Toothpaste and preparation method thereof

Abstract

The invention discloses toothpaste and a preparation method thereof. The toothpaste is prepared from components in percentage by mass as follows: 8%-15% of bamboo salt, 0.03%-0.15% of o-cymene-5-alcohol, 1%-5% of polyglycerol fatty acid ester, 0.5%-3% of calcium salt, 0.05%-0.3% of lysozyme, 0.2%-1% of bromelain, 15%-28% of a friction agent, 0.4%-1.2% of a thickening agent, 0.1%-2% of a pH buffer system, 10%-35% of a humectant, 1.5%-4% of a foaming agent and the balance of water. Glycyrrhizic acid is replaced by polyglycerol ester / calcium ion micelles, so that the problem of IPMP inactivation is thoroughly solved while the pH conflict is avoided.

Description

Technical Field

[0001] The present invention relates to the technical field of oral cleaning products, and in particular to a toothpaste and a preparation method thereof. Background Art

[0002] Since tobacco, tea, coffee, colored foods, etc. in daily life are easily deposited on the surface of teeth, gradually turning teeth yellow or black, forming exogenous stains on teeth, affecting the appearance of teeth, and easily leading to oral problems such as caries and gingivitis, consumers are particularly fond of toothpaste with whitening effect, and the market demand is strong.

[0003] The prior art CN118105324A provides a whitening and antibacterial toothpaste, which is prepared from the following raw materials in percentage by mass: 9-12% bamboo salt, 0.05-0.1% o-cymene-5-ol, 0.1-0.5% enzyme, 1-2% glycyrrhizic acid, 15-25% abrasive silica, 5-10% thickening silica, 0.5-1% thickener, 15-30% moisturizer, 2-3% foaming agent, 0.05-0.1% cooling agent, 0.5-1% flavor, and the balance is water.

[0004] While the strong alkalinity of bamboo salt (pH 10-11) imparts its antibacterial properties, it significantly destroys the molecular structure of o-cymene-5-ol (IPMP). Experiments show that when the pH is greater than 9, the IPMP inhibition rate decreases by 35%-40%. Therefore, glycyrrhizic acid is used to neutralize the alkalinity. However, the acidity of glycyrrhizic acid can cause a burning sensation in the mouth, making it unsuitable for sensitive people. Furthermore, the acidic environment of glycyrrhizic acid inhibits the effectiveness of alkaline active ingredients such as lysozyme, failing to address the problem of thickener degradation caused by the alkalinity of bamboo salt. For example, in Comparative Example 3 of the prior art, when no glycyrrhizic acid was added, the paste began to dehydrate after 6 months and was completely ineffective after 12 months. Even with the addition of glycyrrhizic acid in Comparative Example 4, the acidic environment actually exacerbated the hydrolysis of hydroxyethyl cellulose, resulting in a dehydration rate of over 15% after 24 months.

[0005] Therefore, if the alkalinity of bamboo salt is prioritized, IPMP will be inactivated and the thickener will be degraded. Even if an acidic neutralizer is added, there will be problems of inhibiting the alkaline active ingredients and irritating the mucous membrane. Summary of the Invention

[0006] The present invention aims to provide a toothpaste and a preparation method thereof, which completely solves the problem of IPMP inactivation while avoiding pH conflict by replacing glycyrrhizic acid with polyglycerol ester / calcium ion micelles.

[0007] A toothpaste is composed of the following components in percentage by mass: 8-15% of bamboo salt, 0.03-0.15% of o-cymene-5-ol, 1-5% of polyglycerol fatty acid ester, 0.5-3% of calcium salt, 0.05-0.3% of lysozyme, 0.2-1% of bromelain, 15-28% of abrasive, 0.4-1.2% of thickener, 0.1-2% of pH buffer system, 10-35% of humectant, 1.5-4% of foaming agent, and the balance being water.

[0008] Optimally, the polyglycerol fatty acid ester is polyglycerol-10 laurate or polyglycerol-6 distearate, and the calcium salt is calcium citrate or calcium gluconate.

[0009] Optimized, the pH buffer system consists of trehalose and arginine in a mass ratio of 1:0.5-2, maintaining the pH value of the toothpaste at 8.0-9.2.

[0010] Optimally, the friction agent is a mixture of surface-modified calcium carbonate with a particle size of 5 to 15 μm and spherical silicon dioxide with a particle size of 3 to 8 μm in a mass ratio of 2 to 4:1.

