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Large-scale preparation of two minor polar polyphenols from Phyllanthus emblica Linn. by macroporous resin column chromatography and high temperature preparative high-speed counter-current chromatography.

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In the present study, an efficient strategy for large-scale preparation of two minor polar polyphenols from Phyllanthus emblica L. has been established by macroporous resin column chromatography and high temperature… Click to show full abstract

In the present study, an efficient strategy for large-scale preparation of two minor polar polyphenols from Phyllanthus emblica L. has been established by macroporous resin column chromatography and high temperature preparative high-speed counter-current chromatography. Macroporous resin column chromatography was used for enrichment of the target polyphenols. The target polyphenols could be well enriched in the 10% ethanol fraction and the peak area proportion increased from 2.2% in the crude extract to 85.3% in the 10% ethanol fraction. Then, the 10% ethanol fraction was introduced to preparative high-speed counter-current chromatography for separation using n-butanol-ethyl acetate-water (17:3:20, v/v/v) solvent system. In order to improve the retention of stationary phase, a high temperature preparative high-speed counter-current chromatography had been developed by using 316 L stainless steel pipe as column. A 50°C of column temperature was used and the retention rate of the stationary phase could reach 75%. Finally, 871 mg of compound Ⅰ and 534 mg of compound Ⅱ with purities higher than 98% were obtained from 4 g of the sample. The chemical structures were identified as corilagin and 1, 6-di-O-galloyl-β-D-glucoside by 1 H-NMR and 13 C-NMR. This article is protected by copyright. All rights reserved.

Keywords: high speed; speed counter; counter current; preparative high; column; chromatography

Journal Title: Journal of separation science
Year Published: 2022

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