肺热止咳颗粒制备工艺和质量标准研究  

Study on the preparation process and quality standard of Feire Zhike Granules

作　　者：陈佳 呙敏 邢琪昌 刘征 刘湘 李伟 CHEN Jia;GUO Min;XING Qichang;LIU Zheng;LIU Xiang;LI Wei(Pharmacy Department,Xiangtan Central Hospital,Xiangtan 411100,China;Preparation room,Shaoyang traditional Chinese medicine hospital,Shaoyang 422001,China)

机构地区：[1]湘潭市中心医院药学部,湖南湘潭411100 [2]邵阳市中医医院制剂室,湖南邵阳422001

出　　处：《广东药科大学学报》2024年第3期83-88,共6页Journal of Guangdong Pharmaceutical University

基　　金：湘潭市医学科研项目计划(2020-xtyx-22、2022-xtyx-34、2022-xtyx-36);湖南省自然科学基金项目(2023JJ60497)。

摘　　要：目的初步筛选肺热止咳颗粒的制备工艺,并建立质量标准。方法采用L9(34)正交设计试验,考察浸泡时间、提取时间和加水量对黄芩苷的转移率以及干膏得率的影响,优选肺热止咳颗粒的最佳提取工艺。以制软材情况、颗粒收率、休止角及溶化性为评价指标,对赋形剂种类进行考察,优选制剂成型工艺。采用薄层色谱(TLC)法对陈皮、桑白皮进行定性鉴别;采用高效液相色谱(HPLC)法测定制剂中黄芩苷的质量分数。结果最佳提取工艺为浸泡0.5 h,分别加8倍和6倍水,加热回流提取0.5 h和0.25 h;赋形剂以糊精最优;薄层色谱斑点清晰、分离良好,阴性无干扰,专属性强;黄芩苷在质量浓度0.0075~0.75μg/mL范围内,与峰面积呈良好的线性关系;平均回收率为99.137%;肺热止咳颗粒中黄芩苷平均质量分数为8.25 mg/g。结论该工艺稳定可行,建立的TLC和HPLC法专属性强、灵敏度高、重复性好,为后续研发和质量控制奠定了基础。Objective To preliminarily screen the preparation process of Feire Zhike Granules and establish the quality standards.Methods Using the L9(34)orthogonal design experimental method,the effects of soaking time,extraction time,and water addition on the transfer rate of baicalin and the yield of dry extract were investigated to optimize the optimal extraction process for Feire Zhike Granules.The types of excipients were investigated based on the evaluation indicators of soft material preparation,particle yield,angle of repose,and meltability,and the formulation molding process was optimized.Thin layer chromatography(TLC)was used to qualitatively identify Chenpi and Sangbaipi,and high-performance liquid chromatography(HPLC)was used to determine the content of baicalin in the granules.Results The optimal extraction process was as follows:soaking for 0.5 h,adding 8 times and 6 times of water,respectively,and heating and refluxing for 0.5/0.25 h,and the best excipient was dextrin.The TLC spots were clear,well separated,negative without interference,and highly specific.Baicalin showed a good linear relationship with peak area in the concentration range of 0.0075-0.75μg/mL,with an average recovery rate of 99.137%,the average content of Baicalin in Feire Zhike Granules was 8.25 mg/g.Conclusion The process is stable and feasible,and the established TLC and HPLC methods are highly specific,sensitive,and reproducible,which will lay the foundation for subsequent research and development and quality control.

关 键 词：肺热止咳颗粒 制备工艺 质量标准 薄层色谱 高效液相法 黄芩苷 

分 类 号：R283.6[医药卫生—中药学]