CN114288208A - Tooth whitening composition, oral care cleaning product and preparation method thereof - Google Patents
Tooth whitening composition, oral care cleaning product and preparation method thereof Download PDFInfo
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Abstract
The invention provides a tooth whitening composition, an oral care cleaning product and a preparation method thereof, and belongs to the technical field of oral health care, the tooth whitening composition comprises cross-linked povidone, phosphate and a high-cleaning abrasive, and the mass ratio of the cross-linked povidone to the phosphate to the high-cleaning abrasive is (1-5): (1-10): (5-20); the oral care cleaning product provided by the invention comprises the tooth whitening composition, is an anhydrous formula, and has a remarkable tooth whitening effect. Meanwhile, the product can keep paste not to be separated out and return to coarse in 3 months under the environment of low temperature (-18 ℃) and high temperature (50 ℃), and the PH value and the phosphate content are stable, so that the stability is improved. The preparation method disclosed by the invention is simple in process and environment-friendly.
Description
Technical Field
The invention belongs to the technical field of oral health care, and particularly relates to a tooth whitening composition, an oral care cleaning product and a preparation method thereof.
Background
Various bacterial groups exist on the surface of teeth to form bacterial biofilms, a plurality of viscous substances are secreted on the surface of the teeth, exogenous pigments such as tea drinking, coffee drinking, smoking and the like are usually adhered to the viscous substances to gradually turn yellow or black on the surface of the teeth to form color spots, so that the appearance is influenced, a plurality of adverse effects are brought to the appearance, the mind and the life of a patient, and diseases of dental tissues and periodontal tissues can be caused.
The toothpaste for removing the exogenous pigment from the teeth on the market at present mainly takes effect through three ways. The first is a physical whitening method, in which a highly-clean abrasive is used to whiten teeth, and the mechanism is to remove pigments by enhancing the friction between the abrasive and the surface of the teeth, but the method is a relatively single physical removal method, which can have a certain effect, and has a certain wear risk to teeth after being frequently used, and the effect is often better after chemical whitening is compounded, for example, the compound phosphate compound has a synergistic effect. The second method is a chemical whitening method, which mainly uses phosphate compounds to whiten teeth, the phosphate compounds have an action mechanism of inhibiting the formation of a biological film through phosphate radicals, so that the adhesion of pigments is inhibited, calcium ions are complexed, and the probability of adsorbing pigments such as tea stains, coffee stains and the like on the surfaces of the teeth is further reduced. The third is strong oxidation whitening method, which removes the pigment through the strong oxidation of peroxide, and the side effect is the problem of tooth sensitivity.
Prior art CN02823369.7 discloses a dentifrice composition comprising a low water content phase of a stable phosphate salt and an ionic active ingredient. The composition comprises from 0.1% to 30% of one or more linear polyphosphates having an average chain length of about 4 or greater; and is selected from the group consisting of fluoride ion sources, stannous ion sources, zinc ion sources, copper ion sources, and mixtures thereof. Methods of stabilizing dentifrice compositions by providing such binder systems.
At present, oral care cleaning products in the prior art are not ideal in whitening effect, anhydrous toothpaste is easy to separate out and turn thick, and the content of functional component phosphate is easy to degrade, so that the efficacy and the use experience of the products are influenced.
Disclosure of Invention
In view of the above, the present invention aims to provide a tooth whitening composition, an oral care cleaning product and a preparation method thereof; the tooth whitening composition provided by the invention comprises crospovidone, phosphate and high-cleaning silicon dioxide, and has a remarkable tooth whitening effect under the synergistic effect of the crospovidone, the phosphate and the high-cleaning silicon dioxide. Wherein the crospovidone can be used as a whitening agent to synergistically whiten teeth with phosphate; the toothpaste can also be used as a thickening agent to stabilize the anhydrous formula system toothpaste and ensure that the paste is stable and does not separate out; the cross-linked povidone has high surface area and unique chemical structure, so that the cross-linked povidone has high interfacial activity, can improve the dissolution of phosphate, rapidly expands when meeting water in the process of tooth brushing, increases the action area of the paste and teeth, and improves the whitening effect.
The invention provides a tooth whitening composition which comprises cross-linked povidone, phosphate and a high-cleaning abrasive, wherein the mass ratio of the cross-linked povidone to the phosphate to the high-cleaning abrasive is (1-5): (1-10): (5-20).
