Essence composition based on blueberry extract and preparation method thereof
By modifying the mixed method of blueberry extract wrapped in polylevodopa and surfactant, the problem of blueberry essence retaining fragrance for a short time during high temperature extraction is solved, and the long-term fragrance retention and antibacterial effect of the essence is achieved, and the preservation stability of the essence is improved.
Patent Information
- Application Number
- CN202510497786.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-04-21
- Publication Date
- 2025-07-18
- Estimated Expiration
- 2045-04-21
AI Technical Summary
Among the existing fragrance extraction methods, high temperature extraction leads to instability of the fragrance, difficult to preserve and short fragrance time, especially the extraction method of blueberry fragrance has not effectively solved this problem.
The mixed method of modified polylevodopa-encapsulated blueberry extract, deionized water, surfactant and cosurfactant is used to avoid high temperature extraction. Through the oxidative self-polymerization encapsulation effect of esterified levodopa-prepolymer, the sustained release volatility of blueberry extracts is achieved and the fragrance retention effect is extended.
The obtained flavor composition has a long-term fragrance retention effect, and reduces microbial spoilage through antibacterial activity, thereby improving the storage stability of flavors and fragrance durability.
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of daily chemical flavor preparation, and particularly relates to a flavor composition based on blueberry extract and a preparation method thereof. Background Art
[0002] Fragrances play an increasingly important role in modern life. Whether in food, cosmetics, detergents, perfumes or air fresheners, fragrances not only give products a unique smell, but also influence consumers' perception and purchasing decisions. The main functions of fragrances include: (1) Fragrances can significantly enhance the market value of products. Consumers tend to have a strong reaction to fragrance, and pleasant fragrances can enhance the attractiveness of products, thereby promoting sales. For example, the aroma of foods such as chocolate and coffee can often arouse consumers' appetite and increase their desire to buy; (2) Fragrances can directly affect people's emotions and psychological states. Certain aromas such as lavender and vanilla are believed to help relax and relieve stress, while citrus aromas are believed to refresh the mind. Therefore, fragrances have also been used in psychological and emotional therapy; (3) Fragrances can also be used to mask odors in products to improve the user experience. In cleaners and detergents, fragrances can mask the pungent smell brought by chemical ingredients, making the product more pleasant; (4) Certain fragrance ingredients have antibacterial and antioxidant properties, which can help maintain the freshness of food and extend its shelf life. This is especially important in the food industry.
[0003] The sources of flavors can be divided into two categories: natural and synthetic. Synthetic flavors are fragrances made by chemical synthesis. The advantages of synthetic flavors are that they are low in cost, stable, and can create many aromas that natural flavors cannot achieve. For example, synthetic flavors commonly used in perfumes, such as vanillin and ethyl vanillin, can simulate the characteristics of natural aromas. Natural flavors refer to flavors extracted from plants, animals or minerals. Common sources of natural flavors include: (1) Plant sources: Many flavors come from the flowers, fruits, leaves, roots, bark and other parts of plants. For example, rose essence comes from rose flowers, and mint essence comes from mint leaves; (2) Animal sources: Some flavor ingredients such as musk and ambergris come from secretions in animals. These ingredients are often used in high-end perfumes, but due to ethical and environmental reasons, the use of animal-derived flavors has gradually decreased; (3) Mineral sources: Certain minerals, such as calcite, can also be used to make flavors.
[0004] The composition of essence can be very complex and is usually formed by mixing various fragrance components in specific proportions. The components of fragrance generally include the following categories: (1) Alcohols: such as vanillyl alcohol, phenethyl alcohol, α-terpineol, linalool, etc., which have the characteristics of floral or sweet fragrance; (2) Terpenes: α-pinene, β-pinene, γ-terpinene, etc. (2) Aldehydes: such as vanillin, cinnamaldehyde, etc., which usually have strong and unique aromas; (3) Esters: such as heptyl acetate, neryl acetate, geranyl propionate, etc., which often have fruity aromas; (4) Ethers: such as aromatic ethers, which are often used to create complex aromas; (5) Ketones: such as vanillone, rose ketone, etc., which have unique fragrances.
[0005] At present, the extraction methods of essence mainly include steam distillation method, solvent extraction method, pressing method, etc. The production of essence by steam distillation method is divided into three methods: steam distillation in water, steam distillation on water, and steam distillation with steam. Generally, steam distillation in water is mostly used to extract essence. This method utilizes that water molecules are easy to penetrate into the peel cell tissue, water displaces the essential oil, and the essential oil diffuses into the water, forming an oil-water azeotrope and being distilled out simultaneously under the action of steam. The solvent extraction method mainly relies on the extraction principle of organic solvents to achieve the extraction of essence. Patent CN118207043A discloses a rosemary essential oil composition for slimming and firming the skin. In this invention, rosemary, geranium, lemon, lotus leaf, and marjoram are crushed and mixed, then an ethanol aqueous solution is added, heated, stirred, cooled, filtered, and the filtrate is concentrated to obtain a concentrate; an extractant composed of an aqueous phase and an organic phase of an organic solvent is added, heated for extraction, the aqueous phase is removed, and the organic solvent in the organic phase is removed to finally obtain the rosemary essential oil composition. However, since most essences have low water solubility and high volatility and are very unstable under adverse conditions such as oxygen, light, and high temperature, the amount of extracted essence is small and it is not easy to preserve.
[0006] Patent CN117903875A discloses an endogenous fragrance of aromatic plants, its preparation method, and an atomized essence. This invention uses supercritical CO2 extraction method to extract the fragrance. This method has high costs, expensive equipment, and high requirements for operation technology, and is not suitable for large-scale use.
[0007] Blueberries are edible fruits containing rich natural fragrance components such as alcohols, esters, and terpenes. Extracting from them and then preparing them into essence has the advantages of transparent source and safe components. Designing a preparation method that can avoid the effects of high-temperature volatilization and high-temperature oxidation inactivation, etc., on the extraction of fragrance from blueberries to prepare essence, and thus enable the prepared essence to have a long-lasting fragrance effect, is of great significance. Summary of the Invention
[0008] In view of the deficiencies of the prior art, the present invention mixes and stirs a blueberry extract encapsulated with modified poly-L-dopa, deionized water, a surfactant, and a co-surfactant to form an essence composition, avoiding the defects caused by high-temperature extraction methods such as steam, so that the prepared essence composition has a long-lasting fragrance effect, thereby solving the technical problems raised in the background art. Specifically, the technical solution of the present invention includes the following contents:
[0009] An essence composition based on blueberry extract, the essence composition comprising the following raw materials in parts by weight:
[0010] 14 to 20 parts by weight of blueberry extract inclusion, 50 to 60 parts by weight of deionized water, 3 to 4 parts by weight of surfactant, and 1 to 2 parts by weight of co-surfactant.
