CN107519026B - Dentifrice with stain removing and breath freshening functions and preparation method thereof - Google Patents

Abstract

The invention relates to the technical field of oral care products, in particular to a dentifrice with stain removal and breath freshening functions and a preparation method thereof. According to the invention, a set of brand-new dentifrice formula system is developed through new friction system compounding and new foaming system compounding, the problems of high abrasion value and large irritation of the existing dentifrice are solved, and the dentifrice has strong cleaning stain capacity and breath adsorbing capacity. The raw materials used by the dentifrice disclosed by the invention are common raw materials in the food industry, and the dentifrice has good safety performance.

Description

Dentifrice with stain removing and breath freshening functions and preparation method thereof

Technical Field

The invention relates to the technical field of oral care products, in particular to a dentifrice with stain removing and breath freshening functions and a preparation method thereof.

Background

A lot of consumers form tooth stains due to the fact that a large amount of pigment is deposited on teeth when smoking, eating colored foods and the like, meanwhile, the deposited tooth stains are easy to breed bacteria to generate unpleasant smell, and much trouble is brought to daily life of the consumers, so that an oral cleaning and nursing product with good stain removing and breath freshening effects is developed, the consumers are helped to solve the problems, and great social benefits and economic benefits are achieved.

The research shows that the bamboo charcoal-containing dentifrice products in the market only contain calcium carbonate, bamboo charcoal and calcium hydrophosphate dihydrate, do not contain a foaming agent, a humectant and the like, and have obvious difference with the technical scheme of the invention. Compared with oral cleaning and nursing products such as toothpaste, mouthwash and the like, the existing dentifrice product has the advantages of strong friction force and good cleaning effect, and is popular with consumers with partial tooth stains, but because the addition amount of the friction agent of the existing dentifrice product is too much, the abrasion to teeth is relatively large while the cleaning force is high, and simultaneously because the addition amount of the dentifrice is greatly reduced compared with the addition amount of liquid phases such as a toothpaste product humectant and water, the irritation of the dentifrice product using the traditional sodium lauryl sulfate (K12) as a foaming agent under the condition is far greater than that of the dentifrice product.

Disclosure of Invention

The invention provides a dentifrice product aiming at the problems of great abrasion to teeth and great irritation to oral mucosa in use of the existing dentifrice product, the dentifrice product has strong stain removal and breath adsorption performances, is mild in taste, does not irritate the oral mucosa, is small in abrasion to teeth, can help users to solve the problems of tooth stain deposition and breath, and is good in safety performance.

In order to achieve the purpose, the invention adopts the following technical scheme.

A dentifrice with stain removing and breath freshening functions is composed of the following components in percentage by mass:

the composite friction agent comprises activated carbon and a second friction component, wherein the second friction component is at least one selected from silicon dioxide, calcium carbonate and calcium hydrophosphate dihydrate.

The mass ratio of the active carbon to the second friction component in the composite friction agent is 9: 1-171.

The adsorption value of the activated carbon to methylene blue is more than 150mg/g, and the adsorption value to carbon tetrachloride is more than 500mg/g, so that the dentifrice product has good adsorption performance to tooth deposition stains and breath.

The active carbon is powdery food-grade active carbon and is prepared from plant components such as fruit shells, wood chips and the like.

The humectant is at least one selected from sorbitol, glycerol, polyethylene glycol and propylene glycol. The addition amount of the humectant is not more than 10 percent so as to ensure that the decoloring and adsorbing effects of the active carbon can be better exerted.

The foaming agent is selected from at least one of cocamidopropyl betaine, lauryl glucoside and coco glucoside.

The dentifrice with stain removing and breath freshening functions can also comprise 0.2-0.8% of essence.

