Chinese herbal medicine plant toothpaste and preparation method thereof
By using authentic Yunnan medicinal herbs and advanced preparation technology, this herbal toothpaste addresses the shortcomings of existing toothpastes in targeting various oral health issues, achieving multiple improvements in oral health and ensuring safety.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-01-20
- Publication Date
- 2026-04-10
AI Technical Summary
Existing toothpaste products have limited effectiveness in addressing various oral problems such as mouth ulcers, bleeding gums, periodontitis, and halitosis. They also suffer from issues such as confusing efficacy claims, lack of innovative formulations, and insufficient utilization of traditional Chinese herbal resources.
Using authentic Yunnan medicinal herbs such as Paris polyphylla root, wild mint, and Panax notoginseng root as core raw materials, combined with segmented extraction process and compound matrix excipients, through scientific formulation and advanced preparation process, we have formed a Chinese herbal toothpaste that enhances synergistic effects and addresses a variety of oral problems.
It significantly improves oral health, has the effects of clearing heat and detoxifying, reducing swelling and relieving pain, and anti-inflammatory and antibacterial properties. It is highly safe, conforms to the physiological environment of the oral cavity, has strong cleaning power, and is non-irritating.
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Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the technical field of oral care, in particular to a Chinese herbal plant toothpaste and a preparation method thereof. BACKGROUND
[0002] Toothpaste is an indispensable oral cleaning and care product in people's daily life. Its core function is to clean the surface of teeth by mechanical friction, and at the same time to improve the oral environment and maintain the health of teeth and periodontal tissues. With the improvement of living standards and the enhancement of health consciousness of Chinese residents, consumers' demand for toothpaste has changed from basic cleaning to multi-functional and targeted care. The demand for solving oral ulcer, gum bleeding, periodontal inflammation, halitosis, and gum swelling caused by heat is increasingly urgent.
[0003] According to the data of the fourth national oral health epidemiological survey, the situation of oral health in China is grim: the caries rate of 5-year-old children is as high as 70.9%, which is 5.8 percentage points higher than the last survey; the permanent tooth caries rate of 12-year-old children is 34.5%; the periodontal health rate of 65-74-year-old old people is only 9.3%. Due to factors such as increased life pressure, diversified eating habits, irregular work and rest, the incidence of oral ulcer, gum bleeding, periodontal inflammation, halitosis and other problems continues to rise, and shows a trend of youth. These oral problems not only affect daily diet and communication, but also may cause more serious oral diseases, and even affect the overall health.
[0004] The current toothpaste products on the market mainly focus on whitening, anti-caries, improving cold and acid sensitivity, and basic fresh breath as the core functions. Although they can meet the basic cleaning needs, the improvement effect on oral ulcer, gum bleeding, periodontal inflammation, and heat and other targeted oral problems is limited. Most products only stay at the level of commercial concept propaganda, and lack substantial efficacy support. The existing toothpaste has the following outstanding problems: first, the efficacy claim is chaotic. Some products arbitrarily claim "anti-inflammatory and analgesic", "hemostatic", "stabilizing loose teeth", and other effects beyond the scope of toothpaste functions, which are blurred with drugs and medical devices, seriously misleading consumers, and there is a certain safety hazard. Second, the formula design lacks innovation, mainly relying on simple compounding of chemical processing materials, without fully combining the synergistic effect of natural ingredients, especially lacking scientific application of precious Chinese herbal medicine resources. Third, the efficacy is weak in targeting, and it is difficult to solve multiple complex oral problems such as oral ulcer, inflammation, halitosis, and heat at the same time, which cannot meet the consumers' subdivided and diversified care needs.
[0005] From the current situation of the industry, although the toothpaste industry has been active in recent years, new products with new functions and new ingredients have emerged, and the R&D centers of Yunnan Baiyao, Dengkang and Weimesi have reached the international advanced level, but the industry as a whole still has the phenomenon of emphasizing marketing and neglecting R&D. Most enterprises are unwilling to invest sufficient funds in core formula R&D and efficacy verification in order to control costs and participate in price wars, especially in the R&D of products containing precious Chinese herbal ingredients, which lack the technical support of professional scientific research teams and old Chinese medicine doctors, resulting in insufficient product efficacy improvement and lack of innovation.
[0006] In the prior art, although some Chinese herbal toothpaste products are on the market, there are generally problems of random selection of raw materials, simple formula stacking and insufficient synergistic effect of effective ingredients, and the rich Chinese herbal resource advantage of China has not been fully utilized. As a major producing area of genuine Chinese herbal medicine, Yunnan has many kinds of precious medicinal materials such as Dian Chonglou, Wensan Sanqi and Dian Longdanca grass, which have unique effects such as clearing heat and detoxifying, relieving swelling and pain, promoting blood circulation and removing blood stasis. These medicinal materials have been proven in traditional medicine to have significant effects on inflammation, bleeding and swelling and pain, but they have not been scientifically and efficiently applied in toothpaste products.
