Compositions with fresh breath, whitening teeth efficacy, preparation method and application thereof

Abstract

The application provides a composition with fresh breath and tooth whitening effects and a preparation method and application thereof, and relates to the technical field of oral cleaning and nursing.The composition comprises the following raw materials: saussurea involucrata extract, magnolia officinalis extract, polygonatum extract and tannase;the preparation method of the saussurea involucrata extract is that the saussurea involucrata is extracted through a eutectic solvent, then purified through a macroporous resin, emulsified, homogenized, dried, and obtained;the preparation method of the polygonatum extract is that the rhizome of polygonatum is mixed with ethanol for defatting, the defatted product is enzymatically hydrolyzed, the enzymatic hydrolysate is purified through a macroporous resin, and then sequentially passes through ultrafiltration membranes with molecular weight cut-offs of 100 kDa and 30 kDa, and the 30 kDa cut-off liquid is collected, and obtained.The application significantly improves the whitening and bacteriostatic effects of the prepared composition through specific components and a preparation method, and the stability is better, and the needs of consumers can be met.

Description

Technical Field

[0001] This invention relates to the field of oral hygiene and care technology, specifically to compositions with the effects of freshening breath and whitening teeth, their preparation methods, and applications. Background Technology

[0002] Oral health is closely related to people's physical health and quality of life, and a set of white teeth can increase social confidence. How to safely, gently, and effectively prevent and remove stains on teeth, freshen breath, and maintain oral hygiene is one of the most important oral health concerns for most consumers.

[0003] On the one hand, oral health problems manifest in tooth discoloration: tooth staining is divided into intrinsic and extrinsic staining. Intrinsic tooth staining is caused by abnormal tooth development or pulp infection, such as pulp necrosis, fluorosis, and tetracycline staining. Extrinsic tooth staining is caused by long-term intake of dark-colored foods, beverages, tobacco, or occupational exposure to certain minerals such as iron, sulfur, and copper, leading to changes in tooth color. Currently, the whitening effect of toothpaste is mainly divided into physical whitening, which is the mechanical abrasive effect of abrasives in toothpaste, and chemical whitening, which uses surfactants, calcium chelating agents, enzymes, polymers, oxidants, etc., in toothpaste to whiten teeth through mechanisms such as chelation, biodegradation, and redox reactions. Physical whitening by abrasives alone has limited effect, and excessive friction can easily lead to tooth wear, causing other problems such as tooth sensitivity. It is difficult to achieve good whitening results with surfactants and calcium chelating agents alone, and adding biological enzymes to toothpaste requires very high formulation standards. Oxidizing agents are one of the common methods used by professional medical institutions to whiten teeth. For example, hydrogen peroxide has a good whitening effect, but it is also highly irritating and may cause tooth sensitivity. Adding hydrogen peroxide to toothpaste can easily lead to instability of the paste, resulting in instability problems such as bloating and water separation.

[0004] On the other hand, oral health issues manifest in terms of breath freshening and oral hygiene: the mouth is extremely prone to producing a large number of bacteria and microorganisms; more than 300 types of bacteria have been identified. Some bacteria constantly adhere to the surface of dentures, forming a sticky, colorless film called dental plaque. Each cubic millimeter of dental plaque contains hundreds of millions of bacteria, which produce many harmful substances, damaging the teeth themselves and causing inflammation and destruction of the surrounding tissues. Currently, some commonly used oral care products, such as toothpaste and mouthwash, mainly play a preventative role; their actual antibacterial and anti-inflammatory effects, and their ability to inhibit a limited number of bacterial species, are not ideal for alleviating oral disease symptoms.

[0005] Snow lotus (Saussurea involucrata) is a traditional and precious Chinese herbal medicine with anti-inflammatory, antioxidant, and analgesic effects. However, current applications in the oral health field are mostly limited to gingival inflammation, and no research has yet explored the synergistic effects of specific extracts of snow lotus in removing extrinsic pigmentation, inhibiting oral pigmentation, and providing long-lasting fresh breath. Furthermore, traditional snow lotus extraction methods (such as ethanol reflux) have low extraction rates, and the active ingredients (such as chlorogenic acid, flavonoids like rutin) are unstable in the complex oral environment (salivary enzymes, pH changes), making it difficult to achieve whitening effects.

[0006] Chinese patent application CN111700835A discloses a toothpaste containing snow lotus extract and its preparation method. The toothpaste containing snow lotus extract is prepared from zinc citrate, titanium dioxide, humectant, abrasive, sodium lauryl sulfate, calcium bicarbonate, thickener, sodium benzoate, trichlorogalactose, sodium phytate, snow lotus extract, fragrance, and water. The preparation method of the snow lotus extract is as follows: (1) Pulverize dried snow lotus and pass it through a 50-mesh sieve to obtain snow lotus powder; (2) Add the snow lotus powder obtained in step (1) to a flask, add petroleum ether and reflux for defatting 4 times, each extraction for 0.5 h, filter and dry the filter residue to obtain defatted snow lotus powder; (3) Add the defatted snow lotus powder obtained in step (2) to a flask, add 75% ethanol solution and reflux for extraction 5 times, each extraction for 1 h, filter. (3) Combine the filtrates to obtain a crude extract; (4) Perform dynamic continuous countercurrent extraction on the crude extract obtained in step (3) at an extraction temperature of 45-60℃ for 1 hour to obtain a refined extract; (5) Concentrate the refined extract obtained in step (4) under reduced pressure, let it stand for 24 hours, centrifuge to obtain a supernatant, and obtain the toothpaste containing snow lotus ingredients provided by this invention. The toothpaste has good cleaning, antibacterial, anti-inflammatory and analgesic functions, and can promote the remineralization of tooth enamel surface and enhance the anti-caries ability of enamel. The preparation method of the snow lotus extract involved is simple, low in cost, and easy to realize industrial production, but it does not involve whitening effects.

