摘要
目的:优化黄杞叶总黄酮的提取与纯化工艺,并建立其中3种有效成分的含量测定方法。方法:以落新妇苷的提取转移率为指标,采用单因素试验对提取工艺中的提取溶剂、提取方式、渗漉溶剂乙醇的体积分数、渗漉料液比、渗漉前浸泡时间、渗漉速度和AB-8树脂纯化工艺中洗脱剂乙醇的体积分数进行考察,并采用正交试验优化提取工艺。采用高效液相色谱法对纯化后黄杞叶总黄酮中3种有效成分(落新妇苷、花旗松素、黄杞苷)进行含量测定。结果:优化后的黄杞总黄酮的提取工艺为以70%乙醇体积为提取和渗漉溶剂,采用渗漉法提取,渗漉前浸泡8 h,渗漉料液比1∶16(g/ml),渗漉速度30 ml/(min·kg);纯化工艺为取渗漉液加水稀释至0.5 g(生药)/ml,乙酸乙酯萃取,萃取液蒸干后以50%乙醇溶解,AB-8树脂上样,50%乙醇洗脱,浓缩、干燥;验证试验中落新妇苷提取转移率>80%(RSD=0.42%,n=3)。纯化后黄杞叶总黄酮中落新妇苷、花旗松素、黄杞苷的含量分别为57.94%、3.72%、2.83%,三者含量之和占总黄酮的64.00%。结论:建立的提取和纯化工艺稳定、合理、可靠;黄杞叶总黄酮中3种有效成分的含量测定方法准确、简单、重复性好。
OBJECTIVE： To optimize the extraction and purification technology of total flavonoids from Engelhardia roxburghi- ana, and to establish the method for the content determination of 3 kinds of effective components. METHODS： Using the extrac- tion transfer rate of astilbin as index, single factor test was used to investigate extraction solvent, extraction method, volume frac- tion of percolation solvent ethanol, percolation material-liquid ration, soaking time before percolation and percolation rate of extrac- tion technology, and volume fraction of eluant ethanol in AB-8 resin purification technology. The contents of 3 effective compo- nents as astilbin, texifolin and engelitin in total flavonoids from E. roxburghiana were determined by HPLC. RESULTS： The opti- mal extraction technology was using 70% ethanol as extraction and percolation solvent, percolation extraction, soaking for 8 h be- fore percolation, percolation material-liquid ratio of 1：16 （g/ml）, percolation rate of 30 ml/（min, kg）. The purification technology was diluting the solution to 0.5 g （crude drug）/ml with water, ethyl acetate extraction, dissolved extract with 50% ethanol after evaporated to dryness, AB-8 resin for sampling, eluted with 50% ethanol, concentrating and drying. In verification test, extraction transfer rate of astilbin was more than 80% （RSD=0.42%, n=3）. The contents of astilbin, taxifolin and engeletin in total fiavo- noids from E. roxburghiana by purified were 57.94%, 3.72% and 2.83%, respectively; the contents of 3 components accounted for 64.00% of total fiavonoids. CONCLUSIONS： The extraction and purification technology is stable, rational and reliable; the content determination method of 3 effective components in total flavonoids of E. roxburghiana is accurate, simple and producible.
出处
《中国药房》
CAS
北大核心
2016年第25期3545-3548,共4页
China Pharmacy
基金
天津市应用基础及前沿技术研究计划(青年基金项目)(No.12JCQNJC08700)
关键词
黄杞叶
总黄酮
提取工艺
纯化工艺
正交试验
AB-8树脂
落新妇苷
花旗松素
黄杞苷
含量测定
Engelhardia roxburghiana
Total fiavonoid
Extraction technology
Purification technology
Orthogonal test
AB-8 resin
Astilbin
Taxifolin
Engeletin
Cotent determination
