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采用 Click 寡聚(乙二醇)和 C18 柱二维制备色谱法从降香黄檀中分离化合物。

Purification of compounds from Lignum Dalbergia Odorifera using two-dimensional preparative chromatography with Click oligo (ethylene glycol) and C18 column.

机构信息

Dalian Institute of Chemical Physics, Graduate School of the Chinese Academy of Sciences, Chinese Academy of Sciences, Dalian, PR China.

出版信息

J Sep Sci. 2011 Feb;34(3):299-307. doi: 10.1002/jssc.201000609. Epub 2011 Jan 7.

Abstract

Purification of compounds from traditional Chinese medicines (TCMs) is an important task for understanding the chemical composition of TCMs. However, it is difficult to obtain compounds with high enough purity for identification by NMR due to the complexity of TCMs in chemical composition. In this study, a two-dimensional purification method based on a Click oligo (ethylene glycol) column and a C18 column was developed to realize an orthogonal separation in preparative level for purifying compounds efficiently. The first dimensional preparation was performed on a Click oligo (ethylene glycol) column to simplify the sample into the fractions with good separation repeatability. On the first dimension, 7.2 g sample was separated into 11 fractions with a recovery of 86% within 6 h. A C18 column was taken as the second dimension to realize the high-performance separation and rapid preparation from the fractions collected from the first dimension. Eight compounds in fraction 6 and 2 compounds in fraction 8 were isolated and identified after optimizing the separation and collection parameters. This method is a high-efficient and orthogonal preparation method to improve the separation of a complex sample and increase the purity of the compounds, which benefits from the application of novel materials in the preparation and purification.

摘要

从中药(TCM)中分离化合物是了解 TCM 化学成分的重要任务。然而,由于 TCM 在化学成分上的复杂性,很难获得纯度足够高的化合物进行 NMR 鉴定。在这项研究中,开发了一种基于 Click 寡聚(乙二醇)柱和 C18 柱的二维纯化方法,以在制备水平上实现正交分离,从而有效地纯化化合物。首先在 Click 寡聚(乙二醇)柱上进行一维制备,将样品简化为具有良好分离重复性的馏分。在第一维中,7.2g 样品在 6 小时内分离成 11 个馏分,回收率为 86%。然后采用 C18 柱作为第二维,从第一维收集的馏分中实现高效分离和快速制备。在优化分离和收集参数后,从馏分 6 中分离出 8 种化合物,从馏分 8 中分离出 2 种化合物,并对其进行了鉴定。该方法是一种高效的正交制备方法,可改善复杂样品的分离效果,提高化合物的纯度,这得益于新型材料在制备和纯化中的应用。

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