CN118217214A - An antiinflammatory and antibacterial toothpaste containing bisabolol and rhizoma Zingiberis recens, and its preparation method - Google Patents
An antiinflammatory and antibacterial toothpaste containing bisabolol and rhizoma Zingiberis recens, and its preparation method Download PDFInfo
- Publication number
- CN118217214A CN118217214A CN202410648930.1A CN202410648930A CN118217214A CN 118217214 A CN118217214 A CN 118217214A CN 202410648930 A CN202410648930 A CN 202410648930A CN 118217214 A CN118217214 A CN 118217214A
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- Prior art keywords
- ginger root
- oil
- temperature
- extract
- silicon dioxide
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- RGZSQWQPBWRIAQ-CABCVRRESA-N (-)-alpha-Bisabolol Chemical compound CC(C)=CCC[C@](C)(O)[C@H]1CCC(C)=CC1 RGZSQWQPBWRIAQ-CABCVRRESA-N 0.000 title claims abstract description 67
- RGZSQWQPBWRIAQ-LSDHHAIUSA-N alpha-Bisabolol Natural products CC(C)=CCC[C@@](C)(O)[C@@H]1CCC(C)=CC1 RGZSQWQPBWRIAQ-LSDHHAIUSA-N 0.000 title claims abstract description 67
- 239000000606 toothpaste Substances 0.000 title claims abstract description 67
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- 229940034610 toothpaste Drugs 0.000 title claims abstract description 64
- 238000002360 preparation method Methods 0.000 title claims abstract description 47
- 230000003110 anti-inflammatory effect Effects 0.000 title claims abstract description 41
- WTVHAMTYZJGJLJ-UHFFFAOYSA-N (+)-(4S,8R)-8-epi-beta-bisabolol Natural products CC(C)=CCCC(C)C1(O)CCC(C)=CC1 WTVHAMTYZJGJLJ-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 229940036350 bisabolol Drugs 0.000 title claims abstract description 29
- HHGZABIIYIWLGA-UHFFFAOYSA-N bisabolol Natural products CC1CCC(C(C)(O)CCC=C(C)C)CC1 HHGZABIIYIWLGA-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 229940102465 ginger root Drugs 0.000 claims abstract description 53
- 239000001841 zingiber officinale Substances 0.000 claims abstract description 53
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 146
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 47
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 45
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 42
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 42
- 239000001500 (2R)-6-methyl-2-[(1R)-4-methyl-1-cyclohex-3-enyl]hept-5-en-2-ol Substances 0.000 claims description 38
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- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 21
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Abstract
The invention relates to an anti-inflammatory antibacterial toothpaste containing bisabolol and ginger root components and a preparation method thereof, and belongs to a tooth cleaning preparation.
Description
Technical Field
The invention belongs to the technical field of tooth cleaning preparations, and in particular relates to anti-inflammatory and antibacterial toothpaste containing bisabolol and ginger root components and a preparation method thereof.
Background
Periodontal disease is a multifactorial disease that severely affects the oral health of humans, including mild periodontal disease, also known as gingivitis, and severe periodontal disease, also known as periodontitis. Wherein gingivitis is manifested by red, swelling, pain, bleeding, etc.; periodontitis is manifested by gingival atrophy, loosening of the teeth bones, and the like. Periodontal disease has many etiologies, and is mainly caused by dental plaque and calculus. Among them, plaque biofilm is a major causative factor, and bacteria and products thereof in plaque biofilm are essential initiating factors for initiating periodontal disease. However, dental calculus in the oral cavity can continuously stimulate periodontal tissues, so that the periodontal tissues are easy to be infected by pathogenic bacteria, inflammation is generated, the periodontal tissues are gradually atrophic, and periodontal diseases are further formed.
Bacteria mainly exist in the form of dental plaque in the oral cavity of a human body, the current treatment for gum problems is mainly carried out from the aspects of bacteriostasis, inflammation diminishing, local symptom relieving and the like, and the common method for controlling the dental plaque comprises the following steps: (1) mechanical measures: removing bacterial plaque and food residues in teeth or gingival sulcus by using toothbrushes, dental floss, interdental brushes and the like, preventing a large amount of dental plaque from remaining, and keeping the bacterial count under the gingiva below the level of triggering inflammation; (2) chemical method: the mouthwash or toothpaste containing the antibacterial substances is used for cleaning the oral cavity, and is helpful for preventing or reducing bacterial accumulation and the formation of dental biofilms.
For the initial oral inflammatory reaction, the inflammatory process can be controlled by using toothpaste or mouthwash containing common anti-inflammatory substances to inhibit inflammatory mediators; when inflammation is not effectively controlled and gradually developed into gingival recession, periodontal ligament is destroyed, alveolar bone is destroyed and absorbed, drug treatment such as toothpaste or mouthwash with focus-specific western medicine component is also required. Western medicine components such as triclosan, fluoride and cetylpyridinium chloride, but long-term use of gargle or toothpaste containing Western medicine is extremely liable to cause drug resistance of human body, so that oral care compositions containing natural antibacterial and anti-inflammatory components are attracting attention. CN114306195A, for example, discloses a bacteriostatic composition for use in oral care products, a method of preparation and use thereof. The composition comprises conventional components and antibacterial components, wherein the antibacterial components comprise: bisabolol and ginger root mixed extract, dipotassium glycyrrhizinate, propolis extract and lactic acid bacteria. The four components together have a synergistic effect, and can remarkably improve the inhibition rate of helicobacter pylori in the oral cavity. CN105283166a discloses an antimicrobial composition comprising an essential oil combination, the ingredients comprising bisabolol, citral, carvacrol, oregano extract essential oil, etc. ingredients for oral care. CN115998796a discloses an antibacterial and anti-inflammatory oral rinse solution, and its preparation method and application, the ingredients include thymol, clove oil, peppermint oil, eucalyptus oil, wintergreen oil, astaxanthin, solubilizer, auxiliary materials and purified water, through mutual cooperation of the ingredients, the composition has remarkable inhibition effect on fungi, gram positive bacteria and gram negative bacteria, and is nontoxic and harmless, breaks and rebuilds oral bacteria, and ensures oral health.
However, the existing natural plant antibacterial components have the problem of unsatisfactory antibacterial effect in practical application, and the rapid and continuous formation of dental plaque is prevented by daily tooth brushing, so that the growth retardation degree of the dental plaque is poor. In the research, we find that the specific extraction method of the plant extract determines specific components of the product, the obtained action and efficacy are different, in addition (such as eucalyptus oil, clove oil, bisabolol, ginger root extract and the like), the specific proportion of each component and the mixed preparation method also influence the strength of the anti-inflammatory and antibacterial efficacy, and if the scientific proportion compounding and preparation method are adopted, the component dosage can be reduced, and the better anti-inflammatory and antibacterial effects are exerted. Therefore, how to design an extraction method, how to obtain a plant extract with outstanding action and efficacy, how to select each component and proportion, and how to adopt a compound preparation method, so as to reduce the component dosage, obtain more excellent anti-inflammatory and antibacterial effects, efficiently realize the effects of inhibiting oral pathogenic bacteria, reducing inflammatory factors and rapidly relieving oral inflammation is a problem to be solved, and the technology needs to be continuously developed and improved.
