An oral care composition and method of making the same

Abstract

The present application belongs to the technical field of oral care, and particularly relates to an oral care composition and a preparation method thereof. The oral care composition comprises, by mass percentage, chitosan oligosaccharide 0.1-0.3%, sea hao polysaccharide 0.08-0.14%, forskolin 0.07-0.12%, corn sprout extract 0.05-0.09%, thickening agent 1-3%, humectant 40-50%, and the balance being water. The oral care composition of the present application can effectively inhibit the activity of glucosyltransferase, inhibit the production of dextran, interfere with the formation process of dental plaque, and reduce the adhesion sites of pathogenic bacteria in the oral cavity. In addition, the composition of the present application can promote the proliferation and repair of oral mucosa epithelial cells, and help repair oral mucosa damage. Furthermore, the use of each component in the composition of the present application can balance the oral microbial flora, while achieving the effect of inhibiting pathogenic bacteria and improving the oral environment.

Description

Technical Field

[0001] This invention belongs to the field of oral care technology, and in particular relates to an oral care composition and its preparation method. Background Technology

[0002] The oral cavity is an open and complex micro-ecosystem, in which the formation of dental plaque biofilm and the damage to the integrity of the oral mucosa are two core and interconnected oral health issues. Dental plaque is a biofilm community mainly composed of bacteria that continuously forms on the tooth surface, restorations, or gingival margin, and it is a necessary condition for the occurrence of dental caries. Its continuous acid production can lead to demineralization and even disintegration of tooth hard tissues. At the same time, dental plaque and its metabolites can also directly irritate gingival tissue, causing reversible inflammation such as redness, bleeding on probing, and edema. A truly healthy oral environment requires the unity of three aspects: tooth cleaning and protection, integrity and health of the oral mucosa, and dynamic balance of the microbial community. Dental plaque accumulation aggravates gingival inflammation, thereby damaging the gingival mucosa; while the damaged oral mucosa provides a breeding ground for pathogenic bacteria, further promoting the formation of dental plaque.

[0003] Most oral care products on the market today have relatively limited functions. For example, fluoride toothpaste primarily focuses on enhancing the acid resistance of tooth enamel to prevent cavities; mouthwashes containing antibacterial agents such as cetylpyridinium chloride focus on broad-spectrum bactericidal action, but long-term use may disrupt the oral microecological balance. They are ill-suited to addressing the complex interplay of tooth surface and mucosal issues within the oral microenvironment.

[0004] Therefore, there is an urgent need to develop a novel oral care composition. This composition can not only effectively promote the proliferation and repair of oral mucosal epithelial cells and strengthen the oral cavity's own defense barrier, but also regulate the balance of oral flora, inhibiting pathogenic bacteria while protecting beneficial bacteria, and providing effective physical isolation and protection for damaged mucosa. Summary of the Invention

[0005] To overcome the shortcomings of existing technologies, the primary objective of this invention is to provide an oral care composition. This invention creatively combines forscorin, corn germ extract, chitosan oligosaccharide, and sea lettuce polysaccharide. Through the precise synergy between these components, it not only reduces the attachment sites of pathogenic bacteria in the oral cavity but also promotes the proliferation and repair of oral mucosal epithelial cells, regulates the oral flora, and inhibits the growth of pathogenic bacteria.

[0006] Another object of the present invention is to provide a method for preparing an oral care composition. This preparation process is simple, easy to operate, and plays an important role in practical production.

[0007] The objective of this invention is achieved through the following technical solution:

[0008] An oral care composition, by weight percentage, comprises the following components: 0.1-0.3% chitosan oligosaccharide, 0.08-0.14% seaweed polysaccharide, 0.07-0.12% forscoringin, 0.05-0.09% corn germ extract, 1-3% thickener, 40-50% humectant, and the balance being water.

[0009] Furthermore, the preparation method of the corn sprout extract is as follows:

[0010] (1) Soak corn seeds in water and then remove them for later use;

[0011] (2) Place the corn seeds soaked in step (1) into a germination box lined with absorbent paper for cultivation;

[0012] (3) After the sprouts reach 1-2 cm in length, collect the corn sprouts, wash them, dry and crush them, add them to an ethanol aqueous solution, heat and reflux them, collect the reflux liquid, concentrate it and freeze dry it to obtain the corn sprout extract.