Preferably, the mass ratio of the crospovidone to the phosphate is 1: (1-5).
Preferably, the average particle size of the crospovidone is 1-200 μm.
Preferably, the phosphate is selected from one of polyphosphate, pyrophosphate and hexametaphosphate.
Preferably, the high cleaning abrasive is high cleaning silica.
The invention also provides an oral care cleaning product, which comprises the following components in parts by weight based on 100 parts by weight: 1-5 parts of cross-linked polyvidone, 1-10 parts of phosphate, 5-20 parts of high-cleaning friction agent, 10-30 parts of polyol, 0.1-5 parts of sweetening agent, 0.01-5 parts of anticarious agent, 0.1-5 parts of thickening agent, 1-10 parts of foaming agent, 0.01-5 parts of pH regulator, 0.5-1.5 parts of aromatic and the balance of glycerol.
Preferably, the thickener is one of carbomer, xanthan gum, sodium cellulose and carrageenan.
Preferably, the oral care cleaning product is toothpaste or tooth powder.
Preferably, the pH of the oral care cleaning product is 5.5-8.5.
The invention provides a preparation method of an oral care cleaning product, which comprises the following steps:
1) dispersing a thickening agent in polyhydric alcohol to obtain a mixed solution;
2) mixing the mixed solution obtained in the step 1) with glycerol at the temperature of 60-65 ℃ until no particles exist to obtain a first material;
3) mixing phosphate, sweetener, anticarious agent and pH regulator with the first material obtained in step 2) to obtain a second material;
4) mixing the high-cleanness abrasive, the crospovidone and the second material obtained in the step 3) to obtain a third material;
5) mixing the foaming agent and the aromatic with the third material obtained in the step 4) to obtain the oral care cleaning product.
Compared with the prior art, the invention has the following beneficial effects:
the tooth whitening composition provided by the invention comprises crospovidone, phosphate and high-cleaning silicon dioxide, wherein the crospovidone is formed by cross-linking vinyl pyrrolidone (NVP) monomers with different particle sizes serving as raw materials, is a synthetic, water-insoluble and rapidly-expandable N-vinyl-2-pyrrolidone cross-linked homopolymer, is in a granular porous structure, and has an average particle size of 25-140 microns: the cross-linked polyvidone is used as a whitening agent, and is used for whitening teeth in a synergistic manner with phosphate; the crospovidone is a nonionic copolymer and can be used as a thickening agent to stabilize an anhydrous formula system; the crospovidone has higher surface area and unique chemical structure, leads to stronger interfacial activity, can improve the dissolution of phosphate when being used as a disintegrant, rapidly expands when meeting water in the process of tooth brushing, increases the action area of paste and teeth, and improves the whitening effect.
The oral care product provided by the invention can keep paste body not separated out and not coarsened for 3 months under the environment of low temperature (-18 ℃), room temperature (20-25 ℃) and high temperature (50 ℃), and has stable PH value and phosphate content, thereby improving the stability of the anhydrous toothpaste.
Drawings
FIG. 1 is an uncolored hydroxyapatite sheet;
fig. 2 is a hydroxyapatite sheet after coloring;
fig. 3 is a hydroxyapatite sheet of the oral care cleaning product of example 1 after brushing;
fig. 4 is a hydroxyapatite sheet of the oral care cleaning product of example 2 after brushing;
fig. 5 to 9 show hydroxyapatite sheets after the oral care cleaning products of comparative examples 1 to 5 were brushed and ground, respectively.
Detailed Description
The invention provides a tooth whitening composition which comprises cross-linked povidone, phosphate and a high-cleaning abrasive, wherein the mass ratio of the cross-linked povidone to the phosphate to the high-cleaning abrasive is (1-5): (1-10): (5-20).
In the invention, the average particle size of the crospovidone is preferably 1-200 μm, and more preferably 25-140 μm.
In the present invention, the mass ratio of crospovidone and phosphate is preferably 1: (1-5), more preferably 2: 3. In the present invention, the crospovidone and the phosphate have a synergistic whitening effect on teeth within the above-defined mass ratio range.