[0011] Further, the preparation method of the blueberry extract inclusion comprises the following steps:
[0012] An antibacterial monomer, an enol compound, ammonium persulfate, and an ethanol solution are mixed and dispersed in a weight ratio of 1:1 to 2:0.009:30 and reacted in a temperature environment of 30°C to 40°C for 60 min to 70 min to obtain a hydroxy-terminated modified eugenol prepolymer;
[0013] The hydroxy-terminated modified eugenol prepolymer, L-dopa, dichloromethane, and an esterification catalyst are mixed and ultrasonically dispersed in a weight ratio of 1:1 to 2:80:2.5 and reacted at 25°C for 15 h to 20 h to obtain an esterified L-dopa-prepolymer;
[0014] The esterified L-dopa-prepolymer, blueberry extract, and Tris-HCl buffer are mixed and ultrasonically dispersed in a weight ratio of 2:1:100 and reacted at 25°C for 24 h to 30 h to obtain a blueberry extract inclusion.
[0015] Further, the antibacterial monomer includes eugenol.
[0016] Further, the enol compound includes 3-buten-1-ol.
[0017] Further, the esterification catalyst is composed of EDC hydrochloride, 4-dimethylaminopyridine, and triethylamine in a weight ratio of 1:0.7:0.8.
[0018] Further, the preparation method of the blueberry extract comprises the following steps:
[0019] An oxidized coconut shell activated carbon loaded with hydrolytic enzyme and blueberry slurry are mixed in a weight ratio of 1:80 to 100 to form a mixed solution. After adjusting the pH value of the mixed solution to 4.5 to 5.0, it is hydrolyzed at 40°C to 50°C for 70 min to 80 min to obtain a hydrolyzed solution;
[0020] The hydrolyzate and the mixed extractant are mixed in a weight ratio of 1:1 and placed under the condition of 30°C to 40°C for extraction for 2h to 3h to obtain an extraction phase, and the extraction phase is successively subjected to vacuum distillation and freeze-drying to obtain blueberry extract.
[0021] Furthermore, the preparation method of the oxidized coconut shell activated carbon loaded with hydrolase includes the following steps:
[0022] Coconut shell powder, inorganic acid and purified water are mixed and impregnated in a weight ratio of 1:1-1.2:10-15 to obtain an impregnation solution, and the impregnation solution is pyrolyzed at 500°C to 600°C for 80min to 90min to obtain coconut shell activated carbon;
[0023] The coconut shell activated carbon and the nitric acid solution are mixed in a weight ratio of 1:10-12 and oxidized for 4h to 5h to obtain oxidized coconut shell activated carbon;
[0024] The oxidized coconut shell activated carbon, phosphate buffer solution, hydrolase, ethylenediamine, EDC hydrochloride and N-hydroxysuccinimide are mixed and dispersed in a weight ratio of 5:100:0.1-0.2:0.1:5.5:5.5 and reacted at 25°C for 15h to 18h to obtain oxidized coconut shell activated carbon loaded with hydrolase.
[0025] Furthermore, the inorganic acid is phosphoric acid.
[0026] Furthermore, the mass concentration of the nitric acid solution is 40%.
[0027] Furthermore, the hydrolase is xylanase.
[0028] Furthermore, the mixed extractant is composed of petroleum ether and ethyl acetate mixed in a weight ratio of 4:2.
[0029] Furthermore, the surfactant includes Tween-80.
[0030] Furthermore, the co-surfactant includes ethanol.
[0031] A preparation method of a flavor composition based on blueberry extract, the preparation method includes the following steps:
[0032] The blueberry extract inclusion, deionized water, surfactant and co-surfactant are mixed and homogenized at a rotation speed of 9000-10000r / min for 2-4min to obtain a flavor composition.
[0033] Compared with the prior art, the beneficial effects of the present invention are as follows:
[0034] The present invention first conducts high-temperature pyrolysis carbonization and oxidation on coconut shells with a relatively high cellulose content to prepare oxidized coconut shell activated carbon with a relatively low specific surface area. Cellulose is a natural polymer with a linear chain structure, and it is easy to form a microporous network structure after carbonization. Subsequently, through the cross-linking action of the cross-linking agent ethylenediamine, the hydrolase for hydrolyzing plant cell walls is immobilized on the surface of the oxidized coconut shell activated carbon with a relatively low specific surface area to obtain oxidized coconut shell activated carbon loaded with hydrolase. The advantage of immobilizing the hydrolysis solution on the surface of the oxidized coconut shell activated carbon with a relatively low specific surface area is that, on the one hand, the binding of the hydrolase can be used to further reduce the specific surface area of the oxidized coconut shell activated carbon. The reduction of the specific surface area can weaken the adsorption of the flavor components in blueberries by the oxidized coconut shell activated carbon. On the other hand, since the hydrolase needs to be inactivated at high temperature after hydrolysis, the high-temperature inactivation will cause volatilization and oxidative inactivation of the flavor components in blueberries. By immobilizing the hydrolase on the surface of the oxidized coconut shell activated carbon, after the enzymatic hydrolysis is completed, the oxidized coconut shell activated carbon loaded with hydrolase can be removed by filtration, thus avoiding the process step of high-temperature inactivation, and can retain the essence components in blueberries to a large extent. The blueberry slurry is hydrolyzed and broken by the oxidized coconut shell activated carbon loaded with hydrolase, and then filtered to obtain a hydrolysis solution. Then, an extraction agent composed of a mixture of petroleum ether and ethyl acetate is used to extract the hydrolysis solution to obtain an extraction phase. The extraction phase is freeze-dried after removing the extraction agent by vacuum distillation to obtain a blueberry extract. A terminal hydroxyl group-modified eugenol prepolymer is obtained by reacting the monomer substance eugenol with antibacterial activity and the compound 3-buten-1-ol with an enol structure. The terminal hydroxyl group-modified eugenol prepolymer is reacted with levodopa to obtain an esterified levodopa-prepolymer. The esterified levodopa-prepolymer is reacted with the blueberry extract to obtain a blueberry extract inclusion. The blueberry extract inclusion, deionized water, surfactant, and co-surfactant are mixed and stirred to form a flavor composition. The terminal hydroxyl group-modified eugenol prepolymer can not only weaken the cross-linking density of the oxidative self-polymerization of levodopa through the steric hindrance structure of the carbon chain and benzene ring, reducing the excessive cross-linking degree that causes the encapsulated blueberry extract to be unable to be slowly released. Moreover, eugenol itself has a fragrance and antibacterial activity, which can not only enhance the fragrance synergistically with the blueberry extract but also reduce the defect of the short storage time of the prepared flavor composition caused by microbial parasitism and spoilage through its antibacterial activity. Through the oxidative self-polymerization encapsulation effect of the esterified levodopa-prepolymer, the slow release and volatilization of the blueberry extract are realized, thereby prolonging the fragrance retention effect of the prepared flavor composition. Detailed Embodiments
[0035] The following will clearly and completely describe the technical solutions of the present invention through the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative efforts fall within the protection scope of the present invention.
