pH区带逆流色谱法分离纯化马钱子中马钱子碱和士的宁

Separation and Purification of Brucine and Strychnine from Strychnos Nux-vomica L.by pH-Zone-Refining Counter-Current Chromatography

建立了pH区带逆流色谱分离制备马钱子中生物碱类成分马钱子碱和士的宁的方法。溶剂系统为V(甲基叔丁基醚):V(乙腈):V(水)=2:2:3,静置分层后,上相加入三乙胺,使其浓度为10mmol/L,作为固定相;下相加入HCl,使其浓度为10mmol/L,作为流动相。从308mg马钱子总生物碱中分离得到50mg马钱子碱和120mg士的宁,得率分别为72.8%和85.1%;纯度分别为96.8%和98.3%。并采用LC-ESI-MS和13CNMR对目标化合物的结构进行了鉴定。

pH-zone-refining counter-current chromatography method was successfully applied to separate and purify brucine and strychnine from Strychnos nux-vomica L.,a traditional Chinese herb,with a solvent system composed of methyl tertiary butyl ether-acetonitrile-water(2:2:3,V/V).The lower phase of the system was used as the mobile phase,and the upper phase,as the stationary phase.Triethylamine was added to the upper phase to reach a concentration of 10 mmol/L,while the lower phase was acidified with hydrochloric acid at the same concentration.From 308 mg of total alkaloid-of Strychnos nux-vomica L.,the separation produced 50 mg brucine and 120 mg strychnine with the purity of 96.8% and 98.3% respectively,determined by HPLC.The yields of the method were 72.8% and 85.1% for brucine and strychnine respectively.The structures of isolated compounds were identified by LC-ESI-MS and 13C NMR.