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Method for separating and purifying cnidium lactone and imperatorin from fructus cnidii

An osthole, separation and purification technology, applied in the chemical and pharmaceutical fields, can solve the problems of high recovery cost of organic solvents, difficult to expand the separation scale, difficult solvent system selection, etc., and achieve a short process cycle, easy automatic control, and simple operation. Effect

Inactive Publication Date: 2015-08-19
LIAOCHENG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the silica gel column chromatography is a mature process, 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, silica gel column chromatography and high-speed countercurrent chromatography both need to consume a large amount of organic solvents, the cost of organic solvent recovery is high, recovery and reuse are difficult, and organic reagent residues in products are serious

Method used

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  • Method for separating and purifying cnidium lactone and imperatorin from fructus cnidii
  • Method for separating and purifying cnidium lactone and imperatorin from fructus cnidii

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Weigh 500 grams of Fructus Cnidii, pulverize it with a pulverizer, put it in a glass container, add 2500ml 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 500ml of water, extracted 3 times with 500ml of petroleum ether. The combined petroleum ether extracts were distilled under reduced pressure to recover the petroleum ether to obtain Cnidium Fructus Cnidii Extract.

[0026] The Fructus Cnidii 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 C18 chromatographic column, and the chromatographic column temperature was 40°C. The mobile phase is supercritical carbon dioxide, the flow rate is 3 times column volume / min, and the pressure is 15 MPa. The improver is methanol, and its proportion is 0.1%. The sep...

Embodiment 2

[0029] Weigh 500 grams of Fructus Cnidii, pulverize it with a pulverizer, put it in a glass container, add 3000ml 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 In 1000ml water, extract 3 times with 1000ml petroleum ether. The combined petroleum ether extracts were distilled under reduced pressure to recover the petroleum ether to obtain Cnidium Fructus Cnidii Extract.

[0030] Fructus Cnidii extract is dissolved with methanol, after filtration, carry out supercritical fluid chromatography separation, and chromatographic column is C18 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 improver is methanol, and its ratio is 0.05%. The separation process is detected by an ultraviolet detector with a...

Embodiment 3

[0032] Weigh 500 grams of Fructus Cnidii, pulverize it with a pulverizer, put it in a glass container, add 1500ml 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 800ml of water, extracted 3 times with 800ml of petroleum ether. The petroleum ether extracts were combined, and the petroleum ether was recovered by distillation under reduced pressure to obtain Cnidium Fructus Cnidii Extract.

[0033] Fructus Cnidii extract is dissolved with methanol, after filtration, carry out supercritical fluid chromatography separation, and chromatographic column is C18 chromatographic column, and chromatographic column temperature is 40 ℃. The mobile phase is supercritical carbon dioxide, the flow rate is 4 times column volume / min, and the pressure is 13 MPa. The improver is methanol, and its ratio is 0.08%. The separation process is detected by an ultraviole...

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Abstract

The invention belongs to the chemical and pharmaceutical field, and relates to a method for separating and purifying cnidium lactone and imperatorin from a fructus cnidii extract. The method comprises the steps: crushing a fructus cnidii medicinal material, adding anhydrous ethanol, carrying out cold immersion extraction, filtering the extraction liquid, concentrating under reduced pressure to obtain an extractum, dispersing the extractum in water, and extracting with petroleum ether; merging petroleum ether layers, and carrying out reduced pressure distillation to obtain a fructus cnidii extractum; and dissolving the fructus cnidii extractum in methanol, filtering, and carrying out supercritical fluid chromatography separation, wherein a chromatographic column is a C18 chromatographic column, a mobile phase is a supercritical fluid, and an improving agent is methanol. In the purification process, the supercritical carbon dioxide is used, organic solvents harmful to the environment are not used, the production process is green and environmentally friendly, and the obtained products have no harmful substance residues.

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 osthole and imperatorin from cnidium chinensis extract. Background technique [0002] Cnidium is a plant of the genus Cnidium in the family Umbelliferae cnidium monnieri (L.) The dry ripe fruit of Guss., the coumarins contained in it have important functions such as anti-arrhythmia, anti-osteoporosis, anti-AIDS, anti-fungal, anti-virus, anti-tumor and anti-mutation. [0003] At present, silica gel column chromatography or high-speed countercurrent chromatography are mainly used for the separation and purification of coumarin components in Fructus Cnidii. Although the silica gel column chromatography has a mature technology, 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, silica gel column...

Claims

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Application Information

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IPC IPC(8): C07D311/16C07D493/04
CPCC07D311/16C07D493/04Y02P20/54
Inventor 亢静静孙爱玲李爱峰于琳琳柳仁民
Owner LIAOCHENG UNIV
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