[0036] Unless otherwise specified, the raw materials and reagents used in the present invention below are all commercially available products or can be prepared by known methods.
[0037] Preparation Example 1:
[0038] A method for preparing oxidized coconut shell activated carbon loaded with hydrolase specifically includes the following process:
[0039] Wash the coconut shell with water, then put it in an oven at 60 °C to dry and remove water until constant weight. After cooling to room temperature, take out the coconut shell and crush it with a crusher, and then sieve it with a 50-mesh sieve to obtain coconut shell powder. Weigh 20 g of coconut shell powder and 20 g of phosphoric acid, then add 200 g of purified water and mix and stir at a speed of 400 r / min for 40 min, and then place it in an environment at 50 °C for impregnation treatment for 10 h. After the impregnation treatment, dry and pre-treat the impregnation solution in an oven at 110 °C to remove water, and then put it into a tubular furnace, discharge oxygen with nitrogen and maintain a nitrogen atmosphere. Heat it up to 500 °C at a heating rate of 5 °C / min, and pyrolyze it in this temperature environment for 80 min. After the pyrolysis, cool it naturally to room temperature and take it out, wash it with deionized water until the pH value of the rinsing water is neutral, and then dry it to obtain coconut shell activated carbon. Weigh 10 g of coconut shell activated carbon and put it into a beaker, add 100 g of nitric acid solution with a mass concentration of 40% and mix, and oxidize it in an environment at 25 °C for 4 h. After the oxidation treatment, filter and wash it until the pH value of the rinsing water is neutral, and then dry it to obtain oxidized coconut shell activated carbon (the specific surface area of the oxidized coconut shell activated carbon measured by a static liquid nitrogen adsorption instrument is 307.46 m 2 / g; the carboxyl group content of the oxidized coconut shell activated carbon measured by the "Boehm titration method" is 0.223 mmol / g);
[0040] Add 5 g of oxidized coconut shell activated carbon to 100 g of phosphate buffer solution with a pH value of 6.5, and disperse it with an ultrasonic disperser at an ultrasonic power of 400 W for 15 min to obtain a dispersion liquid. Add 0.1 g of hydrolase xylanase, 0.1 g of ethylenediamine, 5.5 g of EDC hydrochloride and 5.5 g of N-hydroxysuccinimide to the dispersion liquid, mix them and place them in a water bath at a temperature of 25 °C for timing reaction for 15 h. After the reaction, filter and wash with water until the pH of the rinsing water is neutral to obtain oxidized coconut shell activated carbon loaded with hydrolase.
[0041] Preparation Example 2:
[0042] A method for preparing oxidized coconut shell activated carbon loaded with hydrolase specifically includes the following process:
[0043] The coconut shell was washed clean with water and then placed in an oven at 60 °C to dry and remove water until a constant weight was achieved. After cooling to room temperature, the coconut shell was taken out and crushed using a crusher, and then sieved through a 50-mesh sieve to obtain coconut shell powder. 20 g of coconut shell powder was weighed and mixed with 22 g of phosphoric acid, and then 250 g of purified water was added and mixed and stirred at a speed of 400 r / min for 45 min. Subsequently, it was placed in an environment at 50 °C for impregnation treatment for 10 h. After the impregnation treatment was completed, the impregnation solution was placed in an oven at 110 °C for drying and pre-treatment to remove water, and then placed in a tube furnace. Oxygen was discharged with nitrogen and a nitrogen atmosphere was maintained. It was heated to 550 °C at a heating rate of 5 °C / min and pyrolyzed at this temperature for 85 min. After the pyrolysis was completed, it was naturally cooled to room temperature and taken out, rinsed with deionized water until the pH value of the rinsing water was neutral, and then dried to obtain coconut shell activated carbon. 10 g of coconut shell activated carbon was weighed and placed in a beaker, 110 g of a nitric acid solution with a mass concentration of 40% was added and mixed, and oxidation treatment was carried out at a temperature of 30 °C for 4.5 h. After the oxidation treatment was completed, it was filtered and rinsed until the pH value of the rinsing water was neutral, and then dried to obtain oxidized coconut shell activated carbon (the specific surface area of the oxidized coconut shell activated carbon measured by a static liquid nitrogen adsorption instrument was 321.88 m 2 / g; the carboxyl group content of the oxidized coconut shell activated carbon measured by the "Boehm titration method" was 0.226 mmol / g);
[0044] 5 g of oxidized coconut shell activated carbon was added to 100 g of phosphate buffer solution with a pH value of 6.5 and dispersed with an ultrasonic disperser at an ultrasonic power of 400 W for 15 min to obtain a dispersion. 0.15 g of hydrolytic enzyme xylanase, 0.1 g of ethylenediamine, 5.5 g of EDC hydrochloride and 5.5 g of N-hydroxysuccinimide were added to the dispersion and mixed, and placed in a water bath at a temperature of 25 °C for timed reaction for 17 h. After the reaction was completed, it was filtered and washed with water until the pH of the rinsing water was neutral to obtain oxidized coconut shell activated carbon loaded with hydrolytic enzyme.
