Sepia polysaccharide sulfated derivative and preparing method thereof

A technology of polysaccharide sulfuric acid and squid ink, which is applied in the field of biomedicine to achieve the effects of high yield, pure product and simple steps

Inactive Publication Date: 2007-11-28
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

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Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Preparation of sulfated derivatives of squid ink polysaccharides.

[0033] (1) Sulfation of squid ink polysaccharide:

[0034] Weigh 0.5 g of squid ink polysaccharide and dissolve it with 3 ml of anhydrous formamide.

[0035] 0.75 ml of chlorosulfonic acid was added dropwise to 1.5 ml of formamide to prepare a mixed solution.

[0036] Add the mixed solution dropwise to the squid ink polysaccharide solution, stir and react at 25-30°C for 6 hours, after the reaction solution is taken out, immediately add 3 times the volume of absolute ethanol to terminate the reaction, and centrifuge to collect the precipitate.

[0037] The precipitate was made into a 10% solution, the pH was adjusted to neutral, and 3 times the volume of absolute ethanol was added for precipitation.

[0038] Make the precipitate into a 10% solution, add 0.5% sodium bisulfite, adjust the pH to 9.5 with sodium bicarbonate solution, remove ammonia by heating in a 65°C water bath until there is almost no a...

Embodiment 2

[0044] The preparation method of cuttlefish ink polysaccharide sulfated derivative is made up of the following steps:

[0045] (1) Sulfation of squid ink polysaccharide:

[0046] Take by weighing squid ink polysaccharide pure product 15g, dissolve with its anhydrous formamide of 5 times of weight, stand-by;

[0047] Adding chlorosulfonic acid dropwise into formamide with a volume ratio of 1:2 and dissolving it to prepare a mixed solution;

[0048] Add the mixed solution dropwise to the squid ink polysaccharide solution, stir and react at 28°C for 5 hours, after the reaction solution is taken out, immediately add 4 times the volume of absolute ethanol to terminate the reaction, leave it at 4°C overnight, filter or centrifuge to collect the precipitate;

[0049] Make the precipitate into an 8% aqueous solution, adjust the pH to neutral, and add 3 times the volume of absolute ethanol to precipitate;

[0050] Make the precipitate into an 8% aqueous solution, adjust the pH to 8.5...

Embodiment 3

[0056] The preparation method of cuttlefish ink polysaccharide sulfated derivative is made up of the following steps:

[0057] (1) Sulfation of squid ink polysaccharide:

[0058] Take by weighing squid ink polysaccharide pure product 50g, dissolve with its anhydrous formamide of 10 times of weight, stand-by;

[0059] With a ratio of 1:2 by volume, 75ml of chlorosulfonic acid was added dropwise into 150ml of formamide and dissolved to prepare a mixed solution;

[0060] Add the mixed solution dropwise to the squid ink polysaccharide solution, stir and react at 30°C for 10 hours, after the reaction solution is taken out, immediately add 5 times the volume of absolute ethanol to terminate the reaction, leave it at 4°C overnight, filter or centrifuge to collect the precipitate;

[0061] Make the precipitate into a 15% aqueous solution, adjust the pH to neutral, and add 4 times the volume of absolute ethanol to precipitate;

[0062] Make the precipitate into a 15% aqueous solution...

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Abstract

The present invention discloses one kind of cuttlefish ink polysaccharide sulfatizing derivative, which is constituted through connecting sulfuric radical to the free hydroxyl radical in the saccharide chain of cuttlefish ink polysaccharide. The cuttlefish ink polysaccharide sulfatizing derivative has sulfuric radical content of 7-36 wt%, substitution degree Ds of 0.14-0.96, and molecular weight of 3000-45000 D. The present invention also discloses the preparation process of the cuttlefish ink polysaccharide sulfatizing derivative, and the preparation process has the features of less steps, low cost, high yield and high product purity. The cuttlefish ink polysaccharide sulfatizing derivative, experiment shows, has certain antitumor activity and angiogenesis inhibiting activity.

Description

technical field [0001] The invention belongs to the field of biomedicine, in particular to a novel sulfated derivative of squid ink polysaccharide (also known as glycosaminoglycan) and a preparation method thereof. Background technique [0002] The squid ink polysaccharide extracted from the ink of Sepiella maindroni de Rochebrune is a polysaccharide with a new structure. It has immune regulation and anti-mutation activities, and it can improve the effect of anti-tumor drugs when used in combination with anti-tumor drugs. Structural modifications to polysaccharides often increase their biological activity or create new activities. Sulfation of polysaccharides is a commonly used chemical modification method. Studies have shown that sulfated polysaccharides have biological activities such as anti-tumor, anti-virus, and inhibition of angiogenesis. However, after searching, there are no research papers and patent reports on the sulfated structure modification of squid ink polys...

Claims

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Application Information

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IPC IPC(8): C08B37/00A61K31/737
Inventor 王凤山李玉华刘纯慧曹吉超刘玉红
Owner SHANDONG UNIV
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