Complex for whitening and remineralizing teeth, composition based on complex, toothpaste based on composition, gel based on composition, impregnation for strips based on composition, and method for producing composition

Abstract

FIELD: dental hygiene.SUBSTANCE: complex and composition for whitening and remineralizing teeth, method for producing the composition and oral care products containing the said composition. The following are proposed: a complex containing calcium hydroxyapatite, coconut oil and phthalimidoperoxycaproic acid in a mass ratio of components: [coconut oil]: [phthalimidoperoxycaproic acid]: [calcium hydroxyapatite] = 1: [0.2–11]: [0.5–150]; and a composition that contains the above complex and an acceptable carrier. The proposed method for producing a composition for whitening and remineralizing teeth involves preparing a water-glycerin gel base containing a sweetener, a desensitizing agent, and a thickener, which is homogenized until a homogeneous mixture structure is obtained, after which calcium hydroxyapatite is introduced into the resulting mixture, then an oil phase is prepared with coconut oil and substances selected from a group including a surfactant, a solubilizer, a preservative, a flavoring agent, a cooling agent, and a 17% suspension of phthalimidoperoxycaproic acid is introduced into this phase at T = 30-35 °C with subsequent stirring until the said suspension is completely distributed in the oil phase, after which the oil phase is introduced into the water-glycerin base mixture, the pH is controlled, adjusted to pH values of 6.2-6.6, after which the finished composition is placed for deaeration in a vacuum chamber to pump out air. Also the following are proposed: toothpaste, a teeth whitening gel and an impregnation for teeth whitening strips, where each of the said agents contains a composition for whitening and remineralizing teeth, including calcium hydroxyapatite, coconut oil and phthalimidoperoxycaproic acid and a corresponding carrier, wherein the content of the above components in the agent is, wt.%: calcium hydroxyapatite 0.5-15, phthalimidoperoxycaproic acid 0.2–1.1, coconut oil 0.1–1.EFFECT: reliable teeth whitening in combination with a remineralizing effect while ensuring high safety of use.15 cl, 6 tbl, 5 ex

Description

[0001] The invention relates to dentistry and the field of dental hygiene and concerns the production of a therapeutic and prophylactic composition for whitening and remineralizing teeth.

[0002] With age, tooth enamel loses its whiteness, especially if you can't go a morning without a cup of hot tea or coffee. These contain a special pigment that literally eats into your teeth. Smokers suffer even more. There are many ways to whiten your teeth, including at the dentist's office or using folk remedies. For example, enamel whitening with hydrogen peroxide is a fairly common method that can restore a whiter smile at a low cost. The whitening process is based on an oxidation reaction. During this chemical reaction, organic substances break down into carbon dioxide and water. This type of cleaning / whitening falls under the category of whitening using chemically active substances.

[0003] US 2023210729 describes a strip or film for whitening teeth and / or reducing tooth sensitivity, comprising: about 1-20% by weight of hydroxyapatite (HAP). In particular, this invention concerns a thin, orally soluble strip or film for whitening teeth and / or reducing tooth sensitivity, containing hydroxyapatite, which is in both nano- and non-nano form. HAP can be in the form of a paste, such as nanoXIM paste (trade name). The strips can include whitening agents, such as phthalimidoperoxycaproic acid (PPA) and / or hydrogen peroxide.

[0004] GB 2596143 provides a strip or film for teeth whitening and / or reducing tooth sensitivity, containing about 1-20% by weight of hydroxyapatite (HAP). The strip or film may be soluble or substantially soluble in the oral cavity. The strip or film may further contain 10-30% by weight of hydrogen peroxide and / or 0.01-5% by weight of phthalimidoperoxycaproic acid (PPC). The strip or film may contain a soluble film-forming polymer selected from pullulan, pectin, starch, dextrin, chitosan, alginic acid, alginic acid salts, and cellulose derivatives. HAP may be in the form of a nanocrystalline form, a paste, or in the form of pentacalcium hydroxytriphosphate.

[0005] This patent source also describes a method for making this strip, which includes mixing at least one or a combination of polyvinylpyrrolidone (PVP) polymers, 1-20 wt.% HAP and at least one or a combination of polycarbophils with water to produce a tooth whitening liquid; applying the tooth whitening liquid to a substrate; drying the substrate to form a whitening film on the substrate having a thickness of 50 to 500 μm.

[0006] US 2022226218 describes a tooth whitening film comprising a tooth whitening agent comprising a hydrogen peroxide-free whitening agent and hydrogen peroxide in a hydrogen peroxide-polymer complex, one or more polyphosphates, wherein said one or more polyphosphates include one or more cyclic polyphosphates, one or more water-soluble film-forming polymers, one or more plasticizers and one or more emulsifiers, wherein the film thickness is from about 50 μm to about 500 μm. Wherein said hydrogen peroxide-free whitening agent and hydrogen peroxide are present in a total amount of from about 0.01% to about 35% by weight.

[0007] In one embodiment, the hydrogen peroxide-free whitening agent comprises a peroxycarboxylic acid. In a preferred embodiment, the peroxycarboxylic acid is 6-peroxyphthalimidoperoxycaproic acid.

[0008] However, when used in conjunction with teeth whitening, hydrogen peroxide weakens enamel and irritates the oral mucosa. Hydrogen peroxide helps remove yellow plaque, enamel darkening, and certain pigment spots. Typically, a 3-6% concentration is used. Regular or inattentive use of hydrogen peroxide contributes to the destruction of natural enamel, a process that is irreversible. Accidental burns can also result from this whitening. Despite its more pronounced effect than mechanical cleaning, this whitening method has raised a number of concerns among specialists. The outcome of the procedure depends on the dentist's qualifications. The slightest mistake when isolating the gum line can have unpleasant consequences for the patient. High concentrations of hydrogen peroxide (up to 44%) destroy hydroxyapatite, the building block of enamel, and if it comes into contact with the mucosa, it can cause a chemical burn. In-office whitening has a number of contraindications that should also be kept in mind.These include: caries, tooth sensitivity, filled or devitalized teeth in the "smile zone," enamel erosion, and any gum disease. After the procedure, patients often experience tooth hypersensitivity. There is also evidence that with prolonged contact with enamel, peroxides can penetrate beyond the dentin, into the soft tissue of the tooth—the pulp—and cause inflammation.

[0009] Another important point: after professional whitening, it's worth choosing a special remineralizing toothpaste with calcium hydroxyapatite. The hydroxyapatite formula acts as a building material: it penetrates microcracks in the enamel, strengthening it and providing long-lasting results.

[0010] A in RU 2131723, A61K 7 / 16, publ. On June 20, 1999 (accepted as a prototype), a hydrogen peroxide-free therapeutic and prophylactic composition for treating teeth was described, containing an abrasive material - synthetic finely dispersed amorphous silicon dioxide, a surfactant - sodium lauryl sulfate, humectants, a dye - titanium dioxide pigment, a sweetener - saccharin and water, a hydroxyapatite paste consisting of water and hydroxyapatite with particle sizes of 0.0001 - 2.0 μm, and water-alcohol-glycerin extracts of yarrow and nettle, as well as sodium carboxymethylcellulose and food-grade sodium benzoate, and glycerin and sorbitol are used as humectants in the following ratios of components, wt. %:

[0011] Synthetic finely dispersed amorphous silicon dioxide - 16.9 - 22.1

[0012] Sodium carboxymethylcellulose - 0.8 - 1.9

[0013] Sodium benzoate food grade - 0.28 - 0.56

[0014] Titanium dioxide - 0.29 - 0.60

[0015] Hydroxyapatite paste (in terms of 100%) - 0.15 - 5.0

[0016] Yarrow water-alcohol-glycerin extract - 0.1 - 1.4

[0017] Nettle water-alcohol-glycerin extract - 0.1 - 1.4

[0018] Distilled glycerin - 7.1 - 12.9

[0019] Sorbitol - 25.3 - 34.2

[0020] Saccharin - 0.06 - 0.11

[0021] Sodium lauryl sulfate, in terms of 100% - 0.9 - 1.0

[0022] Water - Rest.

[0023] While possessing good preventive properties and the ability to prevent the occurrence of periodontitis and periodontal disease due to the inclusion of therapeutic and preventive additives, this composition does not have good cleaning and whitening properties, despite the inclusion of HAP in the form of a paste.

