Shandong Science ›› 2015, Vol. 28 ›› Issue (1): 1-6.doi: 10.3976/j.issn.1002-4026.2015.01.001

• Traditional Chinese medicine and natural active products •     Next Articles

Separation and preparation of the chemical components of Rheum officinale Baill.by pH-zone-refining counter-current chromatography and HSCCC

WU Qiu-xia,SUN Chang-lei,WANG Xiao,ZHOU Jie,ZHENG Zhen-jia,YANG Bing-tian,SUN Wei-hong   

  1. 1. School of Food and Biology Engineering,Jiangsu University,Zhenjiang 212013,China; 2.Shandong Analysis and Test Center, Shandong Academy of Sciences, Jinan 250014,China; 3.Jinan Sanfeng Biological Engineering Technology Co. Ltd., Jinan 250014, China
  • Received:2014-10-13 Published:2015-02-20 Online:2015-02-20

Abstract: We employed pH-zone-refining counter-current chromatography(pH-ZRCCC)and conventional high-speed counter-current chromatography (HSCCC) to separate and prepare the chemical components in the crude extracts of Rheum officinale Baill.We initially used pH-ZRCCC to separate the crude extracts of Rheum officinale Baill.with petroleum ether-ethyl acetate-methanol-water(3:7:4:6,V/V) as a binary phase solvent system.Trifluoroacetic acid of 10 mmol/L was added to the upper organicstationary phase as a retainer and NaOH of 15 mmol/L was added to the aqueous mobile phase as an eluter.We acquired cinnamic acid (purity of 96.1%)of 140 mg, rhein(purity of 92.5%) of 130 mg and residue of 560 mg from crude extracts of 1.3 g. We further applied conventional HSCCC to the separation of the residue of 260 mg with petroleum ether-ethyl acetate-methanol-water (7:3:7:4,V/V) as a binary phase solvent system, and obtained aboutemodin (purity of 96.5%)of 98 mg and aloeemodin (purity of 96.5%) of 60 mg. We employed HPLC to detect the purity and ESI-MS and1HNMR to identify those structures. Results show that the combination of pH-ZRCCC and HSCCC is an effective method for the separation of chemical compounds from Rheum officinale Baill.

Key words: pH-zone-refining counter-current chromatography, HSCCC, Rheum officinale Baill., rhein, emodin, aloeemodin

CLC Number: 

  • R284.2

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