An antibacterial and anti-inflammatory oral care complex and its use in oral health maintenance products

Abstract

This invention provides an antibacterial and anti-inflammatory oral care complex and its application in oral health maintenance products, relating to the field of antibacterial and anti-inflammatory materials technology. The antibacterial and anti-inflammatory oral care complex of this invention comprises *Curcuma longa*-*Birch* bilayer microcapsules obtained by combining *Curcuma longa* extract with hydroxypropyl-β-cyclodextrin and *Birch* powder, and a concentrated *Birch* sap. The *Birch* powder and concentrated *Birch* sap are obtained by ultrafiltration of *Birch* sap, collecting the ultrafiltration retentate containing large molecules and the ultrafiltration permeate containing small molecules, followed by freeze-drying and concentration, respectively. This invention effectively solves the problems of solubility, stability, and taste of plant active ingredients in oral care products.

Description

Technical Field

[0001] This invention relates to the field of antibacterial and anti-inflammatory materials technology, specifically to an antibacterial and anti-inflammatory oral care compound and its application in products for maintaining oral health. Background Technology

[0002] With the fast pace of modern life and changing dietary habits, oral health problems such as gingivitis, periodontitis, and oral ulcers are becoming increasingly common. Currently, most oral care products on the market (such as mouthwash and oral gels) use chemical antibacterial agents like chlorhexidine, which can easily lead to oral flora imbalance, tooth discoloration, and altered taste with long-term use. Therefore, finding safe and effective plant-derived antibacterial and anti-inflammatory ingredients has become a current research hotspot.

[0003] Curcuma longa extract (essential oil) possesses excellent broad-spectrum antibacterial and anti-inflammatory effects, but its water solubility is extremely poor, its volatility is high, and it has a strong bitter taste and irritating odor. Direct application in oral care products would result in a terrible user experience. Birch sap is rich in birch polyphenols, polysaccharides, and various trace elements, and has healing-promoting and anti-inflammatory effects. However, the natural birch sap system is complex, and large molecular proteins and polysaccharides are prone to flocculation and precipitation in the formulation, leading to a cloudy product appearance and short shelf life. To address these issues, this invention proposes an antibacterial and anti-inflammatory oral care complex and its preparation method. Summary of the Invention

[0004] The purpose of this invention is to provide an antibacterial and anti-inflammatory oral care complex and its application in oral health maintenance products. A double-layer microcapsule system is constructed to address the technical defects of existing plant extracts in oral care products, such as easy volatility, poor taste, difficulty in continuous release of effective ingredients, and unstable formulation system.

[0005] On one hand, the present invention provides an antibacterial and anti-inflammatory oral care complex, comprising turmeric-birch bilayer microcapsules and birch sap concentrate obtained by combining turmeric extract with hydroxypropyl-β-cyclodextrin and birch powder; wherein the birch powder and birch sap concentrate are obtained by ultrafiltration of birch sap to collect ultrafiltration retentate containing large molecules and ultrafiltration permeate containing small molecules, and freeze-drying and concentrating them respectively.

[0006] Furthermore, the preparation steps of the *Curcuma longa*-*Birch bilayer* microcapsules include:

[0007] (1) Hydroxypropyl-β-cyclodextrin was dissolved in deionized water, and then the extract of Curcuma longa was added and subjected to ultrasonic reaction before filtration to obtain the Curcuma longa inclusion complex.

[0008] (2) Disperse birch powder in deionized water, add turmeric inclusion complex, emulsify by high-speed shearing, add chitosan acetate solution to the system and adjust the pH value of the system to 4.5-5.5, stir and spray dry to obtain the turmeric-birch bilayer microcapsules.

[0009] Furthermore, the preparation method of the Curcuma longa extract includes:

[0010] S1. Take fresh turmeric rhizomes, wash and slice them, dry them at a low temperature of 40-50℃ until the moisture content is less than 10%, pulverize them and pass them through a 40-60 mesh sieve to obtain powder;

[0011] S2. The powder is loaded into a supercritical extraction vessel and extracted using supercritical CO2 fluid; then the fluid enters a separation vessel for depressurization separation, and the effluent from the bottom of the separation vessel is collected to obtain turmeric essential oil extract.

[0012] Further, in step S2, the extraction pressure is 25-35 MPa, the extraction temperature is 40-50℃, the extraction time is 2-3 h, the CO2 flow rate is 15-25 L / h, and 95% ethanol is used as the entrainer, with the amount of the entrainer being 1-3% of the material mass.

[0013] Furthermore, in step S2, the decompression separation pressure is 5-8 MPa and the decomposition temperature is 35-45℃.

[0014] Further, in step (1), the weight ratio of the hydroxypropyl-β-cyclodextrin, deionized water and Curcuma longa extract is 1:(4-8):(0.125-0.2).

[0015] Furthermore, in step (1), the temperature when the Curcuma longa extract is added is 45-55℃ and the system rotation speed is 300-500 r / min.

[0016] Further, in step (1), the ultrasonic reaction step is: ultrasonic reaction for 1-2 h under the conditions of ultrasonic frequency 20-40 kHz, ultrasonic power 200-400 W, and constant temperature of 45-55℃.

[0017] Further, in step (1), the filtration is to remove unencapsulated free essential oils by filtration through a 0.45μm microporous membrane.

[0018] Further, the preparation method of the birch powder and birch sap concentrate includes: collecting fresh birch sap, coarsely filtering it through a 300-400 mesh stainless steel filter, and then pumping it into a ceramic inorganic membrane module with a pore size of 0.1-0.2 μm for microfiltration to remove impurities at an operating pressure of 0.1-0.2 MPa and a temperature of 15-25°C; collecting the microfiltration permeate and pumping it into a hollow fiber ultrafiltration membrane module with a molecular weight cutoff of 10000 Da for ultrafiltration at an operating pressure of 0.2-0.4 MPa, collecting the ultrafiltration retentate containing macromolecular substances and the ultrafiltration permeate containing small molecules; freeze-drying the ultrafiltration retentate to obtain birch powder; and concentrating the ultrafiltration permeate to obtain birch sap concentrate.

[0019] Further, the freeze-drying step is as follows: the ultrafiltration retentate is placed in a freeze dryer and pre-frozen at -40°C to -50°C for 4-6 hours, and then sublimated and dried at a cold trap temperature of -60°C and a vacuum degree of less than 20 Pa for 24-36 hours.

[0020] Further, the concentration step is as follows: the ultrafiltration permeate is pumped into a nanofiltration membrane module with a molecular weight cutoff of 150-300 Da, and concentration is carried out at an operating pressure of 1.5-2.5 MPa. During the concentration process, jacket cooling water circulation is used to control the operating temperature at 15-20℃. Concentration is stopped when the solid content of the system reaches 15-20%, and the birch sap concentrate is obtained.

[0021] Further, in step (2), the ratio of the amount of birch powder, deionized water and turmeric inclusion complex is 1-2:100-200:0.5-1.

[0022] Further, in step (2), the shear emulsification speed is 800-1200 r / min and the time is 10-20 min.