[0013] Furthermore, in step (1), the soaking temperature is 15-18℃ and the soaking time is 20-24h.

[0014] Furthermore, in step (2), the cultivation is carried out in the dark, with a temperature of 25-28°C and a humidity of 80-85%.

[0015] Further, in step (3), the amount of the ethanol aqueous solution added is 6-10 times the mass of the corn sprouts, and the mass concentration of the ethanol aqueous solution is 70-80%.

[0016] Furthermore, in step (3), the drying temperature is 45-55℃; the heating reflux temperature is 80-90℃, and the time is 3-5h.

[0017] Furthermore, the average molecular weight of the chitosan oligosaccharide is 1000.

[0018] Furthermore, the thickener is any one of hydroxyethyl cellulose, carrageenan, or guar gum.

[0019] Furthermore, the moisturizer is any one of glycerin, polyethylene glycol, or sorbitol.

[0020] This invention employs a method for preparing an oral care composition, comprising the following steps:

[0021] According to the formula, mix chitosan oligosaccharide, sea hawthorn polysaccharide, forscorin, and corn germ extract evenly, then add thickener, humectant, and water, and stir evenly to obtain the final product.

[0022] The present invention has the following advantages over the prior art:

[0023] 1. The oral care composition of this invention contains forscolin. Glucosyltransferases in the oral cavity can be adsorbed onto the tooth surface and maintain their enzyme activity. Glucosyltransferases can use sucrose as a substrate, catalyzing its decomposition and synthesizing the released glucose monomers into sticky dextran. Dextran helps bacteria adhere to the oral cavity, promoting the formation of dental plaque biofilm. Dental plaque provides a protective barrier for oral pathogens, thereby exacerbating oral problems such as tooth decay. Experiments have shown that forscolin can effectively inhibit the activity of glucosyltransferases, inhibit dextran production, interfere with the formation process of dental plaque, and reduce attachment sites for oral pathogens, thus helping to maintain oral health.

[0024] 2. The oral care composition of this invention contains corn sprout extract. Experiments have shown that corn sprout extract has excellent oral repair capabilities. It can promote the proliferation and repair of oral mucosal epithelial cells, help repair oral mucosal damage, thereby accelerating wound healing and effectively maintaining the health of the oral mucosa.

[0025] 3. To enhance the nursing effect, the oral care composition of this invention innovatively combines chitosan oligosaccharide and sea hazelnut polysaccharide. On the one hand, chitosan oligosaccharide can precisely inhibit oral pathogens, and synergistically with sea hazelnut polysaccharide to balance the oral microbiota, inhibit the growth of oral pathogens, and further improve the oral environment. On the other hand, sea hazelnut polysaccharide has good film-forming properties, which not only provides physical isolation for damaged oral mucosa and relieves pain, but also helps the active ingredients in the nursing composition, such as forscorin and corn germ extract, to work on the oral mucosal surface, thereby achieving long-lasting repair. Detailed Implementation

[0026] The present invention will be further described in detail below with reference to embodiments, but the implementation of the present invention is not limited thereto. Unless otherwise specified, the reagents, methods, and equipment used in the present invention are conventional reagents, methods, and equipment in this technical field. Test methods in the following embodiments that do not specify specific experimental conditions are generally performed according to conventional experimental conditions or experimental conditions recommended by the manufacturer. Unless otherwise specified, the reagents and raw materials used in the present invention are commercially available.

[0027] Example 1

[0028] An oral care composition comprising, by weight percentage: 0.2% chitosan oligosaccharide (average molecular weight 1000), 0.1% seaweed polysaccharide, 0.1% forscoringin, 0.07% corn germ extract, 2% thickener (hydroxyethyl cellulose), 45% humectant (glycerin), and the balance being water.

[0029] The preparation method of the corn sprout extract is as follows:

[0030] (1) Take plump and uniformly sized corn seeds, add them to water, soak them at 18℃ for 20 hours, and then take them out for later use.

