A stable whitening oral composition based on biocatalytic potentiation by enzymes

Abstract

The application discloses a stable whitening oral composition based on bio-enzyme catalysis, and belongs to the technical field of oral care products. The stable whitening oral composition based on bio-enzyme catalysis is characterized in that the components in the formula mainly include a humectant, a polyethylene glycol, a peroxide, an abrasive, an acyl donor, a carboxyl esterase, a sweetener, a fragrance, an anionic surfactant, a fluoride, a compound emulsifier, a thickening agent, a phosphate and an amphoteric surfactant. The compound emulsifier is composed of sucrose palmitate and sucrose stearate. The paste of the composition has high centrifugal stability, high and low temperature storage stability and excellent extrusion performance. The carboxyl esterase has high catalytic activity, and can realize high-efficiency whitening effect under the condition of low-concentration hydrogen peroxide.

Description

Technical Field

[0001] This invention relates to a stable oral whitening composition based on bio-enzyme catalysis enhancement, belonging to the field of oral care product technology. Background Technology

[0002] Tooth stains can severely affect the appearance of teeth. Among them, extrinsic stains, influenced by daily factors such as diet and lifestyle habits, are the most common type of tooth stains in clinical practice. These stains are mainly formed by the deposition of various pigments on the acquired ligament of the tooth surface, negatively impacting consumers' oral aesthetics and social confidence. Therefore, teeth whitening has become one of the mainstream oral care needs today.

[0003] Currently, the whitening mechanisms of oral care compositions are mainly divided into three types: physical friction, chemical complexation, and oxidative whitening. Among them, oxidative whitening has become the mainstream development direction of teeth whitening technology due to its significant whitening effect and high efficiency; and peroxide, as the core active ingredient in the oxidative whitening system, is widely used in various whitening oral care products.

[0004] Hydrogen peroxide, a typical peroxide whitening ingredient, possesses excellent oxidative decomposition capabilities, effectively breaking down pigment deposits on the tooth surface and acquired lamina, thus achieving a teeth whitening effect. However, hydrogen peroxide itself has an inherent defect of high reactivity, causing it to easily decompose into oxygen and water during product storage. This not only poses safety hazards such as expansion or even explosion of product packaging containers but also reduces the content of effective whitening ingredients in the product, thereby affecting the final whitening effect. Furthermore, high concentrations of hydrogen peroxide can easily trigger acid erosion of tooth hard tissues, dentin hypersensitivity, and adverse reactions such as oral mucosal shedding and burning, seriously affecting the safety of product use. Conversely, reducing the hydrogen peroxide concentration to improve safety makes it difficult to achieve the ideal whitening effect expected by consumers, creating a technical bottleneck where safety and whitening effect are difficult to balance.

[0005] To address the technical problem of insufficient whitening effect of low-concentration hydrogen peroxide, an optimized solution has been proposed in the existing technology. This solution involves combining hydrogen peroxide with an acyl donor and a catalytic enzyme. The catalytic enzyme catalyzes the reaction between the acyl donor and hydrogen peroxide to generate a peracid with a stronger whitening effect. This improves the whitening efficacy of the product while reducing the concentration of hydrogen peroxide and ensuring safety. This technology has already been successfully applied to commercial whitening toothpaste products.

[0006] However, these whitening toothpastes still have many technical defects that limit their market application and consumer experience: the formula system used in commercially available products has poor stability, and the paste is prone to separation and oil separation when stored in a high-temperature environment or under centrifugal conditions; in a low-temperature environment, the paste will harden, making it difficult to squeeze out the product, which seriously affects the product's storage stability and actual ease of use.

[0007] Therefore, developing a low-concentration hydrogen peroxide whitening toothpaste that combines excellent storage stability, ease of use, and efficient whitening effect has become a pressing technical problem to be solved in this field. Summary of the Invention

[0008] To address the shortcomings of existing technologies, the purpose of this invention is to provide a stable oral whitening composition based on bio-enzyme catalysis enhancement. The core whitening component of this stable oral whitening composition based on bio-enzyme catalysis enhancement is a reaction system composed of carboxylesterase, acyl donor, and peroxide. Through the screening of specific emulsifier combinations and ratios, this invention achieves a significant improvement in the centrifugal stability and high and low temperature storage stability of the toothpaste formed by this formulation system. At the same time, this emulsifier system can effectively protect the carboxylesterase, maintain the enzyme's catalytic activity, and ensure the stability and high efficiency of the whitening effect. This solves the problems of poor paste stability, poor low-temperature extrudability, and unstable whitening effect caused by easy enzyme inactivation in existing hydrogen peroxide-enzyme whitening toothpastes.

