Composition containing phthaloyl imino peroxyhexanoic acid and application of composition in preparation of tooth whitening product

Abstract

The invention provides a composition containing phthalimide peroxyhexanoic acid. The composition is prepared from the following components: 3 to 10 parts of a whitening agent containing phthalimide peroxyhexanoic acid, 2 to 8 parts of a modified pineapple extract, 0.1 to 0.6 part of a stabilizer, 2 to 8 parts of a surfactant, 2 to 8 parts of a thickening agent, 30 to 45 parts of a humectant, 2 to 5 parts of a modified bacteriostatic agent, 0.1 to 0.7 part of a pH (Potential of Hydrogen) regulator and 20 to 40 parts of water. The whitening effect and the antibacterial property of the composition are obviously improved under the action of the whitening agent containing phthalimide peroxyhexanoic acid, the modified pineapple extract, the modified bacteriostatic agent and the like.

Description

Technical Field

[0001] The invention belongs to the technical field of tooth whitening product preparation, and specifically relates to a composition containing phthalimidoperoxycaproic acid and an application thereof in the preparation of a tooth whitening product. Background Art

[0002] As people's living standards continue to improve, modern people pay more and more attention to the love, protection and beauty of their teeth. The requirements for teeth beauty and whitening are increasing day by day, and the requirements for the methods and effects of teeth beauty and whitening are getting higher and higher. It is required that the teeth should not be damaged during the teeth beauty and whitening process, and it should not cause soreness and irritation to the oral cavity, gums and teeth, which makes the methods and products of teeth whitening face deeper issues.

[0003] At present, the methods and products of teeth whitening and bleaching can be roughly divided into two categories. One is the method of using mechanical or ultrasonic teeth cleaning. The disadvantages of this method are that it only cleans the teeth, but cannot achieve the effect of discoloring and whitening tooth stains. It has certain damage to the tooth texture and must be performed by professionals in hospitals or dental clinics. It takes time and is not convenient. In addition, tooth stains are generated frequently and continuously. It is impossible to achieve the purpose of regular teeth whitening through several or limited cleanings. In addition, mechanical teeth whitening will make the tooth enamel thinner and cause damage to the tooth texture. The most important thing is to operate at a fixed point, and teeth care cannot be performed anytime and anywhere.

[0004] CN01806704.2 discloses a dry-type patch for teeth whitening, comprising a matrix-type adhesive layer and a backing layer, wherein the adhesive layer comprises a peroxide as a teeth whitening agent, a stabilizer for the peroxide and a hydrophilic glassy polymer as a base polymer, and the adhesive layer generates a strong adhesive force on the teeth when hydrated on the enamel layer, and releases the teeth whitening agent at the same time. However, there are still the disadvantages of the existing commercial tooth paste containing hydrogen peroxide. During storage, hydrogen peroxide degradation is prone to occur, and visible bubbles appear in the tooth paste film, which reduces the content of active ingredients and thus reduces the whitening effect. Summary of the invention

[0005] The purpose of the present invention is to provide a composition containing phthalimidoperoxycaproic acid and an application thereof in the preparation of a tooth whitening product. Under the action of a whitening agent containing phthalimidoperoxycaproic acid, a modified pineapple extract, a modified antibacterial agent, etc., the whitening effect and antibacterial performance of the composition are significantly improved.

[0006] In order to achieve the above object, the present invention provides the following technical solutions: A composition containing phthalimidoperoxycaproic acid comprises the following components in parts by weight: 3-10 parts of a whitening agent containing phthalimidoperoxycaproic acid, 2-8 parts of a modified pineapple extract, 0.1-0.6 parts of a stabilizer, 2-8 parts of a surfactant, 2-8 parts of a thickener, 30-45 parts of a moisturizer, 2-5 parts of a modified antibacterial agent, 0.1-0.7 parts of a pH regulator and 20-40 parts of water.

[0007] Preferably, 5-7 parts of a whitening agent containing phthalimidoperoxycaproic acid, 4-6 parts of a modified pineapple extract, 0.3-0.4 parts of a stabilizer, 4-5 parts of a surfactant, 3-5 parts of a thickener, 40-43 parts of a moisturizer, 3-4 parts of a modified antibacterial agent, 0.4-0.5 parts of a pH adjuster and 25-35 parts of water.