[0023] Further, in step (2), the chitosan acetic acid solution is prepared by dissolving chitosan in glacial acetic acid with a volume fraction of 1%, and the dry weight of the chitosan added is 1 / 4 to 1 / 2 of the mass of the birch powder.

[0024] Furthermore, in step (2), the stirring temperature is room temperature and the stirring time is 1-2 hours.

[0025] Furthermore, in step (2), the inlet air temperature of the spray dryer is 140-160℃ and the outlet air temperature is 70-80℃.

[0026] On the other hand, the present invention also provides the application of the aforementioned antibacterial and anti-inflammatory oral care complex in products for maintaining oral health, said products including one or more of oral sprays, mouthwashes, tooth powders, dental care gels, and toothpaste.

[0027] On the other hand, the present invention also provides an antibacterial and anti-inflammatory oral care gel, comprising the aforementioned antibacterial and anti-inflammatory oral care complex, wherein the gel comprises the following components: 5-15 parts of turmeric-birch bilayer microcapsules, 30-50 parts of birch sap concentrate, 0.5-2.0 parts of thickener, 0.1-0.5 parts of sodium hyaluronate, 2-5 parts of sweetener, 0.1-0.3 parts of dipotassium glycyrrhizate, and 30-50 parts of deionized water.

[0028] Furthermore, the thickener is selected from one or more of carbomer 940, hydroxyethyl cellulose, or sodium alginate;

[0029] Furthermore, the sweetener is selected from one or more of xylitol, erythritol, or steviol glycosides.

[0030] On the other hand, the present invention also provides a method for preparing an antibacterial and anti-inflammatory oral care gel, the steps of which include:

[0031] (1) Disperse the thickener and sodium hyaluronate evenly in deionized water, let it stand to swell, and obtain a transparent gel matrix;

[0032] (2) After the birch sap concentrate, sweetener and dipotassium glycyrrhizate are mixed evenly, they are added to the gel matrix and stirred evenly to obtain a primary gel.

[0033] (3) Add the turmeric-birch bilayer microcapsules to the primary gel and stir evenly under a low shear force of 500-800 r / min to make it uniformly suspended;

[0034] (4) Add a neutralizing agent to adjust the pH of the system to 5.5-6.5, and then degas under vacuum to obtain the final product.

[0035] The beneficial effects of this invention are as follows:

[0036] This invention utilizes ultrafiltration membrane technology to separate birch sap into macromolecular polysaccharides and small-molecule active liquids. The macromolecular polysaccharides are freeze-dried and used as the wall material for microcapsules, while the small-molecule liquids are directly used as the active water matrix for gels after cold concentration via nanofiltration. This design avoids flocculation and turbidity of macromolecules in the gel matrix while fully utilizing the medicinal value of birch sap.

[0037] This invention constructs a core-shell bilayer microcapsule by using hydroxypropyl-β-cyclodextrin as the primary inclusion layer and birch powder / chitosan composite agglomeration as the outer wall material. The inner inclusion layer completely masks the bitterness and pungent irritation of turmeric essential oil; the positively charged chitosan in the outer layer readily adheres to the negatively charged oral mucosa, enabling long-term retention of the microcapsule at the gingival site and targeted sustained release of the active ingredients.

[0038] In this invention, the essential oil of Curcuma longa mainly targets broad-spectrum bactericidal activity, while the betulinum polyphenols and organic acids in the small molecule concentrate of birch mainly target tissue repair and eliminate inflammatory factors, forming a perfect pharmacological synergy. It has excellent inhibition rate against Porphyromonas gingivalis, which causes gingivitis, and common Candida albicans. Attached Figure Description

[0039] The accompanying drawings, which form part of this invention, are used to provide a further understanding of the invention. The illustrative embodiments of the invention and their descriptions are used to explain the invention and do not constitute an improper limitation of the invention.

[0040] Figure 1 This is a graph showing the production of methanethiol;

[0041] Figure 2 This is a schematic diagram of a colorimeter.

[0042] Figure 3 This is a schematic diagram showing the results of the blank control group before treatment, 7 days after treatment, and 3 weeks after treatment.

[0043] Figure 4 The diagram shows the results of the sample group before treatment, 7 days after treatment, and 3 weeks after treatment.

[0044] Figure 5 A comparison chart of ΔL* values;

[0045] Figure 6 This is a comparison chart of the color gradation difference results. Detailed Implementation

[0046] The technical solution of the present invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention. It should be noted that the raw materials are all commercially available.

[0047] Example 1

[0048] This embodiment of an antibacterial and anti-inflammatory oral care complex includes turmeric-birch bilayer microcapsules obtained by combining turmeric extract with hydroxypropyl-β-cyclodextrin and birch powder, and birch sap concentrate; wherein, the birch powder and birch sap concentrate are obtained by ultrafiltration of birch sap to collect the ultrafiltration retentate containing large molecules and the ultrafiltration permeate containing small molecules, and then freeze-drying and concentrating them respectively.

[0049] 1. Preparation of Curcuma longa extract

[0050] Take fresh Curcuma aromatica rhizomes, wash and slice them, dry them at a low temperature of 45℃ until the moisture content is less than 10%, and then pulverize them through a 50-mesh sieve to obtain Curcuma aromatica powder.

[0051] The powder was loaded into a supercritical CO2 extraction vessel. The extraction pressure was set to 30 MPa, the extraction temperature to 45℃, and the CO2 flow rate to 20 L / h. 2% (by weight of the material) of 95% ethanol was added as an entrainer, and extraction was carried out for 2.5 h. The fluid then entered a separation vessel for decomposition separation at a pressure of 6.5 MPa and a temperature of 40℃. The effluent from the bottom of the separation vessel was collected to obtain the Curcuma aromatica essential oil extract.

[0052] 2. Preparation of birch powder and birch sap concentrate

[0053] Fresh birch sap was collected, coarsely filtered through a 350-mesh stainless steel filter, and then pumped into a ceramic inorganic membrane module with a pore size of 0.15 μm. Microfiltration was performed at an operating pressure of 0.15 MPa and 20°C to remove impurities. The microfiltration permeate was collected and pumped into a hollow fiber ultrafiltration membrane module with a molecular weight cutoff of 10000 Da. Ultrafiltration was performed at an operating pressure of 0.3 MPa, and the ultrafiltration retentate (containing macromolecules) and ultrafiltration permeate (containing small molecules) were collected separately.

[0054] Birch powder: The ultrafiltration retentate is placed in a freeze dryer and pre-frozen at -45℃ for 5 h, and then sublimated and dried at a cold trap temperature of -60℃ and a vacuum degree of less than 20 Pa for 30 h to obtain the powder.

[0055] Birch sap concentrate: The ultrafiltration permeate is pumped into a nanofiltration membrane module with a molecular weight cutoff of 200 Da, concentrated at an operating pressure of 2.0 MPa and an operating temperature controlled at 18°C, and the concentration is stopped when the solid content of the system reaches 18%.