[0031] (2) Place the corn seeds soaked in step (1) into a germination box lined with absorbent paper and cultivate them in the dark at 25°C and 85% humidity. During the cultivation period, observe the seeds daily and replenish water as needed based on the dryness of the absorbent paper.

[0032] (3) After the sprouts reach 1.5cm in length, collect the corn sprouts, wash them with water, dry them at 50℃, pulverize them to obtain corn sprout powder, add them to an ethanol aqueous solution (75wt%) with 8 times the mass of the corn sprouts, heat and reflux at 85℃ for 4h, collect the reflux liquid, concentrate it and freeze dry it to obtain corn sprout extract.

[0033] The preparation method of the *Hailaria lobata* polysaccharide is as follows:

[0034] a. The preparation process of sea hay polysaccharide is as follows: sea hay is washed, dried, crushed, and sieved to obtain sea hay powder;

[0035] b. Add seaweed powder to water at a ratio of 1g:25mL, soak for 24h, filter to remove residue, centrifuge the filtrate (3000rpm, 20min) and collect the supernatant; concentrate the supernatant to 8% of its original volume, then add 3 times its volume of anhydrous ethanol, precipitate for 12h, and centrifuge again (3000rpm, 20min).

[0036] c. Dissolve the precipitate after centrifugation in water, then add Sevage reagent for deproteinization treatment, then centrifuge at 3000 rpm for 20 min, repeat 3 times, and finally concentrate the filtrate under reduced pressure and freeze dry to obtain sea hay polysaccharide.

[0037] This embodiment also provides a method for preparing the above-mentioned oral care composition, including the following steps:

[0038] According to the formula, mix chitosan oligosaccharide, sea hawthorn polysaccharide, forscorin, and corn germ extract evenly, then add thickener, humectant, and water, and stir evenly to obtain the final product.

[0039] Example 2

[0040] An oral care composition comprising, by weight percentage: 0.1% chitosan oligosaccharide, 0.08% seaweed polysaccharide, 0.07% forscoringin, 0.05% corn germ extract, 1% thickener (carrageenan), 40% humectant (polyethylene glycol), and the balance being water.

[0041] The preparation method of the corn sprout extract is as follows:

[0042] (1) Take plump and uniformly sized corn seeds, add them to water, soak them at 15℃ for 24 hours, and then take them out for later use.

[0043] (2) Place the corn seeds soaked in step (1) into a germination box lined with absorbent paper and cultivate them in the dark at 26°C and 80% humidity. During the cultivation period, observe the seeds daily and replenish water as needed based on the dryness of the absorbent paper.

[0044] (3) After the sprouts reach 1 cm in length, collect the corn sprouts, wash them with water, dry them at 45°C, pulverize them to obtain corn sprout powder, add them to an ethanol aqueous solution (70 wt%) with a mass of 6 times that of the corn sprouts, heat them at 80°C and reflux for 5 h, collect the reflux liquid, concentrate it and freeze dry it to obtain corn sprout extract.

[0045] The preparation method of the polysaccharide from *Hailweed* is the same as in Example 1.

[0046] This embodiment also provides a method for preparing the above-mentioned oral care composition, including the following steps:

[0047] According to the formula, mix chitosan oligosaccharide, sea hawthorn polysaccharide, forscorin, and corn germ extract evenly, then add thickener, humectant, and water, and stir evenly to obtain the final product.

[0048] Example 3

[0049] An oral care composition comprising, by weight percentage: 0.3% chitosan oligosaccharide, 0.14% seaweed polysaccharide, 0.12% forscoringin, 0.09% corn germ extract, 3% thickener (guar gum), 50% humectant (sorbitol), and the balance being water.

[0050] The preparation method of the corn sprout extract is as follows:

[0051] (1) Take plump and uniformly sized corn seeds, add them to water, soak them at 16℃ for 22 hours, and then take them out for later use;

[0052] (2) Place the corn seeds soaked in step (1) into a germination box lined with absorbent paper and cultivate them in the dark at 28°C and 85% humidity. During the cultivation period, observe the seeds daily and replenish water as needed based on the dryness of the absorbent paper.

