Two-phase oral care solution based on natural active ingredients as well as preparation method and application of two-phase oral care solution

Abstract

According to the two-phase oral care solution based on the natural active oily components, specific water-phase and oil-phase components are selected for matching, and proper emulsifiers and surfactants are selected, so that the oral care effect of the oily components can be maintained, and the oral care solution can continuously improve the antibacterial effect, maintain long-lasting cleanliness and also can be used for oral care of the oily components. Meanwhile, the mouth feel is fresh, cool, non-sticky, safe and stable.

Description

Technical Field

[0001] The invention relates to the field of oral care, and in particular to a two-phase oral care solution based on natural active ingredients, and a preparation method and application thereof. Background Art

[0002] As a common oral care product, oral care liquid is mainly used to assist in cleaning the oral cavity, removing food residues, preventing tooth decay, reducing gum inflammation and eliminating bad breath. It plays an important role in maintaining oral hygiene and promoting oral health. Its convenience and refreshing effect make it an important oral care supplement besides brushing and flossing.

[0003] Traditional oral care solutions usually use a single water phase formula. Although they can provide immediate cleaning and refreshing effects, they are limited by the solubility and stability of the single phase, and the product is not as good as when the oil phase formula is added in some aspects. Oil phase formulas with natural active ingredients such as tea tree essential oil components can reduce dental plaque, gingivitis and Streptococcus mutans in the mouth, thereby improving oral health and having a refreshing effect; eucalyptus oil has a broad-spectrum antibacterial effect, which can effectively inhibit harmful bacteria in the mouth and reduce the risk of oral infection. It also has an anti-inflammatory effect, which helps relieve oral inflammation, promotes the repair of oral mucosa, and helps the healing of oral ulcers; peppermint oil can provide a cool feeling, help relieve oral discomfort, reduce swelling, etc. These are effects that cannot be achieved with a single water phase formula.

[0004] However, if an oil phase formula is used, the product often has problems such as short-lasting cleaning effect, difficulty in penetrating into the dead corners of the oral cavity, and high irritation to the oral mucosa. In addition, during long-term storage, the active ingredients of the oral care solution with an oil phase formula may gradually lose their effectiveness due to stability issues. If emulsifiers and surfactants are used in the oil phase formula, commonly used emulsifiers and surfactants may not be stable enough or have poor biocompatibility, causing the emulsion to easily stratify, affecting the overall stability and effectiveness of the product. In addition, the existing combination of emulsifiers and surfactants may cause irritation or allergic reactions to the oral mucosa, a sticky taste, and a large amount of residue in the deep or dead corners of the mouth after spitting out, limiting its application in sensitive oral environments.

[0005] Based on this, there is an urgent need to find an oral care solution that maintains the efficacy of oily ingredients based on natural active oily ingredients, while being able to deeply reach the dead corners of the oral cavity and provide long-lasting cleaning protection. Summary of the invention

[0006] The present invention aims to provide an oral care solution based on natural active oily ingredients, which can reach deep into the dead corners of the oral cavity while maintaining the oral care efficacy of the oily ingredients, and provide long-lasting cleaning protection, ensuring a refreshing, non-greasy mouthfeel, and an oral care solution that can be spit out quickly. The oral care solution provided by the present invention is matched by selecting specific water phase and oil phase components, so that the oral care solution can not only continuously improve the antibacterial effect, maintain long-lasting cleaning, and have a better care effect on the deep part of the oral cavity and dead corners, but also have a refreshing, non-greasy mouthfeel, and are safe and stable. In addition, the present invention also provides a preparation method for the oral care solution and its application in oral care. The details are as follows:

[0007] The present invention provides a dual-phase oral care liquid composition based on natural active ingredients, which comprises the following components based on 100 wt% of the total amount of the oral care liquid composition:

[0008] Water-soluble active ingredient 0.2-5.0wt%;

[0009] Oil-soluble active ingredient 0.5-10.0wt%;

[0010] Emulsifier 0.5-5.0wt%;

[0011] Surfactant 1.0-8.0wt%;

[0012] Fragrance 0.2-0.5wt%;

[0013] Sweetener 0.2-0.5wt%;

[0014] pH regulator 0.2-1wt%;

[0015] and the balance is pure water;

[0016] The water-soluble active ingredient is composed of sodium chloride, ammonium chloride and sodium fluoride, which are compounded in a weight ratio of (1-3): (0.4-0.6): (0.1-0.3);

[0017] Wherein, based on the total amount of the oral care liquid composition, the oil-soluble active ingredient contains at least 0.2wt%-5wt% of tea tree oil, 0.2wt%-3wt% of peppermint oil, and 0.1wt%-2wt% of eucalyptus oil;

[0018] The emulsifier is lauric acid macrogol glyceride, and the surfactant is benzalkonium chloride and polysorbate 80 (Tween 20) compounded at a ratio of 1:5-1:20.

[0019] In one embodiment, the oil-soluble active ingredients further include 0-1 wt% lavender oil, 0-0.2 wt% vitamin E oil, 0-0.5 wt% calendula oil, and 0-0.5 wt% sea buckthorn oil.

