Anti-inflammatory toothpaste based on dendrobium huoshanense stem extract and preparation method thereof

Abstract

The application discloses anti-inflammatory toothpaste based on Dendrobium huoshanense stem extract and a preparation method thereof, and relates to the technical field of toothpaste.The anti-inflammatory toothpaste contains the following raw materials in parts by weight: friction agent 20-30 parts, humectant 15-30 parts, emulsifier 1-2 parts, thickening agent 1-2.5 parts, Dendrobium huoshanense stem extract 1-3 parts, Abelmoschus flower extract 0.5-1.5 parts, Perilla leaf extract 0.5-1.5 parts, anti-allergic agent 3.5-7.5 parts, auxiliary material 1-3.5 parts, and deionized water 20-40 parts.The specific plant extract and the Dendrobium huoshanense stem extract are synergistically used, and the basic formula system is optimized, so that the comprehensive anti-inflammatory effect of the product is effectively improved, and the stability and mildness of the toothpaste are improved.

Description

Technical Field

[0001] This invention relates to the field of toothpaste technology, and in particular to an anti-inflammatory toothpaste based on Dendrobium huoshanense stem extract and its preparation method. Background Technology

[0002] With increasing awareness of oral health, the functional demands for toothpaste are becoming more diverse and sophisticated. Beyond basic cleaning, relieving gum discomfort, reducing inflammation, and alleviating sensitivity have become important requirements. Plant extracts, due to their natural and safe properties, are increasingly widely used in oral care products. Dendrobium huoshanense, a traditional and precious Chinese medicinal herb, is rich in polysaccharides, alkaloids, and other active ingredients, possessing the effects of nourishing yin and clearing heat, benefiting the stomach and promoting the production of body fluids. Modern pharmacological studies have shown that it has antioxidant, anti-inflammatory, and immunomodulatory effects.

[0003] Currently, there are functional toothpastes on the market that contain single plant extracts, but they often suffer from limited efficacy and effectiveness. Directly adding Dendrobium officinale extract to toothpaste presents challenges in terms of the stability, bioavailability, and compatibility with the toothpaste matrix. Furthermore, while sodium lauryl sulfate, a foaming agent in traditional toothpaste formulations, has strong cleaning power, it may pose a potential irritant to some sensitive oral mucosa. Therefore, how to improve the anti-inflammatory properties of toothpaste while optimizing its stability and user comfort is a pressing technical problem that needs to be solved. Summary of the Invention

[0004] Based on the technical problems existing in the background technology, the present invention proposes an anti-inflammatory toothpaste based on Dendrobium huoshanense stem extract and its preparation method. By introducing specific plant extracts to synergistically work with Dendrobium huoshanense stem extract and optimizing the basic formula system, the comprehensive anti-inflammatory efficacy of the product is effectively improved, while the stability and mildness of the paste are also improved.

[0005] This invention proposes an anti-inflammatory toothpaste based on Dendrobium huoshanense stem extract, comprising the following raw materials in parts by weight: 20-30 parts abrasive, 15-30 parts humectant, 1-2 parts emulsifier, 1-2.5 parts thickener, 1-3 parts Dendrobium huoshanense stem extract, 0.5-1.5 parts Hibiscus syriacus flower extract, 0.5-1.5 parts Perilla frutescens leaf extract, 3.5-7.5 parts anti-sensitivity agent, 1-3.5 parts excipients, and 20-40 parts deionized water.

[0006] Preferably, the friction agent is one or more of silicon dioxide, calcium carbonate, and calcium hydrogen phosphate.

[0007] Preferably, the moisturizer is sorbitol and / or polyethylene glycol.

[0008] Preferably, the emulsifier is composed of 0.8-1.2 parts by weight of sodium lauryl sulfate, 0.3-0.5 parts by weight of polyglycerol-10 lauryl ester and 0.1-0.3 parts by weight of hydrogenated lecithin.

[0009] Preferably, the anti-allergen is one or more of strontium salts, potassium salts, phytic acid and its salts, tranexamic acid and arginine.

[0010] Preferably, the excipients are one or more of antioxidants, pH adjusters, preservatives, flavoring agents, and coloring agents.

[0011] Preferably, the thickener is composed of 0.5-1 parts by weight of cellulose gum, 0.3-0.5 parts by weight of xanthan gum, and 0.4-0.6 parts by weight of modified chitosan.

[0012] Preferably, the preparation method of the Dendrobium huoshanense stem extract is as follows: The stems of Dendrobium huoshanense were cleaned, dried, and crushed. The pulverized material is enzymatically hydrolyzed in water using a first complex enzyme. An extraction medium is added to the enzymatically hydrolyzed liquid for auxiliary extraction. After extraction, solid-liquid separation and ultrafiltration fractionation are performed to obtain Dendrobium huoshanense stem extract.

[0013] Preferably, the first compound enzyme is composed of cellulase and pectinase in a mass ratio of 1-3:1, and the amount of the first compound enzyme added is 0.1-1% of the mass of the pulverized material. Preferably, the enzymatic hydrolysis conditions are: pH 4.8-5.5, temperature 45-52℃, time 1-3h, and material-to-liquid ratio 1:10-20.

[0014] Preferably, the extraction medium consists of glycerol and 1,3-propanediol in a mass ratio of 1:0.5-1.5, and the amount of extraction medium added accounts for 15-25% of the mass of water added during enzymatic hydrolysis. The temperature for auxiliary extraction is 50-65℃, and the time is 1-2 hours.

[0015] Preferably, ultrafiltration fractionation retains components with a molecular weight of 10-30 kDa.

[0016] Preferably, the preparation method of the okra flower extract is as follows: the pulverized okra flowers and the second complex enzyme are added to ethanol for ultrasonic extraction. After extraction, the extract is filtered, concentrated under reduced pressure and dried to obtain the okra flower extract.

[0017] Preferably, the second complex enzyme is composed of cellulase and pectinase in a mass ratio of 2:1-4, and the amount added is 1-5% of the total mass of the okra flowers; Preferably, the conditions for ultrasonic extraction are: temperature 40-60℃, time 30-60min, ultrasonic power 300-500W, and system pH 5.5-6.5.

