From medicinal plant to compound: isolation of shikimic acid from Illicium verum by hyphenated expan

来源 :第七届国际逆流色谱会议(The 7th International Conference on Countercurre | 被引量 : 0次 | 上传用户:anavelgato234
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  Counter-current chromatography (CCC) has been developed for over 40 years and been applied in various fields.Those applications,particularly in natural products,have shown great advantages in high recovery and short processing time [1].Natural compounds,which researchers are interested in,are usually present in medicinal plants at very low levels,which make the isolation process tedious and expensive.However,before the separation by CCC,the crude materials need long processing procedure such as extraction,filtration,concentration and preliminary separation to prepare crude samples for CCC.How to achieve the target compounds from medicinal plants in a fast,accurate and comprehensive way will be the main challenge for researchers.Expanded bed adsorption chromatography (EBAC) is a unique technique which integrated clarification,concentration and purification into one operation unit [2].The new operation unit eliminates the steps of centrifugation and filtration,saves operating time,improves the yield of target compounds and reduces the cost of purification.A new method for deriving drug discovery leads from medicinal plants is presented in this paper.This method involves: 1) hyphenating EBAC to CCC via an interface unit,2) in the 1st dimension,preliminary separation of targets by integrated EBAC,3) CCC solvent system selection and matching,4) in the 2nd dimension,fine separation of targets by CCC.This method was used in the following case study.In the extraction step,a certain amount (8.0 g) of Illicium verum was put into the continuous extraction column with an ultrasonic assisted extraction device outside.Ion exchange resins (D293) were packed into the expanded bed chromatography column.Target compound-shikimic acid was extracted in the continuous extraction column and simultaneously the target being extracted was directly exchanged onto the resins packed in the expanded bed column.During this operation,the resins in chromatographic column were in an expanded status and there was space among resins.This character of expanded bed will allow particulate containing feed stock to go through the column without blockage.In the 1st dimension,the expanded bed was eluted by 2% aqueous NaCl solution and part of the fractions with shikimic acid was transferred to the interface unit-a sample loop for matching with the CCC solvent system.In the 2nd dimension,the fractions (containing shikimic acid) were injected into the CCC column.The separation was performed to separate shikimic acid with a butanol-water-acetic acid (4:5:1) solvent system.28-mg of shikimic acid was purified,with 99.6% purity and 50% recovery.This research case study proved the feasibility of the newly developed hyphenated chromatography method.
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