[0020] In one embodiment, the pH adjuster is selected from one or more of acetic acid / sodium acetate, sodium dihydrogen phosphate / disodium hydrogen phosphate, citric acid / sodium citrate, tartaric acid / sodium tartrate and sodium bicarbonate / carbonic acid buffer system, and the pH value of the composition is controlled between 5-8, preferably between 5.5-7.

[0021] In one embodiment, the oral care liquid composition is prepared in advance into two parts, the first part is a combination of water-soluble active ingredients, flavors, sweeteners, pH adjusters and purified water, and the second part is a combination of oil-soluble active ingredients, emulsifiers and surfactants.

[0022] The present invention also provides a method for preparing the dual-phase oral care liquid composition based on natural active ingredients, comprising the following steps:

[0023] 1) preparing a water-soluble active ingredient, including sodium chloride, ammonium chloride and sodium fluoride, which are compounded in a weight ratio of (1-3): (0.4-0.6): (0.1-0.3); dissolving the water-soluble active ingredient in deionized water to form a water-soluble active ingredient solution;

[0024] 2) preparing an oil-soluble active ingredient, which comprises at least 0.2wt%-5wt% of tea tree oil, 0.2wt%-3wt% of peppermint oil and 0.1wt%-2wt% of eucalyptus oil based on the total amount of the oral care liquid composition; adding an emulsifier to the oil-soluble active ingredient to form an oil-soluble active ingredient mixture;

[0025] 3) mixing the surfactant benzalkonium chloride and polysorbate 80 (Tween 20) in a ratio of 1:5-1:20 to form a surfactant solution;

[0026] 4) slowly adding the oil-soluble active ingredient mixture to the water-soluble active ingredient solution under stirring, and simultaneously adding the surfactant solution, flavor and sweetener to form a uniform emulsion;

[0027] 5) The pH value of the oral care solution is adjusted to 5 to 8 by a pH adjuster.

[0028] The present invention also provides another method for preparing a dual-phase oral care liquid composition based on natural active ingredients, comprising the following steps:

[0029] 1) preparing a water-soluble active ingredient, including sodium chloride, ammonium chloride and sodium fluoride, which are compounded in a weight ratio of (1-3): (0.4-0.6): (0.1-0.3); dissolving the water-soluble active ingredient in deionized water, and adding a pH adjuster to form a water-soluble active ingredient solution;

[0030] 2) preparing an oil-soluble active ingredient, which includes at least 0.2wt%-5wt% of tea tree oil, 0.2wt%-3wt% of peppermint oil and 0.1wt%-2wt% of eucalyptus oil based on the total amount of the oral care liquid composition; adding an emulsifier to the oil-soluble active ingredient, and adding a surfactant benzalkonium chloride and polysorbate 80 in a ratio of 1:5-1:20 to mix with the oil-phase active ingredient to form an oil-soluble active ingredient mixture;

[0031] 3) Before use, the water-soluble active ingredient solution and the oil-soluble active ingredient mixture are shaken for 10-40 seconds to obtain an oral care liquid composition ready for use.

[0032] The present invention also provides an application of a dual-phase oral care liquid composition based on natural active ingredients in oral care.

[0033] Compared with the prior art, the present invention has the following beneficial effects:

[0034] (1) The present invention realizes the synergistic effect of water-based formula and oil-based formula by combining water-soluble active ingredients with oil-soluble active ingredients. The water-phase ingredients such as sodium chloride, ammonium chloride and sodium fluoride help clean the oral cavity, prevent tooth decay and reduce gingivitis; while the oil-phase ingredients are natural active ingredients such as tea tree oil, peppermint oil and eucalyptus oil, which provide broad-spectrum antibacterial, anti-inflammatory and oral mucosal repair effects. This superposition not only enhances the overall effect of the oral care solution, but also broadens its scope of application.

[0035] (2) Deep cleaning and long-lasting protection: Due to its hydrophobic nature, the oil phase components may be more likely to wet and penetrate into areas in the mouth that are not easily wetted by water, such as the micropores of teeth and gingival sulci, thereby achieving deep cleaning. At the same time, it is speculated that the oil phase components may form a protective film in the mouth, which can slowly release the oily active ingredients, thereby prolonging their antibacterial and protective effects in the mouth.

[0036] (3) Improved safety and stability: The selected emulsifiers and surfactants reduce the potential irritation to the oral mucosa while ensuring the stability of the oral care solution, reduce the risk of allergic reactions, and the mouthfeel will not be sticky due to the addition of oily formulas. In addition, by controlling the pH value within an appropriate range, the oral care solution of the present invention exhibits better adaptability to the oral environment, ensuring the safety and stability of the product. DETAILED DESCRIPTION

[0037] Although the present invention has been described to a certain extent, it is obvious that appropriate changes in various conditions can be made without departing from the spirit and scope of the present invention. It is understood that the present invention is not limited to the embodiments described, but belongs to the scope of the claims, which includes equivalent replacements of each factor described.

