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采用聚酰胺和 MCI GEL® CHP20P 作为中压色谱固定相,从虎耳草科落新妇属植物大花溲疏中大规模制备性分离分离甘草素标准品。

Large-scale preparative isolation of bergenin standard substance from Saxifraga atrata using polyamide coupled with MCI GEL® CHP20P as stationary phases in medium pressure chromatography.

机构信息

Qinghai Provincial Key Laboratory of Tibetan Medicine Research, Key Laboratory of Tibetan Medicine Research, Northwest Institute of Plateau Biology, Chinese Academy of Sciences, Xining 810001, Qinghai, China.

Qinghai Provincial Key Laboratory of Tibet Plateau Biodiversity Formation Mechanism and Comprehensive Utilization, College of Life Sciences, Qinghai Normal University, Xining 810008, Qinghai, China.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2021 Apr 30;1170:122617. doi: 10.1016/j.jchromb.2021.122617. Epub 2021 Mar 5.

DOI:10.1016/j.jchromb.2021.122617
PMID:33713947
Abstract

In this study, polyamide and MCI GEL® CHP20P were employed as stationary phases in medium pressure chromatography (MPC) for the efficient preparative separation of bergenin from Saxifraga atrata. Ethanol-water, methanol-water, and acetonitrile-water mobile phases all showed good enrichment capacity for bergenin fraction when polyamide was used as a stationary phase. After 5 cycles of polyamide MPC using acetonitrile/water, 1.2 g of bergenin fraction was isolated from 180 g Saxifraga atrata herb. Further purification of this fraction was conducted using MCI GEL® CHP20P styrene-divinylbenzene beads. The bergenin fraction was separated into two fractions, and after three runs of MPC, 714.2 mg of bergenin with purity above 99% was obtained. The results demonstrate that the combination of polyamide and styrene-divinylbenzene MPC can be utilized for preparative isolation of compounds from natural products with high yield and purity.

摘要

在这项研究中,聚酰胺和 MCI GEL® CHP20P 被用作中压色谱(MPC)的固定相,以从虎耳草中高效制备分离山柰酚。当聚酰胺用作固定相时,乙醇-水、甲醇-水和乙腈-水流动相均显示出对山柰酚部分良好的富集能力。使用乙腈/水进行 5 次聚酰胺 MPC 循环后,从 180g 虎耳草中分离出 1.2g 的山柰酚部分。进一步使用 MCI GEL® CHP20P 苯乙烯-二乙烯基苯珠对该部分进行纯化。山柰酚部分被分离成两个部分,经过三次 MPC 运行,获得了 714.2mg 纯度超过 99%的山柰酚。结果表明,聚酰胺和苯乙烯-二乙烯基苯 MPC 的组合可用于从天然产物中以高产率和高纯度制备分离化合物。

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