Toothpaste composition with effects of strengthening teeth and strengthening teeth as well as preparation method and application of toothpaste composition

Abstract

The invention provides a toothpaste composition with tooth strengthening and strengthening effects as well as a preparation method and application thereof, and relates to the technical field of traditional Chinese medicines. The toothpaste composition comprises active components and auxiliary materials, wherein the active components comprise halite, gypsum, fructus psoraleae, pepper, radix angelicae, mint, eclipta alba, divaricate saposhnikovia root, asarum, radix aconiti lateralis praeparata and compound probiotic freeze-dried powder; the compound probiotic freeze-dried powder consists of kluyveromyces marxianus freeze-dried powder and lactobacillus salivarius freeze-dried powder; the auxiliary material comprises a compound bacteriostatic agent; the compound bacteriostatic agent is prepared from chamomile blue and a tussilago farfara extract. The toothpaste composition prepared by respectively extracting the raw materials through a specific preparation method is not only good in stability, but also capable of remarkably improving various inflammations and bleeding of periodontal diseases, improving the tooth health problem of users with dentin sensitivity and meeting the requirements of various users.

Description

Technical Field

[0001] The present invention relates to the technical field of traditional Chinese medicines, and in particular to a toothpaste composition with the effects of strengthening and strengthening teeth, a preparation method and an application thereof. Background Art

[0002] Teeth are the hardest organs in the human body. In addition to performing functions such as cutting and chewing, they also play a role in maintaining facial appearance and assisting pronunciation. As the human body ages, some basic problems will arise in the teeth, such as periodontal disease and dentin hypersensitivity.

[0003] Periodontal disease refers to diseases of the tooth-supporting tissues. It can be categorized into two main types: gingivitis, which affects only the gums, and periodontitis, which affects deeper periodontal tissues such as the periodontal ligament, alveolar bone, and cementum. Periodontal disease is a common oral condition and one of the leading causes of tooth loss in adults. It is also a major oral disease that poses a threat to both dental health and overall health. Early symptoms of periodontal disease are often overlooked, leading to long-term, chronic infection and recurrent inflammation of the periodontal tissues. This not only impairs the function of the oral masticatory system but also seriously impacts overall health.

[0004] Dentin hypersensitivity (DH), also known as hypersensitive dentin, is a common and frequently occurring condition in dentistry. It refers to a brief, sharp pain in the exposed dentin caused by external stimuli such as temperature, chemical, mechanical, or osmotic pressure. This pain cannot be attributed to any other tooth defect or pathology. DH can be caused by a variety of pathological and physiological factors, including abrasion, gum recession, improper brushing techniques, and excessive intake of acidic foods, leading to enamel or cementum loss and dentin exposure.

[0005] Currently, there are many clinical methods for treating dentin hypersensitivity or periodontal disease, but local application of toothpaste containing certain special functional ingredients is the first choice. There are many toothpastes for strengthening and strengthening teeth in the prior art.

[0006] For example, Chinese patent CN114469831A provides a tooth-strengthening toothpaste and its preparation method, which is made from traditional Chinese medicine ingredients; wherein the traditional Chinese medicine ingredients include 30 grams of Caulis Ternifolia, 30 grams of Corydalis yanhusuo, 8 grams of Asarum sieboldii, 15 grams of Saposhnikovia divaricata, 15 grams of Euryale ferox, 30 grams of Coix lachryma-jobi, 3 grams of Cardamomum villosum, 8 grams of Menthol, 8 grams of Angelica dahurica, 6 grams of Clove, 8 grams of Zanthoxylum bungeanum, 6 grams of Borneolum, 30 grams of Lycium bark, 30 grams of Psoralea corylifolia, 15 grams of Eclipta prostrata, 10 grams of Rhizoma Anemarrhenae, 30 grams of Talc, 30 grams of Green Salt, 30 grams of Gypsum, and 10 grams of Perilla frutescens. This toothpaste has good clinical efficacy for various symptoms such as gingival atrophy caused by periodontitis, periodontal pain after tooth extraction, bleeding from the gums, and loose teeth.

[0007] Chinese patent application CN117771311A discloses a traditional Chinese medicine tooth-strengthening tooth powder for treating dental diseases and its preparation method. The powder comprises the following raw materials in parts by weight: 3-8g of green salt, 3-8g of gypsum, 2-8g of psoralea corylifolia, 2-6g of Zanthoxylum bungeanum, 2-6g of Angelica dahurica, 2-8g of Chinese gallnut, 2-8g of mint, 3-8g of Eclipta prostrata, 3-8g of Saposhnikovia divaricata, 2-6g of Asarum, processed Aconite root, 2-6g of Cyperus rotundus, 3-6g of pearl, and 2-4g of oyster. The invention utilizes a combination of different Chinese medicinal materials to prepare the powder, omitting the step of adding abrasives such as calcium carbonate, thus saving manufacturing steps and being environmentally friendly and healthy. However, none of the above technical solutions address the efficacy of treating oral problems such as dentin hypersensitivity.

[0008] A toothpaste recipe that has been made public includes green salt, gypsum, psoralea corylifolia, Sichuan peppercorns, angelica dahurica, mint, Eclipta prostrata, Saposhnikovia divaricata, and Asarum. The recipe involves grinding the ingredients into a fine powder and sealing them for later use. However, the extraction process still needs to be improved.