[0038] As a first aspect of the present invention, in a dual-phase oral care liquid composition based on natural active ingredients provided by the present invention, based on the total amount of the oral care liquid composition being 100wt%, the water-soluble active ingredient is contained in an amount of 0.2-5.0wt%; more preferably 0.5-3.0wt%, wherein the water-soluble active ingredient is composed of sodium chloride, ammonium chloride and sodium fluoride, and the three are compounded in a weight ratio of (1-2): (0.4-0.6): (0.1-0.3); in the oral care liquid, sodium chloride helps to reduce the formation of dental plaque and enhance the freshness of the mouth feel, ammonium chloride has a slight antibacterial effect, can assist in reducing the number of bacteria in the oral cavity, and helps to remove bad breath, while sodium fluoride can effectively prevent caries, enhance the acid resistance of teeth, and reduce the loss of tooth minerals. The use of a specific ratio and the overall content of water-soluble active ingredients can ensure safety, avoid irritation or allergic reaction to the oral mucosa, and maintain cleaning and prevention effects, while providing an acceptable mouth feel.

[0039] The oral care liquid composition of the present invention further comprises 0.5-10.0wt% of an oil-soluble active ingredient; more preferably 1-5wt%, wherein based on the total amount of the oral care liquid composition, the oil-soluble active ingredient contains at least 0.2wt%-5wt% of tea tree oil, 0.2wt%-3wt% of peppermint oil, and 0.1wt%-2wt% of eucalyptus oil; preferably, the oil-soluble active ingredient may also include 0-1wt% of lavender oil, 0-0.2wt% of vitamin E oil, 0-0.5wt% of calendula oil, and 0-0.5wt% of sea buckthorn oil. Among them, tea tree oil has powerful antibacterial and anti-inflammatory properties, which can effectively reduce bacteria and fungi in the mouth and prevent periodontal disease; peppermint oil provides a cooling sensation, helps relieve oral discomfort, reduces swelling, and also has an antibacterial effect; eucalyptus oil has a broad-spectrum antibacterial effect, can effectively inhibit harmful bacteria in the mouth, reduce the risk of oral infection, and also has an anti-inflammatory effect, which helps relieve oral inflammation; lavender oil has soothing and anti-inflammatory properties, which helps reduce oral inflammation and promotes healing; vitamin E oil, as an antioxidant, helps protect oral cells from damage by free radicals and promotes oral health; calendula oil contains anti-inflammatory and healing ingredients, which helps relieve oral ulcers and inflammation; sea buckthorn oil contains a high concentration of vitamins and antioxidants, which helps enhance the protection of the oral mucosa and reduce inflammation.

[0040] Subsequent experiments show that the co-addition of water-soluble components and oil-soluble components has a synergistic effect in antibacterial, anti-inflammatory and healing promotion, and the effect is better than that of a single water-soluble component or a single oil-soluble component. In addition, the co-action of water-soluble components and oil-soluble components also has a certain complementarity. In terms of cleaning effect, water-soluble components help dissolve and remove water-soluble residues and bacteria in the oral cavity, while oil-soluble components can penetrate into the micropores of teeth and gingival sulci and other areas that are not easily wetted by water, providing deep cleaning, so that the oral care solution of the present invention can clean the oral cavity more comprehensively; at the same time, water-soluble components can provide a refreshing taste, while oil-soluble components such as peppermint oil and eucalyptus oil can provide a lasting cool feeling and oral comfort, thereby jointly improving the overall user experience.

[0041] The oral care liquid composition of the present invention also contains essential emulsifiers and surfactants, wherein the emulsifier content is 0.5-5.0wt%; further preferably 1-3wt%, wherein the emulsifier is lauric acid macrogol glyceride; the surfactant is 1.0-8.0wt%; the surfactant is benzalkonium chloride and polysorbate 80 (Tween20) compounded according to 1:5-1:20, preferably 1:8-1:15. The present invention selects lauric acid macrogol glyceride as an emulsifier. In addition to realizing the effect that general emulsifiers can stably mix oil-soluble active ingredients and water-soluble active ingredients together to form a uniform emulsion, it also takes into account that lauric acid macrogol glyceride has good biocompatibility, little stimulation to the oral mucosa, and is suitable for use in sensitive oral environments, and later experiments show that it helps to improve the absorption rate of oil-soluble active ingredients on the oral mucosa, thereby enhancing its antibacterial and anti-inflammatory effects. The combination of benzalkonium chloride and polysorbate 80 (Tween 20) as a surfactant can reduce the surface tension of mouthwash, provide a refreshing and non-sticky taste, and make the oral care solution evenly distributed in the mouth so that it can better cover the teeth and gums. Benzalkonium chloride itself also has antibacterial properties, which can inhibit harmful bacteria in the mouth and reduce the formation of dental plaque. Polysorbate 80 (Tween 20) helps to improve the solubility and stability of benzalkonium chloride, while reducing its potential irritation to the oral mucosa.

[0042] The oral care liquid composition of the present invention further comprises 0.2-1wt% of a pH regulator; the pH regulator is selected from one or more of acetic acid / sodium acetate, sodium dihydrogen phosphate / phosphoric acid, citric acid / sodium citrate, tartaric acid / sodium tartrate and sodium bicarbonate / carbonic acid buffer systems. The pH value of the composition is controlled between 5-8, preferably between 5.5-7, which is beneficial to maintaining the natural balance of the oral environment, while ensuring the mildness of the product to the oral mucosa and teeth, and avoiding discomfort or damage.

