Preparation method of Chinese herbal medicine toothpaste and application of Chinese herbal medicine toothpaste in oral disease treatment

Abstract

The invention relates to the technical field of daily chemical products and oral care, and discloses a preparation method of Chinese herbal medicine toothpaste and application of the Chinese herbal medicine toothpaste in oral disease treatment, and the method prepares paste with double functions of physical shielding and chemical bacteriostasis by constructing a pH steady-state system and adding active components step by step. In the preparation, the broad-spectrum functional active extract is subjected to heat reflux extraction, the bioadhesive repair extract is subjected to low-temperature extraction and alcohol precipitation, and the bioadhesive repair extract is added after being subjected to low-temperature and low-shear conditions so as to retain the polysaccharide conformation. The obtained toothpaste contains honeysuckle, scutellaria baicalensis, bletilla striata and other traditional Chinese medicine components, can stably maintain the drug effect, and forms a biological adhesion film on the mucous membrane surface. The toothpaste can effectively improve oral ulcer, periodontitis, gingival bleeding and xerostomia complicated by diabetes mellitus, solves the problems of low drug retention rate and poor stability of existing products in the oral environment of diabetes mellitus, and realizes treatment of both symptoms and root causes.

Description

Technical Field

[0001] This invention relates to the field of daily chemical products and oral care technology, and in particular to a method for preparing herbal toothpaste and its application in the treatment of oral diseases. Background Technology

[0002] Diabetes mellitus, a systemic metabolic disease, is often accompanied by a variety of serious oral complications, including periodontitis, recurrent oral ulcers, gingival bleeding, and xerostomia. Compared with healthy individuals, the oral microenvironment of diabetic patients is more complex, mainly characterized by reduced saliva secretion, increased salivary glucose concentration, and a more acidic pH. This unique pathological environment leads to a decline in the oral cavity's self-cleaning ability, making it easier for pathogens to colonize, and significantly slowing the healing rate of damaged mucosa.

[0003] While there are many types of herbal toothpastes on the market, most of which use extracts of honeysuckle, scutellaria, and notoginseng to assist in the treatment of oral diseases, their efficacy in practical applications for oral diseases complicated by diabetes is often limited by the manufacturing process and dosage form characteristics. The main problem is that many key active ingredients in traditional Chinese medicine (such as glycosides like baicalin) are sensitive to pH and are easily hydrolyzed or oxidized and deactivated in unsuitable acidic or alkaline environments. Conventional toothpaste manufacturing processes typically do not construct specific pH buffer systems for the acidic oral environment of diabetic patients, leading to rapid degradation of the active ingredients during storage or upon contact with the oral environment, making it difficult to maintain the expected pharmacological activity.

[0004] Furthermore, the oral cavity is a highly moist environment constantly subjected to saliva rinsing and mechanical friction, and the effective retention time of drug components at the lesion site is a key factor determining the efficacy. Current technologies for preparing restorative toothpastes containing polysaccharides (such as Bletilla striata and Dendrobium officinale extracts) often employ a high-speed homogenous shearing process throughout the entire process to achieve a smooth paste. This high-intensity mechanical shearing force disrupts the molecular chain length and spatial structure of large polysaccharide molecules, leading to the loss of their original bioadhesiveness and film-forming properties. Therefore, existing products struggle to form an effective physical protective layer on ulcer surfaces or gingival pockets, and the drug components are easily diluted and removed by saliva, failing to achieve long-lasting physical shielding and chemical antibacterial effects, thus failing to meet the clinical needs of diabetic patients for oral mucosal repair and long-term inflammation control. Summary of the Invention

[0005] The technical problem solved by this invention is that the active ingredients in existing herbal toothpastes are easily degraded by pH in the oral environment of diabetic patients, and it is difficult to form an effective physical protective layer on the mucosal surface, resulting in a short residence time of the drug at the lesion site and a lack of lasting effect on improving oral ulcers and periodontitis.

[0006] To address the above problems, the present invention provides the following technical solution: In a first aspect, the present invention provides a method for preparing herbal toothpaste, wherein the method involves constructing a pH-stable system and adding active ingredients in steps to form a paste with both physical masking and chemical antibacterial functions. The method includes the following steps: S1. Preparation of pH-stable matrix: Mix deionized water and part of the humectant, add pH buffer, adjust the pH of the system to stabilize at 6.5-6.8, and then add sweetener to dissolve; S2. Gel and ointment preparation: The thickener is dispersed into a colloid, which is then drawn into an ointment making machine. Broad-spectrum active extracts and abrasives are added and homogenized under vacuum to prepare the initial ointment. S3. Cooling and Fragrance Adjustment: Add surfactants and fragrances to lower the temperature of the paste to below 45℃; S4. Post-addition of bioadhesion components: The bioadhesion repair extract is pre-dispersed in the reserved moisturizer to form a slurry. The slurry is added to the cooled paste and mixed evenly under the condition that the homogenizer is turned off and only the low-speed stirring is turned on. The product is then discharged. The broad-spectrum active extract is an extract rich in glycosides, obtained by hot reflux extraction. The bioadhesion repair extract is an extract rich in polysaccharides obtained through low-temperature extraction and alcohol precipitation.

[0007] By adopting the above technical solution, the present invention resolves the contradiction between the chemical stability of traditional Chinese medicine components and the integrity of the physical structure of biological macromolecules through a specific process.

[0008] Specifically, the glycosides such as baicalin contained in the broad-spectrum active extracts are sensitive to pH and are prone to hydrolysis or oxidation in alkaline or strongly acidic environments.

[0009] Step S1 introduces a pH buffer to maintain the ointment matrix in a weakly acidic range of pH 6.5–6.8. This range meets the chemical stability requirements of glycoside components, inhibits drug degradation during storage and use, and buffers acidic substances produced by oral metabolism.

[0010] Furthermore, the main active ingredient in bioadhesion repair extracts is macromolecular polysaccharides. The high-speed homogenization shear force in traditional processes can break the long polysaccharide chains, reducing their film-forming properties. This invention employs a gentle process of "pre-dispersion + low-speed stirring + no homogenization" in step S4, preserving the length and spatial conformation of the polysaccharide molecular chains.

[0011] During use, polysaccharide molecules that retain their complete conformation absorb water and swell upon contact with oral moisture, forming a hydrogel film with bioadhesive properties.

[0012] This membrane physically covers the ulcer or periodontal pocket surface, isolating it from external stimuli. At the same time, it adsorbs the antibacterial components in the broad-spectrum active extract, prolonging the drug's residence time at the lesion site and achieving a synergistic effect of physical shielding and sustained drug release.

[0013] Preferably, the herbal toothpaste is made from the following raw materials in parts by weight: 220-360 parts of humectant; 300-400 parts of deionized water; 200-300 parts of abrasive; 8-15 parts of thickener; 15-25 parts of surfactant; 20-35 parts of broad-spectrum active extract; 5-15 parts of bioadhesion repair extract; 2-5 parts of pH buffer; 3-6 parts of sweetener; and 6-12 parts of fragrance.

[0014] By adopting the above technical solution, the components are combined in a specific ratio, and the moisturizer and water form a suitable rheological system to ensure the extrudability and dispersibility of the ointment. The two extracts in a specific ratio ensure the concentration of the active ingredient while controlling the solid content, avoiding the ointment from drying out or separating, and ensuring the physical stability of the product.

