天然产物研究与开发 ›› 2014, Vol. 26 ›› Issue (1): 87-93.

• 开发研究 • 上一篇    下一篇

牡丹皮化学成分系统化色谱分离方法研究

朱靖博1*,韩聪敏1,丁燕1,寇自农2,王振中3,萧伟3   

  1. 1 大连工业大学食品学院;2 大连工业大学分析测试中心,大连 116034;3 江苏康缘药业股份有限公司,连云港 222001
  • 出版日期:2014-01-31 发布日期:2014-12-15

Systematic Chromatographic Separation of Chemical Components of Moutan Cortex

ZHU Jing-bo1*, HAN Cong-min1, DING Yan1, KOU Zi-nong2, WANG Zhen-zhong3, XIAO Wei3   

  1. 1 School of food Science and Technology,Dalian Polytechnic University; 2 Modern Education Technology Branch,Dalian Polytechnic University,Dalian 116034, China; 3 Jiangsu Kanion Pharmaceutical Co.Ltd,Lianyungang 222001,China
  • Online:2014-01-31 Published:2014-12-15

摘要: 以牡丹皮为研究对象,探索中药复杂成分系统化色谱分离方法。通过对牡丹皮甲醇提取物进行系统溶剂萃取,TLC、HPLC分析化合物组成变化,确定牡丹皮化学成分色谱分离的前处理方法;以系统化TLC方法筛选确定了牡丹皮Fr1.3组分制备色谱分离条件;预测了台阶梯度洗脱条件下待分离物质的保留体积。结果显示:牡丹皮甲醇提取物经正己烷、乙酸乙酯依次萃取是有效的色谱分离前处理方法,减少了分离样品复杂性;建立的系统化TLC方法可以快速选定制备柱色谱的分离条件;台阶梯度洗脱分离情况下,分离目标化合物在初始洗脱溶剂下,其0.10<Rf≤0.65时,多阶梯梯度预测方法准确预测了Fr1.3组分制备柱分离各化合物的保留体积;选定台阶梯度洗脱条件下,1/3理论上样量、理论上样量、最大上样量的三次制备柱色谱分离实践表明,Fr1.3组分中的6个化合物均得到TLC单点的纯化合物,其中3个化合物的HPLC纯度在95%以上。该方法也可用于其它中药成分的系统化分离。

关键词: 牡丹皮, 系统化分离, 色谱条件筛选, 台阶梯度预测, 制备色谱

Abstract: In this study,a systematic chromatographic separation method was developed for the extraction and isolation of chemical components of Moutan Cortex.Pretreatment method of chromatographic separation was established through systematic liquidliquid extraction of Moutan Cortex methanol extract.The preparative chromatographic conditions of component Fr1.3 from Moutan Cortex was determined by systematic TLC screening method.The retention volume of targeted compounds was predicted in the step gradient elution conditions.The results showed that effective pretreatment method was liquidliquid extracting the methanol extract of Moutan Cortex using hexane,ethyl acetate sequentially.The systematic TLC methods can quickly select preparative column chromatographic separation conditions.The retention volume of the targeted compounds in Fr1.3 was accurately predicted under step gradient elution chromatographic separation conditions.Three times (with 1/3 theoretical sample loading,theoretical loading and maximum sample loading,respectively) of preparative chromatographic separation were carried out under the developed gradient elution conditions.The results showed that 6 pure compounds were successfully obtained from Fr1.3,in which the purities of 3 compounds were over 95% by HPLC.The method developed in this study can be used for the systematic chromatographic separation of other Chinese medicine components.

Key words: Moutan Cortex, systematic chromatographic separation, screening of chromatographic conditions, step gradient prediction, preparation chromatography

中图分类号: 

R932