[0009] Based on this, a new toothpaste for strengthening and protecting teeth was developed, and the raw materials, auxiliary materials and extraction process were improved to meet the needs of more users, with good efficacy and high stability. Summary of the Invention

[0010] In view of the above problems, the present invention provides a toothpaste composition with the effects of strengthening and strengthening teeth and a preparation method thereof.

[0011] To achieve the above object, the technical solution adopted by the present invention is as follows: On the one hand, the present invention provides a toothpaste composition with the effects of strengthening and invigorating teeth, comprising active components and excipients, wherein the active components are composed of green salt, gypsum, psoralea corylifolia, Zanthoxylum bungeanum, Angelica dahurica, mint, Eclipta prostrata, Saposhnikovia divaricata, Asarum, Aconite root and composite probiotic freeze-dried powder; the composite probiotic freeze-dried powder is composed of Kluyveromyces marxianus freeze-dried powder and Lactobacillus salivarius freeze-dried powder; the excipients include a composite antibacterial agent; and the composite antibacterial agent is composed of azulene and coltsfoot flower extracts.

[0012] Preferably, the mass ratio of the active ingredient to the excipient is 1-10:90-99.

[0013] Preferably, the mass of the composite probiotic freeze-dried powder accounts for 15%-30% of the mass of the active component.

[0014] Preferably, the mass ratio of the freeze-dried Kluyveromyces marxianus powder to the freeze-dried Lactobacillus salivarius powder is 1-3:1.

[0015] Further preferably, the mass ratio of the Kluyveromyces marxianus freeze-dried powder to the Lactobacillus salivarius freeze-dried powder is 2:1.

[0016] Preferably, the preparation method of the composite probiotic freeze-dried powder is: activating and culturing Kluyveromyces marxianus to obtain a Kluyveromyces marxianus base stock solution, freeze-drying and dehydrating the solution to obtain Kluyveromyces marxianus freeze-dried powder, and then mixing the solution with Lactobacillus salivarius freeze-dried powder in proportion to obtain the composite probiotic powder.

[0017] Preferably, the mass of the composite antibacterial agent is 5-10% of the total mass of the excipients.

[0018] Preferably, the active ingredient is composed of the following raw materials in parts by mass: 10-20 parts of green salt, 10-20 parts of gypsum, 8-15 parts of psoralea corylifolia, 2-7 parts of Zanthoxylum bungeanum, 2-7 parts of angelica dahurica, 2-7 parts of mint, 5-10 parts of Eclipta prostrata, 5-10 parts of Saposhnikovia divaricata, 2-7 parts of Asarum, 0.1-2 parts of roasted aconite root, and 5-32 parts of compound probiotic freeze-dried powder; Preferably, the active ingredient is composed of the following raw materials in parts by mass: 13-17 parts of green salt, 13-17 parts of gypsum, 11-13 parts of psoralea corylifolia, 4-6 parts of Zanthoxylum bungeanum, 4-6 parts of angelica dahurica, 4-6 parts of mint, 5-8 parts of Eclipta prostrata, 5-8 parts of siler, 4-6 parts of asarum, 0.5-1.2 parts of roasted aconite root, and 5-25 parts of compound probiotic freeze-dried powder; Further preferably, the active component is composed of the following raw materials in parts by mass: 15 parts of green salt, 15 parts of gypsum, 12 parts of psoralea corylifolia, 4.5 parts of Sichuan pepper, 4.5 parts of angelica dahurica, 4.5 parts of mint, 7.5 parts of Eclipta prostrata, 7.5 parts of Saposhnikovia divaricata, 4.5 parts of Asarum, 1 part of cooked aconite root and 20 parts of compound probiotic freeze-dried powder.

[0019] Among them, green salt is used to treat hematuria, hematemesis, bleeding from the teeth and tongue, red and painful eyes, cataracts, and toothache. It can be decocted into a decoction or made into pills or powders; for external use, it can be ground into a powder and used for brushing teeth or dissolved in water to rinse the mouth and eyes.

[0020] Gypsum: It is a mineral containing hydrated calcium sulfate (CaSO4·2H2O). It has the effects of healing wounds, promoting tissue regeneration, absorbing moisture, and stopping bleeding. It is mainly used for hemostasis and tissue regeneration of gums. It can also effectively remove tartar when used in tooth cleaning powder.

[0021] Psoralea corylifolia is used to treat impotence due to kidney deficiency, soreness and coldness in the waist and knees, spermatorrhea, enuresis, and frequent urination due to kidney deficiency. It is also used to treat early morning diarrhea caused by spleen and kidney yang deficiency. It is also used to treat asthma and cough due to kidney deficiency.

[0022] Zanthoxylum bungeanum warms the middle and dispels cold, removes dampness, relieves pain, kills insects, and detoxifies fishy smell. It is used to treat indigestion, cold pain in the heart and abdomen, vomiting, belching, cough and shortness of breath, wind-cold-dampness arthritis, diarrhea, dysentery, hernia pain, toothache, ascariasis, pinworm disease, vaginal itching, and scabies.

[0023] Angelica dahurica, whose roots are used as medicine, has the properties of dispelling dampness, dispelling pus and promoting tissue regeneration, promoting blood circulation and relieving pain. It is primarily used to treat colds, headaches, rhinitis, and toothaches. It also treats leucorrhea, painful boils, and swellings. It is also used as a spice. Some provinces in northern China cultivate it, mostly for local consumption, with a small amount exported. It typically grows under forests, along forest edges, along streams, in thickets, and in valley grasslands.

