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Method for extracting isoborreverine

A technology for floristine and floristry, which is applied in the field of extracting isorrhizine and achieves the effects of simple operation, high yield and few steps.

Inactive Publication Date: 2012-09-26
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there is no report on the method of preparing Heterocarpine at home and abroad

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Take 10kg of the aboveground part of Verticillium verticillum and crush it, use 10 times the amount of 20% methanol solution (pH3) to reflux extract 4 times, combine the extracts and concentrate until each 1ml is equivalent to 1g of crude drug, add the concentrated solution to the macroporous strong acid cation On the exchange resin, the sample loading speed is 5BV / h, and the impurity is firstly eluted with water, and then eluted with 5% sodium chloride aqueous solution, the elution speed is 3BV / h, and the sodium chloride eluate is collected until the alkaloid reaction is negative , after desalination treatment, concentrated to obtain the total alkaloid extract, mix the extract with basic alumina powder (400 mesh) and put it on the alumina column, and use chloroform-ethyl acetate-methanol (4:2:1~1: 2:4) Segmented elution and segmented collection, collect the fractions with high content of Heterophyllum arginine, combine and concentrate under reduced pressure to obtain th...

Embodiment 2

[0018] Take 10kg of the above-ground part of Verticillium verticillum and crush it, use 4 times the amount of 80% ethanol solution (pH5.5) to reflux extract twice, combine the extracts and concentrate until each 1ml is equivalent to 5g of crude drug, add the concentrate to the gel-type On strong acidic cation exchange resin, the sample loading speed is 2BV / h, and the impurity is firstly eluted with water, and then eluted with 2% sodium chloride aqueous solution, the elution speed is 1BV / h, and the sodium chloride eluate is collected until the biological Alkali reaction is negative, after desalination treatment, concentrated to get the total alkaloid extract, mix the extract with neutral alumina powder (100 mesh) and put it on the alumina column, use chloroform-ethyl acetate-methanol (4:2:1 ~1:2:4) were eluted in sections and collected in sections, and the fractions with high content of Heterocarpine were collected, combined and concentrated under reduced pressure to obtain a sa...

Embodiment 3

[0020] Take 10kg of the aboveground part of Verticillium verticillum and crush it, use 8 times the amount of 40% ethanol solution (pH4) to reflux extract 3 times, combine the extracts and concentrate to 3g of crude drug per 1ml, add the concentrate to the macroporous strong acid On the cation exchange resin, the sample loading speed is 3BV / h, and the impurity is firstly eluted with water, and then eluted with 3% sodium chloride aqueous solution, the elution speed is 3BV / h, and the sodium chloride eluate is collected until the alkaloid reaction Negative, after desalination treatment, concentrated to get the total alkaloid extract, mix the extract with neutral alumina powder (300 mesh) and put it on the alumina column, and use chloroform-ethyl acetate-methanol (4:2:1~1 :2:4) Segmented elution and segmented collection, collect the fractions with high content of Heterocarpine, combine and concentrate under reduced pressure to obtain the sample solution. Take hexane-chloroform-meth...

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Abstract

The invention discloses a method for extracting isoborreverine. The method is characterized by comprising the following steps of: crushing the overground part of borreria verticillata(L.), performing reflux extraction by using acid alcohol, after extraction liquor is concentrated, loading onto a cation exchange resin column, eluting by using water to remove impurities, eluting by using a 2 to 5 percent sodium chloride aqueous solution, collecting sodium chloride eluent until alkaloid reaction is negative, desalting, and concentrating to obtain total alkaloid extract; and uniformly mixing the extract and alumina powder, loading to an alumina column, eluting stepwise by using mixed organic solvents in different ratios and collecting high-content isoborreverine fractions stepwise, mixing and concentrating under reduced pressure, and separating and purifying by a high-speed counter-current chromatography to obtain a high-content isoborreverine product. By the method, the isoborreverine can be separated and purified quickly and efficiently, the product is high in content, the cost can be reduced effectively, and environmental pollution can be reduced.

Description

technical field [0001] The invention belongs to the field of traditional Chinese medicine chemistry, and relates to a method for extracting Heterophyllin. Background technique [0002] Isoborreverine, a brown amorphous solid, is an indole alkaloid. Molecular formula C32H40N4, molecular weight is 480.7. UV λmax (EtOH) nm (lgε): 226 (4.28), 287 (4.10), 294 (4.00). Heterophyllin comes from Rubiaceae (Rubiaceae) Borreria verticillata (L.) G.F.W. Meyer Aerial Parts. Has antimicrobial and cytotoxic activity. It has broad-spectrum antimicrobial effect on Staphylococcus aureus, Candida albicans, Mycobacterium fortuitum, Pneumococcus, Streptococcus viridans, Neisseria gonorrhoeae, etc. When its concentration is 3-6 μg / mL, it has high cytotoxicity. [0003] At present, there is no report on the method of preparing Heterocarpine at home and abroad. Contents of the invention [0004] The purpose of the present invention is to provide an efficient and rapid method for extracting...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D487/04
Inventor 刘东锋杨成东
Owner NANJING ZELANG MEDICAL TECH
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