盐酸青藤碱萃取和精制的新工艺  

New Process of Extraction and Refining of Sinomenine Hydrochloride

作　　者：彭祖仁 任丹丹 颉佳乐 龚行楚[2,3,4] 龙宪军 PENG Zuren;REN Dandan;XIE Jiale;GONG Xingchu;LONG Xianjun(Hunan Zhengqing Pharmaceutical Group Co.,Ltd.,Huaihua 418005;College of Pharmaceutical Sciences,Zhejiang University,Hangzhou 310058;National Key Lab.of Chinese Medicine Modernization,Innovation Center of Yangtze River Delta,Zhejiang University,Jiaxing 314100;Jinhua Institute,Zhejiang University,Jinhua 321016)

机构地区：[1]湖南正清制药集团股份有限公司,湖南怀化418005 [2]浙江大学药学院,浙江杭州310058 [3]浙江大学长三角智慧绿洲创新中心,现代中药创制全国重点实验室,浙江嘉兴314100 [4]浙江大学金华研究院,浙江金华321016

出　　处：《中国医药工业杂志》2024年第10期1399-1405,共7页Chinese Journal of Pharmaceuticals

基　　金：湖南省自然科学基金项目(2022JJ80084)。

摘　　要：设计酸水提取法以及所得青藤碱提取液的精制新工艺步骤,采用计算优化的方法确定萃取精制的试验参数,并且进行试验验证。回收氯仿循环套用10次。采用高效液相色谱法测定制得产品中盐酸青藤碱的含量。所获得的参数范围为:碱性体系(E_(1))的pH值为9~10,萃取时氯仿与E_(1)体积比为1∶10,水洗时有机相(O_(1))与水体积比为1∶3,反萃取时有机相(O_(2))与水体积比为1∶8,水相(A_(1))的pH值为4~5。在相同投料量下,氯仿循环套用5次后,盐酸青藤碱的产量稳定在0.3 g以上,纯度稳定在95%以上。该研究开发了制备盐酸青藤碱的新工艺,证明了氯仿循环套用的可行性,制备得到高纯度盐酸青藤碱,能减少固体废渣、降低生产成本。The acid water extraction method was designed,and a new refining process for the sinomenine extraction solution was developed.Experimental parameters for extraction and purification were determined by computational optimization,and experimental verification was performed.Chloroform was recycled for 10 times.The content of sinomenine hydrochloride in the prepared product was determined by HPLC.The experimental parameter ranges were set as follows:in the alkaline system(E_(1)),the pH value ranged from 9 to 10.During the extraction process,the volume ratio of chloroform to E_(1) was 1∶10.During the water-washing process,the volume ratio of organic phase(O_(1))to water was 1∶3.During the acid-water stripping process,the volume ratio of organic phase(O_(2))to water was 1∶8.In the aqueous phase(A_(1)),the pH value ranged from 4 to 5.Under the same feed amount,after chloroform was reused for five times,the purity of prepared sinomenine hydrochloride maintained stable.This study developed a new process for the preparation of sinomenine hydrochloride,demonstrating the feasibility of recycling chloroform and obtaining high-purity sinomenine hydrochloride,which could reduce solid waste and production costs.

关 键 词：盐酸青藤碱 提取 精制 循环套用 

分 类 号：TQ461[化学工程—制药化工]