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Method for preparing alginate oligosaccharide monomers by using microwave radiation

A technology of alginic acid oligosaccharides and microwave radiation, which is applied in the field of medicinal chemistry, can solve the problems of long preparation period, inability to obtain monomers of oligosaccharides, cumbersome process, etc., and achieve easy separation and purification, high yield, and simple post-treatment Effect

Active Publication Date: 2015-05-20
OCEAN UNIV OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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 the treatment process are removed by dialysis. , and there are environmental protection problems, so the process needs to be further improved

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
Comparison scheme
Effect test

Embodiment 1

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

[0030] The polymannuronic acid (Mw=6.7kD) (the preparation method of the polymannuronic acid of the present invention is to adjust the pH value of the low molecular weight alginic acid solution to 2.85, the supernatant is fractionated with 75% ethanol, and the resulting precipitate is Polymannuronic acid) is prepared into a solution or suspension with a concentration of 100g / L with pure water, and ultrasonicated for 1min to make it fully dissolved. Add the solution or suspension to 3 microwave extraction tanks (30 mL each), microwave degradation at 140°C for 30 min under the condition of 400W power, after cooling the product, filter with double filter paper and freeze-dry to obtain mannose aldehyde The yield of the acid-oligosaccharide mixture was 86.9%. The weight-average molecular weight measured by HPGPC method was 2254Da. The oligosaccharide mixture was separated and purified by Bio-Gel P6 column chr...

Embodiment 2

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

[0038] The polymannuronic acid (Mw=10.6kD) was prepared into a suspension with a concentration of 5g / L with pure water, and ultrasonicated for 1min to make it fully dissolved. Add it to 8 microwave digestion tanks (2mL per tank), set the power to 800W, microwave degradation at 90°C for 20min, after cooling the product, filter with double filter paper and freeze-dry to obtain a mixture of mannuronic acid oligosaccharides. The yield is 84.4%. The weight average molecular weight was 3627 Da measured by HPGPC method. The oligosaccharide mixture was separated and purified by Bio-Gel P4 column chromatography (column volume was 4000 mL), and 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 by the differential detector, collect the samples according to the peaks, and heat to remove NH 4 HCO 3 Then, oligosaccharide monomers with different polymerization deg...

Embodiment 3

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

[0040] The polymannuronic acid (Mw=6.7kD) was prepared into a suspension with a concentration of 200g / L with pure water, and ultrasonicated for 1min to make it fully dissolved. Add it to 16 microwave digestion tanks (2 mL per tank), microwave degradation at 110°C for 15 minutes under the power of 1600W, after cooling the product, filter with double-layer filter paper and freeze-dry to obtain a mixture of mannuronic acid oligosaccharides. The yield is 84.4%. The weight-average molecular weight measured by HPGPC method was 2954Da. The oligosaccharide mixture was separated and purified by Superdex30 column chromatography (column volume was 2000 mL), and the oligosaccharide mixture was purified 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 by the differential detector, collect the samples according to the peaks, and heat to remove NH 4 HCO 3 The...

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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 specifically relates to a method for preparing alginic acid oligosaccharide monomers by microwave radiation. Background technique [0002] Alginic acid is the intercellular polysaccharide of marine brown algae. It is composed of β-D-(1,4)-Mannuronic acid (M) and α-L-(1,4)-Guluronic acid (Guluronic acid). Acid, G) binary linear block compound, because of its unique chemical structure and good biocompatibility, it can be used as food additives, medical materials, drug slow and controlled release carrier materials, etc., and is widely used in food and medicine And chemical industry. 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 Polyguluronate (PG) fragment, PMG fragment in which G and M are alternately copolymerized. After the alginic acid is degraded by different methods and pH graded, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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