[0008] The preparation method of the composition containing phthalimido peroxycaproic acid comprises the following steps: S1: preparing a whitening agent containing phthalimidoperoxycaproic acid; S2: preparing modified pineapple extract; S3: preparing modified antibacterial agent; S4: first, by weight, 3-10 parts of a whitening agent containing phthalimidoperoxycaproic acid and 2-8 parts of a modified pineapple extract are stirred at a temperature of 40-60° C. for 30-50 minutes; then, 0.1-0.6 parts of a stabilizer, 2-8 parts of a surfactant and 2-8 parts of a thickener are added, and stirred at a temperature of 70-90° C. for 25-45 minutes; S5: adding 30-45 parts of moisturizing agent, 2-5 parts of modified antibacterial agent, 0.1-0.7 parts of pH adjusting agent and 20-40 parts of water to step S4, and treating with double-frequency ultrasonic alternating oscillation to obtain the composition containing phthalimidoperoxycaproic acid.

[0009] Preferably, step S1 is specifically as follows: in parts by weight, 0.3-0.6 parts of a 10% copper nitrate aqueous solution, 0.2-0.5 parts of a 15% silver nitrate aqueous solution, 0.3-0.6 parts of titanium dioxide nanoparticles, 2-5 parts of phthalimido peroxycaproic acid and 1-3 parts of sodium formaldehyde sulfoxylate are taken, and ultrasonically treated at a temperature of 40-60°C for 15-25min, and then the temperature is increased to 100-120°C, and the reaction is stirred for 1-3h to obtain a whitening agent containing phthalimido peroxycaproic acid.

[0010] Preferably, step S2 is specifically as follows: by weight, 0.5-2 parts of strawberry puree, 1-3 parts of banana peel puree, 1-4 parts of orange peel puree, 3-6 parts of pineapple extract, 2-5 parts of polydopamine and 20-40 parts of water are mixed, and stirred at a temperature of 60-80° C. for 1-3 hours to obtain a modified pineapple extract.

[0011] Preferably, the preparation process of the pineapple extract is: Preferably, step S3 is specifically as follows: by weight, 15-25 parts of hydroxy-porous carbon, 5-9 parts of povidone iodine, 1-3 parts of sodium carboxymethyl starch and 1-3 parts of nano zinc oxide are taken, and stirred at a temperature of 100-120° C. for a reaction of 1.5-2.5 hours to obtain a modified antibacterial agent.

[0012] Preferably, in step S4, the stabilizer is one or a mixture of disodium ethylenediaminetetraacetate and sodium hexametaphosphate; the surfactant is one or a mixture of sodium fatty alcohol polyoxyethylene ether carboxylate or polyoxyethylene polyoxypropylene alkylphenol ether carboxylate; and the thickener is a mixture of carbomer and hydroxyethyl cellulose, and the mass ratio of the two is 1:1.3-1.6.

[0013] Preferably, the moisturizing agent is one or a mixture of polyethylene glycol or butylene glycol; the regulating agent is a sodium hydroxide aqueous solution with a mass fraction of 25-35%.

[0014] Preferably, in step S5, the dual-frequency ultrasonic alternating frequency is 50-80KHz, the dual-frequency ultrasonic alternating working time is 5-8s, and the ultrasonic power is 200-250W.

[0015] The composition containing phthalimidoperoxycaproic acid obtained by any one of the above methods and its application in preparing tooth whitening products.

[0016] Compared with the prior art, the advantages and beneficial effects of the present invention are: The present invention co-dopes titanium dioxide with copper and silver to form highly oxidizing electron holes under visible light irradiation, and can also synergistically catalyze and decompose phthalimidoperoxycaproic acid and the like to produce ·OH. Both the electron holes and ·OH can quickly oxidize pigments and dirt on the surface of teeth, thereby improving the whitening effect of the whitening gel on teeth. By introducing modified pineapple extract, the increment, whitening, antibacterial and other effects of natural ingredients are brought into play. The hydroxy-porous carbon is fully utilized because there are many pores distributed on the hydroxy-porous carbon, and the inner wall of the pore is modified with hydroxyl groups. The ketone groups in povidone iodine can condense with the hydroxyl groups on the hydroxy-porous carbon, so that the povidone iodine is firmly connected to the inside of the pores of the hydroxy-porous carbon. At the same time, sodium carboxymethyl starch and nano zinc oxide can fill the remaining pores and are slowly released, thereby further improving the antibacterial and whitening effect. Through the synergistic effect between the components of the present invention, the whitening performance is significantly improved, thereby achieving the effect of whitening teeth. DETAILED DESCRIPTION

