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。
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.
出处
《山东科学》
CAS
2014年第3期12-16,共5页
Shandong Science
基金
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)