玄参配方颗粒制备工艺及质量标准研究

Study on Preparation Technology and Quality Standard of Xuanshen Dispensing Granules

目的:制备玄参配方颗粒,并进行质量标准研究。方法:使用正交试验设计优化提取工艺,采用湿法制粒制备玄参配方颗粒,建立薄层色谱(thin layer chromatography,TLC)定性鉴别方法,采用紫外-高效液相色谱法(ultraviolet-high-performance liquid chromatography,UV-HPLC)测定特征性成分哈巴苷和哈巴俄苷的含量。结果:优选的提取工艺为:玄参饮片用水煎煮3次,每次30 min,3次煎煮分别加入10、8和8倍量水;建立的TLC方法,色谱斑点清晰,分离度良好;含量测定方法学考察表明,哈巴苷和哈巴俄苷的线性范围分别为:8.91~89.06μg/mL,R^(2)=1.000;4.81~48.05μg/mL,R^(2)=0.9999;平均加样回收率分别为:102.47%(RSD=1.88%),97.78%(RSD=2.70%)。结论:优化的玄参提取工艺稳定可行,质量控制方法简单,重复性好,可为玄参配方颗粒的质量控制提供参考。

Objective:To prepare Xuanshen(Scrophulariae Radix)dispensing granules and study quality standard.Methods:The orthogonal design was used to optimize the extraction process,wet granulation to prepare Xuanshen dispensing granules,to establish TLC qualitative identification method,UV-HPLC to detect the contents of harpagide and harpagoside.Results:The optimal extraction process was as follows:the slices of Xuanshen were boiled three times with water for 30 minutes each time,ten,eight and eight times of water were added each time;established TLC method showed that chromatographic spots were clear with good resolution;the study on the methodology of content determination displayed that the linear ranges of harpagide and harpagoside ranged between 8.91 and 89.06μg/mL,R^(2)=1.000;4.81 and 48.05μg/mL,R^(2)=0.9999;average recovery rate were 102.47%(RSD=1.88%)and 97.78%(RSD=2.70%)respectively.Conclusion:The optimized extraction process is stable and feasible,the quality control method is simple and has good repeatability,it could provide the reference for quality control of Xuanshen dispensing granules.