期刊
JOURNAL OF SEPARATION SCIENCE
卷 40, 期 3, 页码 804-812出版社
WILEY-V C H VERLAG GMBH
DOI: 10.1002/jssc.201600922
关键词
aqueous two-phase flotation; flavonol glycosides; preparative high-performance liquid chromatography; solanum rostratum Dunal
资金
- National Natural Science Foundation of China (NSFC) [21075007]
- New Century Excellent Talents in University [NCET-110563]
- Beijing Nova Programme Interdisciplinary Cooperation Project [Z161100004916045]
- Central Universities [YS1406]
Aqueous two-phase flotation followed by preparative high-performance liquid chromatography was used to separate four flavonol glycosides from Solanum rostratum Dunal. In the aqueous two-phase flotation section, the effects of sublation solvent, solution pH, (NH4)(2)SO4 concentration in aqueous solution, cosolvent, N-2 flow rate, flotation time, and volumes of the polyethylene glycol phase on the recovery were investigated in detail, and the optimal conditions were selected: 50 wt% polyethylene glycol 1000 ethanol solvent as the flotation solvent, pH 4, 350 g/L of (NH4)(2)SO4 concentration in aqueous phase, 40 mL/min of N-2 flow rate, 30 min of flotation time, 10.0 mL of flotation solvent volume, and two times. After aqueous two-phase flotation concentration, the flotation products were purified by preparative high-performance liquid chromatography. The purities of the final products A and B were 98.1 and 99.0%. Product B was the mixture of three compounds based on the analysis of high-performance liquid chromatography at the temperature of 10 degrees C, while product A was hyperoside after the identification by nuclear magnetic resonance. Astragalin, 3'-O-methylquercetin 3-O-beta-D-galactopyranoside, and 3'-O-methylquercetin 3-O-beta-D-glucopyranoside were obtained with the purity of 93.8, 97.1, and 99.2%, respectively, after the further separation of product B using preparative high-performance liquid chromatography.
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