[0017] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0018] The sources of raw materials used in the present invention are as follows: Phthalic acid imidoperoxycaproic acid was obtained from Hubei Xinkang Pharmaceutical Chemical Co., Ltd. with item number XK6391; sodium formaldehyde sulfoxylate was obtained from Shanghai Yuanye Biotechnology Co., Ltd. with item number S42924; polydopamine was obtained from Xi'an Qiyue Biotechnology Co., Ltd. with item number 5651; hydroxy-porous carbon was obtained from Xi'an Qiyue Biotechnology Co., Ltd. with item number 5325; povidone iodine was obtained from Hangzhou Hengquan Technology Development Co., Ltd. with item number 54; sodium carboxymethyl starch was obtained from Shanghai Yuanye Biotechnology Co., Ltd. with item number S30572; sodium fatty alcohol polyoxyethylene ether carboxylate was obtained from Wuhan Jiye Shenggong Chemical Co., Ltd. with item number 531; carbomer was obtained from Shanghai Yuanye Biotechnology Co., Ltd. with item number S31102; and hydroxyethyl cellulose was obtained from Shanghai Yuanye Biotechnology Co., Ltd. with item number S14167.

[0019] Example 1 This embodiment provides a method for preparing a composition containing phthalimidoperoxycaproic acid, comprising the following steps: S1: Take 0.3g of 10% copper nitrate aqueous solution, 0.2g of 15% silver nitrate aqueous solution, 0.3g of titanium dioxide nanoparticles, 2g of phthalimido peroxycaproic acid and 1g of sodium formaldehyde sulfoxylate, and treat them ultrasonically at 40°C and 500W for 15min, then raise the temperature to 100°C, stir and react at a rate of 500r / min for 1h to obtain a whitening agent containing phthalimido peroxycaproic acid; S2: Cut the pineapple into dices, add aqueous solution thereto at a solid-liquid ratio of 1g:15ml, and extract at a temperature of 80°C for 45min to obtain a pineapple extract; mix 0.5g of strawberry puree, 1g of banana peel puree, 1g of orange peel puree, 3g of pineapple extract, 2g of polydopamine and 20g of water, and stir the mixture at a temperature of 60°C and a speed of 400r / min for 1h to obtain a modified pineapple extract; S3: Take 15g of hydroxy-porous carbon with a pore diameter of 100-300nm, 5g of povidone iodine, 1g of sodium carboxymethyl starch and 1g of nano zinc oxide, stir and react at a temperature of 100°C and a speed of 400r / min for 1.5h to obtain a modified antibacterial agent; S4: First, 3g of a whitening agent containing phthalimidoperoxycaproic acid and 2g of a modified pineapple extract were stirred at a temperature of 40°C at a rate of 600r / min for 30min; then, 0.1g of disodium ethylenediaminetetraacetate, 2g of sodium fatty alcohol polyoxyethylene ether carboxylate and 2g of a mixture of carbomer and hydroxyethyl cellulose (the mass ratio of the two was 1:1.3) were added, and stirred at a temperature of 70°C at a rate of 500r / min for 25min; S5: Add 30g of polyethylene glycol, 2g of modified antibacterial agent, 0.1g of 25% sodium hydroxide aqueous solution and 20g of water to step S4, and use dual-frequency ultrasonic alternating oscillation for 10min, control the frequency to 50KHz, the alternating working time to 5s, and the power to 200W to obtain the composition containing phthalimidoperoxycaproic acid.