[0024] The present invention is aimed at achieving a technical result consisting in increasing the whitening and remineralizing properties while ensuring high safety of use.

[0025] The specified technical result is achieved in that the complex for teeth whitening and remineralization contains calcium hydroxyapatite, coconut oil and phthalimidoperoxycaproic acid in the following mass ratio of components: [coconut oil]: [phthalimidoperoxycaproic acid]: [calcium hydroxyapatite] = 1: [0.2-11]: [0.5-150]

[0026] The specified technical result is achieved in that the composition for whitening and remineralizing teeth contains an acceptable carrier and a complex consisting of calcium hydroxyapatite, coconut oil and phthalimidoperoxycaproic acid in the following mass ratio of the components: [coconut oil]: [phthalimidoperoxycaproic acid]: [calcium hydroxyapatite] = 1: [0.2-11]: [0.5-150]

[0027] The composition can be in the form of toothpaste or be a gel or impregnation for teeth whitening strips.

[0028] A suitable carrier contains a solvent, a humectant, a sweetener, a thickener, an abrasive, a preservative, a flavoring agent, a cooling agent, a surfactant, and an acidity regulator. In particular, the carrier contains a solvent, a humectant, a sweetener, a thickener, an abrasive, a preservative, a flavoring agent, a cooling agent, a surfactant, and an acidity regulator, in the following ratio of components, wt. %:

[0029] Solvent 20-40 Humidifier 25-55 Sweetener 0,1-0,5 Thickener 0,7-1,2 Abrasive 5-20 Preservative 0,5-1 Flavoring agent 0,1-1,5 Cooling agent 0,1-0,5 Surfactant 0,5-1,5 Acidity regulator (pH) qs pH=6.2-6.6

[0030] This composition uses 10% L-Arginine solution as an acidity regulator, sodium hydroxide or sodium bicarbonate or citric acid or sodium citrate as an acidity regulator.

[0031] The said technical result is also achieved in that the toothpaste made on the basis of the composition for whitening and remineralizing teeth includes calcium hydroxyapatite, coconut oil and phthalimidoperoxycaproic acid and a carrier including purified water as a solvent, glycerin and a 70% sorbitol solution as humectants, sodium saccharinate as a sweetener, carboxymethylcellulose as a thickener, hydrated silicon dioxide as an abrasive, phenoxyethanol and ethylhexylglycerin as a preservative, a flavoring agent, natural crystalline menthol as a cooling agent, sodium cocosulfate as a surfactant for foam formation, and a 10% L-Arginine solution as an acidity regulator, in the following ratio of components, wt. %:

[0032] Calcium hydroxyapatite 0,5 - 15 Phthalimidoperoxycaproic acid 0,2 - 1,1 Coconut oil 0,1 - 1 Purified water Up to 100 Glycerol 5-15 Sorbitol 70% solution 20-40 Sodium saccharinate 0,1-0,5 Carboxymethylcellulose 0,7-1,2 Hydrated silicon dioxide 5-20 Preservative (phenoxyethanol and ethylhexylglycerin) 0,5-1 Flavoring agent 0,1-1,5 Natural crystalline menthol 0,1-0,5 Sodium cocosulfate 0,5-1,5 L-Arginine (10% solution) qs pH=6.2-6.6

[0033] The said technical result is also achieved in that the teeth whitening gel made on the basis of the composition contains a composition for whitening and remineralizing teeth, including calcium hydroxyapatite, coconut oil and phthalimidoperoxycaproic acid and a carrier, including purified water as a solvent, glycerin as a humectant, sodium saccharinate as a sweetener, polyvinylpyrrolidone as a thickener and adhesive, carboxymethylcellulose as a thickener, phenoxyethanol and ethylhexylglycerin as a preservative, a flavoring agent, natural crystalline menthol as a cooling agent, hydrogenated castor oil as a surfactant-solubilizer, and a 10% solution of L-Arginine as an acidity regulator, in the following ratio of components, wt. %:

[0034] Calcium hydroxyapatite 0,5 - 15 Phthalimidoperoxycaproic acid 0,2 - 1,1 Coconut oil 0,1 - 1 Purified water Up to 100 Glycerol 5-10 Sodium saccharinate 0,1-0,5 Polyvinylpyrrolidone 3-9 Carboxymethylcellulose 0,5-1,5 Preservative (phenoxyethanol and ethylhexylglycerin) 0,5-1 Flavoring agent 0,1-1 Natural crystalline menthol 0,05-0,3 PEG-40 hydrogenated castor oil 0,5-1,5 L-Arginine (10% solution) qs pH=6.2-6.6

[0035] The said technical result is also achieved in that the impregnation for teeth whitening strips contains a composition for teeth whitening and remineralization, including calcium hydroxyapatite, coconut oil and phthalimidoperoxycaproic acid and a carrier, including purified water as a solvent, glycerin as a humectant, potassium citrate as a desensitizing agent, sodium saccharinate as a sweetener, polyvinylpyrrolidone as a thickener and adhesive, phenoxyethanol and ethylhexylglycerin as a preservative, a flavoring agent, natural crystalline menthol as a cooling agent, PEG-40 hydrogenated castor oil as a surfactant-solubilizer, a 10% solution of L-Arginine as an acidity regulator, in the following ratio of components, wt. %:

[0036] Calcium hydroxyapatite 0,5 - 15 Phthalimidoperoxycaproic acid 0,2 - 1,1 Coconut oil 0,1 - 1 Purified water Up to 100 Potassium citrate 1-5 Glycerol 10-20 Sodium saccharinate 0,1-0,5 Polyvinylpyrrolidone 1-4 Preservative (phenoxyethanol and ethylhexylglycerin) 0,5-1 Flavoring agent 0,1-1 Natural crystalline menthol 0,05-0,3 PEG-40 Hydrogenated Castor Oil 0,5-1,5 L-Arginine (10% solution) qs pH=6.2-6.6

[0037] The said technical result is also achieved in that, according to the method for producing a composition for whitening and remineralizing teeth, a water-glycerin gel base is first prepared, including purified water, sodium saccharinate as a sweetener, glycerin as a humectant, potassium citrate as a desensitizing agent, polyvinylpyrrolidone and / or carboxymethylcellulose as a thickener and homogenized until a homogeneous mixture structure is obtained, and calcium hydroxyapatite is introduced into the resulting mixture, then an oil phase is prepared with coconut oil and substances selected from the group consisting of sodium coco-sulfate as a surfactant, hydrogenated castor oil as a solubilizer, phenoxyethanol and ethylhexylglycerin as a preservative, a flavoring agent, natural crystalline menthol as a cooling agent,and a 17% suspension of phthalimidoperoxycaproic acid is introduced into this phase at T=30-35°C, followed by stirring until the suspension of phthalimidoperoxycaproic acid is completely distributed in the phase, after which the oil phase is introduced into the mixture of the water-glycerin base and the pH is controlled and the acidity level is adjusted to pH values ​​of 6.2-6.6, after which the finished composition is placed for deaeration in a vacuum chamber to pump out air.

[0038] Hydrated silicon dioxide is added to the water-glycerin gel base as an abrasive before the calcium hydroxyapatite is added. The acidity regulator is selected from a group including L-arginine, sodium hydroxide, sodium bicarbonate, citric acid, and sodium citrate.

[0039] These features are essential and form a stable set of essential features sufficient to obtain the required technical result.

[0040] According to the present invention, a new composition of calcium hydroxyapatite (HAP), phthalimidoperoxycaproic acid (PPC) and coconut oil in a composition for a 100% multi-component product composition is provided:

[0041] Calcium hydroxyapatite (HAP) 0,5 - 15 Coconut oil 0,1 - 1 Phthalimidoperoxycaproic acid (PPC) 0,2 - 1,1 Carrier with targeted additives The rest up to 100%

[0042] This tooth whitening and remineralizing composition contains calcium hydroxyapatite, coconut oil and phthalimidoperoxycaproic acid in the following weight ratio: [coconut oil]: [phthalimidoperoxycaproic acid]: [calcium hydroxyapatite] = 1: [0.2-11]: [0.5-150]

[0043] Table 1 shows the ranges of quantitative content of the components used in the developed recipes:

[0044] Table 1

[0045] № Name Purpose % input 1 Purified water Solvent 20-40 2 Glycerol Humidifier 5-15 3 Sorbitol 70% solution Humidifier 20-40 4 Sodium saccharinate Sweetener 0,1-0,5 5 Carboxymethylcellulose Thickener 0,7-1,2 6 Hydrated silicon dioxide Abrasive 5-20 7 Calcium hydroxyapatite Remineralizing and whitening additive 0,5 - 15 8 Phthalimidoperoxycaproic acid Whitening additive 0,2 - 1,1 9 Coconut oil Whitening, antibacterial additive 0,1 - 1 10 Preservative (phenoxyethanol and ethylhexylglycerin) Preservative 0,5-1 11 Flavoring agent Flavoring agent 0,1-1,5 12 Natural crystalline menthol Cooling agent 0,1-0,5 13 Sodium cocosulfate Surfactant (foam) 0,5-1,5 14 L-Arginine (10% solution)* pH regulator qs pH=6.2-6.6**

[0046] *In addition to L-Arginine, sodium hydroxide and sodium bicarbonate can be used as acidity regulators to increase pH; citric acid and sodium citrate can be used to lower pH.