[0045] Preparation Example 3:
[0046] A method for preparing oxidized coconut shell activated carbon loaded with hydrolytic enzyme, specifically including the following process:
[0047] Wash the coconut shell with water, and then place it in an oven at 60 °C to dry and remove water until it reaches a constant weight. After cooling to room temperature, take out the coconut shell and crush it with a crusher, and then sieve it with a 50-mesh sieve to obtain coconut shell powder. Weigh 20 g of coconut shell powder and mix it with 24 g of phosphoric acid, and then add 300 g of purified water and mix and stir at a speed of 400 r / min for 50 min. Subsequently, place it in an environment at 50 °C for impregnation treatment for 10 h. After the impregnation treatment, put the impregnation solution in an oven at 110 °C to dry and pre-treat to remove water, and then put it into a tubular furnace, use nitrogen to discharge oxygen and maintain a nitrogen atmosphere. Heat it up to 600 °C at a heating rate of 5 °C / min, and carry out pyrolysis treatment for 90 min in this temperature environment. After the pyrolysis is completed, naturally cool it to room temperature and take it out, rinse it with deionized water until the pH value of the rinsing water is neutral, and then dry it to obtain coconut shell activated carbon. Weigh 10 g of coconut shell activated carbon and put it into a beaker, add 120 g of nitric acid solution with a mass concentration of 40% and mix, and carry out oxidation treatment at a temperature of 30 °C for 5 h. After the oxidation treatment, filter and rinse until the pH value of the rinsing water is neutral, and then dry it to obtain oxidized coconut shell activated carbon (the specific surface area of the oxidized coconut shell activated carbon measured by a static liquid nitrogen adsorption instrument is 330.27 m 2 / g; the carboxyl group content of the oxidized coconut shell activated carbon measured by the "Boehm titration method" is 0.228 mmol / g);
[0048] Add 5 g of oxidized coconut shell activated carbon to 100 g of phosphate buffer solution with a pH value of 6.5, and disperse it with an ultrasonic disperser at an ultrasonic power of 400 W for 15 min to obtain a dispersion. Add 0.2 g of hydrolytic enzyme xylanase, 0.1 g of ethylenediamine, 5.5 g of EDC hydrochloride and 5.5 g of N-hydroxysuccinimide to the dispersion and mix, and place it in a temperature environment with a water bath temperature of 25 °C and time the reaction for 15 - 18 h. After the reaction, filter and wash with water until the pH of the rinsing water is neutral to obtain oxidized coconut shell activated carbon loaded with hydrolytic enzyme.
[0049] Preparation Example 4:
[0050] A preparation method of oxidized coconut shell activated carbon loaded with hydrolytic enzyme, specifically including the following process:
[0051] Increase the dosage of phosphoric acid in Preparation Example 3 to 30 g, and increase the pyrolysis temperature from 600 °C to 700 °C. The specific surface area of the obtained oxidized coconut shell activated carbon measured by a static liquid nitrogen adsorption instrument is 608.51 m 2 / g; the carboxyl group content of the oxidized coconut shell activated carbon measured by the "Boehm titration method" is 0.311 mmol / g;
[0052] The remaining preparation conditions are the same as those in Preparation Example 3.
[0053] Preparation Example 5:
[0054] Preparation method of oxidized coconut shell activated carbon loaded with hydrolytic enzyme, specifically including the following process:
[0055] Replace the xylanase of the hydrolytic enzyme in Preparation Example 3 with cellulase, and keep the remaining preparation conditions the same as those in Preparation Example 3.
[0056] Preparation Example 6:
[0057] Preparation method of blueberry extract, specifically including the following process:
[0058] Wash the blueberries, and then according to the weight ratio of blueberries to water of 1:50, put the blueberries and water together into a pulverizer to pulverize and beat into a pulp to obtain blueberry slurry. Weigh 1 part by weight of the oxidized coconut shell activated carbon loaded with hydrolytic enzyme obtained in Preparation Example 1 and 80 parts by weight of blueberry slurry, mix and stir them evenly to form a dispersion. Slowly add dilute hydrochloric acid to the dispersion to adjust the pH value of the dispersion to 4.5 - 5.0. Then place it in a water bath at 40 °C for constant temperature hydrolysis for 70 min. After the hydrolysis is completed, first centrifuge to remove the blueberry residue, and then filter to remove the oxidized coconut shell activated carbon loaded with hydrolytic enzyme to obtain a hydrolyzate;
[0059] Weigh equal parts by weight of the hydrolyzate and a mixed extractant (composed of petroleum ether and ethyl acetate mixed according to the weight ratio of 4:2), mix and stir, and place it in a water bath at 30 °C and stir and extract at a rotation speed of 200 r / min for 2 h. After the extraction is completed, let it stand for stratification and collect the extraction phase. Place the extraction phase in a rotary evaporator for reduced pressure evaporation to remove petroleum ether and ethyl acetate, and then put it into a freeze dryer for freeze drying to obtain blueberry extract.
[0060] Preparation Example 7:
[0061] Preparation method of blueberry extract, specifically including the following process:
[0062] Wash the blueberries, and then according to the weight ratio of blueberries to water of 1:50, put the blueberries and water together into a pulverizer to pulverize and beat into a pulp to obtain blueberry slurry. Weigh 1 part by weight of the oxidized coconut shell activated carbon loaded with hydrolytic enzyme obtained in Preparation Example 2 and 90 parts by weight of blueberry slurry, mix and stir them evenly to form a dispersion. Slowly add dilute hydrochloric acid to the dispersion to adjust the pH value of the dispersion to 4.5 - 5.0. Then place it in a water bath at 45 °C for constant temperature hydrolysis for 75 min. After the hydrolysis is completed, first centrifuge to remove the blueberry residue, and then filter to remove the oxidized coconut shell activated carbon loaded with hydrolytic enzyme to obtain a hydrolyzate;
[0063] Weigh equal parts by weight of the hydrolyzate and the mixed extractant (composed of petroleum ether and ethyl acetate mixed in a weight ratio of 4:2), mix and stir them, and place them in a water bath at 35°C and stir and extract at a speed of 200 r / min for 2.5 h. After the extraction is completed, let it stand for layering and collect the extraction phase. Place the extraction phase in a rotary evaporator for reduced-pressure evaporation to remove petroleum ether and ethyl acetate, and then put it into a freeze dryer for freeze-drying to obtain blueberry extract.
[0064] Preparation Example 8:
[0065] A method for preparing blueberry extract, specifically including the following process:
[0066] Wash the blueberries, and then according to the weight ratio of blueberries to water of 1:50, put the blueberries and water together into a crusher for crushing and pulping to obtain blueberry slurry. Weigh 1 part by weight of the oxidized coconut shell activated carbon loaded with hydrolytic enzyme obtained in Preparation Example 1 and 100 parts by weight of blueberry slurry, mix and stir them evenly to form a dispersion. Slowly add dilute hydrochloric acid to the dispersion to adjust the pH value of the dispersion to 4.5 - 5.0. Then place it in a water bath at 50°C for constant-temperature hydrolysis for 80 min. After the hydrolysis is completed, first centrifuge to remove blueberry residues, and then filter to remove the oxidized coconut shell activated carbon loaded with hydrolytic enzyme to obtain the hydrolyzate;
[0067] Weigh equal parts by weight of the hydrolyzate and the mixed extractant (composed of petroleum ether and ethyl acetate mixed in a weight ratio of 4:2), mix and stir them, and place them in a water bath at 40°C and stir and extract at a speed of 200 r / min for 3 h. After the extraction is completed, let it stand for layering and collect the extraction phase. Place the extraction phase in a rotary evaporator for reduced-pressure evaporation to remove petroleum ether and ethyl acetate, and then put it into a freeze dryer for freeze-drying to obtain blueberry extract.