[0056] 3. Preparation of Curcuma longa-Birch bilayer microcapsules

[0057] (1) Weigh out the following proportions by weight: hydroxypropyl-β-cyclodextrin:deionized water:Curcuma wenyujin extract = 1:6:0.16. Dissolve the hydroxypropyl-β-cyclodextrin in deionized water, heat to 50℃, and add the Curcuma wenyujin extract while stirring at 400 r / min. Then, sonicate the mixture for 1.5 h at a constant temperature of 50℃ and a sonic frequency of 30 kHz. After the reaction, filter through a 0.45 μm microporous membrane to remove unencapsulated free essential oils, and obtain the Curcuma wenyujin inclusion complex.

[0058] (2) The following mixture was prepared by weight ratio: birch powder: deionized water: turmeric inclusion complex = 1.5:150:0.8. The birch powder was dispersed in deionized water, and the turmeric inclusion complex was added. The mixture was emulsified by high-speed shearing at 1000 r / min for 15 min. Then, a chitosan acetate solution (chitosan dissolved in 1% glacial acetic acid by volume, and the dry weight of chitosan added was 1 / 3 of the mass of birch powder) was added to adjust the pH of the system to 5.0. The mixture was stirred at room temperature for 1.5 h. Finally, the mixture was spray-dried at an inlet air temperature of 150℃ and an outlet air temperature of 75℃ to obtain the bilayer microcapsules.

[0059] 4. Preparation of antibacterial and anti-inflammatory oral care gel

[0060] Weigh each component according to the following parts by weight:

[0061] 10 parts of turmeric-birch double-layer microcapsules, 40 parts of birch sap concentrate, 1.2 parts of carbomer 940, 0.3 parts of sodium hyaluronate, 3.5 parts of xylitol (purchased from Shandong Fangchang Biotechnology Co., Ltd., CAS No. 87-99-0), 0.2 parts of dipotassium glycyrrhizate, and 40 parts of deionized water.

[0062] (1) Carbomer 940 and sodium hyaluronate are evenly dispersed in deionized water and allowed to stand to swell, resulting in a transparent gel matrix.

[0063] (2) Mix the birch sap concentrate, xylitol and dipotassium glycyrrhizate evenly and add them to the gel matrix, then stir to obtain the primary gel.

[0064] (3) Add the turmeric-birch bilayer microcapsules and stir evenly under low shear force of 650 r / min to make them uniformly suspended.

[0065] (4) Add the neutralizing agent triethanolamine to adjust the pH of the system to 6.0, and after vacuum degassing, the antibacterial and anti-inflammatory oral care gel is obtained.

[0066] Example 2

[0067] This embodiment of an antibacterial and anti-inflammatory oral care complex includes turmeric-birch bilayer microcapsules obtained by combining turmeric extract with hydroxypropyl-β-cyclodextrin and birch powder, and birch sap concentrate; wherein, the birch powder and birch sap concentrate are obtained by ultrafiltration of birch sap to collect the ultrafiltration retentate containing large molecules and the ultrafiltration permeate containing small molecules, and then freeze-drying and concentrating them respectively.

[0068] 1. Preparation of Curcuma longa extract

[0069] Take fresh Curcuma longa rhizomes, wash and slice them, dry them at a low temperature of 40℃ until the moisture content is less than 10%, and then pulverize them through a 40-mesh sieve to obtain Curcuma longa powder.

[0070] The powder was loaded into a supercritical CO2 extraction vessel. The extraction pressure was set to 25 MPa, the extraction temperature to 40℃, and the CO2 flow rate to 15 L / h. 1% (by weight of the material) of 95% ethanol was added as an entrainer, and extraction was carried out for 2 h. The fluid then entered a separation vessel for decomposition at a pressure of 5 MPa and a temperature of 35℃. The effluent from the bottom of the separation vessel was collected to obtain the Curcuma aromatica essential oil extract.

[0071] 2. Preparation of birch powder and birch sap concentrate

[0072] Fresh birch sap was collected, coarsely filtered through a 300-mesh stainless steel filter, and then pumped into a ceramic inorganic membrane module with a pore size of 0.1 μm. Microfiltration was performed at an operating pressure of 0.1 MPa and 15°C to remove impurities. The microfiltration permeate was collected and pumped into a hollow fiber ultrafiltration membrane module with a molecular weight cutoff of 10,000 Da. Ultrafiltration was performed at an operating pressure of 0.2 MPa, and the ultrafiltration retentate (containing macromolecules) and ultrafiltration permeate (containing small molecules) were collected separately.

[0073] Birch powder: The ultrafiltration retentate is placed in a freeze dryer and pre-frozen at -40℃ for 4 h, and then sublimated and dried at a cold trap temperature of -60℃ and a vacuum degree of less than 20 Pa for 24 h to obtain the powder.

[0074] Birch sap concentrate: The ultrafiltration permeate is pumped into a nanofiltration membrane module with a molecular weight cutoff of 150 Da, concentrated at an operating pressure of 1.5 MPa and an operating temperature controlled at 15°C, and the concentration is stopped when the solid content of the system reaches 15%.

[0075] 3. Preparation of Curcuma longa-Birch bilayer microcapsules

[0076] (1) Weigh out the following proportions by weight: hydroxypropyl-β-cyclodextrin:deionized water:Curcuma wenyujin extract = 1:4:0.125. Dissolve the hydroxypropyl-β-cyclodextrin in deionized water, heat to 45℃, and add the Curcuma wenyujin extract while stirring at 300 r / min. Then, sonicate the mixture for 1 h at a constant temperature of 45℃ and a sonic frequency of 20 kHz. After the reaction, filter through a 0.45 μm microporous membrane to remove unencapsulated free essential oils and obtain the Curcuma wenyujin inclusion complex.

[0077] (2) The birch powder, deionized water, and turmeric inclusion complex were prepared in a weight ratio of 1:100:0.5. The birch powder was dispersed in the deionized water, and the turmeric inclusion complex was added. The mixture was emulsified by high-speed shearing at 800 r / min for 10 min. Then, a chitosan acetate solution (chitosan was dissolved in 1% glacial acetic acid by volume, and the dry weight of chitosan added was 1 / 4 of the mass of the birch powder) was added to adjust the pH of the system to 4.5. The mixture was stirred at room temperature for 1 h. Finally, the mixture was spray-dried at an inlet air temperature of 140℃ and an outlet air temperature of 70℃ to obtain the bilayer microcapsules.

[0078] 4. Preparation of antibacterial and anti-inflammatory oral care gel

[0079] Weigh each component according to the following parts by weight:

[0080] Five parts of turmeric-birch double-layer microcapsules, 30 parts of birch sap concentrate, 0.5 parts of carbomer 940, 0.1 parts of sodium hyaluronate, 2 parts of xylitol, 0.1 parts of dipotassium glycyrrhizate, and 30 parts of deionized water.

[0081] (1) Carbomer 940 and sodium hyaluronate are evenly dispersed in deionized water and allowed to stand to swell, resulting in a transparent gel matrix.

[0082] (2) Mix the birch sap concentrate, xylitol and dipotassium glycyrrhizate evenly and add them to the gel matrix, then stir to obtain the primary gel.

