PH-responsive plaque visualization and triple anti-allergy synergistic oral care composition as well as preparation method and application thereof

Abstract

The invention discloses a pH response type plaque visualization and triple anti-allergy synergistic oral care composition as well as a preparation method and application thereof. The composition comprises a pH response microcapsule color developing agent, a triple anti-allergy system compounded by potassium salt, bioactive glass and nano-hydroxyapatite, a periodontal repair system and a mild substrate. The core material of the microcapsule is a food-grade dye which develops color when the pH value is less than or equal to 5.5 and fades color when the pH value is greater than or equal to 6.8, and the wall material of the microcapsule is a biocompatible polymer. The composition does not contain SLS, fluoride and nipagin ester preservatives. The invention further provides a gradient cooling preparation process, a plaque detection method and application. The product realizes plaque specificity visualization and triple anti-allergy synergistic interaction, is stable to store, is safe and non-irritant, is suitable for all people to use, and can be industrially produced.

Description

Technical Field

[0001] This invention belongs to the field of oral care technology, specifically relating to an oral care composition that combines plaque visualization detection, dentin hypersensitivity relief, periodontal repair, and gentle whitening functions, as well as its preparation method and application. Background Technology

[0002] With the increasing awareness of oral health among the public, consumers are demanding more functional and effective toothpaste products. However, existing technologies have the following shortcomings: Limitations of plaque visualization technology: Existing plaque display agents are mostly direct-addition dyes, which suffer from poor stability, premature release, contamination of toothpaste, and staining of teeth and oral mucosa, making it difficult to coexist stably with the toothpaste matrix. Therefore, it is impossible to achieve the precise visualization effect of "staining only plaque, not teeth" during use.

[0003] Defects of anti-sensitivity technology: Traditional anti-sensitivity toothpastes often use ingredients with a single mechanism of action, such as only using potassium nitrate to soothe nerves, only using bioactive glass to block tubules, or only using hydroxyapatite to remineralize. They are difficult to achieve both rapid relief and long-term repair, and their anti-sensitivity effect is limited.

[0004] Defects of multi-component compounding: When multiple functional components such as color developers, anti-allergens, and whitening abrasives are compounded, stability problems such as premature leakage of color developers, inactivation of anti-allergens, water separation of the paste, layering, and pigment migration are prone to occur.

[0005] Safety drawbacks: Regular toothpaste often contains irritating ingredients such as sodium lauryl sulfate, fluoride, and parabens, which may irritate people with periodontal sensitivity, those who have undergone oral surgery, children, and pregnant women, and are not suitable for long-term use.

[0006] Deficiencies in detection methods: Existing technologies lack simple and intuitive methods for visualizing plaque detection, making it difficult for consumers to quantify the effectiveness of brushing and hindering the improvement of oral hygiene habits.

[0007] In the existing technology, there is still a need to develop an integrated oral care product that can simultaneously solve the problems of color development stability, multi-component compatibility, anti-allergy synergy, low irritation safety, and provide a visual detection method. Summary of the Invention

[0008] Purpose of the invention The purpose of this invention is to overcome the shortcomings of the prior art and provide an oral care composition with high component compatibility, excellent long-term stability, and both plaque visualization and multiple repair functions, as well as its preparation method and application.

[0009] Overall Inventive Concept All technical solutions of this invention revolve around the overall inventive concept of a multifunctional oral care system with pH-responsive microcapsule color development, integrating the product, preparation method, detection method, and application into a unified technical solution, which meets the unity of patent requirement and can be filed together. Technical solution

[0010] 1. pH-responsive microcapsule colorimetric reagent This invention comprises a pH-responsive colorimetric reagent encapsulated in microcapsules. The microcapsules consist of a wall material and a core material. • Core material: Selected from food-grade pH-changing dyes, such as gardenia blue, anthocyanin derivatives, or curcumin, which automatically fades in a neutral water environment with a pH of 6.8. Gardenia blue is preferred due to its clear color development, complete fading, and high stability. This design achieves a precise visualization effect of "staining only plaque, not teeth."

[0011] • Wall material: Prepared using gelatin-gum arabic or sodium alginate-chitosan via complex coagulation, exhibiting good film-forming properties, moderate strength, and high biocompatibility. The gelatin-gum arabic system is preferred due to its controllable mechanical strength and ease of shear force response release.

