Formula and preparation method of natural micromolecular toothpaste for inhibiting porphyromonas gingivalis

Abstract

The invention relates to the technical field of oral care, and particularly discloses a formula and a preparation method of natural micromolecular toothpaste for inhibiting porphyromonas gingivalis. The formula of the toothpaste comprises a basic toothpaste component, a basic functional component capable of removing tartar and improving tooth strength, and an antibacterial compound, the basic toothpaste comprises the following components: a friction agent, a humectant, a paste agent, a sweetening agent and an aromatic agent; the basic functional component is prepared from strontium salt, disodium dihydrogen pyrophosphate and nano hydroxyapatite; the components of the antibacterial compound comprise epigallocatechin gallate and nano curcumin, and the components of the basic toothpaste do not contain ions such as Ca < 2 + >, Cu < 2 + >, Fe < 3 + >, Fe < 2 + > and Mg < 2 + >. Nano curcumin and EGCG are compounded, so that the technical problem that in the prior art, toothpaste for inhibiting porphyromonas gingivalis only mechanically added with many antibacterial components, the stable chemical property and dispersion state of the toothpaste cannot be guaranteed, and the antibacterial effect of the toothpaste cannot be broken through is solved.

Description

Technical Field

[0001] The invention relates to the technical field of oral care, and in particular to a natural small molecule toothpaste formula for inhibiting Porphyromonas gingivalis and a preparation method thereof. Background Art

[0002] With the development of society and the improvement of living standards, people are gradually paying attention to oral health. Oral diseases are usually caused by oral bacteria. The number of bacteria in the human oral cavity is very large and there are many types. Among them, Porphyromonas gingivalis is one of the important periodontal pathogens. They will squeeze out bacteria that are beneficial to teeth and replace them, causing gingival inflammation, which will eventually cause the gums to fall off the teeth. It is the main cause of toothache in adults. Not only that, in recent years, clinical epidemiological studies have shown that oral Porphyromonas gingivalis infection is directly related to sporadic Alzheimer's disease, especially in the elderly. In addition, animal experimental results also show that Porphyromonas gingivalis infection can secrete gingipains to accelerate AD pathological changes and cognitive impairment in AD model mice. Therefore, inhibiting the growth of oral Porphyromonas gingivalis and preventing its infection can prevent the occurrence of AD.

[0003] The simplest and most effective way to prevent oral diseases is to pay attention to oral hygiene and choose appropriate oral care products to effectively control the growth of oral bacteria, thereby effectively preventing the occurrence of oral diseases. Existing ordinary toothpaste and ordinary fluoride toothpaste have little inhibitory effect on Porphyromonas gingivalis; and because Porphyromonas gingivalis is an anaerobic bacterium that grows deep in the gums, it is difficult to inhibit its growth. For this reason, a series of anti-Porphyromonas gingivalis toothpastes or mouthwashes have appeared on the market, such as: Patent application number CN202010429960.5 discloses a natural small molecule mouthwash and toothpaste formula that inhibits Porphyromonas gingivalis, which adds curcumin / EGCG natural small molecules as antibacterial ingredients in the formula.

[0004] Although the toothpaste or mouthwash of the above patent can inhibit Porphyromonas gingivalis to a certain extent, curcumin and EGCG (epigallocatechin gallate) having the effect of inhibiting Porphyromonas gingivalis are only mechanically added to the toothpaste, and the properties of EGCG are not stable, and its thermal stability and light stability are very poor. It is only mechanically added to the toothpaste, and it is impossible to ensure that EGCG maintains stable chemical properties in the toothpaste. Therefore, its effective antibacterial effect will gradually weaken over time, and it is impossible to maximize the antibacterial ability of EGCG and achieve a better antibacterial effect. Curcumin has poor dispersibility. When the two are compounded, curcumin easily forms a precipitate, and it is impossible to add it evenly to the toothpaste. Therefore, the simple addition of curcumin and EGCG to the toothpaste in the prior art cannot achieve the expected antibacterial effect. Summary of the invention

[0005] The purpose of the present invention is to provide a natural small molecule toothpaste formula and preparation method for inhibiting Porphyromonas gingivalis, so as to solve the technical problem that the toothpaste for inhibiting Porphyromonas gingivalis in the prior art mentioned above only mechanically adds many antibacterial ingredients, cannot ensure its stable chemical properties and dispersion state, and thus its antibacterial effect cannot be improved.