[0043] The flavors and sweeteners described in the present invention are common flavors and sweeteners in the art. Flavors are usually selected to provide fresh breath and pleasant feelings, such as mint, lemon or fruit flavors. These flavors can not only cover up bad breath, but also give users a fresh and clean feeling. Sweeteners are used to neutralize the bitter or irritating taste that may exist in oral care solutions. Commonly used sweeteners include, but are not limited to: one or more of sucralose, aspartame, erythritol, xylitol, and stevia.

[0044] In the present invention, based on the dual-phase components in the composition, two parts can be prepared in advance, the first part is a combination of water-soluble active ingredients, flavors, sweeteners, pH adjusters and purified water, and the second part is a combination of oil-soluble active ingredients, emulsifiers, and surfactants, which are mixed evenly when used. By preparing the water-soluble and oil-soluble components separately, the possible interaction between them during the mixing process can be reduced, thereby reducing the instability of the emulsified system and reducing the risk of stratification and precipitation.

[0045] As a second aspect of the present invention, the present invention also provides a method for preparing the dual-phase oral care liquid composition based on natural active ingredients, comprising the following steps:

[0046] 1) preparing water-soluble active ingredients, including sodium chloride, ammonium chloride and sodium fluoride, which are compounded in a weight ratio of (1-2): (0.4-0.6): (0.1-0.3); dissolving the water-soluble active ingredients in deionized water according to the weight ratio to form an aqueous solution.

[0047] 2) preparing an oil-soluble active ingredient, which comprises at least 0.2wt%-5wt% of tea tree oil, 0.2wt%-3wt% of peppermint oil and 0.1wt%-2wt% of eucalyptus oil based on the total amount of the oral care liquid composition; adding an emulsifier in a weight ratio to the oil-soluble active ingredient to form an oil phase;

[0048] 3) mixing the surfactant benzalkonium chloride and polysorbate 80 (Tween 20) in a ratio of 1:5-1:20 to form a surfactant solution;

[0049] 4) Under stirring conditions, slowly adding the oil phase to the water phase, and simultaneously adding a surfactant solution, flavor and sweetener in a weight ratio to form a uniform emulsion;

[0050] 5) The pH value of the oral care solution is adjusted to 5 to 8 by a pH adjuster.

[0051] Among them, the emulsifier is first mixed with the oil phase, and then the mixture is gradually added to the water phase containing water-soluble ingredients, and the surfactant is added at the same time. This operation can ensure that the emulsifier and surfactant fully act on the oil-water interface, effectively reduce the interfacial tension, promote the uniform mixing of the oil phase and the water phase, and form a stable emulsion. The benefits of this include improving the stability of the emulsion, preventing product stratification and precipitation, and ensuring the uniform distribution of active ingredients.

[0052] It is also possible to prepare in advance the oil phase and the water phase so that they are mixed when used. In this preparation method, the pH adjuster must be mixed with the water phase in advance, and the surfactant must be mixed with the oil phase first. In the actual product, the two parts are placed in different parts of the package, separated by detachable partitions, and mixed and shaken when used. The advantage of this is that it can ensure that the oil phase and the water phase can be evenly mixed during long-term storage and use.

[0053] As a third aspect of the present invention, the present invention further provides a use of a dual-phase oral care liquid composition based on natural active ingredients in oral care.

[0054] The oral care liquid composition and the preparation method thereof provided by the present invention are described in detail below in conjunction with the examples, but they should not be construed as limiting the scope of protection of the present invention. In addition, if no specific conditions are specified in the examples of the present invention, the conventional conditions or the conditions recommended by the manufacturer are used; if the manufacturer of the reagents or instruments is not specified, they are all conventional products that can be purchased commercially.

[0055] 1. Preparation of oral care liquid composition in Examples and Comparative Examples

[0056] Example 1

[0057] 2.5 g of sodium chloride, 0.5 g of ammonium chloride and 0.2 g of sodium fluoride were dissolved in deionized water as water-soluble active ingredients to form an aqueous solution;

[0058] 2.5 g of tea tree oil, 1.5 g of peppermint oil and 1.0 g of eucalyptus oil were mixed with 3.0 g of emulsifier laurate macrogol glyceride to form an oil phase mixture;

[0059] Under stirring conditions, the oil phase is slowly added to the water phase, and a surfactant is added. The surfactant solution is prepared by mixing 0.75 g of benzalkonium chloride and 5.25 g of polysorbate 80 (Tween 20) in a ratio of 1:7, and 0.3 g of flavor and 0.3 g of sweetener are added to form a uniform emulsion. Finally, 0.7 g of citric acid / sodium citrate (mol ratio 1:3) and the remainder of purified water are added to make the total weight of the oral care solution 100 g, and the pH value of the oral care solution is about 6.5.

