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Method for sulfonating pectin

A pectin and sulfonation technology, applied in the field of polymers, can solve the problems of less data and immature pectin, and achieve the effect of mild method, good anticoagulation and high yield

Inactive Publication Date: 2012-07-18
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At present, the research on the sulfonation of pectin at home and abroad is still immature, and there are relatively few materials.

Method used

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  • Method for sulfonating pectin
  • Method for sulfonating pectin
  • Method for sulfonating pectin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Embodiment 1, a kind of method of pectin sulfonation, carries out following steps successively:

[0042] (1) Preparation of esterification reagent: 2 g of sulfur trioxide-pyridine complex was dissolved in 4 ml of anhydrous dimethyl sulfoxide to obtain sulfonation reagent;

[0043] (2) Preparation of self-extracting pectin suspension:

[0044] Dried citrus peels (moisture content ≤ 90%) are pulverized into powder (passed through a 60-mesh sieve), then soaked in 30 times the volume of water overnight (soaked for 12 hours), centrifuged at a speed of 3000r / min for 40min, The resulting supernatant was precipitated by adding 3 times the volume of absolute ethanol. Water-soluble pectin can be obtained by repeatedly precipitating twice with the same amount of ethanol, and after drying (drying at 50°C to constant weight), citrus pectin can be obtained.

[0045] Put 200 mg of citrus pectin into 10 ml of anhydrous dimethyl sulfoxide and stir for 0.5 hour to obtain a pectin suspe...

Embodiment 2

[0051] Embodiment 2, a kind of preparation method of pectin sulfonation, carries out following steps successively:

[0052] (1) Preparation of esterification reagent: 2 g of sulfur trioxide-pyridine complex was dissolved in 4 ml of anhydrous dimethyl sulfoxide to obtain sulfonation reagent;

[0053] (2) Preparation of commercial pectin suspension:

[0054] First commercial citrus pectin (purchasable from sigma company) is purified by fractional precipitation with ethanol and acetone to obtain purified commercial pectin; details are as follows:

[0055] Take 50ml of commercial citrus pectin, pour it into 50ml of absolute ethanol, ultrasonically dissolve it, and enter the centrifuge at a speed of 3000r / min for 40 minutes; pour off the ethanol layer in the upper layer obtained after centrifugation, take the lower layer and add 50ml of precipitate 80% (volume concentration) of ethanol, after ultrasonic dissolution, enter the centrifuge and centrifuge at a speed of 3000r / min for 4...

Embodiment 3

[0062] Embodiment 3, a kind of preparation method of pectin sulfonation, carries out following steps successively:

[0063] (1), the preparation of esterification reagent:

[0064] Dissolve 2g of sulfur trioxide-pyridine complex in 4ml of anhydrous dimethyl sulfoxide to obtain a sulfonation reagent;

[0065] (2) Put 200 mg of citrus pectin into 10 ml of ultrapure water, stir for 0.5 hour, and completely dissolve the pectin; obtain a pectin solution.

[0066] The preparation method of citrus pectin is with embodiment 1.

[0067] Above-mentioned pectin solution is crossed gel chromatography column, specifically as follows:

[0068] Use Sephacryl S-300column (1.6cm×100cm) Sephadex column, use pH3.5 hydrochloric acid solution as mobile phase, flow rate is 0.5ml / min, start to collect after 160 minutes, collect to 750min, after 800 minutes Stop elution. Obtain the collection fluid.

[0069] Add triethylamine (TBA) dropwise to the above collection solution until the pH is 6.0-6....

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Abstract

The invention discloses a method for sulfonating pectin, which comprises the step of sulfonating pectin or triethylamine pectin salt by using sulfur trioxide-pyridine complex in a dimethylsulfoxide (DMSO) environment so as to obtain sulfonated pectin polysaccharide. The method adopts the following two systems: a trioxide-pyridine complex-DMSO system, and a TBA-trioxide-pyridine complex-DMSO system. The method disclosed by the invention is simple in operation and good in sulfonating effect. The sulfonated pectin polysaccharide prepared by the method is small in degradation in the reaction process, small in side reaction, has good anticoagulation, anti-tumor and anti-virus actives and a wide application range.

Description

technical field [0001] The invention relates to a method for sulfonating pectin, which belongs to the field of polymers. The sulfonated pectin polysaccharide has significant anticoagulant activity. It has good prospects for drug development and health care product research and development. Background technique [0002] Sulfonated polysaccharides are a kind of negatively charged biological macromolecules formed by replacing some hydroxyl groups in polysaccharide molecules with sulfate groups. They are widely found in various organisms in nature and have a wide range of biological activities. With the deepening of research, it is found that most sulfated polysaccharides have significant anticoagulant, antitumor and antiviral activities (Smorenburg et al., 2001; Mao, W. et al., 2009; Huashi, C., 1988). At present, research on acidic polysaccharides at home and abroad is mainly concentrated in the marine field, such as kelp fucoidan sulfate, acidic mucopolysaccharides in sea c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B37/06A61P7/02A61P35/00A61P31/12
Inventor 陈士国尹馨梓刘东红胡亚芹陈建初孙玉敬吴丹叶兴乾
Owner ZHEJIANG UNIV
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