[0018] Preferably, the preparation method of the perilla leaf extract is as follows: dried perilla leaves are pulverized and placed into an extraction vessel. A mixture of supercritical CO2 and ethanol aqueous solution is used as the extraction medium for static extraction and dynamic extraction in sequence. After extraction, the co-solvent is removed by depressurization to obtain the perilla leaf extract.

[0019] Preferably, the static extraction conditions are: temperature 50-60℃, time 10-20 min, and pressure 25-35 MPa.

[0020] Preferably, the conditions for dynamic extraction are: temperature 50-60℃, time 100-130min, pressure 25-35MPa, CO2 flow rate 0.4-0.6g / min, and the ethanol-water solution in the fluid accounts for 10-15% of the total mass of the supercritical CO2 and ethanol-water solution mixture.

[0021] Preferably, the modified chitosan is prepared as follows: lauric acid, 1-ethyl-3-(3-dimethylaminopropyl)-carbodiimide and N-hydroxysuccinimide are mixed and activated, then added to an aqueous solution of carboxymethyl chitosan for reaction. After the reaction, the mixture is purified and dried to obtain the modified chitosan.

[0022] Preferably, the molar ratio of carboxymethyl chitosan, lauric acid, 1-ethyl-3-(3-dimethylaminopropyl)-carbodiimide and N-hydroxysuccinimide is 100:1-3:2-4:2-4.

[0023] Preferably, the reaction conditions are: temperature 40-50℃, time 4-8h, and pH of the reaction system 5-5.5.

[0024] This invention proposes a method for preparing an anti-inflammatory toothpaste based on Dendrobium huoshanense stem extract. The anti-inflammatory toothpaste is as described above, and the method steps are as follows: S1: Mix the humectant and thickener in deionized water to obtain the first mixture; S2: Mix Dendrobium officinale stem extract, Hibiscus syriacus flower extract, Perilla frutescens leaf extract and anti-allergy agent in deionized water to obtain a second mixture; S3: Mix the first mixture with the second mixture, then add abrasive, emulsifier and excipients, and homogenize to obtain an anti-inflammatory toothpaste based on Dendrobium officinale stem extract.

[0025] Beneficial technical effects of the present invention: (1) The present invention has a synergistic promoting effect on improving the anti-inflammatory properties of toothpaste by a specific combination of Dendrobium officinale stem extract, Hibiscus syriacus flower extract and Perilla frutescens leaf extract.

[0026] Specifically, the local soothing environment provided by the Dendrobium huoshanense stem extract is conducive to the further stabilizing and anti-inflammatory effects of the Hibiscus syriacus flower extract on the stimulated interface; the reduction of inflammation transmission by the Hibiscus syriacus flower extract, in turn, allows the Perilla frutescens leaf extract to more effectively inhibit the amplified inflammatory response; and the inhibition of the amplified inflammatory process by the Perilla frutescens leaf extract can conversely reduce the damage to the aforementioned anti-inflammatory environment and stabilizing interface, thereby prolonging the effects of the Dendrobium huoshanense stem extract and the Hibiscus syriacus flower extract. Thus, a synergistic mechanism is formed among the three, mutually creating conditions for action and mutually extending the effective window of action, resulting in the superior anti-inflammatory properties of the toothpaste of this invention.

[0027] (2) The present invention uses sodium lauryl sulfate, polyglycerol-10 lauryl ester and hydrogenated lecithin to construct a compound emulsification / dispersion system. While ensuring the cleaning and dispersing ability, it reduces the dependence on a single strong surfactant, thereby significantly improving the stability of the formulation and improving the mildness of the system.

[0028] Traditional toothpaste systems, which primarily rely on anionic surfactants such as sodium lauryl sulfate for cleaning, foaming, and dispersion, often require relatively high dosages to balance dispersibility and system stability. However, high dosages of a single anionic surfactant can irritate the sensitive oral environment and are detrimental to the stable presence of plant-based active ingredients. This invention, by compounding sodium lauryl sulfate with polyglycerol-10 lauryl ester and hydrogenated lecithin, forms a more rational interface control system. Through the synergistic effect of these three components, this invention not only significantly reduces the dosage of sodium lauryl sulfate while maintaining the basic performance of the toothpaste, thus mitigating the irritation risk associated with excessive use of a single anionic surfactant, but also significantly improves the uniformity of the toothpaste's dispersion and storage stability, reducing the probability of problems such as layering, separation, coarsening, localized agglomeration, and migration of active ingredients.

[0029] (3) The present invention uses a specific modified chitosan, which not only improves the stability of the paste, but also further enhances the anti-inflammatory properties of the system, demonstrating the "dual synergistic" effect of modified chitosan in the present invention.

[0030] Through comparative experiments, the inventors further discovered that when lauric acid-modified chitosan was added to the toothpaste system of this invention, the resulting toothpaste exhibited superior stability and anti-inflammatory properties compared to the control scheme using unmodified carboxymethyl chitosan. This indicates that the modified chitosan used in this invention does not simply serve a conventional thickening function, but rather makes substantial contributions to both system stability and functional performance.

[0031] The reason is that, although unmodified carboxymethyl chitosan has a certain degree of hydrophilicity and biocompatibility, its interaction with the relatively hydrophobic active ingredients and compound surfactant systems in the system is relatively limited. In contrast, the modified chitosan used in this invention, by introducing lauroyl groups, possesses both hydrophilic and hydrophobic segments, giving it stronger amphiphilicity. On one hand, this modified chitosan more easily forms stable interactions with plant-based active ingredients, surfactant components, and abrasive particles in the ointment, improving the spatial network structure strength of the system and thus enhancing the ointment's suspension dispersion ability and storage stability. On the other hand, this modified chitosan can also more effectively adsorb or load some active ingredients and form a more stable adhesion layer or protective layer on the oral cavity surface, prolonging the residence time of active ingredients at the site of local inflammation, improving the local utilization efficiency of active ingredients, and thus further amplifying the anti-inflammatory effect.

[0032] (4) Through the synergistic design of three plant extracts, compound emulsification / dispersion system and modified chitosan, the present invention enables toothpaste to have good anti-inflammatory properties, high formulation stability and superior gentleness.