[0083] (3) Add the turmeric-birch bilayer microcapsules and stir evenly under low shear force of 500 r / min to make them uniformly suspended.

[0084] (4) Add the neutralizing agent triethanolamine to adjust the pH of the system to 5.5, and after vacuum degassing, the antibacterial and anti-inflammatory oral care gel is obtained.

[0085] Example 3

[0086] This embodiment of an antibacterial and anti-inflammatory oral care complex includes turmeric-birch bilayer microcapsules obtained by combining turmeric extract with hydroxypropyl-β-cyclodextrin and birch powder, and birch sap concentrate; wherein, the birch powder and birch sap concentrate are obtained by ultrafiltration of birch sap to collect the ultrafiltration retentate containing large molecules and the ultrafiltration permeate containing small molecules, and then freeze-drying and concentrating them respectively.

[0087] 1. Preparation of Curcuma longa extract

[0088] Take fresh Curcuma longa rhizomes, wash and slice them, dry them at a low temperature of 50℃ until the moisture content is less than 10%, and then pulverize them through a 60-mesh sieve to obtain Curcuma longa powder.

[0089] The powder was loaded into a supercritical CO2 extraction vessel. The extraction pressure was set to 35 MPa, the extraction temperature to 50°C, and the CO2 flow rate to 25 L / h. 3% (by weight) of 95% ethanol was added as an entrainer, and extraction was carried out for 3 h. The fluid then entered a separation vessel for decomposition at a pressure of 8 MPa and a temperature of 45°C. The effluent from the bottom of the separation vessel was collected to obtain the Curcuma aromatica essential oil extract.

[0090] 2. Preparation of birch powder and birch sap concentrate

[0091] Fresh birch sap was collected, coarsely filtered through a 400-mesh stainless steel filter, and then pumped into a ceramic inorganic membrane module with a pore size of 0.2 μm. Microfiltration was performed at an operating pressure of 0.2 MPa and 25°C to remove impurities. The microfiltration permeate was collected and pumped into a hollow fiber ultrafiltration membrane module with a molecular weight cutoff of 10,000 Da. Ultrafiltration was performed at an operating pressure of 0.4 MPa, and the ultrafiltration retentate (containing macromolecules) and ultrafiltration permeate (containing small molecules) were collected separately.

[0092] Birch powder: The ultrafiltration retentate is placed in a freeze dryer and pre-frozen at -50℃ for 6 h, and then sublimated and dried at a cold trap temperature of -60℃ and a vacuum degree of less than 20 Pa for 36 h to obtain the powder.

[0093] Birch sap concentrate: The ultrafiltration permeate is pumped into a nanofiltration membrane module with a molecular weight cutoff of 300 Da, concentrated at an operating pressure of 2.5 MPa and an operating temperature controlled at 20°C, and the concentration is stopped when the solid content of the system reaches 20%.

[0094] 3. Preparation of Curcuma longa-Birch bilayer microcapsules

[0095] (1) Weigh out the following proportions by weight: hydroxypropyl-β-cyclodextrin:deionized water:Curcuma wenyujin extract = 1:8:0.2. Dissolve the hydroxypropyl-β-cyclodextrin in deionized water, heat to 55℃, and add the Curcuma wenyujin extract while stirring at 500 r / min. Then, sonicate the mixture for 2 h at a constant temperature of 55℃ and a sonic frequency of 40 kHz. After the reaction, filter through a 0.45 μm microporous membrane to remove unencapsulated free essential oils and obtain the Curcuma wenyujin inclusion complex.

[0096] (2) The birch powder, deionized water, and turmeric inclusion complex were prepared in a weight ratio of 2:200:1. The birch powder was dispersed in deionized water, and the turmeric inclusion complex was added. The mixture was emulsified by high-speed shearing at 1200 r / min for 20 min. Then, a chitosan acetate solution (chitosan dissolved in 1% glacial acetic acid by volume, and the dry weight of chitosan added was 1 / 2 the mass of the birch powder) was added to adjust the pH of the system to 5.5. The mixture was stirred at room temperature for 2 h. Finally, the mixture was spray-dried at an inlet air temperature of 160℃ and an outlet air temperature of 80℃ to obtain the bilayer microcapsules.

[0097] 4. Preparation of antibacterial and anti-inflammatory oral care gel

[0098] Weigh each component according to the following parts by weight:

[0099] 15 parts of turmeric-birch double-layer microcapsules, 50 parts of birch sap concentrate, 2.0 parts of carbomer 940, 0.5 parts of sodium hyaluronate, 5 parts of xylitol, 0.3 parts of dipotassium glycyrrhizate, and 50 parts of deionized water.

[0100] (1) Carbomer 940 and sodium hyaluronate are evenly dispersed in deionized water and allowed to stand to swell, resulting in a transparent gel matrix.

[0101] (2) Mix the birch sap concentrate, xylitol and dipotassium glycyrrhizate evenly and add them to the gel matrix, then stir to obtain the primary gel.

[0102] (3) Add the turmeric-birch bilayer microcapsules and stir evenly under low shear force of 800 r / min to make them uniformly suspended.

[0103] (4) Add the neutralizing agent triethanolamine to adjust the pH of the system to 6.5, and after vacuum degassing, the antibacterial and anti-inflammatory oral care gel is obtained.

[0104] Comparative Example 1

[0105] Based on Example 1, the preparation and addition of Curcuma longa extract were omitted, while the remaining steps remained the same.

[0106] In the preparation of the turmeric-birch bilayer microcapsules, step (1) is omitted, and step (2) is simply the reaction of birch powder dispersed in deionized water with chitosan acetate solution, followed by spray drying to obtain microcapsules.

[0107] The final oral care gel contains only birch sap concentrate and microcapsules containing the aforementioned turmeric-free ingredients.

[0108] Comparative Example 2

[0109] Based on Example 1, the ultrafiltration step of birch sap was omitted, and birch powder and birch sap concentrate were not added; the remaining steps were the same.

[0110] In the preparation of the turmeric-birch bilayer microcapsules, step (2) does not add birch powder, but only reacts the turmeric inclusion complex with chitosan acetate solution and then spray-drys.

[0111] The final oral care gel does not contain birch sap concentrate.

[0112] Comparative Example 3

[0113] Based on Example 1, the extract of Curcuma longa was used directly for microcapsule preparation without inclusion by hydroxypropyl-β-cyclodextrin.

[0114] Step (1) is omitted. In step (2), the extract of Curcuma longa and birch powder are directly dispersed together in deionized water, and then chitosan acetate solution is added and spray dried.

[0115] Comparative Example 4

[0116] Based on Example 1, the birch sap was directly freeze-dried and concentrated without ultrafiltration. The ultrafiltration step was eliminated, and the permeate after microfiltration was directly divided into two batches: one batch was freeze-dried to obtain "unseparated birch powder", and the other batch was concentrated to obtain "unseparated birch sap concentrate".

