A class of hydroxytyrosol polymers with high oxidation resistance 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 the problems of industrial equipment corrosion environment, poor stability of hydroxytyrosol, weak oxidation resistance, etc., and achieve a high degree of polymerization The effect of product formation, good product quality and short reaction time
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[0034] A kind of preparation method of the hydroxytyrosol polymer of high oxidation resistance and thermal stability, the steps are:
[0035] The first step, enzymatic polymerization: Weigh an appropriate amount of hydroxytyrosol and dissolve it in acetic acid-sodium acetate buffer solution, mix thoroughly with an appropriate amount of laccase solution, put it in a flask and put it in a water bath at a certain temperature, and magnetically stir for several Hour.
[0036] The second step, precipitation and centrifugation: the liquid after the enzymatic reaction is immediately put into high temperature to inactivate the laccase, and placed in the refrigerator at a certain temperature for several hours to make the polymer precipitate. Then, the crude hydroxytyrosol polymer is obtained by centrifuging in a centrifuge at a certain speed and time.
[0037] The third step, washing and vacuum drying: the collected crude hydroxytyrosol polymer is washed several times with a certain pr...
Embodiment 1
[0048] Dissolve 1mM hydroxytyrosol in 30mL acetate buffer (0.05M, pH 4.7). The enzymatic polymerization was initially added with a laccase solution (1.0 mg / mL, enzyme activity 300 U). The flasks loaded with different reagents were placed under magnetic stirring at 35°C for 3h, and then the laccase was inactivated at 90°C. During the enzymatic reaction process, the medium color of the reaction gradually deepens and can be used to indicate the general progress of the polymerization reaction. After the polymerization reaction is completed, the reaction container is placed in a refrigerator at 4°C for 20 hours to precipitate the polymerization product. Then the precipitate was obtained by centrifugation at 3500r / min for 6min, and washed several times with a mixed solvent of acetone and deionized water (1:1, v / v) to remove unreacted hydroxytyrosol and laccase. The generated polymer was placed in a vacuum drying oven with a temperature range of 60° C., a vacuum range of 0.1 Mpa, an...
Embodiment 2
[0050]Dissolve 1.5mM hydroxytyrosol in 50mL acetate buffer (0.1M, pH 5). The enzymatic polymerization was initially added with a laccase solution (2.2 mg / mL, enzyme activity 660 U). The flasks loaded with different reagents were placed under magnetic stirring at 40°C for 3.5 hours, and then the laccase was inactivated at a high temperature of 90°C. During the enzymatic reaction, the medium color of the reaction gradually deepens and can be used to indicate the general progress of the polymerization reaction. After the polymerization reaction is completed, the reaction container 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 several times with a mixed solvent of acetone and chloroform (5:1, v / v) to remove unreacted hydroxytyrosol and laccase. The generated polymer was placed in a vacuum drying oven at a temperature range of 50° C., a vacuum range o...
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