[0011] Preferably, the mass ratio of the lysozyme to bromelain is 1:4-6, and the bromelain activity is ≥2500 U / mg.

[0012] A method for preparing toothpaste comprises the following steps:

[0013] S1. Premix polyglycerol fatty acid ester, o-cymene-5-ol, calcium salt and 30-50% water, and homogenize at 40-50° C. to form micellar inclusions;

[0014] S2. Mix and dissolve bamboo salt, pH buffer system, moisturizer and remaining water, then add abrasive, thickener and foaming agent, and stir under vacuum;

[0015] S3. Add micellar inclusions, lysozyme, and bromelain, and degas for 3 to 8 minutes under a vacuum degree ≥ 0.095 MPa.

[0016] Optimized, the homogenization pressure is 80-120 MPa, circulated 3-5 times; the system temperature is controlled at 25-30 ° C when the enzyme is added

[0017] Working principle and beneficial effects of the present invention:

[0018] Polyglycerol fatty acid esters (such as polyglycerol-10 laurate) are nonionic surfactants. Under homogenization conditions of 40-50°C and 80-120 MPa pressure, they are cycled 3-5 times to form nano-sized micelles, which encapsulate o-cymene-5-ol in the micelle core. The o-cymene-5-ol is stabilized by steric hindrance and charge repulsion, preventing it from being adsorbed by polymer thickeners or inactivated by reaction with the alkaline environment of bamboo salt. This increases the IPMP activity retention rate from 62% in traditional formulas to over 95%. Calcium salts (calcium citrate, calcium gluconate) provide Ca 2+ Enhance the viscosity and stability of the toothpaste system, form a complex with polyglycerol fatty acid esters, strengthen the micelle structure, densify the micelle shell, lock the IPMP molecules in the micelle core, and isolate the bamboo salt OH- attack. 2+ The carboxyl complexation with thickeners (such as sodium carboxymethyl cellulose) improves the viscosity stability of the paste, and calcium-added micelles can extend the water-free life to more than 24 months.

[0019] Trehalose (acidic) and arginine (alkaline) are mixed in a ratio of 1:0.5-2 to form a pH buffer, maintaining the system at 8.0-9.2 (weakly alkaline). This pH not only meets the optimal range for bamboo salt to exert its antibacterial activity (pH>8), but also prevents the inactivation of o-cymene-5-ol at strong alkalinity (pH>9.5). In the existing technology, glycyrrhizic acid needs to be added in excess (≥1.5%) to reduce the pH to below 7, resulting in an acidic system and inhibiting the antibacterial effect of bamboo salt.

[0020] The highly active enzyme bromelain can decompose the polysaccharide-protein complex in tooth stains. Combined with the physical friction of surface-modified calcium carbonate, it forms a dual path of "enzymatic hydrolysis-stripping". Compared with the existing technology of papain that only decomposes protein, the whitening efficiency is improved.

[0021] In summary, by replacing glycyrrhizic acid with polyglycerol ester / calcium ion micelles, the problem of IPMP inactivation can be completely solved while avoiding pH conflict. DETAILED DESCRIPTION

[0022] The following is further described in detail through specific implementation methods:

[0023] Example 1: Composed of the following components in percentage by mass: 12% bamboo salt, 0.1% o-cymene-5-ol, 3% polyglycerol-10 laurate, 1.5% calcium citrate, 0.1% lysozyme, 0.5% bromelain, 24% abrasive (18% modified calcium carbonate, 6% spherical silica), 0.8% xanthan gum, 0.8% trehalose-arginine buffer (1:1), 25% glycerol, 2.5% K12, and the balance is water.

[0024] S1. Premix polyglycerol-10 laurate, o-cymene-5-ol, calcium citrate, and 30% water, and homogenize at 50°C to form micellar inclusions. S2. Dissolve bamboo salt, trehalose-arginine buffer, and glycerol in the remaining water, then add abrasive, xanthan gum, and K12, and stir under vacuum. S3. Add the micellar inclusions, lysozyme, and bromelain, and degas at a vacuum degree of ≥0.095 MPa for 8 minutes.

[0025] Example 2: The polyglyceryl-10 laurate in Example 1 was replaced with polyglyceryl-6 distearate.

[0026] Example 3: The calcium citrate in Example 1 was replaced with calcium gluconate.

[0027] Example 4: Remove the calcium citrate in Example 1.

[0028] Comparative Example: No micelle encapsulation (direct addition of o-cymene-5-ol).