[0047] The pH range can be 5.8-7.2, but based on the research done, 6.2-6.6 is preferable. (described below).

[0048] qs (or QS) is an abbreviation of the Latin quantum satis, meaning "as much as is sufficient."

[0049] This composition contains components that are safe in the stated quantities.

[0050] Calcium hydroxyapatite is a remineralizing agent that, through the physiological action of its hydroxyphosphate microparticles, penetrates into the microcavities of teeth and is capable of restoring the physiological density of enamel and its natural white appearance. Calcium hydroxyapatite mimics the structure of natural hydroxyapatite in teeth and bones, ensuring safety and effectiveness in oral care. It is an alternative for those who are unable to use, even partially, fluoride compounds in oral hygiene products. Calcium hydroxyapatite is a white, odorless powder. Solubility: slightly soluble in water, in the final product it is a suspension. pH: 6.5-7.5. It has a remineralizing effect, reduces tooth sensitivity, and also promotes tooth whitening.

[0051] The mechanism of action aimed at remineralization can be described as follows:

[0052] - Adhesion to the enamel-dentin junction and accumulation of calcium hydroxyapatite in crystalline form on the tooth surface, biofilm and in tooth lesions;

[0053] - "Smart" release of Ca ions 2+ depending on pH. After brushing your teeth (neutral pH), the calcium hydroxyapatite bound to the tooth slowly releases Ca 2+ into saliva. As the pH decreases during the day, calcium hydroxyapatite releases Ca ions 2+More quickly. At acidic pH in the oral cavity, calcium hydroxyapatite begins to release remineralizing ions, while maintaining its crystalline form at physiological pH. This pH-dependent chemical activity is important because the oral pH becomes acidic many times during the day, and the level of tooth-bound calcium hydroxyapatite increases proportionally and "on demand," ensuring the supply of calcium into saliva. The pH-dependent transition of biomimetic calcium hydroxyapatite from crystalline to soluble form enables long-lasting and "intelligent" remineralization.

[0054] - Formation of new calcium hydroxyapatite crystals, repairing damage. Ca 2+ , released into saliva, are used as "building blocks" to build new calcium hydroxyapatite crystals "from scratch".

[0055] In addition to remineralization, calcium hydroxyapatite reduces tooth sensitivity. Calcium hydroxyapatite inhibits the activation of nerves involved in hypersensitivity through a long-term, pH-dependent supply of calcium and phosphate. These ions more effectively form new calcium hydroxyapatite crystals, reducing microdamage and, consequently, reducing surface scratches that expose dental nerves to external agents.

[0056] To confirm the effect, an in vivo test was conducted: 50 participants with very sensitive teeth aged 18 to 70 years used a paste with 5% calcium hydroxyapatite 3 times a day for 2 weeks (testing was carried out at Biobasic Europe srl Università degli studi di Pavia, Department of Internal Medicine and Drug Therapy).

[0057] 80% of participants reported a significant reduction in hypersensitivity. Specifically, a reduction in sensitivity after consuming various beverages after 28 days of using the product:

[0058] - hot drinks: 46.6% felt a decrease in hypersensitivity;

[0059] - Cold drinks: 50% experienced a reduction in hypersensitivity

[0060] During testing, there were also no cases of inflammation or damage to the gums and oral cavity.

[0061] To confirm the whitening effect of calcium hydroxyapatite, a small study was conducted on 12 subjects. Using toothpaste with 10% calcium hydroxyapatite for 1 month (twice daily) resulted in a whitening of 1.4 shades on the Hunter scale (reddish-brown range) and 1.0 shade (yellow-red range). With a concentration of 15% calcium hydroxyapatite, whiteness increased by ~20% over 4 weeks. Pastes with 3% calcium hydroxyapatite increased gloss by 8.7%, and with 15%, by 21.3% (colorimetry data).

[0062] Coconut oil is a promising natural alternative in dentistry, especially for safety-conscious patients. Appearance: Coconut oil is a white or yellow liquid at 22 to 27°C; odorless or with a faint characteristic odor (refined). Solubility: Insoluble in water; in the final product, it exists as droplets surrounded by a surfactant emulsion (sodium cocosulfate or PEG-40 hydrogenated castor oil).

[0063] The effectiveness of coconut oil in toothpaste is due to the following factors. Research confirms that coconut oil has pronounced antimicrobial activity against the main cariogenic microorganisms (Streptococcus mutans, Lactobasillus fermentum, and Streptococcus mitis) and can be considered a promising natural alternative to traditional antiseptics in dental practice. Furthermore, coconut oil's fatty acids have been shown to be comparable in effectiveness to chlorhexidine. No side effects (irritation or allergies) were found in the studies. The toothpaste is also safe if accidentally swallowed. Using coconut oil in toothpaste also reduces the amount of abrasive, which contributes to less damage to tooth enamel. According to a study involving 100 elementary school students, coconut oil safely reduces plaque and tartar levels.And, according to other studies, it also provides a weak whitening effect after 2 weeks of use (Evaluation of Coconut Oil Pulling vs. Whitening Mouthwash as Home Teeth Whitening Methods. Shahad H. Rajab, Lujain K. Al-Hindi, Sahar M. Elmarsafy, AL-AZHAR Dental Journal For Girls. Vol. 8, No. 1, January (2021)).

[0064] Phthalimidoperoxycaproic acid is an organic peroxy acid (peracid) that is an active ingredient in the oxidation reaction of teeth whitening formulas. The pure substance appears as a white, odorless, crystalline powder. Solubility of the pure substance: slightly soluble in water, forms a stable suspension;

[0065] Phthalimidoperoxycaproic acid reacts with dental stains without generating free radicals (as does hydrogen peroxide) and does not cause excessive tooth sensitivity, gum irritation, demineralization, or reduction of the organic matrix in dentin. Phthalimidoperoxycaproic acid has several interesting properties that arise from the fact that the oxygen-oxygen single bond present in the molecule is very easily broken, releasing an oxygen atom, which is then incorporated into the target molecule. PAP reactions are significantly different from those of hydrogen peroxide. Phthalimidoperoxycaproic acid causes epoxidation. The greater the electron density of the double bond in the target, the more susceptible it is to this specific type of attack. This makes phthalimidoperoxycaproic acid ideal for attacking most molecules that cause tooth discoloration, as these aromatic rings are present in its structure.The whitening effect with phthalimidoperoxycaproic acid occurs faster and is more permanent than when using hydrogen peroxide.

[0066] Advantages of phthalimidoperoxycaproic acid over hydrogen peroxide:

[0067] - does not cause demineralization, erosion or etching of dental tissue;

[0068] - Does not cause soft tissue irritation such as bleaching, burning or blistering;

[0069] - does not require the use of a protective mouth guard for gums during the whitening procedure;

[0070] - causes much less sensitivity during or after the procedure compared to hydrogen peroxide.

[0071] To evaluate the efficacy of phthalimidoperoxycaproic acid, a new hydrogen peroxide-free whitening agent, a double-blind, placebo-controlled, short-term study was conducted after a single use. The study involved 40 volunteers (25 women, 15 men), divided into two groups: a test group (whitening gel) and a placebo group. Tooth color was assessed before (E0), immediately after (E1), and 24 hours after whitening (E2) using the VITA classical scale. Side effects (tooth hypersensitivity and gum irritation) were recorded clinically and by the participants. The test group showed a significant improvement in tooth color immediately after whitening (average change: 2.26 units) and after 24 hours (2.15 units), while there were no changes in the placebo group. 59% of teeth in the test group showed color improvement.Side effects were minimal: 10% of the test group participants experienced mild gum irritation and slight tooth hypersensitivity (Effectiveness of a new non-hydrogen peroxide bleaching agent after single use - a double-blind placebocontrolled short-term study. Mozhgan Bizhang. J. Appl. Oral Sci. 25 (5). Sep-Oct. 2017).