[0033] The technical solution of this invention addresses the problems of insufficient anti-inflammatory effect, high irritation from traditional surfactants, and poor stability of plant active ingredients in toothpaste under sensitive oral environments. Three plant extracts constitute a multi-stage synergistic anti-inflammatory system. The compound emulsification / dispersion system improves the uniform distribution of active ingredients in the toothpaste and reduces dependence on high amounts of sodium lauryl sulfate. Modified chitosan further enhances system stability and strengthens local anti-inflammatory effects. These technical features are not isolated but mutually supportive and amplifying: a more stable dispersion system allows the three plant extracts to fully exert their synergistic anti-inflammatory effects; the modified chitosan's adhesion and retention of active ingredients further enhances the functionality of the plant extracts and anti-sensitivity components; and the milder surfactant system helps reduce secondary irritation to sensitive oral environments, making the anti-inflammatory effect more readily apparent. Therefore, the toothpaste obtained by this invention achieves a good balance and unity in terms of anti-inflammation, stability, and mildness. Detailed Implementation

[0034] The present invention will be further explained below with reference to specific embodiments.

[0035] The manufacturers involved are as follows: Example 1 Mix 200g sorbitol, 30g polyethylene glycol-8, 8g cellulose gum, 4g xanthan gum, and 5g modified chitosan in 100g deionized water to obtain the first mixture; mix 20g Dendrobium officinale stem extract, 10g Hibiscus syriacus flower extract, 10g Perilla frutescens leaf extract, 40g strontium chloride hexahydrate, 8g sodium phytate, and 5g tranexamic acid in 200g deionized water to obtain the second mixture; mix the first and second mixtures, and then add 250g hydrated silica, 10g sodium lauryl sulfate, and 4g polyglycerol. -10 laurate, 2g hydrogenated lecithin, 1g tocopheryl acetate, 5g sodium citrate, 2g sodium benzoate, 1.5g sodium saccharin, 8g flavoring, 3g menthol, and 3g polysorbate 20 were mixed. The pH of the mixture was adjusted to 7.5 using a sodium citrate / citric acid buffer system. Then, the mixture was homogenized at 2500 r / min for 15 min under a vacuum of -0.09 MPa at 30°C. After homogenization, the mixture was degassed under vacuum for 10 min to obtain an anti-inflammatory toothpaste based on Dendrobium huoshanense stem extract.

[0036] The preparation method of Dendrobium huoshanense stem extract is as follows: Dendrobium huoshanense stems are washed, dried and pulverized; the pulverized material is enzymatically hydrolyzed in water by a first compound enzyme; an extraction medium is added to the hydrolyzed liquid for auxiliary extraction; after extraction, solid-liquid separation and ultrafiltration are performed to obtain Dendrobium huoshanense stem extract.

[0037] The first complex enzyme consists of cellulase and pectinase in a 2:1 mass ratio, and the amount of the first complex enzyme added is 0.5% of the mass of the pulverized material. The enzymatic hydrolysis conditions are: pH 5, temperature 48℃, time 2h, and material-to-liquid ratio 1:15. The extraction medium consists of glycerol and 1,3-propanediol in a 1:1 mass ratio, and the amount of extraction medium added accounts for 20% of the mass of water added during enzymatic hydrolysis. The auxiliary extraction temperature is 58℃, and the time is 1.5h. Ultrafiltration fractionation retains components with a molecular weight of 10-30kDa.

[0038] The preparation method of okra flower extract is as follows: pulverized okra flowers and a second complex enzyme are added to ethanol for ultrasonic extraction. After extraction, the extract is filtered, concentrated under reduced pressure, and dried to obtain okra flower extract.

[0039] The second complex enzyme consists of cellulase and pectinase in a 1:1 mass ratio, and the amount added is 3% of the total mass of the okra flower. The ultrasonic extraction conditions are: temperature 50℃, time 45min, ultrasonic power 400W, and system pH 6.

[0040] The preparation method of perilla leaf extract is as follows: dried perilla leaves are pulverized and placed into an extraction vessel. A mixture of supercritical CO2 and ethanol aqueous solution is used as the extraction medium for static extraction and dynamic extraction. After extraction, the co-solvent is removed by vacuum separation to obtain perilla leaf extract.

[0041] The static extraction conditions were: temperature 55℃, time 15 min, and pressure 30 MPa; the dynamic extraction conditions were: temperature 55℃, time 115 min, pressure 30 MPa, CO2 flow rate 0.5 g / min, and the ethanol-water solution in the fluid accounted for 12% of the total mass of the supercritical CO2 and ethanol-water solution mixture.

[0042] The modified chitosan is prepared as follows: Lauric acid, 1-ethyl-3-(3-dimethylaminopropyl)-carbodiimide and N-hydroxysuccinimide are mixed and activated, and then added to an aqueous solution of carboxymethyl chitosan for reaction. After the reaction, the mixture is purified and dried to obtain modified chitosan.

[0043] The molar ratio of carboxymethyl chitosan, lauric acid, 1-ethyl-3-(3-dimethylaminopropyl)-carbodiimide and N-hydroxysuccinimide was 100:2:3:3; the reaction conditions were: temperature 50℃, time 6h, and pH of the reaction system 5.2.

[0044] The specific method for purifying modified chitosan is as follows: After the reaction is complete, the reaction solution is cooled to room temperature. The pH of the reaction system is adjusted to 7.0 using sodium hydroxide solution. After standing for 30 minutes, the mixture is centrifuged at 8000 r / min for 10 minutes, and the supernatant is collected. Four times the volume of anhydrous ethanol is slowly added to the supernatant while stirring to precipitate the modified chitosan. After the addition is complete, the mixture is allowed to stand at 4℃ for 8 hours, and then centrifuged at 8000 r / min for 10 minutes to collect the precipitate. The precipitate is redispersed in deionized water, and four times the volume of anhydrous ethanol is added again for alcohol precipitation. The precipitate was subjected to three alcohol precipitation cycles. Subsequently, the precipitate was washed sequentially with 75% ethanol, 95% ethanol, and anhydrous ethanol, twice with each type of ethanol. After each washing, the precipitate was collected by centrifugation. The washed precipitate was redispersed in deionized water and placed in a dialysis bag with a molecular weight cutoff of 3500 Da. Dialysis was performed with deionized water as the dialysis medium for 72 hours. The dialysis water was changed every 6 hours for the first 24 hours of dialysis, and then every 12 hours thereafter. After dialysis, the liquid in the dialysis bag was collected, pre-frozen at -40°C for 8 hours, and then freeze-dried under vacuum for 36 hours to obtain purified modified chitosan.