[0015] Preferably, the broad-spectrum active extract is prepared from the following Chinese herbal raw materials in parts by weight: honeysuckle 100-150 parts, scutellaria baicalensis 100-150 parts, anemarrhena asphodeloides 80-150 parts, rehmannia glutinosa 150-200 parts, salvia miltiorrhiza 100-150 parts, polygonum multiflorum 100-150 parts, notoginseng 100-150 parts, and astragalus membranaceus 150-200 parts.

[0016] Preferably, the preparation steps of the broad-spectrum active extract are as follows: the Chinese herbal raw materials are mixed, water is added and heated under reflux for extraction, the extracts are combined and concentrated to a clear paste with a relative density of 1.18 to 1.20, and finally spray-dried to obtain a dry powder; the air inlet temperature of the spray drying is 175 to 185°C.

[0017] By employing the above-mentioned technical solutions, this formula, based on traditional Chinese medicine theory, combines honeysuckle, scutellaria, anemarrhena, and rehmannia to clear heat and detoxify, nourish yin and cool the blood, thus improving gingival redness and swelling; salvia miltiorrhiza, polygonum multiflorum, and notoginseng are combined to invigorate blood circulation, remove blood stasis, and improve periodontal microcirculation. The heating reflux extraction process effectively extracts heat-resistant glycosides, flavonoids, and saponins from the medicinal materials; spray drying technology ensures the uniformity of the extract powder's particle size and solubility, allowing it to be rapidly dispersed in the toothpaste matrix.

[0018] Preferably, the bioadhesion repair extract is prepared from the following traditional Chinese medicine raw materials in parts by weight: 90-150 parts of Bletilla striata, 80-150 parts of Dendrobium nobile, and 50-100 parts of Polygonatum odoratum.

[0019] Preferably, the preparation steps of the bioadhesion repair extract are as follows: (1) mix the Chinese herbal raw materials, add water and perform low-temperature extraction at a temperature not exceeding 70°C, collect the extract and concentrate it; (2) add ethanol to the concentrate for alcohol precipitation, so that the final concentration of ethanol reaches 70% to 75% v / v, and let it stand to precipitate; (3) collect the precipitate and obtain dry powder by vacuum freeze drying or low-temperature spray drying.

[0020] By employing the above-mentioned technical solutions, Bletilla striata, Dendrobium nobile, and Polygonatum odoratum contain plant polysaccharides with tissue-regenerating and wound-healing effects. Low-temperature extraction prevents the breakage of polysaccharide glycosidic bonds caused by high temperatures; ethanol precipitation utilizes the characteristic that polysaccharides are insoluble in high-concentration ethanol to remove impurities such as proteins and enrich highly adhesive polysaccharide components. This extract is the material basis for the formation of oral bioadhesive films and promotes the repair of damaged mucosa.

[0021] Preferably, in step S1, the pH buffer is composed of citric acid monohydrate and trisodium citrate dihydrate, and the mass ratio of the two is (1.0-1.5):(1.5-3.0).

[0022] By adopting the above technical solution, the buffer system composed of citric acid and sodium citrate has high safety in food-grade applications. A specific mass ratio can stabilize the system pH within the range of 6.5 to 6.8, which is close to the environment of human saliva, reducing the risk of acid erosion of tooth enamel while maintaining the bioactivity of key components such as baicalin.

[0023] Preferably, in step S4, the reserved humectant is glycerin; the speed of the low-speed stirring is controlled at 20-30 rpm, and the mixing time is 10-15 minutes.

[0024] By employing the above technical solution, the high viscosity of glycerol is used to pre-wet and disperse the bioadhesive extract powder, preventing it from absorbing water and clumping when directly applied to the aqueous paste. Controlling the rotation speed and mixing time reduces mechanical shear force while ensuring uniform material dispersion, protecting the integrity of the polysaccharide molecular chains and maintaining the adhesion and film-forming properties of the finished product.

[0025] The formulation of this invention closely follows the traditional Chinese medicine understanding of diabetes (Xiao Ke) as "deficiency of both Qi and Yin as the root cause, and dryness, heat and blood stasis as the manifestations". Combining the physiological and pathological characteristics of the oral cavity ("the gums belong to the stomach, and the teeth are the surplus of the bones"), a compound system of "clearing heat and nourishing Yin, replenishing Qi and promoting blood circulation, and promoting tissue regeneration and strengthening teeth" is constructed.

[0026] 1. Principal herbs (core): Honeysuckle, Scutellaria baicalensis, Anemarrhena asphodeloides, Rehmannia glutinosa When used together, these four ingredients work synergistically to clear heat and purge fire, nourish yin and generate fluids, directly addressing the root cause of yin deficiency and dryness in diabetes, and targeting symptoms of "internal heat" such as periodontitis, dry mouth, and swollen gums.

[0027] Honeysuckle, Scutellaria baicalensis: Traditional Chinese medicine theory: Scutellaria baicalensis is bitter and cold, clearing heat and drying dampness, purging fire and detoxifying, and is good at clearing heat in the upper burner (lung and stomach); Lonicera japonica is sweet and cold, clearing heat and detoxifying, and dispersing wind-heat. The two complement each other and are used to target the symptoms of oral heat, bitter taste, and halitosis caused by the "yin deficiency and dryness-heat" constitution in diabetic patients.

[0028] Modern pharmacology: Scutellaria baicalensis is rich in baicalin, which has broad-spectrum antibacterial and anti-inflammatory effects. It can significantly inhibit periodontal pathogens such as Porphyromonas gingivalis and reduce the release of inflammatory factors. Honeysuckle contains chlorogenic acid and luteolin, which can regulate local oral immunity, enhance the mucosal barrier function, and reduce the risk of oral infection in diabetic patients due to high sugar environment and low immunity.

[0029] Anemarrhena asphodeloides and Rehmannia glutinosa: Traditional Chinese medicine theory: Anemarrhena asphodeloides nourishes yin and moistens dryness, while Rehmannia glutinosa clears heat, cools the blood, nourishes yin, and generates fluids. The combination of these two herbs addresses the deficiency of body fluids caused by heat damaging yin, thus relieving dry mouth and tongue.

[0030] 2. Assistant herbs (for enhancement): Salvia miltiorrhiza, Polygonum multiflorum, Dendrobium nobile, Polygonatum odoratum The assistant medicine is divided into two routes to assist the principal medicine: one route invigorates blood and strengthens teeth, while the other nourishes yin and generates fluids.

[0031] Salvia miltiorrhiza and Polygonum multiflorum: Traditional Chinese medicine theory states that Polygonum multiflorum (He Shou Wu) nourishes the liver and kidneys, replenishes essence and blood; the kidneys govern bones, and teeth are considered an extension of bones, thus strengthening teeth; Salvia miltiorrhiza (Danshen) invigorates blood circulation, removes blood stasis, and relieves pain. Both herbs target the "blood stasis" pathogenesis caused by prolonged diabetes, improving gingival recession and tooth loosening.

[0032] Modern pharmacology: Tanshinone and other components can improve gingival microcirculation, increase blood oxygen supply to periodontal tissues, and promote the metabolism and repair of damaged tissues; Polygonum multiflorum extract helps to inhibit alveolar bone resorption and enhance the stability of periodontal supporting tissues.