The preparation method of the dentifrice with stain removing and breath freshening functions comprises the following steps:

s1, adding the water-soluble material into water, and uniformly stirring to obtain a mixed solution;

s2, uniformly mixing the materials for forming the composite friction agent to obtain mixed powder;

s3, adding the mixed solution into the mixed powder through a sprayer, starting stirring simultaneously, and uniformly mixing the components to obtain a mixture;

and S4, grinding the mixture by a grinder to obtain the dentifrice after uniform grinding.

In the step S1, the method further includes the step of adding essence which accounts for 0.2-0.8% of the dentifrice by mass into the mixed solution and uniformly mixing.

The invention has the beneficial effects that:

aiming at the particularity of color stains and breath deposited on teeth, the food-grade activated carbon with strong adsorption performance on the color stains and the breath on the teeth is screened out to be used as a tooth powder raw material, so that the tooth powder product can be ensured to have good adsorption performance on the color stains and the breath deposited on the teeth, and simultaneously, the content of liquid materials in the tooth powder product is far lower than that of products such as toothpaste and the like, so that the decoloration adsorption performance of the activated carbon is more favorably exerted; in addition, the activated carbon and the second friction component are compounded and applied, so that the tooth powder product has high cleaning power and greatly reduces the abrasion value of the tooth powder product to teeth.

Alkyl glycoside surfactants and betaine surfactants have the advantage of low irritation compared with sodium lauryl sulfate (K12) commonly used in the oral industry, and the surfactant (foaming agent) of the type is not found to be applied to dentifrice products at present. According to the invention, researches show that under the condition of the composite abrasive containing activated carbon, lauryl glucoside, coco glucoside and cocamidopropyl betaine in the foaming agent can well meet the foaming requirement in a dentifrice product, and meanwhile, the dentifrice has mild taste and small irritation to oral mucosa.

According to the invention, a set of brand-new dentifrice formula system is developed through new friction system compounding and new foaming system compounding, the problems of high abrasion value and large irritation of the existing dentifrice are solved, and the dentifrice has strong cleaning stain capacity and breath adsorbing capacity. The raw materials used by the dentifrice disclosed by the invention are common raw materials in the food industry, and the dentifrice has good safety performance.

Detailed Description

In order to more fully understand the technical contents of the present invention, the technical solutions of the present invention will be further described and illustrated with reference to the following specific embodiments.

The features, benefits and advantages of the present invention will become apparent to those skilled in the art from a reading of the present disclosure.

The activated carbon used in the following examples and comparative examples was food grade activated carbon in powder form prepared from plant components such as husks and wood chips, and had an adsorption value of more than 150mg/g for methylene blue and an adsorption value of more than 500mg/g for carbon tetrachloride.

Example 1

The embodiment provides a preparation method of a dentifrice with stain removing and breath freshening functions, wherein the dentifrice is prepared from the following components in percentage by mass:

3% of sorbitol;

3.5 percent of food-grade active carbon;

66.5% of silicon dioxide;

0.5 percent of essence;

coco glucoside 2%;

the balance of water.

The preparation method of the dentifrice comprises the following steps:

1) adding the weighed sorbitol and coco glucoside into water, and uniformly stirring to obtain a mixed solution;

2) uniformly mixing the measured active carbon and silicon dioxide in a mixing pot to obtain mixed powder;

3) adding the metered essence into the mixed solution of the step 1);

4) adding the mixed liquid obtained in the step 3) into the mixed powder obtained in the step 2) through a sprayer, and starting stirring to ensure that the liquid material and the divided material are uniformly mixed to obtain a mixture;

5) grinding the mixture obtained in the step 4) by a grinder to obtain the dentifrice after uniform grinding, and packaging to obtain the dentifrice product.

Example 2

The embodiment provides a preparation method of a dentifrice with stain removing and breath freshening functions, wherein the dentifrice is prepared from the following components in percentage by mass:

7% of glycerol;

81% of food-grade active carbon;

9% of calcium carbonate;

0.2 percent of essence;

cocamidopropyl betaine 8%;

the balance of water.