[0007] Chinese patent application CN106074339A discloses a whitening toothpaste made from the following raw materials in parts by weight: 8-14 parts alumina, 5-7 parts lanthanum chloride, 4-6 parts silica, 3-5 parts hydroxyethyl cellulose, 3-4 parts isopropanol, 7-9 parts Poria cocos, 6-8 parts Angelica dahurica, 2-4 parts Atractylodes macrocephala, 6-8 parts vitamin C, 6-9 parts pearl powder, 5-7 parts dicalcium phosphate, 4-7 parts sorbitol, and 5-8 parts sodium lauryl sulfate. This technical solution primarily uses physical whitening methods, which carries the risk of causing tooth abrasion and lacks antibacterial effects, thus only fulfilling the single requirement of whitening.

[0008] Chinese patent application CN105748377A discloses a traditional Chinese medicine toothpaste comprising the following formula: dicalcium phosphate, water, sorbitol, hydrated silica, polyethylene glycol, sodium lauryl sulfate, edible flavor, cellulose gum, tetrasodium pyrophosphate, hydroxyethyl cellulose, snow lotus extract, honeysuckle extract, wild chrysanthemum extract, sodium benzoate, sodium saccharin, methylparaben, CI75810, and CI19140. The main efficacy of this technical solution is antibacterial and anti-inflammatory, with no whitening effect.

[0009] Therefore, it is of great significance to develop a gentle, effective composition that combines whitening and antibacterial properties to better meet consumers' needs for oral care products. Summary of the Invention

[0010] To address the aforementioned problems, this invention provides a composition that freshens breath and whitens teeth. Through specific components and proportions, a mild, effective composition that combines whitening and antibacterial properties is obtained, better meeting consumers' needs for oral care products.

[0011] To achieve the above objectives, the technical solution adopted by the present invention is as follows: On one hand, the present invention provides a composition with the effects of freshening breath and whitening teeth, comprising the following raw materials: snow lotus extract, magnolia bark extract, Solomon's seal extract and tanninase; the snow lotus extract is prepared by extracting snow lotus with a eutectic solvent, then purifying it with macroporous resin, emulsifying, homogenizing and drying it to obtain the snow lotus extract; the Solomon's seal extract is prepared by mixing Solomon's seal rhizome with ethanol for defatting, enzymatically hydrolyzing the defatted product, purifying the hydrolysate with macroporous resin and then passing it sequentially through ultrafiltration membranes with molecular weight cutoffs of 100kDa and 30kDa, collecting the 30kDa retentate to obtain the Solomon's seal extract.

[0012] Preferably, the preparation method of the snow lotus extract includes the following steps: (1) After the whole plant of snow lotus is crushed, it is frozen at -25℃~-15℃ for 20-26h, and then thawed to obtain whole plant powder of snow lotus; (2) Choline chloride and glycerol are mixed in a molar ratio of 1:1.5-2.5 to obtain a transparent and homogeneous eutectic solvent. Then, water with a mass fraction of 18%-25% is added to the eutectic solvent to obtain extraction solvent A. (3) Mix the whole snow lotus powder with extraction solvent A, extract for 25-35 min, separate, collect the supernatant to obtain crude extract; (4) The crude extract was purified by elution using an AB-8 macroporous adsorption resin column. The eluent was collected, concentrated, and the extract was obtained. (5) The extract, lecithin and cholesterol are mixed in a mass ratio of 1:2.5-5:0.3-0.6, homogenized and dried to obtain snow lotus extract.

[0013] Preferably, in step (1), the whole snow lotus plant needs to be dried.

[0014] Preferably, in step (1), the whole snow lotus plant needs to be pulverized and passed through a 40-100 mesh sieve.

[0015] Preferably, in step (2), the mixing is stirring, the temperature is 50-60℃, and the time is 1-2h.

[0016] Preferably, in step (3), the ratio of the whole snow lotus powder to the extraction solvent A is 1g:25-32mL.

[0017] Preferably, in step (3), the extraction is ultrasonic-microwave extraction, with ultrasonic power of 350-420W, ultrasonic frequency of 35-45kHz, microwave power of 280-320W, extraction temperature of 45-55℃, and extraction time of 25-35min.

[0018] Preferably, in step (4), the elution and purification are performed by first eluting with 2-4 column volumes of deionized water, and then eluting with ethanol solutions of volume fractions of 25-35%, 45-55%, and 65-75% in sequence, and collecting the eluent with a volume fraction of 45-55%.

[0019] Preferably, in step (4), the concentration is a vacuum concentration at 40-45°C.

[0020] Preferably, in step (5), the homogenization pressure is 500-600 bar, and the number of times is 2-3.

