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An Efficient Method for the Preparative Isolation and Purification of Flavonoids from Leaves of Crataegus pinnatifida by HSCCC and Pre-HPLC.
Molecules. 2017 May 09; 22(5)M

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.

Authors+Show Affiliations

College of Pharmacy, Shandong University of Traditional Chinese Medicine, 4655 Daxue Road, Jinan 250355, China. 18363081657@163.com.Shandong Key Laboratory of TCM Quality Control Technology, Shandong Analysis and Test Center, Shandong Academy of Sciences, 19 Keyuan Street, Jinan 250014, China. wodekafei@126.com.Shandong Key Laboratory of TCM Quality Control Technology, Shandong Analysis and Test Center, Shandong Academy of Sciences, 19 Keyuan Street, Jinan 250014, China. lvrm@sdatc.com.cn.Shandong Key Laboratory of TCM Quality Control Technology, Shandong Analysis and Test Center, Shandong Academy of Sciences, 19 Keyuan Street, Jinan 250014, China. yanhuijiao01@163.com.Shandong Key Laboratory of TCM Quality Control Technology, Shandong Analysis and Test Center, Shandong Academy of Sciences, 19 Keyuan Street, Jinan 250014, China. yujinqian87528@126.com.Shandong Key Laboratory of TCM Quality Control Technology, Shandong Analysis and Test Center, Shandong Academy of Sciences, 19 Keyuan Street, Jinan 250014, China. hqzhao2007@163.com.Shandong Key Laboratory of TCM Quality Control Technology, Shandong Analysis and Test Center, Shandong Academy of Sciences, 19 Keyuan Street, Jinan 250014, China. wxjn1998@126.com.Shandong Key Laboratory of TCM Quality Control Technology, Shandong Analysis and Test Center, Shandong Academy of Sciences, 19 Keyuan Street, Jinan 250014, China. wangdaijie@126.com.

Pub Type(s)

Journal Article

Language

eng

PubMed ID

28486427

Citation

Wen, Lei, et al. "An Efficient Method for the Preparative Isolation and Purification of Flavonoids From Leaves of Crataegus Pinnatifida By HSCCC and Pre-HPLC." Molecules (Basel, Switzerland), vol. 22, no. 5, 2017.
Wen L, Lin Y, Lv R, et al. An Efficient Method for the Preparative Isolation and Purification of Flavonoids from Leaves of Crataegus pinnatifida by HSCCC and Pre-HPLC. Molecules. 2017;22(5).
Wen, L., Lin, Y., Lv, R., Yan, H., Yu, J., Zhao, H., Wang, X., & Wang, D. (2017). An Efficient Method for the Preparative Isolation and Purification of Flavonoids from Leaves of Crataegus pinnatifida by HSCCC and Pre-HPLC. Molecules (Basel, Switzerland), 22(5). https://doi.org/10.3390/molecules22050767
Wen L, et al. An Efficient Method for the Preparative Isolation and Purification of Flavonoids From Leaves of Crataegus Pinnatifida By HSCCC and Pre-HPLC. Molecules. 2017 May 9;22(5) PubMed PMID: 28486427.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - An Efficient Method for the Preparative Isolation and Purification of Flavonoids from Leaves of Crataegus pinnatifida by HSCCC and Pre-HPLC. AU - Wen,Lei, AU - Lin,Yunliang, AU - Lv,Ruimin, AU - Yan,Huijiao, AU - Yu,Jinqian, AU - Zhao,Hengqiang, AU - Wang,Xiao, AU - Wang,Daijie, Y1 - 2017/05/09/ PY - 2017/03/08/received PY - 2017/04/24/revised PY - 2017/05/03/accepted PY - 2017/5/10/entrez PY - 2017/5/10/pubmed PY - 2018/2/24/medline KW - Crataegus pinnatifida leaves KW - HSCCC and pre-HPLC combination KW - extrusion mode KW - flavonoids JF - Molecules (Basel, Switzerland) JO - Molecules VL - 22 IS - 5 N2 - 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. SN - 1420-3049 UR - https://www.unboundmedicine.com/medline/citation/28486427/An_Efficient_Method_for_the_Preparative_Isolation_and_Purification_of_Flavonoids_from_Leaves_of_Crataegus_pinnatifida_by_HSCCC_and_Pre_HPLC_ DB - PRIME DP - Unbound Medicine ER -