[0007] In view of the defects of the prior art, the present application develops a Chinese herbal toothpaste. The formula of the toothpaste is based on the old Chinese medicine prescription left by our ancestor Li Shufu, which has been optimized by our three generations and finally formed a best combination of the prescription, and the efficacy and effect of the toothpaste are improved. SUMMARY
[0008] The present application provides a Chinese herbal toothpaste and a preparation method thereof, aiming at a toothpaste product based on genuine Chinese herbal resources, scientific formula and clear efficacy, through reasonable formula matching and advanced preparation process, fully playing the synergistic effect of Chinese herbal ingredients, specifically solving many oral problems such as oral ulcer, gum bleeding, periodontal inflammation, halitosis and heatiness, filling the gap of targeted efficacy toothpaste in the market, and meeting the needs of consumers for high-quality oral care products. At the same time, relevant national standards and industry standards must be strictly followed, the efficacy claim must be standardized, the safety and effectiveness of the product must be ensured, and the toothpaste industry must be developed towards naturalization, efficacy and standardization.
[0009] The present application is implemented as follows. A Chinese herbal toothpaste comprises core raw materials and matrix auxiliary materials. The core raw materials comprise, by weight, 10-20 parts of Chonglou root, 12-18 parts of wild mint, 5-15 parts of Sanqi root, 4-14 parts of dandelion, 3-10 parts of white peony root, 3-8 parts of honeysuckle, 3-8 parts of wild chrysanthemum, 3-8 parts of Dian Longdanca grass, 2-8 parts of Verbena, 2-8 parts of Lantana camara, 1-5 parts of gypsum and 0.1-0.5 parts of ox gall; The matrix excipients consist of compound abrasives, compound buffers, compound humectants, compound surfactants, compound preservatives, and synergists. The components are expressed as follows by weight percentage: compound abrasives 20%-30%, compound buffers 2%-5%, compound humectants 10%-20%, compound surfactants 1%-3%, compound preservatives 0.2%-0.5%, synergists 0.5%-2%, and the remainder is purified water.
[0010] Preferably, the core raw materials are all authentic Yunnan medicinal materials, including Paris polyphylla root selected from the dried rhizome of Paris polyphylla in Yunnan, Panax notoginseng root selected from the dried main root of Panax notoginseng in Wenshan, Gentiana scabra selected from the dried whole herb of the area in northwestern Yunnan at an altitude of 1800-2500m, wild mint selected from the wild dried above-ground parts of the central Yunnan plateau, and bezoar selected from the natural bezoar of locally raised yellow cattle in Yunnan with a purity of ≥95%.
[0011] Preferably, the synergist is tea saponin with a purity of ≥98%, and is treated with β-cyclodextrin inclusion complexation, with an inclusion complexation ratio of tea saponin:β-cyclodextrin = 1:2-3.
[0012] Preferably, the compound abrasive is composed of calcium phosphate and nano-silica in a mass ratio of 1:0.8-1.2, wherein the particle size of the nano-silica is 50-100nm.
[0013] Preferably, the compound buffer is composed of sodium pyrophosphate and sodium carbonate in a mass ratio of 1:0.5-0.8; the compound humectant is composed of sorbitol and glycerin in a mass ratio of 2:1-1.5.
[0014] Preferably, the compound surfactant is prepared by compounding sodium lauroyl sarcosinate and polysorbate-80 at a mass ratio of 1:0.3-0.6; the compound preservative is prepared by compounding sorbic acid and propylparaben at a mass ratio of 1:0.4-0.7.
[0015] This invention also proposes a method for preparing herbal toothpaste, comprising the following steps: S1. Raw material pretreatment: Remove impurities from each core raw material and ultrasonically clean it 2-3 times with purified water for 15-20 minutes each time, with an ultrasonic power of 300-400W; rinse the bezoar separately with sterile purified water 1-2 times and drain the water; dry all raw materials at a low temperature of 45-55℃ with forced air until the moisture content is ≤8%, and then coarsely pulverize them with a high-speed pulverizer. The 11 conventional medicinal materials are passed through a 100-200 mesh sieve, and the bezoar is passed through a 300 mesh sieve separately to obtain single-herb coarse powder for later use. S2. Segmented Extraction: ① Alcohol Extraction Process: Mix the crude powders of wild peppermint, honeysuckle, and wild chrysanthemum, add 8-12 times the amount of 70%-80% food-grade ethanol, place in a reflux extraction tank, control the extraction temperature at 75-85℃, and reflux extract twice. The first extraction lasts 2-2.5 hours, and the second extraction lasts 1.5-2 hours. Combine the two extracts, filter with a 100-mesh filter cloth, and concentrate the filtrate under reduced pressure to obtain an alcohol extract with a relative density of 1.10-1.15 (measured at 60℃), for later use; ② Water extraction process: Take the root of Paris polyphylla, root of Panax notoginseng, dandelion, white peony root, peony bark, Gentiana scabra, Verbena officinalis, Lycopus lucidus, and crude gypsum powder, mix them together, add 10-15 times the amount of purified water, place them in a multi-functional extraction tank, heat to boiling, and then maintain a simmering state to decoct twice. The first decoction is 2.5-3 hours, and the second decoction is 2-2.5 hours. Combine the two decoctions, filter them with a 120-mesh filter cloth, and concentrate the filtrate under reduced pressure to a water extract with a relative density of 1.20-1.25 (measured at 60℃) for later use. S3. Preparation of compound medicinal powder: Mix the alcohol extract and water extract evenly, transfer them to a freeze dryer, pre-freeze at -40℃ to -30℃ for 2-3 hours, then freeze-dry for 12-16 hours under vacuum degree ≤10Pa and shelf temperature 5-15℃ to obtain dried compound medicinal blocks; put the compound medicinal blocks into an ultra-micro pulverizer and perform ultra-micro pulverization under