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A method for separating and purifying emodin methyl ether and emodin from Polygonum cuspidatum

A technology for the separation and purification of emodin methyl ether and emodin, which is applied in the field of separation and purification of emodin methyl ether and emodin, can solve the problems of high organic solvent recovery cost, difficulty in expanding the separation scale, and difficulty in solvent system selection, achieving short process cycle, Ease of automatic control and simple operation

Inactive Publication Date: 2016-08-24
LIAOCHENG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the process is mature, the operation is cumbersome, the choice of solvent system in high-speed countercurrent chromatography is difficult, and the separation scale is difficult to expand
In addition, the macroporous resin separation and purification method and the high-speed countercurrent chromatography method both need to consume a large amount of organic solvents, the cost of organic solvent recovery is high, the recovery and reuse are difficult, and the organic reagent residue in the product is serious

Method used

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  • A method for separating and purifying emodin methyl ether and emodin from Polygonum cuspidatum
  • A method for separating and purifying emodin methyl ether and emodin from Polygonum cuspidatum

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Weigh 100 grams of Polygonum cuspidatum, pulverize with a pulverizer, put it into a glass container, add 500ml of absolute ethanol to cold soak for 12 hours, extract 3 times, filter the extract, concentrate under reduced pressure to obtain an extract, and disperse the extract in 460 In ml methanol-water-ethyl acetate-petroleum ether mixture, extract 3 times according to the ratio of methanol:water:ethyl acetate:petroleum ether=6:10:5:2 (V / V). The upper phases were combined, and the upper phase was recovered by vacuum distillation to obtain Polygonum cuspidatum extract.

[0026] The Polygonum cuspidatum extract is dissolved in methanol, filtered (the filter membrane used is 0.45μm), and then subjected to supercritical fluid chromatography. The column is a glycol-based column and the column temperature is 40°C. The mobile phase is supercritical carbon dioxide, the flow rate is 3 times the column volume / min, and the pressure is 10 MPa. The improver is methanol with a ratio o...

Embodiment 2

[0029] Weigh 100 grams of Polygonum cuspidatum, pulverize with a pulverizer, put it in a glass container, add 600ml of absolute ethanol to cold soak for 24 hours, extract 3 times, filter the extract and concentrate under reduced pressure to obtain an extract, and disperse the extract in 690 In ml methanol-water-ethyl acetate-petroleum ether mixture, extract 3 times according to the ratio of methanol:water:ethyl acetate:petroleum ether=6:10:5:2 (V / V). The upper phases were combined, and the upper phase was recovered by vacuum distillation to obtain Polygonum cuspidatum extract.

[0030] Polygonum cuspidatum extract is dissolved in methanol, filtered, and then subjected to supercritical fluid chromatography. The chromatographic column is a glycol-based chromatographic column and the temperature of the chromatographic column is 45°C. The mobile phase is supercritical carbon dioxide, the flow rate is 5 times the column volume / min, and the pressure is 12 MPa. The improver is methanol...

Embodiment 3

[0032] Weigh 100 grams of Polygonum cuspidatum, pulverize with a pulverizer, put it into a glass container, add 300ml of absolute ethanol to cold soak for 16 hours, extract 3 times, filter the extract, concentrate under reduced pressure to obtain an extract, and disperse the extract in 230 In ml methanol-water-ethyl acetate-petroleum ether mixture, extract 3 times according to the ratio of methanol:water:ethyl acetate:petroleum ether=6:10:5:2 (V / V). The upper phases were combined, and the upper phase was recovered by vacuum distillation to obtain Polygonum cuspidatum extract.

[0033] Polygonum cuspidatum extract is dissolved in methanol, filtered, and then subjected to supercritical fluid chromatography. The chromatographic column is a glycol-based chromatographic column, and the temperature of the chromatographic column is 40°C. The mobile phase is supercritical carbon dioxide, the flow rate is 4 times the column volume / min, and the pressure is 13 MPa. The improver is methanol...

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Abstract

The invention belongs to the field of chemical and pharmaceutical, and relates to a method for separating purified physcion and emodin from giant knot weed extract. Giant knot weed is crushed, added into absolute ethyl alcohol and extracted in a cold-soaked manner, extracting solution is filtered, depressurized and concentrated to obtain extract, the extract is dissolved in mixed solution of methanol, water, ethyl acetate and petroleum ether with the ratio of 6:10:5:2 (V / V) and extracted, top phases are combined, and reduced pressure distillation is performed to obtain the giant knot weed extract. The giant knot weed extract is dissolved by the methanol, filtered and then separated by supercritical fluid chromatography, chromatographic columns are diol group chromatographic columns, flowing phases are supercritical fluids, and a modifier is the methanol. Supercritical carbon dioxide is used in the purification process, organic solvents harmful to environments are omitted, the production process is green and environmentally friendly, and obtained products are free of remaining harmful substances.

Description

Technical field [0001] The invention belongs to the field of chemical industry and pharmacy, and specifically relates to a method for separating and purifying emodin methyl ether and emodin from Polygonum cuspidatum extract. Background technique [0002] Polygonum cuspidatum is the dried rhizome and root of Polygonum Cuspidatum Sieb. et Zucc, a perennial herb in the Polygonum family Polygonum Cuspidatum Sieb. et Zucc. It is a common Chinese herbal medicine that has been included in the Chinese Pharmacopoeia. Among them, anthraquinone compounds such as emodin and emodin methyl ether have antibacterial, anti-inflammatory, anti-viral and anti-tumor effects. [0003] At present, the separation and purification of anthraquinones in Polygonum cuspidatum mainly adopts macroporous resin separation and purification method or high-speed countercurrent chromatography. Although the process is mature, the operation is cumbersome, the choice of solvent system in high-speed countercurrent chroma...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C46/10C07C50/34
CPCC07C46/10C07C50/34Y02P20/54
Inventor 亢静静孙爱玲李爱峰于琳琳柳仁民
Owner LIAOCHENG UNIV
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