[0117] Comparative Example 5

[0118] Based on Example 1, chitosan acetate solution was not added in the preparation of the turmeric-birch bilayer microcapsules. In step (2), after dispersing the birch powder in deionized water, the turmeric inclusion complex was added, and after high-speed shear emulsification, it was directly spray-dried without chitosan coating.

[0119] Comparative Example 6

[0120] Based on Example 1, the amount of chitosan dry weight added was changed to an equal mass of birch powder, while the remaining steps remained the same. That is, the amount of chitosan dry weight added = the mass of birch powder, which exceeds the upper limit of the original range.

[0121] Comparative Example 7

[0122] Based on Example 1, the ultrasonic reaction in step (1) is cancelled and replaced with ordinary magnetic stirring, that is, stirring at 300 r / min and 50℃ for 1.5 h, and the rest of the steps are the same.

[0123] Comparative Example 8

[0124] Based on Example 1, the supercritical CO2 extraction of Curcuma longa extract was performed without the addition of 95% ethanol as an entrainer, while the remaining steps remained the same.

[0125] Comparative Example 9

[0126] Based on Example 1, the Curcuma longa extract was prepared by steam distillation: Curcuma longa powder was soaked in water, steam distilled for 4 hours, the distillate was collected, and the essential oil layer was separated. The remaining steps were the same.

[0127] Comparative Example 10

[0128] Based on Example 1, the birch sap concentrate was concentrated using ordinary rotary evaporation, i.e., at 60°C, under reduced pressure to 18% solids, without nanofiltration membrane treatment, and the remaining steps were the same.

[0129] Comparative Example 11

[0130] Based on Example 1, the antibacterial and anti-inflammatory oral care gel does not contain Curcuma longa-Birch bilayer microcapsules, and the Curcuma longa-Birch bilayer microcapsules are replaced with an equal mass of birch sap concentrate.

[0131] Comparative Example 12

[0132] Based on Example 1, the antibacterial and anti-inflammatory oral care gel does not contain birch sap concentrate, which is replaced with an equal mass of turmeric-birch bilayer microcapsules.

[0133] Experimental Example 1:

[0134] 1. Appearance stability:

[0135] Centrifugation test: Take the sample and put it into a centrifuge tube, centrifuge at 3000 r / min for 30 minutes, and observe whether layering, precipitation or demulsification occurs.

[0136] Cold and heat test: According to the "Cosmetic Stability Testing Specification", the sample is placed in a -15℃ refrigerator for 24 hours, then removed and allowed to return to room temperature before being placed in a 40℃ constant temperature incubator for 24 hours. This constitutes one cycle, and three consecutive cycles are performed. The changes in appearance are observed. The result is either "pass" (√) or "fail" (×).

[0137] 2. Transmittance (%): Take an appropriate amount of gel sample and place it in a 1 cm quartz cuvette. Measure the transmittance at a wavelength of 600 nm using a UV-Vis spectrophotometer. Use deionized water as a blank control (100%). This indicator reflects the clarity of the gel and its compatibility with the matrix.

[0138] 3. Odor / Taste Rating (points): Twenty healthy volunteers (half male and half female) were recruited to conduct oral trial evaluations of the samples using a double-blind method. The samples were rated on a comprehensive basis, with a maximum score of 10 points, considering both odor (presence of medicinal or irritating odors) and taste (presence of bitterness, spiciness, or graininess). Higher scores indicate better taste masking and higher consumer acceptance.

[0139] 4. Retention rate of active ingredient (betu polyphenols) (%): Each sample was placed in a constant temperature and humidity chamber at 40℃ and 75% relative humidity for 3 months for accelerated aging. The content of betu polyphenols before and after accelerated aging was determined by high performance liquid chromatography (HPLC), and the retention rate was calculated.

[0140] 5. In vitro antibacterial rate determination (%): Referring to "QB / T 2738-2023 Evaluation Method for Antibacterial and Antimicrobial Effects of Daily Chemical Products", the antibacterial rates of the samples against Staphylococcus aureus (causing purulent infections), Candida albicans (causing oral fungal infections), and Porphyromonas gingivalis (a core pathogenic anaerobic bacterium of periodontitis) were tested. The bacterial suspension was mixed with an equal volume of sample, incubated for 20 minutes, then serially diluted and plated for culture. The antibacterial rate was calculated.

[0141] 6. Inhibition rate of IL-6 (inflammatory cytokine): Mouse mononuclear macrophages (RAW 264.7) were plated and cultured. Lipopolysaccharide (LPS, 1 μg / mL) was added to stimulate an inflammatory response. Extracts from each example and comparative example (final concentration diluted to 100 μg / mL) were also added. After 24 hours of culture, the supernatant was collected, and the secretion of interleukin-6 (IL-6) was measured using an ELISA kit. The inhibition rate of IL-6 in the drug-treated group was calculated using the secretion level of the untreated LPS model group as the denominator. A higher inhibition rate indicates a better anti-inflammatory effect.

[0142] 7. Oral mucosal adhesion time (min):

[0143] A modified rinsing method was used: isolated porcine buccal mucosa was fixed on a slant (at a 45° angle), and 0.5 g of gel sample was applied to the surface. Artificial saliva was added dropwise at a constant flow rate (1 mL / min) to rinse the mucosal surface. The time required from the start of rinsing until the sample was completely rinsed away from the mucosal surface was recorded. A longer time indicates better targeted retention and long-lasting drug release.

[0144] The test results are shown in the table below.

[0145]

[0146] Based on the aforementioned data, the antibacterial rates of Examples 1-3 all exceeded 98%, and the inhibition rate of the IL-6 inflammatory factor was close to 90%. In contrast, the antibacterial rate of Comparative Example 1, lacking Curcuma longa, decreased significantly, and the anti-inflammatory index (IL-6 inhibition rate) of Comparative Example 2, lacking Birch birch, plummeted to 51.4%. This demonstrates that Curcuma longa essential oil and Birch birch active ingredients have a strong synergistic effect in killing oral pathogens and repairing mucosal inflammation.

[0147] Comparative Example 3 did not use cyclodextrin to encapsulate the essential oil, resulting in a taste score of 4.2, an extremely strong spiciness, and failure to pass centrifugation and hot / cold tests due to essential oil precipitation. Examples 1-3 all achieved taste scores above 9, completely masking the odor. Comparative Example 7, due to the lack of specific frequency ultrasound application, had a low essential oil encapsulation rate, still exhibiting an off-odor and decreased stability.

[0148] Comparative Example 4 did not undergo ultrafiltration fractionation of the birch sap, resulting in the direct mixing of large-molecule polysaccharides into the gel matrix. This caused flocculation, leading to a sharp drop in transmittance to 65.4%, and precipitation occurred during centrifugation. Examples 1-3, however, separated small molecules for the aqueous phase and large molecules for the microcapsule wall material, achieving transmittance exceeding 90%, producing crystal-clear products with excellent stability. Furthermore, Comparative Example 10 used traditional rotary evaporation to concentrate birch sap, but heating caused oxidative degradation of the core active ingredient, birch polyphenols, resulting in a retention rate of only 65.8%. In contrast, the examples using the nanofiltration cold concentration system of this invention achieved a retention rate exceeding 95%.