[0020] Example 2 This embodiment provides a method for preparing a composition containing phthalimidoperoxycaproic acid, comprising the following steps: S1: Take 0.6g of 10% copper nitrate aqueous solution, 0.5g of 15% silver nitrate aqueous solution, 0.6g of titanium dioxide nanoparticles, 5g of phthalimido peroxycaproic acid and 3g of sodium formaldehyde sulfoxylate, and treat them ultrasonically at 60°C and 400W for 25min, then raise the temperature to 120°C, stir and react at a rate of 400r / min for 3h, and obtain a whitening agent containing phthalimido peroxycaproic acid; S2: Cut the pineapple into dices, add aqueous solution thereto at a solid-liquid ratio of 1g:15ml, and extract at a temperature of 80°C for 45min to obtain a pineapple extract; mix 2g of strawberry puree, 3g of banana peel puree, 4g of orange peel puree, 6g of pineapple extract, 5g of polydopamine and 40g of water, and stir the mixture at a temperature of 80°C at a rate of 300r / min for 3h to obtain a modified pineapple extract; S3: Take 25g of hydroxy-porous carbon with a pore diameter of 200-300mn, 9g of povidone iodine, 3g of sodium carboxymethyl starch and 3g of nano zinc oxide, stir and react at a temperature of 120°C and a speed of 500r / min for 2.5h to obtain a modified antibacterial agent; S4: First, 10g of a whitening agent containing phthalimidoperoxycaproic acid and 8g of a modified pineapple extract were stirred at 60°C for 50min at a rate of 350r / min; then, 0.6g of disodium ethylenediaminetetraacetate, 8g of sodium fatty alcohol polyoxyethylene ether carboxylate and 8g of a mixture of carbomer and hydroxyethyl cellulose (the mass ratio of the two was 1:1.6) were added, and stirred at 90°C for 45min at a rate of 500r / min; S5: Add 45g of polyethylene glycol, 5g of modified antibacterial agent, 0.7g of 35% sodium hydroxide aqueous solution and 40g of water to step S4, and use dual-frequency ultrasonic alternating oscillation for 15min, control the frequency to 80KHz, the alternating working time to 8s, and the power to 250W to obtain the composition containing phthalimidoperoxycaproic acid.

[0021] Example 3 This embodiment provides a method for preparing a composition containing phthalimidoperoxycaproic acid, comprising the following steps: S1: Take 0.5g of 10% copper nitrate aqueous solution, 0.3g of 15% silver nitrate aqueous solution, 0.4g of titanium dioxide nanoparticles, 3g of phthalimido peroxycaproic acid and 2g of sodium formaldehyde sulfoxylate, and treat them with ultrasound at 60°C and 600W for 20min, then raise the temperature to 110°C, stir and react at a rate of 450r / min for 2.5h to obtain a whitening agent containing phthalimido peroxycaproic acid; S2: Cut the pineapple into dices, add an aqueous solution thereto at a solid-liquid ratio of 1g:15ml, and extract at a temperature of 80°C for 45min to obtain a pineapple extract; mix 1.5g of strawberry puree, 2.5g of banana peel puree, 3g of orange peel puree, 4.5g of pineapple extract, 3.5g of polydopamine and 35g of water, and stir the mixture at a temperature of 75°C at a rate of 450r / min for 1.5h to obtain a modified pineapple extract; S3: Take 20g of hydroxy-porous carbon with a pore diameter of 150-350nm, 7g of povidone iodine, 2g of sodium carboxymethyl starch and 2g of nano zinc oxide, stir and react at a temperature of 110°C and a speed of 600r / min for 2h to obtain a modified antibacterial agent; S4: First, 7g of a whitening agent containing phthalimidoperoxycaproic acid and 6g of a modified pineapple extract were stirred at a temperature of 55°C at a rate of 600r / min for 45min; then, 0.4g of disodium ethylenediaminetetraacetate, 6g of sodium fatty alcohol polyoxyethylene ether carboxylate and 5g of a mixture of carbomer and hydroxyethyl cellulose (the mass ratio of the two was 1:1.5) were added, and stirred at a temperature of 85°C at a rate of 450r / min for 40min; S5: Add 40g of polyethylene glycol, 3.5g of modified antibacterial agent, 0.5g of 32% by mass sodium hydroxide aqueous solution and 35g of water to step S4, and use dual-frequency ultrasonic alternating oscillation for 16min, control the frequency to 65KHz, the alternating working time to 6s, and the power to 230W to obtain the composition containing phthalimidoperoxycaproic acid.