nitrogen protection, controlling the temperature inside the machine to ≤30℃ during the pulverization process, and pass the pulverized material through a 3000-3500 mesh sieve, collect the sieve material, add the pretreated bezoar crude medicinal powder, place it in a high-speed mixer, stir at 1500-2000r / min for 10-15 minutes, mix evenly to obtain compound medicinal powder for later use; S4. Preparation of matrix excipients: ① Weigh the compound abrasive and compound buffer according to the proportion, put them into a high-speed mixer, and dry mix for 15-20 minutes at a speed of 500-600 r / min to obtain a solid mixed excipient; ② Weigh the compound humectant, compound surfactant, compound preservative, and synergist according to the proportion, add purified water, place in a constant temperature stirring tank, control the temperature at 40-45℃, and stir at a speed of 300-400 r / min until completely dissolved to obtain a liquid mixed excipient; ③ Slowly add the liquid mixed excipient to the solid mixed excipient, and continue stirring for 30-40 minutes at a speed of 600-800 r / min and a temperature of 40-45℃ to form a uniform blank paste for later use; S5. Mixing and Filling: Slowly add the compound powder to the blank paste at a mass ratio of 3%-5%, controlling the stirring temperature at 38-42℃ and the speed at 800-1200r / min for 35-45 minutes to fully integrate the compound powder with the blank paste; then transfer the mixed paste to a vacuum degasser and degas for 20-30 minutes under a vacuum of -0.08MPa to -0.06MPa and a temperature of 35-40℃ to remove air bubbles from the paste; after degassing, fill the paste into toothpaste tubes in a cleanroom with a cleanliness level of 10,000, seal and inspect to obtain the finished product.
[0016] Preferably, the process parameters for vacuum concentration in step S2 are: vacuum degree -0.07MPa to -0.05MPa, concentration temperature 50-60℃, continuous stirring during concentration, and stirring speed 100-150r / min.
[0017] Preferably, the specific operation of ultrafine pulverization in S3 is as follows: first, the composite drug block is crushed into small pieces with a particle size ≤ 5mm, then put into the pulverization chamber of the ultrafine pulverizer, and nitrogen gas is introduced to replace the air in the chamber for 5-10 minutes, with a nitrogen flow rate of 0.5-1m³. 3 / h, then start the grinder, gradually increase the speed to 20000-25000r / min, grind for 20-30 minutes, stop the machine and continue to purge with nitrogen for 10-15 minutes to cool, then collect the powder.
[0018] Preferably, the compound powder in S5 is added by using a screw feeder at a uniform speed of 5-10 kg / h, while simultaneously turning on a shear emulsifier to assist in dispersion at a shearing speed of 3000-4000 r / min, with the shearing time synchronized with the stirring time.
[0019] The core ingredients of this invention are all selected from authentic medicinal herbs from Yunnan. Through scientific formulation, synergistic effects are achieved. The efficacy and synergistic effects of each ingredient are as follows: Paris root: Selected dried rhizomes of Paris polyphylla, containing active ingredients such as Paris saponins I, II, VI, and VII, which have the effects of clearing heat and detoxifying, reducing swelling and dispersing blood stasis, stopping bleeding and relieving pain. It has a significant repairing effect on oral ulcers and gingival bleeding. Wild mint: Selected from wild varieties in the central Yunnan plateau, it contains active ingredients such as menthol, flavonoids, and terpenes, with significantly higher content than ordinary mint. It has a stronger effect in dispelling wind-heat, clearing the head and eyes, and antibacterial and anti-inflammatory properties. It can not only freshen breath but also relieve gum swelling and pain, providing a cool taste to toothpaste. Panax notoginseng root: Selected dried main root of Panax notoginseng from Wenshan, containing Panax notoginseng saponins, Panax notoginseng polysaccharides and other ingredients, promote blood circulation, remove blood stasis, reduce swelling and relieve pain, and have anti-inflammatory and hemostatic effects. It works synergistically with Paris polyphylla root to enhance the repair and hemostatic effects of gum damage. Dandelion, honeysuckle, and wild chrysanthemum: Dandelion contains flavonoids and phenolic acids, which clear heat and detoxify, reduce swelling and dissipate nodules; honeysuckle contains chlorogenic acid and flavonoids, which disperse wind-heat and clear heat and detoxify; wild chrysanthemum contains volatile oils and terpenoids, which clear heat and detoxify, purge fire and calm the liver. The three ingredients work synergistically to enhance antibacterial and anti-inflammatory effects, and have a significant inhibitory effect on oral pathogens such as Porphyromonas gingivalis, Streptococcus mutans, and Staphylococcus aureus. White peony root, peony bark, verbena, and eupatorium: White peony root contains total paeoniflorin, which astringes yin, relieves pain, and has anti-inflammatory properties; peony bark contains paeonol and paeoniflorin, which clears heat, cools the blood, and promotes blood circulation; verbena contains verbenaside and volatile oil, which promotes blood circulation, removes blood stasis, and has anti-inflammatory and analgesic properties; eupatorium contains flavonoids and terpenoids, which promote blood circulation, remove blood stasis, and reduce swelling. The four ingredients work synergistically to improve gingival microcirculation, promote the healing of oral ulcers, and relieve periodontal inflammation. Yunnan Gentian: Selected from the dried whole herb of high-altitude areas in northwestern Yunnan, containing gentiopicrin, swertiamarin and other components, it clears heat and dries dampness, drains liver and gallbladder fire, enhances the effect of reducing stomach fire, and improves bad breath and swollen gums caused by excessive stomach fire. Gypsum: Contains calcium sulfate, calcium hydroxide and other ingredients. It clears heat and reduces