[0072] This shows that this new non-peroxide bleaching agent based on phthalimidoperoxycaproic acid is effective in whitening teeth after just one use, and its effect lasts for 24 hours. Side effects are minimal, making it a safe whitening option.

[0073] For the preparation of compositions based on the complex, a ready-made 17% suspension of phthalimidoperoxycaproic acid is used.

[0074] The following method for producing calcium hydroxyapatite (Ca5(PO4)3OH) is known.

[0075] Preparation of the initial reagents. Calcium hydroxide suspension (Ca(OH)2): prepared by dissolving calcium oxide (CaO) in distilled water at a constant solid:liquid (S:L) ratio of 1:35-40. This ensures a saturated solution suitable for pumping. Phosphoric acid solution (H3PO4): a solution with a concentration of 35-37 wt.% is used.

[0076] Carrying out the reaction in a two-zone closed-loop system. The process is carried out in a setup where the reaction mixture circulates in a closed loop, sequentially passing through two zones. The first zone (intensive mixing zone): a stoichiometric amount of H3PO4 solution is continuously added to the Ca(OH)2 suspension. In this zone, it is critical to maintain a strictly constant pH value in the range of 10.0-11.0. The suspension flow velocity should be 0.8-1.5 m / s. The residence time of the mixture in the first zone is 1.0-1.5 seconds. The second zone (dilution and crystallization zone): the mixture from the first zone is immediately (after 1.0-1.5 s) fed to the second zone. Here, it is diluted 400-500 times with the original calcium hydroxide (Ca(OH)2) suspension. This prevents the mixture from thickening and promotes the proper course of the reaction. After dilution, the mixture is returned to the first zone to continue the process.

[0077] Circulation and completion of the reaction: the described cycle (first zone → second zone → first zone) is repeated, ensuring 4-5 circulations of the entire reaction mixture. The total circulation time with continuous acid supply is 10-20 minutes. After this, the H3PO4 supply is stopped. Final stage: after stopping the acid supply, the suspension of the resulting product is further stirred in a closed cycle for 10-12 minutes to completely form crystals. Product isolation: the resulting suspension is centrifuged, separating the liquid phase. The resulting paste is dried. If necessary, the dry product is ground into powder.

[0078] A two-zone design with rapid mixing and controlled dilution prevents the formation of side phases. Strict pH control (10.0-11.0) eliminates conditions favorable for the formation of acidic calcium phosphates. High flow rates (0.8-1.5 m / s) ensure rapid and uniform mixing of the reagents. A closed circulation loop ensures complete reaction without the need for lengthy (up to 4 days) aging.

[0079] Phthalimidoperoxycaproic acid is a synthetic organic peroxy acid obtained from caprolactam and phthalic anhydride.

[0080] General method for the preparation of ω-phthalimidoperoxyalkanoic acids. The synthesis of the target peroxyacids is carried out in three stages with an overall yield of 60-90%.

[0081] Synthesis circuit:

[0082] Esterification: ω-Bromoalkanoic acid undergoes esterification in an alcoholic solution in the presence of sulfuric acid.

[0083] Preparation of phthalimide ester: ω-bromoalkanoic acid ester reacts with potassium phthalimide in acetonitrile under reflux for 4 hours. This reaction yields ω-phthalimidoalkyl ester.

[0084] Perhydrolysis (oxidation): The final step is the conversion of the resulting ester into a peroxyacid. A general method described in the literature is used for this: 30% hydrogen peroxide (110 volumes) is added to the ω-phthalimidoalkane ester in concentrated sulfuric acid at a temperature below +10°C.

[0085] In industry, a direct method is used - condensation of phthalic anhydride with γ-pyrrolidone or ε-caprolactam in the presence of water at high temperature and under pressure.

[0086] Industrial coconut oil is obtained from fresh or dried copra (flesh) of coconut.

[0087] The main raw material is copra (dried coconut meat). It is dried to 5-7% moisture content in industrial drying ovens to prevent spoilage and mold. The dried copra is crushed into large pieces and then ground into small flakes or granules. This increases the surface area for subsequent extraction. The crushed copra is placed in multi-stage extractors and repeatedly washed with an organic solvent - hexane (C6H). 14). Hexane effectively dissolves and washes fats from copra cells. A solution of oil in hexane—miscella—is formed at the extractor outlet. The miscella is sent to distillation columns, where it is heated. Hexane, having a low boiling point (~69°C), evaporates, separates from the oil, and condenses for reuse. After the hexane is removed, crude, unrefined coconut oil remains. It has a yellow or brownish color, a strong odor, and contains numerous impurities (free fatty acids, phospholipids, coloring agents, hexane particles) and requires mandatory further purification (refining). The oil is heated to 70-80°C and treated with hot water or weak acids (for example, phosphoric acid H3PO4). The impurities hydrate, coagulate, and precipitate, which is removed by centrifugation. The oil is then treated with an alkaline solution (usually sodium hydroxide NaOH). Alkali reacts with acids to form soap (salts of fatty acids).The soap residue is separated from the oil using a centrifuge. The oil is heated to 90-110°C and mixed with adsorbents—bleaching earth (bentonite clay) and / or activated carbon. The adsorbents absorb all coloring substances. After processing, the oil is carefully filtered through filter presses to remove the spent clay. The oil is heated to high temperatures (approximately 200-250°C) under a high vacuum (to prevent oxidation). A stream of superheated steam is passed through the hot oil. Volatile substances evaporate and are removed. After this stage, the oil becomes completely clear, colorless, odorless, and tasteless.

[0088] The composition can be used to make toothpaste, gel, or impregnation for teeth whitening strips.

[0089] Below in Table 2 is example No. 1 of the component composition of toothpaste with a whitening system of calcium hydroxyapatite, phthalimidoperoxycaproic acid and coconut oil.

[0090] Table 2

[0091] Item No. Name Purpose % input 1 Purified water Solvent Up to 100 2 Glycerol Humidifier 5-15 3 Sorbitol 70% solution Humidifier 20-40 4 Sodium saccharinate Sweetener 0,1-0,5 5 Carboxymethylcellulose Thickener 0,7-1,2 6 Hydrated silicon dioxide Abrasive 5-20 7 Calcium hydroxyapatite Remineralizing and whitening additive 0,5 8 Phthalimidoperoxycaproic acid Whitening additive 0.2 (1.18 - 17% suspension) 9 Coconut oil Whitening, antibacterial additive 0,1 10 Preservative (phenoxyethanol and ethylhexylglycerin) Preservative 0,5-1 11 Flavoring agent Flavoring agent 0,1-1,5 12 Natural crystalline menthol Cooling agent 0,1-0,5 13 Sodium cocosulfate Surfactant (foam) 0,5-1,5 14 L-Arginine (10% solution) pH regulator qs pH=6.2-6.6

[0092] Toothpaste production equipment includes a homogenizer with digital speed control (0-3000 rpm) and a lifting mechanism, an overhead stirrer with digital speed control (0-800 rpm) and a propeller-type stirrer, a heated magnetic stirrer with digital speed and temperature control, analytical scales with an accuracy of 0.01 g, a pH meter with calibration buffers, a vacuum chamber for removing air, a glass beaker with a capacity of at least 150 ml, a porcelain bowl for preparing premixes, and other auxiliary accessories for dosing the raw components of the formulation.

[0093] All components are weighed with an accuracy of ±0.01 g of the required mass.

[0094] Add 83% of the calculated amount of purified water, sodium saccharinate, and 70% sorbitol to a glass beaker. Place the beaker on a heated magnetic stirrer and heat to 50-55°C with constant stirring at 150-200 rpm. Prepare a premix of the calculated amount of glycerin and carboxymethyl cellulose in a porcelain bowl. Dispense the carboxymethyl cellulose powder into the bowl, add glycerin using a Pasteur pipette, and then intensively disperse the polymer in the glycerin with a spatula. The resulting dispersion should be homogeneous and lump-free. Add the resulting premix in a thin stream with constant stirring (300-350 rpm) to the beaker containing water, sodium saccharinate, and 70% sorbitol. Stirring is continued at a temperature of 50-55°C for at least 40 minutes until the carboxymethyl cellulose is completely swollen and a transparent, homogeneous gel without particles is formed.

