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Preparative separation of flavone dimers from Dysosma versipellis by counter‐current chromatography: Trifluoroacetic acid as a solvent system modifier

Yang, Zhi, Guo, Peipei, Han, Rui, Gao, Jin‐Ming
Journal of separation science 2018 v.41 no.18 pp. 3631-3643
countercurrent chromatography, emulsifying, ethyl acetate, flavones, hexane, methanol, screening, solvents, spectral analysis
The separation of natural products is grueling and time‐consuming work with repeated isolations needed to obtain purified compounds. However, using counter‐current chromatography, a unique liquid–liquid partition chromatography, constituents can usually be purified efficiently. During the separation of flavone dimers from Dysosma versipellis (Hance) by counter‐current chromatography, the separation resolution and sample loading was impeded by the emulsification of the sample. By screening, trifluoroacetic acid was selected as the solvent modifier to eliminate the emulsification. Then, a quaternary solvent system of hexane/ethyl acetate/methanol/water (4:6:5:5 v/v/v/v) with trifluoroacetic acid at a low concentration of 0.5% v/v was used to purify the components from D. versipellis. Compared to that without trifluoroacetic acid, the separation resolution as well as the sample loading both increased greatly. In addition, flavone dimers in low concentrations could be enriched and purified at high sample loading. As a result, five podophyllotoxins and 11 flavonoids were purified and characterized by interpretation of spectroscopic data, in which two of eight flavone dimers were new and a known flavone dimer was first separated from this species.