Disclosure of Invention
Aiming at the poor growth retardation degree of dental plaque in the existing natural plant antibacterial components, the preparation method is required to be continuously improved in the aspects of component extraction method, preparation proportion, mixed preparation method and the like, so that more excellent anti-inflammatory antibacterial effect is achieved, the effects of inhibiting oral pathogenic bacteria, reducing inflammatory factors and rapidly relieving oral inflammation are realized. The invention provides an anti-inflammatory and antibacterial toothpaste containing bisabolol and ginger root components and a preparation method thereof, and the anti-inflammatory and antibacterial toothpaste comprises hawaii nut oil, eucalyptus oil, vine fruit oil, clove oil, alpha-bisabolol, ginger root extract and locust bean extract, wherein after the polymers of the alpha-bisabolol, the ginger root extract and the locust bean extract are loaded by silicon dioxide, the polymers absorb and wrap part of hawaii nut oil, eucalyptus oil, vine fruit oil and clove oil, fully contact with teeth and gingiva through friction and partially remain, the effects of greatly improving the inhibition and the inflammation delay of various bacteria can be realized under low dosage, dental plaque can be effectively and rapidly removed, pathogenic bacteria in oral cavity can be effectively reduced, inflammatory factors in oral cavity can be reduced, and oral health state can be maintained. The specific technical scheme is as follows:
An anti-inflammatory antibacterial toothpaste containing bisabolol and ginger root components is prepared from the following raw materials in parts by weight: 0.004 to 0.008 part of macadamia nut oil, 0.004 to 0.008 part of eucalyptus oil, 0.004 to 0.008 part of merry-go-round-robinia nut oil, 0.004 to 0.008 part of clove oil, 0.01 to 0.03 part of alpha-bisabolol, 0.005 to 0.008 part of ginger root extract, 0.005 to 0.01 part of locust bean extract, 25 to 35 parts of silicon dioxide, 20 to 25 parts of humectant, 0.5 to 1 part of thickener, 1.8 to 2.5 parts of surfactant, 1 to 2.5 parts of flavoring agent, 0.0005 to 0.001 part of sweetener and 12 to 20 parts of purified water.
In the above technical scheme, the preparation method of the ginger root extract comprises the following steps: taking fresh ginger root, crushing to obtain ginger crushed, adding 3-5 times of water with the crushed mass of ginger into the ginger crushed, crushing and pulping to obtain slurry, adding 0.05-0.1 time of lemon juice with the crushed mass of the slurry into the slurry, soaking for 1-1.5 hours at the temperature of 40-45 ℃, filtering, taking a filter cake, drying, dispersing the filter cake into 6-8 times of water with the filter cake mass, regulating the pH value to 4.8-5.2 by using citric acid, adding hemicellulase, carrying out enzymolysis for 1.5-2 hours at the temperature of 50-60 ℃, carrying out high-temperature enzyme deactivation, reducing the temperature to room temperature, regulating the pH value to 6.8-7.2 by using sodium hydroxide, adding Serratinase and bromelain, carrying out enzymolysis for 1.5-2 hours at the temperature of 40-45 ℃, carrying out high-temperature enzyme deactivation, reducing the temperature to room temperature, filtering by using a 20kDa ultrafiltration membrane, collecting filtrate smaller than 20kDa, concentrating, drying, and crushing into nano-powder, thus obtaining the ginger root extract.
In the technical scheme, the addition amount of the hemicellulase is 0.3-0.8% of the mass of the ginger root, and the enzyme activity of the hemicellulase is 50000U/g-100000U/g; the adding amount of the Serratia peptidase is 0.2-0.5% of the mass of ginger root, and the enzyme activity of the Serratia peptidase is 30000U/g-50000U/g; the addition amount of the bromelain is 1-3% of the mass of ginger root, and the enzyme activity of the bromelain is 100000U/g-200000U/g; the high-temperature enzyme deactivation temperature is 85-100 ℃ and the time is 25-35 min.
In the above technical scheme, the preparation method of the locust bean extract comprises the following steps: crushing fresh locust beans, adding water with the mass of 6-8 times of that of the locust beans, regulating the pH value to 4.8-5.2 by adopting hydrochloric acid, adding hemicellulase, carrying out enzymolysis for 1.5-2 hours at 50-60 ℃, inactivating enzyme at high temperature, cooling to room temperature, continuously regulating the pH value to 1.5-2.0 by adopting hydrochloric acid, adding pepsin, carrying out enzymolysis for 1.5-2 hours at 35-38 ℃, inactivating enzyme at high temperature, cooling to room temperature, regulating the pH value to 7.5-7.8 by adopting sodium hydroxide, adding subtilisin, carrying out enzymolysis for 1-1.5 hours at 32-38 ℃, carrying out high temperature inactivating enzyme, cooling to room temperature, filtering by adopting a 20kDa ultrafiltration membrane, collecting filtrate smaller than 20kDa, concentrating, drying, and crushing into nano-powder to obtain the locust bean extract.
In the technical scheme, the addition amount of the hemicellulase is 0.3-0.8% of the mass of the locust bean, and the enzyme activity of the hemicellulase is 50000U/g-100000U/g; the addition amount of the pepsin is 1-2.5% of the mass of the locust bean, and the enzyme activity of the pepsin is 10000U/g-12000U/g; the addition amount of the subtilisin is 0.2-0.5% of the mass of the locust bean, and the enzyme activity of the subtilisin is 10000U/g-20000U/g; the high-temperature enzyme deactivation temperature is 85-100 ℃ and the time is 25-35 min.
In the technical scheme, the median particle size of the silicon dioxide is 8-20 mu m, the oil absorption value of the silicon dioxide is 100-105 g/100g, the water absorption is 15-20 mL/20g, and the transparency within the range of refractive index 1.440-1.460 is more than or equal to 92%.
In the technical scheme, the humectant comprises the components of sorbitol and propylene glycol, wherein the mass ratio of the sorbitol to the propylene glycol= (5-7.5) is (1-1.5).
In the technical scheme, the thickener comprises sodium carboxymethyl cellulose, xanthan gum and guar gum, wherein the mass ratio of sodium carboxymethyl cellulose to guar gum is (1-1.5), and the mass ratio of sodium carboxymethyl cellulose to guar gum is (0.5-1), and the mass ratio of sodium carboxymethyl cellulose to guar gum is (1-1.5).
In the technical scheme, the surfactant is sodium dodecyl sulfate.
In the technical scheme, the flavoring agent is essence.
In the above technical scheme, the sweetener is sucralose, xylitol or erythritol.
The preparation method of the anti-inflammatory antibacterial toothpaste containing bisabolol and ginger root components comprises the following steps:
s1: dispersing alpha-bisabolol, ginger root extract, locust bean extract and sweetener in an ethanol water solution to obtain a spray, spraying silicon dioxide and the spray in a fluidization way, spraying the ginger root extract and the locust bean extract on the surfaces of silicon dioxide particles, and freeze-drying to obtain silicon dioxide loaded with the extracts;
S2: mixing macadamia nut oil, eucalyptus oil, merry-go-round oil and clove oil according to parts by weight to obtain mixed oil;
s3: evenly mixing the silicon dioxide loaded with the extract, the mixed oil and the humectant to obtain phase A;
S4: uniformly mixing the purified water and the thickener at 80-85 ℃ to obtain phase B, and reducing the temperature to 40-45 ℃ for standby;
S5: evenly mixing the phase A, the phase B, the flavoring agent and the surfactant to obtain the toothpaste.
In the preparation method S1, the ethanol water solution contains 15-25% vol of ethanol; the dosage of the ethanol aqueous solution is 0.15 to 0.25 times of the mass of the silicon dioxide; the parameters of the fluidization spray are as follows: the spray is fed at 25-30 ℃, the spraying speed is 0.2-0.3L/min, the atomization pressure is 0.5-0.7 MPa, and the discharge temperature is 40-45 ℃; the lyophilization is liquid nitrogen lyophilization.
In the S2 of the preparation method, the mixing temperature of the mixed oil is 30-40 ℃.
In the S3 of the preparation method, the uniform mixing temperature of the phase A is 30-40 ℃.