[0095] Then the base temperature is reduced to 45°C, and the beaker is moved under an overhead stirrer. With constant stirring (250-300 rpm), hydrated silicon dioxide is slowly added in portions. After it is evenly distributed (after 15-20 minutes), calcium hydroxyapatite is added in the same manner. Mix for 30 minutes at 200-250 rpm until the calcium hydroxyapatite is completely and evenly distributed throughout the mixture.

[0096] The prepared 17% phthalimidoperoxycaproic acid suspension is carefully injected into the prepared paste mixture in a thin stream using a Pasteur pipette at a temperature of approximately 30-35°C while stirring constantly at 150-200 rpm. The mixture is stirred for approximately 15-20 minutes until the phthalimidoperoxycaproic acid suspension is completely distributed throughout the mixture.

[0097] Next, prepare and add the oil phase containing the active ingredient. Mix 17% purified water (based on the total required amount) and the calculated amount of sodium coco-sulfate in a porcelain bowl at 50°C and 100-150 rpm. Stir until the sodium coco-sulfate is completely dissolved. Cool the premix to 45°C, then add the menthol. Stir at 150-200 rpm until the menthol is completely dissolved in the sodium coco-sulfate solution. Cool the mixture to 35°C, add the flavoring, preservative, and coconut oil, and stir again at 150-200 rpm on a magnetic stirrer until all components are completely dissolved. Gently add the premix in a thin stream into the prepared toothpaste base while stirring constantly. After adding, mix the entire mass at 300-400 rpm for 15-20 minutes until the premix is ​​completely distributed in the mass.

[0098] The pH is checked (6.2-6.6) and adjusted if necessary with a 10% L-Arginine solution. In addition to L-Arginine, sodium hydroxide and sodium bicarbonate can be used as acidity regulators to increase the pH; citric acid and sodium citrate can be used to lower the pH. To remove air bubbles, the finished paste is placed in a vacuum chamber for 30 minutes. The finished product is unloaded into an airtight container.

[0099] Table 3 shows example No. 2 - toothpaste with a whitening system of calcium hydroxyapatite, phthalimidoperoxycaproic acid and coconut oil (see Table 3).

[0100] Table 3

[0101] Item No. Name Purpose % input 1 Purified water Solvent Up to 100 2 Glycerol Humidifier 5-15 3 Sorbitol 70% solution Humidifier 20-40 4 Sodium saccharinate Sweetener 0,1-0,5 5 Carboxymethylcellulose Thickener 0,7-1,2 6 Hydrated silicon dioxide Abrasive 5-20 7 Calcium hydroxyapatite Remineralizing and whitening additive 7,5 8 Phthalimidoperoxycaproic acid Whitening additive 0.65 (3.82 - 17% suspension) 9 Coconut oil Whitening, antibacterial additive 0,5 10 Preservative (phenoxyethanol and ethylhexylglycerin) Preservative 0,5-1 11 Flavoring agent Flavoring agent 0,1-1,5 12 Natural crystalline menthol Cooling agent 0,1-0,5 13 Sodium cocosulfate Surfactant (foam) 0,5-1,5 14 L-Arginine (10% solution) pH regulator qs pH=6.2-6.6

[0102] The method for obtaining the paste is similar to example No. 1.

[0103] Table 4 shows example No. 3 - toothpaste with a whitening system of calcium hydroxyapatite, phthalimidoperoxycaproic acid and coconut oil.

[0104] Table 4

[0105] Item No. Name Purpose % input 1 Purified water Solvent Up to 100 2 Glycerol Humidifier 5-15 3 Sorbitol 70% solution Humidifier 20-40 4 Sodium saccharinate Sweetener 0,1-0,5 5 Carboxymethylcellulose Thickener 0,7-1,2 6 Hydrated silicon dioxide Abrasive 10 7 Calcium hydroxyapatite Remineralizing and whitening additive 15 8 Phthalimidoperoxycaproic acid Whitening additive 1.1 (6.47 - 17% suspension) 9 Coconut oil Whitening, antibacterial additive 1 10 Preservative (phenoxyethanol and ethylhexylglycerin) Preservative 0,5-1 11 Flavoring agent Flavoring agent 0,1-1,5 12 Natural crystalline menthol Cooling agent 0,1-0,5 13 Sodium cocosulfate Surfactant (foam) 0,5-1,5 14 L-Arginine (10% solution) pH regulator qs pH=6.2-6.6

[0106] The method of obtaining is similar to example No. 1.

[0107] Table 5 shows example No. 4 - a whitening gel in the form of a pencil with a brush based on a whitening system of calcium hydroxyapatite, phthalimidoperoxycaproic acid and coconut oil.

[0108] Table 5

[0109] Item No. Name Purpose % input 1 Purified water Solvent up to 100 2 Glycerol Humidifier 5-10 3 Sodium saccharinate Sweetener 0,1-0,5 4 Polyvinylpyrrolidone Thickener and adhesive 3-9 5 Carboxymethylcellulose Thickener 0,5-1,5 6 Calcium hydroxyapatite Remineralizing and whitening additive 4,5 7 Phthalimidoperoxycaproic acid Whitening additive 1 (5.88 - 17% suspension) 8 Coconut oil Whitening, antibacterial additive 0,2 9 Preservative (phenoxyethanol and ethylhexylglycerin) Preservative 0,5-1 10 Flavoring agent Flavoring agent 0,1-1 11 Natural crystalline menthol Cooling agent 0,05-0,3 12 PEG-40 hydrogenated castor oil Solubilizer 0,5-1,5 13 L-Arginine (10% solution) pH regulator qs pH=6.2-6.6

[0110] Below is a description of the method for producing a dental gel with a whitening system from calcium hydroxyapatite, phthalimidoperoxycaproic acid and coconut oil.

[0111] Purified water at room temperature and sodium saccharinate are placed in a glass beaker. The beaker is placed on a heated magnetic stirrer. Heating is started to 50-55°C with constant stirring at 150-200 rpm. The calculated amount of polyvinylpyrrolidone is dispensed into the same beaker and homogenized at 2000-2500 rpm for 5-7 minutes until a homogeneous gel is obtained. A premix of the calculated amount of glycerin and carboxymethyl cellulose is prepared in a porcelain bowl. Carboxymethyl cellulose powder is dispensed into the bowl, glycerin is added there, and then the polymer is intensively dispersed in glycerin using a spatula. The result of dispersion should be a homogeneous mass without lumps. The resulting premix is ​​added to the total mass in a thin stream with constant stirring (300-350 rpm). Stirring is continued at a temperature of 50-55°C for at least 40-60 minutes until the carboxymethyl cellulose is completely hydrated and a homogeneous gel is formed.At the end, homogenization at 2000-2500 rpm for 5-7 minutes is permissible.

[0112] Then the base temperature is reduced to 45°C, and the beaker is moved under an overhead stirrer. With constant stirring (250-300 rpm), calcium hydroxyapatite is slowly added in portions. Mix for 30 minutes at 200-250 rpm until the calcium hydroxyapatite is completely and evenly distributed throughout the mixture.

[0113] The prepared 17% phthalimidoperoxycaproic acid suspension is carefully injected into the prepared paste mixture in a thin stream using a Pasteur pipette at 30-35°C while stirring constantly at 150-200 rpm. The mixture is stirred for approximately 15-20 minutes until the phthalimidoperoxycaproic acid suspension is completely distributed throughout the mixture.

[0114] To prepare the oil phase with the active ingredient, mix PEG-40 hydrogenated castor oil, coconut oil, preservative, flavoring, and natural crystalline menthol in a porcelain bowl at 45°C and 100-150 rpm until smooth. Gently inject the premix in a thin stream into the prepared whitening gel base while stirring constantly. After adding the premix, stir the entire mixture at 300-400 rpm for 15-20 minutes until the premix is ​​completely distributed.

[0115] Then check the pH (6.2-6.6) and adjust it if necessary with a 10% L-Arginine solution. In addition to L-Arginine, sodium hydroxide and sodium bicarbonate can be used as acidity regulators to increase the pH; citric acid and sodium citrate can be used to lower the pH. To remove air bubbles, place the finished paste in a vacuum chamber for 30 minutes. The finished product is unloaded into an airtight container.