[0045] Example 2 150g of sorbitol, 20g of polyethylene glycol-8, 5g of cellulose gum, 3g of xanthan gum, and 4g of modified chitosan were mixed in 50g of deionized water to obtain a first mixture. 10g of Dendrobium huoshanense stem extract, 5g of Hibiscus syriacus flower extract, 5g of Perilla frutescens leaf extract, 30g of strontium chloride hexahydrate, 5g of sodium phytate, and 3g of tranexamic acid were mixed in 150g of deionized water to obtain a second mixture. The first and second mixtures were then mixed, and then 200g of hydrated silica, 8g of sodium lauryl sulfate, 3g of polyglycerol-10 lauryl ester, 1g of hydrogenated lecithin, 0.5g of tocopheryl acetate, 3g of sodium citrate, 1g of sodium benzoate, 1g of sodium saccharin, 5g of flavoring, 2g of menthol, and 2g of polysorbate 20 were added for homogenization. The homogenization and pH adjustment conditions were the same as in Example 1 to obtain an anti-inflammatory toothpaste based on Dendrobium huoshanense stem extract.

[0046] The preparation method of Dendrobium huoshanense stem extract is as follows: Dendrobium huoshanense stems are washed, dried and pulverized; the pulverized material is enzymatically hydrolyzed in water by a first compound enzyme; an extraction medium is added to the hydrolyzed liquid for auxiliary extraction; after extraction, solid-liquid separation and ultrafiltration are performed to obtain Dendrobium huoshanense stem extract.

[0047] The first complex enzyme consists of cellulase and pectinase in a 1:1 mass ratio, and the amount of the first complex enzyme added is 0.1% of the mass of the pulverized material. The enzymatic hydrolysis conditions are: pH 4.8, temperature 45℃, time 1h, and material-to-liquid ratio 1:10. The extraction medium consists of glycerol and 1,3-propanediol in a 2:1 mass ratio, and the amount of extraction medium added accounts for 15% of the mass of water added during enzymatic hydrolysis. The auxiliary extraction temperature is 50℃, and the time is 1h. Ultrafiltration fractionation retains components with a molecular weight of 10-30kDa.

[0048] The preparation method of okra flower extract is as follows: pulverized okra flowers and a second complex enzyme are added to ethanol for ultrasonic extraction. After extraction, the extract is filtered, concentrated under reduced pressure, and dried to obtain okra flower extract.

[0049] The second complex enzyme consists of cellulase and pectinase in a 2:1 mass ratio, and the amount added is 1% of the total mass of okra flowers; the ultrasonic extraction conditions are: temperature 40℃, time 30min, ultrasonic power 300W, and system pH 5.5.

[0050] The preparation method of perilla leaf extract is as follows: dried perilla leaves are pulverized and placed into an extraction vessel. A mixture of supercritical CO2 and ethanol aqueous solution is used as the extraction medium for static extraction and dynamic extraction. After extraction, the co-solvent is removed by vacuum separation to obtain perilla leaf extract.

[0051] The static extraction conditions were: temperature 50℃, time 10 min, and pressure 25 MPa; the dynamic extraction conditions were: temperature 50℃, time 100 min, pressure 25 MPa, CO2 flow rate 0.4 g / min, and the ethanol-water solution in the fluid accounted for 10% of the total mass of the supercritical CO2 and ethanol-water solution mixture.

[0052] The modified chitosan is prepared as follows: Lauric acid, 1-ethyl-3-(3-dimethylaminopropyl)-carbodiimide and N-hydroxysuccinimide are mixed and activated, and then added to an aqueous solution of carboxymethyl chitosan for reaction. After the reaction, the mixture is purified and dried to obtain modified chitosan.

[0053] The molar ratio of carboxymethyl chitosan, lauric acid, 1-ethyl-3-(3-dimethylaminopropyl)-carbodiimide and N-hydroxysuccinimide was 100:1:2:2; the reaction conditions were: temperature 50℃, time 4h, and pH of the reaction system 5.

[0054] The specific method for purifying modified chitosan is as described in Example 1.

[0055] Example 3 Mix 250g sorbitol, 40g polyethylene glycol-8, 10g cellulose gum, 5g xanthan gum, and 6g modified chitosan in 150g deionized water to obtain a first mixture; mix 30g Dendrobium officinale stem extract, 15g Hibiscus syriacus flower extract, 15g Perilla frutescens leaf extract, 50g strontium chloride hexahydrate, 10g sodium phytate, and 7g tranexamic acid in 250g deionized water to obtain a second mixture; combine the first mixture with the second mixture... The mixture was then combined with 300g of hydrated silica, 12g of sodium lauryl sulfate, 5g of polyglycerol-10 lauryl ester, 3g of hydrogenated lecithin, 1.5g of tocopheryl acetate, 7g of sodium citrate, 3g of sodium benzoate, 2g of sodium saccharin, 10g of food flavoring, 4g of menthol, and 4g of polysorbate 20. The mixture was homogenized, and the homogenization and pH adjustment conditions were the same as in Example 1, resulting in an anti-inflammatory toothpaste based on Dendrobium officinale stem extract.

[0056] The preparation method of Dendrobium huoshanense stem extract is as follows: Dendrobium huoshanense stems are washed, dried and pulverized; the pulverized material is enzymatically hydrolyzed in water by a first compound enzyme; an extraction medium is added to the hydrolyzed liquid for auxiliary extraction; after extraction, solid-liquid separation and ultrafiltration are performed to obtain Dendrobium huoshanense stem extract.

[0057] The first complex enzyme consists of cellulase and pectinase in a 3:1 mass ratio, and the amount of the first complex enzyme added is 1% of the mass of the pulverized material. The enzymatic hydrolysis conditions are: pH 5.5, temperature 52℃, time 3h, and material-to-liquid ratio 1:20. The extraction medium consists of glycerol and 1,3-propanediol in a 2:3 mass ratio, and the amount of extraction medium added accounts for 25% of the mass of water added during enzymatic hydrolysis. The auxiliary extraction temperature is 65℃ and the time is 2h. Ultrafiltration fractionation retains components with a molecular weight of 10-30kDa.