The anti-inflammatory antibacterial toothpaste containing bisabolol and ginger root components and the preparation method thereof provided by the invention have the beneficial effects that compared with the prior art:
1. The toothpaste of the invention contains active ingredients such as macadamia nut oil, eucalyptus oil, vine fruit oil, clove oil, alpha-bisabolol, ginger root extract, locust bean extract and the like. Wherein, the eucalyptus oil is a natural product, has good antibacterial, anti-inflammatory, permeation-promoting and antiseptic effects, and can inhibit the growth of microorganisms; the clove oil has pharmacological activities such as anti-inflammatory, analgesic, antioxidant and the like, has antibacterial effect, and can obviously inhibit the growth and propagation of bacteria and fungi. The toothpaste disclosed by the invention is designed to have lower addition amount of eucalyptus oil and clove oil, can reduce the pungent irritation of the eucalyptus oil and the clove oil, can well improve the taste of the toothpaste when being used together with alpha-bisabolol with low addition amount, has good antibacterial and detumescent effects, and has good effects of inhibiting the growth and removal of dental plaque; the alpha-bisabolol and ginger root extract have anti-inflammatory effect, and the combination of eucalyptus oil and clove oil greatly enhances the antibacterial and anti-inflammatory effects, so that the antibacterial and anti-inflammatory effects are obviously improved compared with the independent use effect, and the dosage is obviously reduced; meanwhile, the special spicy taste brought by eucalyptus oil and clove oil can be reduced, and the acceptance of users is improved. The principle of action is that the applicant speculates that the alpha-bisabolol, the ginger root extract and the locust bean extract form macromolecular polymers when the ethanol aqueous solution is added, so that the macromolecular polymers have certain absorption and encapsulation effects on the subsequent eucalyptus oil and clove oil, and the pungent smell and spicy taste of the eucalyptus oil and the clove oil are reduced. In addition, proper amounts of macadamia nut oil and vine fruit oil are added to have fragrance, and the flavor and the smell of the toothpaste can be greatly improved by matching with the flavoring agent and the sweetener, so that good palatability is achieved.
2. The macadamia nut oil and the merry fruit oil also have certain antibacterial, detumescence and anti-inflammatory effects, have good promotion effects on inhibiting dental plaque and improving gingivitis, and can achieve high-content antibacterial and bactericidal effects when being used together with low-content eucalyptus oil and clove oil; in particular, the combination of the Hawaii stone oil and the Meinaria oil can well improve the antibacterial property to Porphyromonas gingivalis, proteus intermedia and Fusobacterium nucleatum.
3. The alpha-bisabolol can inhibit primary reaction of inflammation by regulating cytokines, mainly inhibit IL-1 alpha and TNF-alpha to prevent reaction, and inhibit IL-6 alpha and IL-8 to reduce redness from the source by adding a small amount of alpha-bisabolol and ginger root extract and reasonably proportioning with other components. Ginger root extract mainly inhibits secondary reactions of inflammation by regulating lipid mediators, mainly including COX-2 and PGE-2, thereby preventing redness and erythema. The ginger root extract is subjected to fractional enzymolysis extraction by adopting hemicellulase, serratia peptidase and bromelain, so that a product with lower pungency and better antibacterial effect can be obtained, and the antibacterial property of Porphyromonas gingivalis, fusarium oxysporum and Fusobacterium nucleatum can be relatively improved; achieving the effect of high bacteriostasis with low content.
4. The invention designs adding locust bean extract, and adopts fresh locust beans to carry out graded enzymolysis by adopting hemicellulase, pepsin and subtilisin, so that the obtained locust bean extract has good antibacterial, detumescence and anti-inflammatory effects, can help to repair gingival cells, restore normal state and resist damage of bacteria, dental calculus and inflammation. The locust bean extract, the ginger root extract and the alpha-bisabolol are compounded for use, so that the effect of improving dental plaque and gingivitis is more remarkable, and the nursing of the oral cavity can be realized quickly and efficiently.
5. The preparation method of the invention utilizes the sweetener to increase the viscosity of the spray, and sprays the active ingredients such as alpha-bisabolol, ginger root extract, locust bean extract and the like on the silicon dioxide, when brushing teeth, the silicon dioxide can be used as the abrasive to enable the active ingredients loaded on the surface of the silicon dioxide to adhere to the surface of teeth well through the friction force between the silicon dioxide and the surface of dental plaque, the active ingredients are fully contacted with the dental plaque and remain on the surface of teeth for a long time, so that the dental plaque can be removed well after long-term use, and the speed and effect of removing the dental plaque are greatly improved.
6. The median particle diameter of the silicon dioxide is 8-20 mu m, the oil absorption value of the silicon dioxide is 100-105 g/100g, the water absorption amount is 15-20 mL/20g, and the transparency of the silicon dioxide in the range of 1.440-1.460 is more than or equal to 92%. The silica parameter has good oil absorption, is easy to disperse uniformly, can not be agglomerated, can keep partial residues in the oral cavity after brushing teeth, and has the surface of the silica attached with partial macadamia nut oil, eucalyptus oil, vine fruit oil, clove oil, alpha-bisabolol, ginger root extract and locust bean extract, so that the long-acting antibacterial effect in the oral cavity can be kept.
In conclusion, the macadamia nut oil, the eucalyptus oil, the merry-go-round-robinia nut oil, the clove oil, the alpha-bisabolol, the ginger root extract and the locust bean extract can generate a synergistic effect after being proportioned, the effects of greatly improving the inhibition of various bacteria and delaying inflammation are realized at a low dosage, dental plaque is effectively and rapidly desalted and removed, oral pathogenic bacteria are effectively reduced, oral inflammatory factors are reduced, and therefore oral inflammation is rapidly slowed down, the oral health state is maintained, and the macadamia nut oil tea has good practical value.
Detailed Description
The invention will be further illustrated with reference to specific examples, but the invention is not limited to these examples.
Example 1
An anti-inflammatory antibacterial toothpaste containing bisabolol and ginger root components is prepared from the following raw materials in parts by weight: 0.006 parts of Hawaii stone oil, 0.006 parts of eucalyptus oil, 0.006 parts of vine fruit oil, 0.006 parts of clove oil, 0.02 parts of alpha-bisabolol, 0.006 parts of ginger root extract, 0.008 parts of locust bean extract, 30 parts of silicon dioxide, 22 parts of humectant, 0.8 part of thickener, 2 parts of surfactant, 1.8 parts of flavoring agent, 0.0008 parts of sweetener and 16 parts of purified water; wherein, the median particle diameter of the silicon dioxide is 10.2 mu m, the oil absorption value of the silicon dioxide is 102g/100g, the water absorption capacity is 18mL/20g, and the transparency in the range of refractive index 1.440-1.460 is 93%; the humectant comprises sorbitol and propylene glycol, wherein the mass ratio of sorbitol to propylene glycol=6:1.2; the thickener comprises sodium carboxymethyl cellulose, xanthan gum and guar gum in a mass ratio of sodium carboxymethyl cellulose to xanthan gum=1.2:0.6:1.1; the surfactant is sodium dodecyl sulfate; the flavoring agent is blackberry essence; the sweetener is sucralose.
The preparation method of the ginger root extract in the embodiment comprises the following steps: crushing fresh ginger root to obtain ginger crushed, adding water with the weight of 4 times of the ginger crushed weight into the ginger crushed, crushing and pulping to obtain slurry, adding lemon juice with the weight of 0.08 times of the slurry into the slurry, soaking for 1.5h at 42 ℃, filtering, taking and drying a filter cake, dispersing the filter cake into water with the weight of 7 times of the filter cake, regulating the pH to 5.0 by adopting citric acid, adding hemicellulase with the weight of 0.5% of the ginger root and the enzyme activity of 80000U/g, carrying out enzymolysis for 1.5h at 55 ℃, inactivating enzyme for 30min at 90 ℃, regulating pH7.0 by adopting sodium hydroxide after cooling to room temperature, adding Serratin peptidase with the weight of 0.3% of the ginger root and the enzyme activity of 40000U/g, adding pineapple proteinase with the weight of 2% of the ginger root and the enzyme activity of 150000U/g, carrying out enzymolysis for 1.5h at 42 ℃, carrying out enzymolysis for 30min at high temperature, carrying out enzymolysis for room temperature, filtering by adopting a 20kDa ultrafiltration membrane, collecting filtrate with the weight of less than 20kDa, concentrating, drying, and crushing to obtain the ginger extract.
