高速逆流色谱制备分离紫甘薯花色苷  

Preparative Isolation of Anthocyanins from Purple Sweet Potato by High-speed Counter-current Chromatography

作　　者：陆英[1,2,3] 李佳银[2] 罗晋[2] 李觅路[2] 刘仲华[1,2,3] 

机构地区：[1]国家植物功能成分利用工程技术研究中心,长沙410128 [2]湖南农业大学园艺园林学院,长沙410128 [3]湖南省作物种质创新与资源利用重点实验室,长沙410128

出　　处：《分析化学》2011年第6期851-856,共6页Chinese Journal of Analytical Chemistry

基　　金：湖南省重大科技专项(No.NK07006)资助

摘　　要：采用高速逆流色谱法分离纯化紫甘薯花色苷。以正丁醇-乙酸乙酯-0.5%乙酸(3∶1∶4,V/V)为溶剂体系,上相为固定相,下相为流动相,流速2 mL/min,进样量300 mg,分离得到两种花色苷的混合物;混合物再以0.2%三氟乙酸-正丁醇-甲基叔丁基醚-乙腈(6∶5∶2∶1,V/V)为溶剂体系,上相为固定相,下相为流动相,流速1.5 mL/min,进样量100 mg,分离得到纯度分别为98.5%和96.7%的两个花色苷单体组分。通过紫外-可见光谱、质谱、核磁等技术进行结构鉴定,确定组分1为3-O-{6-O-(E)-咖啡酰-2-O-[6-O-(E)-对羟基苯甲酰-β-D-吡喃葡糖基]-β-D-吡喃葡糖苷}-[5-O-(β-D-吡喃葡糖苷)]芍药素,组分2为3-O-{6-O-(E)-咖啡酰-2-O-[6-O-(E)-阿魏酰-β-D-吡喃葡糖基]-β-D-吡喃葡糖苷}-[5-O-(β-D-吡喃葡糖苷)]芍药素。实验从450 g紫甘薯中获得63 mg组分1和48 mg组分2,为紫甘薯花色苷分离提供了高效、稳定、可靠的方法。High-speed counter-current chromatography（HSCCC） was successfully applied to separate and purify anthocyanins from purple sweet potato.With a two-phase solvent system composed of n-butanol-ethylacetate-0.5% acetic acid（3∶1∶4,V/V）,the upper phase as stationary phase,the lower phase as mobile phase at a flow rate of 2.0 mL/min,and injection volume of 300 mg,a mixgure of two anthocyanins was received by undertaking HSCCC.Subsequently,a refining HSCCC was performed to separate and purify these two compounds,with a two-phase solvent system of 0.2% trifluoroacetic acid-n-butanol-methyl tertiary butyl ether-acetonitrile（6∶5∶2∶1,V/V）,the upper phase as stationary phase,the lower phase as mobile phase at a flow rate of 1.5 mL/min,and injection volume of 100 mg.the two compounds were obtained separately with purities of 98.5% and 96.7%,respectively.The chemical structures of the two isolated compounds were identified by UV-VIS、ESI-MS/MS and NMR.Compound 1 was identified as peonidin 3-O-{6-O-（E）-caffeyl-2-O-[6-O-（E）-p-hydroxybenzoy-β-D-glucopyranoside]-β-D-glucopyranoside}-[5-O-（β-D-glucopyranoside）] and Compound 2 was identified as peonidin3-O-{6-O-（E）-caffeyl-2-O-[6-O-（E）-ferulyl-β-D-glucopyranoside]-β-D-glucopyranoside}-[5-O-（β-D-glucopyranoside）].63 mg of Compound 1 and 48 mg of Compound 2 were obtained from 450 g of purple sweet potato.In conclusion,counter-current chromatography was shown to be an efficient,stable and reliable technique for the isolation of anthocyanins from purple sweet potato.

关 键 词：紫甘薯 花色苷 高速逆流色谱 制备分离 

分 类 号：TQ461[化学工程—制药化工]