[0116] Table 6 shows example No. 5 - impregnation based on a whitening system of calcium hydroxyapatite, phthalimidoperoxycaproic acid and coconut oil for whitening strips.

[0117] Table 6

[0118] Item No. Name Purpose % input 1 Purified water Solvent up to 100 2 Potassium citrate Desensitizing agent 1-5 3 Glycerol Humidifier 10-20 4 Sodium saccharinate Sweetener 0,1-0,5 5 Polyvinylpyrrolidone Thickener and adhesive 1-4 7 Calcium hydroxyapatite Remineralizing and whitening additive 0,5 8 Phthalimidoperoxycaproic acid Whitening additive 1.1 (6.47 - 17% suspension) 9 Coconut oil Whitening, antibacterial additive 0,4 10 Preservative (phenoxyethanol and ethylhexylglycerin) Preservative 0,5-1 11 Flavoring agent Flavoring agent 0,1-1 12 Natural crystalline menthol Cooling agent 0,05-0,3 13 PEG-40 hydrogenated castor oil Solubilizer 0,5-1,5 14 L-Arginine (10% solution) pH regulator qs pH=6.2-6.6

[0119] To prepare a water-glycerin gel base, place purified water at room temperature, sodium saccharinate, glycerin, and potassium citrate in a glass beaker. Place the beaker on a heated magnetic stirrer. Heat to 50-55°C with constant stirring at 150-200 rpm. Add the calculated amount of polyvinylpyrrolidone to the same beaker and homogenize at 2000-2500 rpm for 5-7 minutes until a homogeneous gel is obtained.

[0120] After this, the base temperature is reduced to 45°C, and the beaker is moved under an overhead stirrer. With constant stirring (250-300 rpm), calcium hydroxyapatite is slowly added in portions. Mix for 30 minutes at 200-250 rpm until the calcium hydroxyapatite is completely and evenly distributed throughout the mixture.

[0121] The prepared 17% phthalimidoperoxycaproic acid suspension is carefully injected into the prepared paste mixture in a thin stream at 30-35°C using a Pasteur pipette while stirring constantly at 150-200 rpm. The mixture is stirred for approximately 15-20 minutes until the phthalimidoperoxycaproic acid suspension is completely distributed throughout the mixture.

[0122] To prepare and add the oil phase with the active ingredient, mix PEG-40 hydrogenated castor oil, coconut oil, preservative, flavoring, and natural crystalline menthol in a porcelain bowl at 45°C and 100-150 rpm until smooth. Gently inject the premix in a thin stream into the prepared whitening gel base while stirring constantly. After adding the premix, stir the entire mixture at 300-400 rpm for 15-20 minutes until the premix is ​​completely distributed.

[0123] The pH is checked (6.2-6.6) and adjusted if necessary with a 10% L-Arginine solution or another acidity regulator: sodium hydroxide, sodium bicarbonate (to increase the pH); citric acid, sodium citrate (to lower the pH). To remove air bubbles, the finished paste is placed in a vacuum chamber for 30 minutes. The finished product is unloaded into an airtight container.

[0124] The resulting solution is used as a soak for whitening strips. The strips can be made of a flexible polyethylene carrier, or they can be a silicone or hydrogel base, which ensures a tight fit and adhesion to the teeth. The strips are soaked in a solution containing a whitening complex of calcium hydroxyapatite, phthalimidoperoxycaproic acid, and coconut oil, then placed in a sealed blister to prevent evaporation. Upon contact with the teeth, the soak is released, allowing the active components of the complex to activate and initiate the pigment oxidation process.

[0125] Using the examples of toothpastes #1 and #3 presented above, consumer testing was conducted. Eight consumer groups of 30 people were formed for the study. Participants ranged in age from 20 to 40 years old, and all complained of increased tooth sensitivity. Each group was offered the same formula of toothpaste #1 or #3, but with different pH values ​​within the acceptable range. The testing lasted one month: participants used the toothpaste daily, while simultaneously completing a survey and measuring whitening on the Vita Classical scale once a week. This approach allowed us to evaluate not only the product's stated properties but also to identify additional unexpected, yet valuable, synergies between the three key components of the complex:

[0126] phthalimidoperoxycaproic acid, responsible for whitening;

[0127] calcium hydroxyapatite, which performs remineralizing, whitening and protective functions;

[0128] Coconut oil, softening the action of active ingredients, has antibacterial and whitening properties.

[0129] Different pH values ​​created unique conditions for the interaction of these substances. Therefore, each group demonstrated its own unique effects, varying in intensity and combination of whitening, remineralization, and sensitivity reduction.

[0130] To minimize subjective distortions, comparisons are conducted under standardized lighting conditions. Natural daylight is recommended. Avoid the presence of extraneous color cues (bright clothing, lipstick, or colored surfaces). Whitening progress was monitored using the Vita Classical tooth color comparison scale.

[0131] The comparison was performed on the vestibular surface of the maxillary central incisors, as they are most indicative of the base shade. The middle third of the tooth crown is primarily analyzed, as the cervical region tends to be more saturated, while the incisal edge tends to be lighter.

[0132] The Vita Classical set includes 16 standard ceramic shade samples, divided into four chromatic groups: A (reddish-brown tones: A1-A4), B (reddish-yellow: B1-B4), C (grayish: C1-C4), D (reddish-gray: D2-D4). First, the dominant color tone (group AD) is determined, then the lightness level within the group is specified (e.g., A2, B1, C3).

[0133] The scale sample was applied to the tooth at a distance of 1-2 mm, without overlapping the gingival or incisal edges. The comparison was performed as quickly as possible (≤ 5 seconds) to avoid retinal color adaptation. If in doubt, the procedure may be repeated, temporarily diverting the gaze to a neutral background (gray card).

[0134] The base shade of the tooth (e.g., A3) was initially recorded. After a course of whitening, the procedure was repeated. The result was expressed in conventional units of "shade change" (e.g., 3 shades lighter).