[0053] (3) After the sprouts reach 2cm in length, collect the corn sprouts, wash them with water, dry them at 55℃, pulverize them to obtain corn sprout powder, add them to an ethanol aqueous solution (80wt%) with 10 times the mass of the corn sprouts, heat and reflux at 90℃ for 3h, collect the reflux liquid, concentrate it and freeze dry it to obtain corn sprout extract.

[0054] The preparation method of the polysaccharide from *Hailweed* is the same as in Example 1.

[0055] This embodiment also provides a method for preparing the above-mentioned oral care composition, including the following steps:

[0056] According to the formula, mix chitosan oligosaccharide, sea hawthorn polysaccharide, forscorin, and corn germ extract evenly, then add thickener, humectant, and water, and stir evenly to obtain the final product.

[0057] Comparative Example 1

[0058] Comparative Example 1 provides an oral care composition comprising, by weight percentage: 0.2% chitosan oligosaccharide, 0.1% seaweed polysaccharide, 0.07% corn germ extract, 2% thickener (hydroxyethyl cellulose), 45% humectant (glycerin), and the balance being water. This omits the addition of forscoring.

[0059] Comparative Example 1 also provides a method for preparing the above-mentioned oral care composition, with the specific preparation steps being the same as in Example 1.

[0060] Comparative Example 2

[0061] Comparative Example 2 provides an oral care composition comprising, by weight percentage: 0.2% chitosan oligosaccharide, 0.1% seaweed polysaccharide, 0.1% forscoringin, 2% thickener (hydroxyethyl cellulose), 45% humectant (glycerin), and the balance being water. This omits the addition of corn sprout extract.

[0062] Comparative Example 2 also provides a method for preparing the above-mentioned oral care composition, with the specific preparation steps being the same as in Example 1.

[0063] Experimental Example 1

[0064] To verify the film-forming properties of the oral care compositions obtained in Examples 1-3 and Comparative Examples 1-2 of the present invention, the following experiments were conducted:

[0065] The oral care compositions obtained in Examples 1-3 and Comparative Examples 1-2 of this invention were applied to the surface of culture dishes and placed in a constant temperature incubator at 37°C for incubation. The time required for the formation of a complete and uniform film on the surface of the culture dish was observed and recorded (observed every 10 seconds), i.e. the film formation time. The results are shown in Table 1.

[0066] Table 1

[0067]

[0068] As shown in Table 1, the compositions of Examples 1-3 of this invention have shorter film-forming times, demonstrating their excellent film-forming properties. The shorter film-forming time provides a physical barrier, promoting the activity of the active ingredients on the oral mucosa surface and reducing patient pain. This rapid film-forming characteristic helps to quickly form a physical protective barrier on the oral mucosa surface. This not only isolates external stimuli and reduces pain but also promotes the activity of the active ingredients in the composition, such as forscorin and corn germ extract, on the oral mucosa surface, promoting repair.

[0069] Experimental Example 2

[0070] To verify the inhibitory effect of the oral care compositions obtained in Examples 1-3 and Comparative Example 1 on glucosyltransferase, the following experiments were conducted:

[0071] The coust streptococci were inoculated into THB liquid medium and anaerobically cultured at 37°C for 24 h. Then, the cells were centrifuged at 5000 rpm for 10 min at 4°C to collect the cell pellet. Ten volumes of 8 mol / L urea solution were added to the cell pellet, and the mixture was vortexed for 1 h. Then, the mixture was centrifuged at 10000 rpm for 20 min at 4°C to collect the supernatant. The supernatant was filtered through a 0.8 µm syringe bacterial filter, and the filtrate was dialyzed for 1 day to obtain the crude enzyme solution.

[0072] The crude enzyme solution and PBS solution were mixed evenly at a volume ratio of 1:3, and the volume was adjusted to 3 mL with distilled water. The mixture was reacted at 37 °C for 3 h, and the absorbance value was measured at 550 nm. The solution with an absorbance value of 1.0 was selected as the glucosyltransferase solution for subsequent experiments.