[0009] To achieve the above objectives, the following technical solution is provided: This invention provides a stable oral whitening composition based on bio-enzyme catalysis enhancement. It consists of a whitening core active ingredient combination composed of carboxylesterase, acyl donor, and peroxide, an anhydrous liquid system, a compound emulsifier system, and conventional oral care excipients. The compound emulsifier system is composed of sucrose palmitate and sucrose stearate.

[0010] In one embodiment, the anhydrous liquid system comprises a humectant and polyethylene glycols.

[0011] In one embodiment, the stable whitening oral composition based on bio-enzyme catalysis has the following components in its formula by mass percentage: 20%~60% moisturizer, 1%~15% polyethylene glycol, 0.1%~10% peroxide, 10%~30% abrasive, 1%~20% acyl donor, 0.01%~0.5% carboxylesterase, 0.05%~5% sweetener, 0.5%~2% fragrance, 1%~5% surfactant, 0.5%~2% fluoride, 1%~8% compound emulsifier, 0.5%~10% thickener, 0.1%~15% phosphate, and 0.5%~5% amphoteric surfactant; wherein the compound emulsifier is a mixture of sucrose palmitate and sucrose stearate.

[0012] In one embodiment, the moisturizer includes one or more of propylene glycol, glycerin, and sorbitol.

[0013] In one embodiment, the stable whitening oral composition based on bio-enzyme catalysis has the following components in its formula by mass percentage: 20%~45% moisturizer, 1%~15% polyethylene glycol, 0.1%~5% peroxide, 10%~30% abrasive, 1%~15% acyl donor, 0.01%~0.5% carboxylesterase, 0.05%~5% sweetener, 0.8%~2% fragrance, 1%~5% surfactant, 0.5%~2% fluoride, 1%~6% compound emulsifier, 2%~10% thickener, 0.1%~10% phosphate, and 0.5%~3% amphoteric surfactant; wherein the compound emulsifier is a mixture of sucrose palmitate and sucrose stearate.

[0014] In one embodiment, the polyethylene glycol includes one or more of PEG-300, PEG-400, PEG-600, and PEG-1000.

[0015] In one embodiment, the peroxide is at least one of hydrogen peroxide or a hydrogen peroxide complex; preferably, it is PVP. H2O2 complex.

[0016] In one embodiment, the friction agent is one or more of calcium pyrophosphate, friction-type silica, and calcium carbonate.

[0017] In one embodiment, the acyl donor is one or more of monoacetyl, diacetyl, triacetyl, monopropionic acid glyceride, dipropionic acid glyceride, tripropionic acid glyceride, monobutyric acid glyceride, dibutylpyridine and tributyric acid glyceride, triacetyl, ethyl acetate, propyl acetate, and amyl acetate.

[0018] In one embodiment, the carboxylesterase is a carboxylesterase having catalytic activity for the hydrolysis of acyl donors.

[0019] In one embodiment, the carboxylesterase is derived from the SGNH family esterase SH2 disclosed in Chinese patent CN120866273A.

[0020] In one embodiment, the sweetener is one or more of sucralose, sodium saccharin, steviol glycosides, and mannitol.

[0021] In one embodiment, the surfactant is one or more of sodium lauryl sulfate, sodium methyl cocoyl taurate, cocamidopropyl betaine, and sodium lauryl sarcosinate.

[0022] In one embodiment, the fluoride is one or more of sodium monofluorophosphate, sodium fluoride, and stannous fluoride.

[0023] In one embodiment, the mass ratio of sucrose palmitate to sucrose stearate in the compound emulsifier is 1:5 to 5:1; preferably 1:3 to 3:1; more preferably 2:2.

