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。 A preparative high speed counter-current chromatography(HSCCC)method for isolation,and purification of Chlorogenic acid with high polarity was successfully established by using[C6 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.
机构地区 齐鲁工业大学（山东省科学院）
出处 《食品工业》 CAS 北大核心 2021年第2期107-110,共4页 The Food Industry
基金 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)。
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 ionic liquid 1-hexyl-3-methylimidazolium hexafluorophosphate([C6min][PF6]) high speed counter-current chromatography(HSCCC) chlorogenic acid
分类号 R28 [医药卫生—中药学]