[0149] Examples 1-3 showed a mucosal adhesion time of over 140 minutes, effectively resisting saliva erosion. In contrast, Comparative Example 5, lacking positively charged chitosan in its outer wall material, resulted in the microcapsules losing their electrostatic adhesion ability, causing a sharp drop in mucosal adhesion time to 62 minutes. Although Comparative Example 6 slightly increased the chitosan proportion, it led to an excessively grainy texture and a significant decrease in taste score. This demonstrates that the strictly controlled microcapsule wall material formulation of this application achieves a perfect balance between taste and retention time.

[0150] Comparative Example 11, which removed the microcapsules, while exhibiting an excellent gel appearance (96.8% light transmittance), suffered a significant drop in its antibacterial rate against the three major oral pathogens to the 40-60% range due to the absence of turmeric essential oil. Furthermore, the lack of positively charged chitosan wall material drastically reduced mucosal adhesion time from 145 minutes to 25 minutes, meaning the product was immediately washed away by saliva upon ingestion, completely negating its long-lasting moisturizing function. Comparative Example 12, which forcibly replaced all the concentrate with microcapsules, resulted in severe solids overload within the gel system. This directly led to a cloudy, opaque paste-like consistency, with light transmittance plummeting to 15.2%, and severe stratification and powder precipitation during centrifugation. The intense granular texture also caused the taste score to plummet to the worst level of 3.5. Moreover, the lack of synergistic small-molecule anti-inflammatory substances from the birch sap concentrate limited the anti-inflammatory capacity of the high-concentration essential oil alone, with an IL-6 inhibition rate of only 44.5%.

[0151] Experimental Example 2: A toothpaste was prepared using the oral care complex obtained in Example 1 (calcium carbonate 48g, sorbitol (70%) (purchased from Guangzhou Yehusheng Chemical Co., Ltd.), deionized water 16.5g, glycerin 5g, sodium lauryl sulfate 2.1g, sodium carboxymethyl cellulose 1g, oral care complex 1.5g, sodium monofluorophosphate 0.76g, peppermint flavor 1g, sodium saccharin 0.2g, sodium benzoate 0.1g), and the following tests were performed:

[0152] 1. Antibacterial test: The test was conducted according to QB / T 2738-2023 "Evaluation Method for Antibacterial and Antimicrobial Effects of Daily Chemical Products". The tested bacteria were Streptococcus mutans, Porphyromonas gingivalis, Prevotella intermedius, and Fusobacterium nucleatum. The results are as follows:

[0153]

[0154] Based on the foregoing, after 2 minutes of treatment, the average inhibition rate of the test sample against Streptococcus mutans was >99.97%, against Porphyromonas gingivalis was 98.43%, against Prevotella intermedius was >99.96%, and against Fusobacterium nucleatum was >99.97%, all meeting the efficacy evaluation criteria of QB / T 2738-2023 (inhibition rate ≥90%). Therefore, the sample has a strong antibacterial effect on all tested strains.

[0155] 2. Evaluation of the effect of freshening breath

[0156] This study evaluated the efficacy of methanethiol in freshening breath based on an in vitro saliva-simulated breath-generating system. The specific mechanism is as follows: Methanethiol is the core volatile odor-causing component of oral malodor, primarily produced by the decomposition of sulfur-containing amino acids in saliva by anaerobic bacteria in the oral cavity. This study constructed an in vitro simulation system using hydroxyapatite (HAP) sheets to simulate the tooth surface. A biofilm was formed through pre-culture with saliva, and a breath-generating simulation solution containing anaerobic bacterial nutrients was added to recreate the methanethiol generation process. After sufficient contact between the test sample and the biofilm, if the sample exhibited breath-freshening activity, it could reduce methanethiol generation by inhibiting the metabolic activity of oral anaerobic bacteria, disrupting their living environment, or directly blocking the decomposition pathway of sulfur-containing amino acids. This study used gas chromatography to quantitatively detect the peak area of ​​methanethiol in the headspace vial after sample intervention, clarifying the inhibitory effect and intensity of the sample on methanethiol generation, and thus scientifically evaluating its in vitro breath-freshening efficacy.

[0157] The experimental group design is as follows:

[0158]

[0159] Experimental methods:

[0160] Take ten 15 mL centrifuge tubes, place one HAP tablet in each tube, add 2 mL of fresh saliva, cap the tubes, and incubate in a 37°C water bath for 24 h. Weigh 0.30 g of thioglycolate medium and dissolve it in 10 mL of water. Then prepare a breath-generating simulation solution according to the ratio of thioglycolate medium:water:fresh saliva of 2:13:85.

[0161] Remove the HAP tablets that have been cultured overnight and place one tablet per well in a 12-well plate. Randomize the plates into a negative control group and a sample group, with 5 tablets in each group. Dilute toothpaste with water at a ratio of 1:1.6 (toothpaste:water) and mix thoroughly. According to the experimental groups, add 2 mL of the sample and negative control to each well of the 12-well plate and incubate for 3 min. Remove the HAP tablets and rinse them in 5 mL of water to remove any remaining toothpaste. Then transfer the tablets to headspace vials. Add 2 mL of breath-generating simulation solution to each vial, seal the vials, and incubate at 37°C for 24 h.

[0162] Methanethiol in headspace vials was detected using gas chromatography, and its breath-freshening efficacy was evaluated using peak area as an indicator. The reduction rate of methanethiol peak area was calculated as: (Methanethiol peak area in the negative control group − Methanethiol peak area in the sample group) / Methanethiol peak area in the negative control group × 100%. Experimental data were imported into statistical analysis software to calculate the mean (x̄), standard deviation (SD), and coefficient of variation (CV = SD / x̄ × 100%) for each group. Normality and homogeneity of variance tests were performed on the data. The data conformed to a normal distribution and had homogeneity of variance: an independent samples t-test was used to compare the differences in methanethiol peak area between groups, with a significance level of α = 0.05.

[0163] The judgment criteria were as follows: For experimental validity, the coefficient of variation (CV) between parallel groups was <20%. For results, after co-culturing with the breath-generating simulation solution for a certain period, the peak area of ​​methanethiol generated in the sample group was significantly smaller than that in the negative control group (P<0.05), indicating that the sample had a breath-freshening effect. The methanethiol detection results are shown in the table below:

[0164]

[0165] Note: P<0.05 indicates a significant difference between the sample group and the negative control group.

[0166] The coefficients of variation within each group were all <20%, indicating the validity of the experiment. Furthermore, the test results showed that, compared with the negative control group, co-culturing the sample group with the breath-generating simulation solution for 24 h significantly reduced the production of methanethiol (P<0.05), with a methanethiol peak area reduction rate of 37.9% (comparative results are shown below). Figure 1As shown in the figure, the breath freshening effect improved by 37.9%. This indicates that the Shiyada Fresh Breath Toothpaste sample can effectively inhibit the production of oral odor and has the effect of providing 24-hour long-lasting breath freshness and reducing unpleasant odors.

