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Preparation method of pachyman sulfate

A kind of Poria polysaccharide, sulfate technology

Active Publication Date: 2013-11-13
合肥创新医药技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Such drugs need to be obtained through separation and purification, the sources are limited, the purification process is complicated, the price is expensive, and the product quality is not easy to control

Method used

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  • Preparation method of pachyman sulfate
  • Preparation method of pachyman sulfate
  • Preparation method of pachyman sulfate

Examples

Experimental program
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Effect test

Embodiment 1

[0031] A preparation method of polysaccharide sulfate, characterized in that:

[0032] Include the following steps:

[0033] (1), poria cocos is peeled, dried, pulverized, and dissolved in 0.5mol / L NaOH whose total volume is 10-15 times its total volume for 3-5 times, and the polysaccharides are extracted at 4-10°C for 5-10h each time, and combined Extract the obtained supernatant, neutralize the supernatant to pH 6-8 with about 10% acetic acid, precipitate overnight at 4-10°C, collect the precipitate by centrifugation at low temperature, wash the precipitate with deionized water for 3-5 times, and then use Wash with water, ethanol, acetone and ether in sequence, and dry at 70-90°C to obtain white pachyrhin, which is grinded into powder for later use;

[0034] (2), add sulfamic acid and organic solvent in the reaction flask of rotary evaporator, preheat to about 80 ℃ of reaction temperature, after sulfamic acid dissolves completely, add the dry pachyrhizu powder obtained in s...

Embodiment 2

[0042] 1. Extraction and purification of Poria cocos polysaccharide

[0043] Weigh 100g Poria cocos powder, dissolve in 0.5mol / L NaOH with a total volume of 10 times in 3 times, extract polysaccharides at 4°C for 8 hours each time, combine the leaching supernatants of 3 times, and neutralize with 10% acetic acid to pH6. 5. Precipitate overnight in refrigerator at 4°C. Centrifuge at low temperature to collect the precipitate, wash the precipitate three times with deionized water, wash with absolute ethanol, acetone, and ether in sequence, and dry at 70°C to obtain white polysaccharide, which is ground into powder for use. The polysaccharide content detected by the phenol-sulfuric acid method is 99.2%, and the viscosity-average molecular weight measured by the viscosity method is 2.15×10 5 Da.

[0044] 2. Preparation of Pachyman sulfate (PS)

[0045] (1) Add 200ml of dimethylformamide (DMF) into a 1000ml pear-shaped bottle, heat it in a water bath to 80°C, add 90g of sulfamic...

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Abstract

The invention discloses a preparation method of pachyman sulfate. The preparation method comprises the following steps of: adding sulfamic acid and an organic solvent in a reaction bottle of a rotary evaporator; preheating to reaction temperature; after fully dissolving the sulfamic acid, adding dried pachyman powder; vacuuming a reaction system; cooling to room temperature after the reaction is finished; adjusting the pH of reaction solution to 9-10 with saturated alkali solution; continuously vacuuming to remove ammonia and repeatedly vacuuming until the reaction solution has no ammonia smell; maintaining the pH value to be over 7 until the pH value does not go down; then adding ethanol; precipitating polysaccharide sulfate; filtering and then dissolving in water again; filtering; placing in an ultrafilter to desalinate and concentrate; and detecting residual quantity of free sulfate radicals in eluent by using saturated barium chloride solution until no white precipitate is produced. According to the preparation method, the sulfation efficiency is greatly increased, polysaccharide molecule degradation and production of sugar ring double ring are suppressed, the color of a product becomes light, and the final quality of the product is obviously improved.

Description

technical field [0001] The invention belongs to the field of medicinal chemistry, and in particular relates to a preparation method of polysaccharide sulfate. Background technique [0002] Polysaccharides are the most abundant substances in nature and are composed of monosaccharide residues bonded by covalent bonds. Polysaccharide sulfate is a polysaccharide derivative, which is formed by substituting some hydroxyl groups of monosaccharide residues in the polysaccharide molecular chain with sulfate groups. Among them, the molecular weight and the degree of substitution of sulfate groups (DS) of monosaccharide residues are the two most important physical and chemical parameters. . Polysaccharide sulfate has a wide range of pharmacological activities, such as anticoagulant, antithrombotic, antiviral, hypolipidemic and antitumor activities. In 1987, Beyer of the former Federal Republic of Germany cooperated with Hoechst Company to artificially synthesize sulfated xylan for th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08B37/00A61K31/715A61P7/02
Inventor 陈群
Owner 合肥创新医药技术有限公司
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