[0029] Prior art control group: a whitening and antibacterial toothpaste was prepared according to CN118105324A.

[0030] Experimental method: The micelle Z-average particle size (n=3) was measured using a Malvern laser particle size analyzer.

[0031] IPMP encapsulation efficiency: Free IPMP was separated by ultrafiltration centrifugation (10 kDa filter membrane);

[0032] HPLC detection: C18 column, mobile phase methanol: water = 80:20, detection wavelength 278 nm Encapsulation efficiency (%) = (1-free IPMP amount / total IPMP amount) × 100;

[0033] Alkaline tolerance test: The micelle dispersion was mixed with bamboo salt solution (final pH = 10.5) and shaken at 37°C for 24 h;

[0034] Determination of IPMP residual activity: Referring to QB / T2738-2012 antibacterial rate test (Streptococcus mutans), the following data in Table 1 were obtained:

[0035] Table 1

[0036] Group Micellar particle size (nm) PDI IPMP encapsulation efficiency (%) IPMP activity retention rate (%) Example 1 68.2±3.1 0.121 98.7±0.5 96.3±1.2 Example 2 72.5±2.8 0.135 97.9±0.7 95.1±1.5 Example 3 75.3±4.2 0.142 97.3±0.9 94.8±1.8 Example 4 285.6±15.7 0.362 63.4±2.3 58.2±3.1 Comparative Example 1 - - 0 42.7±2.5 CN118105324A group - - - 68.7±1.9

[0037] When calcium salt is present (Examples 1-3), the micelle particle size is less than 80 nm and the distribution is uniform (PDI <0.15), while the micelles in the calcium-free group (Example 4) are severely aggregated. Calcium ions increase the IPMP encapsulation efficiency by 55%, and the activity retention rate is more than 40% higher than that of the prior art.

[0038] The samples were stored in a constant temperature box at 45°C and 75% humidity, and were sampled and tested monthly for 6 months (equivalent to 24 months at room temperature). The water separation rate, viscosity retention rate, and pH change were tested, and the data in Table 2 were obtained:

[0039] Table 2

[0040]

[0041]

[0042] Note: The CN118105324A group experienced water loss (2.1%) at 3 months and reached 8.5% at 6 months. The calcium-free group (Example 4) had a water loss rate >17% due to the lack of a calcium ion cross-linked thickener network. The calcium-containing formulas of the present invention (Examples 1-3) showed zero water loss at 6 months, with a viscosity retention rate >92%.

[0043] Antibacterial test method: Refer to QB / T2738-2012 suspension quantitative bacteria: Streptococcus mutans (ATCC35668), Porphyromonas gingivalis (ATCC33277) Results are shown in Table 3:

[0044] Table 3

[0045] Group Inhibition rate of Streptococcus mutans (%) Inhibition rate of Porphyromonas gingivalis (%) Example 1 99.3±0.3 98.7±0.5 Example 2 98.9±0.4 98.1±0.6 Example 3 98.5±0.7 97.8±0.8 Example 4 85.2±1.2 83.7±1.5 CN118105324A group 97.9±0.5 96.4±0.9

[0046] Whitening experiment: Bovine enamel blocks were dyed (soaked in a black tea / coffee / tobacco mixture for 7 days) and subjected to 8,000 simulated toothbrushing cycles using a toothbrush (ISO / TS14569-2). ΔE values were measured using a colorimeter (L*a*b* system). The results are shown in Table 4:

[0047] Table 4

[0048]

[0049]

[0050] The calcium-containing micelle system (Examples 1-3) had an antibacterial rate of >98% against Gram-negative / positive bacteria, significantly higher than the calcium-free group (p<0.01). Whitening effect: Calcium ions stabilized the activity of bromelain, increasing the ΔE value to above 4.0 (a difference of >2 color levels visible to the naked eye).

[0051] In summary, the following conclusions are drawn:

[0052] (1) The calcium-containing groups (Examples 1-3) formed stable micelle structures with a particle size of approximately 70 nm (68.2-75.3 nm) and uniform distribution (PDI < 0.15) through calcium ion crosslinking, and the IPMP encapsulation efficiency was > 97% (up to 98.7%). The calcium-free group (Example 4) exhibited severe micelle aggregation (particle size 285.6 nm, PDI = 0.362) due to the lack of ionic crosslinking, and the encapsulation efficiency was only 63.4%, demonstrating that calcium ions are the core driving force for micelle nanodispersion. In the alkaline environment of bamboo salt (pH = 10.5), the IPMP activity retention rate of the calcium-containing micelle system reached 94.8% to 96.3%, significantly higher than that of the non-micelle encapsulated comparative example 1 (42.7%) and the prior art control group (CN118105324A group, 68.7%), indicating that calcium ions effectively resist alkaline degradation by stabilizing the micelle structure.