[0006] In order to solve the above problems, the technical solutions adopted by the present invention are as follows: 1. A natural small molecule toothpaste formula for inhibiting Porphyromonas gingivalis, comprising a basic toothpaste component, a basic functional component capable of removing tartar and improving tooth strength, and an antibacterial complex;

[0007] The basic toothpaste components include abrasives, moisturizers, pastes, sweeteners and aromatics;

[0008] The basic functional components include strontium salt, disodium dihydrogen pyrophosphate, and nano-hydroxyapatite;

[0009] The antibacterial complex components include epigallocatechin gallate and nano-curcumin.

[0010] A method for preparing the natural small molecule toothpaste for inhibiting Porphyromonas gingivalis according to any one of claims 1 to 5, characterized in that it comprises the following steps:

[0011] Step 1: Classification of raw materials: Classify the raw materials of the basic toothpaste components and basic functional components in the formula of any one of claims 1 to 5 according to fat solubility and water solubility, and divide them into fat-soluble raw materials and water-soluble raw materials, except for disodium dihydrogen pyrophosphate;

[0012] Step 2: Mixing and heating the fat-soluble and water-soluble components: Mix the fat-soluble and water-soluble components in proportion and heat them to 75-90° C. The fat-soluble components are mixed and heated to obtain mixture 1, and the water-soluble components are mixed and heated to obtain mixture 2;

[0013] Step 3: Preparation of antibacterial compound: adding the antibacterial compound to disodium dihydrogen pyrophosphate and an appropriate amount of water-soluble ethylene glycol, heating to 35-50° C., stirring until uniform, to obtain mixture 3;

[0014] Step 4: Mixing and homogenizing: Slowly pour mixture 1 into mixture 2, homogenize (2000r / min, 5 minutes), and then stir to cool to room temperature. After cooling, add mixture 3 and deionized water (appropriate amount to 100%), stir evenly, and obtain mixture 4.

[0015] Step 5: Cooling and degassing: Cool the mixture 4 to room temperature, then perform vacuum degassing, and continue stirring until the mixture becomes a paste. Finally, fill it to obtain the final toothpaste product.

[0016] The beneficial effects of this embodiment are:

[0017] 1. In the prior art, the two ingredients that have the effect of inhibiting Porphyromonas gingivalis are only mechanically added to toothpaste, and EGCG (epigallocatechin gallate) is not stable and is prone to isomerization and oxidative degradation. Therefore, mechanically adding EGCG to toothpaste cannot ensure the stability of EGCG in toothpaste. After EGCG undergoes oxidative degradation and isomerization in toothpaste, it cannot achieve the expected effect of inhibiting Porphyromonas gingivalis when used again. Moreover, when curcumin is prepared as a curcumin solution, it cannot form a stable dispersed state and is prone to flocculation in the solution. After standing, there is obvious flocculent precipitation. Therefore, when curcumin is directly added to the toothpaste formula, the dispersed state of curcumin cannot be guaranteed; floccules of curcumin appear in the toothpaste to which curcumin is added, and it cannot be evenly distributed. In toothpaste, when used, only a part of the toothpaste is used. Whether this part contains curcumin and how much curcumin content is uncertain, resulting in unstable antibacterial effect. In the prior art, the two are mechanically added to toothpaste. Although a certain antibacterial effect can be played, the stability of the two cannot be guaranteed. The antibacterial effect cannot reach the expected maximization, and the effect is not ideal. It is impossible to break through the existing addition of a single component (adding curcumin or EGCG alone) D antibacterial effect. In this application, the two are deeply developed and studied, and it is found that the solution dispersion state of curcumin is unstable, but the dispersion state of nano-curcumin is very stable, and a stable solution state can be formed by long-term distribution, and curcumin has antioxidant properties, and can adsorb free radicals. The antioxidant effect of curcumin is mainly achieved by removing free radicals. Free radicals are groups or atoms with non-even electrons, which can contact EGCG, resulting in oxidative degradation of EGCG. Curcumin can capture these free radicals, thereby slowing down or preventing the oxidation process of EGCG. However, ordinary curcumin has poor dispersibility and cannot form a good mixed dispersion system with EGCG, so it cannot play a good protective effect on EGCG. Therefore, this application selects nano-curcumin and EGCG, and utilizes the dispersibility of nano-curcumin to disperse it well in the entire ointment system to create a stable environment for EGCG, so that the chemical properties and dispersion state of curcumin and EGCG in the toothpaste are more stable, and the antibacterial ability of curcumin and EGCG is maximized. According to experimental data, it breaks through the antibacterial effect of adding a single component.