In the present invention, the phosphate is selected from one of polyphosphate, pyrophosphate and hexametaphosphate; the polyphosphate comprises pentasodium tripolyphosphate or pentapotassium tripolyphosphate; the pyrophosphate comprises one of trisodium monohydrogen pyrophosphate, tripotassium monohydrogen pyrophosphate, disodium dihydrogen pyrophosphate, dipotassium dihydrogen pyrophosphate, tetrasodium pyrophosphate and tetrapotassium pyrophosphate, and the hexametaphosphate comprises sodium hexametaphosphate or potassium hexametaphosphate; in the present invention, the phosphate is preferably pyrophosphate, and in the specific implementation process of the present invention, the pyrophosphate is preferably tetrasodium pyrophosphate and/or trisodium monohydrogen pyrophosphate; when the pyrophosphate is tetrasodium pyrophosphate and trisodium monohydrogen pyrophosphate, the mass ratio of the tetrasodium pyrophosphate to the trisodium monohydrogen pyrophosphate is preferably 2: 1.
In the present invention, the high cleaning abrasive is preferably high cleaning silica. According to the whitening cream, the high-cleaning silicon dioxide is used as a matrix, and the cross-linked povidone and the phosphate are compounded, so that the whitening effect can be remarkably improved.
The invention also provides an oral care cleaning product, which comprises the following components in parts by weight based on 100 parts by weight: 1-5 parts of cross-linked polyvidone, 1-10 parts of phosphate, 5-20 parts of high-cleaning friction agent, 10-30 parts of polyol, 0.1-5 parts of sweetening agent, 0.01-5 parts of anticarious agent, 0.1-5 parts of thickening agent, 1-10 parts of foaming agent, 0.01-5 parts of pH regulator, 0.5-1.5 parts of aromatic and the balance of glycerol.
In the present invention, the crospovidone, phosphate and high cleaning abrasive in the oral care cleansing product are the same as those in the above tooth whitening composition, and thus, detailed description thereof is omitted.
In the present invention, the oral care cleaning product preferably comprises 15 to 25 parts of polyhydric alcohol, more preferably 20 parts; the polyalcohol is preferably propylene glycol and PEG-8, and the mass ratio of the propylene glycol to the PEG-8 is preferably 1:1. In the present invention, the polyol functions as a dispersant.
In the invention, the oral care cleaning product preferably comprises 0.2-0.4 part of sweetening agent, more preferably 0.3 part; the invention has no special limitation on the specific type of the sweetening agent, and in the specific implementation process of the invention, the sweetening agent is saccharin sodium.
In the invention, the oral care cleaning product preferably comprises 0.01-5 parts of a caries preventing agent, more preferably 0.1-0.5 part of the caries preventing agent, and the caries preventing agent is preferably one of sodium fluoride, sodium monofluorophosphate and stannous fluoride. In the practice of the invention, the anticaries agent is sodium fluoride.
In the invention, the oral care cleaning product preferably comprises 0.4-1.0 part of thickening agent, more preferably 0.6-0.9 part of thickening agent, and in the invention, the thickening agent is preferably one of carbomer, xanthan gum, sodium cellulose and carrageenan, more preferably carbomer.
In the invention, the oral care cleaning product preferably comprises 0.5-3 parts of foaming agent, and more preferably 1-2.5 parts. In the present invention, the foaming agent is preferably sodium lauryl sulfate.
In the invention, the oral care cleaning product preferably comprises 0.01-1 part of pH regulator, more preferably 0.1-0.6 part of pH regulator, and the pH regulator is preferably anhydrous trisodium phosphate or anhydrous citric acid; in the present invention, the specific amount of the PH adjuster is based on the amount of the oral care cleaning product adjusted to a defined PH range.
In the invention, the oral care cleaning product preferably comprises 0.8-1.2 parts of aromatic, more preferably 1 part; in the present invention, the fragrance is preferably a perfume.
In the present invention, the oral care cleaning product further comprises a balance of glycerin, which functions as a solvent and a humectant.
In the invention, the oral care cleaning product is preferably toothpaste or tooth powder, and the pH of the oral care cleaning product is preferably 5.5-8.5, and is further preferably 6.0-7.5; the oral care cleaning product disclosed by the invention is an anhydrous formula, and the whitening effect is obviously superior to that of a formula with water.
The invention provides a preparation method of an oral care cleaning product, which comprises the following steps: 1) dispersing a thickening agent in polyhydric alcohol to obtain a mixed solution; 2) mixing the mixed solution obtained in the step 1) with glycerol at the temperature of 50-70 ℃ until no particles exist to obtain a first material; 3) mixing phosphate, sweetener, anticarious agent and pH regulator with the first material obtained in step 2) to obtain a second material; 4) mixing the high-cleanness abrasive, the crospovidone and the second material obtained in the step 3) to obtain a third material; 5) mixing the foaming agent and the aromatic with the third material obtained in the step 4) to obtain the oral care cleaning product.
