阅读说明：本技术 一种抗敏感牙膏及其制备方法 (Anti-allergy toothpaste and preparation method thereof ) 是由 江孝亮 何炳梁 于 2021-09-29 设计创作，主要内容包括：本发明公开了一种抗敏感牙膏及其制备方法,抗敏感牙膏由以下重量份的组分制备而成：保湿剂28-42份、润湿剂0.5-2.5份、粘合剂0.1-0.7份、成膜剂0.1-0.7份、羟基磷灰石2-12份、硝酸钾1-5份、凝血酸0.01-0.15份、乳化剂0.2-0.8份、单氟磷酸钠0.24-1.21份、清洁型水合硅石2-10份、增稠型水合硅石2-8份、甜味剂0.10-0.35份、防腐剂0.15-0.30份、摩擦剂0.1-0.3份、表面活性剂1.2-3.2份、发泡剂0.2-0.7份、香精0.4-1.5份以及溶剂29-40份,抗过敏效果良好。(The invention discloses anti-allergy toothpaste and a preparation method thereof, wherein the anti-allergy toothpaste is prepared from the following components in parts by weight: 28-42 parts of humectant, 0.5-2.5 parts of wetting agent, 0.1-0.7 part of adhesive, 0.1-0.7 part of film forming agent, 2-12 parts of hydroxyapatite, 1-5 parts of potassium nitrate, 0.01-0.15 part of tranexamic acid, 0.2-0.8 part of emulsifier, 0.24-1.21 part of sodium monofluorophosphate, 2-10 parts of clean hydrated silica, 2-8 parts of thickening hydrated silica, 0.10-0.35 part of sweetener, 0.15-0.30 part of preservative, 0.1-0.3 part of abrasive, 1.2-3.2 parts of surfactant, 0.2-0.7 part of foaming agent, 0.4-1.5 part of essence and 29-40 parts of solvent, and has good antiallergic effect.)

1. The anti-allergy toothpaste is characterized by being prepared from the following components in parts by weight: 28-42 parts of humectant, 0.5-2.5 parts of wetting agent, 0.1-0.7 part of adhesive, 0.1-0.7 part of film forming agent, 2-12 parts of hydroxyapatite, 1-5 parts of potassium nitrate, 0.01-0.15 part of tranexamic acid, 0.2-0.8 part of emulsifier, 0.24-1.21 part of sodium monofluorophosphate, 2-10 parts of clean hydrated silica, 2-8 parts of thickening hydrated silica, 0.10-0.35 part of sweetener, 0.15-0.30 part of preservative, 0.1-0.3 part of abrasive, 1.2-3.2 parts of surfactant, 0.2-0.7 part of foaming agent, 0.4-1.5 part of essence and 29-40 parts of solvent.

2. The anti-sensitivity toothpaste according to claim 1, which is prepared from the following components in parts by weight: 36 parts of humectant, 2 parts of humectant, 0.45 part of adhesive, 0.4 part of film forming agent, 8 parts of hydroxyapatite, 3 parts of potassium nitrate, 0.1 part of tranexamic acid, 0.5 part of emulsifier, 0.76 part of sodium monofluorophosphate, 7 parts of clean hydrated silica, 6 parts of thickening hydrated silica, 0.22 part of sweetening agent, 0.25 part of preservative, 0.2 part of abrasive, 2.2 parts of surfactant, 0.5 part of foaming agent, 1.2 parts of essence and 32 parts of solvent.

3. The anti-sensitivity toothpaste according to claim 1 or 2, wherein the humectant consists of 20 to 30 parts by mass of sorbitol and 8 to 12 parts by mass of glycerin

4. The anti-sensitivity toothpaste according to claim 3, wherein the binder is cellulose gum, the film-forming agent is guar gum, the emulsifier is tetrasodium pyrophosphate, the sweetener is sodium saccharin, the preservative is sodium benzoate, the abrasive is silica, the surfactant is sodium lauryl sulfate, the foaming agent is sodium lauroyl sarcosinate, and the wetting agent is polyethylene glycol-8.