The preparation method of the dentifrice comprises the following steps:

1) adding the measured glycerol and the cocamidopropyl betaine into water, and uniformly stirring to obtain a mixed solution;

2) uniformly mixing the measured active carbon and calcium carbonate in a mixing pot to obtain mixed powder;

3) adding the metered essence into the mixed solution of the step 1);

4) adding the mixed liquid obtained in the step 3) into the mixed powder obtained in the step 2) through a sprayer, and starting stirring to ensure that the liquid material and the divided material are uniformly mixed to obtain a mixture;

5) grinding the mixture obtained in the step 4) by a grinder to obtain the dentifrice after uniform grinding, and packaging to obtain the dentifrice product.

Example 3

The embodiment provides a preparation method of a dentifrice with stain removing and breath freshening functions, wherein the dentifrice is prepared from the following components in percentage by mass:

6% of glycerol;

40% of food-grade active carbon;

40% of silicon dioxide;

0.8% of essence;

5% of lauryl glucoside;

the balance of water.

The preparation method of the dentifrice comprises the following steps:

1) adding the measured glycerol and lauryl glucoside into water, and uniformly stirring to obtain a mixed solution;

2) uniformly mixing the measured active carbon and silicon dioxide in a mixing pot to obtain mixed powder;

3) adding the metered essence into the mixed solution of the step 1);

4) adding the mixed liquid obtained in the step 3) into the mixed powder obtained in the step 2) through a sprayer, and starting stirring to ensure that the liquid material and the divided material are uniformly mixed to obtain a mixture;

5) grinding the mixture obtained in the step 4) by a grinder to obtain the dentifrice after uniform grinding, and packaging to obtain the dentifrice product.

Example 4

The embodiment provides a preparation method of a dentifrice with stain removing and breath freshening functions, wherein the dentifrice is prepared from the following components in percentage by mass:

10% of sorbitol;

63% of food-grade active carbon;

7% of silicon dioxide;

0.5 percent of essence;

coco glucoside 5%;

the balance of water.

The preparation method of the dentifrice comprises the following steps:

1) adding the weighed sorbitol and coco glucoside into water, and uniformly stirring to obtain a mixed solution;

2) uniformly mixing the measured active carbon and silicon dioxide in a mixing pot to obtain mixed powder;

3) adding the metered essence into the mixed solution of the step 1);

4) adding the mixed liquid obtained in the step 3) into the mixed powder obtained in the step 2) through a sprayer, and starting stirring to ensure that the liquid material and the divided material are uniformly mixed to obtain a mixture;

5) grinding the mixture obtained in the step 4) by a grinder to obtain the dentifrice after uniform grinding, and packaging to obtain the dentifrice product.

Example 5

The embodiment provides a preparation method of a dentifrice with stain removing and breath freshening functions, wherein the dentifrice is prepared from the following components in percentage by mass:

1% of glycerol;

4.5 percent of food-grade active carbon;

85.5 percent of calcium carbonate;

0.5 percent of essence;

coco glucoside 2%;

the balance of water.

The preparation method of the dentifrice comprises the following steps:

1) adding the measured glycerol and the coco glucoside into water, and uniformly stirring to obtain a mixed solution;

2) uniformly mixing the measured active carbon and calcium carbonate in a mixing pot to obtain mixed powder;

3) adding the metered essence into the mixed solution of the step 1);

4) adding the mixed liquid obtained in the step 3) into the mixed powder obtained in the step 2) through a sprayer, and starting stirring to ensure that the liquid material and the divided material are uniformly mixed to obtain a mixture;

5) grinding the mixture obtained in the step 4) by a grinder to obtain the dentifrice after uniform grinding, and packaging to obtain the dentifrice product.

Comparative example 1

The present comparative example provides a method for preparing a dentifrice, the dentifrice being prepared from the following components in mass percent:

7% of glycerol;

81% of silicon dioxide;

9% of calcium carbonate;

0.2 percent of essence;

cocamidopropyl betaine 8%;

the balance of water.