[0058] The preparation method of okra flower extract is as follows: pulverized okra flowers and a second complex enzyme are added to ethanol for ultrasonic extraction. After extraction, the extract is filtered, concentrated under reduced pressure, and dried to obtain okra flower extract.

[0059] The second complex enzyme consists of cellulase and pectinase in a 1:2 mass ratio, and the amount added is 5% of the total mass of okra flowers; the ultrasonic extraction conditions are: temperature 60℃, time 60min, ultrasonic power 500W, and system pH 6.5.

[0060] The preparation method of perilla leaf extract is as follows: dried perilla leaves are pulverized and placed into an extraction vessel. A mixture of supercritical CO2 and ethanol aqueous solution is used as the extraction medium for static extraction and dynamic extraction. After extraction, the co-solvent is removed by vacuum separation to obtain perilla leaf extract.

[0061] The static extraction conditions were: temperature 60℃, time 20 min, and pressure 35 MPa; the dynamic extraction conditions were: temperature 60℃, time 130 min, pressure 35 MPa, CO2 flow rate 0.6 g / min, and the ethanol-water solution in the fluid accounted for 15% of the total mass of the supercritical CO2 and ethanol-water solution mixture.

[0062] The modified chitosan is prepared as follows: Lauric acid, 1-ethyl-3-(3-dimethylaminopropyl)-carbodiimide and N-hydroxysuccinimide are mixed and activated, and then added to an aqueous solution of carboxymethyl chitosan for reaction. After the reaction, the mixture is purified and dried to obtain modified chitosan.

[0063] The molar ratio of carboxymethyl chitosan, lauric acid, 1-ethyl-3-(3-dimethylaminopropyl)-carbodiimide and N-hydroxysuccinimide was 100:3:4:4; the reaction conditions were: temperature 50℃, time 8h, and pH of the reaction system 5.5.

[0064] The specific method for purifying modified chitosan is as described in Example 1.

[0065] Comparative Example 1 200g sorbitol, 30g polyethylene glycol-8, 8g cellulose gum, 4g xanthan gum, and 5g modified chitosan were mixed in 100g deionized water to obtain a first mixture. 25g Dendrobium huoshanense stem extract, 15g Hibiscus syriacus flower extract, 40g strontium chloride hexahydrate, 8g sodium phytate, and 5g tranexamic acid were mixed in 200g deionized water to obtain a second mixture. The first and second mixtures were then mixed, and then 250g hydrated silica, 10g sodium lauryl sulfate, 4g polyglycerol-10 laurate, 2g hydrogenated lecithin, 1g tocopheryl acetate, 5g sodium citrate, 2g sodium benzoate, 1.5g sodium saccharin, 8g flavoring, 3g menthol, and 3g polysorbate 20 were added for homogenization. The homogenization and pH adjustment conditions were the same as in Example 1, resulting in an anti-inflammatory toothpaste based on Dendrobium huoshanense stem extract.

[0066] All other conditions are the same as in Example 1.

[0067] Comparative Example 2 200g sorbitol, 30g polyethylene glycol-8, 8g cellulose gum, 4g xanthan gum, and 5g modified chitosan were mixed in 100g deionized water to obtain a first mixture. 25g Dendrobium huoshanense stem extract, 15g Perilla frutescens leaf extract, 40g strontium chloride hexahydrate, 8g sodium phytate, and 5g tranexamic acid were mixed in 200g deionized water to obtain a second mixture. The first and second mixtures were then mixed, and then 250g hydrated silica, 10g sodium lauryl sulfate, 4g polyglycerol-10 laurate, 2g hydrogenated lecithin, 1g tocopheryl acetate, 5g sodium citrate, 2g sodium benzoate, 1.5g sodium saccharin, 8g flavoring, 3g menthol, and 3g polysorbate 20 were added for homogenization. The homogenization and pH adjustment conditions were the same as in Example 1, resulting in an anti-inflammatory toothpaste based on Dendrobium huoshanense stem extract.

[0068] All other conditions are the same as in Example 1.

[0069] Comparative Example 3 200g sorbitol, 30g polyethylene glycol-8, 8g cellulose gum, 4g xanthan gum, and 5g modified chitosan were mixed in 100g deionized water to obtain a first mixture. 20g Hibiscus syriacus flower extract, 20g Perilla frutescens leaf extract, 40g strontium chloride hexahydrate, 8g sodium phytate, and 5g tranexamic acid were mixed in 200g deionized water to obtain a second mixture. The first and second mixtures were then mixed, and then 250g hydrated silica, 10g sodium lauryl sulfate, 4g polyglycerol-10 laurate, 2g hydrogenated lecithin, 1g tocopheryl acetate, 5g sodium citrate, 2g sodium benzoate, 1.5g sodium saccharin, 8g flavoring, 3g menthol, and 3g polysorbate 20 were added for homogenization. The homogenization and pH adjustment conditions were the same as in Example 1, resulting in an anti-inflammatory toothpaste based on Dendrobium huoshanense stem extract.

[0070] All other conditions are the same as in Example 1.

[0071] Comparative Example 4 200g sorbitol, 30g polyethylene glycol-8, 8g cellulose gum, 4g xanthan gum, and 5g carboxymethyl chitosan were mixed in 100g deionized water to obtain a first mixture. 20g Dendrobium huoshanense stem extract, 10g Hibiscus syriacus flower extract, 10g Perilla frutescens leaf extract, 40g strontium chloride hexahydrate, 8g sodium phytate, and 5g tranexamic acid were mixed in 200g deionized water to obtain a second mixture. The first and second mixtures were then mixed, and then 250g hydrated silica, 10g sodium lauryl sulfate, 4g polyglycerol-10 laurate, 2g hydrogenated lecithin, 1g tocopheryl acetate, 5g sodium citrate, 2g sodium benzoate, 1.5g sodium saccharin, 8g flavoring, 3g menthol, and 3g polysorbate 20 were added for homogenization. The homogenization and pH adjustment conditions were the same as in Example 1, resulting in an anti-inflammatory toothpaste based on Dendrobium huoshanense stem extract.

[0072] All other conditions are the same as in Example 1.

