超声提取-高压液相色谱法制备高纯度獐牙菜苦苷  

Extraction and Isolation of Swertiamarin by Ultrasonic Extraction-High Pressure Preparation Liquid Chromatography

作　　者：庞国伟[1] 贺吉香[1] 贺灵剑 田原[1] PANG Guowei;HE Jixiang;HE Lingjian;TIAN Yuan(Shandong University of Traditional Chinese Medicine,Jinan 250355,China;Jinan Dongyuan Biomedical Technology Co.,Ltd.,Jinan 250101,China)

机构地区：[1]山东中医药大学,山东济南250355 [2]济南东源生物医药技术有限公司,山东济南250101

出　　处：《山东中医杂志》2020年第7期732-737,742,共7页Shandong Journal of Traditional Chinese Medicine

基　　金：2018年山东省重点研发计划项目(编号:2060902);济南市科技型中小企业技术创新基金(编号:201502039)。

摘　　要：目的:建立一种从青叶胆(Swertia mileensis)中快速、高效分离制备獐牙菜苦苷的方法。方法 :首先对青叶胆原料进行前处理,然后采用超声波提取法制备青叶胆提取物,再使用高压制备液相色谱法(HPPLC)对所得的青叶胆提取物进行分离纯化,将所得富含獐牙菜苦苷的流分冷冻干燥后,用高效液相色谱法(HPLC)进行纯度分析。结果:前处理方式为去根茎取花叶;最佳超声提取工艺:20倍量75%乙醇,超声提取3次,每次10 min;高压制备液相色谱纯化工艺:反相C18填料,压力10 MPa,以30%甲醇-水为流动相洗脱,所得獐牙菜苦苷纯度经HPLC法分析质量分数为98.17%(峰面积归一化法)。结论:该方法制备獐牙菜苦苷简便、快捷,所得产物的纯度高,适合青叶胆中獐牙菜苦苷的快速制备,同时工艺放大验证其也适用于工业生产。Objective:To develop an effective and rapid method for the preparation of swertiamarin from Swertia mileensis.Methods:The raw materials of Swertia mileensis were pre-treated,then the extract was prepared by ultrasonic extraction method,and then the extract was separated by ultrasonic extraction method and purified by high pressure preparative liquid chromatography(HPPLC).After freeze-drying the part rich in swertiamarin was analyzed for purity by high performance liquid chromatography(HPLC).Results:The pre-treatment method was as follows:The roots and stems were removed and the flowers and leaves were left;the optimized ultrasonic extraction process was described as follows:20 times of 75%ethanol,ultrasonic extraction 3 times,10 minutes each time;HPPLC purification process:reversed phase C18 packing,pressure 10 MPa,30%methanol-water as mobile phase elution,the purity of swertiamarin was 98.17%(peak area normalization).Conclusion:The established method is relatively simple,fast,and suitable for the fast preparation of swertiamarin in Swertia mileensis,and it is also suitable for industrial production.

关 键 词：青叶胆 前处理 超声波提取 高压制备液相色谱法 高纯度 獐牙菜苦苷 

分 类 号：R284.2[医药卫生—中药学]