Method for preparing alginate oligosaccharide monomers by using microwave radiation

A technology of alginic acid oligosaccharide and microwave irradiation, applied in the field of medicinal chemistry, can solve the problems of long preparation period, cumbersome process, unable to obtain monomers of oligosaccharide, etc., and achieves easy separation and purification, simple post-processing and high yield Effect

Active Publication Date: 2013-04-24
OCEAN UNIV OF CHINA
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  • Abstract
  • Description
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Problems solved by technology

Although this method is fast, acid is added in the degradation process, and it needs to be neutralized with alkali, and the salts generated in

Method used

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  • Method for preparing alginate oligosaccharide monomers by using microwave radiation
  • Method for preparing alginate oligosaccharide monomers by using microwave radiation
  • Method for preparing alginate oligosaccharide monomers by using microwave radiation

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Embodiment 1: Preparation of mannuronic acid oligosaccharide monomer

[0030] Polymannuronic acid (Mw=6.7kD) (the preparation method of polymannuronic acid described in the present invention is to adjust the pH value of the low molecular weight alginic acid solution to 2.85, the supernatant is graded with 75% ethanol, and the obtained precipitate is Polymannuronic acid) was prepared into a solution or suspension with a concentration of 100g / L in pure water, and ultrasonicated for 1min to fully dissolve it. Add the solution or suspension to 3 microwave extraction tanks (30mL per tank), microwave degradation at 140°C for 30min under the power of 400W, after the product is cooled, filter through double-layer filter paper, and freeze-dry to obtain mannuraldehyde Acid-oligosaccharide mixture, its yield was 86.9%. Its weight-average molecular weight was determined to be 2254 Da by HPGPC method. The oligosaccharide mixture was separated and purified by Bio-Gel P6 column chro...

Embodiment 2

[0037] Embodiment 2: Preparation of mannuronic acid oligosaccharide monomer

[0038] Prepare polymannuronic acid (Mw=10.6kD) into a suspension with a concentration of 5g / L in pure water, and ultrasonicate for 1min to fully dissolve it. Put it into 8 microwave digestion tanks (2mL per tank), set the power at 800W, microwave degradation at 90°C for 20 minutes, after the product is cooled, filter through double-layer filter paper, and freeze-dry to obtain the mannuronic acid oligosaccharide mixture. The yield was 84.4%. Its weight-average molecular weight was determined to be 3627 Da by HPGPC method. The oligosaccharide mixture was separated and purified by Bio-Gel P4 column chromatography (column volume is 4000mL), with 0.1mol / L NH 4 HCO 3 As the mobile phase, set the flow rate to 2.5mL / min, collect 10mL in each tube, detect with a differential detector, collect samples according to peaks, and heat to remove NH 4 HCO 3 Finally, oligosaccharide monomers with different polyme...

Embodiment 3

[0039] Embodiment 3: Preparation of mannuronic acid oligosaccharide monomer

[0040] Prepare polymannuronic acid (Mw=6.7kD) into a suspension with a concentration of 200g / L in pure water, and sonicate for 1min to fully dissolve it. Add it to 16 microwave digestion tanks (2mL per tank), and microwave degradation at 110°C for 15min under the condition of power of 1600W. After the product is cooled, it is filtered with double-layer filter paper and freeze-dried to obtain a mixture of mannuronic acid oligosaccharides. The yield was 84.4%. Its weight-average molecular weight was determined to be 2954 Da by HPGPC method. The oligosaccharide mixture was separated and purified by Superdex30 column chromatography (column volume is 2000mL), with 0.1mol / L NH 4 HCO 3 As the mobile phase, set the flow rate to 1.5mL / min, collect 3mL in each tube, detect with a differential detector, collect samples according to peaks, and heat to remove NH 4 HCO 3 Finally, oligosaccharide monomers with...

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Abstract

The invention provides a method for preparing alginate oligosaccharide monomers by using microwave radiation. The method comprises the following steps of: preparing polymannuronic acid or polyguluronic acid in algin, subjected to graded purification, into solutions or suspensions with different concentrations; performing microwave radiation in a microwave reaction system for degradation for 5 to 30 minutes; then cooling, filtering and freeze-drying the degradation product to obtain an oligosaccharide mixture; and separating and purifying the oligosaccharide mixture by using a gel column chromatography to obtain oligosaccharide monomers with different polymerization degrees. The method has the advantages that the degradation efficiency is high, the yield of oligosaccharide is high, acid or a buffer salt is not added during the degradation, few byproducts are generated, the after-treatment is simple and convenient, the product is easy to separate and purify, clean and environment-friendly effects are achieved, the cost is low, oligosaccharide mixtures with different molecular weight distributions and oligosaccharide monomers with different polymerization degrees can be prepared according to different aims and purposes, and the product is applied to various fields of foods, medicaments, chemical industry and the like.

Description

technical field [0001] The invention belongs to the technical field of medicinal chemistry, and in particular relates to a method for preparing alginic acid oligosaccharide monomers by utilizing microwave radiation. Background technique [0002] Alginic acid is the intercellular polysaccharide of marine brown algae. acid, G), the binary linear block compound composed of unique chemical structure and good biocompatibility, can be widely used in food and medicine as food additives, medical materials, drug slow and controlled release carrier materials, etc. and chemical industries. There are mainly three structural fragments in the alginic acid molecule: β-D-(1,4)-linked polymannuronate (PM) fragment, α-L-(1,4)-linked polygu Glucuronic acid (polyguluronate, PG) fragments, PMG fragments in which G and M are alternately copolymerized. After alginic acid is degraded by different methods and pH fractionated, two kinds of alginic acid fragments, polymannuronic acid and polyguluro...

Claims

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Application Information

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IPC IPC(8): C08B37/04C13K13/00
Inventor 管华诗胡婷李春霞赵峡李全才刘红兵
Owner OCEAN UNIV OF CHINA
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