摘要
目的:探索出黄连五种主要生物碱的最优提取纯化方法及含量测定方法,为制剂研究奠定基础。方法:采用HPLC进行生物碱的含量测定,以黄连五种主要生物碱加和得率为指标,优选黄连五种主要生物碱提取及纯化工艺。盐酸药根碱、盐酸表小檗碱、盐酸黄连碱、盐酸巴马汀、盐酸小檗碱的浓度,分别在0. 48～4. 80、3. 52～35. 2、2. 04～20. 4、1. 72～17. 2、10. 2～102μg·m L^(-1)(r均大于0. 999)范围内,与峰面积呈良好的线性关系。结果:黄连提取最优的条件为黄连饮片,加8倍量1. 5%的硫酸溶液,煎煮3次,每次40 min。纯化最佳工艺为黄连提取液用Ca(OH)2调节p H 5～6,滤液加HCl调节p H 1～2,加5%NaCl,冰箱冷藏静置过夜,沉淀物干燥。结论:所建立的黄连五种主要生物碱提取纯化工艺及含量测定方法简单可靠。
Objective： To study the optimal conditions of extraction and purification process for five alkaloids and determination for five alkaloids from Rhizome Coptidis, and provide the basis for preparation research of Rhizome Coptidis. Methods： The alkaloids were determined by HPLC. The yield ratio of five alkaloids was used for indication. The extraction technology and the purification technology of five alkaloids were optimised. Rhizine hydrochloride,epiberberine hydrochloride,coptisine hydrochloride,palmatine hydrochloride and berberine hydrochloride showed good linear relationship with the peak area at the range of 0. 48-4. 80,3. 52-35. 2,2. 04-20. 4,1. 72-17. 2,10. 2-102 μg·m L-1（ r〉 0. 999）. Results：The optimal extraction technique was as follows： refluxing extraction 3 times by 1. 5% sulfur acid with liquid-material ratio at8： 1,40 min every time. The optimal purification process was as follows： adjusting extraction liquid to p H value being 5-6 by Ca（ OH）2,adjusting the filtrate to p H value being 1. 5-2 with HCl,adjusting the salinity of solution up to 5% by Na Cl,keeping the solution in the refrigerator for one night,and then filtrating,drying the residue at 50 ℃. Conclusion： The optimal extraction and purification process of five alkaloids from Rhizoma Coptidis and the method for the content determination of five kinds of alkaloids are simple and feasible.
作者
张纯刚
唐静雅
于琛琛
程兰
康廷国
ZHANG Chun-gang;TANG Jing-ya;YU Chen-chen;CHENG Lan;KANG Ting-guo(College of Pharmacy,Liaoning University of Traditional Chinese Medicine,Dalian 116620,China;Department of Pharmacy,The first hospital affiliated to dalian medical university,Dalian 116011,China)
出处
《中国现代中药》
CAS
2018年第9期1146-1149,1156,共5页
Modern Chinese Medicine
基金
国家自然科学基金(81503257)
辽宁省博士启动基金(201501098)
关键词
黄连
生物碱
提取纯化工艺
含量测定
Rhizoma Coptidis
alkaloid
extraction and purity process
determination