[0060] Example 2

[0061] 0.5g tea tree oil, 1.2g peppermint oil and 1.0g eucalyptus oil, the amount of purified water added is adaptively adjusted so that the total weight of the oral care solution is 100g, the pH value of the oral care solution is about 6.4, and the other components and addition conditions remain unchanged.

[0062] Example 3

[0063] 2.5 g of sodium chloride, 0.5 g of ammonium chloride and 0.2 g of sodium fluoride were dissolved in deionized water as water-soluble active ingredients, and 0.3 g of flavor, 0.3 g of sweetener and 0.7 g of citric acid / sodium citrate (mol ratio 1:3) were added, and the balance was 81.5 g of water to form an aqueous phase solution;

[0064] 2.5 g of tea tree oil, 1.5 g of peppermint oil and 1.0 g of eucalyptus oil were mixed with 3.0 g of emulsifier laurate macrogol glyceride to form an oil phase mixture, and a surfactant prepared by mixing 0.75 g of benzalkonium chloride and 5.25 g of polysorbate 80 (Tween 20) in a ratio of 1:7 was added and mixed to form an oil phase viscous solution;

[0065] Before use, shake the aqueous phase solution and the oil phase viscous solution for 30 seconds to obtain the product.

[0066] Example 4

[0067] 0.15 g of sodium chloride, 0.037 g of ammonium chloride and 0.013 g of sodium fluoride were dissolved in deionized water as water-soluble active ingredients to form an aqueous solution;

[0068] 0.2 g of tea tree oil, 0.2 g of peppermint oil and 0.1 g of eucalyptus oil were mixed with 0.5 g of emulsifier laurate macrogol glyceride to form an oil phase mixture;

[0069] Under stirring conditions, the oil phase is slowly added to the water phase, and a surfactant is added, wherein the surfactant solution is prepared by mixing 0.15 g of benzalkonium chloride and 0.85 g of polysorbate 80 (Tween 20) at a ratio of 1:5.7, and 0.2 g of flavor and 0.2 g of sweetener are added to form a uniform emulsion. Finally, 0.5 g of sodium dihydrogen phosphate / disodium hydrogen phosphate (mol ratio 1:1) and the remainder of purified water are added to make the total weight of the oral care solution 100 g, and the pH value of the oral care solution is about 7.2.

[0070] Example 5

[0071] 4.0 g of sodium chloride, 0.7 g of ammonium chloride and 0.3 g of sodium fluoride were dissolved in deionized water as water-soluble active ingredients to form an aqueous solution;

[0072] 5.0 g of tea tree oil, 3.0 g of peppermint oil and 2.0 g of eucalyptus oil were mixed with 5.0 g of emulsifier laurate macrogol glyceride to form an oil phase mixture;

[0073] Under stirring conditions, the oil phase is slowly added to the water phase, and a surfactant is added. The surfactant solution is prepared by mixing 0.75 g of benzalkonium chloride and 7.25 g of polysorbate 80 (Tween 20) at a ratio of 1:9.7, and 0.5 g of flavor and 1.0 g of sweetener are added to form a uniform emulsion. Finally, 0.8 g of citric acid / sodium citrate (mol ratio 1:9) and the remainder of purified water are added to make the total weight of the oral care solution 100 g, and the pH value of the oral care solution is about 6.0.

[0074] Comparative Example 1

[0075] Compared with Example 1, 2.5 g of tea tree oil, 1.5 g of peppermint oil and 1.0 g of eucalyptus oil were not added to form an oil phase mixture mixed with 3.0 g of emulsifier laurate macrogol glyceride, and the amount of pure water added was adaptively adjusted so that the total weight of the oral care solution was 100 g, and the other components and addition conditions remained unchanged.

[0076] Comparative Example 2

[0077] Compared with Example 1, 2.5 g of sodium chloride, 0.5 g of ammonium chloride and 0.2 g of sodium fluoride were not added as water-soluble active ingredients, the amount of purified water added was adaptively adjusted so that the total weight of the oral care solution was 100 g, and the other components and addition conditions remained unchanged.

[0078] Comparative Example 3

[0079] Compared with Example 1, 3.0 g of lauric acid macrogol glyceride was not used as an emulsifier, and the amount of pure water added was adaptively adjusted so that the total weight of the oral care solution was 100 g. The other components and addition conditions remained unchanged.

[0080] Comparative Example 4

[0081] Compared with Example 1, 0.75 g of benzalkonium chloride and 5.25 g of polysorbate 80 (Tween 20) were not mixed in a ratio of 1:7 as a surfactant, the amount of pure water added was adaptively adjusted so that the total weight of the oral care solution was 100 g, and the other components and addition conditions remained unchanged.

[0082] Comparative Example 5

[0083] Compared with Example 1, the emulsifier is lecithin, and the other components and addition conditions remain unchanged.

[0084] Comparative Example 6

[0085] Compared with Example 1, the surfactant is sodium dodecylbenzene sulfonate, and the other components and addition conditions remain unchanged.

