Preparation method of carboxymethyl chito-oligosaccharide

A technology of carboxymethyl chitosan oligosaccharide and chitosan oligosaccharide is applied in the field of preparation of carboxymethyl chitosan oligosaccharide, which can solve the problems of immature carboxymethyl chitosan oligosaccharide technology, unoptimized process and parameters, etc., and achieve excellent antibacterial properties. Antioxidant activity, reduced preparation time, no pollution residue effect

Active Publication Date: 2019-10-22
SOUTHWEST UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the current technology for preparing carboxymethyl chitosan oligosaccharides by chemi

Method used

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  • Preparation method of carboxymethyl chito-oligosaccharide
  • Preparation method of carboxymethyl chito-oligosaccharide
  • Preparation method of carboxymethyl chito-oligosaccharide

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Example Embodiment

[0030] The technical scheme adopted in the present invention is a preparation method of carboxymethyl chitosan oligosaccharide, which includes the following steps:

[0031] Step 1. Add chitosan oligosaccharide to isopropanol and shake at room temperature to obtain swollen chitosan oligosaccharide; the ratio of chitosan oligosaccharide to isopropanol is 2g: 15ml~25ml, where the chitosan oligosaccharide is calculated by mass, and isopropanol is calculated by mass. Volume calculation

[0032] Step 2. Add NaOH solution to the swollen chitosan oligosaccharide obtained in Step 1, and shake and alkalize at room temperature to obtain an alkaline feed solution; the mass percentage concentration of the NaOH solution is 30%, and the alkalinization time is 2h-12h; chitosan and NaOH solution The ratio is 2g:6.67ml-20ml, among which, the chitosan oligosaccharide is calculated by mass, and the NaOH solution is calculated by volume.

[0033] Step 3. Add the isopropanol solution of chloroacetic acid...

Example Embodiment

[0040] Example 1

[0041] Step 1. Weigh 2g of chitosan oligosaccharides in a 1L volume beaker, stick a plastic wrap, add 15ml of isopropanol, and swell with shaking at room temperature for 30 minutes;

[0042] Step 2: Add 6.67 ml of a 30% NaOH solution with a concentration of 30% to the swollen chitosan obtained in Step 1, and then shake and alkalize at room temperature for 2 hours to obtain an alkaline feed solution;

[0043] Step 3. Add the isopropanol solution of chloroacetic acid to the alkaline feed solution obtained in Step 2 for carboxylation reaction at 35°C for 4h, wherein the mass of chloroacetic acid in the isopropanol solution of chloroacetic acid is 2g, and the volume of isopropanol Is 50ml;

[0044] Step 4. Adjust the pH of the feed solution after step 3 carboxylation to neutral with HCl with a mass percentage of 9.5%, then precipitate with ethanol for 6.5 hours, discard the supernatant, and dissolve the sediment on the bottom of the cup in an appropriate amount Ethanol...

Example Embodiment

[0046] Example 2

[0047] The implementation steps are the same as in Example 1, except that the alkalization time, the amount of chloroacetic acid added, and the carboxylation time are different. The remaining steps are the same. In this example, the alkalization time is 7h, the amount of chloroacetic acid added is 3g, and the carboxylation time is 12h.

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Abstract

The invention discloses a preparation method of carboxymethyl chito-oligosaccharide. The method comprises the steps that 1, chitosan oligosaccharide is added into isopropanol, room temperature oscillationis conducted, andswellingchitosan oligosaccharide is obained; 2, a NaOH solution is added into the swellingchitosan oligosaccharide obtained in step 1; 3, an isopropanol solution of chloroacetic acid is added in alkaline feed liquid obtained in step 2, and a hydroxylation reaction is performed; 4, the feed liquid obtained after hydroxylation in step 3 is adjusted with an HCl solution to reachthe pH being neutral, then absolute ethyl alcohol is used for ethanol precipitation, and the feed liquid containing precipitation is obtained; 5, the feed liquidcontaining the precipitation in step 4is subjected to centrifugation, the precipitation is collected and washed multiple times, the washed precipitation is dried, powdering is conducted, and carboxymethyl chito-oligosaccharide powder is obtained. According to the preparation method, preparation is conducted through a chemical method, the carboxymethyl chito-oligosaccharide can be obtained, operation is easy, a high substitution degreeproduct can be obtained, and the product has the excellent antibacterial and antioxidant properties.

Description

technical field [0001] The invention belongs to the field of biotechnology, and in particular relates to a preparation method of carboxymethyl chitosan oligosaccharide. Background technique [0002] Oligochitosan is a small molecular oligosaccharide with amino groups. It is derived from chitin in shrimp and crab shells, degraded and deacetylated. It is pure natural and non-toxic. At the same time, oligochitosan has no immunogenicity, and when it is used to inhibit bacteria, the risk of drug-resistant strains is greatly reduced, and it has the advantages of low molecular weight, good water solubility, great function, easy absorption, and high biological activity. In the research on the activity of chitosan oligosaccharides, it was found that antibacterial and antibacterial effects and anti-oxidation effects are the most important activities of chitosan oligosaccharides. However, the antibacterial agents and antioxidants prepared with chitosan oligosaccharides are not ideal, ...

Claims

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Application Information

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IPC IPC(8): C07H5/06C07H1/00C08B37/08A01N43/16A01P3/00A01P1/00
CPCA01N43/16C07H1/00C07H5/06C08B37/003
Inventor 甘玲黄华宇孙梦嫄陈贵凤张慧
Owner SOUTHWEST UNIVERSITY
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