望江南茎中大黄素提取工艺优化、纯化及鉴定  

Extraction Process Optimization,Purification and Identification of Emodin from Senna occidentalis Stem

作　　者：周昊[1] 杨瑾 张玉红[2] Zhou Hao;Yang Jin;Zhang Yuhong(Jilin University,Changchun 130026,P.R.China;Northeast Forestry University)

机构地区：[1]吉林大学,长春130026 [2]东北林业大学

出　　处：《东北林业大学学报》2023年第8期65-70,76,共7页Journal of Northeast Forestry University

基　　金：国家科技计划项目(2012BADB0501-07)。

摘　　要：以望江南茎为试验材料,进行最优提取溶剂的筛选,选取盐酸用量、乙醇体积分数、提取时间和提取温度4个因素,在单因素试验的基础上,以望江南茎中大黄素的质量分数为响应值,应用Design-Expert V.12软件中心组合试验(Box-Benhnken)设计进行四因素三水平试验,通过响应面法优化得到热回流法提取望江南茎中大黄素的最佳提取工艺,同时在此基础上进行大黄素的分离纯化,探讨从望江南茎中获得高纯度大黄素的可行性,并建立一套合理可行的鉴定方法。结果表明:望江南中大黄素热回流最佳工艺参数以乙醇为提取溶剂,每20 mL提取溶剂需盐酸用量2 mL,乙醇体积分数88%,提取时间86 min,提取温度为84℃。采用三氯甲烷萃取法结合pH梯度碱液法分离及硅胶柱色谱法纯化利用最优条件下得到大黄素提取物,利用高效液相色谱法(HPLC)、液质联用(LC-MS)联合定性定量分析,所得到纯化后的大黄素纯度达到95.8%。Taking the stem of Senna occidentalis as the experimental material,the optimal extraction solvent was screened,four factors including hydrochloric acid dosage,ethanol concentration,extraction time and extraction temperature were selected,on the basis of the single-factor experiment,and the content of emodin in S.occidentalis stem as the response value,the Design-Expert V.12 software Box-Benhnken design was used to carry out a four-factor and three-level experiment.The optimal process of Heating Reflux Method(HRM)for extracting emodin from S.occidentalis stems was optimized by response surface methodology,and the separation and purification of emodin was performed on this basis.The feasibility of obtaining high-purity emodin from S.occidentalis stems was discussed,and a set of reasonable and feasible identification methods were established.The results showed that the optimal process parameters for HRM of emodin in S.occidentalis stem were:ethanol was used as extraction solvent,2 mL of hydrochloric acid per 20 mL of extraction solvent,88%ethanol concentration,86 min of extraction time,and 84℃of extraction temperature.The emodin extract was obtained under the most optimal conditions by using chloroform extraction combined with pH gradient alkaline solution separation and silica gel column chromatography.HPLC and LC-MS were used for qualitative and quantitative analysis,the purity of emodin obtained after purification was 95.8%.

关 键 词：望江南茎 大黄素 响应面法 纯化方法 柱层析 液相质谱 高效液相色谱 

分 类 号：Q949.95[生物学—植物学]