[0167] 3. Evaluation of teeth whitening efficacy (extracted bovine teeth method)

[0168] Weigh the sample toothpaste at a weight ratio of 1:1.6, add water, mix the sample toothpaste and water evenly to make toothpaste slurry.

[0169] The experimental procedure is as follows:

[0170] (1) Place the enamel grinding block in a beaker, add 1% hydrochloric acid solution to ensure that the liquid surface completely submerges the enamel grinding block, stir with a glass rod for 60 s, rinse with water 3 times, and then treat with saturated sodium carbonate solution and 1% phytic acid solution in sequence according to the above steps.

[0171] (2) Place the acid-etched enamel abrasive block into the staining solution and place it on a shaker at 37°C for staining. The staining solution should be changed daily.

[0172] (3) After staining, remove the enamel abrasive block, rinse off the surface dirt, wipe the surface moisture, and retain the enamel abrasive block with uniform enamel staining. Within 10 min, use a spectrophotometer to measure the whiteness value (L* before staining) of the enamel after staining. Select enamel abrasive blocks with L* values ​​in the range of 40~50 and randomly assign them to the sample group and the blank control group, with 8 blocks in each group. After grouping, use a colorimeter to measure the color gradation of the enamel before treatment. Use a two-sample t test or rank-sum test to analyze the whiteness value (L* before) and color gradation of the two groups. It is required that there is no significant difference between the two groups (P>0.05).

[0173] (4) After mounting the standard toothbrush and enamel abrasive block onto the brushing device, set the brushing device's reciprocating frequency to 150 r / min, adjust the total weight of the toothbrush head and handle to 150±2 g, and add an appropriate amount of toothpaste paste to each paste cup to immerse the enamel abrasive block. The sample group used the sample toothpaste paste for brushing, while the blank control group used water for brushing.

[0174] (5) Use a brushing device to brush your teeth once a day, brushing 200 times each time, for 7 days and 3 weeks of simulated brushing.

[0175] (6) After the procedure, rinse the enamel abrasive block and dry the surface moisture. Within 10 minutes, use a spectrophotometer to measure the whiteness value (L*) of the treated enamel and use a colorimeter to measure the color gradation of the treated enamel.

[0176] The calculation formulas are as follows: ΔL* = L*after - L*before; Whiteness improvement factor = Sample group ΔL̅* / Blank control group ΔL̅*; Spot reduction rate = ΔL̅* / L̅*before × 100%; Where: ΔL*: Whiteness value difference; ΔL̅*: Average value of ΔL*; L̅*before: Average value of L*before.

[0177] A diagram of a colorimeter is shown below. Figure 2 As shown, the color gradation scores for the color chart are as follows:

[0178]

[0179] For example, if the test sample's color level before brushing is 4M2 (score 5) and after brushing is 2M2 (score 9), then using the sample improved the color level by 4 levels. If the experimental data all conform to a normal distribution, a two-sample t-test is used to analyze the significant difference (two-tailed test, significance level α = 0.05). If the experimental data do not conform to a normal distribution, a rank-sum test is used to analyze the significant difference (two-tailed test, significance level α = 0.05).

[0180] If the whiteness difference ΔL of the sample group is significantly greater than (P<0.05) the whiteness difference ΔL of the blank control group, or the color gradation difference of the sample group is significantly higher than (P<0.05) the color gradation difference of the blank control group, the sample can be considered to have the effect of removing extrinsic stains and whitening teeth. The L* value test results are shown in the table below:

[0181]

[0182] Note: P>0.05 indicates that there was no significant difference between the blank control group and the sample group before L*.

[0183] The results of the enamel shade and scoring test are shown in the table below:

[0184]

[0185] Note: P>0.05 indicates that there was no significant difference between the blank control group and the sample group before L*.

[0186] Therefore, the ΔL* values ​​(7 days) are shown in the table below:

[0187]

[0188] Note: P<0.05 indicates that there is a significant difference in ΔL* between the blank control group and the sample group.

[0189] The ΔL* values ​​(3 weeks) are shown in the table below:

[0190]

[0191] Note: P<0.05 indicates that there is a significant difference in ΔL* between the blank control group and the sample group.

[0192] Table 4. Color gradation difference (7 days)

[0193]

[0194] Note: P<0.05 indicates that there is a significant difference in color gradation between the blank control group and the sample group.

[0195] Table 5. Color gradation differences (3 weeks)

[0196]

[0197] Note: P<0.05 indicates that there is a significant difference in color gradation between the blank control group and the sample group.

[0198] This test, based on an isolated bovine tooth enamel abrasion block staining model, examines the efficacy of the sample in removing extrinsic stains and whitening teeth. The results for the blank control group before treatment, 7 days after treatment, and 3 weeks after treatment are illustrated in the diagram below. Figure 3 As shown in the diagram, the results of the sample group before treatment, 7 days after treatment, and 3 weeks after treatment are illustrated below. Figure 4 As shown in the figure; a comparison chart of ΔL* values ​​is presented. Figure 5 As shown in the figure, the comparison chart of color level difference results is as follows: Figure 6 As shown, * indicates P < 0.05.

[0199] The experimental results showed that after 7 days of in vitro simulated use of the sample, the ΔL value of the sample group was significantly greater than (P<0.05) the ΔL value of the blank control group. The ΔL value of the sample group was 29.3±4.1, while that of the blank control group was 2.3±1.1. The extrinsic pigmentation in the sample group decreased by 68%, while that in the blank control group decreased by 5%. The color gradation difference of the sample group was significantly higher than (P<0.05) the color gradation difference of the blank control group. The color gradation difference of the sample group was 10±2, while that of the blank control group was 0±0. This indicates that after 7 days of continuous use, the sample group improved by 10 color gradations, reduced extrinsic pigmentation by 68%, and compared with the blank control group, the whitening and stain-removing power of the sample group was increased by 12.74 times, improving by 10 color gradations. After 3 weeks of in vitro simulated use of the sample, the ΔL value of the sample group was significantly greater than (P<0.05) the ΔL value of the blank control group. The ΔL value of the sample group was 34.4±3.6, while that of the blank control group was 3.6±1.0. The extrinsic stains in the sample group decreased by 79%, while those in the blank control group decreased by 8%. The color difference in the sample group was significantly higher than (P<0.05) the color difference in the blank control group. The color difference in the sample group was 13±1, while that in the blank control group was 1±1. This indicates that after 3 weeks of continuous use, the sample group improved by 13 shades, reduced extrinsic stains by 79%, and compared with the blank control group, the whitening and stain-removing power of the sample group was increased by 9.56 times, improving by 12 shades. In conclusion, the toothpaste can effectively remove extrinsic stains caused by black tea, coffee, and soy sauce. Continuous use of this product for 7 days and 3 weeks both effectively improve tooth whiteness and whiten teeth.

[0200] Based on the above embodiments and experimental data, it can be seen that the antibacterial and anti-inflammatory oral care complex provided by the present invention has excellent and stable antibacterial, anti-inflammatory, and oral mucosal repair effects. Therefore, the present invention is not limited to the toothpaste and dental care gel shown in the specific embodiments above. As a highly efficient active ingredient, it can also be widely used in various other products aimed at maintaining oral health, including but not limited to oral sprays, mouthwashes, and dental powders.