[0022] Comparative Example 1 The difference between this comparative example and Example 1 is that no copper nitrate aqueous solution or silver nitrate aqueous solution is added in step S1, and the other steps are the same.

[0023] Comparative Example 2 The difference between this comparative example and Example 1 is that titanium dioxide nanoparticles are not added in step S1, and the other steps are the same.

[0024] Comparative Example 3 The difference between this comparative example and Example 1 is that step S2 is omitted, and unmodified pineapple extract is directly used, and the other steps are the same.

[0025] Comparative Example 4 The difference between this comparative example and Example 1 is that hydroxyl-porous carbon is not added in step S3, and the other steps are the same.

[0026] Comparative Example 5 The difference between this comparative example and Example 1 is that sodium carboxymethyl starch is not added in step S3, and the other steps are the same.

[0027] Comparative Example 6 The difference between this comparative example and Example 1 is that in step S5, dual-frequency ultrasonic alternating oscillation treatment is not used, but ordinary mixing is performed.

[0028] The compositions containing phthalimidoperoxycaproic acid prepared in the examples and comparative examples are applied to prepare tooth paste, wherein the tooth paste comprises a matrix layer, a backing layer and a protective layer; the matrix layer is the composition containing phthalimidoperoxycaproic acid.

[0029] Performance Testing: Antibacterial ring test: strains: Streptococcus mutans suspension CNCC32400, Lactobacillus acidophilus suspension ATCC4356, Porphyromonas gingivalis suspension ATCC33277; culture medium: nutrient agar; preparation of antibacterial samples: weigh 1.0 g of antibacterial gel, add 3 mL of deionized water and stir evenly, and use a micropipette on sterile filter paper under sterile conditions. 20 μl was added dropwise and stored in a refrigerator for later use; antibacterial test: using the paper diffusion method, the culture medium was dissolved and poured into a plate, and after cooling and solidification, the above three 0.1 mL bacterial suspensions (concentrations of 5×105 cfu / mL-5×106 cfu / mL) were added respectively, and evenly spread on the agar surface with a sterile glass rod to prepare three bacterial samples; using sterile tweezers, the paper pieces of antibacterial gel prepared in different embodiments and comparative examples were placed on the agar surface, with equal spacing between each paper piece; placed in a 37°C incubator for 24 hours, and the size of the antibacterial ring around the paper piece was measured, and the antibacterial test was repeated 3 times. Adhesive patch whitening effect test. In vitro bovine teeth (enamel) close to human enamel were selected as efficacy test samples. 1% hydrochloric acid, saturated sodium carbonate solution, and 1% phytic acid were used to treat the enamel blocks for 1 minute respectively. The residual liquid was absorbed with filter paper, and then the treated enamel was immersed in the compositions of each embodiment and comparative example. The whiteness value (L) of the stained enamel was measured using an X-Rite spectrophotometer (Ci6x). ), select the whiteness value (L ) in the range of 25-35. The results are shown in Table 1.

[0030] Table 1 Performance test results

[0031] It can be seen from the above performance test results that Examples 1-3 have good antibacterial and whitening properties, and in particular, the comprehensive performance of Example 3 is the most outstanding. However, since Comparative Examples 1-6 do not adopt the necessary technical solutions, their corresponding performance tests are significantly worse than those of the Examples. The above experimental results further prove the importance of the technical solutions defined in the present invention for its technical effects.

[0032] The above is a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principles of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. A composition containing phthalimidoperoxycaproic acid, characterized in that, The invention comprises the following components in parts by weight: 3-10 parts of a whitening agent containing phthalimidoperoxycaproic acid, 2-8 parts of a modified pineapple extract, 0.1-0.6 parts of a stabilizer, 2-8 parts of a surfactant, 2-8 parts of a thickener, 30-45 parts of a moisturizer, 2-5 parts of a modified antibacterial agent, 0.1-0.7 parts of a pH regulator and 20-40 parts of water.

