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An efficient procedure for preparing main acylated pentasaccharides from Polygalae Radix using integrated extraction-adsorption method followed by semi-preparative high performance liquid chromatography

机译:集成萃取-吸附法然后半制备高效液相色谱法从远志制备主要酰化五糖的有效方法

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In the present study, an efficient preparative procedure was developed for the preparation of three main acylated pentasaccharides from Polygalae Radix using integrated extraction-adsorption method followed by semi-preparative high performance liquid chromatography. Firstly, the acylated pentasaccharides were simultaneously extracted and purified by column chromatographic extraction integrated with macroporous resin purification. Comparing this integrated process to conventional one, some obvious advantages were observed, namely more than 38.9% enhancement of the recovery of acylated pentasaccharides, about 49.4% and 50.4% reduction in water and ethanol consumption, respectively. And then, the obtained extracts were further purified by semi-preparative high performance liquid chromatography. Finally, three known acylated pentasaccharides were purified from 100 g of Polygalae Radix, including tenuifoliose I (13 mg), tenuifoliose H (15 mg), and tenuifoliose A (21 mg). The purities of the compounds were determined by high performance liquid chromatography and the chemical structures were confirmed by mass spectrometric and NMR analysis. (C) 2015 Elsevier B.V. All rights reserved.
机译:在本研究中,开发了一种有效的制备方法,该方法使用集成萃取-吸附法,然后用半制备高效液相色谱法,从远志制备三种主要的酰化五糖。首先,通过柱色谱萃取与大孔树脂纯化相结合,同时提取和纯化酰化的五糖。与传统方法相比,该方法具有明显的优势,即酰化五糖的回收率提高了38.9%以上,水和乙醇的消耗量分别降低了约49.4%和50.4%。然后,将获得的提取物通过半制备高效液相色谱进一步纯化。最后,从100克的远志中纯化了三种已知的酰化五糖,其中包括tenuifoliose I(13 mg),tenuifoliose H(15 mg)和tenuifoliose A(21 mg)。通过高效液相色谱法测定化合物的纯度,并通过质谱和NMR分析确认化学结构。 (C)2015 Elsevier B.V.保留所有权利。

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