fire, relieves irritability and thirst, astringes and stops bleeding, enhances antibacterial and tooth-strengthening effects, and works synergistically with other ingredients to reduce the growth rate of oral pathogens. Bezoar: Selected from natural bezoar from locally raised yellow cattle in Yunnan, with a purity of ≥95%, containing active ingredients such as bilirubin, bile acid, cholesterol, and taurine. It has the traditional effects of clearing heat and detoxifying, resolving phlegm and calming the nerves, and opening the orifices and refreshing the mind. Modern pharmacological research shows that it has significant anti-inflammatory, antibacterial, and mucosal repair promoting effects. It can enhance the repair ability of oral ulcer wounds, strengthen the antibacterial effect, and synergistically enhance the hemostatic and anti-inflammatory effects with Paris polyphylla root and Panax notoginseng root. The matrix excipients of this invention adopt a compound system that takes into account cleaning power, gentleness, stability, and synergistic effects. Compound abrasive: Calcium phosphate and nano silica are combined to ensure cleaning power while avoiding damage to tooth enamel. Nano silica can adsorb the effective ingredients of traditional Chinese medicine and prolong the duration of efficacy. Compound buffer: Sodium pyrophosphate and sodium carbonate are compounded to adjust the pH value of toothpaste to 6.5-7.5, which is in line with the oral physiological environment and enhances product stability; Compound moisturizer: Sorbitol and glycerin are compounded to make the toothpaste texture uniform and prevent the tube opening from drying out, while also promoting the integration of the effective ingredients of Chinese herbal medicine with the paste; Compound surfactant: Sodium lauroyl sarcosinate and polysorbate-80 are compounded together. It is mild and non-irritating, foams evenly, and enhances cleaning power while avoiding damage to the oral mucosa. Compound preservatives: Sorbic acid and propylparaben are combined, which have a broad antibacterial spectrum, low concentration, high safety, and extend the product's shelf life; Synergist tea saponin: After being encapsulated with β-cyclodextrin, its stability and bioavailability are improved. It has both natural surface activity and antibacterial effects, which can promote the penetration of the effective ingredients of traditional Chinese medicine into the oral mucosa, while enhancing the foaming and cleaning effects of toothpaste.
[0020] Compared with related technologies, the herbal toothpaste and its preparation method provided by this invention have the following beneficial effects: 1. Innovative Formula: It selects authentic Yunnan Chinese herbal medicines, especially Panax notoginseng root and Paris polyphylla, and adds authentic Yunnan gentian and wild mint. It extracts the effective components of each plant and adds bezoar. It is scientifically formulated to address various potential oral health problems and has certain preventive and protective effects on oral health, solving a variety of oral health issues. 2. Advanced technology: Innovative segmented extraction (alcohol extraction + water extraction) process to target the extraction of effective components with different polarities, combined with freeze drying and nitrogen-protected ultra-fine pulverization (3000-3500 mesh), which greatly improves the utilization rate and stability of effective components; the matrix excipient compounding system is optimized to balance cleaning power and gentleness. 3. Significant efficacy: Experimental data has verified that it has significant effects in clearing heat and reducing inflammation, preventing gum bleeding, preventing oral ulcers, cleaning teeth, removing dental plaque, and improving bad breath. It is also highly safe and non-irritating. Detailed Implementation
[0021] The present invention will be further described below with reference to specific embodiments.
[0022] Example 1: This invention provides a herbal toothpaste, comprising: Core ingredients (parts by weight): 12 parts wild mint, 15 parts Paris polyphylla root, 10 parts Panax notoginseng root, 8 parts dandelion, 6 parts white peony root, 5 parts peony bark, 5 parts honeysuckle, 5 parts wild chrysanthemum, 5 parts Yunnan gentian, 5 parts verbena, 5 parts eupatorium, 3 parts gypsum, 0.3 parts bezoar. Matrix excipients (by weight percentage): compound abrasive (calcium phosphate: nano silica = 1:1) 25%, compound buffer (sodium pyrophosphate: sodium carbonate = 1:0.6) 3%, compound humectant (sorbitol: glycerin = 2:1.2) 15%, compound surfactant (sodium lauroyl sarcosinate: polysorbate-80 = 1:0.4) 2%, compound preservative (sorbic acid: propylparaben = 1:0.5) 0.3%, synergist (tea saponin: β-cyclodextrin = 1:2.5) 1%, balance being purified water; The present invention provides a method for preparing a herbal toothpaste, comprising the following steps: (1) Raw material pretreatment: Remove impurities from each core raw material, and ultrasonically clean it 3 times with purified water for 18 minutes each time with an ultrasonic power of 350W; the bezoar is rinsed twice with sterile purified water and drained; all raw materials are dried at 50℃ with a low temperature blower until the moisture content is 6%, and coarsely pulverized with a high-speed pulverizer. The 11 conventional medicinal materials are passed through a 150-mesh sieve, and the bezoar is passed through a 300-mesh sieve to obtain single-herb coarse powder. (2) Segmented extraction: ① Alcohol extraction process: Mix the crude powders of wild peppermint, honeysuckle and wild chrysanthemum, add 10 times the amount of 75% food grade ethanol, place in a reflux extraction tank, and reflux extract twice at 80℃, the first time for 2.2 hours and the second time for 1.8 hours. Combine the extracts, filter with a 100-mesh filter cloth, and concentrate the filtrate under vacuum of -0.06MPa and 55℃ to an alcohol extract with a relative density of 1.12 (measured at 60℃); ② Water extraction process: Mix the crude powders of the remaining 9 core raw materials, add 12 times the amount of purified water, boil in a multi-functional extraction tank and then simmer twice, the first time for 2.8 hours and the second time for 2.2 hours. Combine the decoctions, filter with a 120-mesh filter cloth, and concentrate the filtrate under vacuum of -0.06MPa and 55℃ to an water extract with a relative density of 1.22 (measured at 60℃). (3) Preparation of compound powder: The alcohol extract and water extract were mixed evenly and transferred to a freeze dryer. The mixture was pre-frozen at -35°C for 2.5 hours, and then freeze-dried at a vacuum of 8 Pa and a shelf temperature of 10°C for 14 hours to obtain compound powder blocks. The powder blocks were crushed to ≤5 mm and fed into an ultrafine pulverizer. Nitrogen gas was introduced to replace the air for 8 minutes (flow rate 0.8 m³ / min). 