Gradual Gradient Two-Dimensional Preparative Liquid Chromatography System for Preparative Separation of Complex Natural Products

Gradual Gradient Two-Dimensional Preparative Liquid Chromatography System for Preparative Separation of Complex Natural Products
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用于制备分离复杂天然产物的渐进梯度二维制备液相色谱系统

DOI:
10.1007/s10337-018-3652-8
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发表时间:
2018-11
期刊:
影响因子:
1.7
通讯作者:
Qiu Ying Kun
Qiu Ying Kun
中科院分区:
化学4区
文献类型:
--
作者:
Wang Zheng;Xie Ting Ting;Yan Xia;Xue Shi;Chen Jing Wei;Wu Zhen;Qiu Ying Kun

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为了从复杂的天然产物中制备分离感兴趣的化合物,开发了一种低成本、渐变梯度的在线二维制备液相色谱系统。第一维度采用中压液相色谱(MPLC),第二维度采用制备型高效液相色谱(HPLC)。还使用了两个捕捉柱和一个化妆泵。二维柱以反相十八烷基硅胶(Ods)为填充物,用带有梯度混合装置的等度泵洗脱,其中一、二维溶剂按样品洗脱要求进行渐变。通过对中华大蟾蜍毒液甲醇粗提物的克级分离,评价了该 × 制备高效液相系统的仪器操作和性能。结果表明,在一次345min的2D分离中,从0.5 mg粗提物中分离出18个二烯内酯(1-18),各化合物的纯度均大于90%。我们预计,这种改进的低成本制备2D-LC系统在同时分离和纯化其他复杂样品基质中的多种成分方面具有广泛的应用前景。
A low-cost and gradual gradient online two-dimensional preparative liquid chromatography system was developed for the preparative separation of compounds of interest from complex natural products. Medium-pressure liquid chromatography (MPLC) was applied as the first dimension and preparative high-performance liquid chromatography (HPLC) was employed as the second dimension. Two trapping columns and a makeup pump were also used. Each of the two dimension columns was packed with reversed-phase ostadecyl-silca (ODS), and eluted by an isocratic pump with a gradient mixing device, in which the solvent of the first and the second dimensions were gradiently changed to fit the demand of the sample elution. The instrument operation and the performance of this MPLC × preparative HPLC system were evaluated via gram-scale isolation of a crude methanol extract of toad venom fromBufo bufo gargarizans. As a result, in a single 2D separation run (345 min), 18 bufadienolides (1–18) were isolated from 0.5 g crude extract, and the purity of each compound was higher than 90%. We anticipate that this improved low-cost preparative 2D-LC system has broad applications for the simultaneous isolation and purification of multiple components from other complex sample matrices.
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发表时间: 2015-09
影响因子: 6.2
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DOI: 10.1016/j.aca.2014.02.023
发表时间: 2014-04-11
影响因子: 6.2
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发表时间: 2011-01
影响因子: 1.7
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发表时间: 2015-07
期刊: Journal of chromatography. A
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