[0018] 2. Compared with ordinary curcumin powder, nano-curcumin not only has better dispersibility, but also has a larger specific surface area. The antioxidant effect of curcumin is mainly achieved by scavenging free radicals, and the larger specific surface area gives curcumin more opportunities to contact with free radicals, so the EGCG stable environment it forms in toothpaste is better.

[0019] 3. In the prior art, curcumin is mechanically added, and there is a flocculent precipitate of turmeric color in the toothpaste. When using it, the user has a foreign body sensation, and the user experience is not good. However, nano-curcumin is added in the present application, and the dispersion effect is better. Therefore, there is no precipitation and no foreign body sensation, so the user experience is better.

[0020] 4. The present application found that EGCG is more easily oxidized and decomposed in an alkaline environment. Therefore, the use of disodium dihydrogen pyrophosphate, a slightly acidic substance, in toothpaste provides a better stable environment for EGCG and further prevents EGCG from oxidizing.

[0021] 5. There are many components in toothpaste, some of which are fat-soluble and some are water-soluble. Fat-soluble materials refer to those substances that are easily soluble in non-polar solvents such as oils and organic solvents, such as many oils and waxes. Water-soluble materials refer to those substances that are easily soluble in water, such as salt and sugar. There are obvious differences in the chemical properties of these two types of materials, so when they are mixed. If the two are directly mixed, different fat-soluble and water-soluble materials may undergo phase separation when mixed, and the mixing effect is not very good. Therefore, the two are first mixed separately to form a relatively good fat-soluble dispersion system (mixture 1) and a water-soluble dispersion system (mixture 2). When they are mixed again, the surfactant (sodium lauryl sulfate) is evenly distributed in the water-soluble dispersion system (mixture 2), and the molecular structure of the surfactant has two properties: one end is a hydrophilic group and the other end is a hydrophobic group; the hydrophobic group is often a non-polar group. Therefore, when mixed again, the hydrophobic group of the surfactant can well disperse the raw materials of the fat-soluble dispersion system (mixture 2), and the mixing effect is better.

[0022] 6. Since EGCG itself has unstable chemical properties and very poor thermal stability, toothpaste production requires heating to improve its fluidity in order to ensure uniform mixing. Therefore, the antibacterial complex is mixed separately from the fat-soluble and water-soluble components to avoid EGCG being at a high temperature during the production process, ensuring that it does not degrade or isomerize.

[0023] 7. Subsequent experiments have proved that the toothpaste of this application also has the functions of freshening breath, assisting gingival bleeding, and healing oral ulcers, and its functionality is richer.

[0024] Furthermore, the antibacterial complex component also includes an EGCG stabilizing formula that works synergistically with nano-curcumin to maintain the stability of EGCG. The antioxidant properties of nano-curcumin are combined with the EGCG stabilizing formula to create a suitable environment for maintaining the stability of EGCG.

[0025] Furthermore, the EGCG stabilization formula is polylysine hydrochloride, VC and polylysine. Experimental results show that the composite system formed by nano-curcumin, polylysine hydrochloride, VC and polylysine can maintain the stability of EGCG well. Therefore, after adding polylysine hydrochloride, VC and polylysine, the effective ingredients of EGCG can be retained for a longer time, and the antibacterial effect can be maximized.

[0026] Furthermore, the friction agent is silicon dioxide.