5. A method of preparing an anti-sensitivity toothpaste according to claim 1 comprising the steps of:

uniformly mixing a solvent, a humectant, a wetting agent, potassium nitrate, tranexamic acid, an emulsifier, sodium monofluorophosphate, a sweetening agent and a preservative, and then placing the mixture in a vacuum environment of-0.07 MPa to-0.08 MPa;

adding an adhesive, a friction agent, a surfactant, a film forming agent, hydroxyapatite, clean hydrated silica and thickening hydrated silica into the powder, stirring the mixture at the same time, and after the powder is added, continuously stirring the mixture for 25 to 30 minutes and simultaneously improving the vacuum degree;

when the vacuum degree is-0.092 MPa to-0.08 MPa, stopping stirring, adding essence and foaming agent, and stirring for 5-10 minutes;

degassing for 15-30 min, and discharging gas until the vacuum degree is 0 when the vacuum degree is less than or equal to-0.092 MPa to obtain the anti-allergy toothpaste.

6. The method of claim 5, wherein the temperature during the preparation of the anti-sensitivity toothpaste is 45 ℃ or less.

7. The method according to claim 5, wherein the degree of vacuum at which the essence is added is-0.085 MPa.

8. The method of claim 5, wherein the degassing time is 20 minutes.

9. The method of claim 6, wherein the temperature during the preparation of the anti-sensitivity toothpaste is 30 ℃.

Technical Field

The invention belongs to the technical field of oral care, and particularly relates to anti-allergy toothpaste and a preparation method thereof.

Background

Toothpaste is the most frequently used oral cavity cleaning and nursing product which is the most convenient and effective in people's life, and with the increase of age, gingival tissue begins to shrink, thereby causes the dentin to expose and arouses the hypersensitive symptom of tooth, causes the tooth pain, has the component that changes the abrasive substance among the prior art to reduce the wearing and tearing of friction to the tooth, thereby avoids the serious and anaphylaxis that leads to of tooth wearing and tearing, also has the pore of the tubule that adopts the dentin opening of closing, thereby stops the sense of ache, specifically is: strontium salt is neutral salt, strontium has strong adsorbability to all calcified tissues including dentin, and strontium has an effect of improving dentin hypersensitivity by blocking open dentin tubules in the form of strontium calcium apatite; potassium nitrate has also been used to alter the stimulated endodontic nerve valves to reduce nerve activity; however, the antiallergic ingredients in the toothpastes are single and the effect is not obvious.

Disclosure of Invention

Aiming at the problems of single component and unobvious effect of the existing antiallergic toothpaste, the invention provides the antiallergic toothpaste and the preparation method thereof.

The technical scheme of the invention is as follows: an anti-allergy toothpaste is prepared from the following components in parts by weight: 28-42 parts of humectant, 0.5-2.5 parts of wetting agent, 0.1-0.7 part of adhesive, 0.1-0.7 part of film forming agent, 2-12 parts of hydroxyapatite, 1-5 parts of potassium nitrate, 0.01-0.15 part of tranexamic acid, 0.2-0.8 part of emulsifier, 0.24-1.21 part of sodium monofluorophosphate, 2-10 parts of clean hydrated silica, 2-8 parts of thickening hydrated silica, 0.10-0.35 part of sweetener, 0.15-0.30 part of preservative, 0.1-0.3 part of abrasive, 1.2-3.2 parts of surfactant, 0.2-0.7 part of foaming agent, 0.4-1.5 part of essence and 29-40 parts of solvent.

Further limited, the anti-allergy toothpaste is prepared from the following components in parts by weight: 36 parts of humectant, 2 parts of humectant, 0.45 part of adhesive, 0.4 part of film forming agent, 8 parts of hydroxyapatite, 3 parts of potassium nitrate, 0.1 part of tranexamic acid, 0.5 part of emulsifier, 0.76 part of sodium monofluorophosphate, 7 parts of clean hydrated silica, 6 parts of thickening hydrated silica, 0.22 part of sweetening agent, 0.25 part of preservative, 0.2 part of abrasive, 2.2 parts of surfactant, 0.5 part of foaming agent, 1.2 parts of essence and 32 parts of solvent.

The humectant is further limited to be composed of 20-30 parts by mass of sorbitol and 8-12 parts by mass of glycerin.

Further defined, the binder is a cellulose gum, the film-forming agent is guar gum, the emulsifier is tetrasodium pyrophosphate, the sweetener is sodium saccharin, the preservative is sodium benzoate, the abrasive is silicon dioxide, the surfactant is sodium lauryl sulfate, the foaming agent is sodium lauroyl sarcosinate, and the wetting agent is polyethylene glycol-8.

