Method for simultaneously separating four sedum purpureum flavones by employing online two-dimensional serial chromatography technology

A technology of two-dimensional chromatography and rose bengal, applied in the field of two-dimensional chromatography for simultaneous separation of flavonoids from Rhodiola rosea

Inactive Publication Date: 2015-01-14
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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So far, there is no report on the separation of rhodi

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  • Method for simultaneously separating four sedum purpureum flavones by employing online two-dimensional serial chromatography technology

Examples

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Embodiment 1

[0014] (1) On-line extraction and enrichment: after Rhodiola rosea is crushed, add 1.5mol / L 1-ethyl-3-methylimidazolium chloride aqueous solution, and conduct online ultrasonic extraction for 60min at 40°C and 350W ultrasonic power ; While extracting, the extract flowed through the solid-phase extraction column that the polyamide filler was housed on-line, and the extract flow velocity was 1BV (column volume) / h; The lower phase and upper phase of butanol-water are eluted, the elution flow rate is 1BV / h, and the elution volume is 1 column volume and 2 column volumes respectively, and the eluate of the upper phase solvent is collected; the elution of the upper phase The liquid is directly injected into a high-speed countercurrent chromatographic column for separation, the solvent system is ethyl acetate-n-butanol-water, the volume ratio is 4:1:5, the upper phase is fixed, and the lower phase is mobile phase. During the separation process, the flow rate of the mobile phase is 1.5...

Embodiment 2

[0016] On-line extraction and enrichment: after Rhodiola rosea is crushed, add 1.5 mol / L 1-ethyl-3-methylimidazolium bromide aqueous solution, and conduct online ultrasonic extraction for 45 minutes at 25°C and 400W ultrasonic power; At the same time, the extract flowed through the solid-phase extraction column equipped with LX-8 packing on-line, and the flow rate of the extract was 1.5BV / h; Phase and upper phase were eluted, the elution flow rate was 2BV / h, and the elution volumes were 0.5 column volume and 1.5 column volume respectively, and the eluent of the upper phase solvent was collected; the eluent of the upper phase was directly injected into high-speed countercurrent The chromatographic column is used for separation, the solvent system is ethyl acetate-n-butanol-water, the volume ratio is 3:2:5, the upper phase is fixed, and the lower phase is mobile phase. During the separation process, the flow rate of the mobile phase is 1.0ml / min, the rotation speed is 850rpm, an...

Embodiment 3

[0018] (1) On-line extraction and enrichment: after Rhodiola rosea was crushed, 2mol / L 1-butyl-3-methylimidazolium chloride aqueous solution was added, and at 30°C and 450W ultrasonic power, online ultrasonic extraction was performed for 50 minutes; While extracting, the extract flows through the solid-phase extraction column equipped with CT-8 packing on-line, and the flow rate of the extract is 1.5BV / h; after the extraction, the balanced solvent system ethyl acetate-n-butanol- The lower phase and upper phase of water were eluted, the elution flow rate was 1BV / h, and the elution volumes were 1 column volume and 2.5 column volumes respectively, and the eluate of the upper phase solvent was collected; the eluent of the upper phase was directly Inject into a high-speed countercurrent chromatographic column for separation, the solvent system is ethyl acetate-n-butanol-water, the volume ratio is 3.5:1.5:5, the upper phase is fixed, and the lower phase is mobile phase. During the s...

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Abstract

The invention discloses a method for separating and purifying four sedum purpureum flavones by employing online two-dimensional chromatography (liquid chromatography-high-speed counter-current chromatography). The method comprises the following steps: carrying out online ultrasonic extraction and liquid-solid adsorption chromatography enrichment on sedum purpureum flavones through an ionic liquid water solution serving as an extracting agent; carrying out online elution on the enriched sedum purpureum flavones; and then directly carrying out online high-speed counter-current chromatography separation on the eluted sedum purpureum flavones to obtain four flavones monomers of which the purity exceeds 95%. According to the method, through series connection of extraction, column chromatography and high-speed counter-current chromatography, fussy solvent extraction and repeated column chromatography processes are avoided, the separation method is simple, and the separation efficiency and the product purity are high.

Description

technical field [0001] The invention relates to a method for simultaneously separating rhodiola rosea flavonoids by two-dimensional chromatography, which belongs to the field of chemical industry. Background technique [0002] The flavonoids in Rhodiola rosea have anti-oxidation, anti-fatigue, anti-microwave radiation, antibacterial, anti-tumor, liver protection, and regulation of myocardial contraction, etc., showing its application prospects in medicine and functional foods, so the extraction and separation of rose Rhodiola rosea flavonoids are of great significance. [0003] Traditional extraction solvents are mainly organic solvents, which have the disadvantages of being volatile, flammable, toxic and polluting the environment. Recently, room temperature ionic liquids are considered as an environmentally friendly solvent that can replace traditional volatile organic solvents, and some room temperature ionic liquids have begun to be used in the extraction of active compo...

Claims

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Application Information

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IPC IPC(8): C07H17/07C07H1/08B01D15/10
CPCC07H17/07B01D15/10C07H1/08
Inventor 王洪新马朝阳樊琛
Owner JIANGNAN UNIV
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