[0027] Furthermore, the ratio of epigallocatechin gallate to nano-curcumin in the antibacterial compound is 1: 1. Experiments have shown that the stability of EGCG can be improved after adding nano-curcumin, and the ratio of 1: 1 is the best.

[0028] Furthermore, the heating temperature in step 2 is 80°C.

[0029] Furthermore, the heating temperature in step 3 is 40°C.

[0030] Furthermore, in step 3, disodium dihydrogen pyrophosphate is first mixed evenly with an appropriate amount of water-soluble ethylene glycol, and then nano-curcumin, polylysine hydrochloride, VC and polylysine are added for mixing, and finally EGCG is added. EGCG is more easily oxidized and decomposed in an alkaline environment, so disodium dihydrogen pyrophosphate is first added to form an acidic environment, and nano-curcumin, polylysine hydrochloride, VC and polylysine are added to stabilize the formula to avoid the reduction of EGCG effective ingredients during the preparation process. BRIEF DESCRIPTION OF THE DRAWINGS

[0031] Figure 1 The following is a bar graph showing the antibacterial test results of Example 1 of the present invention and Comparative Examples 1, 2 and 3.

[0032] Figure 2 This is a comparison diagram of the curcumin dispersion experiment of the present invention.

[0033] Figure 3 is the absorption spectrum of nano-curcumin in the curcumin dispersion experiment of the present invention,

[0034] Figure 4 is the absorption spectrum of common curcumin in the curcumin dispersion experiment of the present invention,

[0035] Figure 5This is the mass spectrum of EGCG using high performance liquid chromatography in the configuration experiment of the EGCG stability test of the present invention. DETAILED DESCRIPTION

[0036] The following is a further detailed description through specific implementation methods: the technical solutions in the embodiments of the present invention are clearly and completely described. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0037] Implementation example Figures 1 to 5 As shown:

[0038] Example 1

[0039] A natural small molecule toothpaste formula for inhibiting Porphyromonas gingivalis includes three components: a basic toothpaste component, a basic functional component and an antibacterial complex.

[0040] The basic toothpaste components include the following components: silicon dioxide: 8% (abrasive, provides mild cleaning), glycerin: 5% (humectant, keeps moist), polyethylene glycol: 4% (humectant, increases hydration), sorbitol: 20% (humectant, provides a soft taste), liquid paraffin: 2% (ointment, lubricant, increases smoothness), sodium benzoate: 0.3% (preservative, extends shelf life), surfactant (sodium lauryl sulfate): 1.5% (ointment, foaming agent, enhances cleaning effect), xanthan gum: 0.3% (ointment, thickener, adjusts consistency), flavor: 1% (sweetener and fragrance, improves taste), pigment: 0.05%, zinc oxide: 0.3% (sweetener and fragrance, used for fresh breath).

[0041] The basic functional components include the following components: strontium salt: 2% (prevent tooth decay, enhance mineralization), disodium dihydrogen pyrophosphate: 6% (prevent tartar formation) and nano-hydroxyapatite: 1.5% (repair tooth enamel, enhance remineralization).

[0042] The antibacterial compound is composed of 0.5% curcumin, 0.5% EGCG and a stable EGCG formula. In this embodiment, the stable EGCG formula is 0.05% polylysine hydrochloride, 0.02% VC and 0.05% polylysine.

[0043] And replenish with water to 100%.

[0044] A method for preparing a natural small molecule toothpaste for inhibiting Porphyromonas gingivalis comprises the following steps:

[0045] Step 1: Classification of raw materials: Classify the raw materials of the basic toothpaste components and basic functional components in the formula of any one of claims 1 to 5 according to fat solubility and water solubility, and divide them into fat-soluble raw materials and water-soluble raw materials, except for disodium dihydrogen pyrophosphate;

[0046] Fat-soluble components: liquid paraffin (2%), polyethylene glycol (4%), flavor 1%, pigment: 0.05%; water-soluble components: sorbitol (20%), surfactant (sodium lauryl sulfate) 1.5%, disodium dihydrogen pyrophosphate (6%), silicon dioxide (8%), glycerin (5%), zinc oxide 0.3%, strontium salt 2%, sodium benzoate (0.3%) and xanthan gum (0.3%).