[0033] Dendrobium, Polygonatum: Traditional Chinese medicine theory: It benefits the stomach and promotes the production of body fluids, nourishes yin and clears heat, assists the principal medicine in solving the "dryness" of diabetes, and significantly relieves the symptoms of dry mouth.

[0034] Modern pharmacology: Rich in Dendrobium polysaccharides and Polygonatum polysaccharides, it can not only promote salivary gland secretion and improve salivary flow rate, but also form a hydration film on the surface of oral mucosa, enhance the antioxidant capacity of mucosal cells, and reduce oxidative stress damage in a high-sugar environment.

[0035] 3. Adjuvant herbs (for harmonization and synergy): Panax notoginseng, Bletilla striata, Astragalus membranaceus Adjuvant drugs are responsible for addressing specific symptoms (bleeding, ulcers) and improving overall function.

[0036] Panax notoginseng, Bletilla striata: Traditional Chinese medicine theory: Panax notoginseng disperses blood stasis, stops bleeding, reduces swelling, and relieves pain, and is specifically used to treat bleeding gums; Bletilla striata astringes and stops bleeding, reduces swelling and promotes tissue regeneration, and is specifically used to treat non-healing ulcers.

[0037] Modern pharmacology: Panax notoginseng saponins reduce capillary permeability and resolve gingival bleeding caused by increased vascular fragility in diabetic patients; Bletilla striata gum has excellent film-forming and bioadhesive properties, which can physically cover the ulcer surface, promote the release of growth factors, and accelerate wound healing.

[0038] Astragalus: Traditional Chinese medicine theory: Tonify Qi and strengthen the exterior, promote tissue regeneration and detoxification. Qi generates blood and body fluids, so tonifying Qi helps generate Yin fluids; at the same time, it embodies the idea of ​​"supporting the body's resistance and eliminating pathogens," enhancing the local defense capabilities of the oral cavity.

[0039] Modern pharmacology: It enhances the body's non-specific immune function, promotes fibroblast proliferation, and has a significant effect on improving recurrent oral ulcers and slow wound healing common in diabetic patients.

[0040] In a second aspect, the present invention provides the application of a traditional Chinese medicine toothpaste in the preparation of a product for treating or alleviating oral diseases complicated by diabetes, wherein the traditional Chinese medicine toothpaste is prepared by the method described in the first aspect above.

[0041] By adopting the above technical solution, the herbal toothpaste prepared by this invention can effectively target the oral pathological environment of diabetic patients, characterized by high sugar content, acidity, and microcirculation disorders, and exert a synergistic therapeutic effect. Its specific application effects are reflected in the following aspects: First, for periodontitis and gingival bleeding: by utilizing the antibacterial and microcirculation-improving effects of baicalin, tanshinone, and other components in the broad-spectrum active extract, it significantly reduces the gingival index and bleeding index, reduces the depth of periodontal pockets, and inhibits alveolar bone resorption.

[0042] Secondly, for oral ulcers and mucosal repair: the bioadhesion layer constructed from Bletilla striata polysaccharide and Dendrobium officinale polysaccharide in the bioadhesion repair extract physically isolates the wound from the stimulation of high-sugar saliva and food residue, and acts as a drug reservoir to continuously release tissue-regenerating and ulcer-healing components, significantly shortening the ulcer healing time and reducing the recurrence rate.

[0043] Third, for dry mouth syndrome: the formula uses yin-nourishing and fluid-generating components (Rehmannia glutinosa, Dendrobium nobile, Polygonatum odoratum) to stimulate salivary gland secretion, and at the same time, the polysaccharide components form a hydration film on the mucosal surface, which effectively improves oral moisture and relieves swallowing difficulties and mucosal burning caused by dry mouth.

[0044] Preferably, the oral diseases associated with diabetes include recurrent oral ulcers, gingival redness and bleeding caused by periodontitis, loose teeth, and xerostomia.

[0045] By adopting the above technical solution, the indications for this toothpaste have been clarified, covering the most common and most disruptive oral complications in the quality of life of diabetic patients, demonstrating the "multi-target, all-round" oral care and treatment value of the product of this invention.

[0046] In summary, the present invention has at least one of the following beneficial technical effects: 1. This invention addresses the pathological characteristics of low and fluctuating saliva pH in diabetic patients. By constructing a stable buffer system with a pH of 6.5–6.8 during the preparation process, it effectively inhibits the hydrolysis and oxidative degradation of glycosides such as baicalin, ensuring the stability of the drug's chemical activity. Simultaneously, a bioadhesive component post-addition process fully preserves the spatial conformation of the macromolecular polysaccharide, enabling it to form a highly adhesive hydrogel film on the oral mucosa. This film not only physically shields the ulcer surface but also acts as a drug carrier, "locking" the active ingredients at the lesion site, resisting saliva erosion, and significantly prolonging the drug's duration of action. This solves the problem of rapid drug loss in the high-humidity environment of the oral cavity, a common issue with traditional herbal toothpastes.

[0047] 2. This invention is based on the pathogenesis of "deficiency of both Qi and Yin, dryness and heat with blood stasis," and scientifically combines heat-clearing herbs such as honeysuckle and scutellaria, blood-activating herbs such as salvia miltiorrhiza and notoginseng, and Yin-nourishing and tissue-regenerating herbs such as dendrobium and bletilla striata. This formula addresses the symptoms of gingival redness, bleeding, and periodontitis by antibacterial and anti-inflammatory effects and improving gingival microcirculation; it also addresses the underlying deficiency of dry mouth and fragile mucous membranes by nourishing Yin, promoting fluid production, and increasing saliva secretion. Clinical data show that this toothpaste is significantly superior to ordinary herbal toothpaste in reducing plaque index, gingival index, and shortening ulcer healing time, demonstrating the multi-target therapeutic advantages of compound ingredients in complex pathological environments.

[0048] 3. This invention breaks through the traditional "one-pot" or single-mixing preparation mode of toothpaste, and designs a graded processing technology based on the characteristics of the raw materials. For heat-resistant, broad-spectrum efficacy groups that require extraction of intracellular active ingredients (such as honeysuckle and scutellaria), hot reflux extraction and high-temperature spray drying are used to ensure the full release of active ingredients and powder uniformity. For heat-sensitive groups that rely on long-chain bioadhesion (such as bletilla and dendrobium), low-temperature extraction, alcohol precipitation enrichment, and freeze / low-temperature drying are used, combined with a low-shear post-addition process to avoid the damage to polysaccharide molecular structures caused by high temperature and mechanical shear. This differentiated process control maximizes the preservation of the bioactivity and physical functions of each component, providing a process guarantee for the high efficacy of the product. Detailed Implementation

[0049] The present invention will be further described in detail below with reference to specific embodiments. These descriptions are for explanation purposes only and are not intended to limit the scope of the invention.

[0050] The main raw materials and reagents used in the following examples and comparative examples have the following sources and specifications. Reagents not specifically mentioned are all commercially available analytical grade or higher grade products.

[0051] Bletilla striata, Dendrobium nobile, Polygonatum odoratum, Lonicera japonica, Scutellaria baicalensis, Anemarrhena asphodeloides, Rehmannia glutinosa, Salvia miltiorrhiza, Polygonum multiflorum, Panax notoginseng, and Astragalus membranaceus are all Chinese medicinal herbs purchased from regular pharmaceutical companies. They have been identified as meeting the medicinal standards stipulated in the Pharmacopoeia of the People's Republic of China (2020 edition) and have not undergone sulfur fumigation treatment.

