Method for preparing seleno-polysaccharide by organic method

A selenized polysaccharide and organic technology, which is applied in the field of organic selenized polysaccharide preparation, can solve the problems of complex reaction process, complex preparation process, and many reaction by-products, and achieve high selenium content in products, simple reaction process, and low reaction by-products. little effect

Active Publication Date: 2010-01-13
NORTHWEST NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Patent CN101104644A discloses a method for preparing polysaccharide selenite and its application. In this method, dextrin, dextran, arabinoxylan and selenium oxyfluoride are added to pyridine, and heated for 0.1-100 hours to obtain A polysaccharide selenite, the highest selenium content can reach 45%, but the reaction time of this method is too long, and the selenium oxyfluoride used is not easy to synthesize, so it is not suitable for large-scale industrial production; patent ZL88103347 authorized a selenized carrageenan The preparation method, the selenized carrageenan prepared by this method has a low selenium content (2500-15000ppm), and generates toxic by-products such as hydrogen selenide; patent CN 101024664A discloses selenium galactose and its chemical synthesis, and this method is Reaction of galactose with organic selenide reagent, the preparation process of this method is complicated, and monosaccharide does not have the pharmacological activity that natural polysaccharide has; Patent CN 101190951A discloses a kind of preparation method of polysaccharide selenate, this method is in dioxygen The selenization reaction of polysaccharides in hexacyclic or toluene adopts heterogeneous reaction. The polysaccharides used are anhydrous dextran or anhydrous astragalus polysaccharides, and selenate is synthesized. The reaction time is about 5 hours, and the selenium content is 769-2250μg / g; patent ZL200410071806.6 authorizes a selenate polysaccharide and its preparation method, the method is to first synthesize selenous acid, selenous acid is reduced to selenic acid, then selenate is introduced into the polysaccharide, and the selenium content is 3mg-200mg / g; Patent CN 1560088A discloses a preparation method of selenized glucomannan, in a Se 6+ Add ethanol and hydrochloric acid to the solution to make a selenized reaction liquid, then add glucomannan to make selenized glucomannan, the selenium content is 125.4-197.3 mg / kg; patent CN1284509A discloses chitosan selenous acid Salt and its preparation method, the method is to react the amino group of chitosan with the added selenous acid, the selenium content of the product is 0-26%
[0005] The selenization technology mentioned in the above patents has the disadvantages of long reaction time, many reaction by-products, generally low selenium content, and complicated reaction process.
Documents at home and abroad do not relate to the synthesis of selenium reagents with selenous acid and thionyl chloride, the method for preparing selenium polysaccharides

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  • Method for preparing seleno-polysaccharide by organic method
  • Method for preparing seleno-polysaccharide by organic method

Examples

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Embodiment 1

[0024] A kind of preparation method of selenized fern fructus polysaccharide of the present invention, comprises the following steps:

[0025] 1) Weighing 0.4 g of Polysaccharides from Poria japonica with a purity of more than 90% and putting it into a reactor, adding 10 ml of N,N-dimethylformamide, and stirring at room temperature for 30 minutes to obtain a suspension A;

[0026] (2) Weigh 1g of selenous acid and add it to the reactor, add 10ml of thionyl chloride dropwise with a dropping funnel, under nitrogen protection, stir with a magnetic stirrer, and react for 40min in an ice bath, at a pressure of 0.07MPa and a temperature of 40°C Under reduced pressure distillation, obtain solid substance B;

[0027] (3) Dissolve the solid substance B with 10ml of N,N-dimethylformamide, drop it completely into the suspension A under ice-bath conditions, finish the dropping within 15 minutes, and seal the reaction at 30°C for 5 hours under the protection of nitrogen to obtain Reaction...