[0021] Preferably, the preparation method of the Polygonatum odoratum extract is as follows: S1: After crushing the rhizome of Polygonatum odoratum, mix it with 4-6 times its weight of ethanol for defatting. Reflux defatting at 35-45℃ for 1-2 hours, filter, discard the ethanol liquid, and obtain the defatted product. S2: The defatted product is mixed with water at a material-to-liquid ratio of 1g:15-20mL. A mixture of cellulase and pectinase at a mass ratio of 1-3:1 is added for enzymatic hydrolysis. The pH is adjusted to 5-6, the temperature is 45-55℃, and the time is 1.5-2.5h to inactivate the enzyme and obtain the enzymatic hydrolysate. S3: The enzymatic hydrolysate is purified by an AB-8 macroporous adsorption resin column. First, it is eluted with 2-4 times deionized water, then eluted with a 40%-60% (v / v) ethanol aqueous solution, and the eluent is collected. Then, it is passed sequentially through ultrafiltration membranes with molecular weight cutoffs of 100kDa and 30kDa, and the 30kDa cutoff is collected. The solution is concentrated under reduced pressure and dried to obtain the final product.

[0022] The mass ratio of the snow lotus extract, magnolia bark extract, Solomon's seal extract and tannin enzyme is 1-3:0.2-0.5:1-2:0.05-0.2.

[0023] Secondly, the present invention provides a method for preparing the above-mentioned composition, comprising the following steps: (a) Tanninase and Polygonatum odoratum extract were mixed at pH 5.8-6.2 to obtain mixture 1; (b) Mixture 1: Snow lotus extract and magnolia bark extract are mixed and dried to obtain a composition.

[0024] Thirdly, the present invention provides the use of the above composition in the preparation of oral care products.

[0025] Preferably, the oral care product comprises the above-described composition and excipients.

[0026] Preferably, the oral care product includes toothpaste, mouthwash, tooth powder, dental tablets, or dental strips.

[0027] More preferably, the oral care product is toothpaste.

[0028] Preferably, the excipients are selected from at least one of humectants, abrasives, solvents, foaming agents, fragrances, thickeners, preservatives, stabilizers, colorants, cooling agents, sweeteners, and antioxidants.

[0029] More preferably, the excipients are selected from humectants, abrasives, solvents, foaming agents, fragrances, thickeners, preservatives, stabilizers, colorants, cooling agents, sweeteners, and antioxidants.

[0030] Preferably, the moisturizer is selected from at least one of sorbitol, glycerin, polyethylene glycol, and propylene glycol; More preferably, the moisturizer is selected from at least one of sorbitol, glycerin, and propylene glycol.

[0031] Preferably, the abrasive is selected from at least one of hydrated silica, hydroxyapatite, silicon dioxide, sodium pyrophosphate, calcium carbonate, calcium bicarbonate, pearl powder, titanium dioxide, and aluminum hydroxide.

[0032] More preferably, the abrasive is selected from at least one of hydrated silica, hydroxyapatite, silicon dioxide, sodium pyrophosphate, calcium carbonate, and pearl powder.

[0033] Preferably, the solvent is selected from at least one of water and polyethylene glycol.

[0034] More preferably, the solvent is selected from water and polyethylene glycol.

[0035] Preferably, the foaming agent is selected from at least one of sodium lauroyl sarcosinate and sodium lauryl sulfate.

[0036] More preferably, the foaming agent is selected from sodium lauroyl sarcosinate.

[0037] Preferably, the fragrance is a flavoring.

[0038] Preferably, the thickener is selected from at least one of cellulose gum, xanthan gum, carrageenan, guar gum, sodium carboxymethyl cellulose, and carboxyethyl cellulose.

[0039] More preferably, the thickener is selected from cellulose gum and xanthan gum.

[0040] Preferably, the preservative is selected from at least one of sodium benzoate, potassium sorbate, phenoxyethanol, p-hydroxyacetophenone, methylparaben, and propylparaben.

[0041] More preferably, the preservative is selected from sodium benzoate, potassium sorbate, phenoxyethanol, and p-hydroxyacetophenone.

[0042] Preferably, the stabilizer is selected from at least one of tetrasodium pyrophosphate, Tween, and Span.

[0043] More preferably, the stabilizer is at least one of tetrasodium pyrophosphate, Tween, and Span.

[0044] Preferably, the colorant is selected from titanium dioxide.

[0045] More preferably, the colorant is CI 77891.

[0046] Preferably, the cooling agent is selected from at least one of methyl diisopropyl propionamide, menthol, and peppermint oil.

[0047] More preferably, the cooling agent is selected from methyl diisopropylpropionamide and menthol carbamoyl ethylamine.

[0048] Preferably, the sweetener is selected from at least one of trichlorogalactose, sodium saccharin, acesulfame potassium, stevioside, and mogroside.

[0049] More preferably, the sweetener is selected from at least one of trichlorogalactose, sodium saccharin, and acesulfame potassium.

[0050] Preferably, the antioxidant is selected from at least one of stannous chloride, butylated hydroxytoluene, 2,6-di-tert-butyl-4-methylphenol, and vitamin E.

[0051] More preferably, the antioxidant is selected from stannous chloride and butylated hydroxytoluene.

[0052] Preferably, the mass ratio of the excipient to the composition is 97-99:1-3.

[0053] More preferably, the mass ratio of the excipient to the composition is 97.895:2.105.

[0054] Preferably, the toothpaste preparation process includes the following steps: S1: Mix the humectant and thickener evenly to obtain component A; S2: Sweetener, solvent, stabilizer, preservative, antioxidant, and other components are stirred and dissolved evenly to obtain component B; S3: Abrasive and colorant are mixed to obtain component C; S4: Fragrance and cooling agent are mixed to obtain component D; S5: Add component B to component A, stir, then add component C and disperse homogenously; then add foaming agent and mix; finally add component D, degas, discharge, fill, and package to obtain the final product.