[0201] Specifically, when the compound of this invention is applied to mouthwash (or gargle), it can be directly dispersed or dissolved in an aqueous matrix using an appropriate amount of surfactant. Due to the good fluidity of mouthwash, it can penetrate deep into the gaps between teeth and hard-to-reach areas of the mouth. The compound of this invention can then quickly cover the entire oral environment, exerting a comprehensive antibacterial effect and soothing the redness and swelling of the gums. When the compound of this invention is applied to an oral spray, it can be formulated into an aqueous or hydroalcoholic solution of appropriate concentration and filled into a spray container equipped with a pump head or propellant. Using a spray device, the compound of this invention can be sprayed out in the form of fine droplets, uniformly and densely adhering to the oral mucosa, pharynx, and gum surface. This formulation is not only fast-acting but also convenient to carry, meeting consumers' needs for oral antibacterial and anti-inflammatory effects and fresh breath anytime, anywhere, after meals or while traveling. When the compound of this invention is applied to dental powder, it can be uniformly mixed with a solid abrasive (such as calcium carbonate, hydrated silica powder, etc.), foaming agent, sweetener, and other dry powder matrix. When consumers use the tooth-cleaning powder to brush their teeth, the physical friction of the tooth-cleaning powder, combined with the dual effects of the bio-antibacterial and anti-inflammatory properties of the compound of this invention, can more effectively break down stubborn dental plaque and tartar, while preventing or improving periodontitis and gingival bleeding.

[0202] Finally, it should be noted that the above embodiments are only used to illustrate the present invention and are not intended to limit the technical solutions described in the present invention; those skilled in the art should understand that modifications or equivalent substitutions can still be made to the present invention; and all technical solutions and improvements that do not depart from the spirit and scope of the present invention should be covered within the scope of the claims of the present invention.

Claims

1. An antibacterial and anti-inflammatory oral care complex, characterized in that, The invention includes turmeric-birch bilayer microcapsules and birch sap concentrate obtained by combining turmeric extract with hydroxypropyl-β-cyclodextrin and birch powder; wherein the birch powder and birch sap concentrate are obtained by ultrafiltration of birch sap to collect the ultrafiltration retentate containing large molecules and the ultrafiltration permeate containing small molecules, and then freeze-drying and concentrating them respectively.

2. The bacteriostatic and anti-inflammatory oral care complex according to claim 1, wherein, The preparation steps of the Curcuma longa-Birch bilayer microcapsules include: (1) Hydroxypropyl-β-cyclodextrin was dissolved in deionized water, and then the extract of Curcuma longa was added and subjected to ultrasonic reaction before filtration to obtain the Curcuma longa inclusion complex. (2) Disperse birch powder in deionized water, add turmeric inclusion complex, emulsify by high-speed shearing, add chitosan acetate solution to the system and adjust the pH value of the system to 4.5-5.5, stir and spray dry to obtain the turmeric-birch bilayer microcapsules.

3. The bacteriostatic and anti-inflammatory oral care complex of claim 1, wherein, The preparation method of the Curcuma longa extract includes: S1. Take fresh turmeric rhizomes, wash, slice, dry, and pulverize them through a 40-60 mesh sieve to obtain powder; S2. The powder is loaded into a supercritical extraction vessel and extracted using supercritical CO2 fluid; then the fluid enters a separation vessel for depressurization separation, and the effluent from the bottom of the separation vessel is collected to obtain turmeric essential oil extract.

4. The bacteriostatic anti-inflammatory oral care complex of claim 3, wherein, The extraction process involves an extraction pressure of 25-35 MPa, an extraction temperature of 40-50℃, an extraction time of 2-3 h, a CO2 flow rate of 15-25 L / h, and the use of 95% ethanol as an entrainer, with the amount of entrainer being 1-3% of the material mass.

5. The bacteriostatic anti-inflammatory oral care complex according to claim 1, wherein, The method for preparing birch powder and birch sap concentrate includes: collecting fresh birch sap, coarsely filtering it through a 300-400 mesh stainless steel filter, and then pumping it into a ceramic inorganic membrane module with a pore size of 0.1-0.2 μm for microfiltration at an operating pressure of 0.1-0.2 MPa and a temperature of 15-25°C; collecting the microfiltration permeate and pumping it into a hollow fiber ultrafiltration membrane module with a molecular weight cutoff of 10000 Da for ultrafiltration at an operating pressure of 0.2-0.4 MPa, collecting the ultrafiltration retentate containing macromolecular substances and the ultrafiltration permeate containing small molecules; freeze-drying the ultrafiltration retentate to obtain birch powder; and concentrating the ultrafiltration permeate to obtain birch sap concentrate.

6. The antibacterial and anti-inflammatory oral care compound according to claim 5, characterized in that, The freeze-drying steps are as follows: the ultrafiltration retentate is placed in a freeze dryer and pre-frozen at -40°C to -50°C for 4-6 hours, and then sublimated and dried at a cold trap temperature of -60°C and a vacuum degree of less than 20 Pa for 24-36 hours.

7. The antibacterial and anti-inflammatory oral care compound according to claim 5, characterized in that, The concentration step is as follows: the ultrafiltration permeate is pumped into a nanofiltration membrane module with a molecular weight cutoff of 150-300 Da, and concentration is carried out at an operating pressure of 1.5-2.5 MPa. During the concentration process, jacket cooling water circulation is used to control the operating temperature at 15-20℃. Concentration is stopped when the solid content of the system reaches 15-20%, and the birch sap concentrate is obtained.

8. The use of the antibacterial and anti-inflammatory oral care complex according to any one of claims 1-7 in oral health maintenance products, characterized in that, The products include one or more of the following: oral spray, mouthwash, tooth powder, dental care gel, and toothpaste.

9. An antibacterial and anti-inflammatory oral care gel, characterized in that, The oral care complex comprising the antibacterial and anti-inflammatory compound of claim 1, wherein the gel comprises the following components: 5-15 parts of turmeric-birch bilayer microcapsules, 30-50 parts of birch sap concentrate, 0.5-2.0 parts of thickener, 0.1-0.5 parts of sodium hyaluronate, 2-5 parts of sweetener, 0.1-0.3 parts of dipotassium glycyrrhizate, and 30-50 parts of deionized water.

10. The method for preparing an antibacterial and anti-inflammatory oral care gel according to claim 9, characterized in that the step... include: (1) Disperse the thickener and sodium hyaluronate evenly in deionized water, let it stand to swell, and obtain a transparent gel matrix; (2) After the birch sap concentrate, sweetener and dipotassium glycyrrhizate are mixed evenly, they are added to the gel matrix and stirred evenly to obtain a primary gel. (3) Add the turmeric-birch bilayer microcapsules to the primary gel and stir evenly under a low shear force of 500-800 r / min to make it uniformly suspended; (4) Add a neutralizing agent to adjust the pH of the system to 5.5-6.5, and then degas under vacuum to obtain the final product.

Images