[0073] Comparative Example 5 200g sorbitol, 30g polyethylene glycol-8, 8g cellulose gum, 4g xanthan gum, and 5g modified chitosan were mixed in 100g deionized water to obtain a first mixture. 20g Dendrobium huoshanense stem extract, 10g Hibiscus syriacus flower extract, 10g Perilla frutescens leaf extract, 40g strontium chloride hexahydrate, 8g sodium phytate, and 5g tranexamic acid were mixed in 200g deionized water to obtain a second mixture. The first and second mixtures were then mixed, and then 250g hydrated silica, 12g sodium lauryl sulfate, 4g polyglycerol-10 laurate, 1g tocopheryl acetate, 5g sodium citrate, 2g sodium benzoate, 1.5g sodium saccharin, 8g flavoring, 3g menthol, and 3g polysorbate 20 were added for homogenization. The homogenization and pH adjustment conditions were the same as in Example 1, resulting in an anti-inflammatory toothpaste based on Dendrobium huoshanense stem extract.

[0074] All other conditions are the same as in Example 1.

[0075] Comparative Example 6 200g sorbitol, 30g polyethylene glycol-8, 8g cellulose gum, 4g xanthan gum, and 5g modified chitosan were mixed in 100g deionized water to obtain a first mixture. 20g Dendrobium huoshanense stem extract, 10g Hibiscus syriacus flower extract, 10g Perilla frutescens leaf extract, 40g strontium chloride hexahydrate, 8g sodium phytate, and 5g tranexamic acid were mixed in 200g deionized water to obtain a second mixture. The first and second mixtures were then mixed, and then 250g hydrated silica, 14g sodium lauryl sulfate, 2g hydrogenated lecithin, 1g tocopheryl acetate, 5g sodium citrate, 2g sodium benzoate, 1.5g sodium saccharin, 8g flavoring, 3g menthol, and 3g polysorbate 20 were added for homogenization. The homogenization and pH adjustment conditions were the same as in Example 1, resulting in an anti-inflammatory toothpaste based on Dendrobium huoshanense stem extract.

[0076] All other conditions are the same as in Example 1.

[0077] Comparative Example 7 200g sorbitol, 30g polyethylene glycol-8, 8g cellulose gum, 4g xanthan gum, and 5g modified chitosan were mixed in 100g deionized water to obtain a first mixture. 20g Dendrobium huoshanense stem extract, 10g Hibiscus syriacus flower extract, 10g Perilla frutescens leaf extract, 40g strontium chloride hexahydrate, 8g sodium phytate, and 5g tranexamic acid were mixed in 200g deionized water to obtain a second mixture. The first and second mixtures were then mixed, and then 250g hydrated silica, 16g sodium lauryl sulfate, 1g tocopheryl acetate, 5g sodium citrate, 2g sodium benzoate, 1.5g sodium saccharin, 8g flavoring, 3g menthol, and 3g polysorbate 20 were added for homogenization. The homogenization and pH adjustment conditions were the same as in Example 1, resulting in an anti-inflammatory toothpaste based on Dendrobium huoshanense stem extract.

[0078] All other conditions are the same as in Example 1.

[0079] Comparative Example 8 200g sorbitol, 30g polyethylene glycol-8, 8g cellulose gum, 4g xanthan gum, and 5g modified chitosan were mixed in 100g deionized water to obtain a first mixture. 20g Dendrobium huoshanense stem extract, 10g Hibiscus syriacus flower extract, 10g Perilla frutescens leaf extract, 40g strontium chloride hexahydrate, 8g sodium phytate, and 5g tranexamic acid were mixed in 200g deionized water to obtain a second mixture. The first and second mixtures were then mixed, and then 250g hydrated silica, 25g sodium lauryl sulfate, 1g tocopheryl acetate, 5g sodium citrate, 2g sodium benzoate, 1.5g sodium saccharin, 8g flavoring, 3g menthol, and 3g polysorbate 20 were added for homogenization. The homogenization and pH adjustment conditions were the same as in Example 1, resulting in an anti-inflammatory toothpaste based on Dendrobium huoshanense stem extract.

[0080] All other conditions are the same as in Example 1.

[0081] The anti-inflammatory properties of the anti-inflammatory toothpastes prepared in Examples 1-3 and Comparative Examples 1-4 were tested, and the results are shown in Table 1.

[0082] Anti-inflammatory assay method: Seventy healthy mice were randomly divided into 7 groups of 10 each. During the experiment, 0.1 ml of xylene was applied to both the anterior and posterior surfaces of the left ear of each mouse to induce inflammation. The right ear was left untreated as a blank control. Thirty minutes after xylene application, 0.1 g of anti-inflammatory toothpaste prepared in Examples 1-3 and Comparative Examples 1-4 was evenly applied to both sides of the left ear of each mouse in each group. Two hours later, the mice were euthanized by cervical dislocation. Both ears were cut off along the auricle edge. The toothpaste in the left ear was washed off with saline solution, and the ear was cleaned with a dry cotton ball. Two circular ear pieces were then chiseled from the same location using a punch. The weight of the left ear piece minus the weight of the right ear piece was the swelling value.

[0083] Table 1 Results of anti-inflammatory performance test As shown in Table 1, when evaluating the anti-inflammatory properties of each group of toothpastes using a xylene-induced mouse ear swelling model, the lower the average swelling value of the ear flap, the stronger the inhibitory effect on inflammatory swelling and the better the anti-inflammatory performance. The average swelling values ​​of the anti-inflammatory toothpastes prepared in Examples 1-3 were 12.43 mg, 14.27 mg, and 13.46 mg, respectively, all significantly lower than those in Comparative Examples 1-4. Among them, Example 1 had the lowest average swelling value, indicating that it had the best anti-inflammatory performance; Example 3 was second best; Example 2 also showed a good anti-inflammatory effect.

[0084] Further comparison revealed that the average swelling values ​​of Comparative Examples 1-3 were 22.71 mg, 22.44 mg, and 23.15 mg, respectively, all significantly higher than those of Examples 1-3. Since Comparative Examples 1-3 lacked one of the following extracts—Perilla leaf extract, Hibiscus flower extract, and Dendrobium officinale stem extract—their anti-inflammatory effects were significantly reduced even when the total amount of the three extracts remained essentially the same. This indicates that the combination of Dendrobium officinale stem extract, Hibiscus flower extract, and Perilla leaf extract can more effectively inhibit inflammatory ear swelling, and that there is a synergistic effect among the three extracts in improving the anti-inflammatory properties of the toothpaste.