[0055] Compared with the prior art, the present invention has the following beneficial effects: 1. The composition of this invention uses snow lotus extract, magnolia bark extract, Solomon's seal extract, and tanninase as core raw materials, with each component having a clear function and synergistic effect. Among them, magnolia bark extract is rich in volatile oils and other active ingredients, which can effectively inhibit harmful bacteria in the oral cavity that cause halitosis and reduce the production of odor-causing substances such as volatile sulfur compounds, thus achieving fresh breath from the root and with a long-lasting freshness effect. Snow lotus extract and Solomon's seal extract can supplement the active nutrients needed by the oral cavity, soothe the oral mucosa, reduce the adhesion of pigments to the tooth surface, and help inhibit the formation of dental plaque. Tanninase can specifically decompose tannins in the oral cavity that affect the whiteness of teeth, reduce the rate of pigment deposition, and work synergistically with the above-mentioned plant extracts to significantly improve the teeth whitening effect. Compared with single raw materials, the dual effects are more significant and stable, and can solve the two major oral problems of bad breath and tooth discoloration at the same time.

[0056] 2. This invention employs targeted preparation processes based on the characteristics of different raw materials, effectively avoiding the loss of active ingredients and enhancing the efficacy of the composition. Snow lotus extract utilizes a low-melting-point solvent extraction combined with macroporous resin purification, which fully extracts active flavonoids, polysaccharides, and other components from snow lotus. Subsequent macroporous resin purification removes impurities, improving the purity of the extract. Emulsification, homogenization, and drying further ensure good dispersibility and strong stability of the extract, resulting in highly effective whitening, antioxidant, and antibacterial effects. Polygonatum odoratum extract employs an ethanol defatting-enzymatic hydrolysis-macroporous resin purification-double ultrafiltration process. Ethanol defatting removes fat-soluble impurities to avoid interfering with the extraction of active ingredients. Enzymatic hydrolysis disrupts the cell wall structure of the Polygonatum odoratum rhizome, promoting the dissolution of active ingredients. Subsequent macroporous resin purification further purifies the extract. Double ultrafiltration (with molecular weight cutoffs of 100kDa and 30kDa) screens out components with suitable molecular weights and stronger activity (30kDa cutoff), ensuring the activity and efficacy stability of the Polygonatum odoratum extract, thereby enhancing the overall effect of the composition.

[0057] 3. The raw materials used in the composition of this invention are all natural plant extracts and biological enzymes, which are naturally derived, highly safe, and free of artificial preservatives, pigments, and other harmful ingredients. They will not irritate the oral mucosa or teeth, avoiding the dryness, sensitivity, and other discomfort problems that may be caused by the chemical components in traditional oral care products. It is safe for use by people with sensitive skin, children, and the elderly, covering a wide range of people and possessing strong practicality.

[0058] 4. The composition of the present invention not only achieves immediate breath freshening and teeth whitening effects, but also supplements oral nutrition, improves the oral microenvironment, and enhances the defense ability of the oral mucosa through the active ingredients in plant extracts. Long-term use can reduce the recurrence of halitosis and tooth discoloration, and at the same time help prevent the formation of dental plaque and tartar, achieving a three-in-one oral care effect of "whitening + freshening + maintenance", providing long-term protection for oral health. Attached Figure Description

[0059] Figure 1 A shade guide for the color gradations of tooth enamel.

[0060] Figure 2 This is a graph showing the color gradation of tooth enamel before and after brushing with the toothpaste prepared in Example 4. Detailed Implementation

[0061] To make the technical means, creative features, achieved objectives, and effects of this invention readily understandable, the invention is further illustrated below with specific embodiments. However, these embodiments are merely preferred embodiments and not all embodiments. Other embodiments obtained by those skilled in the art based on the embodiments described herein without creative effort are all within the scope of protection of this invention. It is worth noting that the raw materials used in this invention are all common commercially available products, and their sources are not specifically limited. The technical and scientific terms used in the embodiments have the meanings commonly understood by those skilled in the art to which this invention pertains.

[0062] Magnolia officinalis extract: purchased from Xi'an Yahua Biotechnology Co., Ltd., product number YH-2022082321.

[0063] Tanninase: Purchased from Ningxia Xiasheng Industrial Group Co., Ltd., product number 20250702.

[0064] Example 1 A composition with the effects of freshening breath and whitening teeth is composed of the following raw materials: snow lotus extract, magnolia bark extract, Solomon's seal extract and tannin enzyme in a mass ratio of 2:0.4:1.5:0.15.

[0065] The preparation method of snow lotus extract includes the following steps: (1) The whole plant of snow lotus is dried, pulverized and passed through a 60-mesh sieve, frozen at -20℃ for 24 hours, and then thawed to obtain whole plant powder of snow lotus; (2) Choline chloride and glycerol were mixed at a molar ratio of 1:2 and stirred at 55°C for 1.5 h to obtain a transparent and homogeneous eutectic solvent. Then, water with a mass fraction of 20% was added to the eutectic solvent to obtain extraction solvent A. (3) The whole herb powder of snow lotus was mixed with extraction solvent A at a material-liquid ratio of 1g:28mL, and ultrasonic-microwave extraction was performed for 30min. The ultrasonic power was 400W, the ultrasonic frequency was 40kHz, the microwave power was 300W, and the extraction temperature was 50℃. The supernatant was collected to obtain the crude extract. (4) The crude extract was purified by elution using an AB-8 macroporous adsorption resin column. The elution and purification process was as follows: first, elution was performed with 3 column volumes of deionized water, followed by elution with 30%, 50%, and 70% ethanol solutions, respectively. The 50% eluent was collected. The extract was then concentrated under reduced pressure at 40°C to obtain the extract. (5) The extract, lecithin and cholesterol were mixed in a mass ratio of 1:3.5:0.4, homogenized three times at 550 bar, and dried to obtain snow lotus extract.

