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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 chemical methods is not mature enough, and the production process and parameters are not optimized.

Method used

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

Examples

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preparation example Construction

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

[0031] Step 1, add chitosan oligosaccharide into isopropanol and shake at room temperature to obtain swelling chitosan oligosaccharide; the ratio of chitosan oligosaccharide to isopropanol is 2g: 15ml~25ml, wherein, chitosan oligosaccharide is calculated by mass, and isopropanol is calculated by mass volume calculation;

[0032] Step 2, add NaOH solution to the swelling chitosan oligosaccharide obtained in step 1, and oscillate at room temperature to obtain an alkaline feed liquid; the mass percentage concentration of the NaOH solution is 30%, and the alkalization time is 2h to 12h; the chitosan oligosaccharide and NaOH solution The ratio is 2g: 6.67ml ~ 20ml, wherein, chitosan oligosaccharide is calculated by mass, and NaOH solution is calculated by volume.

[0033] Step 3, add isopropanol solution of chloro...

Embodiment 1

[0041] Step 1, weigh 2g of chitosan oligosaccharide into a 1L beaker, stick a plastic wrap, add 15ml of isopropanol, swell at room temperature for 30min;

[0042] Step 2, first add 6.67ml of NaOH solution with a mass percentage concentration of 30% to the swollen chitosan oligosaccharide 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 isopropanol solution of chloroacetic acid to the alkaline feed solution obtained in step 2 for carboxylation reaction at 35°C for 4h, wherein the quality of chloroacetic acid in the isopropanol solution of chloroacetic acid is 2g, and the volume of isopropanol 50ml;

[0044] Step 4, adjust the pH of the feed solution after carboxylation in step 3 to neutral with 9.5% HCl by mass percentage, then ethanol alcohol precipitation for 6.5 hours, pour off the supernatant, and dissolve the precipitate at the bottom of the cup in an appropriate amount of Ethanol alc...

Embodiment 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, and the rest of the steps are the same. The alkalization time in this example 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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