[0068] Preparation Example 9:
[0069] A method for preparing blueberry extract, specifically including the following process:
[0070] Replace the oxidized coconut shell activated carbon loaded with hydrolytic enzyme in Preparation Example 8 with the oxidized coconut shell activated carbon loaded with hydrolytic enzyme obtained in Preparation Example 4, and keep the other preparation conditions the same as those in Preparation Example 8.
[0071] Preparation Example 10:
[0072] A method for preparing blueberry extract, specifically including the following process:
[0073] Replace the oxidized coconut shell activated carbon loaded with hydrolytic enzyme in Preparation Example 8 with the oxidized coconut shell activated carbon loaded with hydrolytic enzyme obtained in Preparation Example 5, and keep the other preparation conditions the same as those in Preparation Example 8.
[0074] Preparation Example 11:
[0075] Preparation method of blueberry extract inclusion body, specifically including the following process:
[0076] Add 1 part by weight of eugenol and 1 part by weight of 3-buten-1-ol into 30 parts by weight of ethanol solution, mix and stir, then add 0.009 part by weight of ammonium persulfate and continue to mix and stir until completely dispersed. Then place the dispersed mixture in a water bath at 30 °C and time the reaction for 60 min. Immediately pour the reaction mixture into a dialysis bag with a molecular weight cut-off of 500 Da after the reaction is completed, and dialyze with deionized water for 2 days to obtain a hydroxy-terminated modified eugenol prepolymer;
[0077] Add 1 part by weight of hydroxy-terminated modified eugenol prepolymer and 1 part by weight of levodopa into 80 parts by weight of dichloromethane. Subsequently, add an esterification catalyst composed of 1 part by weight of EDC hydrochloride, 0.7 part by weight of 4-dimethylaminopyridine, and 0.8 part by weight of triethylamine, mix and stir, and place it in an ultrasonic disperser for dispersion treatment at a power of 300 W for 20 min. After the dispersion treatment is completed, place it in a temperature environment of 25 °C and time the reaction for 15 h. Immediately pour the reaction mixture into a dialysis bag with a molecular weight cut-off of 500 Da after the reaction is completed, and dialyze with deionized water for 2 days to obtain an esterified levodopa-prepolymer;
[0078] Weigh 2 parts by weight of esterified levodopa-prepolymer and 1 part by weight of the blueberry extract obtained in Preparation Example 6, add them to 100 parts by weight of Tris-hydrochloride buffer solution, mix, and place it in an ultrasonic disperser for dispersion treatment at a power of 400 W for 20 min. After the dispersion treatment is completed, place it in a temperature environment of 25 °C and time the reaction for 24 h. Immediately pour the reaction mixture into a dialysis bag with a molecular weight cut-off of 500 Da after the reaction is completed, and dialyze with deionized water for 2 days to obtain a blueberry extract inclusion body.
[0079] Preparation Example 12:
[0080] Preparation method of blueberry extract inclusion body, specifically including the following process:
[0081] Add 1 part by weight of eugenol and 1.5 parts by weight of 3-buten-1-ol into 30 parts by weight of ethanol solution, mix and stir, then add 0.009 part by weight of ammonium persulfate and continue to mix and stir until completely dispersed. Then place the dispersed mixture in a water bath at 35 °C and time the reaction for 65 min. Immediately pour the reaction mixture into a dialysis bag with a molecular weight cut-off of 500 Da after the reaction is completed, and dialyze with deionized water for 2 days to obtain a hydroxy-terminated modified eugenol prepolymer;
[0082] 1 part by weight of the hydroxyl-terminated modified eugenol prepolymer and 1.5 parts by weight of levodopa were added to 80 parts by weight of dichloromethane. Subsequently, an esterification catalyst composed of 1 part by weight of EDC hydrochloride, 0.7 part by weight of 4-dimethylaminopyridine, and 0.8 part by weight of triethylamine was added, and the mixture was stirred and placed in an ultrasonic disperser for dispersion treatment at a power of 300 W for 20 min. After the dispersion treatment, it was placed in a temperature environment of 25 °C and timed for reaction for 18 h. After the reaction was completed, it was immediately poured into a dialysis bag with a molecular weight cut-off of 500 Da and dialyzed with deionized water for 2 days to obtain the esterified levodopa-prepolymer;
[0083] 2 parts by weight of the esterified levodopa-prepolymer and 1 part by weight of the blueberry extract obtained in Preparation Example 7 were weighed and added to 100 parts by weight of Tris-hydrochloride buffer solution, mixed, and placed in an ultrasonic disperser for dispersion treatment at a power of 400 W for 20 min. After the dispersion treatment, it was placed in a temperature environment of 25 °C and timed for reaction for 28 h. After the reaction was completed, it was immediately poured into a dialysis bag with a molecular weight cut-off of 500 Da and dialyzed with deionized water for 2 days to obtain the blueberry extract inclusion;
[0084] Preparation Example 13:
[0085] A preparation method of a blueberry extract inclusion, specifically including the following process:
[0086] 1 part by weight of eugenol and 2 parts by weight of 3-buten-1-ol were added to 30 parts by weight of an ethanol solution, mixed and stirred, 0.009 part by weight of ammonium persulfate was added, and the mixture was continuously stirred until completely dispersed. Then, the dispersed mixture was placed in a water bath at 40 °C and timed for reaction for 70 min. After the reaction was completed, it was immediately poured into a dialysis bag with a molecular weight cut-off of 500 Da and dialyzed with deionized water for 2 days to obtain the hydroxyl-terminated modified eugenol prepolymer;
[0087] 1 part by weight of the hydroxyl-terminated modified eugenol prepolymer and 2 parts by weight of levodopa were added to 80 parts by weight of dichloromethane. Subsequently, an esterification catalyst composed of 1 part by weight of EDC hydrochloride, 0.7 part by weight of 4-dimethylaminopyridine, and 0.8 part by weight of triethylamine was added, and the mixture was stirred and placed in an ultrasonic disperser for dispersion treatment at a power of 300 W for 20 min. After the dispersion treatment, it was placed in a temperature environment of 25 °C and timed for reaction for 20 h. After the reaction was completed, it was immediately poured into a dialysis bag with a molecular weight cut-off of 500 Da and dialyzed with deionized water for 2 days to obtain the esterified levodopa-prepolymer;
[0088] Weigh 2 parts by weight of esterified L-DOPA-prepolymer and 1 part by weight of the blueberry extract obtained in Preparation Example 8, add them together to 100 parts by weight of Tris-hydrochloride buffer solution, mix them, and place them in an ultrasonic disperser for dispersion treatment at a power of 400 W for 20 min. After the dispersion treatment, place them in a temperature environment of 25 °C and start timing the reaction for 30 h. Immediately after the reaction is completed, pour them into a dialysis bag with a molecular weight cut-off of 500 Da and dialyze them with deionized water for 2 days to obtain blueberry extract inclusion bodies.