[0066] The preparation method of Polygonatum odoratum extract is as follows: S1: The root and stem of Polygonatum odoratum are crushed and mixed with 5 times the mass of ethanol for defatting. The mixture is refluxed at 40°C for 1.5 hours, filtered, and the ethanol liquid is discarded to obtain the defatted product. S2: The defatted product was mixed with water at a material-to-liquid ratio of 1g:18mL. A mixture of cellulase and pectinase at a mass ratio of 2:1 was added for enzymatic hydrolysis. The pH was adjusted to 5.5, the temperature was set at 50℃, and the time was 2h to inactivate the enzymes and obtain the enzymatic hydrolysate. S3: The enzymatic hydrolysate is purified by an AB-8 macroporous adsorption resin column. First, it is eluted with 3 times the amount of deionized water, and then eluted with a 45% (v / v) ethanol aqueous solution. The eluent of the ethanol aqueous solution is collected. Then, it is passed through ultrafiltration membranes with molecular weight cutoffs of 100 kDa and 30 kDa in sequence. The 30 kDa cutoff is collected, concentrated under reduced pressure, and dried to obtain the final product.

[0067] The method for preparing the composition includes the following steps: (a) Tanninase and Polygonatum odoratum extract were mixed at pH 6.0 to obtain mixture 1; (b) Mixture 1: Snow lotus extract and magnolia bark extract are mixed and dried to obtain a composition.

[0068] Example 2 A composition with the effects of freshening breath and whitening teeth is composed of the following raw materials: snow lotus extract, magnolia bark extract, Solomon's seal extract and tanninase in a mass ratio of 1:0.5:1:0.2.

[0069] The preparation method of snow lotus extract includes the following steps: (1) The whole plant of snow lotus is dried, pulverized and passed through a 40-mesh sieve, frozen at -25℃ for 20 hours, and then thawed to obtain whole plant powder of snow lotus; (2) Choline chloride and glycerol were mixed at a molar ratio of 1:2.5 and stirred at 50°C for 2 hours to obtain a transparent and homogeneous eutectic solvent. Then, water with a mass fraction of 18% was added to the eutectic solvent to obtain extraction solvent A. (3) The whole snow lotus powder and extraction solvent A were mixed at a ratio of 1g:25mL, and ultrasonic-microwave extraction was performed for 25min. The ultrasonic power was 420W, the ultrasonic frequency was 35kHz, the microwave power was 320W, and the extraction temperature was 45℃. The supernatant was collected to obtain the crude extract. (4) The crude extract was purified by elution using an AB-8 macroporous adsorption resin column. The elution and purification process was as follows: first, elution was performed with 3 column volumes of deionized water, followed by elution with 25%, 55%, and 65% ethanol solutions, respectively. The eluent with a volume fraction of 55% was collected. The extract was then concentrated under reduced pressure at 45°C to obtain the extract. (5) The extract, lecithin and cholesterol were mixed in a mass ratio of 1:2.5:0.6, homogenized three times at 500 bar, and dried to obtain snow lotus extract.

[0070] The preparation method of Polygonatum odoratum extract is as follows: S1: The root and stem of Polygonatum odoratum are crushed and mixed with 6 times the mass of ethanol for defatting. The mixture is refluxed at 35°C for 2 hours, filtered, and the ethanol liquid is discarded to obtain the defatted product. S2: The defatted product was mixed with water at a material-to-liquid ratio of 1g:20mL. A mixture of cellulase and pectinase at a mass ratio of 1:1 was added for enzymatic hydrolysis. The pH was adjusted to 5.0, the temperature was 45℃, and the time was 2.5h to inactivate the enzymes and obtain the enzymatic hydrolysate. S3: The enzymatic hydrolysate is purified by an AB-8 macroporous adsorption resin column. First, it is eluted with 2 times the amount of deionized water, and then eluted with a 60% (v / v) ethanol aqueous solution. The eluent of the ethanol aqueous solution is collected. Then, it is passed through ultrafiltration membranes with molecular weight cutoffs of 100 kDa and 30 kDa in sequence. The 30 kDa cutoff is collected, concentrated under reduced pressure, and dried to obtain the final product.

[0071] The method for preparing the composition includes the following steps: (a) Tanninase and Polygonatum odoratum extract were mixed at pH 5.8 to obtain mixture 1; (b) Mixture 1: Snow lotus extract and magnolia bark extract are mixed and dried to obtain a composition.

[0072] Example 3 A composition with the effects of freshening breath and whitening teeth is composed of the following raw materials: snow lotus extract, magnolia bark extract, Solomon's seal extract and tannin enzyme in a mass ratio of 3:0.2:2:0.05.