[0135] Example No. 1 Calcium hydroxyapatite - 0.5% Phthalimidoperoxycaproic acid - 0.2% Coconut oil - 0.1% Example No. 2. Calcium hydroxyapatite - 15% Phthalimidoperoxycaproic acid - 1.1% Coconut oil - 1% Group A, pH 5.8: Approximately 72% of participants reported an enamel lightening effect of 1-1.5 shades by the end of the first week, which is likely due to the increased oxidative activity of phthalimidoperoxycaproic acid in a slightly acidic environment. Seventy percent of participants reported a decrease in the severity of dental hypersensitivity when exposed to thermal stimuli (cold / heat). This effect can be explained by the partial solubility of calcium hydroxyapatite at pH below 6, accompanied by the release of Ca2+ ions and their subsequent integration into the dentinal tubules. The remaining 30% of participants noted dynamic changes in sensitivity throughout the day. It can be indirectly concluded that at pH 5.8, remineralization is more dynamic and "reactive" in nature due to the rapid release of Ca2+ ions and a decrease in the ion reserve in the calcium hydroxyapatite "depot." 20% of respondents reported fresher breath after sleep. In Group A2 (pH 5.8), phthalimidoperoxycaproic acid also demonstrated maximum activity in a slightly acidic environment. Nearly 80% of participants demonstrated enamel lightening of 2.5-3 shades, but only by the end of week 4. This delayed effect may be related to the shielding effect of calcium hydroxyapatite, which precipitates on the tooth surface, slowing the oxidation of pigments that color tooth enamel. Hypersensitivity was recorded in only 15% of respondents; the remaining participants noticed a decrease in sensitivity. Symptoms manifested primarily upon exposure to temperature irritants (cold, acidic drinks). Most likely, the increased calcium hydroxyapatite intake, although not completely, neutralized the increased oxidative activity of phthalimidoperoxycaproic acid at low pH.No dynamic changes in sensitivity were observed throughout the day, which may be due to the relatively high calcium hydroxyapatite content of the toothpaste and the resulting formation of a so-called "depot" of Ca2+ ions, which reduces tooth sensitivity. Sixty percent of respondents reported fresher breath after sleep. Group B, pH 6.2: Phthalimidoperoxycaproic acid maintained high oxidative activity (whitening by 1 tone), while calcium hydroxyapatite formed a more stable mineralizing layer. Over 80% of participants reported a decrease in hyperesthesia by the end of the first week. Sensitivity did not increase until the end of testing, which is associated with the process of dentinal tubule blockage. Almost 60% of respondents noted an increase in the gloss and smoothness of enamel, likely due to the combined effect of organic pigment oxidation and calcium hydroxyapatite deposition on the tooth surface. Such effects may be related to the solubility of calcium hydroxyapatite. At pH 6.2, solubility decreases but remains sufficient to maintain a stable ion flow. Remineralization in this case was slow but steady. Respondents did not note a change in sensitivity during the day. As with pH 5.8, approximately 18% of respondents reported fresher breath after sleep. Group B2 (pH 6.2): ​​Approximately 90% of participants observed a sustained whitening effect of 1.5-2 shades by the first week of testing. The decrease in whitening effect may be due to a decrease in the activity of phthalimidoperoxycaproic acid, as well as the shielding effect of calcium hydroxyapatite. Mild hypersensitivity was reported in <10% of participants. The tooth surface exhibited a higher gloss compared to the toothpaste with 3% calcium hydroxyapatite, indirectly indicating remineralization, compaction, and smoothing of the surface layer of the teeth. As with pH 5.8, approximately 50% of respondents reported fresher breath after sleep. Group C (pH 6.6): The whitening level remained the same as at pH 6.2, at approximately 1 shade. Most respondents reported maximum comfort: there were virtually no complaints of sensitivity, even with frequent consumption of cold beverages, indicating the pronounced remineralizing and desensitizing properties of calcium hydroxyapatite under neutral to slightly acidic conditions. Sixteen percent of respondents reported fresher breath after sleep. Group C2 pH 6.6: Whitening remained at the same level as with pH 6.2, reaching approximately 1.5-2 shades. The incidence of hypersensitivity at this point was minimal for this formula—approximately 5% of participants reported mild, transient reactions to temperature stimuli. Fifty-seven percent of respondents reported fresher breath and reduced plaque buildup after sleep. Group D (pH=7.2): 90% of participants reported comfortable use; even those with increased hyperesthesia reported virtually no sensitivity episodes. The whitening effect was less pronounced (0.6-1 shade), but participants noted shine and a smoother enamel surface that lasted throughout the day. Nineteen percent of respondents reported fresher breath and reduced plaque buildup after sleep. The D2 pH=7.2 group experienced virtually no hypersensitivity. Increased calcium hydroxyapatite administration virtually eliminated tooth sensitivity. The whitening effect in a slightly alkaline environment decreased, with PAP activity limited to 1-1.5 shades of whitening by the end of testing for nearly 90% of respondents. An additional unexpected observation was a reduction in morning plaque and a lower tendency to absorb food pigments the following day during evening brushing. This can be interpreted as a temporary anti-adhesive effect associated with the modification of the enamel surface by calcium hydroxyapatite. Eighty percent of respondents also noted significant shine and smoothness of their enamel, which can also be attributed to the modification of the tooth surface by calcium hydroxyapatite. Fifty percent of respondents reported fresher breath and reduced plaque buildup after sleep.

[0136] Based on the research conducted, the following conclusions can be drawn:

[0137] In a slightly acidic environment with a pH of 5.8, the maximum whitening capacity of phthalimidoperoxycaproic acid was observed for both formulas, and moderate sensitivity was noted even at a high dosage of phthalimidoperoxycaproic acid (1.1%) in Group A.2. In Group A, we expected a more rapid whitening effect and enamel shine, as well as greater tooth sensitivity during use. In contrast, in Group A, due to the low content of phthalimidoperoxycaproic acid, we expected lower and more stable sensitivity throughout the day. Most likely, this difference is due to the accumulation of a large "depot" of calcium hydroxyapatite on the teeth and its gradual release, which reduced tooth sensitivity but prevented whitening in Group A.2. In the case of group A, the hydroxyapatite “depot” was smaller, which is why a dynamic change in sensitivity was observed during the day, but a faster whitening of the enamel.

[0138] At a medium pH range of 6.2 and 6.6, the most pronounced synergy of phthalimidoperoxycaproic acid and calcium hydroxyapatite is achieved. Effective whitening is combined with the formation of a remineralizing layer, which reduces sensitivity.

[0139] A slightly alkaline pH of 7.2 is characterized by decreased whitening, but increased barrier and remineralizing properties. A surprising decrease in morning plaque and food pigments was observed in the D2 group. This is likely due to a temporary adhesion effect that prevents pigment absorption by the enamel surface.

[0140] The virtually constant percentage of respondents who reported a reduction in morning plaque and fresher breath may indicate the positive effect of coconut oil in synergy with phthalimidoperoxycaproic acid on oral hygiene. Despite the decreased activity of phthalimidoperoxycaproic acid and increased mineralization due to calcium hydroxyapatite with increasing pH, respondents did not report a decrease in morning oral freshness. Even with 0.1% coconut oil, the claimed effects persisted, albeit in a much smaller number of respondents.

[0141] It is also worth noting that during the development of products using a whitening complex of calcium hydroxyapatite, phthalimidoperoxycaproic acid and coconut oil, some effects that were not immediately obvious were also discovered:

[0142] 1. Loss of activity of phthalimidoperoxycaproic acid on the surface of calcium hydroxyapatite

[0143] It was found that, in the same formulation, the method and temperature of adding phthalimidoperoxycaproic acid directly impact the stability of the final product. The authors examined two methods of adding phthalimidoperoxycaproic acid to the product.

[0144] Method #1. Phthalimidoperoxycaproic acid is added at the very end at a temperature of 30-35°C, before pH adjustment and deaeration. With constant stirring (~150-200 rpm), slowly add the prepared 17% phthalimidoperoxycaproic acid suspension in portions. Stir for 15-20 minutes to ensure the suspension is evenly distributed throughout the product. Next, adjust the pH to 6.2-6.6 and place the product in a vacuum chamber to evacuate air. pH adjustments are also performed only with stirring, without homogenization.

[0145] Method #2. Phthalimidoperoxycaproic acid is added before the introduction of the oil phase with active components at T = 45°C. Also, with constant stirring (~150-200 rpm), the prepared 17% suspension of phthalimidoperoxycaproic acid is slowly added in portions. Then, the mass is homogenized at 2000-2500 rpm for 5-7 minutes until a homogeneous white suspension is obtained. Then, the temperature of the mass is reduced to 35-40°C and the introduction of the oil phase with active components is started, as previously described. The pH is adjusted to 6.2-6.6 and the product is placed in a vacuum chamber to evacuate air. pH adjustment is also carried out with homogenization (2000-2500 rpm) for 3-5 minutes.

[0146] After preparation, the samples were packaged in airtight containers and placed in a preheated oven at 40°C. After two weeks, a preliminary inspection of the preheated samples was conducted. These samples were compared with a freshly prepared sample and the same sample stored under normal conditions for two weeks. It turned out that the sample prepared using method #1 did not change its appearance or odor, and the pH remained within the range of 6.2-6.6. The sample prepared using method #2 differed significantly in appearance from the reference samples. The paste increased in volume, which led to slight deformation of the container in which it was stored. Significant microbubbles were visible—the product became airy, and the texture was uneven. The pH of the product also shifted to a more acidic range, reaching 4.91. A rancid oil smell also developed, while the reference samples had a fruity aroma with menthol notes.

[0147] The next checks were carried out at 4, 8, and 12 weeks of storage at 40°C. The results were comparable to those observed after the first check at 2 weeks.

[0148] Similar effects were also observed in pastes #1 and #2, prepared using method #2, but to a lesser degree. The pH of paste #1 shifted to 5.72, while that of paste #2 shifted to 5.43. Microbubbling was also observed for these samples: weakly for paste #1 and more pronounced for paste #2. It's worth noting that no change in odor was observed for paste #1, while paste #2 only experienced a decrease in aroma intensity.

[0149] Such effects can most likely be explained by the interaction of the alkaline centers of calcium hydroxyapatite with phthalimidoperoxycaproic acid, which accelerates its decomposition and conversion to an inactive form. The difference in stability between the pastes prepared using the two different methods can be explained by the increased specific surface area of ​​interaction between the alkaline centers of calcium hydroxyapatite and phthalimidoperoxycaproic acid. During homogenization, this surface area increases, making the interaction more active, leading to the deactivation of phthalimidoperoxycaproic acid. An additional factor accelerating this interaction during homogenization could be the higher temperature (45°C) compared to method 1 (30-35°C).