[0073] The glucosyltransferase solution and PBS solution were mixed at a volume ratio of 1:3, and the compositions of Examples 1-3 and Comparative Example 1 were added respectively. The final concentration of the composition was controlled at 5 mg / mL. After mixing thoroughly, the volume was adjusted to 3 mL with distilled water and reacted at 37°C for 3 h. The absorbance value was then measured at 550 nm. A blank control group was set up, which did not undergo any treatment. The inhibition rate was calculated as [1 - (absorbance value of experimental group / absorbance value of blank control group)] × 100%. The experimental results are shown in Table 2.

[0074] Table 2

[0075]

[0076] As shown in Table 2, the oral care compositions of Examples 1-3 of this invention generally exhibited higher inhibition rates against glucosyltransferases than the comparative examples. In Comparative Example 1, omitting forscorin significantly reduced the inhibition rate. These results indicate that forscorin introduced into the compositions of this invention can inhibit glucosyltransferase activity, thereby inhibiting the production of glucan, reducing attachment sites for pathogenic bacteria in the oral cavity, and contributing to maintaining oral health.

[0077] Experimental Example 3

[0078] To verify the proliferative effect of the oral care compositions obtained in Examples 1-3 and Comparative Examples 1-2 of the present invention on oral mucosal epithelial cells, the CCK-8 assay was used for detection.

[0079] Human oral mucosal epithelial cells in the logarithmic growth phase (P3 generation) were selected and cultured using complete culture medium for human oral mucosal epithelial cells to obtain 1×10⁻⁶ cells / years. 6 Cell suspensions of 1 cell / mL were seeded into 96-well plates and cultured at 37°C for 24 hours. The compositions of Examples 1-3 and Comparative Examples 1-2 were prepared into 5 mg / mL test solutions using complete human oral mucosal epithelial cell culture medium and added to 96-well plates, with three replicates per group. A blank group (containing only complete human oral mucosal epithelial cell culture medium) and a control group (containing only complete human oral mucosal epithelial cell culture medium and normal cells) were also included. After culturing at 37°C for another 24 hours, the culture medium was discarded, and CCK-8 solution was added to each well. The plates were incubated in the dark for 1 hour, and the absorbance at 490 nm was measured using a microplate reader. The average value was taken as the final result, and the cell proliferation rate was calculated as: Cell proliferation rate = (Experimental group absorbance value - Blank group absorbance value) / (Control group absorbance value - Blank group absorbance value) × 100%. The results are shown in Table 3.

[0080] Table 3

[0081]

[0082] When the cell proliferation rate is close to 100%, it indicates that the number of cells in this group is comparable to that in the blank control group. When the cell proliferation rate is greater than 100%, it indicates an increase in the number of proliferating cells. As shown in Table 3, the cell proliferation rates of the oral care compositions of Examples 1-3 of this invention are significantly higher than those of the comparative examples, proving that the oral care compositions of this invention can promote the proliferation of oral mucosal epithelial cells and help repair damaged oral mucosa. Comparative Example 2, by omitting the addition of corn sprout extract to its composition, has a lower cell proliferation rate than Example 1. This result confirms that corn sprout extract can promote the proliferation of oral mucosal epithelial cells and plays an important role in repairing damaged oral mucosa.

[0083] Test Example 4

[0084] To verify the antibacterial properties of the oral care compositions obtained in Examples 1-3 and Comparative Examples 1-2 of the present invention, the following experiments were conducted:

[0085] Candida albicans was selected as the experimental strain, and after being cultured to the logarithmic growth phase, its concentration was adjusted to 5 × 10⁻⁶. 6 CFU / mL, the bacterial culture was added to a 96-well plate and incubated at 37°C for 2 h. The culture medium was discarded, and the plate was washed three times with PBS. 100 µL of RPMI 1640 medium was added and inoculated into the 96-well plate. The oral care compositions of Examples 1-3 and Comparative Examples 1-2 were added. A blank control group (containing no Candida albicans) and a negative control group (containing no composition) were set up. Each group was set up with 3 replicates. The plate was incubated at 37°C for another 48 h. The culture medium was discarded, and 100 µL of XTT solution (final concentration 1 µmol / L) was added to each well. The plate was shaken well and incubated at 37°C in the dark for 2 h. The absorbance value at a wavelength of 490 nm was measured, and the inhibition rate was calculated based on the absorbance value. Inhibition rate = 1 - (absorbance value of experimental group - absorbance value of blank control group) / (absorbance value of negative control group - absorbance value of blank control group) × 100%. The results are shown in Table 4.