[0073] The preparation method of snow lotus extract includes the following steps: (1) The whole plant of snow lotus is dried, pulverized and passed through a 100-mesh sieve, frozen at -15℃ for 26 hours, and then thawed to obtain whole plant powder of snow lotus; (2) Choline chloride and glycerol were mixed at a molar ratio of 1:1.5 and stirred at 60°C for 1 h to obtain a transparent and homogeneous eutectic solvent. Then, water with a mass fraction of 25% was added to the eutectic solvent to obtain extraction solvent A. (3) The whole snow lotus herb powder and extraction solvent A were mixed at a material-liquid ratio of 1g:32mL, and ultrasonic-microwave extraction was performed for 35min. The ultrasonic power was 350W, the ultrasonic frequency was 45kHz, the microwave power was 280W, and the extraction temperature was 55℃. The supernatant was collected to obtain the crude extract. (4) The crude extract was purified by elution using an AB-8 macroporous adsorption resin column. The elution and purification process was as follows: first, elution was performed with 3 column volumes of deionized water, followed by elution with 35%, 45%, and 75% ethanol solutions, respectively. The eluent with a volume fraction of 45% was collected. The extract was then concentrated under reduced pressure at 45°C to obtain the extract. (5) The extract, lecithin and cholesterol were mixed in a mass ratio of 1:5:0.3, homogenized twice at 600 bar, and dried to obtain snow lotus extract.

[0074] The preparation method of Polygonatum odoratum extract is as follows: S1: The root and stem of Polygonatum odoratum are crushed and mixed with 4 times the mass of ethanol for defatting. The mixture is refluxed at 45°C for 1 hour, filtered, and the ethanol liquid is discarded to obtain the defatted product. S2: The defatted product was mixed with water at a material-to-liquid ratio of 1g:15mL. A mixture of cellulase and pectinase at a mass ratio of 3:1 was added for enzymatic hydrolysis. The pH was adjusted to 6.0, the temperature was 55℃, and the time was 1.5h to inactivate the enzyme and obtain the enzymatic hydrolysate. S3: The enzymatic hydrolysate is purified by an AB-8 macroporous adsorption resin column. First, it is eluted with 4 times the amount of deionized water, and then eluted with a 40% (v / v) ethanol aqueous solution. The eluent of the ethanol aqueous solution is collected. Then, it is passed through ultrafiltration membranes with molecular weight cutoffs of 100 kDa and 30 kDa in sequence. The 30 kDa cutoff is collected, concentrated under reduced pressure, and dried to obtain the final product.

[0075] The method for preparing the composition includes the following steps: (a) Tanninase and Polygonatum odoratum extract were mixed at pH 6.2 to obtain mixture 1; (b) Mixture 1: Snow lotus extract and magnolia bark extract are mixed and dried to obtain a composition.

[0076] Example 4 A toothpaste with the effects of freshening breath and whitening teeth has the following components and formulation as shown in Table 1: Table 1

[0077] The preparation method includes the following steps: S1: Add the humectant and thickener to a vacuum mixer and stir at low speed for 30 minutes until a uniform, semi-transparent gel phase is formed, to obtain component A; S2: Sweetener, solvent, stabilizer, preservative, antioxidant, and other components are stirred and dissolved evenly to obtain component B; S3: Abrasive and colorant are mixed to obtain component C; S4: A mixture of fragrance and cooling agent yields component D; S5: Add component B to component A and stir at medium speed until the system is homogeneous; under vacuum conditions of -0.08-0.095 MPa and shear rate of 2000 rpm, slowly add component C in batches and homogenize until no visible particles are visible; then add foaming agent and mix at low speed; finally add component D, degas under vacuum for 5-10 min, discharge, fill, and package to obtain the final product.

[0078] Example 5 A toothpaste with the effects of freshening breath and whitening teeth has the following components and formulation as shown in Table 2: Table 2

[0079] The preparation method is the same as in Example 4.

[0080] Example 6 A toothpaste with the effects of freshening breath and whitening teeth has the following components and formulation as shown in Table 3: Table 3

[0081] The preparation method is the same as in Example 4.

[0082] Comparative Example 1 A composition with the effects of freshening breath and whitening teeth is different from that in Example 1 in that the mass ratio of snow lotus extract, magnolia bark extract, Solomon's seal extract and tanninase is changed to 0.5:3:2.5:0.01; the rest is the same as in Example 1.

[0083] Comparative Example 2 A composition with the effects of freshening breath and whitening teeth is composed of snow lotus extract, and the rest is the same as in Example 1.

[0084] Comparative Example 3 A composition having the effects of freshening breath and whitening teeth is composed of the following raw materials: Magnolia officinalis extract, Polygonatum odoratum extract and tanninase in a mass ratio of 0.4:1.5:0.15; the rest is the same as in Example 1.

[0085] Comparative Example 4 A composition with the effects of freshening breath and whitening teeth, which differs from Example 1 in that the snow lotus extract is replaced with honeysuckle extract.

[0086] Comparative Example 5 A toothpaste with breath-freshening and teeth-whitening effects is described below. The only difference between this toothpaste and Example 4 is that the composition was prepared using the methods described in Comparative Examples 1-4. Details are shown in Table 4 below. Table 4

[0087] The rest is the same as in Example 4.

[0088] Comparative Example 6 Toothpaste was prepared according to Example 1 of Chinese patent application CN111700835A.

[0089] Test Example 1 Skin whitening test: (1) Preparation of staining solution First, dissolve the gastric mucoprotein in hot water. Then, add coffee, soy sauce, black tea, and ferric chloride, stir well, and store at 2-8℃ for later use. The staining solution has a shelf life of 3 days.