[0052] Hydrated silica (precipitated silica), toothpaste-grade high-friction type, with an average particle size (d50) of 8–10 μm and an oil absorption value of 1.1–1.3 mL / g; sodium carboxymethyl cellulose (CMC-Na), with a degree of substitution of 0.8–0.9, and a viscosity of 800–1200 mPa·s for a 2% aqueous solution (25℃); sodium lauroyl sarcosinate, in powder form, with an active ingredient content ≥95%.

[0053] Citric acid monohydrate and trisodium citrate dihydrate both have a purity of ≥99.0%, meeting the standards for food additives; xylitol, 70% sorbitol aqueous solution, glycerin, menthol, and ethanol are all commercially available food-grade or pharmaceutical-grade products that meet the relevant national standards.

[0054] Preparation Example 1: This preparation example provides a bioadhesion repair extract, including the following steps: (1) Pretreatment: Weigh 120g of Bletilla striata, 120g of Dendrobium nobile and 80g of Polygonatum odoratum, wash them to remove impurities, dry them in an oven at 50℃ until constant weight, pulverize them and pass them through a 60-mesh sieve, and mix them evenly to obtain coarse powder.

[0055] (2) Low-temperature extraction: Place the coarse powder in an extraction tank and add 12 times the weight of the coarse powder in deionized water. Turn on the stirrer, control the speed at 40 rpm, heat to 65°C, and maintain this temperature for 2.5 hours. After extraction, filter with a 200-mesh filter cloth and collect the filtrate; repeat the extraction of the residue under the above conditions once, and combine the two filtrates.

[0056] (3) Vacuum concentration: The combined filtrate is pumped into a rotary evaporator and concentrated under reduced pressure at a vacuum of -0.07 MPa and a temperature of 52°C until the relative density of the concentrate measured at 50°C is 1.12, thus obtaining a clear paste.

[0057] (4) Alcohol precipitation and enrichment: Cool the clear extract to 25°C, and slowly add 95% (v / v) ethanol while stirring (60 rpm) until the final ethanol concentration of the solution reaches 72% (v / v). Stop stirring, seal the container, and place it in a 4°C cold storage to settle for 18 hours.

[0058] (5) Drying and powdering: The upper clear liquid is aspirated, and the colloidal precipitate at the bottom is collected. The precipitate is spread evenly in a tray and placed in a vacuum freeze dryer. The cold trap temperature is set to -45℃ and the vacuum degree is 15Pa. The mixture is dried for 30 hours to obtain a loose block. After being pulverized and passed through a 100-mesh sieve, a light white bioadhesion repair extract powder is obtained.

[0059] Preparation Example 2: This preparation example provides a bioadhesion repair extract, including the following steps: (1) Pretreatment: Weigh 90g of Bletilla striata, 80g of Dendrobium nobile and 50g of Polygonatum odoratum, wash and dry them respectively, pulverize them through a 60-mesh sieve, and mix them to obtain coarse powder.

[0060] (2) Low-temperature extraction: Place the crude powder in an extraction tank and add 10 times the weight of the crude powder in deionized water. Turn on the stirring (30 rpm), control the temperature at 60℃, and extract for 3.0 hours. Filter, extract the residue again, and combine the filtrates.

[0061] (3) Vacuum concentration: The filtrate is concentrated under reduced pressure at a vacuum of -0.08 MPa and a temperature of 50°C until the relative density of the concentrate measured at 50°C is 1.10, thus obtaining the clear extract.

[0062] (4) Alcohol precipitation enrichment: Cool the clear extract to 25°C, add 95% ethanol while stirring, so that the final ethanol concentration of the system reaches 70% (v / v). Let it stand at 4°C for 24 hours to precipitate.

[0063] (5) Drying and powdering: Collect the precipitate, place it in a vacuum freeze dryer, set the cold trap temperature to -40℃ and the vacuum degree to 20Pa, and dry for 36 hours. Pulverize it through a 100-mesh sieve to obtain a light white bioadhesion repair extract powder.

[0064] Preparation Example 3: This preparation example provides a bioadhesion repair extract, including the following steps: (1) Pretreatment: Weigh 150g of Bletilla striata, 150g of Dendrobium nobile and 100g of Polygonatum odoratum, and treat them in the same way as in Preparation Example 1.

[0065] (2) Low-temperature extraction: Add 12 times the weight of the crude powder in deionized water. Turn on the stirring (50 rpm), control the temperature at 70℃, and extract for 2.0 hours. Filter, extract the residue again, and combine the filtrates.

[0066] (3) Vacuum concentration: The filtrate is concentrated under reduced pressure at a vacuum of -0.06 MPa and a temperature of 55°C until the relative density of the concentrate measured at 50°C is 1.15, thus obtaining the clear extract.

[0067] (4) Alcohol precipitation enrichment: Cool the clear extract to 25°C, add 95% ethanol while stirring, so that the final ethanol concentration of the system reaches 75% (v / v). Let it stand at 4°C for 12 hours to precipitate.

[0068] (5) Drying and powdering: Collect the precipitate and spray dry it at low temperature. Dissolve the precipitate in a small amount of water to make a slurry with a solid content of 20%, pump it into the spray drying tower, set the inlet air temperature to 130°C and the outlet air temperature to 65°C, collect the powder at the bottom of the tower, and pass it through a 100-mesh sieve to obtain the dry powder of the bioadhesion repair extract.

[0069] Preparation Example 4: This preparation example provides a broad-spectrum active extract, comprising the following steps: (1) Mixed soaking: Weigh out 120g of honeysuckle, 100g of scutellaria, 80g of anemarrhena, 150g of rehmannia, 120g of salvia miltiorrhiza, 120g of polygonum multiflorum, 100g of notoginseng, and 150g of astragalus. After mixing, add 10 times the total weight of deionized water and soak at room temperature for 30 minutes.

[0070] (2) Reflux extraction: Heat the soaked medicinal materials to boiling and reflux for 1.5 hours while maintaining a gentle boil. Filter the mixture using a 100-mesh filter and temporarily store the filtrate. Add 8 times the amount of deionized water to the residue and reflux for 1.0 hour again, then filter.

[0071] (3) Combining and concentrating: Combine the two filtrates, pump them into a vacuum concentrator, and concentrate them under vacuum conditions of -0.07MPa and temperature of 65℃ until the relative density of the concentrate measured at 60℃ is 1.18.

[0072] (4) Spray drying: Heat the concentrate to 60°C and pump it into a spray dryer for drying. Set the inlet air temperature to 175°C, the outlet air temperature to 85°C, and the atomizing disc speed to 16000 rpm. Collect the powder in the drying chamber and below the cyclone separator, and pass it through an 80-mesh sieve to obtain a dark brown broad-spectrum active extract powder.

[0073] Preparation Example 5: This preparation example provides a broad-spectrum active extract, comprising the following steps: (1) Mixed soaking: Weigh out 150g of honeysuckle, 150g of scutellaria, 150g of anemarrhena, 200g of rehmannia, 150g of salvia miltiorrhiza, 150g of polygonum multiflorum, 150g of notoginseng, and 200g of astragalus. After mixing, add 8 times the total weight of deionized water and soak for 30 minutes.