3 / h), start the pulverizer and gradually increase the speed to 22000r / min, pulverize for 25 minutes, continue to cool with nitrogen for 12 minutes, pass through a 3200 mesh sieve, collect the powder, add the pretreated bezoar coarse powder, place in a high-speed mixer, stir at 1800r / min for 12 minutes, and after mixing evenly, obtain the compound powder; (4) Preparation of matrix excipients: ① Weigh the compound abrasive and compound buffer, dry mix them in a high-speed mixer at 550 r / min for 18 minutes to obtain solid mixed excipients; ② Weigh the compound humectant, compound surfactant, compound preservative and synergist, add purified water, and stir in a constant temperature stirring tank at 42℃ and 350 r / min until completely dissolved to obtain liquid mixed excipients; ③ Slowly add the liquid mixed excipients to the solid mixed excipients, stir at 650 r / min and 42℃ for 35 minutes to form a blank paste; (5) Mixing and filling: The compound powder is added to the blank paste at a uniform rate of 4% by mass using a screw feeder (feeding speed 8kg / h). At the same time, the shear emulsifier is turned on at 3500r / min to assist dispersion. The temperature is controlled at 40℃ and the stirring speed is 1000r / min. The mixture is stirred for 40 minutes. Then it is transferred to a vacuum degasser and degassed at -0.07MPa and 38℃ for 25 minutes. The paste is filled, sealed and inspected in a Class 10,000 cleanroom to obtain the finished product.
[0023] Example 2: This invention provides a herbal toothpaste, comprising: Core ingredients (by weight): 12 parts wild mint, 10 parts Paris polyphylla root, 5 parts Panax notoginseng root, 4 parts dandelion, 3 parts white peony root, 3 parts peony bark, 3 parts honeysuckle, 3 parts wild chrysanthemum, 3 parts Yunnan gentian, 2 parts verbena, 2 parts eupatorium, 1 part gypsum, 0.1 parts bezoar. Matrix excipients (by weight percentage): compound abrasive (calcium phosphate: nano silica = 1:0.8) 20%, compound buffer (sodium pyrophosphate: sodium carbonate = 1:0.5) 2%, compound humectant (sorbitol: glycerin = 2:1) 10%, compound surfactant (sodium lauroyl sarcosinate: polysorbate-80 = 1:0.3) 1%, compound preservative (sorbic acid: propylparaben = 1:0.4) 0.2%, synergist (tea saponin: β-cyclodextrin = 1:2) 0.5%, balance being purified water; The present invention provides a method for preparing a herbal toothpaste, comprising the following steps: (1) Raw material pretreatment: Remove impurities from each core raw material, and ultrasonically clean it twice with purified water for 15 minutes each time with an ultrasonic power of 300W; quickly rinse the bezoar with sterile purified water once and drain it; dry all raw materials at 45℃ with a low temperature blower until the moisture content is 8%; coarsely pulverize the conventional medicinal materials and pass them through a 100-mesh sieve, and pass the bezoar separately through a 300-mesh sieve to obtain single-herb coarse powder. (2) Segmented extraction: ① Alcohol extraction process: Mix the crude powders of wild peppermint, honeysuckle and wild chrysanthemum, add 8 times the amount of 70% ethanol, reflux at 75℃ twice, the first time for 2 hours and the second time for 1.5 hours, filter with 100 mesh filter cloth, and concentrate the filtrate under vacuum at -0.05MPa and 50℃ to a relative density of 1.10 (measured at 60℃) to obtain an alcohol extract; ② Water extraction process: Mix the crude powders of the remaining 9 core raw materials, add 10 times the amount of purified water, boil and then simmer twice, the first time for 2.5 hours and the second time for 2 hours, filter with 120 mesh filter cloth, and concentrate the filtrate under vacuum at -0.05MPa and 50℃ to a relative density of 1.20 (measured at 60℃) to obtain an water extract; (3) Preparation of compound powder: The alcohol extract and water extract were mixed, pre-frozen at -40℃ for 2 hours, and freeze-dried at a vacuum of 10Pa and a shelf temperature of 5℃ for 12 hours to obtain compound powder blocks; the blocks were crushed to ≤5mm and purged with nitrogen in an ultrafine pulverizer for 5 minutes (flow rate 0.5m). 3 / h), grind at 20000r / min for 20 minutes, cool with nitrogen for 10 minutes, pass through a 3000-mesh sieve, collect the powder, add coarse bezoar powder, stir at 1500r / min in a high-speed mixer for 10 minutes to obtain compound powder; (4) Preparation of matrix excipients: ① The compound abrasive and the compound buffer are dry-mixed in a high-speed mixer at 500 r / min for 15 minutes to obtain a solid compound excipient; ② The compound humectant, compound surfactant, compound preservative and synergist are added to purified water and stirred at 40℃ and 300 r / min to dissolve them to obtain a liquid compound excipient; ③ The liquid excipient is added to the solid excipient and stirred at 600 r / min and 40℃ for 30 minutes to form a blank paste; (5) Mixing and filling: The compound powder is added at a mass ratio of 3% by the screw feeder (feeding speed 5kg / h), and the dispersion is assisted by the shear emulsifier at 3000r / min. The mixture is stirred at 38℃ and 800r / min for 35 minutes. The vacuum degasser is degassed at -0.06MPa and 35℃ for 20 minutes. The finished product is filled, sealed and inspected in a Class 10,000 cleanroom.
