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pH区带逆流色谱法分离纯化马钱子中马钱子碱和士的宁
引用本文:李嬛,刘晓,蔡皓,徐自升,蔡宝昌. pH区带逆流色谱法分离纯化马钱子中马钱子碱和士的宁[J]. 分析化学, 2010, 38(12). DOI: 10.3724/SP.J.1096.2010.01703
作者姓名:李嬛  刘晓  蔡皓  徐自升  蔡宝昌
作者单位:1. 南京中医药大学药学院,南京,210046;南京中医药大学国家教育部中药炮制规范化及标准化工程研究中心,南京,210029;南京中医药大学江苏省中药炮制重点实验室,南京,210029
2. 南京海昌中药饮片有限公司,南京,210061
3. 南京中医药大学药学院,南京,210046;南京中医药大学国家教育部中药炮制规范化及标准化工程研究中心,南京,210029;南京中医药大学江苏省中药炮制重点实验室,南京,210029;南京海昌中药饮片有限公司,南京,210061
基金项目:科技部“十一五”重大新药创制科技重大专项(No.2009ZX09103-342)资助项目
摘    要: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。

关 键 词:pH区带逆流色谱法  马钱子  马钱子碱  士的宁  

Separation and Purification of Brucine and Strychnine from Strychnos Nux-vomica L.by pH-Zone-Refining Counter-Current Chromatography
LI Huan,LIU Xiao,CAI Hao,XU Zi-Sheng,CAI Bao-Chang. Separation and Purification of Brucine and Strychnine from Strychnos Nux-vomica L.by pH-Zone-Refining Counter-Current Chromatography[J]. Chinese Journal of Analytical Chemistry, 2010, 38(12). DOI: 10.3724/SP.J.1096.2010.01703
Authors:LI Huan  LIU Xiao  CAI Hao  XU Zi-Sheng  CAI Bao-Chang
Affiliation:LI Huan1,2,3,LIU Xiao* 1,CAI Hao1,XU Zi-Sheng4,CAI Bao-Chang* 1,4 1(College of Pharmacy,Nanjing University of Chinese Medicine,Nanjing 210046) 2(Engineering Center of State Ministry of Education for Standardization of Chinese Medicine Processing,Nanjing 210029) 3(Jiangsu Key Laboratory of Chinese Medicine Processing,Nanjing 210029) 4(Nanjing Haichang Chinese Medicine Yinpian Co.,Ltd,Nanjing 210061)
Abstract: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 ...
Keywords:pH-Zone-refining counter-current chromatography  Strychnos nux-vomica L.  Brucine  Strychnine  
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