[0024] In one embodiment, the thickener is at least one of silica or polyvinylpyrrolidone.

[0025] In one embodiment, the phosphate is one of sodium hexametaphosphate, pentasodium tripolyphosphate, sodium pyrophosphate, sodium phytate, anhydrous tetrasodium pyrophosphate, anhydrous trisodium phosphate, sodium dihydrogen phosphate, disodium hydrogen phosphate, or a combination thereof, as well as the corresponding potassium salt.

[0026] In one embodiment, the amphoteric surfactant is one or more of betaine and cocamidopropyl betaine.

[0027] In one embodiment, the whitening core active ingredient combination is a carboxylesterase + acyl donor + hydrogen peroxide complex, wherein hydrogen peroxide is added in the form of a complex, the carboxylesterase can specifically catalyze the hydrolysis of the acyl donor to generate carboxylic acid, and the carboxylic acid reacts with hydrogen peroxide to generate peracetic acid, thereby enhancing the oxidative whitening effect.

[0028] The present invention also provides a method for preparing the above-described stable whitening oral composition based on bio-enzyme catalysis, wherein the method comprises cutting and mixing the components until a homogeneous composition is obtained to prepare an oral care composition (monophase).

[0029] In one embodiment, the shearing rate is 200~500 rpm / min.

[0030] The present invention also provides the application of the above-mentioned stable oral whitening composition based on bio-enzyme catalysis enhancement in oral care.

[0031] Beneficial effects: The stable oral whitening composition based on bio-enzyme catalysis of the present invention has the following advantages: (1) Significantly improved stability of the paste: The emulsifier system is composed of sucrose fatty acid esters. The paste can maintain a good shape after centrifugation, high temperature and low temperature treatment. There are no problems such as layering, gas release, oil separation and shelling. The paste is soft and easy to squeeze out at low temperature, which overcomes the defects of commercial products and achieves the storage stability of the paste in the whole temperature range. (2) Carboxylesterase activity is effectively protected: The compound emulsifier system has a specific protective effect on carboxylesterase, avoiding the denaturation and inactivation of the enzyme in the formulation system caused by surfactants, alkaline substances and other factors, maintaining the catalytic efficiency of the enzyme for acyl donors, ensuring the conversion rate of hydrogen peroxide to peracetic acid, and thus maintaining the stability of the whitening effect; just like the SGNH family esterase SH2 mentioned in patent CN 120866273 A, although the carboxylesterase has high heat resistance, salt resistance and organic solvent resistance in the reaction system composed of carboxylesterase + acyl donor + peroxide; in the actual toothpaste preparation and application process, some uncontrollable effects will still occur; such as the enzyme activity being limited to a certain extent and the whitening effect not obvious; the compound emulsifier system used in this invention has a significant specific protective effect on the enzyme; (3) Good compatibility of the formula system: The compound emulsifier system has good synergy with the anhydrous liquid system and conventional oral care excipients. The paste is delicate, has a moderate oily feel, and has no irritating odor, which meets the requirements for use of oral care products. At the same time, the formula contains fluoride, which has the effect of preventing cavities, achieving the dual effect of whitening and preventing cavities.

[0032] (4) Wide applicability of the formula: The toothpaste formula of the present invention has a wide range of raw material selection and flexible proportion range. The raw material matching and ratio can be adjusted according to actual production needs and product positioning to adapt to different production processes and market demands, and has good prospects for industrial application. Attached Figure Description

[0033] Figure 1 The images show the actual appearance of the paste samples obtained in the examples and comparative examples after centrifugation. Detailed Implementation

[0034] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention. The specific embodiments described below further illustrate the present invention.

[0035] The source of raw materials involved in this invention: The carboxylesterase was obtained by inducing the expression of SGNH family esterase SH2 from recombinant bacteria of SGNH family esterase SH2 screened from the hot spring environment of Tibet, as disclosed in patent publication number CN 120866273 A, and the pure enzyme system of carboxylesterase was obtained according to the carboxylesterase chromatography purification scheme disclosed in the scheme.

[0036] Colloidal fumed silica was purchased from Evonik Specialty Chemicals (Shanghai) Co., Ltd., Aerosil 200 Pharm. PVP The H2O2 compound was purchased from Ashland (China) Investment Co., Ltd., peroxydoneTMxl-10 complx.