[0024] Example 3 This invention provides a herbal toothpaste, comprising: Core ingredients (parts by weight): 18 parts wild mint, 20 parts Paris polyphylla root, 15 parts Panax notoginseng root, 14 parts dandelion, 10 parts white peony root, 8 parts peony bark, 8 parts honeysuckle, 8 parts wild chrysanthemum, 8 parts Yunnan gentian, 8 parts verbena, 8 parts eupatorium, 5 parts gypsum, 0.5 parts bezoar. Matrix excipients (by weight percentage): compound abrasive (calcium phosphate: nano silica = 1:1.2) 30%, compound buffer (sodium pyrophosphate: sodium carbonate = 1:0.8) 5%, compound humectant (sorbitol: glycerin = 2:1.5) 20%, compound surfactant (sodium lauroyl sarcosinate: polysorbate-80 = 1:0.6) 3%, compound preservative (sorbic acid: propylparaben = 1:0.7) 0.5%, synergist (tea saponin: β-cyclodextrin = 1:3) 2%, balance being purified water; Preparation method: (1) Raw material pretreatment: Remove impurities from each core raw material, and ultrasonically clean it 3 times with purified water for 20 minutes each time with an ultrasonic power of 400W; quickly rinse the bezoar twice with sterile purified water and drain it; dry all raw materials at 55℃ with a low temperature blower until the moisture content is 5%; coarsely pulverize the conventional medicinal materials and pass them through a 200-mesh sieve, and pass the bezoar separately through a 300-mesh sieve to obtain single-herb coarse powder. (2) Segmented extraction: ① Alcohol extraction process: Mix the crude powders of wild peppermint, honeysuckle and wild chrysanthemum, add 12 times the amount of 80% ethanol, reflux at 85℃ twice, the first time for 2.5 hours and the second time for 2 hours, filter with 100 mesh filter cloth, and concentrate the filtrate under vacuum of -0.07MPa and 60℃ to a relative density of 1.15 (measured at 60℃) to obtain an alcohol extract; ② Water extraction process: Mix the crude powders of the remaining 9 core raw materials, add 15 times the amount of purified water, boil and then simmer twice, the first time for 3 hours and the second time for 2.5 hours, filter with 120 mesh filter cloth, and concentrate the filtrate under vacuum of -0.07MPa and 60℃ to a relative density of 1.25 (measured at 60℃) to obtain a water extract; (3) Preparation of compound powder: The alcohol extract and the water extract were mixed, pre-frozen at -30℃ for 3 hours, and freeze-dried at a vacuum of 5 Pa and a shelf temperature of 15℃ for 16 hours to obtain compound powder blocks; the blocks were crushed to ≤5 mm and purged with nitrogen in an ultra-micro pulverizer for 10 minutes (flow rate 1 m³ / min). 3 The powder was pulverized at 25,000 r / min for 30 minutes, cooled with nitrogen for 15 minutes, passed through a 3500-mesh sieve, collected, and mixed with coarse bezoar powder. The mixture was then stirred at 2000 r / min for 15 minutes in a high-speed mixer to obtain the compound powder. (4) Preparation of matrix excipients: ① The compound abrasive and the compound buffer are dry-mixed in a high-speed mixer at 600 r / min for 20 minutes to obtain a solid mixed excipient; ② The compound humectant, compound surfactant, compound preservative and synergist are added to purified water and stirred at 45℃ and 400 r / min to dissolve them to obtain a liquid mixed excipient; ③ The liquid excipient is added to the solid excipient and stirred at 800 r / min and 45℃ for 40 minutes to form a blank paste; (5) Mixing and filling: The compound powder is added at a mass ratio of 5% by the screw feeder (feeding speed 10kg / h), and the dispersion is assisted by the shear emulsifier at 4000r / min. The mixture is stirred at 42℃ and 1200r / min for 45 minutes. The vacuum degasser is degassed at -0.08MPa and 40℃ for 30 minutes. The finished product is filled, sealed and inspected in a Class 10,000 cleanroom.