[0024] Mint: It mainly contains peppermint oil, menthol, menthone, isomenthone, rosmarinic acid and other ingredients, which can invigorate the stomach, dispel wind, eliminate phlegm, promote bile secretion, and resist spasms. It can improve fever, sore throat, swelling and pain, and eliminate headaches, toothaches, and nausea. Adding mint to tooth powder can not only make the powder have a certain fragrance, leave a fragrance in the mouth, and eliminate bad breath, but also has a certain bactericidal function.

[0025] Eclipta prostrata: The whole herb is used medicinally, and has the effects of astringing, cooling blood, stopping bleeding, and nourishing the liver and kidneys. It is used to strengthen teeth, reduce swelling and stop bleeding.

[0026] Saposhnikovia divaricata: It has the effects of sweating, expectorant, wind-dispelling, diaphoretic and analgesic, and is used to relieve toothache.

[0027] Asarum: It has the effects of dispelling wind, dispersing cold, promoting water circulation and opening the orifices. It is also effective in treating wind-cold headache, sinusitis, toothache, phlegm-induced cough, rheumatism and pain.

[0028] Pao Fu Zi is the processed product of the dried root bark of Aconitum carmichaeli Debx. of the Ranunculaceae family; it tastes pungent and sweet, and is hot in nature; it enters the heart, spleen, and kidney meridians; it can restore yang and rescue adverse conditions, replenish fire and enhance yang.

[0029] Preferably, the mass ratio of the azulene indigo plant extract to the coltsfoot flower extract is 3-8:5-10.

[0030] Further preferably, the mass ratio of the azulene indigo and coltsfoot flower extracts is 5:6.

[0031] Preferably, the preparation method of the coltsfoot flower extract is: The coltsfoot flower is crushed, mixed with 45wt%-65wt% alcohol solution, and ultrasonically extracted for 10-30min. Then, the concentration of the alcohol solution is adjusted to 70wt%-80wt%, ultrasonically extracted for a second time for 10-30min, and the alcohol extracts are combined to obtain the product.

[0032] Preferably, the ultrasonic parameters are: power 300-400w, temperature 50-55°C.

[0033] Preferably, the secondary ultrasound parameters are: power 200-300w, temperature 65-75°C.

[0034] Preferably, the alcohol solution is an ethanol solution.

[0035] Preferably, the preparation method of the coltsfoot flower extract is: The coltsfoot flowers were washed, dried, and crushed, mixed with a 55wt% ethanol solution, and subjected to ultrasonic extraction for 20 min at a power of 300w and a temperature of 55°C; then the concentration of the alcohol solution was adjusted to 75wt%, and ultrasonic extraction was performed a second time for 15 min at a power of 200w and a temperature of 75°C. The alcohol extracts were combined, filtered, and spray-dried to obtain the product.

[0036] Preferably, the preparation method of the composite antibacterial agent is: azulene and coltsfoot flower extract are mixed evenly.

[0037] Preferably, the auxiliary material further comprises at least one of a friction agent, a moisturizing agent, an adhesive and a foaming agent.

[0038] Preferably, the friction agent is selected from at least one of calcium carbonate, dibasic calcium phosphate dihydrate, anhydrous dibasic calcium phosphate, calcium pyrophosphate, anhydrous silicon dioxide, aluminum hydroxide, aluminum oxide trihydrate, calcite powder, and chlorite. Further preferably, the friction agent is alumina trihydrate.

[0039] Preferably, the moisturizing agent is at least one selected from glycerol, sorbitol, propylene glycol, polyethylene glycol, and glycerin.

[0040] More preferably, the moisturizing agent is sorbitol.

[0041] Preferably, the binder is at least one of silica powder, carboxymethyl cellulose, hydroxyethyl cellulose, carbomer, and xanthan gum.

[0042] Further preferably, the adhesive is xanthan gum.

[0043] Preferably, the foaming agent is selected from at least one of sodium lauryl sulfate, sodium N-lauroyl sarcosinate, sodium methyl cocoyl taurate, and sodium acyl glutamate.

[0044] More preferably, the foaming agent is sodium acyl glutamate.

[0045] Preferably, the auxiliary materials include the following raw materials in parts by mass: 32-48 parts of abrasive, 25-39 parts of moisturizing agent, 2-8 parts of adhesive, 1-5 parts of foaming agent and 2-10 parts of compound antibacterial agent.

[0046] Further preferably, the auxiliary materials include the following raw materials in parts by mass: 45 parts of friction agent, 35 parts of moisturizing agent, 5 parts of adhesive, 4 parts of foaming agent and 8 parts of compound antibacterial agent.

[0047] In a second aspect, the present invention provides a method for preparing the toothpaste composition described above, comprising the following steps: S1: Green salt and gypsum are calcined and then crushed to obtain extract 1; S2: Mix Eclipta prostrata, Saposhnikovia divaricata, and Radix Aconiti Lateralis Preparata with water, reflux the water extract, and concentrate the water extract to obtain an extract; S3: Angelica dahurica, Psoralea corylifolia, Zanthoxylum bungeanum, Asarum sieboldii and Menthol were mixed and extracted with a deep eutectic solvent-alcohol solution, wherein the deep eutectic solvent was choline chloride and L-menthol, to obtain Extract 2; S4: extract 1, the extract and extract 2 are mixed and dried to obtain a composition; S5: The composition, the freeze-dried compound probiotic powder, the auxiliary materials and water are mixed and homogenized to obtain the product.