[0150] Another unobvious effect was the oxidation (rancidity) of coconut oil in the paste containing 1% of this component. A change in odor was noted only in paste #3, produced using method #2. The paste produced using method #1 retained its original aroma even after 12 weeks at 40°C. Phthalimidoperoxycaproic acid, a strong oxidizer, likely initiated lipid peroxidation when interacting with the unsaturated components of coconut oil. This led to the formation of secondary oxidation products, accompanied by changes in organoleptic characteristics (atypical odor, rancidity) and a potential decrease in the stability of the entire composition. It should be noted that the coconut oil was added at a temperature no higher than 35°C, which could not have affected its stability.

[0151] The stability and maximum effectiveness of the whitening complex of calcium hydroxyapatite, phthalimidoperoxycaproic acid and coconut oil in the toothpastes given as examples can be ensured under the following conditions:

[0152] optimal pH level=6.2-6.6, which provides gentle whitening and remineralization,

[0153] The correct technology for introducing phthalimidoperoxycaproic acid, which will ensure greater stability of phthalimidoperoxycaproic acid in the finished product throughout the entire shelf life of the paste.

Claims

1. A complex for teeth whitening and remineralization, characterized by the fact that it contains calcium hydroxyapatite, coconut oil and phthalimidoperoxycaproic acid in the following mass ratio of components: [coconut oil]: [phthalimidoperoxycaproic acid]: [calcium hydroxyapatite] = 1: [0.2-11]: [0.5-150].

2. A composition for whitening and remineralizing teeth, characterized in that it contains an acceptable carrier and a complex consisting of calcium hydroxyapatite, coconut oil and phthalimidoperoxycaproic acid in the following mass ratio of components: [coconut oil]: [phthalimidoperoxycaproic acid]: [calcium hydroxyapatite] = 1: [0.2-11]: [0.5-150].

3. The composition according to claim 2, characterized in that the acceptable carrier contains a solvent, a humectant, a sweetener, a thickener, an abrasive, a preservative, a flavoring agent, a cooling agent, a surfactant, an acidity regulator.

4. The composition according to claim 2, characterized in that the acceptable carrier contains a solvent, a humectant, a sweetener, a thickener, an abrasive, a preservative, a flavoring agent, a cooling agent, a surfactant, an acidity regulator, in the following ratio of components, wt. %: Solvent 20-40 Humidifier 25-55 Sweetener 0,1-0,5 Thickener 0,7-1,2 Abrasive 5-20 Preservative 0,5-1 Flavoring agent 0,1-1,5 Cooling agent 0,1-0,5 Surfactant 0,5-1,5 Acidity regulator (pH) qs pH 6,2-6,6 5. The composition according to paragraph 3 or 4, characterized in that a 10% solution of L-Arginine is used as an acidity regulator.

6. The composition according to paragraph 3 or 4, characterized in that sodium hydroxide or sodium bicarbonate or citric acid or sodium citrate is used as an acidity regulator.

7. The composition according to claim 3, characterized in that it is a toothpaste.

8. The composition according to claim 3, characterized in that it is a gel.

9. The composition according to claim 3, characterized in that it is an impregnation for teeth whitening strips.

10. A toothpaste characterized in that it contains a composition for whitening and remineralizing teeth, including calcium hydroxyapatite, coconut oil and phthalimidoperoxycaproic acid and a carrier including purified water as a solvent, glycerin and a 70% sorbitol solution as humectants, sodium saccharinate as a sweetener, carboxymethylcellulose as a thickener, hydrated silicon dioxide as an abrasive, phenoxyethanol and ethylhexylglycerin as a preservative, a flavoring agent, natural crystalline menthol as a cooling agent, sodium cocosulfate as a surfactant for foam formation, and a 10% L-Arginine solution as an acidity regulator, in the following ratio of components, wt. %: Calcium hydroxyapatite 0,5-15 Phthalimidoperoxycaproic acid 0,2 - 1,1 Coconut oil 0,1-1 Purified water Up to 100 Glycerol 5-15 Sorbitol 70% solution 20-40 Sodium saccharinate 0,1-0,5 Carboxymethylcellulose 0,7-1,2 Hydrated silicon dioxide 5-20 Preservative (phenoxyethanol and ethylhexylglycerin) 0,5-1 Flavoring agent 0,1-1,5 Natural crystalline menthol 0,1-0,5 Sodium cocosulfate 0,5-1,5 L-Arginine (10% solution) qs pH=6.2-6.6 11. A teeth whitening gel characterized in that it contains a composition for whitening and remineralizing teeth, including calcium hydroxyapatite, coconut oil and phthalimidoperoxycaproic acid and a carrier including purified water as a solvent, glycerin as a humectant, sodium saccharinate as a sweetener, polyvinylpyrrolidone as a thickener and adhesive, carboxymethylcellulose as a thickener, phenoxyethanol and ethylhexylglycerin as a preservative, a flavoring agent, natural crystalline menthol as a cooling agent, hydrogenated castor oil as a surfactant-solubilizer, and a 10% solution of L-Arginine as an acidity regulator, in the following ratio of components, wt. %: Calcium hydroxyapatite 0,5-15 Phthalimidoperoxycaproic acid 0,2 -1,1 Coconut oil 0,1-1 Purified water Up to 100 Glycerol 5-10 Sodium saccharinate 0,1-0,5 Polyvinylpyrrolidone 3-9 Carboxymethylcellulose 0,5-1,5 Preservative (phenoxyethanol and ethylhexylglycerin) 0,5-1 Flavoring agent 0,1-1 Natural crystalline menthol 0,05-0,3 PEG-40 hydrogenated castor oil 0,5-1,5 L-Arginine (10% solution) qs pH=6.2-6.6 12. An impregnation for teeth whitening strips, characterized in that it contains a composition for whitening and remineralizing teeth, including calcium hydroxyapatite, coconut oil and phthalimidoperoxycaproic acid and a carrier including purified water as a solvent, glycerin as a humectant, potassium citrate as a desensitizing agent, sodium saccharinate as a sweetener, polyvinylpyrrolidone as a thickener and adhesive, phenoxyethanol and ethylhexylglycerin as a preservative, a flavoring agent, natural crystalline menthol as a cooling agent, hydrogenated castor oil as a surfactant-solubilizer, and a 10% solution of L-Arginine as an acidity regulator, in the following ratio of components, wt. %: Calcium hydroxyapatite 0,5-15 Phthalimidoperoxycaproic acid 0,2 - 1,1 Coconut oil 0,1-1 Purified water up to 100 Potassium citrate 1-5 Glycerol 10-20 Sodium saccharinate 0,1-0,5 Polyvinylpyrrolidone 1-4 Preservative (phenoxyethanol and ethylhexylglycerol) 0,5-1 Flavoring 0,1-1 Menthol Crystalline Natural 0,05-0,3 PEG-40 hydrogenated castor oil 0,5-1,5 L-Arginine (10% solution) qs pH=6.2-6.6 13. A method for producing a composition for whitening and remineralizing teeth, which consists in first preparing a water-glycerin gel base including purified water, sodium saccharinate as a sweetener, glycerin as a humectant, potassium citrate as a desensitizing agent, polyvinylpyrrolidone and / or carboxymethylcellulose as a thickener and homogenizing until a homogeneous structure of the mixture is obtained and calcium hydroxyapatite is introduced into the resulting mixture, then an oil phase is prepared with coconut oil and substances selected from the group consisting of sodium coco-sulfate as a surfactant, hydrogenated castor oil as a solubilizer, phenoxyethanol and ethylhexylglycerin as a preservative, a flavoring agent, natural crystalline menthol as a cooling agent,and a 17% suspension of phthalimidoperoxycaproic acid is introduced into this phase at T = 30-35°C, followed by stirring until the suspension of phthalimidoperoxycaproic acid is completely distributed in the phase, after which the oil phase is introduced into the mixture of the water-glycerin base, the pH is controlled and the acidity level is adjusted to pH values ​​of 6.2-6.6, after which the finished composition is placed for deaeration in a vacuum chamber to pump out air.

14. The method according to claim 13, characterized in that hydrated silicon dioxide is introduced into the water-glycerin gel base as an abrasive before introducing calcium hydroxyapatite.

15. The method according to claim 13, characterized in that the acidity regulator is selected from the group including L-Arginine, sodium hydroxide, sodium bicarbonate, citric acid, sodium citrate.