Relayed chromatography - Countercurrent chromatography in series with liquid chromatography for the separation of natural products

化学 色谱法 逆流色谱法 水相正相色谱法 色谱柱 亲水作用色谱法 超临界流体色谱法 高效液相色谱法 逆流分布
作者
Jiao Huang,Jianming He,Qing Mu
出处
期刊:Journal of Chromatography A [Elsevier BV]
卷期号:1676: 463205-463205 被引量:10
标识
DOI:10.1016/j.chroma.2022.463205
摘要

Chromatography is an essential method for separating natural products. In this study, we proposed the concept of 'relayed chromatography', based on the strategy of combining different chromatography with relayed resolution by in-situ concentration technique. The following chromatographic methods were used: high-speed countercurrent chromatography (HSCCC), silica gel liquid chromatography (silica gel LC), and reverse phase liquid chromatography (reverse phase LC). The proposed strategy was effectively applied to the preparative separation of naturally existing naphthaquinones. After the first separation stage (silica gel LC), acetylalkannin (1) was directly collected, while fractions 1, 4 and 5 were collected and respectively subjected to recycling CCC separation after concentration. Thus, deoxyshikonin (2), 8-O-methyl-11-O-acetylshikonin (6), β-acetoxyisovalerylalkannin (7) and alkannin (8) were collected. Fraction 2 was concentrated and injected in reverse phase LC separation. After collection of isobutyrylalkannin (3), the remaining effluent from reverse phase LC retained the peak resolution (R4,5=0.45) and was injected into a recycling CCC elution. Finally, β, β-dimethylacrylalkannin (4), and isovalerylalkannin (5) were collected with sufficient resolution (R4,5=1.25). Eight naturally occurring naphthaquinones were thus isolated from Arnebia euchroma. The purities of all the compounds were determined by HPLC to be > 90%, and the chemical structures were determined by spectral method. Among the aforementioned compounds, 8-O-methyl-11-O-acetylshikonin (6) was separated as a new compound from A. euchroma. In conclusion, the relayed strategy that retains the resolution of the previous chromatographic stage can improve CCC separation efficiency, which may expand the range of application of CCC combined with different chromatography to the separation of natural products.
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