[0090] (2) Sample preparation Weigh the sample toothpaste into a 2000mL beaker, add deionized water to dissolve and stir until the toothpaste is evenly dispersed. The mass ratio of toothpaste to water is 1:1.6.

[0091] (3) Experimental process 1. Take several enamel grinding blocks and perform acid etching.

[0092] 2. Place the etched enamel abrasive block into the staining solution and stain it on a shaker at 37°C. The staining solution should be changed daily.

[0093] 3. After staining, remove the enamel abrasive block, rinse off any surface contaminants, and dry the surface. Keep the enamel abrasive block with evenly stained enamel and measure the whiteness value (L) of the stained enamel using a spectrophotometer within 10 minutes. Select L Tooth enamel grinding blocks with whiteness values ​​in the range of 45-55 were randomly assigned to a sample group and a control group, with 8 blocks in each group. After grouping, a two-sample t-test was used to compare the whiteness values ​​(L) between the two groups. To conduct the test, it is required that there is no significant difference between the two groups (P>0.05), and the color gradation of the enamel of the teeth before brushing is measured using a shade guide.

[0094] 4. After mounting the standard toothbrush and enamel abrasive block onto the brushing device, set the brushing device's reciprocating frequency to 100 r / min, and adjust the total weight of the toothbrush head and handle to 150 ± 2 g. Add an appropriate amount of toothpaste paste to each paste cup to submerge the enamel abrasive block. The sample group used the corresponding sample toothpaste (toothpaste prepared in Examples 4-6 and Comparative Example 5) for brushing, while the control group used deionized water for brushing.

[0095] 5. Use a brushing device to simulate brushing teeth externally for 7, 14, and 21 days.

[0096] 6. After brushing your teeth, remove the enamel polishing block, rinse and dry the surface. Use a shade guide to measure the shade of the enamel after brushing.

[0097] (4) Testing standards according to Figure 1 The colors were compared using color charts, and the color gradation scores for the color charts are shown in Table 5 below: Table 5

[0098] The test results are shown in Table 6 below: Table 6

[0099] Note: Compared with the control group, # P < 0.05 ## P < 0.01.

[0100] Compared with Example 4, % P < 0.05 %% P < 0.01.

[0101] As can be seen from the data in Table 6, the whitening effect of the toothpaste prepared in Examples 4-6 of this invention is significantly improved compared with the toothpaste prepared in Comparative Examples 5-6.

[0102] Test Example 2 Fresh breath test: (1) Test model: Hydroxyapatite flakes (HAP) (2) Main equipment: digital display constant temperature water bath, gas chromatograph.

[0103] (3) Experimental design and methods 1. Experimental Grouping This experiment included a negative control group and a sample group, with 5 parallel trials in each group.

[0104] 2. Biofilm pre-culture Take 50 15mL centrifuge tubes, place one HAP tablet in each tube, add 2mL of fresh saliva, cap, and incubate in a 37℃ water bath for 24h. Weigh 0.3g of thioglycolate medium and dissolve it in 10mL of deionized water. Then prepare a breath-generating simulation solution according to the ratio of thioglycolate medium:deionized water:fresh saliva of 2:13:85.

[0105] 3. After overnight incubation, remove the HAP tablets from the sample contact plate and place one tablet per well in a 12-well plate. Randomly group the plates into a negative control group and a sample group (toothpaste prepared in Examples 4-6 and Comparative Examples 5-6), with 5 tablets in each group. Dilute the toothpaste with deionized water at a ratio of 1:1.6 (toothpaste:deionized water) and mix thoroughly. According to the experimental groups, add 3 mL of the sample and negative control to each well of the 12-well plate, incubate for 3 minutes, remove the HAP tablets, rinse them in 5 mL of deionized water to remove any remaining toothpaste, and then transfer them to headspace vials. Add 2 mL of breath-generating simulation solution to each vial, seal the vial, and incubate in a 37°C water bath for 16 hours.

[0106] 4. Determination of Methanethiol Production The methanethiol in the headspace vial was detected using gas chromatography, and the peak area was used as an indicator to evaluate the sample's efficacy in reducing halitosis.

[0107] (4) Determination of methanethiol production The methanethiol in the headspace vial was detected using gas chromatography, and the peak area was used as an indicator to evaluate the sample's efficacy in reducing halitosis.

[0108] (5) The test results are shown in Table 7 below: Table 7

[0109] Note: Compared with the control group, # P < 0.05 ## P < 0.01.

[0110] Compared with Example 4, % P < 0.05 %% P < 0.01.

[0111] As can be seen from the data in Table 7, the fresh breath effect of the toothpaste prepared in Examples 4-6 of this invention is significantly improved compared with that of the toothpaste prepared in Comparative Examples 5-6.

[0112] Finally, it should be noted that the above content is only used to illustrate the technical solution of the present invention, and is not intended to limit the scope of protection of the present invention. Simple modifications or equivalent substitutions made by those skilled in the art to the technical solution of the present invention do not depart from the essence and scope of the technical solution of the present invention.