[0047] Step 2: Mixing and heating the fat-soluble and water-soluble components: Mix the fat-soluble and water-soluble components in proportion and heat them to 80° C. The fat-soluble components are mixed and heated to obtain a mixture 1, and the water-soluble components are mixed and heated to obtain a mixture 2;

[0048] Step 3: Preparation of antibacterial compound: adding the antibacterial compound to disodium dihydrogen pyrophosphate and an appropriate amount of water-soluble ethylene glycol, heating to 40° C., stirring until uniform, to obtain a mixture 3;

[0049] In step 3, disodium dihydrogen pyrophosphate and an appropriate amount of water-soluble ethylene glycol are first mixed evenly, and then nano-curcumin, polylysine hydrochloride, VC and polylysine are added and mixed, and finally EGCG is added.

[0050] Step 4: Mixing and homogenizing: Slowly pour mixture 1 into mixture 2, homogenize (2000r / min, 5 minutes), and then stir to cool to room temperature. After cooling, add mixture 3 and deionized water (appropriate amount to 100%), stir evenly, and obtain mixture 4.

[0051] Step 5: Cooling and degassing: Cool the mixture 4 to room temperature, then perform vacuum degassing, and continue stirring until the mixture becomes a paste. Finally, fill it to obtain the final toothpaste product.

[0052] In the above process, EGCG and curcumin are used as natural antibacterial and anti-inflammatory ingredients to enhance the antibacterial effect of toothpaste, and nano-hydroxyapatite is introduced to repair tooth enamel, ensuring the product's multiple functions such as antibacterial, whitening, and repairing tooth enamel.

[0053] Example 2

[0054] A natural small molecule toothpaste formula for inhibiting Porphyromonas gingivalis includes three components: a basic toothpaste component, a basic functional component and an antibacterial complex.

[0055] The basic toothpaste components include the following: silicon dioxide: 8% (abrasive, provides mild cleaning), glycerin: 5% (humectant, keeps moist), polyethylene glycol: 4% (humectant, increases hydration), sorbitol: 20% (humectant, provides a soft taste), liquid paraffin: 2% (lubricant, increases smoothness), sodium benzoate: 0.3% (preservative, extends shelf life), surfactant (sodium lauryl sulfate), 1.5% (foaming agent, enhances cleaning effect), xanthan gum: 0.3% (thickener, adjusts consistency), flavor: 1% (improves taste), pigment: 0.05%, zinc oxide: 0.3% (for fresh breath).

[0056] The basic functional components include the following components: strontium salt: 2% (prevent tooth decay, enhance mineralization), disodium dihydrogen pyrophosphate: 6% (prevent tartar formation) and nano-hydroxyapatite: 1.5% (repair tooth enamel, enhance remineralization).

[0057] The antibacterial compound is composed of 0.5% curcumin, 0.5% EGCG and a stable EGCG formula. In this embodiment, the stable EGCG formula is 0.05% polylysine hydrochloride, 0.02% VC and 0.05% polylysine.

[0058] And replenish with water to 100%.

[0059] Example 3

[0060] A natural small molecule toothpaste formula for inhibiting Porphyromonas gingivalis includes three components: a basic toothpaste component, a basic functional component and an antibacterial complex.

[0061] The basic toothpaste components include the following: silicon dioxide: 8% (abrasive, provides mild cleaning), glycerin: 5% (humectant, keeps moist), polyethylene glycol: 4% (humectant, increases hydration), sorbitol: 20% (humectant, provides a soft taste), liquid paraffin: 2% (lubricant, increases smoothness), sodium benzoate: 0.3% (preservative, extends shelf life), surfactant (sodium lauryl sulfate), 1.5% (foaming agent, enhances cleaning effect), xanthan gum: 0.3% (thickener, adjusts consistency), flavor: 1% (improves taste), pigment: 0.05%, zinc oxide: 0.3% (for fresh breath).