[0012] • Particle size and response properties: The average particle size of the microcapsules is 8-20 μm, preferably 10-15 μm; the wall thickness is 0.5-2 μm, preferably 0.8-1.2 μm. Within this parameter range, the microcapsules remain intact under low shear forces and can be controlled to rupture and release the core material under brushing shear forces.

[0013] • Microporous structure: The surface of the microcapsule has a microporous structure with a pore size of 0.1-0.5μm, which can further improve the controllability of rupture and the uniformity of release.

[0014] 2. Triple Synergistic Anti-allergy System It is composed of potassium nitrate, bioactive glass and nano hydroxyapatite, with the weight ratio of the three being 1:0.5-1.5:1.5-2.5, preferably 1:1.0-1.2:2.0-2.2.

[0015] Potassium nitrate: It rapidly blocks pain transmission through nerve depolarization, achieving fast-acting analgesia.

[0016] • Bioactive glass: Releases calcium and phosphorus ions to effectively seal dentinal tubules for a long time.

[0017] • Nano-hydroxyapatite: directly participates in the remineralization and repair of tooth enamel, continuously enhancing tooth hardness.

[0018] The three components work synergistically to achieve rapid analgesia, long-lasting occlusion, and continuous remineralization, which is significantly better than single components or combinations of two components.

[0019] 3. Deep Periodontal Repair System Composed of Centella asiatica extract, dipotassium glycyrrhizate, zinc citrate, and sodium hyaluronate, it effectively inhibits harmful bacteria in the oral cavity, reduces gingival inflammation, and improves problems such as bleeding, redness, and fragility of the gums.

[0020] 4. Gentle physical whitening system Using soft hydrated silica as a physical abrasive, combined with nano-hydroxyapatite, it achieves the removal of extrinsic pigments and brightening of tooth surfaces through a gentle physical polishing method without abrading the enamel.

[0021] 5. Fluorine-free, SLS-free, mild and safe system Surfactant: Sodium lauroyl sarcosinate is used instead of traditional sodium lauryl sulfate, which has low irritation and good biodegradability.

[0022] • Anti-corrosion system: It uses a combination of 1,2-hexanediol and p-hydroxyacetophenone to replace parabens as preservatives, which is safe, mild and hypoallergenic.

[0023] • Ingredient-free: The composition is free of sodium lauryl sulfate, fluoride, alcohol, and parabens, making it suitable for all people, including those with sensitive skin, children, pregnant women, and those who have undergone dental procedures.

[0024] 6. Gradient cooling preparation process This invention provides a gradient cooling preparation process that ensures the integrity of the microcapsule structure and the stability of the paste without separation: • (1) High-temperature adhesive preparation: The aqueous components and thickener are mixed and swollen at 70-80℃ to form a stable adhesive base; • (2) Medium-temperature mixing: Cool down to 40-50℃, add abrasive and mineral powder, and stir evenly under vacuum; • (3) Low temperature protection: Continue to cool down to ≤38℃, add microcapsule color developer, and control the stirring speed to be below 500rpm to avoid microcapsule breakage; • (4) Post-processing: After mixing evenly, the mixture is degassed under vacuum, allowed to stand for 24 hours to mature, and then aseptically filled and molded.

[0025] This process avoids damage to microcapsules from high temperatures by using gradient cooling, while ensuring uniform dispersion of each component and long-term stability of the paste.

[0026] 7. Plaque Colorimetric Detection Method This invention provides a method for detecting plaque using the above composition: the composition is applied to the tooth surface, and brushing the teeth causes the microcapsules to rupture under shear force, releasing the core material. In the acidic environment of plaque (pH 6.8), the color disappears automatically without residue.

[0027] This method is simple and intuitive, and can help consumers effectively improve their brushing habits and enhance oral hygiene. Beneficial effects

[0028] 1. Clear, safe, and stain-free plaque visualization: Microencapsulation technology ensures stable storage of the chromogenic agent, releasing color only in the acidic environment of plaque, and automatically fading after rinsing. Clinical trials with 30 volunteers showed that plaque visibility was ≥90% before brushing, and residual plaque was significantly reduced after cleaning; staining completely disappeared within 2 minutes after rinsing, with no staining of teeth or mucosa, achieving a precise visualization effect of "staining only plaque, not teeth."

