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Method for extracting and separating poliumoside from Gallicarpa kwangtungensis Chun

A technology of chrysoside and purple bead, applied in the field of medicine, can solve the problem of inability to meet the requirements of high-purity active ingredients, and achieve the effects of easy industrial production, high separation efficiency, and easy control.

Inactive Publication Date: 2011-10-26
NANJING ZELANG AGRI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The above methods are to obtain the crude extract of Guangdong Zizhu, which cannot meet the market's demand for high-purity active ingredients

Method used

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  • Method for extracting and separating poliumoside from Gallicarpa kwangtungensis Chun

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Crush the stems and leaves of Guangdong Zizhu, put 1kg into the extraction tank, add 8 times the amount of 50% ethanol to ultrasonically extract 4 times, each time for 30min, combine the extracts, concentrate by rotary evaporation to obtain 72g of extract, use 0.36kg above 90°C Dissolve the extract in hot water, keep a constant temperature of 60°C, filter and separate through an ultrafiltration membrane with a molecular weight cut-off of 2000, collect the permeate, and pass the permeate through polyamide column chromatography, first elute with 3BV of 10% ethanol aqueous solution, and then use 6BV is eluted with 50% ethanol aqueous solution, collects 50% ethanol eluate, concentrates under reduced pressure until there is no alcohol smell, recovers ethanol, adds methanol to dissolve to make the concentration of the sample solution contain 1.1 mg / ml of crude drug, and is prepared by preparative high-efficiency liquid phase separation Chrysoside, the purity can reach 98%. Pr...

Embodiment 2

[0021] Crush the stems and leaves of Guangdong Zizhu, put 3kg into the extraction tank, add 10 times the amount of 30% ethanol to ultrasonically extract twice, each time for 60min, combine the extracts, concentrate by rotary evaporation to obtain 223g of extract, and use 0.67kg above 90°C Dissolve the extract in hot water, keep a constant temperature of 70°C, filter and separate through an ultrafiltration membrane with a molecular weight cut off of 3000, collect the permeate, and pass the permeate through polyamide column chromatography, first elute with 4BV of 15% ethanol aqueous solution, and then use 5BV is eluted with 70% ethanol aqueous solution, collects 70% ethanol eluate, concentrates under reduced pressure until there is no alcohol smell, recovers ethanol, adds methanol to dissolve so that the concentration of the sample solution is 1.0mg / ml containing crude drugs, and is prepared by preparative high-efficiency liquid phase separation Chrysoside, the purity can reach 9...

Embodiment 3

[0023] Crush the stems and leaves of Guangdong Zizhu, put 5kg into the extraction tank, add 6 times the amount of 60% ethanol to ultrasonically extract 6 times, each time for 45min, combine the extracts, concentrate by rotary evaporation to obtain 405g of extract, use 1.8kg above 90°C Dissolve the extract in hot water, maintain a constant temperature of 65°C, filter and separate through an ultrafiltration membrane with a molecular weight cut-off of 3000, collect the permeate, and pass the permeate through polyamide column chromatography, elute with 4BV of 20% ethanol aqueous solution, and then use 8BV is eluted with 55% ethanol aqueous solution, collects 55% ethanol eluate, concentrates under reduced pressure until there is no alcohol smell, recovers ethanol, dissolves in methanol to make the concentration of the sample solution contain crude drug 1.1mg / ml, and is prepared by preparative high-efficiency liquid phase separation Chrysoside, the purity can reach 98%. Preparative ...

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Abstract

The invention discloses a method for extracting and separating poliumoside from Gallicarpa kwangtungensis Chun. The method comprises the following steps: step 1, smashing Gallicarpa kwangtungensis Chun stems or leaves, carrying out ultrasonic extraction with ethanol, and concentrating an extracting solution so as to obtain extract; step 2, dissolving the extract with hot water with the amount being 3-5 times of the extract, carrying out membrane filtering separation at the temperature of 60-80 DEG C, collecting filtrate, and eluting with an alcohol-water solution on a polyamine resin column; and step 3, concentrating eluent until the eluent is free of alcohol smell, carrying out separation and purification with preparative liquid chromatography, eluting with a mixed solution of a polar organic solvent and water, concentrating corresponding components and carrying out vacuum drying. The preparation method is simple, and has the advantages of high efficiency, low cost and large separation preparation amount and is easy to repeat, and the purity of poliumoside prepared by the method can reach 98%.

Description

Technical field: [0001] The invention belongs to the field of medicine, and relates to a method for extracting and separating chrysoside from Guangdong purple pearl. Background technique: [0002] Guangdong Zizhu is the dried stem, branch and leaves of the Verbenaceae plant Guangdong Zizhu Gallicarpa kwangtungensis Chun. Jiangxi, Fujian, Hubei, Hunan and other places. This product is bitter, astringent, cool, has the effects of astringent and hemostasis, clearing away heat and detoxification, etc. It is used for hemoptysis, blood in the stool, lung and stomach bleeding, metrorrhagia, cough due to lung heat, sore throat, burns, heat ulcers, and traumatic bleeding. Zhou Boting et al. found that Guangdong Zizhu extract (95% ethanol extract extract) has a strong inhibitory effect on Staphylococcus aureus and Salmonella typhi in vitro, and can significantly inhibit the inflammatory response to the early exudation of experimental inflammation. Shorten the bleeding and coagulatio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/18C07H1/08
Inventor 苏刘花
Owner NANJING ZELANG AGRI DEV
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