Preparation method of LMWF (Low Molecular Weight Fucoidan)

A technology of fucoidan and low molecular weight, which is applied in the field of preparation of low molecular weight fucoidan sulfate, can solve the problems of cumbersome processing, violent reaction, complex equipment and process, etc., and achieve the effect of simple process, simple follow-up treatment and no pollution to the environment

Inactive Publication Date: 2016-03-23
YANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The traditional oxidation method mainly uses hydrogen peroxide or hypochlorous acid, the reaction is violent, the equipment and technology are complicated, and the follow-up treatment is cumbersome

Method used

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  • Preparation method of LMWF (Low Molecular Weight Fucoidan)

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Embodiment 1, the impact of different temperatures on the degradation of fucoidan sulfate

[0022] Take fucoidan sulfate with a weight average molecular weight of 240-2400kDa, add distilled aqueous solution to prepare 6 parts of fucoidan sulfate solution with a mass concentration of 1%, and keep the temperature at 50°C, 60°C, 70°C, 80°C, and 90°C respectively , 100°C. Put 6 parts of the solution into the reactor respectively, add concentrated persulfate solution, control the concentration of persulfate to 100mM, stir rapidly to carry out the degradation reaction, cool down after 60min to stop the reaction, and dialyze the obtained solution with a cut-off molecular weight of 2000Da After bag dialysis and desalination, concentrate the dialysate, add absolute ethanol to a final concentration of 75-80%, let it stand for more than 12 hours, filter, and vacuum-dry the obtained solid to obtain low molecular weight fucoidan sulfate. It can be seen from Table 1 that temperature...

Embodiment 2

[0025] Embodiment 2, the influence of different reaction time solution fucoidan sulfate ester

[0026] Take fucoidan sulfate with a weight average molecular weight of 240-2400kDa, add distilled aqueous solution to prepare 4 parts of fucoidan sulfate solution with a mass concentration of 1%, and keep the temperature at 100°C. Put the 4 solutions into the reactor respectively, add concentrated persulfate solution, control the concentration of persulfate to 100mM, stir rapidly to carry out the degradation reaction, cool down after 10min, 30min, 60min, and 120min respectively to stop the reaction, and the obtained After dialysis and desalination of the solution with a dialysis bag with a cut-off molecular weight of 2000Da, after concentrating the dialysate, add absolute ethanol to a final concentration of 75-80% and let it stand for 12 hours, filter it with suction, and dry the obtained solid in vacuum to obtain a low molecular weight Fucoidan Sulfate. It can be seen from Table 2...

Embodiment 3

[0029] Embodiment 3, the impact of different persulfate concentrations on microwave degradation of fucoidan sulfate

[0030] Take fucoidan sulfate with a weight average molecular weight of 240-2400kDa, add distilled aqueous solution to prepare 7 parts of fucoidan sulfate solution with a mass concentration of 1%, keep the temperature at 100°C, add concentrated persulfate solution respectively, and control persulfate Concentrations were 10mM, 20mM, 50mM, 100mM, 200mM, 500mM, 1000mM, and the degradation reaction was carried out by rapid stirring. After 60 minutes, the temperature was lowered to stop the reaction. The concentrated solution is spray-dried to obtain low molecular weight fucoidan sulfate ester. It can be seen from Table 3 that the concentration of persulfate has a great influence on the degradation of fucoidan sulfate. Generally, the higher the concentration, the better the degradation effect. However, when the concentration is too high, over-oxidation often occurs. ...

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Abstract

The invention belongs to the field of fine chemical engineering, and in particular relates to a preparation method of LMWF (Low Molecular Weight Fucoidan). The preparation method comprises the steps of dissolving HMWF (High Molecular Weight Fucoidan) into water to prepare a fucoidan solution, and heating the fucoidan solution to reaction temperature for standby use; then adding a prepared sodium persulfate solution of which the concentration is 10 to 1000 mM in the fucoidan solution, setting constant reaction temperature to be 50 to 100 DEG C, and reacting for 10 to 120 minutes; then concentrating after desalting through a dialysis method or an ultrafiltration method, and preparing the LMWF after carrying out spray drying, freeze drying or alcohol precipitation. According to the preparation method disclosed by the invention, the LMWF is quickly prepared through a heat-activated persulphate oxidation method; persulfate can be reduced into sulfate, so that more fucoidan can be obtained from a chemical equilibrium angle; through the preparation method, new chemical components are not introduced in during and after a preparation process, so that the preparation method is environment-friendly, and industrialization can be easily realized.

Description

technical field [0001] The invention belongs to the field of green fine chemical production, and in particular relates to a preparation method of low molecular weight fucoidan sulfate. Background technique [0002] Fucoidan sulfate is a sulfated heteropolysaccharide from brown algae and echinoderms, also known as fucoidan, laminarin, fucoidan sulfate, fucoidan, etc. It has various clinical special effects such as inhibiting tumor cell growth, treating cancer, treating cardiovascular and cerebrovascular diseases, and treating renal failure. Fucoidan sulfate directly from organisms has a large molecular weight, which is prone to antigenicity and obvious side effects. However, after conversion to low molecular weight and low polymerization degree fucoidan sulfate, the antigenicity, toxicity and side effects are also reduced or disappeared. The literature shows that the clinical efficacy of fucoidan sulfate is negatively correlated with its degree of polymerization. [0003] C...

Claims

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Application Information

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IPC IPC(8): C08B37/00
CPCC08B37/0063
Inventor 董昆明缪莉周晓见靳翠丽
Owner YANGZHOU UNIV
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