[0029] 2. The triple anti-sensitivity system has a significant synergistic effect: The results of in vitro dentinal tubule sealing and nerve analgesia experiments show that the nerve potential inhibition rate and tubule blockage rate of the compound system of this invention are significantly better than those of single components or combinations of two components, demonstrating a synergistic effect.

[0030] 3. Significantly improved system stability: After accelerated stability testing by thermal cycling from -5℃ to 45℃ (3 months), the paste was uniform, with no water separation, no layering, no color leakage, and no premature breakage of microcapsules; commercially available ordinary pigment toothpaste showed obvious pigment migration and layering after 1 month under the same conditions.

[0031] 4. Excellent safety: According to GB / T 16886.10, the oral mucosa irritation test of this product shows an irritation index of 0.35, which is classified as non-irritating; according to GB / T 16886.5, the cytotoxicity test shows a cell survival rate of 96.8%, indicating no cytotoxicity; suitable for adults, children, people with sensitive skin, and people who have undergone oral surgery.

[0032] 5. The detection method is intuitive and effective: The plaque detection method provided by this invention is simple and easy to implement, which can help consumers quantify the effect of brushing teeth, improve oral hygiene habits, and has important public health significance.

[0033] 6. High industrial feasibility: The gradient cooling process is simple and controllable, with no special requirements for equipment, making it easy to scale up industrial production. The stability indicators of a single batch of 500kg products meet the quality control standards. Detailed Implementation

[0034] Example of preparation of microcapsule colorimetric reagent 0.5g of gardenia blue pigment was dissolved in 100mL of deionized water to prepare the core material solution. 2g of gelatin and 2g of gum arabic were dissolved separately in 100mL of deionized water, and the pH was adjusted to 4.0. The core material solution was added dropwise to the wall material solution at 40℃ and stirred for 30min to emulsify. The temperature was lowered to 5℃, and genipin was added for cross-linking and curing for 2h. After filtration, washing, and drying, pH-responsive microcapsule powder with an average particle size of 12μm and a wall thickness of approximately 1μm was obtained. Testing showed that the microcapsules turned blue within 10 seconds in pH 5.0 buffer and completely faded within 30 seconds in pH 7.0 buffer. Shear resistance testing showed that the integrity rate was >95% after stirring at 500rpm for 30 minutes, and the rupture rate was >85% after stirring at 1000rpm.

[0035] Example 1: Adult toothpaste Prepared by weight percentage: Component weight % Deionized water 55.03 Sorbitol 28.00 Polyethylene glycol-8 3.50 Soft hydrated silica 5.00 Nano-hydroxyapatite 2.00 Bioactive glass 1.00 Sodium lauroyl sarcosinate 1.40 Microencapsulated colorimetric reagent (preparation example) 0.16 Potassium nitrate 1.00 Dipotassium glycyrrhizate 0.10 Centella asiatica extract 0.12 Sodium hyaluronate 0.10 Zinc citrate 0.08 Xanthan gum 0.55 Guar gum 0.25 Edible flavoring (white tea flavor) 0.80 WS-23 cooling agent 0.01 Stevioside 0.04 Vitamin E 0.05 1,2-Hexanediol 0.45 p-Hydroxyacetophenone 0.36 Preparation method: (1) High temperature preparation of adhesive: Deionized water, sorbitol and polyethylene glycol-8 are put into an aqueous phase pot and heated to 75°C to dissolve. Xanthan gum and guar gum are added and stirred at high speed until fully swollen to form a stable adhesive base.

[0036] (2) Medium temperature powder mixing: Cool down to 45°C, add soft hydrated silica, nano hydroxyapatite and bioactive glass in sequence, and vacuum homogenize and stir until the powder is evenly dispersed.

[0037] (3) Adding efficacy: Add sodium lauroyl sarcosinate, sodium hyaluronate, centella asiatica extract, dipotassium glycyrrhizate, potassium nitrate, zinc citrate and vitamin E at 45℃ and stir at medium speed until uniform.

[0038] (4) Low-temperature protection: Continue cooling to ≤38℃, add microcapsule colorant and WS-23 cooling agent, and stir gently at low speed (6.8 rpm). The color will automatically fade in a neutral environment, achieving "only staining plaque, not teeth". This invention also provides a gradient cooling preparation process, adult and children's special formulas, plaque visualization detection methods, and multi-purpose applications. The product has plaque display, anti-allergy, repair, and whitening functions. It is highly stable, safe and non-irritating, can be industrially produced, and is suitable for use by all people.

