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Preparation method of dogwood polysaccharides

A polysaccharide of Cornus officinalis and Cornus officinalis technology, which is applied in the field of extraction and purification of Cornus officinalis polysaccharide by means of ultrasonic extraction, membrane separation and fractional precipitation, can solve the problems of loss of effective components, large dosage, and various types of organic solvents, and achieves the effects of simple solvent and low cost.

Inactive Publication Date: 2011-04-06
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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
[0004] 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 The resulting polysaccharides from Cornus officinalis have low purity
[0005] Chinese patent "A method for extracting polysaccharides from Cornus officinalis by enzymatic hydrolysis" (application number: 200810120569.6), the method disclosed in this patent is to take the dry pulp of Cornus officinalis and grind it to make dry cornus officinalis powder, add distilled water whose quality is 15 to 60 times that of the dry cornus officinalis powder, add Enzyme hydrolyzed at 35-60°C, pH 3.5-7.0 for 0.5h-4h, after the enzymolysis, the enzyme was inactivated, the extract was concentrated and alcohol-precipitated, and centrifuged to dry to obtain the polysaccharide extract of Cornus officinalis, the product purity is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Take 1 kg of dry residue after alcohol extraction of total glycosides from Cornus officinalis pulp, add 5 L of warm water at 60°C for ultrasonic extraction for 2 hours, repeat 3 times, and combine the extracts. The extract was concentrated to 1 / 2 of the original volume, cooled to 25°C, and 1.8 L of 30% H 2 o 2 , stir until light yellow, add 3% trichloroacetic acid until no turbidity occurs, add centrifuge and centrifuge until there is no white suspension at the junction of the chaotropic surface, separate the clear liquid, ultrafilter with an ultrafiltration membrane, add the retentate Add 400ml of water, add 400ml of 30% ethanol for precipitation, add 600ml of 50% ethanol to the filtrate, filter, add 1400ml of 90% ethanol to the filtrate, place the precipitate, filter out the precipitate, wash with 200ml of acetone, 150ml of ethanol in turn, and vacuum dry to obtain 11.8g of Cornus officinalis polysaccharide, As detected by HPLC, the purity was 91.5%.

Embodiment 2

[0022] Take 1kg of the dry residue after alcohol extraction of total glycosides from Cornus officinalis pulp, add 10L of 30°C warm water for ultrasonic extraction for 1 hour, repeat twice, combine the extracts, concentrate the extracts to 1 / 2 of the original volume, cool to 25°C, add 2.5L of 30% H 2 o 2 , stir until light yellow, add 3% trichloroacetic acid until no turbidity occurs, add centrifuge and centrifuge until there is no white suspension at the junction of the chaotropic surface, separate the clear liquid, ultrafilter with an ultrafiltration membrane, add the retentate Add 650ml of water to 650ml of 30% ethanol for precipitation, add 940ml of 50% ethanol to the filtrate, filter, add 2250ml of 90% ethanol to the filtrate, place the precipitate, filter out the precipitate, wash with acetone and ethanol in turn, and vacuum dry to obtain 12..9g of Cornus officinalis polysaccharide, As detected by HPLC, the purity was 95.6%.

Embodiment 3

[0024] Take 1 kg of dry residue after alcohol extraction of total glycosides from Cornus officinalis pulp, add 8 L of 70°C warm water for ultrasonic extraction for 1.5 h, repeat twice, and combine the extracts. The extract was concentrated to 1 / 2 of the original volume, cooled to 25°C, and 3.8 L of 30% H 2 o 2 , stir until light yellow, add 3% trichloroacetic acid until no turbidity occurs, add centrifuge and centrifuge until there is no white suspension at the junction of the chaotropic surface, separate the clear liquid, ultrafilter with an ultrafiltration membrane, add the retentate Add 500ml of water, add 500ml of 30% ethanol for precipitation, add 750ml of 50% ethanol to the filtrate, filter, add 1750ml of 90% ethanol to the filtrate, place the precipitate, filter out the precipitate, wash with acetone and ethanol in turn, and dry in vacuum to obtain 13.8g of Cornus officinalis polysaccharide, which was analyzed by HPLC Detection, the purity is 87.2%.

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PUM

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Abstract

The invention relates to a preparation method of dogwood polysaccharides. The process comprises the following steps of: taking dry residues obtained after extracting total glucoside from dogwood pulp alcohol as a raw material, adding 5-10 (V / W) times of warm water, ultrasonically extracting for 1-2 h, combining the extracting solutions, concentrating, adding 30% of H2O2 and 3% trichloroacetic acid, centrifuging, taking the supernate, ultrafiltering, firstly adding a right amount of water into entrapped matter, then adding different concentrations of alcohol for fractional precipitation, filtering out high concentration alcohol precipitates and drying to obtain the product. The process has the advantages of simple operation, lower cost and higher purity and is beneficial to large production operation.

Description

Technical field: [0001] The invention relates to a preparation method of cornus officinalis polysaccharides, in particular to a method for extracting and purifying cornus officinalis polysaccharides by means of ultrasonic extraction, membrane separation and fractional precipitation. 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. Documents "Research Progress on Effective Chemical Components of Cornus officinalis (Zhou Jinghua, Li Chunsheng, Li Diandong. Chinese Journal of New Drugs, 2001, 10(11): 808.)" and "Chemical Researc...

Claims

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Application Information

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