In the present invention, the thickener is first dispersed in the polyol to obtain a mixed solution, and in the present invention, the stirring is accompanied in the dispersing process, and the rotation speed and time of the stirring are not particularly limited, based on the uniform dispersion.
After the mixed solution is obtained, mixing the obtained mixed solution with glycerol at the temperature of 50-70 ℃ until no particles exist to obtain a first material; the temperature of the glycerol is preferably 58-63 ℃; stirring is carried out in the mixing process, and the stirring time is preferably 0.5-1.5 h, more preferably 0.8-1.2 h, and most preferably 1 h; the rotating speed of the stirring is preferably 800-1000 rpm.
After the first material is obtained, phosphate, a sweetening agent, an anticaries agent and a pH regulator are mixed with the obtained first material to obtain a second material. Then mixing the high-cleanness rubbing agent, the crospovidone and the obtained second material to obtain a third material; and finally, mixing the foaming agent, the aromatic and the obtained third material to obtain the oral care cleaning product. In the preparation process of the second material, the third material and the oral care cleaning product, stirring is preferably accompanied, and the stirring is used for uniformly mixing.
After obtaining the oral care cleaning product, the method preferably further comprises the steps of detecting, aging, discharging and filling. In the invention, the detection indexes preferably comprise characters, pH values and phosphate contents (the detection method is shown in QB/T5529-2020). In the invention, the aging temperature is preferably 20-25 ℃, and the aging time is preferably 24-30 h. In the present invention, the discharging and filling are performed by methods conventional in the art, and are not described herein.
The technical solutions provided by the present invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
The composition of the toothpaste of this example is shown in Table 1.
Table 1 example 1 raw material composition of whitening toothpaste
| Composition (I) | Specific substance | Mass percentage content (%) |
| Glycerol | Glycerol | Complement 100 |
| Povidone | Cross-linked polyvidone | 2 |
| Phosphate salts | Trisodium monohydrogen pyrophosphate | 3 |
| Friction agent | Silicon dioxide | 15 |
| Polyhydric alcohols | Propylene glycol + PEG-8 | 20 |
| Thickening agent | Carbomer | 0.8 |
| Sweetening agent | Saccharin sodium salt | 0.3 |
| Anticariogenic agent | Sodium fluoride | 0.32 |
| PH regulator | Trisodium phosphate | 0.5 |
| Foaming agent | Sodium lauryl sulfate | 2 |
| Aromatic agent | Essence | 1 |
Wherein the mass percent of the propylene glycol is 10 percent, and the mass percent of the PEG-8 is 10 percent.
The preparation method comprises the following steps:
uniformly dispersing the thickening agent in the polyhydric alcohol, and uniformly stirring and mixing for later use;
heating glycerol to 63 ℃, adding the mixed solution into hot glycerol, stirring for 1h at 900rpm, and stirring until the mixed solution is uniformly mixed without particles;
sequentially adding phosphate, sweetener, anticarious agent and pH regulator into a reaction kettle to dissolve the materials, and stirring at 900rpm until the materials are uniformly mixed;
adding the friction agent and the povidone into a reaction kettle, and stirring at 900rpm until the materials are uniformly mixed;
adding the foaming agent and the aromatic into a reaction kettle, and stirring at 900rpm until the mixture is uniformly mixed.
Detecting, aging, discharging and filling.
Example 2
The composition of the toothpaste of this example is shown in Table 2.
Table 2 example 2 raw material composition of whitening toothpaste
| Composition (I) | Specific substance | Mass percentage content (%) |
| Glycerol | Glycerol | Complement 100 |
| Povidone | Cross-linked polyvidone | 2 |
| Phosphate salts | Tetrasodium pyrophosphate | 2 |
| Phosphate salts | Trisodium monohydrogen pyrophosphate | 1 |
| Friction agent | Silicon dioxide | 15 |
| Polyhydric alcohols | Propylene glycol + PEG-8 | 20 |
| Thickening agent | Carbomer | 0.8 |
| Sweetening agent | Saccharin sodium salt | 0.3 |
| Anticariogenic agent | Sodium fluoride | 0.32 |
| PH regulator | Trisodium phosphate | 0.2 |
| Foaming agent | Sodium lauryl sulfate | 2 |
| Aromatic agent | Essence | 1 |
Wherein the mass percent of the propylene glycol is 10 percent, and the mass percent of the PEG-8 is 10 percent.