Claims

1. A pH-responsive plaque visualization and triple anti-sensitivity synergistic oral care composition, characterized in that, Include: (a) pH-responsive microcapsule colorimetric agent, wherein the microcapsule is composed of a wall material and a core material, the core material is a food-grade pH-changing dye that fades in a pH 6.8 environment, the wall material is a biocompatible polymer film-forming material, and the particle size of the microcapsule is 8-20 μm; (b) A triple anti-allergy system composed of potassium salt, bioactive glass and nano hydroxyapatite, with a weight ratio of 1:0.5-1.5:1.5-2.

5. (c) Periodontal repair system, composed of Centella Asiatica extract, dipotassium glycyrrhizate, sodium hyaluronate and zinc citrate; (d) Mild base containing soft hydrated silica abrasive, sodium lauroyl sarcosinate as a surfactant, 1,2-hexanediol and p-hydroxyacetophenone as preservatives, and free of sodium lauryl sulfate, fluorides, and parabens.

2. The oral care composition according to claim 1, characterized in that, The core material is selected from at least one of gardenia blue pigment, anthocyanin derivatives, or curcumin; the wall material is selected from a gelatin-gum arabic system or a sodium alginate-chitosan system; the surface of the microcapsule is provided with a microporous structure with a pore size of 0.1-0.5 μm.

3. The oral care composition according to claim 2, characterized in that, The oral care composition is a toothpaste formulation, and by weight percentage, the adult formulation includes: 55.03% deionized water, 28.00% sorbitol, 3.50% polyethylene glycol-8, 5.00% soft hydrated silica, 2.00% nano hydroxyapatite, 1.00% bioactive glass, 1.40% sodium lauroyl sarcosinate, 0.16% microcapsule colorant, 1.00% potassium nitrate, 0.10% dipotassium glycyrrhizate, 0.12% Centella asiatica extract, 0.10% sodium hyaluronate, 0.08% zinc citrate, 0.55% xanthan gum, 0.25% guar gum, 0.80% flavoring, 0.01% WS-23 cooling agent, 0.04% steviol glycosides, 0.05% vitamin E, 0.45% 1,2-hexanediol, and 0.36% p-hydroxyacetophenone.

4. The oral care composition according to claim 2, characterized in that, The oral care composition is a children's toothpaste formulation, free of potassium nitrate and bioactive glass; by weight percentage, the children's formula includes: 56.41% deionized water, 28.50% sorbitol, 3.20% polyethylene glycol-8, 4.80% ultra-soft hydrated silica, 1.80% nano hydroxyapatite, 1.10% sodium lauroyl sarcosinate, 0.15% microencapsulated colorant, 0.06% dipotassium glycyrrhizate, 0.08% centella asiatica extract, 0.06% vitamin B5, 0.50% xanthan gum, 0.25% guar gum, 0.80% flavoring, 0.04% steviol glycosides, 0.40% 1,2-hexanediol, and 0.32% p-hydroxyacetophenone.

5. A method for preparing the oral care composition according to any one of claims 1-4, characterized in that, Including gradient cooling process: (1) High-temperature adhesive preparation: The aqueous components and thickener are mixed and swollen at 70-80℃ and a vacuum degree of -0.06 to -0.08MPa to form an adhesive base; (2) Medium-temperature mixing: Cool down to 40-50℃, add abrasive and mineral powder, and vacuum stir for 20-30 minutes until uniform; (3) Low temperature protection: Continue to cool down to ≤38℃, add microcapsule color developer, and control the stirring speed to 300-500rpm; (4) Post-processing: After mixing evenly, vacuum degas for 30 minutes, let stand and mature for 20-24 hours, and then aseptically fill and shape.

6. The method according to claim 5, characterized in that, The microcapsule colorimetric agent mentioned in step (3) is prepared in advance by complex coagulation method, with an average particle size of 10-15 μm.

7. A method for detecting plaque using the oral care composition according to any one of claims 1-4, characterized in that, Includes the following steps: The oral care composition is applied to the tooth surface, and brushing for 1-2 minutes causes the microcapsules to rupture under shear force. In the acidic environment of plaque (pH 6.8), the color disappears automatically.

8. The use of the oral care composition according to any one of claims 1-4 in the preparation of oral care products for relieving dentin hypersensitivity, inhibiting plaque, repairing periodontal tissue, or gently whitening teeth.