Claims

1. A composition having the effects of freshening breath and whitening teeth, characterized in that, It is made from the following raw materials: snow lotus extract, magnolia bark extract, Solomon's seal extract, and tannin enzyme; the mass ratio of the snow lotus extract, magnolia bark extract, Solomon's seal extract, and tannin enzyme is 1-3:0.2-0.5:1-2:0.05-0.2; The preparation method of the Polygonatum odoratum extract is as follows: Polygonatum odoratum rhizome is mixed with ethanol for defatting, the defatting product is enzymatically hydrolyzed, the enzymatic hydrolysate is purified by macroporous resin and then passed through ultrafiltration membranes with molecular weight cutoffs of 100kDa and 30kDa in sequence, and the 30kDa cutoff is collected to obtain the extract. The preparation method of the snow lotus extract includes the following steps: (1) After the whole plant of snow lotus is crushed, it is frozen at -25℃~-15℃ for 20-26h, and then thawed to obtain whole plant powder of snow lotus; (2) Choline chloride and glycerol are mixed in a molar ratio of 1:1.5-2.5 to obtain a transparent and homogeneous eutectic solvent. Then, water with a mass fraction of 18%-25% is added to the eutectic solvent to obtain extraction solvent A. (3) Mix the whole snow lotus powder with extraction solvent A, extract for 25-35 min, separate, collect the supernatant to obtain crude extract; (4) The crude extract was purified by elution using an AB-8 macroporous adsorption resin column. The eluent was collected, concentrated, and the extract was obtained. (5) The extract, lecithin and cholesterol are mixed in a mass ratio of 1:2.5-5:0.3-0.6, homogenized and dried to obtain snow lotus extract.

2. The composition according to claim 1, characterized in that, In step (3), the extraction is ultrasonic-microwave extraction, with ultrasonic power of 350-420W, ultrasonic frequency of 35-45kHz, microwave power of 280-320W, extraction temperature of 45-55℃, and extraction time of 25-35min; in step (4), the elution purification is as follows: first, elute with 2-4 column volumes of deionized water, and then elute sequentially with ethanol solutions of volume fractions of 25-35%, 45-55%, and 65-75%, and collect the eluent of volume fraction of 45-55%.

3. The composition according to claim 1, characterized in that, The preparation method of the Polygonatum odoratum extract is as follows: S1: After crushing the rhizome of Polygonatum odoratum, mix it with 4-6 times its weight of ethanol for defatting. Reflux defatting at 35-45℃ for 1-2 hours, filter, discard the ethanol liquid, and obtain the defatted product. S2: The defatted product is mixed with water at a material-to-liquid ratio of 1g:15-20mL. A mixture of cellulase and pectinase at a mass ratio of 1-3:1 is added for enzymatic hydrolysis. The pH is adjusted to 5-6, the temperature is 45-55℃, and the time is 1.5-2.5h to inactivate the enzyme and obtain the enzymatic hydrolysate. S3: The enzymatic hydrolysate is purified by an AB-8 macroporous adsorption resin column. First, it is eluted with 2-4 times deionized water, then eluted with a 40%-60% (v / v) ethanol aqueous solution, and the eluent is collected. Then, it is passed sequentially through ultrafiltration membranes with molecular weight cutoffs of 100kDa and 30kDa, and the 30kDa cutoff is collected. The solution is concentrated under reduced pressure and dried to obtain the final product.

4. The use of the composition according to any one of claims 1-3 in the preparation of oral care products.

5. The application according to claim 4, characterized in that, The oral care product is toothpaste, comprising the composition and excipients as described in any one of claims 1-3, wherein the mass ratio of the excipients to the composition is 97-99:1-3.

6. The application according to claim 5, characterized in that, The excipients are selected from at least one of humectants, abrasives, solvents, foaming agents, fragrances, thickeners, preservatives, stabilizers, colorants, cooling agents, sweeteners, and antioxidants; the humectant is selected from at least one of sorbitol, glycerin, polyethylene glycol, and propylene glycol; the abrasive is selected from at least one of hydrated silica, hydroxyapatite, sodium pyrophosphate, calcium carbonate, calcium bicarbonate, pearl powder, titanium dioxide, and aluminum hydroxide; the solvent is selected from at least one of water and polyethylene glycol; the foaming agent is selected from at least one of sodium lauroyl sarcosinate and sodium lauryl sulfate; the fragrance is a flavoring; the thickener is selected from cellulose gum, xanthan gum, and carboxylic acid. The product contains at least one of the following: guar gum, guar gum, sodium carboxymethyl cellulose, and carboxyethyl cellulose; the preservative is selected from at least one of sodium benzoate, potassium sorbate, phenoxyethanol, p-hydroxyacetophenone, methylparaben, and propylparaben; the stabilizer is selected from at least one of tetrasodium pyrophosphate, Tween, and Span; the colorant is selected from titanium dioxide; the cooling agent is selected from at least one of methyl diisopropylpropionamide, menthyl methylformamide, menthol, and peppermint oil; the sweetener is selected from at least one of trichlorogalactose, sodium saccharin, acesulfame potassium, stevioside, and mogroside; and the antioxidant is selected from at least one of stannous chloride, butylated hydroxytoluene, and vitamin E.

7. The application according to claim 6, characterized in that, The toothpaste preparation process includes the following steps: S1: Mix the humectant and thickener evenly to obtain component A; S2: Sweetener, solvent, stabilizer, preservative, antioxidant, and other components are stirred and dissolved evenly to obtain component B; S3: Abrasive and colorant are mixed to obtain component C; S4: Fragrance and cooling agent are mixed to obtain component D; S5: Add component B to component A, stir, then add component C and disperse homogenously; then add foaming agent and mix; finally add component D, degas, discharge, fill, and package to obtain the final product.

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