[0074] (2) Reflux extraction: Heat to boiling and reflux for 2.0 hours. Filter; add 6 times the amount of water to the residue and extract again for 1.5 hours, then filter.

[0075] (3) Combining and concentrating: Combine the filtrates and concentrate them under vacuum of -0.08 MPa and temperature of 70°C until the relative density of the concentrate measured at 60°C is 1.20.

[0076] (4) Spray drying: Pump the concentrate into the spray dryer. Set the inlet air temperature to 180℃, the outlet air temperature to 90℃, and the atomizing disc speed to 18000rpm. Collect the powder and pass it through an 80-mesh sieve to obtain a dark brown broad-spectrum active extract powder.

[0077] Example 1: This embodiment provides a method for preparing herbal toothpaste, including the following steps: (1) Preparation of pH-stable matrix: Add 373g of deionized water, 150g of 70% sorbitol aqueous solution and 100g of glycerol (reserve 50g for subsequent steps) to the mixing tank and stir until homogeneous. Weigh 1.2g of citric acid monohydrate and 1.8g of trisodium citrate dihydrate, dissolve them in a small amount of water and add them to the tank. Stir and check the pH value, and fine-tune the ratio to stabilize the pH value of the system at 6.6. Then add 3g of xylitol and stir until completely dissolved.

[0078] (2) Gel preparation: Turn on the high-speed disperser (speed 1200 rpm), slowly sprinkle in 10g of sodium carboxymethyl cellulose (CMC-Na), stir for 15 minutes until a uniform transparent colloid is formed, and let it stand to swell for 20 minutes.

[0079] (3) Preparation and homogenization: The colloid was drawn into the main pot of the vacuum ointment maker. 25g of the broad-spectrum active extract powder obtained in Preparation Example 4 was added under scraper stirring (35 rpm) and mixed for 5 minutes. Then 250g of hydrated silica was drawn in, and the homogenizer (2200 rpm) and scraper stirring (45 rpm) were turned on under a vacuum of -0.09 MPa. The mixture was homogenized for 12 minutes until the ointment was smooth.

[0080] (4) Cooling and Fragrance Adjustment: Maintain a vacuum state and inhale 18g of sodium lauroyl sarcosinate and 8g of menthol. Turn off the homogenizer and keep only the scraper stirring (40rpm). Pass cooling water through to lower the temperature of the paste to 42℃ and stir for 8 minutes.

[0081] (5) Post-addition of bioadhesion component: Take 50g of reserved glycerin and fully disperse 10g of the bioadhesion repair extract powder obtained in Preparation Example 1 into it, and stir into a uniform slurry. Inhale the slurry into the main pot of the ointment maker, and gently stir for 12 minutes under low shear conditions with the homogenizer off and only the scraper stirring (25rpm) on, so that the material is evenly dispersed.

[0082] (6) Discharge: Break the vacuum, filter the paste through an 80-mesh sieve, pump it into a storage tank for aging for 12 hours, and then fill it into a container.

[0083] Example 2: This embodiment provides a method for preparing herbal toothpaste, including the following steps: (1) Preparation of pH-stable matrix: Add 356.5g of deionized water, 180g of 70% sorbitol aqueous solution and 120g of glycerol (reserve 50g for subsequent steps) to the mixing tank and stir well. Add a buffer solution consisting of 1.5g of citric acid monohydrate and 2.0g of trisodium citrate dihydrate to adjust the pH of the system to 6.5. Add 4g of xylitol to dissolve.

[0084] (2) Gel preparation: Turn on the high-speed disperser (1400rpm), add 9g of CMC-Na, stir to form a colloid, and let it stand to swell.

[0085] (3) Preparation and homogenization: The colloid is drawn into the main pot. 20g of the broad-spectrum active extract powder obtained in Preparation Example 4 is added and mixed evenly. 220g of hydrated silica is drawn in and homogenized (2000rpm) for 15 minutes under a vacuum of -0.09MPa.

[0086] (4) Cooling and Fragrance Adjustment: Inhale 16g of sodium lauroyl sarcosinate and 6g of menthol. Cool to 40°C, stirring only with a scraper.

[0087] (5) Post-addition of bioadhesion components: Take 50g of reserved glycerin and disperse 15g of the bioadhesion repair extract powder obtained in Example 2 (high adhesion formulation) to make a slurry. Inhale into the main pot and stir at low speed (20rpm) for 15 minutes.

[0088] (6) Discharge: sieve, age, and fill.

[0089] Example 3: This embodiment provides a method for preparing herbal toothpaste, including the following steps: (1) Preparation of pH-stable matrix: Add 389g of deionized water, 120g of 70% sorbitol aqueous solution and 80g of glycerol (reserve 40g for subsequent steps) to the mixing tank and stir well. Add a buffer solution consisting of 1.0g of citric acid monohydrate and 3.0g of trisodium citrate dihydrate to adjust the pH of the system to 6.8. Add 5g of xylitol to dissolve.

[0090] (2) Gel preparation: Turn on the high-speed disperser (1500rpm), add 12g of CMC-Na, and stir to make a colloid.

[0091] (3) Paste preparation and homogenization: The colloid is drawn into the main pot. 35g of the broad-spectrum active extract powder (high-activity formula) obtained in Preparation Example 5 is added and mixed evenly. 280g of hydrated silica is drawn in and homogenized (2500rpm) for 10 minutes under a vacuum of -0.09MPa.

[0092] (4) Cooling and fragrance adjustment: Inhale 20g of sodium lauroyl sarcosinate and 10g of menthol. Cool down to 45℃.

[0093] (5) Post-addition of bioadhesion components: Take 40g of reserved glycerin and disperse 5g of the bioadhesion repair extract powder obtained in Example 3 to make a slurry. Inhale into the main pot and stir at low speed (30rpm) for 10 minutes.

[0094] (6) Discharge: sieve, age, and fill.

[0095] Comparative Example 1: Compared with Example 1, the difference is that citric acid monohydrate and trisodium citrate dihydrate were not added, and this part of the weight was replaced with deionized water. The pH adjustment step was not performed, and the final toothpaste pH value was about 8.2 (natural pH). All other raw materials and preparation steps were the same.

[0096] Comparative Example 2: Compared to Example 1, the difference lies in the preparation process of the herbal extract. Specifically, all the herbal raw materials described in Example 1 and Example 4 are mixed and processed uniformly using the reflux extraction and spray drying process described in Example 4 to obtain a mixed extract powder. In the toothpaste preparation process, this mixed extract powder is added entirely in step 3, and the post-addition operation in step 5 is omitted; all other steps remain the same.

[0097] Comparative Example 3: Compared with Example 1, the difference lies in the timing and mixing method of adding the extract powder obtained in Example 1. Specifically, in step 3, the extract powder obtained in Example 1 and the extract powder obtained in Example 4 are added to the main pot simultaneously, and the homogenizer (2200 rpm) is turned on for high-shear mixing. The post-addition operation in step 5 is omitted, and the rest are the same.

[0098] Comparative Example 4: Compared with Example 1, the difference is that the extract powder obtained in Preparation Example 1 was not added, its weight was replaced with deionized water, and step 5 was omitted; all other operations are the same.

