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Preparation and purification method for heparitin sulfate disaccharide, and purified product thereof

A technology of heparin sulfate and purification method is applied in the field of preparation and purification of natural products, which can solve the problems of high price, inability to prepare disaccharide structure, and numerous preparation steps, and achieve the effect of simple purification method.

Inactive Publication Date: 2011-09-28
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method cannot prepare a large number of specific desired disaccharide structures, and the preparation steps are numerous and the price is relatively expensive

Method used

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  • Preparation and purification method for heparitin sulfate disaccharide, and purified product thereof

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preparation example Construction

[0033] 1. Preparation of pyridinebiose

[0034] ⑴. Calculate the amount of sodium ions (mol) that can be exchanged by 1 gram of H-type cation exchange resin (Amberlite IR-120 H-type) according to the exchange capacity E of the resin in the specification;

[0035] ⑵. Calculate the amount of resin needed to exchange 1 gram of HS disaccharide. The typical disaccharide molecular weight of HS is about 649, and there are 4 sodium ions in one molecule of disaccharide. The calculation method is as follows:

[0036] The amount of sodium ions contained in 1 gram of HS disaccharide (mol) (1g / 649) x4=0.0062mol

[0037] Required resin amount (g): 0.0062 / E=Y grams

[0038] ⑶. Select a glass column with a diameter-to-height ratio of 1:20. Soak Y grams of resin in pure water, rinse repeatedly until neutral, and then pack the column.

[0039] ⑷. Dissolve 100mg of HS disaccharide in 10mL of distilled water, put it together with 300mL of distilled water and the packed resin column at 4°C ov...

Embodiment 1

[0065] The preparation method of described heparin pyridinebiose comprises:

[0066] 1) Pass the heparin disaccharide aqueous solution through the cation exchange resin at 2°C, and then elute with distilled water of 1 times the volume of the resin;

[0067] 2) At room temperature, use pyridine to neutralize the obtained eluent to a pH of 6-6.5 under stirring;

[0068] 3) Freezing the neutralized solution at -70° C. for more than 5 hours, and then freeze-drying in a vacuum freeze dryer to obtain the heparin pyridinediose.

[0069] Described free aminodisaccharide is by following preparation purification method:

[0070] 1) Dissolve heparin pyridinedisaccharide in a mixed solution of 1-methyl-2-pyrrolidone / water, react in a water bath for 8 hours, and the temperature of the water bath is 60°C. The mixture of 1-methyl-2-pyrrolidone and water The volume ratio is: 8:2;

[0071] 2) Cool the reacted solution, add NaOH solution, and place it at -4°C overnight;

[0072] 3) Pass the...

Embodiment 2

[0088] The preparation method of described heparin pyridinebiose comprises:

[0089] 1) Pass the heparin disaccharide aqueous solution through the cation exchange resin at 5°C, and then elute with distilled water 3 times the volume of the resin;

[0090] 2) At room temperature, use pyridine to neutralize the obtained eluent to a pH of 6-6.5 under stirring;

[0091] 3) Freezing the neutralized solution at -70° C. for more than 5 hours, and then freeze-drying in a vacuum freeze dryer to obtain the heparin pyridinediose.

[0092] Described free aminodisaccharide is by following preparation purification method:

[0093] 1) Dissolve heparin pyridinedisaccharide in a mixed solution of 1-methyl-2-pyrrolidone / water, react in a water bath for 8-12 hours, and the temperature of the water bath is 60-70°C. The 1-methyl-2- The volume ratio of pyrrolidone to water is: 9:1;

[0094] 2) Cool the reacted solution, add NaOH solution, and place it at -4°C overnight;

[0095] 3) Pass the reac...

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Abstract

The invention relates to a preparation and purification method for heparitin sulfate disaccharide, and a purified product thereof. The preparation and purification method comprises the following steps: eluting heparin disaccharide used as a raw material with a cation exchange resin, and regulating the pH value of the eluate to be weak acidic with pyridine to obtain heparin pyridine disaccharide; separately enabling the heparin pyridine disaccharide to react with a 1-methyl-2-pyrrolidone aqueous solution and an acetic anhydride, Na2CO3 and sulfur trioxide trimethylamine complex; and separating the reaction liquid with a gel resin, and purifying to obtain free amino disaccharide, N-acetyl disaccharide and N-sulfated disaccharide. The preparation and purification method is simple, solves the problems that a specific disaccharide structure can not be prepared in large scale, the preparation process comprises too many steps and the product price is expensive, and simultaneously further develops the study on the correlation between the special structure and function of heparitin sulfate.

Description

technical field [0001] The invention belongs to the field of preparation and purification of natural products, and more specifically relates to a preparation and purification method of heparan sulfate disaccharide and its purified product. Background technique [0002] Heparan sulfate is composed of three regions with different degrees of sulfation alternately: the N-acetylated region (NA) is composed of completely unsulfated GlcNAc-GlcUA disaccharide units; the N-sulfated region (NS) is composed of Highly sulfated GlcNS(±6S)-IdoUA(2S) disaccharide composition, each disaccharide has 2-3 sulfate groups; and N-acetylation / N-sulfation region (NA / NS) is a transition region, Contains both sulfur-free and sulfur-containing disaccharides and crossed arrangements, the sequence is roughly GlcNAc-GlcUA-GlcNS-IdoA. The 12 representative disaccharide structures present in heparan sulfate are as follows figure 1 shown, which contains GlcNAc, GlcNSO 3 The disaccharide of the residue is...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H5/06C07H1/00C07H1/06
Inventor 魏峥林江慧魏可镁
Owner FUZHOU UNIV
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