A strategy based on isocratic and linear-gradient high-speed counter-current chromatography for the comprehensive separation of platycosides from Platycodi radix,Analytical Methods

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A strategy based on isocratic and linear-gradient high-speed counter-current chromatography for the comprehensive separation of platycosides from Platycodi radix
Analytical Methods ( IF 2.7 ) Pub Date : 2021-1-7 , DOI: 10.1039/d0ay02029j
Jinqian Yu _{1,

2,

3,

4} , Xiangwei Chang _{4,

5,

6,

7,

8} , Huasheng Peng _{4,

5,

6,

7} , Xiao Wang _{1,

2,

3,

4} , Jutao Wang _{4,

5,

6,

7} , Daiyin Peng _{4,

5,

6,

7} , Shuangying Gui _{4,

5,

6,

7,

9}

Affiliation

Platycosides, the generally recognized main active constituents of Platycodi radix, have been studied extensively for their wide pharmacological activities. Herein, we have successfully developed an efficient method for the enrichment and comprehensive isolation of platycosides from Platycodi radix by MCI resin column chromatography (CC) and two different modes of high-speed counter-current chromatography (HSCCC). MCI resin CC was the preferable enrichment operation for platycosides from the 70%-ethanol extract of Platycodi radix and rendered target platycosides when eluted by 60% aqueous methanol solution. As for the separation, two different modes, including isocratic HSCCC and linear-gradient HSCCC, were applied together to separate the platycosides using a mixture of ethyl acetate, n-butanol and water coupled with evaporative light scattering detection, for the first time. Isocratic HSCCC was applied to separate crude platycosides from Platycodi radix using ethyl acetate–n-butanol–water (1 : 1 : 2, v/v), yielding seven pure platycosides (compounds 1–6, 8) and two fractions of enriched mixtures of compounds 7, 9, 10, and 11. Linear-gradient HSCCC was employed to rapidly separate compounds 7, 9, 10, and 11 by constantly changing the proportions of ethyl acetate and n-butanol in the ethyl acetate–n-butanol–water solvent system. Finally, platycoside E (1), deapio-platycodin D₃ (2), platycodin D₃ (3), deapio-platycodin D₂ (4), platycodin D₂ (5), platycodin D (6), polygalacin D₂ (7), polygalacin D (8), and three tautomers, namely 2′′-O-acetylplatycodin D (9) and 3′′-O-acetylplatycodin D (9′), 2′′-O-acetylpolygalacin D₂ (10) and 3′′-O-acetylpolygalacin D₂ (10′), and 2′′-O-acetylpolygalacin D (11) and 3′′-O-acetylpolygalacin D (11′), were obtained from 300 mg of crude platycosides from Platycodi radix.

中文翻译：

基于等度和线性梯度高速逆流色谱的一种策略，用于从桔梗中综合分离板状苷

桔梗是常见的桔梗主要活性成分，由于其广泛的药理活性已被广泛研究。在这里，我们已经成功地开发了一种有效的方法，可通过MCI树脂柱色谱法（CC）和两种不同模式的高速逆流色谱法（HSCCC）从Platycodi根中富集和广泛分离板状苷。当用60％甲醇水溶液洗脱时，MCI树脂CC是从Platycodi根的70％乙醇提取物中提取的板状苷的最佳浓缩操作，并提供了目标板状苷。作为分离，两种不同的模式，包括无梯度HSCCC和线性梯度HSCCC，施加一起使用乙酸乙酯的混合物中分离platycosides，Ñ-丁醇和水首次结合蒸发光散射检测。等度HSCCC法分离从桔梗粗platycosides使用乙酸乙酯-基数Ñ丁醇-水（1：1：2，V / V），得到7个纯platycosides（化合物1-6，8）和富集的混合物的两种级分的化合物7，9，10，和11。线性梯度HSCCC物采用迅速分开的化合物7，9，10，和11通过不断变化的乙酸乙酯和比例Ñ丁醇在乙酸乙酯- Ñ-丁醇-水溶剂体系。最后，桔梗甙E（1），葡糖苷D ₃（2），桔素D ₃（3），桔皮素D ₂（4），桔素D ₂（5），桔素D（6），聚半乳聚糖D ₂（7），聚半乳聚糖D（8）和三个互变异构体，即2''- O-乙酰基铂霉素D（9）和3''- O-乙酰基铂霉素D（9'），2''- O-乙酰基聚半乳糖D ₂（10）和3''- O-乙酰基聚半乳糖D ₂（10'）和2''- O-乙酰基聚半乳糖D（11）和3''- O-乙酰基聚半乳糖D（11'）由300毫克粗桔梗获得。来自Platycodi radix。

更新日期：2021-01-18

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