[0086] Comparative Example 7

[0087] 2.5 g of sodium chloride, 0.5 g of ammonium chloride and 0.2 g of sodium fluoride were dissolved in deionized water as water-soluble active ingredients to form an aqueous solution;

[0088] 2.5 g of tea tree oil, 1.5 g of peppermint oil and 1.0 g of eucalyptus oil were added to form an oil phase mixture;

[0089] Under stirring conditions, the oil phase is slowly added to the water phase, and an emulsifier and a surfactant are added, wherein the emulsifier is 3.0g of the emulsifier lauric acid macrogol glyceride, and the surfactant solution is prepared by mixing 0.75g of benzalkonium chloride and 5.25g of polysorbate 80 (Tween20) in a ratio of 1:7, and 0.3g of flavor and 0.3g of sweetener are added to form a uniform emulsion. Finally, by adding 0.7g of citric acid / sodium citrate (mol ratio 1:3) and the remainder of purified water, the total weight of the oral care solution is 100g, and the pH value of the oral care solution is about 6.5.

[0090] 2. In vitro antibacterial effect verification test

[0091] The Streptococcus mutans bacterial solution was adjusted to 0.5 McFarland standard and evenly coated on the culture medium. A sterile punch was used to punch holes on the culture medium with a hole diameter of 10 mm and a hole depth of 10 mm. The oral care solutions of Examples 1-5 and Comparative Examples 1-7 were added to the holes and filled up respectively. Sterile water was selected as the control group. After being placed at room temperature for 30 minutes, the mixture was placed in a constant temperature incubator at 37° C. and cultured for 24 hours. The diameter of the inhibition zone (defined as the shortest distance from the edge of the hole in the culture medium to the edge of the area where bacteria cannot grow) was observed and measured.

[0092] Table 1 is the in vitro antibacterial effect verification results of Examples 1-5, Comparative Examples 1-7 and the control group:

[0093] Sample No. Measured antibacterial zone diameter (mm) Example 1 17.2 Example 2 16.8 Example 3 15.6 Example 4 13.9 Example 5 16.5 Comparative Example 1 7.5 Comparative Example 2 8.0 Comparative Example 3 6.9 Comparative Example 4 7.1 Comparative Example 5 11.2 Comparative Example 6 12.3 Comparative Example 7 12.4 Control group 0.1

[0094] In the antibacterial effect verification test, the larger the diameter of the inhibition zone, the better the antibacterial effect is usually. The size of the inhibition zone diameter reflects the ability of the oral care solution to inhibit bacterial growth. When the oral care solution has antibacterial activity, it will form a clear area on the bacterial culture medium, where bacteria cannot grow, and this area is the inhibition zone. The larger the diameter of the inhibition zone, the stronger the antibacterial effect of the care solution in this area. In Examples 1-5, due to the presence of oil-soluble components known to have antibacterial properties such as tea oil, peppermint oil and eucalyptus oil, and water-soluble active ingredients such as sodium chloride, ammonium chloride and sodium fluoride, it has a good antibacterial effect. In Comparative Examples 1-4, due to the lack of necessary components such as oil-soluble components, water-soluble components, specific surfactants and emulsifiers, the antibacterial effect will be significantly reduced. In Comparative Examples 5 and 6, although alternative emulsifiers and surfactants are used, as expected, these substitutes may not be as effective as those in the original formula, so the antibacterial effect is slightly reduced. In comparative example 7, the timing of adding the emulsifier and the surfactant was wrong, which affected the formation and stability of the emulsion, thereby affecting the antibacterial effect. The control group used sterile water, which had no antibacterial effect, so the diameter of the inhibition zone was close to 0.

[0095] 3. Oral mucosal inflammation inhibition test

[0096] Healthy adult rats were selected, weighing between 200-250g, and 10% phenol solution was applied topically on the oral mucosa of the rats to induce inflammation. The induction time was 1 hour. The rats were grouped with Examples 1-5, Comparative Examples 1-7, and a control group, with 5 rats in each group, and the control group was sterile water. After induction, 10 ml of the formula of Examples 1-5, Comparative Examples 1-7, and a control group was injected into the rats' oral cavity to act on the oral mucosa. The degree of redness and swelling of the oral mucosa of the animals was observed at specific time points after administration (30 minutes, 24 hours, 48 ​​hours, and 72 hours, respectively), and the area of ​​the inflammatory area was measured using image analysis software.

[0097] Table 2 is the in vitro inflammation area verification results of Examples 1-5, Comparative Examples 1-7 and the control group:

[0098]

[0099] It can be seen that compared with the control group, all formulations have an inhibitory effect on the inflammatory area. As time goes by, the area of ​​the inflammatory area decreases. The oil phase and the water phase of Examples 1-5 work together to have a better inhibitory effect on inflammation, and the use of specific emulsifiers and surfactants to act on the oil phase is also more conducive to the oil-soluble components to exert their inhibitory effect on inflammation.

[0100] 4. Oral mucosal repair effect test

[0101] Oral mucosal tissue was obtained from healthy volunteers. After digestion with neutral protease and trypsin, the obtained mucosal epithelial cells were inoculated in a culture medium containing 10% fetal bovine serum for primary culture. After the cells adhered to the wall, they were digested with 0.40% Dispase, the epithelial cells were separated, and subcultured.