2. A composition containing phthalimidoperoxycaproic acid according to claim 1, characterized in that: 5-7 parts of a whitening agent containing phthalimidoperoxycaproic acid, 4-6 parts of a modified pineapple extract, 0.3-0.4 parts of a stabilizer, 4-5 parts of a surfactant, 3-5 parts of a thickener, 40-43 parts of a moisturizer, 3-4 parts of a modified antibacterial agent, 0.4-0.5 parts of a pH regulator and 25-35 parts of water.

3. A method for preparing a composition containing phthalimidoperoxycaproic acid, characterized in that: The steps include: S1: preparing a whitening agent containing phthalimidoperoxycaproic acid; S2: preparing modified pineapple extract; S3: preparing modified antibacterial agent; S4: first, by weight, 3-10 parts of a whitening agent containing phthalimidoperoxycaproic acid and 2-8 parts of a modified pineapple extract are stirred at a temperature of 40-60° C. for 30-50 minutes; then, 0.1-0.6 parts of a stabilizer, 2-8 parts of a surfactant and 2-8 parts of a thickener are added, and stirred at a temperature of 70-90° C. for 25-45 minutes; S5: adding 30-45 parts of moisturizing agent, 2-5 parts of modified antibacterial agent, 0.1-0.7 parts of pH adjusting agent and 20-40 parts of water to step S4, and treating with double-frequency ultrasonic alternating oscillation to obtain the composition containing phthalimidoperoxycaproic acid.

4. The method for preparing a composition containing phthalimidoperoxycaproic acid according to claim 3, characterized in that: Step S1 is specifically as follows: in parts by weight, 0.3-0.6 parts of a 10% copper nitrate aqueous solution, 0.2-0.5 parts of a 15% silver nitrate aqueous solution, 0.3-0.6 parts of titanium dioxide nanoparticles, 2-5 parts of phthalimido peroxycaproic acid and 1-3 parts of sodium formaldehyde sulfoxylate are taken, and ultrasonic treatment is performed at a temperature of 40-60° C. for 15-25 minutes, and then the temperature is increased to 100-120° C., and the reaction is stirred for 1-3 hours to obtain a whitening agent containing phthalimido peroxycaproic acid.

5. The method for preparing a composition containing phthalimidoperoxycaproic acid according to claim 3, characterized in that: Step S2 is specifically as follows: by weight, 0.5-2 parts of strawberry puree, 1-3 parts of banana peel puree, 1-4 parts of orange peel puree, 3-6 parts of pineapple extract, 2-5 parts of polydopamine and 20-40 parts of water are mixed, and stirred at a temperature of 60-80° C. for 1-3 hours to obtain a modified pineapple extract.

6. The method for preparing a composition containing phthalimidoperoxycaproic acid according to claim 5, characterized in that: The preparation process of the pineapple extract is as follows: The method for preparing a composition containing phthalimidoperoxycaproic acid according to claim 3, characterized in that step S3 is specifically: taking 15-25 parts of hydroxy-porous carbon, 5-9 parts of povidone iodine, 1-3 parts of sodium carboxymethyl starch and 1-3 parts of nano zinc oxide by weight, stirring and reacting at a temperature of 100-120° C. for 1.5-2.5 hours to obtain a modified antibacterial agent.

7. The method for preparing a composition containing phthalimidoperoxycaproic acid according to claim 5, characterized in that: In step S4, the stabilizer is one of disodium ethylenediaminetetraacetate and sodium hexametaphosphate or a mixture thereof; the surfactant is one of sodium fatty alcohol polyoxyethylene ether carboxylate or polyoxyethylene polyoxypropylene alkylphenol ether carboxylate or a mixture thereof; and the thickener is a mixture of carbomer and hydroxyethyl cellulose, and the mass ratio of the two is 1:1.3-1.

6.

8. The method for preparing a composition containing phthalimidoperoxycaproic acid according to claim 5, characterized in that: The moisturizing agent is one of polyethylene glycol and butylene glycol or a mixture thereof; the regulating agent is a sodium hydroxide aqueous solution with a mass fraction of 25-35%.

9. The method for preparing a composition containing phthalimidoperoxycaproic acid according to claim 5, characterized in that: In step S5, the dual-frequency ultrasonic alternating frequency is 50-80KHz, the dual-frequency ultrasonic alternating working time is 5-8s, and the ultrasonic power is 200-250W.

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