The preparation method of the locust bean extract in the embodiment comprises the following steps: pulverizing fresh locust bean, adding 7 times of water, regulating pH to 5.0 with hydrochloric acid, adding hemicellulase with pH of 0.5% and enzyme activity of 80000U/g, performing enzymolysis at 55deg.C for 1.5 hr, inactivating enzyme at 90deg.C for 30min, cooling to room temperature, regulating pH to 1.8 with hydrochloric acid, adding pepsin with pH of 2% and enzyme activity of 10000U/g, performing enzymolysis at 37deg.C for 1.5 hr, inactivating enzyme at 90deg.C for 30min, cooling to room temperature, regulating pH to.6 with sodium hydroxide, adding subtilisin with pH of 0.3% and enzyme activity of 10000U/g, performing enzymolysis at 36deg.C for 1 hr, inactivating enzyme at 90deg.C for 30min, cooling to room temperature, filtering with 20kDa ultrafiltration membrane, collecting filtrate of less than 20kDa, concentrating, drying, and pulverizing into nanometer powder to obtain locust bean extract.
The preparation method of the anti-inflammatory antibacterial toothpaste containing bisabolol and ginger root components comprises the following steps:
s1: dispersing alpha-bisabolol, ginger root extract, locust bean extract and sweetener in an ethanol water solution to obtain a spray, spraying silicon dioxide and the spray in a fluidization way, spraying the ginger root extract and the locust bean extract on the surfaces of silicon dioxide particles, and freeze-drying by liquid nitrogen to obtain silicon dioxide loaded with the extract;
Wherein the ethanol aqueous solution contains 20% vol of ethanol; the dosage of the ethanol aqueous solution is 0.2 times of the mass of the silicon dioxide; the parameters of the fluidization spray are: the spray temperature is 28 ℃, the spray speed is 0.25L/min, the atomization pressure is 0.6MPa, and the discharge temperature is 42 ℃;
S2: mixing macadamia nut oil, eucalyptus oil, merry fruit oil and clove oil according to parts by weight at 35 ℃ to obtain mixed oil;
s3: uniformly mixing the silicon dioxide loaded with the extract, the mixed oil and the humectant at 35 ℃ to obtain a phase A;
S4: uniformly mixing the purified water and the thickener at 82 ℃ to obtain phase B, and cooling to 42 ℃ for later use;
S5: evenly mixing the phase A, the phase B, the flavoring agent and the surfactant to obtain the toothpaste.
Example 2
An anti-inflammatory antibacterial toothpaste containing bisabolol and ginger root components is prepared from the following raw materials in parts by weight: 0.008 parts of Hawaii stone oil, 0.008 parts of eucalyptus oil, 0.008 parts of merry-go-round oil, 0.008 parts of clove oil, 0.03 parts of alpha-bisabolol, 0.008 parts of ginger root extract, 0.01 parts of locust bean extract, 35 parts of silicon dioxide, 25 parts of humectant, 1 part of thickener, 2.5 parts of surfactant, 2.5 parts of flavoring agent, 0.001 part of sweetener and 20 parts of purified water; wherein, the median particle diameter of the silicon dioxide is 20 mu m, the oil absorption value of the silicon dioxide is 105g/100g, the water absorption capacity is 20mL/20g, and the transparency in the range of refractive index 1.440-1.460 is 94%; the humectant comprises sorbitol and propylene glycol, wherein the mass ratio of sorbitol to propylene glycol=7.5:1.5; the thickener comprises sodium carboxymethyl cellulose, xanthan gum and guar gum in a mass ratio of sodium carboxymethyl cellulose to xanthan gum=1.5:1:1.5; the surfactant is sodium dodecyl sulfate; the flavoring agent is strawberry essence; the sweetener is xylitol.
The preparation method of the ginger root extract in the embodiment comprises the following steps: crushing fresh ginger root to obtain ginger crushed, adding water with the mass of 5 times of ginger crushed, crushing and pulping to obtain slurry, adding lemon juice with the mass of 0.1 time of slurry into the slurry, soaking for 1.5h at 45 ℃, filtering, taking and drying a filter cake, dispersing the filter cake into water with the mass of 8 times of filter cake, adopting citric acid to adjust pH to 5.2, adding hemicellulase with the mass of 0.8% of ginger root and the enzyme activity of 100000U/g, carrying out enzymolysis at 60 ℃ for 2h, carrying out high-temperature enzyme deactivation at 100 ℃ for 35min, cooling to room temperature, adopting sodium hydroxide to adjust pH to.2, adding Serratin enzyme with the mass of 0.5% of ginger root and the enzyme activity of 50000U/g, adding bromelain with the mass of 3% of ginger root and the enzyme activity of 200000U/g, carrying out enzymolysis at 45 ℃ for 2h, carrying out high-temperature enzyme deactivation at 100 ℃ for 35min, cooling to room temperature, adopting a 20kDa ultrafiltration membrane to filter, collecting filtrate with the concentration, drying, and crushing into the ginger root extract.
The preparation method of the locust bean extract in the embodiment comprises the following steps: pulverizing fresh locust bean, adding 8 times of water, regulating pH to 5.2 with hydrochloric acid, adding 0.8% of hemicellulase with enzyme activity of 100000U/g, performing enzymolysis at 60deg.C for 2 hr, inactivating enzyme at 100deg.C for 35min, cooling to room temperature, regulating pH to 2.0 with hydrochloric acid, adding 2.5% of pepsin with enzyme activity of 12000U/g, performing enzymolysis at 38deg.C for 2 hr, inactivating enzyme at 100deg.C for 35min, cooling to room temperature, regulating pH to 8 with sodium hydroxide, adding 0.5% of subtilisin with enzyme activity of 20000U/g, performing enzymolysis at 38deg.C for 1.5 hr, inactivating enzyme at 100deg.C for 35min, cooling to room temperature, filtering with 20kDa ultrafiltration membrane, collecting filtrate smaller than 20kDa, concentrating, drying, pulverizing into nanometer powder to obtain locust bean extract.
The preparation method of the anti-inflammatory antibacterial toothpaste containing bisabolol and ginger root components comprises the following steps:
s1: dispersing alpha-bisabolol, ginger root extract, locust bean extract and sweetener in an ethanol water solution to obtain a spray, spraying silicon dioxide and the spray in a fluidization way, spraying the ginger root extract and the locust bean extract on the surfaces of silicon dioxide particles, and freeze-drying by liquid nitrogen to obtain silicon dioxide loaded with the extract;
wherein the ethanol aqueous solution contains 25% vol of ethanol; the dosage of the ethanol aqueous solution is 0.25 times of the mass of the silicon dioxide; the parameters of the fluidization spray are: the spray is heated to 30 ℃, the spraying speed is 0.3L/min, the atomization pressure is 0.7MPa, and the discharge temperature is 45 ℃;
S2: mixing macadamia nut oil, eucalyptus oil, merry fruit oil and clove oil according to parts by weight at 40 ℃ to obtain mixed oil;
S3: uniformly mixing the silicon dioxide loaded with the extract, the mixed oil and the humectant at 40 ℃ to obtain a phase A;
S4: uniformly mixing the purified water and the thickener at 85 ℃ to obtain a phase B, and cooling to 45 ℃ for standby;
S5: evenly mixing the phase A, the phase B, the flavoring agent and the surfactant to obtain the toothpaste.