[0102] The cultured human oral epithelial cells (hOECs) were inoculated in 24-well plates, with 2×10 4 cells, and the formulations of Examples 1-5, Comparative Examples 1-7 and a blank control group were added to each well, with three replicate wells set for each formulation.

[0103] 10 μL of CCK-8 reagent was added to each well, and the culture plate was gently shaken to help the reagent mix with the culture medium, and then cultured at 37°C in a 5% CO2 concentration for 4 hours until a color change appeared in the culture plate.

[0104] The absorbance of each well was then measured using a microplate reader at a wavelength of 450 nm.

[0105] The cell proliferation rate was calculated using the formula: (OD value of the experimental group - OD value of the blank control) / OD value of the blank control × 100%.

[0106] Blank control wells contained no cells but only culture medium and CCK-8 reagent.

[0107] Table 3 shows the cell repair and proliferation verification results of Examples 1-5, Comparative Examples 1-7 and the control group:

[0108] Sample No. OD value of experimental group Blank control OD value Cell proliferation rate (%) Example 1 0.65 0.4 62.50％ Example 2 0.60 0.4 50.00％ Example 3 0.62 0.4 55.00％ Example 4 0.58 0.4 45.00％ Example 5 0.68 0.4 70.00％ Comparative Example 1 0.50 0.4 25.00％ Comparative Example 2 0.52 0.4 30.00％ Comparative Example 3 0.48 0.4 20.00％ Comparative Example 4 0.49 0.4 22.50％ Comparative Example 5 0.55 0.4 37.50％ Comparative Example 6 0.54 0.4 35.00％ Comparative Example 7 0.53 0.4 32.50％

[0109] In the cell proliferation experiment, the OD value (absorbance) is measured by a microplate reader, which reflects the number and activity of cells. When other conditions remain unchanged, it can be seen that the co-addition of the water-soluble components and the oil-soluble components of Examples 1-5 has a better effect in promoting the proliferation of healing cells.

[0110] 5. Deep cleaning effect and durability simulation test

[0111] Use a ceramic 3D printer (Qiyu Technology) to 3D print bionic zirconia to create a simulated tooth model.

[0112] Brain heart infusion (BHI) culture medium was selected, the pH value was adjusted to 6.8, 0.2% to 0.5% glucose and mucin based on the total weight of the culture medium were added, high pressure steam sterilization was performed at 121°C for 20 minutes and then restored to room temperature, and then the simulated tooth model was immersed in the culture medium and cultured at 37°C and 5% CO2 for 7 days before being taken out.

[0113] The simulated tooth model was immersed in 100 ml of the oral care solution of Examples 1-5, Comparative Examples 1-7 and the control group sterile water for 1 min to simulate the mouthwash process, and then the simulated tooth model was taken out and placed in a culture medium simulating the oral environment.

[0114] The oral care solutions of Examples 1-5, Comparative Examples 1-7 and the control group of sterile water after immersion were counted for bacteria under a microscope using a blood cell technology plate to evaluate the cleaning effect.

[0115] The bacteria adhering to the surface of the simulated tooth model were counted after 2 hours, 4 hours, 8 hours, 16 hours and 24 hours in the culture medium to evaluate the long-lasting antibacterial effect.

[0116] Table 4 is the experimental effect data of the cleaning effect and the lasting antibacterial effect of Examples 1-5 and Comparative Examples 1-7:

[0117]

[0118]

[0119] As shown in Table 4, after cleaning the simulated tooth model, the number of bacteria in Examples 1-5 after cleaning is lower than that in the comparative example, and is also lower than that in the sterile water in the control group. At the same time, in terms of persistent inhibition, the growth trend of bacteria is also significantly lower than that in the comparative example 1-7 and the control group. It can be seen that the oral care solution of the present invention has a deep cleaning effect on the simulated tooth model and also has persistent antibacterial properties.

[0120] 6. Taste Test

[0121] The oral care solutions of Examples 1-5 and Comparative Examples 1-7 were subjected to sensory tests, which were conducted by 8 test subjects in the test group. Each test subject was a healthy individual arranged on an objective basis according to the specified requirements. Sensory analysis was conducted according to ISO4121-2003 under the test conditions of ISO8589, and 8 test subjects were counted to evaluate different samples.

[0122] Good - clear taste, no stickiness when spit out

[0123] Normal - no obvious feeling, different from pure water when spit out, but acceptable

[0124] Discomfort - sticky mouth feeling, can't spit out completely

[0125] Table 2 is the sensory test results of Examples 1-5 and Comparative Examples 1-7

[0126] sample good generally Discomfort Example 1 8 0 0 Example 2 8 0 0 Example 3 8 0 0 Example 4 8 0 0 Example 5 6 2 0 Comparative Example 1 8 0 0 Comparative Example 2 2 1 5 Comparative Example 3 3 3 2 Comparative Example 4 2 4 2 Comparative Example 5 6 2 0 Comparative Example 6 8 0 0 Comparative Example 7 7 1 0

[0127] It can be seen that for Comparative Examples 2-4 which lack emulsifiers, lack surfactants, or do not add water-soluble components, the test subjects have a significantly poor taste, while for Examples 1-5, when the water-soluble active ingredients and the oil-soluble active ingredients are added simultaneously with the emulsifiers and surfactants, they have a more acceptable taste.