The preparation method of the dentifrice comprises the following steps:

1) adding the measured glycerol and the cocamidopropyl betaine into water, and uniformly stirring to obtain a mixed solution;

2) uniformly mixing the weighed silicon dioxide and calcium carbonate in a mixing pot to obtain mixed powder;

3) adding the metered essence into the mixed solution of the step 1);

4) adding the mixed liquid obtained in the step 3) into the mixed powder obtained in the step 2) through a sprayer, and starting stirring to ensure that the liquid material and the divided material are uniformly mixed to obtain a mixture;

5) grinding the mixture obtained in the step 4) by a grinder to obtain the dentifrice after uniform grinding, and packaging to obtain the dentifrice product.

Comparative example 2

The present comparative example provides a method for preparing a dentifrice, the dentifrice being prepared from the following components in mass percent:

7% of glycerol;

90% of food-grade activated carbon;

0.2 percent of essence;

cocamidopropyl betaine 8%;

the balance of water.

The preparation method of the dentifrice comprises the following steps:

1) adding the measured glycerol and the cocamidopropyl betaine into water, and uniformly stirring to obtain a mixed solution;

2) adding the metered essence into the mixed solution of the step 1);

3) adding the mixed liquid obtained in the step 2) into food-grade activated carbon through a sprayer, and starting stirring to ensure that the liquid material and the divided material are uniformly mixed to obtain a mixture;

4) grinding the mixture obtained in the step 3) by a grinder to obtain the dentifrice after uniform grinding, and packaging to obtain the dentifrice product.

Comparative example 3

The present comparative example provides a method for preparing a dentifrice, the dentifrice being prepared from the following components in mass percent:

7% of glycerol;

81% of food-grade active carbon;

9% of calcium carbonate;

0.2 percent of essence;

sodium lauryl sulfate 8%;

the balance of water.

The preparation method of the dentifrice comprises the following steps:

1) adding the measured glycerol and sodium lauryl sulfate into water, and uniformly stirring to obtain a mixed solution;

2) uniformly mixing the measured active carbon and calcium carbonate in a mixing pot to obtain mixed powder;

3) adding the metered essence into the mixed solution of the step 1);

4) adding the mixed liquid obtained in the step 3) into the mixed powder obtained in the step 2) through a sprayer, and starting stirring to ensure that the liquid material and the divided material are uniformly mixed to obtain a mixture;

5) grinding the mixture obtained in the step 4) by a grinder to obtain the dentifrice after uniform grinding, and packaging to obtain the dentifrice product.

The dentifrice described in examples and comparative examples were tested for stain removal effect comparative test, oral mucosa irritation test, fresh breath effect comparative test, and tooth abrasion value comparative test, respectively, as follows. The test methods and test results are shown below.

1. Extrinsic stain removal test

1) Test sample

Experimental groups: examples 1 to 5; control group: comparative examples 1 to 3

2) Test apparatus and feedstock

Tooth brushing machine, ox tooth, slicer, polisher, coloring agent, whiteness meter, black tea, coffee, saliva mucin

3) Brief description of the test methods

Processing the ox teeth into sixteen slices with the same size by a cutting machine and a grinding machine, dyeing the processed ox teeth slices by using a solution prepared from black tea, coffee, salivary mucin and the like, drying the slices after dyeing, measuring the L value of the slices by using a whiteness instrument, embedding the ox teeth slices by using resin, randomly dividing the sixteen embedded ox teeth slices into eight groups, fixing the groups of the two slices on a tooth brushing machine, adding 5g of test tooth powder and 5g of water into each tooth brushing groove, using the same formula tooth powder for the same group of ox teeth slices, performing tooth brushing test on the ox teeth on the tooth brushing machine by using the same brush toothbrush, simulating the tooth brushing for 1200 times, taking out the slices of the ox teeth after brushing, drying the slices, measuring the L value of the difference △L value between the slices of the ox teeth before technical brushing and after technical brushing by using the whiteness instrument, calculating the average whiteness value of the two slices, and accordingly calculating the removal capacity of the different tooth powders on the stains, wherein the test results are shown in the following.