[0099] Test Example 1: The experimental steps are as follows: (1) Select fresh isolated porcine small intestinal mucosa, remove fat and connective tissue, and wash with physiological saline. Cut the mucosa into 2.5cm×2.5cm square segments, lay them flat on a glass slide, and place them in a constant temperature and humidity chamber at 37℃ and 95% relative humidity for 30 minutes to equilibrate.

[0100] (2) Weigh 0.50g of the toothpaste samples prepared in Examples 1-3 and Comparative Examples 1-4 respectively, spread them evenly on the mucosa surface, control the coating area to be 2.0cm×2.0cm, and let stand for 2 minutes.

[0101] (3) Fix the glass slide on the tilted support at a tilt angle of 45 degrees. Use a peristaltic pump to control the flow rate of deionized water at 50 mL / min and continuously rinse the mucosal surface of the coated sample for 30 seconds.

[0102] (4) After rinsing, collect the residue on the mucosal surface and disperse it in 10 mL of distilled water to dissolve it by sonication. Take 1.0 mL of the supernatant, add 1.0 mL of 5% phenol solution and 5.0 mL of concentrated sulfuric acid, shake to mix, and let stand at room temperature for 20 minutes. Use a UV-Vis spectrophotometer to measure the absorbance at a wavelength of 490 nm. Use the absorbance of the unrinsed initial coated sample as a control to calculate the residual rate of polysaccharides.

[0103] The bioadhesion retention rate test results for each group of samples are shown in the table below: Table 1: Bioadhesion retention rate test data of toothpastes in simulated oral environment Table 1 shows that the residual rates of Examples 1-3 remained between 71.84% and 86.18%. Among them, Example 2, which used a higher proportion of the extract obtained from Example 2, achieved a residual rate of 86.18%, indicating that the polysaccharide components in the extract helped to construct the erosion-resistant layer.

[0104] The residual rate of Comparative Example 2 was 45.13%, lower than that of Example 1. Comparative Example 2 used a mixed reflux extraction process. The high temperature and acidic environment caused by coexisting components led to the glycosidic bond breakage of Bletilla striata mannan and Dendrobium officinale polysaccharides, resulting in a decrease in molecular weight and weakening the physical entanglement and hydrogen bonding between the molecular chains and the mucosal surface.

[0105] The residual rate of Comparative Example 3 was 54.16%, lower than that of Example 1. Comparative Example 3 employed a high-shear homogenization process during ointment preparation. The strong mechanical shear force damaged the polymer polysaccharide chain structure, disrupting the integrity of the gel network and reducing its physical film-forming properties.

[0106] The residue rate of Comparative Example 4 was 12.76%, mainly reflecting the base viscosity of sodium carboxymethyl cellulose in the toothpaste matrix. This data indicates that conventional thickeners cannot provide sufficient bioadhesion protection under water rinsing, confirming the core role of the extracts obtained in Preparation Examples 1-3 in the formulation. The above results demonstrate that stepwise extraction and subsequent addition of low-shear processes can reduce the degradation of functional polysaccharides, which is key to improving the retention performance of products in humid environments.

[0107] Test Example 2: The experimental steps are as follows: (1) The toothpaste samples prepared in Examples 1-3 and Comparative Examples 1-4 were packaged into clean aluminum-plastic composite tubes and the tube ends were sealed. Each group of samples was divided into two batches. One batch was placed in a 4°C refrigerator as a control group (initial value), and the other batch was placed in a 50°C constant temperature drying oven for accelerated aging test for 30 days.

[0108] (2) After aging, accurately weigh about 1.0g of each toothpaste sample and place it in a 50mL stoppered conical flask. Add 25mL of methanol precisely. Seal the flask tightly, weigh it, and sonicate it (power 250W, frequency 40kHz) for 30 minutes. Remove it, let it cool, weigh it again, replenish the lost weight with methanol, and shake well.

[0109] (3) Filter the extract through a 0.45 μm microporous membrane and use the filtrate as the test solution.

[0110] (4) The content of baicalin in the filtrate was determined by high performance liquid chromatography (HPLC). The chromatographic conditions were set as follows: C18 column (250 mm × 4.6 mm, 5 μm); mobile phase: methanol-0.2% phosphoric acid solution (volume ratio 47:53); flow rate: 1.0 mL / min; detection wavelength: 280 nm; column temperature: 30 °C; injection volume: 10 μL.

[0111] (5) Calculate the content of baicalin in each sample according to the external standard method, and calculate the retention rate according to the formula: retention rate (%) = (content after aging at 50℃ for 30 days / content of control group at 4℃) × 100%.

[0112] Table 2 shows the baicalin retention rate data of each group of samples under simulated aging conditions.

[0113] Table 2: Retention rate test data of baicalin in toothpaste of different groups under accelerated aging conditions According to the data in Table 2, the baicalin retention rates in Examples 1-3 were all between 92.80% and 95.01%, indicating that baicalin has high chemical stability in a weakly acidic environment of pH 6.5-6.8. Example 3, with a pH of 6.8 (close to neutral), had a slightly higher retention rate (95.01%) than Example 2 (pH 6.5), showing that this pH range is suitable for the preservation of baicalin.

[0114] The average retention rate of Comparative Example 1 was only 67.18%, significantly lower than that of the other examples. Comparative Example 1 did not include a citric acid-sodium citrate buffer system, and the toothpaste matrix exhibited its natural pH (approximately 8.2). Baicalin contains a glucuronic acid structure and phenolic hydroxyl groups in its molecular structure, making it highly susceptible to glycosidic bond hydrolysis under alkaline conditions to generate baicalein, or oxidation to quinones, leading to a significant decrease in the content of the active ingredient and browning of the toothpaste color.

[0115] The retention rate of Comparative Example 2 was 88.23%, lower than that of Example 1. Although Comparative Example 2 had a buffer system, it used a mixed reflux extraction process. The interaction between different medicinal components and the long thermal process during extraction may have introduced some impurities or precursors that promote degradation, resulting in a slight decrease in the stability of baicalin in the final product.

[0116] The retention rate of Comparative Example 4 was 93.84%, which was close to that of Example 1. Although Comparative Example 4 lacked the bioadhesive extract, it retained the same pH buffer system, further confirming that pH control is the decisive factor affecting the stability of baicalin, while the presence or absence of the bioadhesive extract has no significant interference with the chemical stability of baicalin.

[0117] In summary, by anchoring the pH of the system to the range of 6.5–6.8 using a citrate-sodium citrate buffer pair, the hydrolysis and oxidative degradation of baicalin during storage were effectively inhibited, ensuring the content of the effective ingredients in the product during its shelf life.

[0118] Test Example 3: The experimental steps are as follows: (1) Preparation of bacterial suspension: The standard strain of Candida albicans (ATCC 10231) was inoculated into Sabouraud dextrose liquid medium and cultured at 37°C with shaking for 18 hours. The bacterial cells were washed with sterile physiological saline and the concentration of the bacterial suspension was adjusted to 1×10⁻⁶. 6 CFU / mL.

[0119] (2) Preparation of bacterial plates: Heat and melt Sabouraud dextrose agar medium, cool to about 50°C, add the above bacterial suspension at an inoculation rate of 5% (v / v), mix thoroughly and pour into sterile Petri dishes, cool and solidify to prepare bacterial plates.