[0025] Detection experiments and result analysis 1. Experimental subjects The toothpaste prepared in Examples 1-3, commercially available ordinary herbal toothpaste (control group 1), and commercially available functional gum-protecting toothpaste (control group 2) were used, with 3 parallel samples in each group.
[0026] 2. Experimental Basis The tests were conducted in accordance with GB / T 8372-2017 "Toothpaste", QB / T 2966-2014 "Efficacy Toothpaste", and WS / T 326 series "Evaluation of Toothpaste Efficacy" standards.
[0027] 3. Experimental Items and Results 3.1 Antibacterial effect test (incubation for 24 hours)
[0028] 3.2 Oral Ulcer Repair Experiment (60 patients with recurrent oral ulcers were randomly divided into groups of 12 each, and brushed their teeth twice a day)
[0029] 3.3 Gingival health improvement experiment (60 patients with gingival bleeding and periodontal inflammation were randomly divided into groups of 12 each, and the treatment lasted for 14 consecutive days)
[0030] 3.4 Plaque Removal and Halitosis Improvement Experiment
[0031] 3.5 Safety Testing All test samples met the requirements of GB / T 8372-2017 standard. Skin irritation test (repeated contact) showed no irritation, oral mucosa irritation test showed no irritation, and no allergic reactions were observed.
[0032] 4. Results Analysis (1) Antibacterial effect: The antibacterial rate of the three oral pathogens in Example 1 exceeded 97%, which was significantly higher than that of other groups, indicating that its formula ratio and preparation process can give full play to the synergistic antibacterial effect of traditional Chinese medicine. (2) Oral ulcer repair: The average ulcer healing time in Example 1 was only 3.1 days, and the pain relief time was 12.5 hours, demonstrating the advantages of rapid wound repair and pain relief; (3) Improved gum health: After 14 days of use in Example 1, the incidence of gum bleeding was only 6.7% and the periodontal inflammation score was 0.5, indicating that it has significant effects in protecting gums, stopping bleeding, and reducing inflammation; (4) Cleaning and halitosis improvement: Example 1 showed a plaque removal rate of 95.6% and a VSC content of 32 ppb 4 hours after brushing, indicating strong cleaning power and long-lasting fresh breath effect; (5) Comprehensive comparison: All efficacy indicators of Example 1 are the best, proving that the formulation optimization, selection of authentic raw materials and advanced preparation process of the present invention can maximize the efficacy of the product and have significant progress compared with existing products.
[0033] The above embodiments are only used to illustrate the technical solutions of the present invention, and are not intended to limit the scope of protection of the invention. Obviously, the described embodiments are only some embodiments of the present invention, not all embodiments. Based on these embodiments, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention. Although the present invention has been described in detail with reference to the above embodiments, those skilled in the art can still combine, add, delete, or otherwise adjust the features of the various embodiments of the present invention according to the circumstances without conflict or creative effort, thereby obtaining different technical solutions that do not fundamentally depart from the concept of the present invention. These technical solutions also fall within the scope of protection of the present invention.
Claims
1. A herbal toothpaste, characterized in that, Including core raw materials and matrix additives: The core ingredients, by weight, include: 10-20 parts of Paris polyphylla root, 12-18 parts of wild peppermint, 5-15 parts of Panax notoginseng root, 4-14 parts of dandelion, 3-10 parts of white peony root, 3-8 parts of peony bark, 3-8 parts of honeysuckle, 3-8 parts of wild chrysanthemum, 3-8 parts of Yunnan gentian, 2-8 parts of verbena, 2-8 parts of eupatorium, 1-5 parts of gypsum, and 0.1-0.5 parts of bezoar. The matrix excipients consist of compound abrasives, compound buffers, compound humectants, compound surfactants, compound preservatives, and synergists. The components are expressed as follows by weight percentage: compound abrasives 20%-30%, compound buffers 2%-5%, compound humectants 10%-20%, compound surfactants 1%-3%, compound preservatives 0.2%-0.5%, synergists 0.5%-2%, and the remainder is purified water.
2. The herbal toothpaste according to claim 1, characterized in that, The core raw materials are all authentic Yunnan medicinal herbs. Among them, the root of Paris polyphylla is selected from the dried rhizome of Paris polyphylla in Yunnan, the root of Panax notoginseng is selected from the dried main root of Panax notoginseng in Wenshan, the whole herb of Gentiana scabra is selected from the dried herb of the area in northwestern Yunnan at an altitude of 1800-2500m, the wild mint is selected from the wild dried above-ground parts of the central plateau of Yunnan, and the bezoar is selected from the natural bezoar of the yellow cattle raised in Yunnan, with a purity of ≥95%.
3. The herbal toothpaste according to claim 1, characterized in that, The synergist is tea saponin with a purity of ≥98%, and it is encapsulated by β-cyclodextrin with an encapsulation ratio of tea saponin:β-cyclodextrin = 1:2-3.
4. The herbal toothpaste according to claim 1, characterized in that, The compound abrasive is composed of calcium phosphate and nano silica in a mass ratio of 1:0.8-1.2, wherein the nano silica has a particle size of 50-100 nm.
5. The herbal toothpaste according to claim 1, characterized in that, The compound buffer is composed of sodium pyrophosphate and sodium carbonate in a mass ratio of 1:0.5-0.8; the compound moisturizer is composed of sorbitol and glycerin in a mass ratio of 2:1-1.
5.