[0048] Preferably, in step S1, the pulverization is performed with a particle size controlled to be ≤15 μm; Preferably, in step S2, the solid-liquid ratio of the total mass of the Angelica dahurica, Eclipta prostrata, Saposhnikovia divaricata and Aconiti Lateralis Preparata to water is 1g:15-20L; further preferably, in step S2, the solid-liquid ratio of the total mass of the Angelica dahurica, Eclipta prostrata, Saposhnikovia divaricata and Aconiti Lateralis Preparata to water is 1g:18L.

[0049] Preferably, in step S2, the reflux water extraction time is 2-3 hours.

[0050] Preferably, in step S2, the specific gravity of the extract is 1.20-1.25 (concentrated under reduced pressure at 60°C).

[0051] Preferably, in step S3, the molar ratio of choline chloride to L-menthol is 1:1.8-2.5. Further preferably, in step S3, the molar ratio of choline chloride to L-menthol is 1:2.

[0052] Preferably, in step S3, the alcohol solution is a 55wt%-65wt% ethanol solution; Preferably, in step S3, the preparation method of the deep eutectic solvent-alcohol solution is: Mix choline chloride and L-menthol in proportion, stir at 50-60°C until uniform, add alcohol solution, and seal for storage.

[0053] In a third aspect, the present invention provides the use of the toothpaste composition described above in the preparation of an oral care product having the effects of strengthening teeth, strengthening teeth, and resisting sensitivity.

[0054] Compared with the prior art, the present invention has the following beneficial effects: 1. The present invention significantly improves the stability and antibacterial properties of the obtained product by adding a composite antibacterial agent, and the extracts of azulene and coltsfoot flower play a synergistic role.

[0055] 2. The present invention adopts a specific preparation method to extract the raw materials separately, and the toothpaste composition prepared can significantly improve various inflammations and bleeding of periodontal disease, improve the dental health problems of users with dentin hypersensitivity, and meet the needs of various users. DETAILED DESCRIPTION

[0056] In order to make the technical means, creative features, purpose and effect of the present invention easy to understand, the present invention is further illustrated below in conjunction with specific embodiment, but the following embodiment is only a preferred embodiment of the present invention, not all. Based on the embodiment in the embodiment, other embodiments obtained by those skilled in the art without making creative work all fall within the protection scope of the present invention. It is worth noting that the raw materials used in the present invention are all common commercial products, and their source is not specifically limited. The technology and scientific terms used in the embodiment have the meaning commonly understood by those of ordinary skill in the art to which the present invention belongs.

[0057] Kluyveromyces marxianus: strain number SHBCC D81683, purchased from Shanghai Collection Biotechnology Center.

[0058] Lactobacillus salivarius freeze-dried powder was purchased from Shandong Gushuo Biotechnology Co., Ltd.

[0059] Example 1 A toothpaste composition having the effects of strengthening and strengthening teeth, comprising, by weight, an active component and an auxiliary material, wherein the mass ratio of the active component to the auxiliary material is 1:99, specifically as follows: (1) Active ingredients: 15 parts of green salt, 15 parts of gypsum, 12 parts of psoralea corylifolia, 4.5 parts of Zanthoxylum bungeanum, 4.5 parts of Angelica dahurica, 4.5 parts of mint, 7.5 parts of Eclipta prostrata, 7.5 parts of Saposhnikovia divaricata, 4.5 parts of Asarum, 1 part of Radix Aconiti Lateralis Preparata and 20 parts of compound probiotic freeze-dried powder.

[0060] The preparation method of the composite probiotic freeze-dried powder is as follows: activating and culturing Kluyveromyces marxianus to obtain a Kluyveromyces marxianus basic stock solution, freeze-drying and dehydrating the stock solution to obtain Kluyveromyces marxianus freeze-dried powder, and then mixing the stock solution with Lactobacillus salivarius freeze-dried powder at a mass ratio of 2:1 to obtain the composite probiotic freeze-dried powder.

[0061] (2) Auxiliary materials: 45 parts of aluminum oxide trihydrate, 35 parts of sorbitol, 5 parts of xanthan gum, 4 parts of sodium acyl glutamate and 8 parts of compound antibacterial agent.

[0062] The composite antibacterial agent is prepared by uniformly mixing the azulene indigo and coltsfoot flower extracts in a mass ratio of 5:6.

[0063] The preparation method of the coltsfoot flower extract is: The coltsfoot flowers were washed, dried, and crushed, mixed with a 55wt% ethanol solution, and subjected to ultrasonic extraction for 20 min at a power of 300w and a temperature of 55°C; then the concentration of the alcohol solution was adjusted to 75wt%, and ultrasonic extraction was performed a second time for 15 min at a power of 200w and a temperature of 75°C. The alcohol extracts were combined, filtered, and spray-dried to obtain the product.