Example 3
An anti-inflammatory antibacterial toothpaste containing bisabolol and ginger root components is prepared from the following raw materials in parts by weight: 0.008 parts of macadamia nut oil, 0.004 parts of eucalyptus oil, 0.008 parts of merry-go-round oil, 0.004 parts of clove oil, 0.03 parts of alpha-bisabolol, 0.005 parts of ginger root extract, 0.01 part of locust bean extract, 25 parts of silicon dioxide, 25 parts of humectant, 0.5 part of thickener, 2.5 parts of surfactant, 2.5 parts of flavoring agent, 0.0005 parts of sweetener and 16 parts of purified water; wherein, the median particle diameter of the silicon dioxide is 8 mu m, the oil absorption value of the silicon dioxide is 105g/100g, the water absorption capacity is 15mL/20g, and the transparency in the range of refractive index 1.440-1.460 is 94%; the humectant comprises sorbitol and propylene glycol, wherein the mass ratio of sorbitol to propylene glycol=7:1.5; the thickener comprises sodium carboxymethyl cellulose, xanthan gum and guar gum in a mass ratio of sodium carboxymethyl cellulose to xanthan gum=1:1:1; the surfactant is sodium dodecyl sulfate; the flavoring agent is pineapple essence; the sweetener is erythritol.
The preparation method of the ginger root extract in the embodiment comprises the following steps: crushing fresh ginger root to obtain ginger crushed, adding 5 times of water with the crushed mass of the ginger into the ginger crushed, crushing and pulping to obtain slurry, adding 0.05 times of lemon juice with the crushed mass of the ginger into the slurry, soaking for 1h at 45 ℃, filtering, taking a filter cake, drying, dispersing the filter cake into 8 times of water with the crushed mass of the filter cake, adopting citric acid to adjust pH to 4.8, adding hemicellulase with the weight of 0.8% of the ginger root and the enzyme activity of 50000U/g, carrying out enzymolysis at 60 ℃ for 1.5h, carrying out high-temperature enzyme deactivation at 100 ℃ for 25min, cooling to room temperature, adopting sodium hydroxide to adjust pH7.2, adding the pineapple proteinase with the weight of 0.2% of the ginger root and the enzyme activity of 50000U/g, carrying out enzymolysis at 40 ℃ for 2h, carrying out enzymolysis at 85 ℃ for 35min, carrying out enzymolysis at 85 ℃ and cooling to room temperature, adopting a 20kDa ultrafiltration membrane to filter, collecting filtrate with the weight of less than 20kDa, concentrating, drying, and crushing into ginger nano-powder.
The preparation method of the locust bean extract in the embodiment comprises the following steps: pulverizing fresh locust bean, adding 6 times of water, regulating pH to 5.2 with hydrochloric acid, adding hemicellulase with 0.3% of the mass of locust bean and enzymatic activity of 100000U/g, performing enzymolysis at 50deg.C for 2h, inactivating enzyme at 85deg.C for 35min, cooling to room temperature, continuously regulating pH to 1.5 with hydrochloric acid, adding pepsin with 2.5% of the mass of locust bean and enzymatic activity of 10000U/g, performing enzymolysis at 38deg.C for 1.5h, inactivating enzyme at 100deg.C for 25min, cooling to room temperature, regulating pH to.8 with sodium hydroxide, adding subtilisin with 0.2% of the mass of locust bean and enzymatic activity of 20000U/g, performing enzymolysis at 32deg.C for 1.5h, inactivating enzyme at 85deg.C for 35min, cooling to room temperature, filtering with 20kDa ultrafiltration membrane, collecting filtrate of less than 20kDa, concentrating, drying, pulverizing into nanometer powder to obtain the extract.
The preparation method of the anti-inflammatory antibacterial toothpaste containing bisabolol and ginger root components comprises the following steps:
s1: dispersing alpha-bisabolol, ginger root extract, locust bean extract and sweetener in an ethanol water solution to obtain a spray, spraying silicon dioxide and the spray in a fluidization way, spraying the ginger root extract and the locust bean extract on the surfaces of silicon dioxide particles, and freeze-drying by liquid nitrogen to obtain silicon dioxide loaded with the extract;
Wherein the ethanol aqueous solution contains 15% vol of ethanol; the dosage of the ethanol aqueous solution is 0.25 times of the mass of the silicon dioxide; the parameters of the fluidization spray are: the spray is heated to 25 ℃, the spraying speed is 0.3L/min, the atomization pressure is 0.5MPa, and the discharge temperature is 45 ℃;
S2: mixing macadamia nut oil, eucalyptus oil, merry fruit oil and clove oil according to parts by weight at 30 ℃ to obtain mixed oil;
S3: uniformly mixing the silicon dioxide loaded with the extract, the mixed oil and the humectant at 40 ℃ to obtain a phase A;
s4: uniformly mixing the purified water and the thickener at 80 ℃ to obtain a phase B, and cooling to 45 ℃ for standby;
S5: evenly mixing the phase A, the phase B, the flavoring agent and the surfactant to obtain the toothpaste.
Example 4
An anti-inflammatory antibacterial toothpaste containing bisabolol and ginger root components is prepared from the following raw materials in parts by weight: 0.004 parts of Hawaii stone oil, 0.008 parts of eucalyptus oil, 0.004 parts of merry-go-round oil, 0.008 parts of clove oil, 0.01 parts of alpha-bisabolol, 0.008 parts of ginger root extract, 0.005 parts of locust bean extract, 35 parts of silicon dioxide, 20 parts of humectant, 1 part of thickener, 1.8 parts of surfactant, 1 part of flavoring agent, 0.001 part of sweetener and 17 parts of purified water; wherein, the median particle diameter of the silicon dioxide is 20 mu m, the oil absorption value of the silicon dioxide is 100g/100g, the water absorption capacity is 20mL/20g, and the transparency in the range of refractive index 1.440-1.460 is 92%; the humectant comprises sorbitol and propylene glycol, wherein the mass ratio of sorbitol to propylene glycol=5.5:1; the thickener comprises sodium carboxymethyl cellulose, xanthan gum and guar gum in a mass ratio of sodium carboxymethyl cellulose to xanthan gum=1.5:0.5:1.5; the surfactant is sodium dodecyl sulfate; the flavoring agent is apple essence; the sweetener is sucralose.
The preparation method of the ginger root extract in the embodiment comprises the following steps: crushing fresh ginger root to obtain ginger crushed, adding 3 times of water with the crushed mass into the ginger crushed, crushing and pulping to obtain slurry, adding 0.1 time of lemon juice with the crushed mass into the slurry, soaking for 1.5h at 40 ℃, filtering, taking and drying a filter cake, dispersing the filter cake into water with the weight which is 6 times of that of the filter cake, adopting citric acid to adjust the pH value to 5.2, adding hemicellulase with the weight which is 0.3% of that of the ginger root and the enzyme activity to 100000U/g, carrying out enzymolysis at 50 ℃ for 2h, carrying out high-temperature enzyme deactivation at 85 ℃ for 35min, reducing to room temperature, adopting sodium hydroxide to adjust the pH value to 6.8, adding the pineapple proteinase with the weight which is 0.5% of that of the ginger root and the enzyme activity to 30000U/g, carrying out enzymolysis at 45 ℃ for 1.5h, carrying out enzymolysis at 100 ℃ for 25min, carrying out enzymolysis at 100 kDa, adopting a 20kDa ultrafiltration membrane to filter, collecting filtrate which is smaller than 20kDa, concentrating, drying, and crushing into nano-rice powder, thus obtaining ginger root extract.
