摘要
目的:优选小承气汤颗粒的干法制粒工艺,并制定其质量控制方法。方法:以颗粒一次性成型率、休止角、吸湿率及溶化性为考察指标,在单因素考察干法制粒机压片压力、辅料(糊精∶可溶性淀粉)比例和二氧化硅用量的基础上,结合正交实验,优选小承气汤颗粒的干法制粒最佳工艺。采用薄层色谱法(TLC)鉴别方法和高效液相色谱法(HPLC)测定小承气汤颗粒中游离蒽醌、总蒽醌(以大黄酸、大黄素、大黄酚)含量,建立其质控标准。结果:优化后的小承气汤颗粒干法制备工艺为:干膏粉∶辅料=7∶3,辅料(糊精∶可溶性淀粉=1∶1),二氧化硅用量5%,压片压力22 MPa。颗粒中大黄、厚朴和枳实饮片的TLC鉴别斑点清晰,阴性无干扰。大黄酸在36.22~362.20 ng、大黄素在36.80~368.00 ng、大黄酚在38.44~384.40 ng范围内线性关系良好(R^(2)=0.9999)。游离大黄酸、大黄素、大黄酚的平均回收率分别为98.46%,102.25%,99.02%;总大黄酸、大黄素、大黄酚的平均回收率分别为95.18%,93.84%,97.94%。结论:优选的干法制粒工艺条件稳定可行,适合规模化生产;质量控制方法简单准确,可用于小承气汤颗粒的质量控制。
Objective:To optimize the dry preparation technology of Xiaochengqitang granules and establish its quality control method.Methods:Taking the one-time forming rate,angle of repose,hygroscopicity and solubility of the granules as the inspection indexes,on the basis of single factor inspection of the tablet pressure of the dry granulator,the proportion of excipients(dextrin:soluble starch)and the amount of silica,combined with the orthogonal test,the best dry preparation technology of Xiaochengqitang granules was optimized.The contents of free and total anthraquinones(including rhein,emodin and chrysophanol)in Xiaochengqitang granules were determined by thin layer chromatography(TLC)and HPLC,and its quality control standard was established.Results:The optimized dry preparation technology of Xiaochengqitang granules was as follows:dry paste powder∶excipients=7∶3,excipients(dextrin∶soluble starch=1∶1),silica dosage 5%,tablet pressure 22 MPa.The TLC identification spots of Rhubarb,Magnolia officinalis and Fructus Aurantii in the granules are clear and negative without interference.The linearity was good in the range of 36.22~362.20 ng for rhein,36.80~368.00 ng for emodin,and 38.44~384.40 ng for chrysophanol(R^(2)=0.9999).The average recoveries of free rhein,emodin and chrysophanol were 98.46%,102.25% and 99.02%,respectively;The average recoveries of total rhein,emodin and chrysophanol were 95.18%,93.84% and 97.94% respectively.Conclusion:The optimized dry preparation technology conditions are stable,feasible and suitable for large-scale production;The quality control method is simple and accurate,and can be used for the quality control of Xiaochengqitang granules.
作者
朱文杰
单家明
杨元丰
熊豪
郭文慧
叶喜德
杨武亮
ZHU Wen-jie;SHAN Jia-ming;YANG Yuan-feng;XIONG Hao;GUO Wen-hui;YE Xi-de;YANG Wu-liang(Key Laboratory of Modern Chinese Medicine Pharmaceutics of Ministry of Education,Jiangxi University of Traditional Chinese Medicine,Nanchang 330004,China)
出处
《中国新药杂志》
CAS
CSCD
北大核心
2024年第6期588-597,共10页
Chinese Journal of New Drugs
基金
国家自然科学基金资助项目(81760680)
江西中医药大学校级科技创新团队发展计划资助项目(CXTD22003)。
关键词
小承气汤颗粒
干法制粒
薄层色谱法鉴别
高效液相色谱法测定
质量标准
Xiaochengqitang granules
dry granulation
thin layer chromatography identification
HPLC determination
quality standard