[0085] Furthermore, the average swelling value of Comparative Example 4 was 17.39 mg, which was also higher than that of Example 1 (12.43 mg). The main difference between Comparative Example 4 and Example 1 is that the former used carboxymethyl chitosan, while the latter used modified chitosan. This indicates that the modified chitosan used in this application not only contributes to system stability but also further improves the anti-inflammatory properties of the toothpaste, thereby resulting in a superior anti-inflammatory effect in the obtained anti-inflammatory toothpaste.

[0086] The stability of the anti-inflammatory toothpastes prepared in Examples 1-3 and Comparative Examples 4-8 was tested, and the results are shown in Table 2.

[0087] Stability testing method: Toothpaste samples prepared in Examples 1-3 and Comparative Examples 4-8 were placed in containers of the same size, sealed, and subjected to a thermal cycling test. Each thermal cycle included the following steps: the sample was first stored at -8±1℃ for 8 hours, then transferred to 45±1℃ for 8 hours, and then restored to room temperature and stored for 8 hours, which constituted one cycle. After 5 thermal cycles, the separation rate and viscosity retention rate of the samples were measured to evaluate the stability of the toothpaste.

[0088] Separation rate detection: After the thermal cycling process, weigh 20.0g of toothpaste sample and place it in a centrifuge tube. Centrifuge at 3000rpm for 10min. If separation occurs, carefully aspirate or decant the separation and weigh it, recording it as m1. The initial sample mass of toothpaste is recorded as m0. Calculate the separation rate using the following formula: Liquid separation rate (%) = m1 / m0 × 100% The lower the separation rate, the more stable the toothpaste system is after hot and cold cycling, and the stronger its resistance to stratification and separation.

[0089] Viscosity retention rate test: Toothpaste samples without thermal cycling and those after thermal cycling were taken and their apparent viscosity was measured using a rotational viscometer at 25±1℃. Toothpaste is a typical thixotropic / shear-thinning system, and rotational rheology or viscometry are common methods for characterizing apparent viscosity. The initial apparent viscosity is recorded as V0, and the apparent viscosity after thermal cycling is recorded as V1. The viscosity retention rate was calculated using the following formula: Viscosity retention rate (%) = V1 / V0 × 100% A higher viscosity retention rate indicates that the paste structure of the sample is more intact after thermal cycling, and the rheological stability is better.

[0090] Table 2 Stability test results As shown in Table 2, after hot and cold cycling, the anti-inflammatory toothpastes prepared in Examples 1-3 all exhibited low separation rates and high viscosity retention rates, indicating that the toothpaste system of this application has good structural and storage stability under alternating hot and cold conditions. Among them, Example 1 had the lowest separation rate, only 0.21%, and the highest viscosity retention rate, reaching 95.8%, indicating that its paste structure was the most stable; Example 3 was second, with a separation rate of 0.33% and a viscosity retention rate of 93.6%; although Example 2 was slightly lower than Examples 1 and 3, the separation rate was still only 0.46%, and the viscosity retention rate reached 91.7%, still showing good overall stability. These results indicate that within the defined formulation range, this application, through the combined action of the three extracts, modified chitosan, and the compound emulsification / dispersion system composed of sodium lauryl sulfate, polyglycerol-10 laurate, and hydrogenated lecithin, can effectively maintain the integrity of the internal structure of the toothpaste paste, reduce aqueous phase migration and local phase separation during hot and cold cycling, thereby improving the paste stability.

[0091] Further comparison of Example 1 and Comparative Example 4 shows that the liquid separation rate of Comparative Example 4 is 1.12%, which is significantly higher than that of Example 1 (0.21%), and its viscosity retention rate also decreased from 95.8% in Example 1 to 84.9%. This indicates that the modified chitosan used in this application does not merely act as a thickener, but can more effectively enhance the internal network structure of the system, improve the dispersion stability of abrasives, plant extracts, and other functional components in the paste, reduce the tendency for liquid separation under hot and cold cycling conditions, and is more conducive to maintaining the original viscosity of the paste.

[0092] Comparative Examples 5-8 further reflect the impact of the compound emulsification / dispersion system on stability. Comparative Example 5 increased the amount of sodium lauryl sulfate but lacked hydrogenated lecithin; Comparative Example 6 further lacked polyglycerol-10 lauryl ester, retaining only hydrogenated lecithin; Comparative Examples 7 and 8 both relied solely on sodium lauryl sulfate to maintain system dispersion, with Comparative Example 7 using 16g of sodium lauryl sulfate and Comparative Example 8 increasing it to 25g. As shown in Table 2, the separation rates of Comparative Examples 5, 6, and 7 increased sequentially, to 1.38%, 1.79%, and 2.41%, respectively, while the viscosity retention rates decreased sequentially, to 82.4%, 78.1%, and 72.8%, respectively. This indicates that without polyglycerol-10 lauryl ester and / or hydrogenated lecithin, relying solely on sodium lauryl sulfate cannot maintain system stability comparable to the examples. Furthermore, as the auxiliary emulsifying / dispersion components are further reduced, the paste's resistance to thermal cycling significantly decreases.

[0093] It is worth noting that Comparative Example 8 exhibited a separation rate of 0.74% and a viscosity retention rate of 86.3%, demonstrating significantly better stability than Comparative Examples 5-7, especially Comparative Example 7. However, although Comparative Example 8 showed improvement over Comparative Example 7, its separation rate and viscosity retention rate were still significantly inferior to Example 1. This indicates that simply increasing the amount of sodium lauryl sulfate cannot replace the compound emulsification / dispersion system constructed from sodium lauryl sulfate, polyglycerol-10 lauryl ester, and hydrogenated lecithin in this application. This is because the compounding of these three components not only improves the compatibility between different polar components but also more stably maintains the multiphase dispersion structure within the paste. While increasing the amount of sodium lauryl sulfate can improve the initial dispersion effect to some extent, it is difficult to achieve the same interfacial synergistic stabilizing effect as the compound system, thus its final stability is still inferior to the system in the examples. Therefore, this invention, through improvements to the emulsification system, significantly reduces the amount of sodium lauryl sulfate while also improving the stability of the anti-inflammatory toothpaste, thus optimizing its stability and user comfort.

