芪蛭益肺颗粒成型工艺及质量标准研究

Study on the molding process and quality standard of Qizhi Yifei granules

目的确定芪蛭益肺颗粒的成型工艺,建立芪蛭益肺颗粒的质量标准。方法应用休止角测定仪分别测定浸膏粉和颗粒的流动性;以吸湿百分率、颗粒成型率、软材状态、制粒难易为考察指标,确定成型所用辅料、药辅比及润湿剂浓度;分别测定颗粒的溶化性、堆密度及临界相对湿度;采取薄层色谱(thin layer chromatography,TLC)法对方中的黄芪、酒黄精、制水蛭、清半夏、浙贝母、当归、化橘红、前胡进行定性鉴别,高效液相色谱法-蒸发光散射检测器(high performance liquid chromatography-evaporative light scattering detector,HPLC-ELSD)对芪蛭益肺颗粒中黄芪甲苷进行含量测定。结果通过制粒改善了浸膏粉的流动性,确定最佳辅料为糊精,最佳药辅比浸膏粉∶糊精(1∶1);润湿剂为90%乙醇。处方中各味药薄层色谱斑点分离好,无阴性干扰;黄芪甲苷在0.02502～0.70056 mg/mL范围内呈良好的线性关系(R2=0.9994),平均加样回收率(n=6)为96.76%,RSD为0.52%。结论该成型方法成型率高,溶化性好,临界相对湿度升高,质量标准方法稳定可行,重复性好,可用于芪蛭益肺颗粒的质量控制。

Objective To determine the molding process of Qizhi Yifei granules, and establish the quality standard of Qizhi Yifei granules. Methods The flowability of extract powder and granule were determined by resting angle meter respectively. The percentage of moisture absorption, particle formation rate, shape of soft wood and degree of difficulty of granulation were taken as the indexes to determine the excipients, the ratio of drugs and additives and the concentration of wetting agents. The solubility, bulk density and critical relative humidity of the particles were determined respectively. Qualitative identification of Radix Astragali seu Hedysari, alcohol processed Rhizoma Polygonati, processed Hirudo, Rhizoma Pinelliae Preparata, Bulbus Fritillariae Thunbergii, Radix Angelicae Sinensis, Exocarpium Citri Grandis and Radix Peucedani in the granules were performed by thin layer chromatography （TLC）. The high performance liquid chromatography-evaporative light scattering detector method （ HPLC-ELSD ） was used to determine the contents of astragaloside IV in Qizhi Yifei granules. Results The flowability of extract powder was improved by granulation, and the best excipient was dextrin, with the best ratio of extract to powder∶dextrin（1∶1）. The wetting agent was 90% ethanol. The TLC spots were clear without interference of the negative control. The linear range of astragaloside IV was 0.02502~0.70056 mg/mL （ r =0.9994 ）, with the average recovery of 96.76% and RSD 0.52%. Conclusion The molding method has high molding rate, good melting property and critical relative humidity. The method is accurate, reliable, specific and reproducible, and can be used for the quality control of Qizhi Yifei granules.