4) Test results

TABLE 1 results of the stain removal experiments

Group of	Whiteness difference (△L value)
		Example 1	7.5
Example 2	13.4
		Example 3	21.6
Example 4	11.3
		Example 5	10.5
Comparative example 1	6.5
		Comparative example 2	15.6
Comparative example 3	13.1

According to stain tests, the dentifrice prepared in the embodiment has a good stain removing effect on common tea stains, coffee stains and the like of teeth, wherein when the compounding ratio of a common abrasive (a second friction component) to food-grade activated carbon is 1:1 (embodiment 3), the product can take both the high cleaning power of a traditional abrasive and the pigment decolorizing capacity of activated carbon into consideration, and the stain removing effect is the best.

2. Mucosal irritation test

1) Test sample

Test groups: example 2; control group: comparative example 3

Each group of samples was prepared as a 50% aqueous solution for testing.

2) Test animal

SD rats 6, male, 9 weeks old, about 300g, were purchased from the center of medical laboratory animals in Guangdong province. Groups were randomized into 2 groups of three.

3) Brief description of the test methods

The test method comprises the following steps: animals were anesthetized by intraperitoneal injection with 3% sodium pentobarbital, and the cheek pouch was inverted and washed with saline to check for abnormalities. The left buccal pouch was used as the test side and the right buccal pouch was used as the control side. The samples of the test group were placed in the left buccal pouch and the samples of the control group were placed in the other buccal pouch. The contact time was 5 min. Taking out the cotton balls and wiping off the residual leaching liquor. The above procedure was repeated 1 time per hour for a total of 4 times. The buccal pouch was examined after each contact and before repeated placements. The buccal pouch was visually observed 24 hours after the last contact. The animals were sacrificed. Taking mucosa and surrounding tissues of a contact part of a sample in a test group, taking the sample with the thickness of about 0.3cm, fixing the sample by 10% formalin, embedding the sample by conventional paraffin, semi-continuously slicing, taking 5 slices at intervals, wherein the labels are 1, 2, 3, 4 and 5, the slice thickness is 4 mu m, and H-E staining.

3) Test results

Visual evaluation: the mucous membrane condition at the sample-placing site was visually observed at each observation period. The animal observations were added at each observation period and divided by the total number of animals observed to give an average score per animal.

And (3) histological observation: tissue reflectance scores were calculated for each animal. The microscopic evaluation scores of all animals in the test group were added and divided by the total number of observations to give the average score for the test group. The control group is calculated by the same method.

And performing comprehensive evaluation on the scores by visual observation and histological observation to obtain the stimulation index. The results are shown in Table 2.

TABLE 2 mucosal irritation test results

Group of	Stimulation index	Extent of reaction
			Experimental group (example 2)	4	Is extremely light
Control group (comparative example 3)	7	Mild degree of

The results show that the dentifrice prepared according to the present invention (example 2) has significantly reduced irritation to the oral mucosa compared to the dentifrice containing K12 (comparative example 3).

3. Fresh breath test

1) Test sample

Experimental groups: examples 1 to 5; control group: comparative examples 1 to 3

2) Testing instrument

Halimeter mouth gas tester

3) Test method

36 testers were selected, each halitosis value was measured and recorded using a breath tester, then the dentifrice prepared in example 1 was used to brush teeth for 2-3min, the halitosis value was measured and recorded 5 minutes after gargling, the difference between the halitosis values before and after the use of the dentifrice by the same person was calculated, and the statistical check of the average value was performed. The dentifrice prepared in examples 2 to 5 and comparative examples 1 to 3 were each subjected to the test in the same manner. The number of instruments is limited, and the testing time of each person needs 2-3min, so that different groups of experiments need to be carried out in days. The test results are shown in table 3.