[0089] Preparation Example 14:
[0090] A method for preparing blueberry extract inclusion bodies, specifically including the following process:
[0091] Replace the blueberry extract in Preparation Example 13 with the blueberry extract obtained in Preparation Example 9, and keep the remaining preparation conditions the same as those in Preparation Example 13.
[0092] Preparation Example 15:
[0093] A method for preparing blueberry extract inclusion bodies, specifically including the following process:
[0094] Replace the blueberry extract in Preparation Example 13 with the blueberry extract obtained in Preparation Example 10, and keep the remaining preparation conditions the same as those in Preparation Example 13.
[0095] Preparation Example 16:
[0096] A method for preparing blueberry extract inclusion bodies, specifically including the following process:
[0097] Increase the ammonium persulfate in Preparation Example 13 to 0.12 parts by weight and extend the reaction time of 70 min to 2 h, and keep the remaining preparation conditions the same as those in Preparation Example 13.
[0098] Preparation Example 17:
[0099] A method for preparing blueberry extract inclusion bodies, specifically including the following process:
[0100] Replace 3-buten-1-ol in Preparation Example 13 with cis-3-hexen-1-ol, and keep the remaining preparation conditions the same as those in Preparation Example 13.
[0101] Preparation Example 18:
[0102] A method for preparing blueberry extract inclusion bodies, specifically including the following process:
[0103] Add 1 part by weight of chitosan and 2 parts by weight of levodopa to 80 parts by weight of deionized water, and then place it in an ultrasonic disperser for dispersion treatment at a power of 300 W for 20 min. After the dispersion treatment, place it in a temperature environment of 25 °C and time the reaction for 20 h. Immediately after the reaction, pour it into a dialysis bag with a molecular weight cut-off of 500 Da and dialyze it with deionized water for 2 days to obtain a chitosan crosslinked levodopa mixture;
[0104] Weigh 2 parts by weight of the chitosan crosslinked levodopa mixture and 1 part by weight of the blueberry extract obtained in Preparation Example 8, add them to 100 parts by weight of Tris-hydrochloride buffer solution, mix them, and place them in an ultrasonic disperser for dispersion treatment at a power of 400 W for 20 min. After the dispersion treatment, place it in a temperature environment of 25 °C and time the reaction for 30 h. After the reaction, it was found that the gel solidified and the preparation failed.
[0105] This may be because although chitosan also has antibacterial properties and can form crosslinked adsorption with levodopa through hydrogen bonds, thereby realizing the encapsulation of the blueberry extract. However, since chitosan itself contains more functional groups that form hydrogen bond crosslinks, it is easy to form a relatively dense three-dimensional network structure through crosslinking, which may lead to serious gelation phenomenon, resulting in the failure of the preparation and making it unusable. It can be seen that the selection of antibacterial monomers has relatively strict requirements in the system of the present invention. If a natural polymer antibacterial material is used, although antibacterial can be achieved, improper proportion control is likely to cause gel solidification, which is not conducive to use.
[0106] Preparation Example 19:
[0107] A preparation method of a blueberry extract inclusion, specifically including the following process:
[0108] Add 1 part by weight of 3-buten-1-ol and 2 parts by weight of levodopa to 80 parts by weight of dichloromethane, and then add an esterification catalyst composed of 1 part by weight of EDC hydrochloride, 0.7 part by weight of 4-dimethylaminopyridine, and 0.8 part by weight of triethylamine, mix and stir, and place it in an ultrasonic disperser for dispersion treatment at a power of 300 W for 20 min. After the dispersion treatment, place it in a temperature environment of 25 °C and time the reaction for 20 h. Immediately after the reaction, pour it into a dialysis bag with a molecular weight cut-off of 500 Da and dialyze it with deionized water for 2 days to obtain an esterified levodopa prepolymer;
[0109] Weigh 2 parts by weight of esterified levodopa-prepolymer and 1 part by weight of the blueberry extract obtained in Preparation Example 8, add them to 100 parts by weight of Tris-hydrochloride buffer solution, mix them, and place them in an ultrasonic disperser for dispersion treatment at a power of 400 W for 20 min. After the dispersion treatment, place them in a temperature environment of 25 °C and time the reaction for 30 h. Immediately after the reaction is completed, pour them into a dialysis bag with a molecular weight cut-off of 500 Da, and perform dialysis treatment with deionized water for 2 days to obtain blueberry extract inclusion bodies.
[0110] Example 1:
[0111] A preparation method of a flavor composition based on blueberry extract specifically includes the following process:
[0112] Weigh 14 parts by weight of the blueberry extract inclusion bodies obtained in Preparation Example 11, 50 parts by weight of deionized water, 3 parts by weight of the surfactant Tween-80, and 1 part by weight of the co-surfactant ethanol, mix them and put them into a homogenizer, and then perform homogenization treatment at a rotation speed of 9000 r / min for 2 min to obtain a flavor composition.
[0113] Example 2:
[0114] A preparation method of a flavor composition based on blueberry extract specifically includes the following process:
[0115] Weigh 18 parts by weight of the blueberry extract inclusion bodies obtained in Preparation Example 12, 55 parts by weight of deionized water, 3.5 parts by weight of the surfactant Tween-80, and 1.5 parts by weight of the co-surfactant ethanol, mix them and put them into a homogenizer, and then perform homogenization treatment at a rotation speed of 10000 r / min for 3 min to obtain a flavor composition.
[0116] Example 3:
[0117] A preparation method of a flavor composition based on blueberry extract specifically includes the following process:
[0118] Weigh 20 parts by weight of the blueberry extract inclusion bodies obtained in Preparation Example 13, 60 parts by weight of deionized water, 4 parts by weight of the surfactant Tween-80, and 2 parts by weight of the co-surfactant ethanol, mix them and put them into a homogenizer, and then perform homogenization treatment at a rotation speed of 10000 r / min for 4 min to obtain a flavor composition.