[0120] (3) Sample preparation: Accurately weigh 2.0g of toothpaste samples from Examples 1-3 and Comparative Examples 1-4, add 8.0mL of sterile deionized water, shake thoroughly to mix, and prepare a toothpaste dispersion with a mass concentration of 20%.

[0121] (4) Punching and adding samples: Using a sterile punch with a diameter of 6 mm, punch holes in a quincunx pattern on the bacterial plate and remove the agar from the wells. Use a micropipette to draw 100 μL of toothpaste dispersion from each group and inject it into the well. Set up 3 parallel replicates for each sample group.

[0122] (5) Incubation and measurement: Place the petri dishes in a 37℃ constant temperature incubator and incubate upright for 24 hours. Use vernier calipers to measure the diameter of the inhibition zone (including the pore size) using the cross-section method and record the data.

[0123] Table 3 lists the measurement results of the inhibition zone diameter for each group of toothpaste samples against Candida albicans.

[0124] Table 3: In vitro anti-Candida albicans inhibition zone diameter test data for each group of toothpastes Based on the data analysis in Table 3, the embodiments of the present invention demonstrate significant advantages in antifungal performance, and the specific conclusions are as follows: The average inhibition zone diameters of Examples 1-3 ranged from 20.12 mm to 21.91 mm, demonstrating extremely strong anti-Candida albicans activity. Among them, Example 3 (high-activity formulation, pH 6.8) had a slightly higher value, but the difference from Example 1 (pH 6.6) was not significant, indicating that the formulation system could maintain highly efficient antibacterial ability within the pH range of 6.5-6.8.

[0125] The average inhibition zone diameter of Comparative Example 1 was 13.64 mm, a decrease of approximately 35% compared to Example 1. Comparative Example 1 lacked a pH buffer system, and its substrate pH was approximately 8.2. *Candida albicans* exhibits strong environmental adaptability, and its cell wall structure becomes more compact in a slightly alkaline environment, increasing drug permeation resistance. Furthermore, the active ingredients (such as baicalin and berberine) in Preparation Examples 4 and 5 showed altered dissociation and decreased lipid solubility under alkaline conditions, resulting in a weakened ability to penetrate the fungal cell membrane. The weakly acidic environment constructed using the citrate buffer system in Example 1 directly inhibited the growth and metabolism of alkalophilic fungi while maintaining the molecular proportions of active molecules, enhancing transmembrane transport efficiency, and demonstrating the synergistic effect of a suitable pH environment and active ingredients.

[0126] The average inhibition zone diameter of Comparative Example 2 was 16.77 mm, which was lower than that of Example 1. Comparative Example 2 used a mixed extraction process, and the long-term high-temperature reflux caused some heat-sensitive antibacterial components (such as chlorogenic acid in honeysuckle and catalpol in rehmannia glutinosa) to degrade or isomerize, resulting in a decrease in the total content of effective ingredients, thereby weakening the antibacterial efficacy of the final product.

[0127] The data from Comparative Examples 3 and 4 (20.98 mm and 20.88 mm, respectively) are close to those from Example 1 (21.12 mm). This indicates that the change in the shearing process (Comparative Example 3) and the absence of the adhesive component (Comparative Example 4) mainly affect the physical adhesion and film-forming properties, while having a smaller impact on the chemical drug dissolution and diffusion inhibition. This result indirectly confirms that the antibacterial activity mainly originates from the broad-spectrum active extract obtained in Preparation Examples 4 / 5 and the regulation of the pH environment. It complements the physical performance test of Test Example 1, jointly supporting the dual mechanism of physical adhesion and chemical antibacterial action of this invention.

[0128] Test Example 4: The experimental steps are as follows: (1) Prepare a 20% (w / v) gelatin solution, heat to dissolve, pour into a petri dish, and place in a 4℃ refrigerator to cool and solidify for 2 hours to prepare a gelatin gel model with a smooth surface and a certain hardness. Use a standard scalpel blade to draw standardized grooves with a length of 20mm, a width of 2mm, and a depth of 2mm on the gel surface to simulate oral ulcer wounds.

[0129] (2) Mix the toothpaste samples of Examples 1-3 and Comparative Examples 1-4 with deionized water at a mass ratio of 1:3 and stir magnetically for 3 minutes to prepare a uniform slurry. Take 0.5 mL of each slurry and add it to the above scratches, ensuring that the grooves are completely covered, and let it stand for 1 minute.

[0130] (3) Tilt the gel model at 45 degrees and rinse the scratched area directly with constant flow deionized water at a flow rate of 40 mL / min for 20 seconds to remove the paste that did not adhere effectively.

[0131] (4) Immediately apply 0.1% (w / v) methylene blue staining solution to the scratched area and cover for 30 seconds. Then rinse the surface with plenty of deionized water until there is no residual stain in the non-scratched areas.

[0132] (5) The treated gel was placed under a stereomicroscope to acquire images. The gray values ​​of the scratched areas were read using ImageJ image analysis software. The gray value range was 0 to 255, where 0 represented pure black (deepest staining, complete penetration) and 255 represented pure white (unstained, complete blocking). Three parallel samples were prepared for each group for measurement.

[0133] Table 4 lists the grayscale value test results of the scratched areas after processing of each group of samples.

[0134] Table 4: Methylene blue staining gray values ​​of simulated ulcer surfaces after toothpaste treatment in each group Based on the data analysis in Table 4, the technical solution provided by this invention shows significant differences in physical shielding and film-forming protection performance. The specific conclusions are as follows: The average grayscale values ​​of the scratched areas in Examples 1-3 ranged from 190.1 to 219.8, indicating very light staining. This demonstrates that the extracts obtained in Examples 1-3 formed a dense and continuous bioadhesive film on the gel surface. This film exhibits strong resistance to water erosion and effectively blocks the permeation and diffusion of methylene blue molecules, confirming its physical sealing and isolation effect on the damaged wound. Example 2, due to its higher content of the adhesive component, formed the thickest film with the best barrier effect.

[0135] The average gray value of Comparative Example 4 was only 45.9, close to the state of deep staining. Comparative Example 4 contained only the basic thickener (CMC-Na), most of which was removed during the water rinsing step. The residual layer could not form an effective mass transfer resistance, causing the dye to quickly penetrate into the deep layer of the gel.

[0136] Comparative Examples 2 (average gray value 88.4) and 3 (average gray value 103.0) performed significantly worse than Example 1. The mixing and reflux process in Comparative Example 2 caused thermal degradation of the polysaccharide, while the high-shear process in Comparative Example 3 caused mechanical chain breakage of the polysaccharide. The reduction in molecular weight and chain length directly resulted in the inability of polysaccharide molecules to form a tight physical entanglement network, leading to increased pore size and decreased density of the membrane, which could not effectively block the passage of dye molecules. This result explains, from a microstructural perspective, why the "low-temperature stepwise extraction" and "low-shear post-addition" processes must be used: only by maintaining the integrity of the long-chain structure of plant polysaccharides can a repair layer with effective physical barrier function be constructed.

[0137] The average gray value of Comparative Example 1 was 180.9, slightly lower than that of Example 1. Although its physical adhesion components were the same as those of Example 1, the slightly alkaline environment may have affected the stretching state of the polysaccharide molecular chains and the electrostatic interaction with the gelatin matrix (simulating collagen), resulting in a slight weakening of the interfacial binding force of the film layer. However, its overall physical shielding ability was still significantly better than that of the process-damaged groups (Comparative Examples 2 and 3).