The preparation method comprises the following steps:
uniformly dispersing the thickening agent in the polyhydric alcohol, and uniformly stirring and mixing for later use;
heating glycerol to 60 ℃, adding the mixed solution into hot glycerol, stirring for 1h at 800rpm, and stirring until the mixed solution is uniformly mixed without particles;
sequentially adding phosphate, sweetener, anticarious agent and pH regulator into a reaction kettle to dissolve the materials, and stirring at 800rpm until the materials are uniformly mixed;
adding the friction agent and the povidone into a reaction kettle, and stirring at 800rpm until the materials are uniformly mixed;
adding the foaming agent and the aromatic into a reaction kettle, and stirring at 800rpm until the mixture is uniformly mixed.
Detecting, aging, discharging and filling.
Comparative example 1
The comparative example uses glycerin instead of crospovidone in example 1, the types and contents of the rest components are consistent with example 1, and the preparation method is consistent with example 1.
Comparative example 2
This comparative example uses glycerin instead of the phosphate (trisodium monohydrogen pyrophosphate) in example 1, and the kinds and amounts of the remaining ingredients were the same as in example 1, and the preparation method was the same as in example 1.
Comparative example 3
In the comparative example, povidone in a non-crosslinked form is used instead of crospovidone in example 1, the types and contents of the rest of the components are the same as those in example 1, and the preparation method is the same as that in example 1.
Comparative example 4
The toothpaste of this comparative example was in an aqueous formulation and the ingredients are shown in table 3.
Table 3 comparative example 4 aqueous formulation toothpaste composition
| Composition (I) | Specific substance | Mass percentage content (%) |
| Water (W) | Water (W) | Complement 100 |
| Glycerol | Glycerol | 5 |
| Sorbitol | Sorbitol | 50 |
| Phosphate salts | Trisodium monohydrogen pyrophosphate | 3 |
| Friction agent | Silicon dioxide | 15 |
| Thickening agent | Xanthan gum/CMC | 0.8 |
| Sweetening agent | Saccharin sodium salt | 0.3 |
| Anticariogenic agent | Sodium fluoride | 0.32 |
| PH regulator | Trisodium phosphate | 0.1 |
| Foaming agent | Sodium lauryl sulfate | 2 |
| Aromatic agent | Essence | 1 |
The preparation method comprises the following steps:
uniformly dispersing the thickening agent in glycerol, and uniformly stirring and mixing for later use;
adding water, polyalcohol, stabilizer, sweetener, anticarious agent, and pH regulator into a reaction kettle in sequence to dissolve the materials, and stirring at 900rpm to mix well;
slowly adding the mixed solution of the glycerol and the thickening agent into a reaction pot, and stirring at 900rpm until the mixture is uniformly mixed;
adding a friction agent into a reaction kettle, and stirring at 900rpm until the friction agent is uniformly mixed;
adding the foaming agent and the aromatic into a reaction kettle, and stirring at 900rpm until the mixture is uniformly mixed.
Detecting, aging, discharging and filling.
Comparative example 5
The toothpaste of this comparative example was in an aqueous formulation and the ingredients are shown in table 4.
Table 4 comparative example 5 aqueous formulation toothpaste composition
The preparation method comprises the following steps:
uniformly dispersing the thickening agent in glycerol, and uniformly stirring and mixing at 800rpm for later use;
adding water, polyalcohol, stabilizer, sweetener, anticarious agent, and pH regulator into a reaction kettle in sequence to dissolve the materials, and stirring at 800rpm to mix well;
slowly adding the mixed solution of the glycerol and the thickening agent into a reaction pot, and stirring at 800rpm until the mixture is uniformly mixed;
adding the friction agent and the povidone into a reaction kettle, and stirring at 800rpm until the materials are uniformly mixed;
adding the foaming agent and the aromatic into a reaction kettle, and stirring at 800rpm until the mixture is uniformly mixed.
Detecting, aging, discharging and filling.