[0037] The testing method involved in this invention: 1. Centrifugal stability test Place the pastes from each embodiment and comparative example into centrifuge tubes, centrifuge at 3000 rpm for 30 min, observe whether the pastes separate into layers, and record the results.

[0038] 2. High-temperature stability test The paste was poured into toothpaste tubes, sealed, and placed in a 50°C constant temperature oven for one week. The appearance of the paste was observed to see if it was uniform, whether there was any gas release, oil separation, or shelling. The extrudability was also tested.

[0039] 3. Low-temperature extrudability test The paste was poured into toothpaste tubes, sealed, and placed in a -5°C refrigerator for one week. After removal, the difficulty of extruding the paste was tested at room temperature and rated as "easy to extrude, slightly difficult to extrude, and difficult to extrude".

[0040] 4. Whitening effect test Hydroxyapatite (HAP) sheets were used to simulate the tooth surface. Various pastes were applied to the surface of the HAP sheets and left to stand for the same amount of time. The initial L0 value and the L1 value after treatment of the HAP sheets were tested with a colorimeter, and the ΔL value (ΔL=L1-L0) was calculated. The larger the ΔL value, the better the whitening effect.

[0041] 5. Detection of carboxylesterase activity The compound paste was incubated at 50℃ for 3 days, and enzyme activity was measured. Approximately 3g of each sample was weighed into 50mL centrifuge tubes, and 10g of pure water was added to each tube. The mixture was thoroughly mixed, centrifuged at 7500 rpm for 30 min, and the supernatant was transferred to a sterile petri dish and lyophilized for 30 h. 2g of ultrapure water was used to dissolve the lyophilized powder to obtain a concentrated solution. An appropriate amount of the concentrated solution was placed in a 1.5mL EP tube, and the activity test components (500μL PBS and 175μL sterile water) were added and thoroughly dissolved. 48μL of triacetin and 227μL of hydrogen peroxide solution were added, and the reaction was allowed to proceed for 2 min. The reaction system was diluted to 10mL (10-fold dilution) with sterile water, and the peracetic acid content was determined using test strips (sensitivity 0-40mg / L). One enzyme activity unit (U) is defined as the amount of enzyme required to decompose the substrate triacetin to produce 1µL of peracetic acid per minute under the test conditions.

[0042] Example 1 A stable oral whitening composition based on bio-enzyme catalysis enhancement, comprising the following raw materials in weight percentages: Propylene glycol 31.22%, anhydrous calcium pyrophosphate 25%, PEG-400 10%, triacetin 12%, sucrose palmitate 2%, sucrose stearate 2%, polyvinylpyrrolidone 7%, carboxylesterase 0.2%, trichlorogalactose 0.15%, sodium lauryl sulfate 1.5%, sodium methyl cocoyl taurate 0.5%, fragrance 1%, colloidal fumed silica 2%, PVP H2O2 complex (hydrogen peroxide content 20.0 wt.%) 1.67%, PEG 1000% is 1%, sodium monofluorophosphate is 0.76%, and anhydrous tetrasodium pyrophosphate is 2%; Its preparation method is as follows: Mix the above ingredients (by weight percentage) at a moderate shear rate of 200 rpm / min until a homogeneous composition is obtained, thus obtaining the paste.

[0043] Example 2 The only difference from Example 1 is that the mass ratio of the compound emulsifier sucrose palmitate to sucrose stearate is adjusted to 1:3, while all other parameters and conditions are the same as in Example 1.

[0044] Example 3 The only difference from Example 1 is that the mass ratio of the compound emulsifier sucrose palmitate to sucrose stearate is adjusted to 3:1, while all other parameters and conditions are the same as in Example 1.

[0045] Comparative Example 1 The only difference from Example 1 is that the mass ratio of the compound emulsifier sucrose palmitate to sucrose stearate is adjusted to 4:0, while all other parameters and conditions are the same as in Example 1.

[0046] Comparative Example 2 The only difference from Example 1 is that the mass ratio of the compound emulsifier sucrose palmitate to sucrose stearate is adjusted to 0:4, while all other parameters and conditions are the same as in Example 1.