[0119] Comparative Example 1:
[0120] A preparation method of a flavor composition based on blueberry extract specifically includes the following process:
[0121] Weigh 20 parts by weight of the blueberry extract inclusion obtained in Preparation Example 14, 60 parts by weight of deionized water, 4 parts by weight of the surfactant Tween-80, and 2 parts by weight of the co-surfactant ethanol, mix them and put them into a homogenizer, and then homogenize them at a speed of 10,000 r / min for 4 min to obtain the flavor composition.
[0122] Comparative Example 2:
[0123] A method for preparing a flavor composition based on blueberry extract specifically includes the following process:
[0124] Weigh 20 parts by weight of the blueberry extract inclusion obtained in Preparation Example 15, 60 parts by weight of deionized water, 4 parts by weight of the surfactant Tween-80, and 2 parts by weight of the co-surfactant ethanol, mix them and put them into a homogenizer, and then homogenize them at a speed of 10,000 r / min for 4 min to obtain the flavor composition.
[0125] Comparative Example 3:
[0126] A method for preparing a flavor composition based on blueberry extract specifically includes the following process:
[0127] Weigh 20 parts by weight of the blueberry extract inclusion obtained in Preparation Example 16, 60 parts by weight of deionized water, 4 parts by weight of the surfactant Tween-80, and 2 parts by weight of the co-surfactant ethanol, mix them and put them into a homogenizer, and then homogenize them at a speed of 10,000 r / min for 4 min to obtain the flavor composition.
[0128] Comparative Example 4:
[0129] A method for preparing a flavor composition based on blueberry extract specifically includes the following process:
[0130] Weigh 20 parts by weight of the blueberry extract inclusion obtained in Preparation Example 17, 60 parts by weight of deionized water, 4 parts by weight of the surfactant Tween-80, and 2 parts by weight of the co-surfactant ethanol, mix them and put them into a homogenizer, and then homogenize them at a speed of 10,000 r / min for 4 min to obtain the flavor composition.
[0131] Comparative Example 5:
[0132] A method for preparing a flavor composition based on blueberry extract specifically includes the following process:
[0133] Weigh 20 parts by weight of the blueberry extract inclusion obtained in Preparation Example 19, 60 parts by weight of deionized water, 4 parts by weight of the surfactant Tween-80, and 2 parts by weight of the co-surfactant ethanol, mix them and put them into a homogenizer, and then homogenize them at a speed of 10,000 r / min for 4 min to obtain the flavor composition.
[0134] Comparative Example 6:
[0135] A preparation method of an essence composition based on blueberry extract specifically includes the following process:
[0136] Weigh 20 parts by weight of the blueberry extract inclusion obtained in Preparation Example 13, 60 parts by weight of deionized water, 4 parts by weight of the surfactant Tween-80, and 2 parts by weight of the co-surfactant ethanol, mix them and put them into a homogenizer, and then homogenize at a speed of 15,000 r / min for 2 min to obtain the essence composition.
[0137] The essence compositions prepared in Examples 1 to 3 and Comparative Examples 1 to 6 are dropped on the surface of a 5 cm × 2 cm paper, and then at the 1st hour, 12th hour, 24th hour, and 7th day respectively, through volunteers smelling the fragrance, the scores are statistically counted according to the 0-10 scores representing the fragrance from none to strong to evaluate their aroma intensity and fragrance retention time. The results are shown in Table 1 below.
[0138] Table 1 Aroma performance test
[0139] Material source 1st hour fraction 12th hour fraction 24th hour fraction 7th day fraction Example 1 8 8 7 3 Example 2 8 7 7 3 Example 3 6 6 5 4 Comparative Example 1 2 1 0 0 Comparative Example 2 3 2 0 0 Comparative Example 3 3 1 0 0 Comparative Example 4 3 0 0 0 Comparative Example 5 1 0 0 0 Comparative Example 6 8 3 0 0
[0140] Dip the essence compositions prepared in Examples 1 to 3 and Comparative Examples 1 to 6 with a sterilized loop and coat them on a bacterial culture dish until the surface is completely covered. Subsequently, spread the Staphylococcus aureus bacterial solution with a bacterial concentration of 1×10 8 CFU / ml evenly on the bacterial culture dish, then incubate it upside down in a constant temperature incubator at 37°C for 24 h, then take it out to measure the number of bacteria, and calculate the antibacterial rate (using the bacterial culture medium without the essence composition as the blank group, and irradiating and sterilizing the blank group for 12 h under an ultraviolet lamp after culturing for 24 h). The results are shown in Table 2 below.
[0141] Table 2 Antibacterial performance
[0142] Material source Bacteriostatic rate (%) Example 1 48.3 Example 2 52.6 Example 3 54.1 Comparative Example 1 53.4 Comparative Example 2 53.5 Comparative Example 3 53.1 Comparative Example 4 53.5 Comparative Example 5 6.3 Comparative Example 6 53.8 Blank group 61.4
[0143] From the test results in Table 1 and Table 2 above, the following conclusions can be drawn:
[0144] (1) Through Examples 1 to 3, it can be found that in the present invention, the blueberry extract encapsulated by modified poly-L-dopa, deionized water, a surfactant, and a co-surfactant are mixed and stirred to form an essence composition, avoiding the defect problems caused by high-temperature extraction methods such as steam. The prepared essence composition not only has a long-lasting fragrance effect, but also the improvement of the antibacterial effect promotes the reduction of the spoilage of the essence composition caused by microbial parasitism, which is beneficial to storage.
[0145] (2) It can be found from Comparative Example 1 that the aroma intensity of the prepared flavor composition is relatively low and the duration is relatively short. This may be because in this system, when the dosage of inorganic acid phosphoric acid is increased and the pyrolysis temperature is raised, the specific surface area of the prepared activated coconut shell is greatly increased. The increase in the specific surface area enables more adsorption sites to adsorb spice components such as alcohols, esters, and terpenes released after the hydrolysis of blueberries, thereby weakening the original aroma degree. Thus, it can be seen that the present invention has relatively strict restrictions on the specific surface area of the activated carbon. Although a too large specific surface area is beneficial to the loading and fixation of hydrolase, it will also increase the adsorption of spice components, thus weakening the aroma intensity and fragrance retention time of the finally prepared flavor composition.
[0146] (3) It can be found from Comparative Example 2 that the aroma intensity of the prepared flavor composition is relatively low and the duration is relatively short. This may be because although both cellulase and xylanase have the function of hydrolyzing plant cell walls, in this system, the constructed hydrolysis conditions are not conducive to the enzymatic hydrolysis of cellulase, and the hydrolysis effect of blueberries is poor, which may result in less release of spice components such as alcohols, esters, and terpenes, leading to poor performance of the aroma intensity and fragrance retention time of the finally prepared flavor composition.