Embodiment 2

[0030]A kind of preparation method of selenized fern fructus polysaccharide of the present invention, comprises the following steps:

[0031] (1) Weighing 0.5 g of Polysaccharides from Poria japonica with a purity of more than 90% and putting it into a reactor, adding 10 ml of N,N-dimethylformamide, and stirring at room temperature for 30 minutes to obtain a suspension A;

[0032] (2) Weigh 1.1g of selenous acid and add it to the reactor, add 11ml of thionyl chloride dropwise with a dropping funnel, under nitrogen protection, stir with a magnetic stirrer, react in an ice bath for 30min, at a pressure of 0.06MPa, a temperature of 45 Under reduced pressure distillation at ℃, solid substance B was obtained;

[0033] (3) Dissolve the solid substance B with 10ml of N,N-dimethylformamide, drop it completely into the suspension A under ice-bath conditions, finish the dropping within 20 minutes, and seal the reaction at 50°C for 2 hours under the protection of nitrogen to obtain Reac...

Embodiment 3

[0036] A kind of preparation method of selenized fern fructus polysaccharide of the present invention, comprises the following steps:

[0037] (1) Weigh 0.6 g of P. japonicus polysaccharide with a purity of more than 90% and put it into a reactor, add 10 ml of N,N-dimethylformamide, and stir at room temperature for 30 minutes to obtain a suspension A;

[0038] (2) Weigh 1.5g of selenous acid and add it to the reactor, add 15ml of thionyl chloride dropwise with a dropping funnel, under nitrogen protection, stir with a magnetic stirrer, react in an ice bath for 35min, at a pressure of 0.08MPa, a temperature of 50 Under reduced pressure distillation at ℃, solid substance B was obtained;

[0039] (3) Dissolve the solid substance B with 10ml of N,N-dimethylformamide, drop it completely into the suspension A under ice-bath conditions, finish the dropping within 25 minutes, and seal the reaction at 70°C for 3 hours under the protection of nitrogen to obtain Reaction solution C;

[...

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Abstract

The invention relates to a method for preparing seleno-polysaccharide by an organic method, which comprises the following steps: (1) placing potentilla anserine polysaccharide and artemisia seed polysaccharide into a reactor, adding N,N-dimethyl formamide into the reactor, and stirring to obtain suspension A; (2) dripping thionyl chloride into selenious acid for reacting, carrying out reduced pressure distillation on the reacted solution to obtain solid matter B; (3) dissolving the solid matter B with the N,N-dimethyl formamide, and adding the mixed solution into the suspension A for reaction to obtain reaction solution C; and (4) dissolving the reaction solution C with distilled water, adjusting the pH value to be 7 with sodium hydroxide, carrying out centrifugation, filling supernatant fluid into a bag filter with the interception quantity of 8,000 to 140,000Da, introducing tap water for dialysis, and carrying out the dialysis with deioned water; and carrying out reduced pressure distillation on the solution in the bag filter, adding ethanol into concentrated solution, standing the mixed solution at room temperature, carrying out centrifugation, collecting deposition on the lower layer and freezing and drying to finally obtain the potentilla anserine polysaccharide or the artemisia seed polysaccharide. The method has the advantages of short reaction time, few byproducts, simple reaction process, high selenium content of products and the like.

Description

technical field [0001] The invention relates to a method for preparing selenized polysaccharides, in particular to an organic method for preparing selenized polysaccharides. Background technique [0002] Selenium is an essential trace element for humans and animals. It is the active component of glutathione peroxidase, which can prevent the oxidative damage of pancreatic islet β cells, make them function normally, promote glucose metabolism, reduce blood sugar and urine sugar, and improve the symptoms of diabetic patients; selenium can protect the retina, enhance The smoothness of the vitreous body improves vision and prevents cataracts; it is also an important element to maintain normal heart function, and has the effect of protecting and repairing the heart body. Current research shows that the reduction of human blood selenium level will lead to the decline of the function of scavenging free radicals in the body, resulting in increased deposition of harmful substances, i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B37/00
Inventor 张继王俊龙赵保堂王小芳姚健王云普梁俊玉马君义赵美荣吴秀琴王邦
Owner NORTHWEST NORMAL UNIVERSITY
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