[0062] The basic functional components include the following components: strontium salt: 2% (prevent tooth decay, enhance mineralization), disodium dihydrogen pyrophosphate: 6% (prevent tartar formation) and nano-hydroxyapatite: 1.5% (repair tooth enamel, enhance remineralization).

[0063] The antibacterial compound is composed of 0.5% curcumin, 0.5% EGCG and a stable EGCG formula. In this embodiment, the stable EGCG formula is 0.05% polylysine hydrochloride, 0.02% VC and 0.05% polylysine.

[0064] And replenish with water to 100%.

[0065] Comparative Example 1

[0066] The difference between Comparative Example 1 and Example 1 is that the antibacterial compound is 1% tinidazole, and the other contents are exactly the same as those of Example 1.

[0067] Comparative Example 2

[0068] The difference between Comparative Example 2 and Example 1 is that the antibacterial compound is 1% ordinary curcumin, and the rest is exactly the same as Example 1.

[0069] Comparative Example 3

[0070] The difference between Comparative Example 2 and Example 1 is that the antibacterial compound contains 1% EGCG, and the other contents are exactly the same as those of Example 1.

[0071] In order to compare the combined antibacterial effect of nano-curcumin and EGCG in the toothpaste of the present application, the present application conducted the following verification test:

[0072] 1. Purpose of the experiment

[0073] The antibacterial effects of curcumin, epigallocatechin gallate (EGCG) and their combination were examined.

[0074] 5. Experimental equipment

[0075] Equipment Name model Anaerobic incubator DNP-9052 Centrifuge 5430R ELISA reader InfiniteM200 Sterile flat bottom 96-well plate Beaver

[0076] Procedure

[0077] 3.1 Reagent configuration

[0078] Example 1, Comparative Example 1, Comparative Example 2 and Comparative Example 3 prepared toothpaste respectively: 40g of toothpaste was weighed and dissolved in 1000ml, filtered and sterilized, and then divided for use (40g / L).

[0079] 3.2 Bacterial culture

[0080] The strain P.gingialis33277 was inoculated into a TSB culture plate containing 5% sterile defibrinated sheep blood, 5% yeast extract, 5ug / ml hemin and 0.5ug / m vitamin K. After culturing at 37°C in an anaerobic environment (10% H2, 10% CO2 and 80% N2) for 6 days, the bacteria were subcultured in liquid TSB±E base containing 5μg / m hemin and 0.5pgimL vitamin K, and cultured anaerobically at 37°C for 16-18h. The bacteria were collected, centrifuged at 4°C, 3000rpm / min for 5min, and then the bacterial concentration was adjusted to 3x10mL (625nm absorbance 0.16-0.20) using an MCF turbidimetric tube for use.

[0081] 3.3 Layout

[0082]

[0083]

[0084] Add 100 μl of the bacterial solution prepared in step 3.2 to each well of the plate.

[0085] 3.4 On-machine testing

[0086] The culture medium prepared in 3.3 was cultured in an anaerobic environment for 72 hours. After the culture was completed, the absorbance value was detected at 625 nm using UV-visible spectrophotometry.

[0087]

[0088] The column chart drawn is as follows Figure 1 Shown

[0089] From the above data, it can be seen that if toothpaste containing antibacterial complex is not added to the culture medium, the culture medium prepared in 3.3 is cultured in an anaerobic environment for 72 hours. After the culture is completed, the absorbance value is detected at 625nm by UV-visible spectrophotometry, and its absorbance hovers around 0.64. However, the values ​​of the culture medium with antibacterial complex toothpaste added are lower than this data.

[0090] However, the inhibitory effect of the present application on Porphyromonas gingivalis is significantly higher than that of ordinary curcumin and EGCG used alone. At 40g / L, the average absorbance of the present application is only 0.2126, while that of curcumin used alone is 0.2809, and that of EGCG used alone is 0.5435. The effect of inhibiting Porphyromonas gingivalis is 24% higher than that of curcumin used alone, and its antibacterial effect is higher than that of EGCG used alone. Compared with tinidazole (average value is 0.3924), a commonly used antibacterial agent in toothpaste on the market, its antibacterial effect is also 45.8% higher. Therefore, the present application has a good antibacterial effect of inhibiting Porphyromonas gingivalis.