[0064] (3) The preparation method is as follows: S1: Green salt and gypsum are calcined and then crushed, and the particle size is controlled to be ≤15μm to obtain extract 1; S2: Mixing Eclipta prostrata, Saposhnikovia divaricata, and Radix Aconiti Lateralis Preparata with water at a material-liquid ratio of 1 g:18 L of the total mass of Angelica dahurica, Eclipta prostrata, Saposhnikovia divaricata, and Radix Aconiti Lateralis Preparata. Heating to reflux water for 2-3 hours, concentrating the aqueous extract to obtain an extract having a specific gravity of 1.20 (concentrated under reduced pressure at 60°C). S3: Angelica dahurica, Psoralea corylifolia, Zanthoxylum bungeanum, Asarum sieboldii and Menthol were mixed and extracted with a deep eutectic solvent-alcohol solution, wherein the deep eutectic solvent was choline chloride and L-menthol, to obtain Extract 2; The preparation method of the deep eutectic solvent-alcohol solution is: Choline chloride and L-menthol were mixed in a molar ratio of 1:2, stirred at 50-60°C until uniform, added with 60 wt% ethanol solution, mixed evenly, and sealed for storage.

[0065] S4: Extract 1, the extract and extract 2 are stirred and mixed uniformly, and dried to obtain a composition; S5: The composition, the freeze-dried compound probiotic powder, the auxiliary materials and water are mixed evenly and homogenized to obtain the product.

[0066] Example 2 A toothpaste composition having the effects of strengthening and strengthening teeth, comprising, by weight, an active component and an auxiliary material, wherein the mass ratio of the active component to the auxiliary material is 3:97, specifically as follows: (1) Active ingredients: 10 parts of green salt, 20 parts of gypsum, 8 parts of psoralea corylifolia, 7 parts of Zanthoxylum bungeanum, 2 parts of Angelica dahurica, 7 parts of mint, 5 parts of Eclipta prostrata, 10 parts of Saposhnikovia divaricata, 7 parts of Asarum, 0.1 parts of Radix Aconiti Lateralis Preparata and 5 parts of compound probiotic freeze-dried powder.

[0067] The preparation method of the composite probiotic freeze-dried powder is as follows: activating and culturing Kluyveromyces marxianus to obtain a Kluyveromyces marxianus basic stock solution, freeze-drying and dehydrating the stock solution to obtain Kluyveromyces marxianus freeze-dried powder, and then mixing the stock solution with Lactobacillus salivarius freeze-dried powder at a mass ratio of 1:1 to obtain the composite probiotic freeze-dried powder.

[0068] (2) Excipients: 32 parts of alumina trihydrate, 25 parts of sorbitol, 2 parts of xanthan gum, 1 part of sodium acyl glutamate and 3 parts of compound antibacterial agent.

[0069] The composite antibacterial agent is prepared by uniformly mixing azulene and coltsfoot flower extract in a mass ratio of 3:5.

[0070] The preparation method of the coltsfoot flower extract is: The coltsfoot flowers were washed, dried, and crushed, mixed with a 45 wt% ethanol solution, and subjected to ultrasonic extraction for 10 min at a power of 400 W and a temperature of 50° C.; the concentration of the alcohol solution was then adjusted to 70 wt%, and ultrasonic extraction was performed for a second time for 10 min at a power of 300 W and a temperature of 65° C. The alcohol extracts were combined, filtered, and spray-dried to obtain the product.

[0071] (3) The preparation method is as follows: S1: Green salt and gypsum are calcined and then crushed, and the particle size is controlled to be ≤15μm to obtain extract 1; S2: Mixing Eclipta prostrata, Saposhnikovia divaricata, and Radix Aconiti Lateralis Preparata with water at a material-liquid ratio of 1 g:15 L of the total mass of Angelica dahurica, Eclipta prostrata, Saposhnikovia divaricata, and Radix Aconiti Lateralis Preparata to water, heating to reflux and extracting for 2-3 hours, concentrating the aqueous extract to obtain an extract having a specific gravity of 1.25 (concentrated under reduced pressure at 60°C); S3: Angelica dahurica, Psoralea corylifolia, Zanthoxylum bungeanum, Asarum sieboldii and Menthol were mixed and extracted with a deep eutectic solvent-alcohol solution, wherein the deep eutectic solvent was choline chloride and L-menthol, to obtain Extract 2; The preparation method of the deep eutectic solvent-alcohol solution is: Choline chloride and L-menthol were mixed in a molar ratio of 1:1.8, stirred at 50-60°C until uniform, 55 wt% ethanol solution was added, mixed evenly, and sealed for storage.

[0072] S4: Extract 1, the extract and extract 2 are stirred and mixed uniformly, and dried to obtain a composition; S5: The composition, the freeze-dried compound probiotic powder, the auxiliary materials and water are mixed evenly and homogenized to obtain the product.

[0073] Example 3 A toothpaste composition having the effects of strengthening and strengthening teeth, comprising an active component and an auxiliary material in a mass ratio of 10:90, calculated by weight, as follows: (1) Active ingredients: 20 parts of green salt, 10 parts of gypsum, 15 parts of psoralea corylifolia, 2 parts of Zanthoxylum bungeanum, 7 parts of Angelica dahurica, 2 parts of mint, 10 parts of Eclipta prostrata, 5 parts of Saposhnikovia divaricata, 2 parts of Asarum, 2 parts of Radix Aconiti Lateralis Preparata and 32 parts of compound probiotic freeze-dried powder.