[0094] Although embodiments of this application have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and variations can be made to these embodiments without departing from the principles and spirit of this application. The scope of this application is defined by the appended claims and their equivalents, all of which should be included within the protection scope of this application.

Claims

1. An anti-inflammatory toothpaste based on Dendrobium huoshanense stem extract, characterized in that, The product contains the following ingredients in parts by weight: 20-30 parts abrasive, 15-30 parts humectant, 1-2 parts emulsifier, 1-2.5 parts thickener, 1-3 parts Dendrobium officinale stem extract, 0.5-1.5 parts Hibiscus syriacus flower extract, 0.5-1.5 parts Perilla frutescens leaf extract, 3.5-7.5 parts anti-allergen, 1-3.5 parts excipients, and 20-40 parts deionized water. The excipients are one or more of the following: antioxidants, pH adjusters, preservatives, flavoring agents, and coloring agents; The preparation method of the Dendrobium huoshanense stem extract is as follows: The stems of Dendrobium huoshanense were cleaned, dried, and crushed. The pulverized material is enzymatically hydrolyzed in water using a first complex enzyme. An extraction medium is added to the enzymatically hydrolyzed liquid for assisted extraction. After extraction, solid-liquid separation and ultrafiltration fractionation are performed to obtain Dendrobium huoshanense stem extract. The first compound enzyme consists of cellulase and pectinase in a mass ratio of 1-3:1, and the amount of the first compound enzyme added is 0.1-1% of the mass of the pulverized material. The extraction medium consists of glycerol and 1,3-propanediol in a mass ratio of 1:0.5-1.5, and the amount of extraction medium added accounts for 15-25% of the mass of water added during enzymatic hydrolysis. Ultrafiltration fractionation retains components with a molecular weight of 10-30 kDa; The preparation method of the okra flower extract is as follows: the pulverized okra flowers and the second complex enzyme are added to ethanol for ultrasonic extraction. After extraction, the extract is filtered, concentrated under reduced pressure and dried to obtain the okra flower extract. The second complex enzyme consists of cellulase and pectinase in a mass ratio of 2:1-4, and the amount added is 1-5% of the total mass of the okra flowers; The preparation method of the perilla leaf extract is as follows: dried perilla leaves are pulverized and placed into an extraction vessel. A mixture of supercritical CO2 and ethanol aqueous solution is used as the extraction medium for static extraction and dynamic extraction in sequence. After extraction, the co-solvent is removed by depressurization to obtain the perilla leaf extract. The static extraction conditions are: temperature 50-60℃, time 10-20 min, and pressure 25-35 MPa; The conditions for dynamic extraction are: temperature 50-60℃, time 100-130min, pressure 25-35MPa, CO2 flow rate 0.4-0.6g / min, and ethanol aqueous solution in the fluid accounting for 10-15% of the total mass of the supercritical CO2 and ethanol aqueous solution mixture.

2. The anti-inflammatory toothpaste based on Dendrobium officinale stem extract according to claim 1, characterized in that, The friction agent is one or more of silicon dioxide, calcium carbonate, and calcium hydrogen phosphate. And / or, the moisturizer is sorbitol and / or polyethylene glycol.

3. The anti-inflammatory toothpaste based on Dendrobium officinale stem extract according to claim 1, characterized in that, The emulsifier consists of 0.8-1.2 parts by weight of sodium lauryl sulfate, 0.3-0.5 parts by weight of polyglycerol-10 lauryl ester, and 0.1-0.3 parts by weight of hydrogenated lecithin.

4. The anti-inflammatory toothpaste based on Dendrobium officinale stem extract according to claim 1, characterized in that, The anti-allergen is one or more of the following: strontium salts, potassium salts, phytic acid and its salts, tranexamic acid and arginine.

5. The anti-inflammatory toothpaste based on Dendrobium huoshanense stem extract according to claim 1, characterized in that, The thickener consists of 0.5-1 parts by weight of cellulose gum, 0.3-0.5 parts of xanthan gum, and 0.4-0.6 parts of modified chitosan.

6. The anti-inflammatory toothpaste based on Dendrobium officinale stem extract according to claim 5, characterized in that, The modified chitosan is prepared as follows: Lauric acid, 1-ethyl-3-(3-dimethylaminopropyl)-carbodiimide and N-hydroxysuccinimide are mixed and activated, and then added to an aqueous solution of carboxymethyl chitosan for reaction. After the reaction, the mixture is purified and dried to obtain modified chitosan. And / or, the molar ratio of carboxymethyl chitosan, lauric acid, 1-ethyl-3-(3-dimethylaminopropyl)-carbodiimide and N-hydroxysuccinimide is 100:1-3:2-4:2-4; And / or, the reaction conditions are: temperature 40-50℃, time 4-8h, and pH of the reaction system 5-5.

5.

7. The anti-inflammatory toothpaste based on Dendrobium officinale stem extract according to claim 1, characterized in that, In the preparation method of Dendrobium officinale stem extract, the enzymatic hydrolysis conditions are: pH 4.8-5.5, temperature 45-52℃, time 1-3h, and material-to-liquid ratio 1:10-20; the auxiliary extraction temperature is 50-65℃, and the time is 1-2h.

8. The anti-inflammatory toothpaste based on Dendrobium officinale stem extract according to claim 1, characterized in that, In the preparation method of okra flower extract, the ultrasonic extraction conditions are: temperature 40-60℃, time 30-60min, ultrasonic power 300-500W, and system pH 5.5-6.

5.

9. A method for preparing an anti-inflammatory toothpaste based on Dendrobium huoshanense stem extract, wherein the anti-inflammatory toothpaste is as described in any one of claims 1-8, characterized in that, The steps are as follows: S1: Mix the humectant and thickener in deionized water to obtain the first mixture; S2: Mix Dendrobium officinale stem extract, Hibiscus syriacus flower extract, Perilla frutescens leaf extract and anti-allergy agent in deionized water to obtain a second mixture; S3: Mix the first mixture with the second mixture, then add abrasive, emulsifier and excipients, and homogenize to obtain an anti-inflammatory toothpaste based on Dendrobium officinale stem extract.

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