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大孔树脂 DIAION HP-20 与硅胶柱色谱联用同时从中制备红景天苷和酪醇。

Simultaneous Preparation of Salidroside and -Tyrosol from by DIAION HP-20 Macroporous Resin Chromatography Combined with Silica Gel Chromatography.

机构信息

National Engineering Laboratory for Tree Breeding, College of Biological Sciences and Biotechnology, Beijing Forestry University, Beijing 100083, China.

School of Nature Conservation, Beijing Forestry University, Beijing 100083, China.

出版信息

Molecules. 2018 Jul 2;23(7):1602. doi: 10.3390/molecules23071602.

Abstract

The species have a long history of utilization in traditional medicine and have been considered as a source of adaptation to environmental challenges; salidroside and -tyrosol are the major responsible compounds. Here we propose a novel UPLC-guided two-step method consisting of a DIAION HP-20 adsorption and silica gel column chromatographies, which can simultaneously prepare high purities of salidroside and -tyrosol with noticeable yields from the rhizome of . Results demonstrated that DIAION HP-20 could successfully remove all impurities except crenulatin during a gradient elution with 5⁻20% ethanol, which could achieve an optimal purification of salidroside and -tyrosol with increasing rates of 29.19% and 33.44%, respectively. Furthermore, chloroform was selected as an ideal solvent for separating -tyrosol with salidroside, and thus crenulatin was subsequently applied in the silica gel chromatography, and the separation of salidroside with crenulatin could be achieved using silica gel chromatography with a mixture of chloroform and methanol at a volume ratio of 4:1. High purity rates of 94.17% and 97.29% and overall yields of 39.09% and 43.73% for salidroside and -tyrosol were simultaneously achieved. Our method provides a new way to simultaneously obtain salidroside and -tyrosol from , as well as other related plant species.

摘要

该物种在传统医学中的应用历史悠久,被认为是适应环境挑战的来源;其中,红景天苷和酪醇是主要的活性成分。在这里,我们提出了一种新的 UPLC 引导的两步法,包括 DIAION HP-20 吸附和硅胶柱色谱法,可以从该植物的根茎中同时高纯度制备红景天苷和酪醇,产率可观。结果表明,DIAION HP-20 可以在 5⁻20%乙醇的梯度洗脱过程中成功去除除垂头菊素以外的所有杂质,分别使红景天苷和酪醇的最佳纯化率提高了 29.19%和 33.44%。此外,氯仿被选为分离红景天苷和酪醇的理想溶剂,因此随后将垂头菊素应用于硅胶柱色谱,使用氯仿和甲醇体积比为 4:1 的混合物可以在硅胶柱色谱上实现红景天苷与垂头菊素的分离。红景天苷和酪醇的纯度分别达到 94.17%和 97.29%,总产率分别达到 39.09%和 43.73%。我们的方法为同时从该植物以及其他相关植物物种中获得红景天苷和酪醇提供了一种新途径。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/e577/6100379/b14dc1bd6e8e/molecules-23-01602-g001.jpg

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