Test examples
Performance evaluation:
laboratory evaluation of whitening efficacy
Selecting a hydroxyapatite wafer close to human enamel, putting the hydroxyapatite wafer into a mixed solution of type III pig stomach mucin and simulated saliva, putting the mixed solution into a constant temperature incubator, and culturing overnight (20h) at 37 ℃ and 200rpm, thereby simulating the acquired sialoprotein film on the surface of the tooth. In order to research the whitening effect of the stained teeth, the hydroxyapatite tablets are placed into a black tea solution and stained for 30min, so that exogenous tooth stains of the teeth are simulated. The stained hydroxyapatite sheet was fixed on a sampling plate, mounted in a L8-II brush mill (purchased from shanghai mei jia jing japan chemical limited), water and toothpaste (toothpaste prepared in examples 1 and 2 and comparative examples 1 to 5) were stirred and mixed uniformly at a dilution ratio of 1:1.6, added to a slurry cup of an L8-II brush mill, the toothbrush load pressure was adjusted to 150g, and the brush milling was performed 1000 times at a speed of 80rpm, to simulate a human tooth brushing process. After the brushing test was completed, the L a b values of the hydroxyapatite sheets before staining and after brushing were measured using an X-Rite spectrophotometer.
The color difference of Hydroxyapatite (HAP) sheets was evaluated using the international commission on illumination (CIE) L, a, b color space system. Where L represents the whiteness value of the object, with L being 0 for a perfect black body and 100 for a perfect reflector. In this system, L denotes the apparent lightness, and a and b denote the hue and chroma.
By passing
To calculate the whiteness value of the hydroxyapatite in Δ W*＝W*(Baseline) -W*(treatment) to evaluate whitening effect of the toothpaste. Δ W*The larger the value, the better the whitening effect.
The laboratory evaluation results of the whitening toothpaste are shown in table 5, and the whitening effect of the hydroxyapatite after brushing is shown in table 5:
(1) comparative example 2 using only high cleaning silica and crospovidone as whitening agent, aw thereof*The value is only 1.85, the effect is poor, and the whitening effect is not obvious. In contrast, comparative examples 1 and 4, Δ using high cleaning silica and phosphate as whitening agentsW*The value was slightly higher, but the whitening effect was still not ideal.
(2) By contrast, comparative example 3, example 1 and example 2, in which aw of example 1 and example 2 of the tooth whitening effect composition was used, all had higher whitening effects*The value can reach more than 20, compared with examples 1 and 2, the whitening effect of the non-crosslinked povidone used in the comparative example 3 is relatively poor, and the difference of the whitening effect of different forms of povidone is obvious.
(3) Δ W of example 1*The value is 1.81 times of that of comparative example 5, and the delta W of the anhydrous formula is equal to that of the composition with the same tooth whitening effect*The value is about 2 times of that of the aqueous formula, which shows that the whitening effect of the anhydrous formula is better than that of the aqueous formula.
(4) Example 1 compares the Δ W with example 2*The value difference is not obvious, under the condition of the same phosphate addition amount, the phosphate has no compound synergistic effect, and the whitening effect of the whitening agent has no obvious difference with the effect of using a single phosphate.
Therefore, the whitening effect of the whitening toothpaste is obviously improved by compounding the high-cleaning silicon dioxide serving as a matrix, the cross-linked povidone and the phosphate, and the whitening effect of the anhydrous formula is better than that of the aqueous formula.
TABLE 5 whitening Effect of the respective test groups
| Group of | W*(Baseline) | W*(treatment) | ΔW*Value of |
| Comparative example 1 | 45.09 | 39.31 | 5.78 |
| Comparative example 2 | 39.23 | 37.38 | 1.85 |
| Comparative example 3 | 35.8 | 27.43 | 8.37 |
| Example 1 | 42.92 | 19.74 | 23.18 |
| Example 2 | 40.11 | 18.24 | 21.87 |
| Comparative example 4 | 38.45 | 35.98 | 2.47 |
| Comparative example 5 | 42.56 | 28.77 | 12.79 |
Evaluation of whitening efficacy in human body
The toothpaste of example 1 and comparative example 4 were stored at normal temperature for three months from the date of production. Example 1 was used as a positive test group sample, and comparative example 4 was used as a negative control group sample.
Screening testers, wherein the patients mainly complain about tooth staining, have daily eating habits of smoking, drinking red wine, drinking coffee, chewing betel nuts and the like, and 100 testers with Lobene color spot index of 3 are selected in the test and randomly divided into two groups, wherein 50 patients in each group comprise 45 male patients, 55 female patients, 55 patients with the maximum age and 18 patients with the minimum age.