The preparation method of the locust bean extract in the embodiment comprises the following steps: pulverizing fresh locust bean, adding 8 times of water, regulating pH to 4.8 with hydrochloric acid, adding hemicellulase with pH of 0.8% and enzyme activity of 50000U/g, performing enzymolysis at 60deg.C for 1.5 hr, inactivating enzyme at 100deg.C for 25min, cooling to room temperature, regulating pH to 2.0 with hydrochloric acid, adding pepsin with pH of 1% and enzyme activity of 12000U/g, performing enzymolysis at 35deg.C for 2 hr, inactivating enzyme at 85deg.C for 35min, cooling to room temperature, regulating pH to 5 with sodium hydroxide, adding subtilisin with pH of 0.5% and enzyme activity of 10000U/g, performing enzymolysis at 38deg.C for 1 hr, inactivating enzyme at 100deg.C for 25min, cooling to room temperature, filtering with 20kDa ultrafiltration membrane, collecting filtrate of less than 20kDa, concentrating, drying, and pulverizing into nanometer powder to obtain locust bean extract.
The preparation method of the anti-inflammatory antibacterial toothpaste containing bisabolol and ginger root components comprises the following steps:
s1: dispersing alpha-bisabolol, ginger root extract, locust bean extract and sweetener in an ethanol water solution to obtain a spray, spraying silicon dioxide and the spray in a fluidization way, spraying the ginger root extract and the locust bean extract on the surfaces of silicon dioxide particles, and freeze-drying by liquid nitrogen to obtain silicon dioxide loaded with the extract;
wherein the ethanol aqueous solution contains 25% vol of ethanol; the dosage of the ethanol aqueous solution is 0.15 times of the mass of the silicon dioxide; the parameters of the fluidization spray are: the spray is heated to 30 ℃, the spraying speed is 0.2L/min, the atomization pressure is 0.7MPa, and the discharge temperature is 40 ℃;
S2: mixing macadamia nut oil, eucalyptus oil, merry fruit oil and clove oil according to parts by weight at 40 ℃ to obtain mixed oil;
S3: uniformly mixing the silicon dioxide loaded with the extract, the mixed oil and the humectant at 30 ℃ to obtain a phase A;
S4: uniformly mixing the purified water and the thickener at 85 ℃ to obtain a phase B, and cooling to 40 ℃ for standby;
S5: evenly mixing the phase A, the phase B, the flavoring agent and the surfactant to obtain the toothpaste.
Example 5
An anti-inflammatory antibacterial toothpaste containing bisabolol and ginger root components is prepared from the following raw materials in parts by weight: 0.004 part of macadamia nut oil, 0.004 part of eucalyptus oil, 0.004 part of merry-go-round oil, 0.004 part of clove oil, 0.01 part of alpha-bisabolol, 0.005 part of ginger root extract, 0.005 part of locust bean extract, 25 parts of silicon dioxide, 20 parts of humectant, 0.5 part of thickener, 1.8 part of surfactant, 1 part of flavoring agent, 0.0005 part of sweetener and 12 parts of purified water; wherein, the median particle diameter of the silicon dioxide is 8 mu m, the oil absorption value of the silicon dioxide is 100g/100g, the water absorption capacity is 15mL/20g, and the transparency in the range of refractive index 1.440-1.460 is 92%; the humectant comprises sorbitol and propylene glycol, wherein the mass ratio of sorbitol to propylene glycol=5:1; the thickener comprises sodium carboxymethyl cellulose, xanthan gum and guar gum in a mass ratio of sodium carboxymethyl cellulose to xanthan gum=1:0.5:1; the surfactant is sodium dodecyl sulfate; the flavoring agent is litchi essence; the sweetener is sucralose.
The preparation method of the ginger root extract in the embodiment comprises the following steps: crushing fresh ginger root to obtain ginger crushed, adding 3 times of water with the crushed mass into the ginger crushed, crushing and pulping to obtain slurry, adding 0.05 time of lemon juice with the crushed mass into the slurry, soaking for 1h at 40 ℃, filtering, taking a filter cake, drying, dispersing the filter cake into 6 times of water with the crushed mass, adopting citric acid to adjust pH to 4.8, adding hemicellulase with the weight of 0.3% of ginger root and the enzyme activity of 50000U/g, carrying out enzymolysis for 1.5h at 50 ℃, carrying out high-temperature enzyme deactivation for 25min at 85 ℃, reducing to room temperature, adopting sodium hydroxide to adjust pH to 6.8, adding Serratin enzyme with the weight of 0.2% of ginger root and the enzyme activity of 30000U/g, adding pineapple proteinase with the weight of 1% of ginger root and the enzyme activity of 100000U/g, carrying out enzymolysis for 1.5h at 40 ℃, carrying out high-temperature enzyme deactivation for 25min at 85 ℃, carrying out ultrafiltration membrane filtration for 20kDa, collecting filtrate with the enzyme activity of less than 20kDa, concentrating, drying, and crushing to obtain the ginger root extract.
The preparation method of the locust bean extract in the embodiment comprises the following steps: pulverizing fresh locust bean, adding water with the mass of 6 times of the locust bean, regulating pH to 4.8 with hydrochloric acid, adding hemicellulase with the mass of 0.3% of the locust bean and the enzyme activity of 50000U/g, carrying out enzymolysis at 50 ℃ for 1.5h, inactivating enzyme at 85 ℃ for 25min, cooling to room temperature, continuing regulating pH to 1.5 with hydrochloric acid, adding pepsin with the mass of 1% of the locust bean and the enzyme activity of 10000U/g, carrying out enzymolysis at 35 ℃ for 1.5h, inactivating enzyme at 85 ℃ for 25min, cooling to room temperature, regulating pH to.5 with sodium hydroxide, adding subtilisin with the mass of 0.2% of the locust bean and the enzyme activity of 10000U/g, carrying out enzymolysis at 32 ℃ for 1h, inactivating enzyme at 85 ℃ for 25min, cooling to room temperature, filtering with a 20kDa ultrafiltration membrane, collecting filtrate with the viscosity of less than 20kDa, concentrating, drying, and pulverizing into nano powder to obtain the locust bean extract.
The preparation method of the anti-inflammatory antibacterial toothpaste containing bisabolol and ginger root components comprises the following steps:
s1: dispersing alpha-bisabolol, ginger root extract, locust bean extract and sweetener in an ethanol water solution to obtain a spray, spraying silicon dioxide and the spray in a fluidization way, spraying the ginger root extract and the locust bean extract on the surfaces of silicon dioxide particles, and freeze-drying by liquid nitrogen to obtain silicon dioxide loaded with the extract;
Wherein the ethanol aqueous solution contains 15% vol of ethanol; the dosage of the ethanol aqueous solution is 0.15 times of the mass of the silicon dioxide; the parameters of the fluidization spray are: the spray is heated to 25 ℃, the spraying speed is 0.2L/min, the atomization pressure is 0.5MPa, and the discharge temperature is 40 ℃;
S2: mixing macadamia nut oil, eucalyptus oil, merry fruit oil and clove oil according to parts by weight at 30 ℃ to obtain mixed oil;
S3: uniformly mixing the silicon dioxide loaded with the extract, the mixed oil and the humectant at 30 ℃ to obtain a phase A;
s4: uniformly mixing the purified water and the thickener at 80 ℃ to obtain a phase B, and cooling to 40 ℃ for standby;
S5: evenly mixing the phase A, the phase B, the flavoring agent and the surfactant to obtain the toothpaste.
Preparation of comparative example 1
The ginger root extract was replaced with Jiang Gengan powder, and the other methods and parameters were the same as in example 1.
Preparation of comparative example 2
The locust bean extract was replaced by dry powder of locust bean, and the other methods and parameters were the same as in example 1.
Preparation of comparative example 3
The procedure and parameters were as in example 1 without the addition of α -bisabolol and ginger root extract.
Preparation of comparative example 4
The procedure and parameters were as in example 1, except that the macadamia nut oil and the mayonnaise oil were not added.