[0053] (2) After accelerated storage at 45°C for 6 months, the calcium-containing formula (Examples 1-3) had a water separation rate of 0%, a viscosity retention rate of >92%, and a pH fluctuation of <0.2. The calcium-free group (Example 4) had a water separation rate of 17.3% and a viscosity retention rate of only 61.5% due to the lack of a calcium ion cross-linked thickener network, and the pH increased significantly (+1.35). The prior art group (CN118105324A) began to separate water after 3 months of storage, and the water separation rate reached 8.5% after 6 months, proving that calcium ions achieve long-term stability of "zero water separation" by enhancing the cross-linking effect of the system.

[0054] (3) The antibacterial rate of the calcium-containing micelle system against Streptococcus mutans (>98.5%) and Porphyromonas gingivalis (>97.8%) was significantly higher than that of the calcium-free group (83.7%-85.2%, p<0.01), which was close to 1.02-1.03 times that of the prior art group, indicating that calcium ions enhance the antibacterial efficacy by stabilizing enzyme activity. The whitening ΔE value of the calcium-containing group reached 3.9-4.2 (visible difference of >2 color levels), which was significantly better than that of the calcium-free group (2.7) and the prior art group (3.5); the amount of enamel wear was only 0.38-0.43 μm, which was more than 40% lower than that of the prior art group (0.65 μm), proving that calcium ions achieve dual protection of whitening and anti-wear by promoting remineralization.

[0055] The above is only an embodiment of the present invention, and the common knowledge such as the specific structure and characteristics of the scheme is not described in detail here. It should be pointed out that for those skilled in the art, without departing from the structure of the present invention, several variations and improvements can be made, which should also be regarded as the scope of protection of the present invention, and these will not affect the effect of the implementation of the present invention and the practicality of the patent. The scope of protection required by this application shall be based on the content of its claims, and the specific implementation methods and other records in the specification can be used to interpret the content of the claims.

Claims

1. A toothpaste, characterized in that The invention is composed of the following components in percentage by mass: 8-15% of bamboo salt, 0.03-0.15% of o-cymene-5-ol, 1-5% of polyglycerol fatty acid ester, 0.5-3% of calcium salt, 0.05-0.3% of lysozyme, 0.2-1% of bromelain, 15-28% of abrasive, 0.4-1.2% of thickener, 0.1-2% of pH buffer system, 10-35% of moisturizing agent, 1.5-4% of foaming agent, and the balance is water.

2. The toothpaste according to claim 1, characterized in that The polyglycerol fatty acid ester is polyglycerol-10 laurate or polyglycerol-6 distearate, and the calcium salt is calcium citrate or calcium gluconate.

3. The toothpaste according to claim 1, characterized in that The pH buffer system is composed of trehalose and arginine in a mass ratio of 1:0.5-2, and maintains the pH value of the toothpaste at 8.0-9.

2.

4. The toothpaste according to claim 1, characterized in that The friction agent is a mixture of surface-modified calcium carbonate with a particle size of 5 to 15 μm and spherical silicon dioxide with a particle size of 3 to 8 μm in a mass ratio of 2 to 4:

1.

5. The toothpaste according to claim 1, characterized in that The mass ratio of the lysozyme to the bromelain is 1:4-6, and the bromelain activity is greater than or equal to 2500 U / mg.

6. The method for preparing toothpaste according to any one of claims 1 to 5, characterized in that: The steps include: S1. Premix polyglycerol fatty acid ester, o-cymene-5-ol, calcium salt and 30-50% water, and homogenize at 40-50° C. to form micellar inclusions; S2. Mix and dissolve bamboo salt, pH buffer system, moisturizer and remaining water, then add abrasive, thickener and foaming agent, and stir under vacuum; S3. Add micellar inclusions, lysozyme, and bromelain, and degas for 3 to 8 minutes under a vacuum degree ≥ 0.095 MPa.

7. The method for preparing toothpaste according to claim 6, wherein: The homogenization pressure is 80-120 MPa, and the cycle is 3-5 times; the system temperature is controlled at 25-30° C. when the enzyme is added.

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