摘要
建立了高速逆流色谱分离川西獐牙菜中3种酮苷元的方法。溶剂系统为V(正己烷)∶V(乙酸乙酯)∶V(甲醇)∶V(水)=5∶5∶6∶4,上相为固定相,下相为流动相,转速为850 r/min,流速为2.5 mL/min,温度为25℃。从川西獐牙菜氯仿萃取部位的酮苷元混合物中制备得到18 mg 1,8二-羟基-3,7-二甲氧基酮(Meth-ylswertianin,Ⅰ),26 mg 1,7-二羟基-3,8-二甲氧基酮(Gentiacaulein,Ⅱ)和14 mg 1羟-基-3,7,8三-甲氧基酮(Decussatin,Ⅲ),纯度均大于98%。采用1H NMR,13C NMR和2D NMR对目标化合物的结构进行了鉴定。
High speed counter-current chromatographic(HSCCC) method was used to purify and separate methylswertianin,gentiacaulein and decussatin from Swertia mussotti Franch.with a two-phase solvent system composed of hexane-ethyl acetate-ethanol-water(5∶5∶6∶4,V/V).The upper phase was used as the stationary phase and the lower phase was used as the mobile phase at a flow rate of 2.5 mL/min.The experimental conditions were controlled at 850 r/min and 25 ℃,and the effluent was detected at 254 nm.The separation producs of methylswertianin,gentiacaulein and decussatin with the purity of over 98% were obtained by high performance liquid chromatography,and identification of their structures was performed by 1H NMR,13C NMR and 2D NMR.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2011年第4期584-587,共4页
Chinese Journal of Analytical Chemistry
基金
国家自然科学基金项目(No.20875099)
中国科学院知识创新工程重要方向项目(No.KSCX2-YW-R-216)资助