[0074] The preparation method of the composite probiotic freeze-dried powder is as follows: activating and culturing Kluyveromyces marxianus to obtain a Kluyveromyces marxianus basic stock solution, freeze-drying and dehydrating the stock solution to obtain Kluyveromyces marxianus freeze-dried powder, and then mixing the stock solution with Lactobacillus salivarius freeze-dried powder at a mass ratio of 3:1 to obtain the composite probiotic freeze-dried powder.

[0075] (2) Auxiliary materials: 48 parts of aluminum oxide trihydrate, 39 parts of sorbitol, 8 parts of xanthan gum, 5 parts of sodium acyl glutamate and 10 parts of compound antibacterial agent.

[0076] The composite antibacterial agent is prepared by uniformly mixing azulene and coltsfoot flower extract in a mass ratio of 8:10.

[0077] The preparation method of the coltsfoot flower extract is: The coltsfoot flowers were washed, dried, and crushed, mixed with a 65wt% ethanol solution, and ultrasonically extracted for 30 min at a power of 300w and a temperature of 55°C; then the concentration of the alcohol solution was adjusted to 80wt%, ultrasonically extracted for a second time for 30 min at a power of 400w and a temperature of 75°C, the alcohol extracts were combined, filtered, and spray-dried to obtain the product.

[0078] (3) The preparation method is as follows: S1: Green salt and gypsum are calcined and then crushed, and the particle size is controlled to be ≤15μm to obtain extract 1; S2: Mixing Eclipta prostrata, Saposhnikovia divaricata, and Radix Aconiti Lateralis Preparata with water at a material-liquid ratio of 1 g to 20 L of the total mass of Angelica dahurica, Eclipta prostrata, Saposhnikovia divaricata, and Radix Aconiti Lateralis Preparata. Heating to reflux water for 2-3 hours, concentrating the aqueous extract to obtain an extract having a specific gravity of 1.25 (concentrated under reduced pressure at 60°C). S3: Angelica dahurica, Psoralea corylifolia, Zanthoxylum bungeanum, Asarum sieboldii and Menthol were mixed and extracted with a deep eutectic solvent-alcohol solution, wherein the deep eutectic solvent was choline chloride and L-menthol, to obtain Extract 2; The preparation method of the deep eutectic solvent-alcohol solution is: Choline chloride and L-menthol were mixed in a molar ratio of 1:2.5, stirred at 50-60°C until uniform, added with 65 wt% ethanol solution, mixed evenly, and sealed for storage.

[0079] S4: Extract 1, the extract and extract 2 are stirred and mixed uniformly, and dried to obtain a composition; S5: The composition, the freeze-dried compound probiotic powder, the auxiliary materials and water are mixed evenly and homogenized to obtain the product.

[0080] Comparative Example 1 According to the raw materials and preparation method of Example 1 in Chinese patent application CN 117771311 A, a traditional Chinese medicine tooth-strengthening tooth powder was prepared.

[0081] Comparative Example 2 A toothpaste composition having the effects of strengthening and strengthening teeth, which differs from Example 1 in that the components of the composite antibacterial agent are different: The composite antibacterial agent is obtained by uniformly mixing azulene and honeysuckle extracts in a mass ratio of 5:6.

[0082] The honeysuckle extract is obtained according to the extraction method of Example 1 in Chinese patent CN108113951A.

[0083] The rest is the same as Example 1.

[0084] Comparative Example 3 A toothpaste composition having the effect of strengthening and strengthening teeth is different from Example 1 in that the mass fractions of the raw materials are different, as follows: Calculated by weight, it is composed of active ingredients and excipients, with the mass ratio of active ingredients to excipients being 1:99, as follows: (1) Active ingredients: 22 parts of green salt, 8 parts of gypsum, 20 parts of psoralea corylifolia, 1 part of Zanthoxylum bungeanum, 10 parts of Angelica dahurica, 1 part of mint, 4 parts of Eclipta prostrata, 12 parts of Saposhnikovia divaricata, 10 parts of Asarum, 4 parts of Aconite fructus and 4 parts of compound probiotic freeze-dried powder.

[0085] (2) Auxiliary materials: 30 parts of aluminum oxide trihydrate, 40 parts of sorbitol, 10 parts of xanthan gum, 2 parts of sodium acyl glutamate and 15 parts of compound antibacterial agent.

[0086] The rest is the same as Example 1.

[0087] Comparative Example 4 A toothpaste composition with the effects of strengthening and strengthening teeth, which differs from Example 1 in that the composition of the composite probiotic freeze-dried powder is different.

[0088] The composite probiotic freeze-dried powder is a mixture of freeze-dried Lactobacillus salivarius powder and freeze-dried Bifidobacterium powder in a ratio of 2:1 by mass, and is prepared according to the method described in Example 1 of Chinese patent application CN110559253A.

[0089] The rest is the same as Example 1.

[0090] Comparative Example 5 A toothpaste composition having the effect of strengthening and strengthening teeth, which differs from Example 1 in that the preparation method is different, specifically: Crush 15 parts of green salt, 15 parts of gypsum, 12 parts of psoralea corylifolia, 4.5 parts of Zanthoxylum bungeanum, 4.5 parts of Angelica dahurica, 4.5 parts of mint, 7.5 parts of Eclipta prostrata, 7.5 parts of Saposhnikovia divaricata, 4.5 parts of Asarum and 1 part of Radix Aconiti Lateralis Preparata. After sieving, mix evenly with 20 parts of freeze-dried compound probiotic powder, 45 parts of alumina trihydrate, 35 parts of sorbitol, 5 parts of xanthan gum, 4 parts of sodium acyl glutamate and 8 parts of compound antibacterial agent to obtain the product.

