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Hydroxytyrosol polymer having high antioxidation and thermal stability and preparation method thereof

A technology of hydroxytyrosol and thermal stability, which is applied in the field of preparation of hydroxytyrosol polymers, can solve problems such as poor stability of hydroxytyrosol, corrosion environment of industrial equipment, weak oxidation resistance, etc., and achieve good product quality and green cycle Good economic performance and the effect of improving production efficiency

Active Publication Date: 2017-07-28
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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Problems solved by technology

[0005] The invention provides a hydroxytyrosol polymer with high oxidation resistance and thermal stability and a preparation method thereof, which solves the problems of poor stability of hydroxytyrosol, weak oxidation resistance, strong acid, As a catalyst, strong alkali can easily cause problems such as corrosion of industrial equipment and environmental pollution, while the use of biological enzymes for oxidative polymerization of phenols is not only beneficial to the green production of the factory, but also conducive to improving the application range of hydroxytyrosol

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  • Hydroxytyrosol polymer having high antioxidation and thermal stability and preparation method thereof
  • Hydroxytyrosol polymer having high antioxidation and thermal stability and preparation method thereof
  • Hydroxytyrosol polymer having high antioxidation and thermal stability and preparation method thereof

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preparation example Construction

[0034] A method for preparing hydroxytyrosol polymer with high oxidation resistance and thermal stability, the steps are:

[0035] The first step, enzymatic polymerization: Weigh an appropriate amount of hydroxytyrosol, dissolve it in acetic acid-sodium acetate buffer, mix it with an appropriate amount of laccase solution, place it in a flask and put it in a water bath at a certain temperature, and stir it magnetically. hour.

[0036] The second step, precipitation and centrifugation: the liquid after the enzymatic reaction is immediately placed at a high temperature to inactivate the laccase, and placed in the refrigerator at a certain temperature for several hours to precipitate the polymer. Under certain speed and time conditions, the crude hydroxytyrosol polymer is obtained by centrifugation through a centrifuge.

[0037] The third step, washing, vacuum drying: the collected crude hydroxytyrosol polymer is washed several times with a certain proportion of mixed organic solvents ...

Embodiment 1

[0048] Dissolve 1 mM hydroxytyrosol in 30 mL acetate buffer (0.05M, pH 4.7). In the enzymatic polymerization reaction, laccase solution (1.0 mg / mL, enzyme activity 300 U) was initially added. Place the flasks containing different reagents at 35°C with magnetic stirring for 3h, and then inactivate the laccase at 90°C. During the enzymatic reaction, the color of the reaction medium gradually darkens and can be used to indicate the general progress of the polymerization reaction. After the polymerization reaction is completed, the reaction vessel is placed in a refrigerator at 4°C for 20 hours to precipitate the polymerization product. Then the precipitate was obtained by centrifugation at 3500 r / min for 6 min, and washed several times with a mixed solvent of acetone and deionized water (1:1, v / v) to remove unreacted hydroxytyrosol and laccase. The resulting polymer is placed in a temperature range of 60°C, a vacuum degree of 0.1Mpa, and a time range of 18 hours to remove the sol...

Embodiment 2

[0050] Dissolve 1.5mM hydroxytyrosol in 50mL acetate buffer (0.1M, pH 5). In the enzymatic polymerization reaction, laccase solution (2.2 mg / mL, enzyme activity 660 U) was initially added. Place the flasks containing different reagents at 40°C with magnetic stirring for 3.5 hours, and then inactivate laccase at a high temperature of 90°C. During the enzymatic reaction, the color of the reaction medium gradually darkens and can be used to indicate the general progress of the polymerization reaction. After the polymerization reaction is completed, the reaction vessel is placed in a refrigerator at 0°C for 16 hours to precipitate the polymerization product. Then the precipitate was obtained by centrifugation at 4000r / min for 15min, and washed with a mixed solvent of acetone and chloroform (5:1, v / v) several times to remove unreacted hydroxytyrosol and laccase. The resulting polymer is placed in a temperature range of 50°C, a vacuum degree of 0.07Mpa, and a time range of 72 hours ...

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Abstract

The invention discloses a hydroxytyrosol polymer having high antioxidation and thermal stability and a preparation method thereof. The method comprises the following steps: firstly, enzymatic polymerization: dissolving hydroxytyrosol in acetic acid-sodium acetate buffer, and fully mixing with a laccase solution to generate water bath reaction; secondly, precipitation and centrifugation: placing liquid obtained from enzymatic polymerization immediately in a high temperature condition to enable laccase to inactivate, cooling to enable the polymer to precipitate, and centrifuging again to obtain crude hydroxytyrosol polymer; thirdly, washing and vacuum drying: washing collected crude hydroxytyrosol polymer with a mixed organic solvent for a plurality of times, to remove unreacted hydroxytyrosol and laccase, and performing vacuum drying to remove the solvent to obtain the final hydroxyl group butyrol polymer. The stability of a product is good, the oxidation resistance is strong, and the production process is green.

Description

Technical field [0001] The invention relates to the technical field of enzymatic oxidative polymerization of natural active substances, and relates to a method for preparing an antioxidant and thermally stable hydroxytyrosol polymer. Background technique [0002] Hydroxytyrosol (3,4-dihydroxyphenethyl alcohol) is a natural small molecule phenolic compound widely found in olive fruit, leaves, virgin olive oil and especially rich in wastewater from olive oil mills. In 1950, it was discovered in the form of echinacea in Echinacea angustifolia, which has antioxidant, anti-inflammatory, anti-cancer, cardiovascular disease protection and blood sugar lowering activities. In particular, it is considered to be one of the most natural antioxidants capable of scavenging free radicals. Its free radical scavenging rate is twice that of quercetin and three times that of epicatechin, making it popular in the fields of health products, medicines and cosmetics. There are extremely wide applicati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L65/00C08L73/00C12P7/22
CPCC08L65/00C08L73/00C08L2201/08C12P7/22
Inventor 黄立新谢普军张彩虹丁莎莎邓叶俊王晓杰
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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