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Use of pH-Zone Refining Countercurrent Chromatography for Preparative Separation of Fangchinoline and Tetrandrine from Stephania tetrandra

Author:
Lijin, Zhang, Xiao, Wang, Jianhua, Liu, Wenjuan, Duan, Daijie, Wang, Yanling, Geng
Source:
Chromatographia 2009 v.69 no.9-10 pp. 959-962
ISSN:
0009-5893
Subject:
Stephania tetrandra, countercurrent chromatography, electrospray ionization mass spectrometry, hydrochloric acid, nuclear magnetic resonance spectroscopy, petroleum, refining, solvents, triethylamine
Abstract:
pH-Zone-refining countercurrent chromatography with a multilayer coil planet centrifuge has been successfully used for separation of fangchinoline and tetrandrine from crude extracts of Stephania tetrandra. The two target compounds were completely resolved by use of the two-phase solvent system petroleum ether (60-90 °C)-ethyl acetate-methanol-water 5:5:1:9 (v/v), with 10 mm triethylamine in the organic stationary phase and 5 mm hydrochloric acid in the aqueous mobile phase. Separation of 3.5 g sample yielded 126 mg fangchinoline (LC purity >93%) and 249 mg tetrandrine (LC purity >95%). The structures of the compounds were confirmed by use of electrospray ionization mass spectrometry and ¹H NMR.
Agid:
2178426