[0091] Test Example 1 Antibacterial test: (1) Storage stability test: The products prepared in Examples 1-3 and Comparative Examples 1-5 were tested for antibacterial activity. Specifically, the samples were tested for 48-hour antibacterial rate using a film-applying method in accordance with the Light Industry Standard of the People's Republic of China, QB / T2591-2003. The total bacterial count was calculated in accordance with GB / T4789.2-2003. The specific antibacterial rate comparison data are shown in Table 1 below: The calculation formula of the antibacterial rate is: R(%)=(BC) / B×100%.

[0092] Where: R-antibacterial rate, %; B-average number of bacteria recovered from blank control samples, cfu / tablet; C-average number of bacteria recovered from antibacterial ointment samples, cfu / tablet.

[0093] Table 1. Antibacterial rate (%)

[0094] As can be seen from Table 1, compared with the comparative example, the specific components, proportions and preparation method of the present invention significantly improve the antibacterial property of the prepared composition.

[0095] Test Example 2 Research on anti-inflammatory and hemostatic functions: (1) Research on the anti-inflammatory effect of toothpaste Seventy-two Kunming white mice (18±22g, 7 weeks old) were purchased from Tai'an Taibang Biotechnology Co., Ltd., half male and half female. After one week of adaptive feeding, they were randomly divided into nine groups: a blank control group (normal group), consisting of eight mice; and experimental groups (Examples 1-3 and Comparative Examples 1-5), consisting of eight mice each. 0.05mL of xylene was applied to the anterior and posterior surfaces of the right auricle of the mice to induce inflammation; the left auricle served as a control. Thirty minutes after inflammation, the right ear of each experimental group (except the blank control group) was coated with the corresponding toothpaste (1g / mouse). One hour after application, the mice were sacrificed by cervical dislocation. The ear medication was removed, and a No. 9 ear punch was used to punch out the same portion of the left and right ears and weigh them. The difference between the right ear weight and the left ear weight was used to calculate the degree of right ear swelling. The anti-inflammatory effects of the drugs were compared and the degree of swelling was calculated.

[0096] Swelling degree (%) = (right ear weight - left ear weight) / left ear weight * 100%.

[0097] Analgesia percentage (%) = (number of writhings in the blank control group - number of writhings in the drug-treated group) / number of writhings in the blank control group × 100%.

[0098] (2) Research on the hemostatic function of toothpaste Seventy-two Kunming mice (18±22g, 7 weeks old) were purchased from Tai'an Taibang Biotechnology Co., Ltd., half male and half female. After one week of adaptive feeding, they were randomly divided into nine groups: a blank control group (normal group) consisting of eight mice; and experimental groups (Examples 1-3 and Comparative Examples 1-5), each consisting of eight mice. Each mouse was anesthetized by injecting 0.2mL of 30% urethane solution. The liver was then removed and a 1cm-long wound was incised. Except for the blank control group, the other two groups were coated with different medicated toothpastes (1g / mouse). The wounds were observed every 30 seconds until bleeding ceased. Bleeding time was calculated (bleeding time exceeding 3 minutes was rounded to 3 minutes).

[0099] (4) Statistical analysis Statistical analysis One-way ANOVA test was performed using GraphPad Prism program ver. 4.0. The results are shown as mean ± standard deviation. P < 0.05 was considered to be significantly different. The results are shown in Table 2-Table 3: Table 2. Effects of xylene on ear swelling in mice (±s)

[0100] Compared with the blank control group, **P<0.01, *P<0.05.

[0101] Table 3. Effects on hemostasis time of mouse liver bleeding (±s)

[0102] Compared with the blank control group, **P<0.01, *P<0.05.

[0103] As can be seen from Tables 2 and 3, compared with the comparative example, the specific components, proportions and preparation method of the present invention significantly improve the anti-inflammatory and hemostatic effects of the prepared composition.

[0104] Test Example 3 Treatment and Prevention of Tooth Sensitivity Tests: A double-blind trial was conducted, randomly selecting 160 volunteers with tooth sensitivity, who had symptoms of tooth aches, sensitivity to hot and cold, stinging pain from sweet and sour foods, pain when brushing, discomfort when biting, and spontaneous pain. The volunteers were randomly divided into 8 equal groups. The selected volunteers used the toothpaste or tooth powder prepared in Examples 1-3 and Comparative Examples 1-5 on the basis of their daily habits (brushing their teeth twice a day) for three months. The volunteers were interviewed and questionnaires were collected to record the oral symptoms after using the test toothpastes. Statistical comparisons were performed. The statistical results are shown in Table 4.

[0105] The scoring criteria are: Significant effect: symptoms such as toothache, sensitivity to hot and cold, stinging pain from sweet and sour foods, pain when brushing teeth, discomfort when biting, and spontaneous pain have basically disappeared; Good effect: It can significantly relieve symptoms such as toothache, hot and cold sensitivity, sour and sweet stinging, toothbrushing pain, biting discomfort, and spontaneous pain; Some effect: relieves symptoms such as toothache, hot and cold sensitivity, sweet and sour tingling, toothbrushing pain, biting discomfort, and spontaneous pain; No effect: symptoms such as toothache, sensitivity to hot and cold, tingling sensations of sweet and sour foods, pain when brushing teeth, discomfort when biting, and spontaneous pain remain the same.

