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Molecules 2017, 22(5), 767; doi:10.3390/molecules22050767

An Efficient Method for the Preparative Isolation and Purification of Flavonoids from Leaves of Crataegus pinnatifida by HSCCC and Pre-HPLC

1
College of Pharmacy, Shandong University of Traditional Chinese Medicine, 4655 Daxue Road, Jinan 250355, China
2
Shandong Key Laboratory of TCM Quality Control Technology, Shandong Analysis and Test Center, Shandong Academy of Sciences, 19 Keyuan Street, Jinan 250014, China
*
Author to whom correspondence should be addressed.
Academic Editor: Stefan Berger
Received: 8 March 2017 / Revised: 24 April 2017 / Accepted: 3 May 2017 / Published: 9 May 2017
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Abstract

In this work, flavonoid fraction from the leaves of Crataegus pinnatifida was separated into its seven main constituents using a combination of HSCCC coupled with pre-HPLC. In the first step, the total flavonoid extract was subjected to HSCCC with a two-solvent system of chloroform/methanol/water/n-butanol (4:3:2:1.5, v/v), yielding four pure compounds, namely (–)-epicatechin (1), quercetin-3-O-(2,6-di-α-l-rhamnopyranosyl)-β-d-galactopyranoside (2), 4′′-O-glucosylvitexin (3) and 2′′-O-rhamnosylvitexin (4) as well as a mixture of three further flavonoids. An extrusion mode was used to rapidly separate quercetin-3-O-(2,6-di-α-l-rhamnopyranosyl)-β-d-galactopyranoside with a big KD-value. In the second step, the mixture that resulted from HSCCC was separated by pre-HPLC, resulting in three pure compounds including: vitexin (5), hyperoside (6) and isoquercitrin (7). The purities of the isolated compounds were established to be over 98%, as determined by HPLC. The structures of these seven flavonoids were elucidated by ESI-MS and NMR spectroscopic analyses. View Full-Text
Keywords: Crataegus pinnatifida leaves; flavonoids; HSCCC and pre-HPLC combination; extrusion mode Crataegus pinnatifida leaves; flavonoids; HSCCC and pre-HPLC combination; extrusion mode
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This is an open access article distributed under the Creative Commons Attribution License which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited. (CC BY 4.0).

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MDPI and ACS Style

Wen, L.; Lin, Y.; Lv, R.; Yan, H.; Yu, J.; Zhao, H.; Wang, X.; Wang, D. An Efficient Method for the Preparative Isolation and Purification of Flavonoids from Leaves of Crataegus pinnatifida by HSCCC and Pre-HPLC. Molecules 2017, 22, 767.

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