[0138] Test Example 5: The experimental steps are as follows: (1) Sixty-eight volunteers who met the diagnostic criteria for type 2 diabetes and had oral problems were selected, including 38 males and 30 females, aged 45 to 72 years.

[0139] (2) Subjects stopped using other functional toothpastes or mouthwashes and used the toothpaste prepared in Example 1.

[0140] (3) Brush your teeth twice a day, morning and evening, for at least 3 minutes each time; for ulcers or red and swollen areas, rinse your mouth with the foam for 1 minute after brushing and then spit it out.

[0141] (4) Use continuously for 3 months and record the time of symptom improvement and outcome.

[0142] Table 5 summarizes the improvement of oral symptoms associated with diabetes by the toothpaste in Example 1.

[0143] Table 5: Clinical data of toothpaste in Example 1 for oral symptoms in diabetic patients Table 5 shows that 30 patients with ulcers healed within 2–7 days without recurrence. Honeysuckle, Scutellaria baicalensis, Anemarrhena asphodeloides, and Rehmannia glutinosa are the core ingredients of the formula, targeting the "yin deficiency and dryness-heat" pathogenesis of diabetes, exerting the effects of clearing heat and purging fire, nourishing yin and promoting fluid production, thus eliminating the root cause of mucosal inflammation; combined with the astringent and tissue-regenerating effects of Bletilla striata, it promotes wound repair. Combined with the results of test case 4, the bio-adhesive membrane formed in Example 1 provides physical isolation for the ulcer surface, preventing secondary bacterial stimulation and shortening the healing cycle.

[0144] Ten patients with loose teeth experienced symptom improvement after two weeks of use. Polygonum multiflorum (He Shou Wu) has liver- and kidney-tonifying effects, while Salvia miltiorrhiza (Danshen) has blood-activating and stasis-removing effects. Together, they improve periodontal microcirculation, increase the nutrient supply of the gums to the alveolar bone, and address the periodontal tissue atrophy caused by blood stasis in diabetic patients, thus achieving tooth strengthening.

[0145] Sixteen patients with bleeding and 12 patients with periodontitis experienced symptom resolution within one week. Panax notoginseng exerted its hemostatic and blood-activating effects, combined with the blood-cooling properties of Rehmannia glutinosa, reducing capillary fragility and eliminating inflammatory congestion. Baicalin and other components maintained high activity under a stable pH of 6.6 (see Test Case 2), continuously inhibiting periodontal pathogens.

[0146] The above clinical results confirm that the present invention effectively intervenes in oral diseases caused by "qi and yin deficiency, dryness and heat, and blood stasis" in diabetic patients through the combined effects of physical adhesion, chemical antibacterial action, and traditional Chinese medicine formulation. Without bioadhesive components (such as Comparative Example 4) or a pH-stabilized system (such as Comparative Example 1), the drug cannot remain at the lesion site for a long time or will degrade, making it difficult to achieve the clinical efficacy described in Table 5.

[0147] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A method for preparing a Chinese herbal toothpaste, characterized in that, The method forms a paste with physical shielding and chemical bacteriostatic functions by constructing a pH steady-state system and adding active components step by step, and comprises the following steps: S1, preparing a pH steady-state matrix: mixing deionized water and part of a humectant, adding a pH buffer to adjust the pH value of the system to be stable at 6.5-6.8, and then dissolving a sweetener; S2, glue preparation and paste preparation: dispersing a thickening agent to prepare a glue, sucking into a paste preparation machine, adding a broad-spectrum active extract and an abrasive, and homogeneously mixing under vacuum conditions to prepare an initial paste; S3, temperature reduction and fragrance adjustment: adding a surfactant and a fragrance, and reducing the paste temperature to below 45℃; S4, post-addition of a bioadhesion component: dispersing a bioadhesion repair extract in a reserved humectant to form a slurry, adding the slurry to the paste after temperature reduction, homogeneously mixing under the condition of closing the homogenizer and only opening a low-speed stirrer, and discharging to obtain the product. The broad-spectrum active extract is an extract rich in glycoside components prepared by hot reflux extraction. The bioadhesion repair extract is an extract rich in polysaccharide components prepared by low-temperature extraction and alcohol precipitation.

2. The method for preparing herbal toothpaste according to claim 1, characterized in that, The Chinese herbal toothpaste is prepared from raw materials comprising the following weight parts: humectant 220-360 parts; deionized water 300-400 parts; abrasive 200-300 parts; thickening agent 8-15 parts; surfactant 15-25 parts; broad-spectrum active extract 20-35 parts; bioadhesion repair extract 5-15 parts; pH buffer 2-5 parts; sweetener 3-6 parts; fragrance 6-12 parts.

3. The method of preparing the Chinese herbal toothpaste according to claim 2, characterized in that, The broad-spectrum active extract is prepared from the following weight parts of Chinese medicinal raw materials: honeysuckle 100-150 parts, radix scrophulariae 100-150 parts, anemarrhena 80-150 parts, radix rehmanniae 150-200 parts, salvia 100-150 parts, radix polygoni multiflori 100-150 parts, panax 100-150 parts, and radix astragali 150-200 parts.

4. The method of preparing the Chinese herbal toothpaste according to claim 3, characterized in that, The preparation steps of the broad-spectrum active extract are as follows: mixing the Chinese medicinal raw materials, adding water for hot reflux extraction, combining the extract and concentrating to a clear paste with a relative density of 1.18-1.20, and finally spray drying to obtain a dry powder; the inlet air temperature of the spray drying is 175-185℃.

5. The method of preparing the Chinese herbal toothpaste according to claim 2, wherein, The bioadhesion repair extract is prepared from the following weight parts of Chinese medicinal raw materials: white yam 90-150 parts, dendrobium 80-150 parts, and polygonatum 50-100 parts.

6. The method of preparing the Chinese herbal toothpaste according to claim 5, characterized in that, The preparation steps of the bioadhesion repair extract are as follows: (1) mixing the Chinese medicinal raw materials, adding water for low-temperature extraction at a temperature not higher than 70℃, collecting the extract and concentrating; (2) adding ethanol to the concentrated solution for alcohol precipitation, so that the final concentration of ethanol is 70%-75% v / v, and standing for precipitation; (3) collecting the precipitate, and vacuum freeze-drying or low-temperature spray drying to obtain a dry powder.

7. The method of preparing the Chinese herbal toothpaste according to claim 1, wherein, In the S1 step, the pH buffer is composed of citric acid monohydrate and trisodium citrate dihydrate, and the mass ratio of the two is (1.0-1.5):(1.5-3.0).

8. The method of preparing the Chinese herbal toothpaste according to claim 1, wherein, In the step S4, the reserved moisturizer is glycerin; the rotating speed of the low speed stirring is controlled at 20-30 rpm, and the mixing time is 10-15 minutes.

9. Use of the Chinese herbal toothpaste prepared by the preparation method of any one of claims 1-8 in the preparation of a product for treating or relieving oral diseases caused by diabetes.

10. Use according to claim 9, characterized in that, The oral diseases caused by diabetes include recurrent oral ulcer, gum redness and bleeding caused by periodontitis, tooth loosening, and xerostomia.

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