Method for combinedly extracting Morroniside, dogwood polysaccharide and ursolic acid from dogwood

A technology of combined extraction of polysaccharides from Cornus officinalis, applied in chemical instruments and methods, sugar derivatives, sugar derivatives, etc., can solve the problems of loss of active ingredients, long process flow, large dosage, etc., and achieve high raw material utilization and economic benefits high quality effect

Inactive Publication Date: 2011-07-20
NANJING ZELANG MEDICAL TECH
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  • Claims
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Problems solved by technology

The existing method is degreasing raw materials, water extraction, concentration, washing, and drying to obtain products, such as Zhao Xiaohua et al. "Study on Extraction Technology and Physical and Chemical Properties of Cornus officinalis Polysaccharides". Degreasing uses petroleum ether, which has a large amount and high toxicity; there are many types of organic solvents used in the process , easily lead to the loss of active ingredients
Zhang Lijuan et al. "Optimization of Extraction Process of Cornus officinalis Polysaccharides and Its Protective Effect on Focal Cerebral Ischemia-Reperfusion Injury in Rats", the method disclosed in this document is ultrasonic water extraction, concentration, ultrafiltration, alcohol precipitation, protein removal, washing and drying Cornus officinalis polysaccharide is obtained, the polysaccharide concentrate is thicker, the ultrafiltration membrane is easy to block, the operation is more difficult, and the obtained product is not high in purity
Chinese patent "A method of enzymatically extracting polysaccharides from Cornus officinalis" (Application No.: 200810120569.6), the method disclosed in this patent is to take the dry pulp of Cornus officinalis and pulverize it to obtain dry cornus officinalis powder, adding distilled water that is 15 to 60 times the amount of dry cornus officinalis powder, adding Enzyme hydrolyzes at 35~60℃, pH3.5~7.0 for 0.5h~4h. After the enzymolysis, the enzyme is inactivated, the extract is concentrated and alcoholized, and centrifuged to dry to obtain the polysaccharide extract of Cornus officinalis. Under acidic conditions, polysaccharides may be decomposed. The cleavage of glycosidic bonds affects the purity and activity of the product
[0006] At present, the extraction and separation of ursolic acid mainly adopts the methods of organic solvent extraction and step-by-step elution of silica gel column chromatography. These methods have long process flow, low yield, and use toxic organic solvents.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Crush Cornus officinalis, take 1kg, add 10L of water, heat to 50°C, soak and extract for 3 hours, extract twice, combine the extracts, add HPD100 macroporous resin column for adsorption, collect the next column liquid, first elute with 3L of water, remove the water Combine the eluent and the lower column solution, add ethanol to a concentration of 70%, precipitate, filter and dry the precipitate to obtain 13.6g of Cornus officinalis polysaccharide, with a content of 74.9%, and then elute with 3L of 70% ethanol solution, collect the alcohol eluate, and concentrate Alcohol-free, add 300ml of water to disperse, add equal volume of n-butanol to extract 3 times, concentrate the n-butanol extract to recover n-butanol, and dry to obtain 8.9g of morroniside, with a content of 71.2%. Add 6L of 90% alcohol to the residue for reflux extraction, concentrate the extract, adsorb on X-5 macroporous resin column, elute with 3L of 90% ethanol, collect the eluate, add 15g of activated car...

Embodiment 2

[0022] Crush Cornus officinalis, take 1kg, add 15L water, heat to 40°C, soak and extract for 2 hours, extract 3 times, combine the extracts, add LSA-20 macroporous resin column for adsorption, collect the next column liquid, and first elute with 3.5L water , combine the water eluate with the lower column liquid, add ethanol to a concentration of 70%, precipitate, filter and dry the precipitate to obtain 11.5 g of Cornus officinalis polysaccharide, with a content of 80.1%, and then elute with 3L of 70% ethanol solution, collect and wash with ethanol Deliquoring, concentration without alcohol, adding 350ml of water to disperse, adding an equal volume of n-butanol to extract 4 times, n-butanol extract was concentrated to recover n-butanol, and dried to obtain morroniside 9.2g with a content of 67.8%. Add 8L of 90% alcohol to the residue after water extraction for reflux extraction, concentrate the extract, absorb on LSA-10 macroporous resin column, elute with 4L of 90% ethanol, co...

Embodiment 3

[0024] Crush Cornus officinalis, take 1kg, add 12L water, heat to 60°C, soak and extract for 3 hours, extract twice, combine the extracts, add LSA-20 macroporous resin column for adsorption, collect the next column liquid, first elute with 4L water, Combine the water eluate and the lower column solution, add ethanol to a concentration of 70%, precipitate, filter and dry the precipitate to obtain 11.7g of Cornus officinalis polysaccharide, with a content of 72.7%, and then elute with 3L of 70% ethanol solution, collect the ethanol for elution solution, concentrate without alcohol, add 400ml of water to disperse, add equal volume of n-butanol to extract twice, n-butanol extract is concentrated to recover n-butanol, and dry to obtain morroniside 8.1g, the content is 69.9%. Add 7L of 90% alcohol to the residue after extraction for reflux extraction, concentrate the extract, absorb on LSA-10 macroporous resin column, elute with 3L of 90% ethanol, collect the eluate, add 30g of activ...

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Abstract

The invention relates to a method for combinedly extracting Morroniside, dogwood polysaccharide and ursolic acid from dogwood. The method comprises the following steps of: crushing the dogwood; adding water in an amount which is 10 to 15 times of the weight of the dogwood and performing heating extraction for 2 to 3 times; mixing the extracting liquid; loading the extracting liquid to a macroporous resin column I for adsorption; collecting liquid which flows down the column; eluting by using water and ethanol solution sequentially; mixing the water eluent with the liquid which flows down the column; adding alcohol for precipitation; filtering precipitates out and drying to obtain the dogwood polysaccharide; collecting the alcohol eluent, concentrating until alcohol does not exist, adding water for dispersion, adding isometric n-butyl alcohol for extraction, concentrating an n-butyl alcohol layer to recover the n-butyl alcohol, and drying to obtain the Morroniside; adding alcohol into the residues obtained after water extraction to perform reflux extraction, concentrating the extracting liquid, loading the extracting liquid to a macroporous resin column II for adsorption, eluting by using 90 percent ethanol; and adding active carbon into the eluent to perform reflux decoloring, filtering the active carbon out, cooling naturally for crystallization, filtering out crystals, and drying to obtain the ursolic acid. In the method, toxic reagents do not exist in the preparation process; the process is simple; the utilization ratio of the raw materials is high; cost is low; and the method is suitable for industrialized production.

Description

Technical field: [0001] The invention belongs to the field of separation of natural products, in particular to a method for jointly extracting morroniside, cornus polysaccharide and ursolic acid from Cornus officinalis. Background technique: [0002] Cornus officinalis (Fructus Corni) is the dry pulp of Cornus officinalis Sieb.et Zucc. It is a kind of nourishing and precious medicinal material, which has the effects of nourishing the liver and kidney, astringent essence and detoxification. Studies in recent years have shown that Cornus officinalis has anti-hemorrhagic shock, inhibition of platelet aggregation, immune regulation, anti-inflammation, hypoglycemic, anti-oxidation, anti-cancer, and antibacterial effects. Cornus officinalis mainly contains iridoid glycosides, polysaccharides, organic acids, tannins and other components. Among the iridoid morronisides in Cornus officinalis, the content of morroniside was the highest. [0003] Since ancient times, there have been...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J63/00C07H17/04C07H1/08C08B37/00
Inventor 刘东锋万冬梅杨成东
Owner NANJING ZELANG MEDICAL TECH
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