[0091] The antibacterial effect of EGCG showed the worst value among the four. It is speculated that the culture medium prepared in 3.3 may be isomerized and degraded during the 72h culturing in an anaerobic environment, which greatly reduced its antibacterial performance.

[0092] This application involves other related experiments

[0093] 1. Curcumin dispersion experiment

[0094] Ordinary curcumin powder was dissolved in an ethanol-water (50%) solvent. Since turmeric is insoluble in water, after standing for 12 hours, there was an obvious precipitate. The nano-curcumin prepared by hydrothermal synthesis of ordinary curcumin, the solvents were water and ethanol, and the reaction mode was as follows:

[0095]

[0096] The prepared curcumin quantum dots are bright yellow and clear in solution. Figure 2 As shown, the two were analyzed by UV-visible absorption spectroscopy. Figure 3 As shown, ordinary curcumin Figure 4 As shown in the results, the absorption peak of nano-curcumin at 340nm is significantly higher than that of ordinary curcumin, proving that the dispersion stability of nano-curcumin is higher.

[0097] 2. EGCG stability test

[0098] EGCG is not stable in nature, and its thermal stability and light stability are very poor. If it is directly added to toothpaste, it will undergo oxidative degradation and isomerization. When used for a long time, its effective time is very short. After opening and using, the toothpaste is not used up, and its effective ingredients are already very low. Therefore, stability tests are needed to explore the stability environment of EGCG.

[0099] 1. Factors affecting EGCG stability:

[0100]

[0101]

[0102] 2. The conditions that can improve the stability of tea polyphenols (EGCG) are as follows:

[0103] Protect from light, low temperature, pH value less than 5, citric acid, vitamin C, polylysine, polylysine hydrochloride, arginine, lactoferrin, carbomer 940, collagen peptide, CAB35 (cocamidopropyl betaine), casein peptide.

[0104] 3. Stability formula screening:

[0105]

[0106] After EGCG was prepared, since the solution of EGCG itself was anhydrous, in order to detect the presence of EGCG before the experiment, the prepared EGCG solution was analyzed by high performance liquid chromatography. The results are as follows: Figure 5 As mentioned above, it is proved that it contains EGCG.

[0107] 4. Accelerated stability test

[0108] Since EGCG itself is not stable enough, it is easy to change color and cause pH changes when isomerization and oxidative decomposition occur. Therefore, the stability of EGCG was judged by observing the color changes of the samples every day, whether precipitation occurred, and pH value testing at 50°C for 2 weeks.

[0109] 5. Experimental Results

[0110]

[0111] Since EGCG will change color and precipitate after oxidation or isomerization, the experimental results are based on the color change time and precipitation state observed by naked eye; the experimental results data show that in the first group of test samples, EGCG is easily severely degraded and isomerized at 50°C in just one hour without any additives, with a significant color change, and the solution changes from clear to dark black, and brown precipitates appear after 6 hours.

[0112] In the second group of test samples with the addition of polylysine and VC, the stability of EGCG was significantly improved, and the first color change phenomenon occurred after 1 day. If it is at room temperature, its stability can be greatly prolonged. Therefore, polylysine and VC can greatly improve its stability.

[0113] As for the third component, the best performance was achieved in the 5th test sample of VC + polylysine + carbomer, which took 3 days to change color, but still showed slight precipitation after two weeks. For the 7th group (arginine + polylysine + VC) and the 8th group (polylysine hydrochloride + polylysine + VC), the first color change time was 4 days later, and no precipitation appeared after two weeks of acceleration.

[0114] When the formulas of Group 7 (arginine + polylysine + VC) and Group 8 (polylysine hydrochloride + polylysine + VC) with better effects were mixed with nano-curcumin to form Group 11 and Group 12 test samples, it was found that the effect of adding nano-curcumin to the test sample of Group 11 (arginine polylysine + VC) was the same as that of the scheme of Group 7, but after two weeks of acceleration, the test sample of Group 12 only showed a light yellow color, compared with the dark yellow color of the previous Group 7 and Group 8, and its stability was greatly improved.

