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Method for separating purified physcion and emodin from giant knot weed

A technology for separation and purification of emodin methyl ether, which is applied in the field of separation and purification of emodin methyl ether and emodin, can solve the problems of high recovery cost of organic solvents, difficulty in expanding the separation scale, difficulty in selecting solvent systems, etc. Easy-to-automate, simple-to-operate effects

Inactive Publication Date: 2015-08-05
LIAOCHENG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • Method for separating purified physcion and emodin from giant knot weed

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Weigh 100 grams of Polygonum cuspidatum, pulverize it with a pulverizer, put it in a glass container, add 500ml of absolute ethanol to extract by cold soaking 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 of 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 was dissolved in methanol, filtered (the filter membrane used was 0.45 μm filter membrane), and separated by supercritical fluid chromatography. The chromatographic column was a glycol-based chromatographic column, and the chromatographic column temperature was 40°C. The mobile phase is supercritical carbon dioxide, the flow rate is 3 times colum...

Embodiment 2

[0029] Weigh 100 grams of Polygonum cuspidatum, pulverize it with a pulverizer, put it in a glass container, add 600ml of absolute ethanol to extract by cold soaking for 24 hours, extract 3 times, filter the extract, concentrate under reduced pressure to obtain an extract, and disperse the extract in 690 In ml of 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 with methanol, after filtration, carry out supercritical fluid chromatography separation, and chromatographic column is glycol-based chromatographic column, and chromatographic column temperature is 45 ℃. The mobile phase is supercritical carbon dioxide, the flow rate is 5 times column volume / min, and the pressure is 12 MPa. The improve...

Embodiment 3

[0032] Weigh 100 grams of Polygonum cuspidatum, pulverize it with a pulverizer, put it in a glass container, add 300ml of absolute ethanol to extract by cold soaking 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 of 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 with methanol, after filtration, carry out supercritical fluid chromatographic separation, the chromatographic column is a glycol-based chromatographic column, and the chromatographic column temperature is 40°C. The mobile phase is supercritical carbon dioxide, the flow rate is 4 times column volume / min, and the pressure is 13 MPa. The ...

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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 in particular relates to a method for separating and purifying emodin methyl ether and emodin from polygonum cuspidatum extract. Background technique [0002] Polygonum cuspidatum is a perennial herb of Polygonaceae Polygonum cuspidatum Polygonum Cuspidatum Sieb The dried rhizome and root of et Zucc is a relatively common Chinese herbal medicine that has been included in the Chinese Pharmacopoeia. The compounds have antibacterial, anti-inflammatory, anti-viral and anti-tumor effects. [0003] At present, the separation and purification of anthraquinone components in Polygonum cuspidatum mainly adopt 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 chromatography is difficult, and the separation scale is difficult...

Claims

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Application Information

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Patent Type & Authority Applications(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