[0128] The above is only a preferred embodiment of the present invention, but the protection scope of the present invention is not limited thereto. Any person skilled in the art can easily think of changes or substitutions within the technical scope disclosed by the present invention, which should be included in the protection scope of the present invention. Therefore, the protection scope of the present invention should be based on the protection scope of the claims.

Claims

1. A dual-phase oral care liquid composition based on natural active ingredients, characterized in that: Based on the total amount of the oral care liquid composition being 100 wt%, the composition comprises the following components: Water-soluble active ingredient 0.2-5.0wt%; Oil-soluble active ingredient 0.5-10.0wt%; Emulsifier 0.5-5.0wt%; Surfactant 1.0-8.0wt%; Fragrance 0.2-0.5wt%; Sweetener 0.2-0.5wt%; pH regulator 0.2-1wt%; and the balance is pure water; The water-soluble active ingredient is composed of sodium chloride, ammonium chloride and sodium fluoride, which are compounded in a weight ratio of (1-3): (0.4-0.6): (0.1-0.3); Wherein, based on the total amount of the oral care liquid composition, the oil-soluble active ingredient contains at least 0.2wt%-5wt% of tea tree oil, 0.2wt%-3wt% of peppermint oil, and 0.1wt%-2wt% of eucalyptus oil; The emulsifier is lauric acid macrogol glyceride, and the surfactant is benzalkonium chloride and polysorbate 80 compounded in a weight ratio of 1:5-1:

20.

2. The oral care liquid composition according to claim 1, characterized in that The oil-soluble active ingredients further include 0-1 wt% lavender oil, 0-0.2 wt% vitamin E oil, 0-0.5 wt% calendula oil, and 0-0.5 wt% sea buckthorn oil.

3. The oral care liquid composition according to claim 1, characterized in that The pH regulator is selected from one or more of acetic acid / sodium acetate, sodium dihydrogen phosphate / disodium hydrogen phosphate, citric acid / sodium citrate, tartaric acid / sodium tartrate and sodium bicarbonate / carbonic acid buffer system, and the pH value of the oral care liquid composition is controlled between 5-8.

4. The oral care liquid composition according to claim 1, characterized in that The oral care liquid composition is prepared in advance into two parts, the first part is a combination of water-soluble active ingredients, flavors, sweeteners, pH adjusters and purified water, and the second part is a combination of oil-soluble active ingredients, emulsifiers and surfactants.

5. A method for preparing a dual-phase oral care liquid composition based on natural active ingredients according to any one of claims 1 to 3, characterized in that: The steps include: 1) preparing a water-soluble active ingredient, including sodium chloride, ammonium chloride and sodium fluoride, which are compounded in a weight ratio of (1-3): (0.4-0.6): (0.1-0.3); dissolving the water-soluble active ingredient in deionized water to form a water-soluble active ingredient solution; 2) preparing an oil-soluble active ingredient, which comprises at least 0.2wt%-5wt% of tea tree oil, 0.2wt%-3wt% of peppermint oil and 0.1wt%-2wt% of eucalyptus oil based on the total amount of the oral care liquid composition; adding an emulsifier to the oil-soluble active ingredient to form an oil-soluble active ingredient mixture; 3) mixing the surfactant benzalkonium chloride and polysorbate 80 in a ratio of 1:5-1:20 to form a surfactant solution; 4) under stirring, slowly adding the oil-soluble active ingredient mixture to the water-soluble active ingredient solution according to the ratio of any one of claims 1 to 3, and simultaneously adding the surfactant solution, flavor and sweetener to form a uniform emulsion; 5) The pH value of the oral care solution is adjusted to 5 to 8 by a pH adjuster.

6. A method for preparing the oral care liquid composition according to claim 4, characterized in that: The steps include: 1) According to the composition ratio of claim 4, preparing a water-soluble active ingredient, including sodium chloride, ammonium chloride and sodium fluoride, which are compounded in a weight ratio of (1-3): (0.4-0.6): (0.1-0.3); dissolving the water-soluble active ingredient in deionized water, and adding a pH adjuster to form a water-soluble active ingredient solution; 2) according to the composition ratio of claim 4, preparing an oil-soluble active ingredient, based on the total amount of the oral care liquid composition, at least comprising 0.2wt%-5wt% tea tree oil, 0.2wt%-3wt% peppermint oil and 0.1wt%-2wt% eucalyptus oil; adding an emulsifier to the oil-soluble active ingredient, and adding a surfactant benzalkonium chloride and polysorbate 80 in a ratio of 1:5-1:20 to mix with the oil phase active ingredient to form an oil-soluble active ingredient mixture; 3) before use, the water-soluble active ingredient solution and the oil-soluble active ingredient mixture are shaken for 10-40 seconds to obtain the oral care liquid composition.

7. Use of the dual-phase oral care liquid composition based on natural active ingredients according to claims 1-4 in oral care.

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