Preparation of comparative example 5
Step S1 is omitted;
S2: mixing macadamia nut oil, eucalyptus oil, merry fruit oil and clove oil according to parts by weight at 30 ℃ to obtain mixed oil;
s3: uniformly mixing alpha-bisabolol, rhizoma Zingiberis recens extract, locust bean extract, sweetener, silicon dioxide, mixed oil and humectant at 30deg.C to obtain phase A;
s4: uniformly mixing the purified water and the thickener at 80 ℃ to obtain a phase B, and cooling to 40 ℃ for standby;
S5: evenly mixing the phase A, the phase B, the flavoring agent and the surfactant to obtain the toothpaste.
Plaque test, toxicity test, bacteriostasis test, and trial evaluation were performed on the toothpastes of examples 1 to 5 and the toothpastes of comparative examples 1 to 5 described above.
1. Patch test detection
Diluting each toothpaste with water to 5 times of the mass of the toothpaste to obtain each toothpaste diluent; selecting 20 subjects, placing 0.025g of each toothpaste diluent sample into a small chamber of a plaque tester by adopting a closed plaque test method, applying the sample into the arms of the subjects for testing, removing the plaque tester after 24 hours, and observing skin conditions within 48 hours, wherein no adverse reactions such as irritation, allergy, red swelling and the like exist, and toothpaste components belong to a safety level.
2. Toxicity test detection
Diluting each toothpaste with water to 5 times of the mass of the toothpaste to obtain each toothpaste diluent; 100 mice are selected, the average of the mice is divided into 10 groups (5 males and 5 females in each group), each group corresponds to one toothpaste, each toothpaste diluent is respectively subjected to an acute stomach-filling toxicity test of the mice, the stomach-filling toothpaste diluent is 0.02g/kg body weight, the reaction condition is observed, and the mice have no adverse reaction; the mice were fed daily at a weight of 0.02g/kg for 15 consecutive days, and the organs were examined for no abnormal phenomenon, resulting in safety.
3. Antibacterial test detection
Control groups (toothpaste without added Hawaii nut oil, eucalyptus oil, meinaria fruit oil, clove oil, alpha-bisabolol, ginger root extract and locust bean extract) were prepared. Porphyromonas gingivalis, proteus intermedia, fusarium, fusobacterium nucleatum, actinobacillus, streptococcus mutans and Lactobacillus are respectively inoculated into respective solid culture mediums, toothpaste particles with the diameter of 3mm are inoculated in the middle of each culture medium, 3 parallel samples are prepared for each sample, after culturing for 48 hours, the diameter of a bacteriostasis ring is measured, and the average value of the 3 parallel samples is taken, so that the results are shown in the following table 1:
TABLE 1 antibacterial test results (antibacterial circle diameter mm)
According to the antibacterial result, the ginger root is extracted through a special enzymolysis step, so that the ginger root peptide-containing extract has a good antibacterial effect, and the antibacterial property of the toothpaste to Porphyromonas gingivalis, fusarium and Fusobacterium nucleatum can be improved; after the locust bean is extracted by a special enzymolysis step, the obtained locust bean peptide extract has good antibacterial effect, and can improve the antibacterial property of the toothpaste on intermediate Proteus, fusobacterium nucleatum, actinobacillus and Streptococcus mutans; the alpha-bisabolol and ginger root extract are matched for use, so that the antibacterial property of the toothpaste to porphyromonas gingivalis can be greatly improved, and the antibacterial property of the toothpaste to other bacteria can be improved to a certain extent; the Hawaii stone oil and the Meinaria oil are matched for use, so that the antibacterial property of the toothpaste to Porphyromonas gingivalis, proteus intermedia and Fusobacterium nucleatum can be improved; the silicon dioxide loaded with the extract is not prepared, and the components are directly mixed, so that the antibacterial property of the toothpaste is not affected.
4. Trial evaluation
80 Subjects (age: 21 to 38 years; 40 men, 40 women; no denture and repair, etc.) were selected, with a Quigley-Hein plaque index of 1.5 or more and a Loe-Silness gingivitis index of 1.0 or more.
(1) Supragingival plaque was evaluated using a quegley-Hein modified Turesky plaque index; supragingival plaque was stained and recorded according to grade criteria: 0-sterile plaque; 1-plaque scattered at the edge of the dental neck; 2-the edge of the dental neck visible a continuous thin plaque band (up to lmm wide); 3-the cervical plaque band is greater than lmm, but less than 1/3 of the tooth face; 4-plaque covers 1/3-2/3 of the tooth surface; the 5-bacterial plaque covers more than 2/3 of the tooth surface.
Checking the buccal and lingual surfaces of the teeth, the maximum count being 10 for each tooth; the average of the plaque index for each subject was equal to the sum of the counts from all dental examinations of the individual (2 records per tooth) divided by the total number of measurements (number of teeth times 2).
(2) Gingivitis is measured using the modified Loe-Silness gingivitis index, and gingival condition is measured before stain measurement of plaque index; gingivitis counting method and grade criteria: 0-gingivitis free; 1-mild gingivitis with slight changes in gum color and texture, but no bleeding in the visit; 2-moderate inflammation, bright gums, redness, swelling, hyperplasia and bleeding detection; 3-severe inflammation, obvious redness, proliferation and spontaneous bleeding of gums.
Each dental examination recorded the buccal and lingual surfaces as well as the plaque index, with a maximum tooth count of 6. The mean of the gingivitis index for each subject Loe-Silness is equal to the sum of all dental values (2 faces per tooth) divided by the total number of measured faces (measured teeth by 2).
(3) After the baseline examination of plaque and gingivitis before the test is completed, all subjects are divided into 10 balance groups (4 men and 4 women in each group, no statistical difference among the groups) according to plaque and gingivitis conditions, and each group is used for brushing teeth after daily breakfast and supper respectively; meanwhile, the teeth are brushed after daily breakfast and supper without toothpaste is adopted as a blank example. Each brushing with a soft-haired toothbrush for 1min, after 6 months of continuous trial, plaque index and gingivitis index were examined as shown in table 2 below; mouthfeel evaluation, as shown in table 3 below:
TABLE 2 plaque index and gingivitis index (average of 8 people)
From the above results, the toothpastes of examples 1 to 5 are excellent in inhibiting and removing plaque, and gingivitis is well improved. The macadamia nut oil, the merry nut oil, the alpha-bisabolol, the ginger root extract and the locust bean extract all have certain effects of inhibiting bacteria and removing bacterial plaques and improving gingivitis, and the synergistic effect of the macadamia nut oil, the merry nut oil, the alpha-bisabolol, the ginger root extract and the locust bean extract is better, so that the use effect can be greatly improved. In addition, the viscosity of the spray is increased by using the sweetener, active ingredients such as alpha-bisabolol, ginger root extract, locust bean extract and the like are loaded on the silicon dioxide through spraying, and when brushing teeth, the silicon dioxide can be used as an abrasive, the active ingredients loaded on the surface of the silicon dioxide can be well adhered to the surface of teeth through the friction force between the silicon dioxide and the surface of dental plaque, fully contacts with the dental plaque, remains on the surface of the teeth for a long time, can well remove the dental plaque after long-term use, and greatly improves the speed and effect of removing the dental plaque.
Table 3 taste evaluation (8 people average)
The eucalyptus oil and the clove oil have certain pungent and pungent taste, and the direct administration of the eucalyptus oil and the clove oil can cause irritation to oral mucosa, thereby causing canker sore. In addition, the special spicy taste brought by the eucalyptus oil and the clove oil is not easy to be accepted by people, and the addition of the eucalyptus oil and the clove oil into the product can influence the overall taste of the product. The alpha-bisabolol has remarkable improvement effects on the aspects of neuropathic pain, chronic inflammatory pain, postoperative pain and the like, the anti-hyperalgesia effect of the alpha-bisabolol is related to the reduction of proliferation of active glial cells, and the alpha-bisabolol can regulate the release of pro-inflammatory and anti-inflammatory cytokines and improve the pungent stimulation reactivity of the oral cavity; the polymerization of alpha-bisabolol and plant extract has the function of absorbing and wrapping oil, so that the pungency stimulation is further reduced; in addition, the macadamia nut oil and the merry fruit oil also have the effect of improving the spicy taste and the pungent and irritation reactivity of the oral cavity. Therefore, after the alpha-bisabolol, the macadamia nut oil and the merry fruit oil are added, the taste of the toothpaste can be greatly improved, and the pungent irritation reactivity is well reduced.