[0106] Table 4. Results of treatment and prevention of tooth sensitivity tests

[0107] As can be seen from Table 4, compared with the comparative example, the specific components, proportions and preparation method of the present invention significantly improve the treatment and prevention effect of the prepared composition on tooth sensitivity.

[0108] Finally, it should be noted that the above content is only used to illustrate the technical solution of the present invention, rather than to limit the scope of protection of the present invention. Simple modifications or equivalent substitutions of the technical solution of the present invention by ordinary technicians in this field do not deviate from the essence and scope of the technical solution of the present invention.

Claims

1. A toothpaste composition having the effect of strengthening and strengthening teeth, characterized in that: The invention comprises active components and auxiliary materials, wherein the active components are composed of green salt, gypsum, psoralea corylifolia, Zanthoxylum bungeanum, angelica dahurica, mint, Eclipta prostrata, Saposhnikovia divaricata, asarum, Aconite fructus and compound probiotic freeze-dried powder; the compound probiotic freeze-dried powder is composed of Kluyveromyces marxianus freeze-dried powder and Lactobacillus salivarius freeze-dried powder; the auxiliary materials include a compound antibacterial agent; and the compound antibacterial agent is composed of azulene and coltsfoot flower extracts.

2. The toothpaste composition according to claim 1, characterized in that The mass ratio of the active component to the excipient is 1-10:90-99; the mass of the composite probiotic freeze-dried powder accounts for 15%-30% of the mass of the active component; and the mass ratio of the Kluyveromyces marxianus freeze-dried powder to the Lactobacillus salivarius freeze-dried powder is 1-3:

1.

3. The toothpaste composition according to claim 1, characterized in that The mass of the composite antibacterial agent is 5-10% of the total mass of the excipients.

4. The toothpaste composition according to claim 1, characterized in that The active ingredient is composed of the following raw materials in parts by mass: 10-20 parts of green salt, 10-20 parts of gypsum, 8-15 parts of psoralea corylifolia, 2-7 parts of Sichuan pepper, 2-7 parts of angelica dahurica, 2-7 parts of mint, 5-10 parts of Eclipta prostrata, 5-10 parts of Saposhnikovia divaricata, 2-7 parts of Asarum, 0.1-2 parts of cooked aconite root and 5-32 parts of compound probiotic freeze-dried powder.

5. The toothpaste composition according to claim 1, characterized in that The mass ratio of the azulene indigo extract to the coltsfoot flower extract is 3-8:5-10.

6. The toothpaste composition according to claim 1, characterized in that The preparation method of the coltsfoot flower extract is: The coltsfoot flower is crushed, mixed with 45wt%-65wt% alcohol solution, and ultrasonically extracted for 10-30min. Then, the concentration of the alcohol solution is adjusted to 70wt%-80wt%, ultrasonically extracted for a second time for 10-30min, and the alcohol extracts are combined to obtain the product.

7. The toothpaste composition according to claim 1, wherein The auxiliary materials also include at least one of a friction agent, a moisturizing agent, a binder and a foaming agent; the friction agent is selected from at least one of calcium carbonate, dihydrated calcium hydrogen phosphate, anhydrous calcium hydrogen phosphate, calcium pyrophosphate, anhydrous silicon dioxide, aluminum hydroxide, trihydrated aluminum oxide, calcite powder and clinocladium; the moisturizing agent is selected from at least one of glycerol, sorbitol, propylene glycol, polyethylene glycol and glycerol; the binder is at least one of silica powder, carboxymethyl cellulose, hydroxyethyl cellulose, carbomer and xanthan gum; the foaming agent is selected from at least one of sodium lauryl sulfate, sodium N-lauroyl sarcosinate, sodium methyl cocoyl taurate and sodium acyl glutamate.

8. The toothpaste composition according to claim 7, characterized in that The auxiliary materials include the following raw materials in parts by mass: 32-48 parts of abrasive, 25-39 parts of moisturizing agent, 2-8 parts of adhesive, 1-5 parts of foaming agent and 2-10 parts of compound antibacterial agent.

9. The method for preparing the toothpaste composition according to any one of claims 1 to 8, characterized in that: The following steps are involved: S1: Green salt and gypsum are calcined and then crushed to obtain extract 1; S2: Mix Eclipta prostrata, Saposhnikovia divaricata, and Radix Aconiti Lateralis Preparata with water, reflux the water extract, and concentrate the water extract to obtain an extract; S3: Angelica dahurica, Psoralea corylifolia, Zanthoxylum bungeanum, Asarum sieboldii and Menthol were mixed and extracted with a deep eutectic solvent-alcohol solution, wherein the deep eutectic solvent was choline chloride and L-menthol, to obtain Extract 2; S4: extract 1, the extract and extract 2 are mixed and dried to obtain a composition; S5: The composition, the freeze-dried compound probiotic powder, the auxiliary materials and water are mixed and homogenized to obtain the product.

10. Use of the toothpaste composition according to any one of claims 1 to 8 in the preparation of oral care products having the effects of strengthening teeth, strengthening teeth and preventing sensitivity.

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