese Medicine Formula Particles Key Technology National United Engineering Research Center, Beijing Chinese Medicine Formula Particles Engineering Technology Research Center, Beijing 101301)
摘要:
目的:建立金樱子配方颗粒的质量控制方法。 方法:采用 TLC 法对金樱子配方颗粒进行定性鉴别,采用醇溶 性浸出物法中的热浸法测定,对水分、粒度、溶化性指标进行检查,采用 UPLC 法测定金樱子配方颗粒中儿茶素的含量,并研究金樱子配方颗粒指纹图谱。 结果:TLC 法中金樱子配方颗粒与对照药材相应的位置上呈现相同颜色的斑点;水分、粒度和溶化性符合《中国药典》2015 版中的相关要求;儿茶素含量的线性范围为 0.0207 ~ 0.2073 mg·mL - 1 (R2 = 0.9996),平均回收率为 100.22% (RSD = 2.6% );图谱中共标记 5 个共有峰,其中 1 号峰为没食子酸峰,2 号峰为原儿茶酸峰,4 号峰为儿茶素峰,5 号峰为鞣花酸峰。 4 号峰儿茶素峰保留时间适中,峰面积较大,分离度较好,确定 为 S 峰。 指纹图谱研究显示 18 批金樱子配方颗粒相似度良好,均大于 0.90。 结论:该方法准确稳定,重复性好,可有 效控制金樱子配方颗粒的质量。
关键词：金樱子 配方颗粒 质量标准 超高效液相色谱 指纹图谱
Abstract：
Objective: To establish the quality control method of Rosa laevigata dispensing granules. Methods: TLC method was used for qualitative identification of Rosa laevigata dispensing granules. Hot leaching method of alcohol soluble extract method was used to determine the extract, for testing the moisture, particle size and solubility indexes. The content of catechin in the Rosa laevigata granules was determined by UPLC method, and the fingerprint of Rosa laevigata dispensing granules was studied. Results: The results showed that same color spots were found in the corresponding positions of Rosa laevigata granules and the reference medicinal materials in TLC method. The water content, particle size and solubility meet the relevant requirements of 2015 Edition of Chinese Pharmacopoeia. The linear range of catechin content was 0. 0207 ~ 0. 2073 mg·mL - 1 (R2 = 0. 9996). The average recovery was 100. 22% (RSD = 2. 6% ). There were 5 common peaks marked in the fingerprint, among which the no. 1 peak was gallic acid, the no. 2 peak was protocatechuic acid, the no. 4 peak was catechin, and the no. 5 peak was ellagic acid. Among them, the no. 4 catechin peak had a moderate retention time, a large peak area and a good separation degree, so was determined as the S peak. The fingerprint study showed that the similarity of 18 batches of particles was good, all of which were greater than 0. 90. Conclusion: The method is accurate, stable and reproducible, which can effectively control the quality of Rosa laevigata dispensing granules.
Keywords：Rosa laevigata; dispensing granules; quality standard; ultra performance liquid chromatography; fingerprint