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应用离子液体逆流色谱系统分离制备金银花中的绿原酸
引用本文:张伟,董红敬,刘伟,王晓,刘峰.应用离子液体逆流色谱系统分离制备金银花中的绿原酸[J].食品工业,2021(2):107-110.
作者姓名:张伟  董红敬  刘伟  王晓  刘峰
作者单位:齐鲁工业大学(山东省科学院)
基金项目:山东省2017年度农业重大应用技术创新项目;山东省科学院国际科技合作项目(2019GHZD07);现代农业产业技术体系建设专项(CARS-21);山东省生物工程技术创新中心重大创新项目(2019JSWGCCXZX001)。
摘    要:采用离子液体为高速逆流色谱两相溶剂系统的改良剂,分离金银花中的高极性的活性成分绿原酸。首先采用乙酸乙酯萃取、HCl调节p H等方法,将金银花提取液中的绿原酸进行初步富集。通过逆流色谱溶剂系统的选择,以V(乙酸乙酯)︰V(水)︰V(C6min]PF6])=5︰5︰0.5为溶剂系统,上相有机相为固定相,下相水相为流动相。一次进样300 mg粗样,制备得到30 mg绿原酸,经高效液相色谱测定,其纯度为97.5%。并经过ESI-MS和1H NMR确定其化学结构。

关 键 词:离子液体  1-己基-3-甲基咪唑六氟磷酸盐  高速逆流色谱  绿原酸

Purification of Chlorogenic Acid from Lonicera japonica Thunb.by High-Speed Counter-Current Chromatography Using[Cmin][PF]as the Modifier of Two-Phase Solvent System
ZHANG Wei,DONG Hongjing,LIU Wei,WANG Xiao,LIU Feng.Purification of Chlorogenic Acid from Lonicera japonica Thunb.by High-Speed Counter-Current Chromatography Using[Cmin][PF]as the Modifier of Two-Phase Solvent System[J].The Food Industry,2021(2):107-110.
Authors:ZHANG Wei  DONG Hongjing  LIU Wei  WANG Xiao  LIU Feng
Affiliation:(Qilu University of Technology(Shandong Academy of Sciences),Shandong Analysis and Test Center,Jinan 250014)
Abstract:A preparative high speed counter-current chromatography(HSCCC)method for isolation,and purification of Chlorogenic acid with high polarity was successfully established by usingC6 min]PF6]as the modifier of the two-phase solvent system.Chlorogenic acid in lonicerae extract was preliminarily enriched by means of ethyl acetate extraction and pH adjustment of HCl.In HSCCC separation,the two-phase solvent system was composed of V(ethyl acetate)︰V(water)︰V(C6min]PF6])at the volume ratio of 5︰5︰0.5,the upper organic phase was stationary phase,and the lower aqueous phase was the mobile phase.As a result,30 mg of chlorogenic acid was successfully obtained in one-step separation by HSCCC from 300 mg of crude extract.The purity of chlorogenic acid was 97.5%based on peak area normalization method as determined by HPLC,and the structure of the compound was identified by ESI-MS and 1 H NMR.
Keywords:ionic liquid  1-hexyl-3-methylimidazolium hexafluorophosphate([C6min][PF6])  high speed counter-current chromatography(HSCCC)  chlorogenic acid
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