6. The herbal toothpaste according to claim 1, characterized in that, The compound surfactant is prepared by compounding sodium lauroyl sarcosinate and polysorbate-80 at a mass ratio of 1:0.3-0.6; the compound preservative is prepared by compounding sorbic acid and propylparaben at a mass ratio of 1:0.4-0.
7.
7. A method for preparing a herbal toothpaste as described in any one of claims 1-6, characterized in that, Includes the following steps: S1. Raw material pretreatment: Remove impurities from each core raw material and ultrasonically clean it 2-3 times with purified water for 15-20 minutes each time, with an ultrasonic power of 300-400W; rinse the bezoar separately with sterile purified water 1-2 times and drain the water; dry all raw materials at a low temperature of 45-55℃ with forced air until the moisture content is ≤8%, and then coarsely pulverize them with a high-speed pulverizer. The 11 conventional medicinal materials are passed through a 100-200 mesh sieve, and the bezoar is passed through a 300 mesh sieve separately to obtain single-herb coarse powder for later use. S2. Segmented Extraction: ① Alcohol Extraction Process: Mix the crude powders of wild peppermint, honeysuckle, and wild chrysanthemum, add 8-12 times the amount of 70%-80% food-grade ethanol, place in a reflux extraction tank, control the extraction temperature at 75-85℃, and reflux extract twice. The first extraction lasts 2-2.5 hours, and the second extraction lasts 1.5-2 hours. Combine the two extracts, filter with a 100-mesh filter cloth, and concentrate the filtrate under reduced pressure to an alcohol extract with a relative density of 1.10-1.15 for later use; ② Water extraction process: Take the root of Paris polyphylla, root of Panax notoginseng, dandelion, white peony root, peony bark, Gentiana scabra, Verbena officinalis, Lycopus lucidus, and crude gypsum powder, mix them together, add 10-15 times the amount of purified water, place them in a multi-functional extraction tank, heat to boiling, and then maintain a simmering state to decoct twice. The first decoction is 2.5-3 hours, and the second decoction is 2-2.5 hours. Combine the two decoctions, filter them with a 120-mesh filter cloth, and concentrate the filtrate under reduced pressure to a water extract with a relative density of 1.20-1.25 for later use. S3. Preparation of compound medicinal powder: Mix the alcohol extract and water extract evenly, transfer them to a freeze dryer, pre-freeze at -40℃ to -30℃ for 2-3 hours, then freeze-dry for 12-16 hours under vacuum degree ≤10Pa and shelf temperature 5-15℃ to obtain dried compound medicinal blocks; put the compound medicinal blocks into an ultra-micro pulverizer and perform ultra-micro pulverization under nitrogen protection, controlling the temperature inside the machine to ≤30℃ during the pulverization process, and pass the pulverized material through a 3000-3500 mesh sieve, collect the sieve material, add the pretreated bezoar crude medicinal powder, place it in a high-speed mixer, stir at 1500-2000r / min for 10-15 minutes, mix evenly to obtain compound medicinal powder for later use; S4. Preparation of matrix excipients: ① Weigh the compound abrasive and compound buffer according to the proportion, put them into a high-speed mixer, and dry mix for 15-20 minutes at a speed of 500-600 r / min to obtain a solid mixed excipient; ② Weigh the compound humectant, compound surfactant, compound preservative, and synergist according to the proportion, add purified water, place in a constant temperature stirring tank, control the temperature at 40-45℃, and stir at a speed of 300-400 r / min until completely dissolved to obtain a liquid mixed excipient; ③ Slowly add the liquid mixed excipient to the solid mixed excipient, and continue stirring for 30-40 minutes at a speed of 600-800 r / min and a temperature of 40-45℃ to form a uniform blank paste for later use; S5. Mixing and Filling: Slowly add the compound powder to the blank paste at a mass ratio of 3%-5%, controlling the stirring temperature at 38-42℃ and the speed at 800-1200r / min for 35-45 minutes to fully integrate the compound powder with the blank paste; then transfer the mixed paste to a vacuum degasser and degas for 20-30 minutes under a vacuum of -0.08MPa to -0.06MPa and a temperature of 35-40℃ to remove air bubbles from the paste; after degassing, fill the paste into toothpaste tubes in a cleanroom with a cleanliness level of 10,000, seal and inspect to obtain the finished product.
8. The herbal toothpaste according to claim 7, characterized in that, The process parameters for vacuum concentration in step S2 are: vacuum degree -0.07MPa to -0.05MPa, concentration temperature 50-60℃, continuous stirring during concentration, and stirring speed 100-150r / min.
9. The herbal toothpaste according to claim 7, characterized in that, The specific operation of ultrafine pulverization in S3 is as follows: First, the composite drug block is crushed into small pieces with a particle size ≤ 5mm, then put into the pulverization chamber of the ultrafine pulverizer, and nitrogen gas is introduced to replace the air in the chamber for 5-10 minutes at a flow rate of 0.5-1m³. 3 / h, then start the grinder, gradually increase the speed to 20000-25000r / min, grind for 20-30 minutes, stop the machine and continue to purge with nitrogen for 10-15 minutes to cool, then collect the powder.
10. The herbal toothpaste according to claim 7, characterized in that, The compound powder in S5 is added in the following manner: a screw feeder is used to add the powder at a uniform speed of 5-10 kg / h, while a shear emulsifier is turned on to assist in dispersion at a shearing speed of 3000-4000 r / min, and the shearing time is synchronized with the stirring time.