[0115] The above is only an embodiment of the present invention, and the common knowledge such as the known specific structure and characteristics in the scheme is not described in detail here. It should be pointed out that for those skilled in the art, several deformations and improvements can be made without departing from the structure of the present invention, which should also be regarded as the protection scope of the present invention, and these will not affect the effect of the implementation of the present invention and the practicality of the patent. The scope of protection required by this application shall be based on the content of its claims, and the specific implementation methods and other records in the specification can be used to interpret the content of the claims.

Claims

1. A natural small molecule toothpaste formula for inhibiting Porphyromonas gingivalis, characterized in that: It includes 40-45% basic toothpaste components, 8-10% basic functional components that can remove tartar and improve tooth strength, and 5-7% antibacterial complexes, and is supplemented to 100% with water; The basic toothpaste components include 6-10% abrasive, 28-30% moisturizer, 3-4% paste, and 1-2% sweetener and fragrance; The basic functional component includes 5-7% disodium dihydrogen pyrophosphate; The antibacterial complex components include epigallocatechin gallate and nano-curcumin.

2. The natural small molecule toothpaste formula for inhibiting Porphyromonas gingivalis according to claim 1, characterized in that: The antibacterial complex component also includes an EGCG stabilizing formula that works synergistically with nano-curcumin to maintain the stability of EGCG.

3. The natural small molecule toothpaste formula for inhibiting Porphyromonas gingivalis according to claim 2, characterized in that: The EGCG stabilizing formula is polylysine hydrochloride, polylysine and VC.

4. The natural small molecule toothpaste formula for inhibiting Porphyromonas gingivalis according to claim 1, characterized in that: The friction agent is silicon dioxide, and the basic functional component also includes 1-2% nano hydroxyapatite.

5. The natural small molecule toothpaste formula for inhibiting Porphyromonas gingivalis according to claim 1, characterized in that: The ratio of epigallocatechin gallate to nano-curcumin in the antibacterial complex is 1:

1.

6. A method for preparing the natural small molecule toothpaste for inhibiting Porphyromonas gingivalis according to any one of claims 1 to 5, characterized in that: The following steps are involved: Step 1: Classification of raw materials: Classify the raw materials of the basic toothpaste components and basic functional components in the formula of any one of claims 1 to 5 according to fat solubility and water solubility, and divide them into fat-soluble raw materials and water-soluble raw materials, except for disodium dihydrogen pyrophosphate; Step 2: Mixing and heating the fat-soluble and water-soluble components: Mix the fat-soluble and water-soluble components in proportion and heat them to 75-90° C. The fat-soluble components are mixed and heated to obtain mixture 1, and the water-soluble components are mixed and heated to obtain mixture 2; Step 3: Preparation of antibacterial compound: adding the antibacterial compound to disodium dihydrogen pyrophosphate and an appropriate amount of water-soluble ethylene glycol, heating to 35-50° C., stirring until uniform, to obtain mixture 3; Step 4: Mixing and homogenizing: Slowly pour mixture 1 into mixture 2, homogenize (2000r / min, 5 minutes), and then stir to cool to room temperature. After cooling, add mixture 3 and deionized water (appropriate amount to 100%), stir evenly, and obtain mixture 4. Step 5: Cooling and degassing: Cool the mixture 4 to room temperature, then perform vacuum degassing, and continue stirring until the mixture becomes a paste. Finally, fill it to obtain the final toothpaste product.

7. The method for preparing a natural small molecule toothpaste for inhibiting Porphyromonas gingivalis according to claim 6, characterized in that: The heating temperature in step 2 is 80°C.

8. The method for preparing a natural small molecule toothpaste for inhibiting Porphyromonas gingivalis according to claim 6, characterized in that: The heating temperature in step 3 is 40°C.

9. The method for preparing a natural small molecule toothpaste for inhibiting Porphyromonas gingivalis according to claim 6, characterized in that: In the step 3, disodium dihydrogen pyrophosphate and an appropriate amount of water-soluble ethylene glycol are first mixed evenly, and then nano-curcumin, polylysine hydrochloride, VC and polylysine are added and mixed, and finally EGCG is added.

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