基于粉体学表征技术的浙贝母配方颗粒处方和工艺研究

Study on prescription and process of Fritillariae Thunbergii Bulbus formula granules based on characterization of powdery

目的研究浙贝母配方颗粒处方和工艺。方法采用煎煮法对浙贝母进行提取;采用喷雾干燥法制备浙贝母浸膏粉;采用湿法挤压制粒、挤出-滚圆制粒、流化床制粒3种方法制备浙贝母配方颗粒,设定以粉体流动性参数休止角、最终体积减少度(a)、充填速度常数(b、k)及颗粒一次收得率为指标的综合评价方法,优选颗粒的最佳制备工艺、处方辅料及其配比;采用HPLC法测定颗粒中有效成分贝母素甲和贝母素乙含量,色谱柱为Agilent Zorbax Eclipse XDB-C18(150 mm×4.6mm,5μm);流动相为乙腈-水-二乙胺(70∶30∶0.03);检测器为蒸发光散射;体积流量为1.0 m L/min;柱温为30℃。结果流化床制粒法制得的浙贝母配方颗粒综合评分最高,最佳处方为浸膏粉-糊精-95%乙醇(100∶100∶160),颗粒一次收得率为91.3%,休止角为30.73°,a值为0.109 1,b值为0.025 5,k值为0.030 1,流动性好,得率高;高效液相色谱法测得颗粒中贝母素甲含量为0.305%,贝母素乙含量为0.098%。结论优化的浙贝母配方颗粒处方和工艺均达到设计要求,可用于工艺化大生产。

Objective To study the prescription and process of Fritillariae Thunbergii Bulbus（FTB） formula granules. Methods FTB was extracted by decocting method. FTB extract powder was prepared by spray drying method. Wet-extruding granulating, extruded-rolling granulating, and one-step granulating were adopted for preparing the formula granules. A comprehensive evaluation method was based on the powder fluidity parameters such as the rest angle, the final volume reduction degree（a）, the filling velocity constant（b, k）, and the yield of the particles, to optimize the optimum preparation process, prescription excipients and their proportion. An HPLC method was used to determine the contents of peimine and peiminine. The chromatographic column was the Agilent Zorbax Eclipse XDB-C18 column（150 mm × 4.6 mm, 5 μm）, and the flow phase was Acetonitrile-water-diethylamine（70∶30∶0.03）; The volume flow was 1.0 m L/min; The column temperature was 30 ℃. Results The synthesis score of the FTB formula granules prepared by one-step granulating method was the highest. The best prescription was the extract powder-dextrin-95% ethanol solution（100∶100∶160）. The particle yield was 91.3%, the rest angle was 30.73°, the value of a was 0.109 1, the value of b was 0.025 5 and the value of k was 0.030 1, the fluidity of the granules was good and the yield was high. The content of peimine was 0.305% and the content of peiminine was 0.098% in the particles by HPLC. Conclusion In this experiment, the formulation and process of FTB formula granules were designed to met the design requirements, which could be used in the production of the technology.