摘要
目的优化三仁颗粒制备工艺,并进行质量控制研究。方法采用HPLC法建立苦杏仁苷、厚朴酚、和厚朴酚的含量测定方法,并以出膏量、苦杏仁苷含量、厚朴酚含量、和厚朴酚含量、50%乙醇浸出物为评价指标,以熵权法分配各指标权重,采用正交试验优选三仁汤最佳提取工艺;以成型率、休止角、堆密度和吸湿率为评价指标,采用星点设计-响应面法优化三仁颗粒最佳成型工艺;建立10批三仁颗粒的指纹图谱并进行相似度分析和共有色谱峰归属鉴定,结合薄层鉴别和含量测定对三仁颗粒进行质量控制。结果以苦杏仁苷、厚朴酚、和厚朴酚的含量作为三仁汤质控标准,测得三仁汤中3种指标性成分的质量分数分别为苦杏仁苷0.536~1.054 mg/g,厚朴酚0.015~0.062 mg/g,和厚朴酚0.013~0.053 mg/g;三仁汤最佳提取工艺为加8倍量水,煎煮2次,每次1 h;三仁颗粒最佳成型工艺为糊精为辅料,药辅比1∶1.5,乙醇体积分数78%,乙醇用量为药粉和辅料总量的21%;建立了苦杏仁、薏苡仁、厚朴的薄层鉴别方法和苦杏仁苷、厚朴酚、和厚朴酚的含量测定方法;建立了10批三仁颗粒的指纹图谱,相似度为0.939~0.999,共指认15个共有峰,1号峰归属于苦杏仁、厚朴,2、7、13号峰归属于豆蔻、厚朴、淡竹叶,3、4、8、9号峰为苦杏仁专属峰,5号峰归属于苦杏仁、豆蔻、厚朴、淡竹叶,6、11、12、14、15号峰为厚朴专属峰,10号峰归属于厚朴、淡竹叶。结论该提取方法有效成分提取率高,稳定可靠;成型工艺方法成型率高,流动性好;质量控制和指纹图谱各检查项方法均稳定可靠,能够为三仁颗粒的质量控制提供参考。
Objective The preparation process of Sanren Granules was optimized and the quality control was studied.Methods The content determination method of amygdalin,magnolol and honokiol was established by HPLC.The extraction amount,amygdalin content,magnolol content,honokiol content and 50%ethanol extract were used as evaluation indexes,the entropy weight method was used to assign the weight of each index,the optimum extraction process of Sanren Decoction was optimized by orthogonal test.The optimum molding process of Sanren Granules was optimized by central composite design-response surface method with molding rate,angle of repose,packing density and hygroscopic rate as evaluation indexes.The fingerprints of 10 batches of Sanren Granules were established and the similarity analysis and common chromatographic peaks were identified,the quality control of Sanren Granules was carried out combined with thin-layer chromatography and content determination.Results The contents of amygdalin,magnolol and honokiol were used as the quality control standard of Sanren Decoction.The contents of three index components in Sanren Decoction were as follows:amygdalin was 0.536—1.054 mg/g,magnolol was 0.015—0.062 mg/g,honokiol was 0.013—0.053 mg/g.The best extraction process of Sanren Decoction was as follows:add 8 times the amount of water,boiled twice,one hour each time.The best molding process of Sanren Granules was as follows:dextrin is the excipient,the ratio of drug to excipient was 1∶1.5,the volume fraction of ethanol was 78%,and the amount of ethanol was 21%of the total amount of powder and excipient.The thin-layer chromatography method of Kuxingren(Armeniacae Semen Amarum),Yiyiren(Coicis Semon)and Houpo(Magnolia officinalis Rehd.et Wils.)and the content determination method of amygdalin,magnolol and honokiol were established.The fingerprints of 10 batches of Sanren Granules was established,and the similarity was 0.939—0.999.It was confirmed that there were 15 common peaks.Peak 1 belonged to Armeniacae Semen Amarum and M.
作者
冯禹壮
徐伟
肖春萍
赵淑月
翁丽丽
FENG Yu-zhuang;XU Wei;XIAO Chun-ping;ZHAO Shu-yue;WENG Li-li(School of Pharmaceutical Sciences Changchun University of Chinese Medicine,Changchun 130117,China)
出处
《中草药》
CAS
CSCD
北大核心
2023年第11期3512-3523,共12页
Chinese Traditional and Herbal Drugs
基金
吉中医药发([2021]11号)中医药事业传承发展资金支持项目《重大疫情防治中药方剂储备库建设项目》
吉林省科技厅科研项目(20220204062YY)。
关键词
三仁颗粒
提取工艺
成型工艺
星点设计-响应面法
质量控制
指纹图谱
苦杏仁苷
厚朴酚
和厚朴酚
成型率
休止角
堆密度
吸湿率
Sanren Granules
extraction process
molding process
central composite design-response surface method
quality control
fingerprint
amygdalin
magnolol
honokiol
molding rate
angle of repose
packing density
hygroscopic rate