4) Test results

TABLE 3 breath test results

The results show that the dentifrice prepared in the examples has a remarkable breath reduction effect compared with the dentifrice prepared in comparative example 1, and the breath freshening effect is remarkably improved along with the increase of the addition amount of the food-grade activated carbon.

4. Tooth wear test

1) Test sample

Experimental groups: examples 1 to 5; control group: comparative examples 1 to 3

2) Testing instrument

Tooth brushing machine, hydroxyapatite sheet and one ten thousandth balance

3) Test method

Taking sixteen hydroxyapatite sheets with the same size and weight, randomly dividing the hydroxyapatite sheets into eight groups, randomly testing the weight of each group of two hydroxyapatite sheets by using a one-ten-thousandth balance, recording the weight of each group of two hydroxyapatite sheets, numbering the hydroxyapatite sheets, fixing the hydroxyapatite sheets on a tooth brushing machine, adding 5g of test dentifrice and 5g of water into each tooth brushing groove, using the same formula dentifrice for the hydroxyapatite sheets in the same group, using the same brush-hair toothbrush to perform tooth brushing test on the hydroxyapatite sheets on the tooth brushing machine, simulating tooth brushing for 1200 times, taking out the brushed hydroxyapatite sheets, cleaning, drying, weighing, calculating the weight difference between the hydroxyapatite sheets before brushing and after brushing, and calculating the average value of the two hydroxyapatite sheets so as to measure the wear conditions of different dentifrices. The test results are shown in table 4 below.

4) Test results

TABLE 4 hydroxyapatite plate abrasion results

As can be seen from the tooth abrasion test, the tooth abrasion value of the dentifrice prepared in the example was lower than that of the dentifrice prepared in comparative example 1, and the abrasion value decreased significantly as the amount of food grade activated carbon added was increased.

The technical contents of the present invention are further illustrated by the examples, so as to facilitate the understanding of the reader, but the embodiments of the present invention are not limited thereto, and any technical extension or re-creation based on the present invention is protected by the present invention.

Claims (8)

1. The dentifrice for removing stains and refreshing breath is characterized by comprising the following components in percentage by mass:

the composite friction agent consists of activated carbon and a second friction component, wherein the second friction component is selected from at least one of silicon dioxide, calcium carbonate and calcium hydrophosphate dihydrate;

the foaming agent is selected from at least one of cocamidopropyl betaine, lauryl glucoside and coco glucoside.

2. The dentifrice for stain removal and breath freshening as claimed in claim 1 further comprising 0.2-0.8% by weight of a flavor.

3. The dentifrice for removing stains and refreshing breath as claimed in claim 1, wherein the mass ratio of the activated carbon to the second friction component in the composite abrasive is 9: 1-171.

4. A dentifrice for stain removal and breath freshening as claimed in claim 1 in which the activated carbon has an adsorption of methylene blue greater than 150mg/g and an adsorption of carbon tetrachloride greater than 500 mg/g.

5. The dentifrice of claim 4, wherein the activated carbon is food grade activated carbon in a powder form and is made of fruit shell and wood chips.

6. A dentifrice for stain removal and breath freshening as claimed in claim 1 in which the humectant is selected from at least one of sorbitol, glycerin, polyethylene glycol, propylene glycol.

7. A method of preparing a dentifrice for stain removal and breath freshening as claimed in claim 1 comprising the steps of:

s1, adding the water-soluble material into water, and uniformly stirring to obtain a mixed solution;

s2, uniformly mixing the materials for forming the composite friction agent to obtain mixed powder;

s3, adding the mixed solution into the mixed powder through a sprayer, starting stirring simultaneously, and uniformly mixing the components to obtain a mixture;

and S4, grinding the mixture by a grinder to obtain the dentifrice after uniform grinding.

8. The method according to claim 7, wherein the dentifrice further comprises 0.2 to 0.8% by mass of an essence, and the step of adding the essence to the mixture and uniformly mixing the essence and the mixture in the step S1.