[0147] (4) It can be found from Comparative Example 3 that the aroma intensity of the prepared flavor composition is relatively low and the duration is relatively short. This may be because ammonium persulfate is used as a radical initiator, and in this system, the dosage is too large and the initiation time is too long, which may lead to too long carbon chain growth. Then, when preparing the esterified levodopa-prepolymer by grafting and introducing levodopa, due to the too long carbon chain, the oxidative self-polymerization of levodopa in a weakly alkaline environment is greatly affected by the carbon chain, and the polymerization crosslinking is poor, which may result in poor encapsulation of blueberry extract, leading to poor performance of the aroma intensity and fragrance retention time of the finally prepared flavor composition.
[0148] (5) It can be found from Comparative Example 4 that the aroma intensity of the prepared flavor composition is relatively low and the duration is relatively short. This may be because cis-3-hexen-1-ol has a longer carbon chain than 3-buten-1-ol. During prepolymerization in this system, it may lead to too long carbon chain growth. Then, when preparing the esterified levodopa-prepolymer by grafting and introducing levodopa, due to the too long carbon chain, the oxidative self-polymerization of levodopa in a weakly alkaline environment is greatly affected by the carbon chain, and the polymerization crosslinking is poor, which may result in poor encapsulation of blueberry extract, leading to poor performance of the aroma intensity and fragrance retention time of the finally prepared flavor composition.
[0149] (6) It can be found from Comparative Example 5 that the aroma intensity of the prepared fragrance composition is relatively low, the duration is relatively short, the antibacterial effect is poor, and the storage time is short. This may be because although 3-buten-1-ol can affect the oxidative self-polymerization of levodopa through the carbon chain, in this system, the amount used may cause the ability to weaken the oxidative self-polymerization of levodopa to be relatively weak, which may result in an overly dense cross-linking degree of oxidative self-polymerization and is not conducive to the release of aroma. Moreover, due to the abandonment of using eugenol, in this system, relying solely on the release of fragrance components such as alcohols, esters, and terpenes in blueberry extract results in relatively weak aroma, and the loss of antibacterial effect may lead to a relatively short storage time of the prepared fragrance composition, which is not conducive to practical use.
[0150] (7) It can be found from Comparative Example 6 that the fragrance retention time of the prepared fragrance composition is relatively poor. This may be because during the homogenization process, although increasing the rotation speed can shorten the homogenization time, an overly high rotation speed may significantly increase the shearing effect, causing the inclusion body to withstand multiple high-intensity shears in a short time, resulting in rupture and loss of the sustained-release effect.
[0151] The above-described embodiments have detailed the technical solutions and beneficial effects of the present invention. It should be understood that the above are only specific embodiments of the present invention and are not used to limit the present invention. Without departing from the spirit and scope of the present invention, the present invention will have various changes and improvements, and these changes and improvements fall within the scope of the present invention claimed.
Claims
1. An essence composition based on blueberry extract, characterized in that, The flavor composition comprises the following raw materials in parts by weight: 14-20 parts by weight of blueberry extract inclusion, 50-60 parts by weight of deionized water, 3-4 parts by weight of surfactant and 1-2 parts by weight of co-surfactant.
2. The essence composition based on blueberry extract according to claim 1, characterized in that, The preparation method of the blueberry extract inclusion comprises the following steps: An antibacterial monomer, an enol compound, ammonium persulfate and an ethanol solution are mixed and dispersed in a weight ratio of 1:1-2:0.009:30 and reacted for 60-70 minutes in a temperature environment of 30°C-40°C to obtain a hydroxy-terminated modified eugenol prepolymer; The hydroxy-terminated modified eugenol prepolymer, L-dopa, dichloromethane and an esterification catalyst are mixed and ultrasonically dispersed in a weight ratio of 1:1-2:80:2.5 and reacted for 15-20 hours at 25°C to obtain an esterified L-dopa-prepolymer; The esterified L-dopa-prepolymer, blueberry extract and Tris-hydrochloride buffer are mixed and ultrasonically dispersed in a weight ratio of 2:1:100 and reacted for 24-30 hours at 25°C to obtain the blueberry extract inclusion.
3. The essence composition based on blueberry extract according to claim 2, characterized in that, The antibacterial monomer includes eugenol.
4. The essence composition based on blueberry extract according to claim 2, characterized in that, The enol compound includes 3-buten-1-ol.
5. The essence composition based on blueberry extract according to claim 2, characterized in that, The preparation method of the blueberry extract comprises the following steps: An oxidized coconut shell activated carbon loaded with hydrolase and blueberry slurry are mixed in a weight ratio of 1:80-100 to form a mixed solution. After adjusting the pH value of the mixed solution to 4.5-5.0, it is hydrolyzed for 70-80 minutes under the condition of 40°C-50°C to obtain a hydrolyzed solution; The hydrolyzed solution and a mixed extractant are mixed in a weight ratio of 1:1 and extracted for 2-3 hours under the condition of 30°C-40°C to obtain an extraction phase. The extraction phase is successively subjected to vacuum distillation and freeze-drying to obtain the blueberry extract.
6. The essence composition based on blueberry extract according to claim 5, characterized in that, The preparation method of the oxidized coconut shell activated carbon loaded with hydrolase comprises the following steps: Coconut shell powder, inorganic acid and purified water are mixed and impregnated in a weight ratio of 1:1-1.2:10-15 to obtain an impregnated solution. The impregnated solution is pyrolyzed at 500°C-600°C for 80-90 minutes to obtain coconut shell activated carbon; The coconut shell activated carbon and a nitric acid solution are mixed and oxidized in a weight ratio of 1:10-12 for 4-5 hours to obtain oxidized coconut shell activated carbon; The oxidized coconut shell activated carbon, phosphate buffer solution, hydrolase, ethylenediamine, EDC hydrochloride and N-hydroxysuccinimide are mixed and dispersed in a weight ratio of 5:100:0.1-0.2:0.1:5.5:5.5 and reacted at 25°C for 15-18 hours to obtain the oxidized coconut shell activated carbon loaded with hydrolase.
7. The essence composition based on blueberry extract according to claim 6, characterized in that, The hydrolase is xylanase.
8. The essence composition based on blueberry extract according to claim 1, wherein, The surfactant includes Tween-80.
9. The essence composition based on blueberry extract according to claim 1, wherein, The co-surfactant includes ethanol.
10. A method for preparing an essence composition based on blueberry extract according to any one of claims 1 to 9, characterized in that, The preparation method comprises the following steps: The blueberry extract inclusion, deionized water, surfactant and co-surfactant are mixed and homogenized at a speed of 9000-10000 r / min for 2-4 minutes to obtain the flavor composition.
Citation Information
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