[0047] Comparative Example 3 The only difference from Example 1 is that the compound emulsifiers sucrose palmitate and sucrose stearate are replaced with Tween-80: polyglycerol-10 stearate = 2:2. All other parameters and conditions are the same as in Example 1.

[0048] Results Analysis The compositions obtained in the examples and comparative examples were subjected to performance tests, and the results are shown in Tables 1 and 2: Table 1. Performance Results

[0049] Table 2. Enzyme activity of each sample

[0050] As shown in Tables 1 and 2, the stable oral whitening composition based on bio-enzyme catalysis of this invention exhibits the best performance in centrifugal stability, high-temperature stability, low-temperature extrusion performance, and whitening effect during preparation using a compound emulsifier system of sucrose palmitate and sucrose stearate, with a ΔL value of 6.52. This indicates that the compound emulsifier system can achieve a synergistic improvement in stability and whitening effect, significantly outperforming single-component systems and other compound emulsifier types. For example, Comparative Example 3, which also uses other emulsifier systems with similar HLB values, produces a paste with comparable stability to this invention, but the difference in whitening effect is significant. This result indirectly demonstrates that the compound emulsifier system of this invention not only stabilizes the paste but also effectively protects carboxylesterase, allowing it to better exert its whitening effect. In contrast, other emulsifier systems with similar HLB values ​​cannot protect carboxylesterase, resulting in extremely poor whitening effects.

[0051] Further testing of the enzyme activity of the ointments prepared in Examples 1-3 and Comparative Example 3 at 50°C for 3 days showed that the enzyme activity of Examples 1-3 was significantly better than that of Comparative Example 3. This indicates that the emulsifier compound system of the present invention can effectively protect carboxylesterase in the formulation composition, thereby enabling it to better exert its whitening effect.

[0052] The embodiments provided above are not intended to limit the scope of the invention, nor are the described steps intended to limit the order of execution. Any obvious modifications made to the invention by those skilled in the art based on existing common knowledge also fall within the scope of protection defined by the claims.

Claims

1. A stable oral whitening composition based on bio-enzyme catalysis enhancement, characterized in that, It consists of a whitening core active ingredient combination composed of carboxylesterase, acyl donor, and peroxide, an anhydrous liquid system, a compound emulsifier system, and conventional oral care excipients. The compound emulsifier system is composed of sucrose palmitate and sucrose stearate; the mass ratio of sucrose palmitate to sucrose stearate is 1:3 to 3:

1.

2. The oral whitening composition according to claim 1, characterized in that, The anhydrous liquid system consists of humectants and polyethylene glycols.

3. The oral whitening composition according to claim 1 or 2, characterized in that, The components in its formula, by mass percentage, are as follows: humectant 20%~60%, polyethylene glycol 1%~15%, peroxide 0.1%~10%, abrasive 10%~30%, acyl donor 1%~20%, carboxylesterase 0.01%~0.5%, sweetener 0.05%~5%, flavor 0.5%~2%, surfactant 1%~5%, fluoride 0.5%~2%, compound emulsifier 1%~8%, thickener 0.5%~10%, phosphate 0.1%~15%, and amphoteric surfactant 0.5%~5%; among which, the compound emulsifier is a mixture of sucrose palmitate and sucrose stearate.

4. The oral whitening composition according to claim 3, characterized in that, The moisturizer includes one or more of propylene glycol, glycerin, and sorbitol.

5. The oral whitening composition according to claim 3, characterized in that, The friction agent is one or more of calcium pyrophosphate, friction-type silica, and calcium carbonate.

6. The oral whitening composition according to claim 3, characterized in that, The carboxylesterase is the SGNH family esterase SH2.

7. The oral whitening composition according to claim 3, characterized in that, The sweetener is one or more of sucralose, sodium saccharin, steviol glycosides, and mannitol.

8. A method for preparing the oral whitening composition according to any one of claims 1 to 7, characterized in that, The method involves cutting and mixing the components until a homogeneous composition is obtained.

9. The use of the oral whitening composition according to any one of claims 1 to 7 in the preparation of oral care products.

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