Claims (8)
1. An anti-inflammatory antibacterial toothpaste containing bisabolol and ginger root components is characterized by being prepared from the following raw materials in parts by weight: 0.004 to 0.008 part of macadamia nut oil, 0.004 to 0.008 part of eucalyptus oil, 0.004 to 0.008 part of merry-go-round-robinia nut oil, 0.004 to 0.008 part of clove oil, 0.01 to 0.03 part of alpha-bisabolol, 0.005 to 0.008 part of ginger root extract, 0.005 to 0.01 part of locust bean extract, 25 to 35 parts of silicon dioxide, 20 to 25 parts of humectant, 0.5 to 1 part of thickener, 1.8 to 2.5 parts of surfactant, 1 to 2.5 parts of flavoring agent, 1 to 2.5 parts of sweetener and 12 to 20 parts of purified water;
the preparation method of the ginger root extract comprises the following steps: taking fresh ginger root, crushing to obtain ginger crushed, adding 3-5 times of water with the crushed mass of the ginger into the ginger crushed, crushing and pulping to obtain slurry, adding 0.05-0.1 time of lemon juice with the crushed mass of the slurry into the slurry, soaking for 1-1.5 hours at the temperature of 40-45 ℃, filtering, taking a filter cake, drying, dispersing the filter cake into 6-8 times of water with the filter cake mass, regulating the pH value to 4.8-5.2 by adopting citric acid, adding hemicellulase, carrying out enzymolysis for 1.5-2 hours at the temperature of 50-60 ℃, carrying out high-temperature enzyme deactivation, reducing the temperature to room temperature, regulating the pH value to 6.8-7.2 by adopting sodium hydroxide, adding Serratinase and bromelain, carrying out enzymolysis for 1.5-2 hours at the temperature of 40-45 ℃, carrying out high-temperature enzyme deactivation, reducing the temperature to room temperature, filtering by adopting a 20kDa ultrafiltration membrane, collecting filtrate smaller than 20kDa, concentrating, drying, and crushing into nano-powder to obtain ginger root extract;
The preparation method of the locust bean extract comprises the following steps: crushing fresh locust beans, adding water with the mass of 6-8 times of that of the locust beans, regulating the pH value to 4.8-5.2 by adopting hydrochloric acid, adding hemicellulase, carrying out enzymolysis for 1.5-2 hours at 50-60 ℃, inactivating enzyme at high temperature, cooling to room temperature, continuously regulating the pH value to 1.5-2.0 by adopting hydrochloric acid, adding pepsin, carrying out enzymolysis for 1.5-2 hours at 35-38 ℃, inactivating enzyme at high temperature, cooling to room temperature, regulating the pH value to 7.5-7.8 by adopting sodium hydroxide, adding subtilisin, carrying out enzymolysis for 1-1.5 hours at 32-38 ℃, carrying out high temperature inactivating enzyme, cooling to room temperature, filtering by adopting a 20kDa ultrafiltration membrane, collecting filtrate smaller than 20kDa, concentrating, drying, and crushing into nano-powder to obtain the locust bean extract.
2. The anti-inflammatory and antibacterial toothpaste containing bisabolol and ginger root ingredients according to claim 1, wherein in the preparation method of the ginger root extract, the addition amount of hemicellulase is 0.3% -0.8% of the weight of the ginger root, and the enzyme activity of the hemicellulase is 50000U/g-100000U/g; the adding amount of the Serratia peptidase is 0.2-0.5% of the mass of ginger root, and the enzyme activity of the Serratia peptidase is 30000U/g-50000U/g; the addition amount of the bromelain is 1-3% of the mass of ginger root, and the enzyme activity of the bromelain is 100000U/g-200000U/g; the high-temperature enzyme deactivation temperature is 85-100 ℃ and the time is 25-35 min.
3. The anti-inflammatory and antibacterial toothpaste containing bisabolol and ginger root ingredients according to claim 1, wherein in the preparation method of the locust bean extract, the addition amount of the hemicellulase is 0.3% -0.8% of the mass of the locust beans, and the enzyme activity of the hemicellulase is 50000U/g-100000U/g; the addition amount of the pepsin is 1-2.5% of the mass of the locust bean, and the enzyme activity of the pepsin is 10000U/g-12000U/g; the addition amount of the subtilisin is 0.2-0.5% of the mass of the locust bean, and the enzyme activity of the subtilisin is 10000U/g-20000U/g; the high-temperature enzyme deactivation temperature is 85-100 ℃ and the time is 25-35 min.
4. The anti-inflammatory and antibacterial toothpaste containing bisabolol and ginger root ingredients according to claim 1, wherein the median particle size of the silicon dioxide is 8-20 μm, the oil absorption value of the silicon dioxide is 100-105 g/100g, the water absorption amount is 15-20 mL/20g, and the transparency of the silicon dioxide in the range of 1.440-1.460 is more than or equal to 92%.
5. The anti-inflammatory and antibacterial toothpaste containing bisabolol and ginger root components according to claim 1, wherein the humectant comprises sorbitol and propylene glycol in a mass ratio of (1-1.5) and comprises sorbitol and propylene glycol= (2-2.5); the thickener comprises sodium carboxymethyl cellulose, xanthan gum and guar gum in a mass ratio of sodium carboxymethyl cellulose to xanthan gum to guar gum= (1-1.5): (0.5-1): (1-1.5); the surfactant is sodium dodecyl sulfate; the flavoring agent is essence; the sweetener is sucrose, maltose or fructose.
6. The method for preparing the anti-inflammatory and antibacterial toothpaste containing bisabolol and ginger root ingredients as claimed in claim 1, which is characterized by comprising the following steps:
s1: dispersing alpha-bisabolol, ginger root extract, locust bean extract and sweetener in an ethanol water solution to obtain a spray, spraying silicon dioxide and the spray in a fluidization way, spraying the ginger root extract and the locust bean extract on the surfaces of silicon dioxide particles, and freeze-drying to obtain silicon dioxide loaded with the extracts;
S2: mixing macadamia nut oil, eucalyptus oil, merry-go-round oil and clove oil according to parts by weight to obtain mixed oil;
s3: evenly mixing the silicon dioxide loaded with the extract, the mixed oil and the humectant to obtain phase A;
S4: uniformly mixing the purified water and the thickener at 80-85 ℃ to obtain phase B, and reducing the temperature to 40-45 ℃ for standby;
S5: evenly mixing the phase A, the phase B, the flavoring agent and the surfactant to obtain the toothpaste.
7. The method for preparing the anti-inflammatory and antibacterial toothpaste containing bisabolol and ginger root ingredients according to claim 6, wherein in the step S1, the ethanol aqueous solution contains 15-25% vol of ethanol; the dosage of the ethanol aqueous solution is 0.15 to 0.25 times of the mass of the silicon dioxide; the parameters of the fluidization spray are as follows: the spray is fed at 25-30 ℃, the spraying speed is 0.2-0.3L/min, the atomization pressure is 0.5-0.7 MPa, and the discharge temperature is 40-45 ℃; the lyophilization is liquid nitrogen lyophilization.
8. The method for preparing the anti-inflammatory and antibacterial toothpaste containing bisabolol and ginger root ingredients according to claim 6, wherein in the step S2, the mixing temperature of the mixed oil is 30-40 ℃; in S3, the uniform mixing temperature of the phase A is 30-40 ℃.
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