The using method comprises the following steps: brushing teeth with toothpaste in the morning and evening for 2-3 minutes each time, and rechecking after 7 days and 14 days.
Examination index and index used:
lobene color spot index grading scoring is adopted, and the area of the color spot part and the color spot degree are evaluated in 0-3 grades (see table 6).
Table 6 Lobene stain index grading
| Grading scoring | Area of | Degree |
| 0 | Absence of colorless spots | Absence of colorless spots |
| 1 | 1/3 for mottling up to tooth surface | Slight color spot (yellow or yellow brown) |
| 2 | The mottle does not exceed 2 of the tooth surface/3 | Moderate color spots (moderate brown) |
| 3 | 2/3 color spot larger than tooth surface | Severe mottle (dark brown or black) |
TABLE 7 human 14-day test results
Specific test results are shown in table 7, and according to the human body test data shown in table 7, the overall whitening effect of the negative control group to the ratio 4 is poor, the ratio of the Lobene stain index to 3 is 70%, and the ratio of the Lobene stain index to 2 and 3 is 96%. The whitening effect of the positive test group in example 1 is better, the Lobene color spot index is 60% of 0 and 1, and the Lobene color spot index is 96% of 0, 1 and 2. As can be seen from the test data in table 7, example 1 has a significant whitening effect compared to comparative example 4.
Stability of
And filling the sample aged for 24 hours into a toothpaste tube, standing for 3 months in low-temperature (-18 ℃), room-temperature (20-25 ℃) and high-temperature (50 ℃) environments respectively, and observing whether the appearance of the toothpaste body is separated out or not and whether the PH value and the phosphate content are changed or not (see table 8). The PH value detection method refers to GB/T8372-2017, and the phosphate content detection method refers to QB/T5529-2020.
Table 8 stability test results
As is clear from Table 8, in examples 1 and 2, the stability was improved by maintaining the pH and the phosphate content in a stable state, and by preventing precipitation and coarsening in the low temperature (-18 ℃ C.), room temperature (20 to 25 ℃ C.) and high temperature (50 ℃ C.).
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The tooth whitening composition is characterized by comprising crospovidone, phosphate and a high-cleaning abrasive, wherein the mass ratio of the crospovidone to the phosphate to the high-cleaning abrasive is (1-5): (1-10): (5-20).
2. The tooth whitening composition according to claim 1, wherein the crospovidone is a N-vinyl-2-pyrrolidone cross-linked homopolymer and the mass ratio of crospovidone to phosphate is 1: (1-5).
3. The tooth whitening composition according to claim 1 or 2, wherein the crospovidone has an average particle size of 1 to 200 μm.
4. The tooth whitening composition according to claim 1, wherein the phosphate is selected from one of polyphosphate, pyrophosphate and hexametaphosphate.
5. The tooth whitening composition according to claim 1, wherein the high cleaning abrasive is high cleaning silica.
6. An oral care cleaning product is characterized by comprising the following components in parts by weight based on 100 parts by weight: 1-5 parts of cross-linked polyvidone, 1-10 parts of phosphate, 5-20 parts of high-cleaning friction agent, 10-30 parts of polyol, 0.1-5 parts of sweetening agent, 0.01-5 parts of anticarious agent, 0.1-5 parts of thickening agent, 1-10 parts of foaming agent, 0.01-5 parts of pH regulator, 0.5-1.5 parts of aromatic and the balance of glycerol.
7. The oral care cleaning article of claim 6 wherein the thickening agent is one of carbomer, xanthan gum, sodium cellulose and carrageenan.
8. The oral care cleaning product of claim 6 or 7, wherein the oral care cleaning product is a toothpaste or a tooth powder.
9. The oral care cleaning product of claim 6 or 7, wherein the oral care cleaning product has a pH of 5.5 to 8.5.
10. The method of making an oral care cleaning product of any one of claims 6 to 9, comprising the steps of:
1) dispersing a thickening agent in polyhydric alcohol to obtain a mixed solution;
2) mixing the mixed solution obtained in the step 1) with glycerol at the temperature of 50-70 ℃ until no particles exist to obtain a first material;
3) mixing phosphate, sweetener, anticarious agent and pH regulator with the first material obtained in step 2) to obtain a second material;
4) mixing the high-cleanness abrasive, the crospovidone and the second material obtained in the step 3) to obtain a third material;
5) mixing the foaming agent and the aromatic with the third material obtained in the step 4) to obtain the oral care cleaning product.
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Cited By (1)
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