黄芩中黄芩苷提取精制工艺研究  

Study on the extraction and purification technology of baicalin from Scutellaria baicalensis Georgi

作　　者：郑艳红[1,2] 常艳芬[1,2] 周玉枝[1] 秦雪梅[1] 杜冠华[3] 

机构地区：[1]山西大学中医药现代研究中心,太原030006 [2]山西大学化学化工学院 [3]中国医学科学院北京协和医学院药物研究所"药物靶点研究与新药筛选"北京市重点实验室

出　　处：《山西医科大学学报》2015年第11期1106-1110,共5页Journal of Shanxi Medical University

基　　金：山西省重点技术创新基金资助项目(财2013-007号)

摘　　要：目的优选黄芩中提取黄芩苷的最佳制备工艺。方法采用单因素试验,对黄芩苷制备工艺的影响因素进行了考察。以提取液中黄芩苷含量和出膏率为评价指标,考察了提取工艺中提取方法(回流提取法、超声提取法和微波提取法)、提取溶剂(水和乙醇)、提取温度(60,70,80,90℃)、料液比(10,15,20倍)、提取次数(1,2,3次)等因素对黄芩苷提取效果的影响;以精制品中黄芩苷含量及收率为评价指标,考察了酸沉pH(1.0,1.5,2.0)、酸沉保温时间(15,30,60 min)、静置时间(3,6,12,18 h)及洗酸次数(0,1,2,5次)对黄芩苷精制的影响,确定纯化工艺中各因素最佳水平。结果制备黄芩苷的最佳工艺条件为:10倍量水80℃回流提取2次,抽滤,合并两次提取液,加6 mol/L盐酸调节pH至1.0,80℃下保温60 min,酸沉静置12 h,离心,沉淀依次用水及50%、95%乙醇各洗涤1次,洗至pH值为中性,即得。在此条件下,可以得到纯度≥80%的黄芩苷产品。结论该优选工艺稳定、可行,为工业大规模生产黄芩苷提供理论依据。Objective To optimize the parameters of the extracting technology of baicalin from Scutellaria baicalensis Georgi. Methods The influential factors of the baicalin preparation process were investigated by single factor test. With the content of baicalin in extracts and extraction rate as assessing indexes,the extraction methods（ reflux extraction,ultrasonic extraction and microwave extraction）,the extraction solvention（ water and ethanol）,the extraction temperature（ 60,70,80,90 ℃）,the solid-liquid ratio（ 10,15,20）and the extraction times（ 1,2,3） were investigated to evaluate their influences on the extraction efficacy and the optimal level of each factor was screened. With the content of baicalin and yield rate in refined products as assessing indexes,the effects of acid-precipitation pH（ 1. 0,1. 5,2. 0）,the incubation temperature（ 15,30 60 min）,the holding time（ 3,6,12,18 h） and the washing acid times（ 0,1,2,5） on the purification were investigated to explore the optimal level of each factor. Results The best extraction conditions were as follows： extraction for twice with 10 folds of water at 80 ℃ for 90 min each time. After filtrated,the extracts were mixed together,and then the pH of the filtrate was adjusted to 1. 0 with hydrochloric acid. The solution was kept in a water bath at the temperature of 80 ℃for 60 min,then laid for 12 h to deposit completely. The upper liquid was centrifuged to spill out. The deposit was washed with water,50% ethanol and 95% ethanol for once,respectively,till the pH value to neutral. Under this condition,the baicalin with purity ≥80% was achieved. Conclusion The optimal process is stable and feasible,thus it can provide a theoretical basis for the industrial large-scale production of baicalin.

关 键 词：黄芩 黄芩苷 制备工艺 单因素实验 

分 类 号：TQ460[化学工程—制药化工]