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高速逆流色谱(盐溶液体系)分离制备白芍中的芍药苷
引用本文:刘浩,;杭伟,;周晓晶,;陈义伦,;王晓,;段文娟. 高速逆流色谱(盐溶液体系)分离制备白芍中的芍药苷[J]. 山东科学, 2014, 27(3): 12-16. DOI: 10.3976/j.issn.1002-4026.2014.03.003
作者姓名:刘浩,  杭伟,  周晓晶,  陈义伦,  王晓,  段文娟
作者单位:1. 山东农业大学食品科学与工程学院,山东 泰安 271018;2. 山东省科学院中药过程控制研究中心,山东省分析测试中心,山东 济南 250014;3. 北京理化分析测试中心, 北京 100089
基金项目:山东省自然科学基金(ZR2013HM075);北京市科学技术研究院市级财政项目(PXM2013_178305_000009)
摘    要:建立应用高速逆流色谱分离纯化芍药中的芍药苷的方法。以正丁醇-乙酸乙酯-5%Na2SO4(4:1:5,V/V)为两相溶剂体系,在流速为2.0 mL/min、主机转速为800 r/min、检测波长为254 nm的条件下进行分离,从100 mg芍药粗提物中一次性分离制备得到56.13 mg芍药苷,高效液相色谱分析其纯度在98%以上,通过质谱、核磁共振氢谱和核磁共振碳谱鉴定化合物的结构。该方法简便、快捷且重现性好,适合芍药苷的制备型分离。

关 键 词:芍药  高速逆流色谱  Na2SO4溶液  芍药苷  
收稿时间:2013-12-25

Separation and preparation of paeoniflorin from Paeonia lactiflora Pall.by HSCCC with salt solution system
LIU Hao,HANG Wei,ZHOU Xiao-Jing,CHEN Yi-Lun,WANG Xiao,DUAN Wen-Juan. Separation and preparation of paeoniflorin from Paeonia lactiflora Pall.by HSCCC with salt solution system[J]. Shandong Science, 2014, 27(3): 12-16. DOI: 10.3976/j.issn.1002-4026.2014.03.003
Authors:LIU Hao  HANG Wei  ZHOU Xiao-Jing  CHEN Yi-Lun  WANG Xiao  DUAN Wen-Juan
Affiliation:1. School of Food Science and Engineering, Shandong Agriculture University, Taian 271018, China;2. Process Control Research Center of Traditional Chinese Medicine, Shandong Analysis and Test Center, Jinan 250014, China;3. Beijing Center for Physical and Chemical Analysis, Beijing 100089, China
Abstract:We established a method of separation and preparation of paeoniflorin from Paeonia lactiflora Pall.by highspeed counter current chromatography (HSCCC) with salt solution system.The separation was performed with butanolethyl acetate-5% Na2SO4 (aq) (4∶1∶5,V/V) as a two-phase solvent system,flow rate of 2.0 mL/min,rotation number of 800 r/min and detection wavelength of 254 nm.We obtained paeoniflorin of 56.13 mg from the crude extracts of 100 mg at one time.Its purity was more than 98%,which was determined by high performance liquid chromatography(HPLC).The structure of the target compound was identified by electrospray ionisation mass spectrometry (ESI-MS),1H-nuclear magnetic resonance (1H-NMR) and 13C-nuclear magnetic resonance (13C-NMR).The method is simple and reproducible and suitable for separation and preparation of paeoniflorin.
Keywords:Paeonia lactiflora Pall.  HSCCC  Na2SO4 (aq)  paeoniflorin
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