[0086] Table 4

[0087]

[0088] As shown in Table 4, the compositions of Examples 1-3 of this invention have a good inhibitory effect on Candida albicans, and the effect is significantly better than that of the comparative examples. This result confirms that the compositions of this invention can effectively inhibit Candida albicans, thereby reducing the risk of oral mucosal infections and inflammation caused by it.

[0089] The above embodiments are merely preferred embodiments of the present invention and should not be construed as limiting the scope of protection of the present invention. Any non-substantial changes and substitutions made by those skilled in the art based on the present invention shall fall within the scope of protection claimed by the present invention.

Claims

1. An oral care composition, characterized in that, By weight percentage, it consists of the following ingredients: chitosan oligosaccharide 0.1-0.3%, sea hawthorn polysaccharide 0.08-0.14%, forscorin 0.07-0.12%, corn sprout extract 0.05-0.09%, thickener 1-3%, humectant 40-50%, and the balance being water; The preparation method of the *Hailaria lobata* polysaccharide is as follows: a. The preparation process of sea hay polysaccharide is as follows: sea hay is washed, dried, crushed, and sieved to obtain sea hay powder; b. Add sea hay powder to water, with a ratio of sea hay powder to water of 1g:25mL, soak for 24h, filter to remove residue, centrifuge the filtrate at 3000rpm for 20min, and collect the supernatant; concentrate the supernatant to 8% of its original volume, then add 3 times its volume of anhydrous ethanol, precipitate for 12h, and centrifuge again at 3000rpm for 20min; c. Dissolve the precipitate after centrifugation in water, then add Sevage reagent for deproteinization treatment, then centrifuge at 3000 rpm for 20 min, repeat 3 times, and finally concentrate the filtrate under reduced pressure and freeze dry to obtain sea hay polysaccharide. The preparation method of the corn sprout extract is as follows: (1) Soak corn seeds in water and then remove them for later use; (2) Place the corn seeds soaked in step (1) into a germination box lined with absorbent paper for cultivation; (3) After the sprouts reach 1-2 cm in length, collect the corn sprouts, wash them, dry and crush them, add them to an ethanol aqueous solution, heat and reflux them, collect the reflux liquid, concentrate it and freeze dry it to obtain the corn sprout extract.

2. The oral care composition according to claim 1, characterized in that, In step (1), the soaking temperature is 15-18℃ and the soaking time is 20-24h.

3. The oral care composition according to claim 1, characterized in that, In step (2), the cultivation is carried out in the dark, with a temperature of 25-28℃ and a humidity of 80-85%.

4. The oral care composition according to claim 1, characterized in that, In step (3), the amount of the ethanol aqueous solution added is 6-10 times the mass of the corn sprouts, and the mass concentration of the ethanol aqueous solution is 70-80%.

5. The oral care composition according to claim 1, characterized in that, In step (3), the drying temperature is 45-55℃; the heating reflux temperature is 80-90℃, and the time is 3-5h.

6. The oral care composition according to claim 1, characterized in that, The average molecular weight of the chitosan oligosaccharide is 1000.

7. The oral care composition according to claim 1, characterized in that, The thickener is any one of hydroxyethyl cellulose, carrageenan, or guar gum.

8. The oral care composition according to claim 1, characterized in that, The moisturizer is any one of glycerin, polyethylene glycol, or sorbitol.

9. A method for preparing an oral care composition according to any one of claims 1-8, characterized in that, Includes the following steps: According to the formula, mix chitosan oligosaccharide, sea hawthorn polysaccharide, forscorin, and corn germ extract evenly, then add thickener, humectant, and water, and stir evenly to obtain the final product.

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