The invention also discloses a preparation method of the anti-allergy toothpaste, which comprises the following steps:

uniformly mixing a solvent, a humectant, a wetting agent, potassium nitrate, tranexamic acid, an emulsifier, sodium monofluorophosphate, a sweetening agent and a preservative, and then placing the mixture in a vacuum environment of-0.07 MPa to-0.08 MPa;

adding an adhesive, a friction agent, a surfactant, a film forming agent, hydroxyapatite, clean hydrated silica and thickening hydrated silica into the powder, stirring the mixture at the same time, and after the powder is added, continuously stirring the mixture for 25 to 30 minutes and simultaneously improving the vacuum degree;

when the vacuum degree is-0.092 MPa to-0.08 MPa, stopping stirring, adding essence and foaming agent, and stirring for 5-10 minutes;

degassing for 15-30 min, and discharging gas until the vacuum degree is 0 when the vacuum degree is less than or equal to-0.092 MPa to obtain the anti-allergy toothpaste.

Further limiting, the temperature in the process of preparing the anti-allergy toothpaste is less than or equal to 45 ℃.

Further limiting, the vacuum degree is-0.085 MPa when the essence is added.

Further defined, the degassing time was 20 minutes.

Further defined, the temperature during the preparation of the anti-sensitivity toothpaste was 30 ℃.

Has the advantages that: in the anti-allergic toothpaste disclosed by the invention, hydroxyapatite is used for plugging enamel dental tubules, potassium nitrate is used for changing the dental pulp nerve stimulated valve to weaken nerve activity to block nerve response, and the two synergistically act to achieve an anti-allergic effect; the hydroxyapatite has excellent biocompatibility, can be used as an induction factor of bones or teeth, and has a good remineralization effect on the teeth; the hydroxyapatite has good biocompatibility and high affinity with enamel, and the mineralized liquid can effectively form remineralization deposition, thereby achieving the effect of plugging the dental tubules and playing the anti-allergy role.

Drawings

FIG. 1 is an under-mirror image of the control non-treated area;

FIG. 2 is an under-the-mirror image of the control treatment zone;

FIG. 3 is an under-mirror image of the non-treated area of the experimental group;

FIG. 4 is an under-the-mirror image of the treatment zone of the experimental group.

Detailed Description

In the following examples 1 to 4, the powder was: binders, abrasives, surfactants, film formers, hydroxyapatite, cleaning hydrated silica, and thickening hydrated silica, or their progeny;

the liquid phase is as follows: a solvent, a humectant, a wetting agent, potassium nitrate, tranexamic acid, an emulsifier, sodium monofluorophosphate, a sweetener, a preservative, or a combination thereof.

Example 1

This example was carried out in a toothpaste maker, model ZG1300, dedicated to the preparation of toothpaste.

The anti-allergy toothpaste is prepared by the following specific steps:

s1, weighing 200kg of sorbitol, 80kg of glycerol, 85 kg of polyethylene glycol, 1kg of cellulose gum, 1kg of guar gum, 20kg of hydroxyapatite, 10kg of potassium nitrate, 0.1kg of tranexamic acid, 2kg of tetrasodium pyrophosphate, 2.4kg of sodium monofluorophosphate, 20kg of clean hydrated silica, 20kg of thickening hydrated silica, 1kg of saccharin sodium, 1.5kg of sodium benzoate, 2kg of silicon dioxide, 12kg of sodium lauryl sulfate, 2kg of sodium lauroyl sarcosinate, 4kg of essence and 290kg of water;

s2, adding water into a pre-dispersion pot, and adding a liquid-phase raw material to obtain a liquid-phase mixed solution;

s3, opening vacuum to-0.04 MPa, sucking liquid phase mixed liquid, and opening a scraper and stirring;

s4, feeding powder to a feeding hole, and keeping stirring in the feeding process;

s5, when the vacuum is increased to-0.07 MPa, opening a scraper and double stirring, starting a powder tank to stir when powder is sucked, continuing stirring for 25 minutes after the powder is sucked, and gradually increasing the vacuum degree (taking no top rushing as a principle);

s6, stopping stirring and scraping when the vacuum degree is increased to-0.092 MPa, closing the vacuumizing switch, and sucking essence;

s7, opening double stirring and scraping knives after the essence is fed, opening a vacuum pump switch, and maintaining for 5 min;

s8, stopping double stirring, maintaining the stirring of a scraper, and beginning degassing for at least 15 min;

and S9, when the vacuum degree is equal to-0.092 MPa, deflating until the vacuum degree is zero.

In the preparation process, when the temperature of the paste making machine exceeds 45 ℃, cooling water is started to cool, and the temperature of the paste is maintained to be not more than 45 ℃.

Example 2

This example was carried out in a toothpaste maker, model ZG1300, dedicated to the preparation of toothpaste.

The anti-allergy toothpaste is prepared by the following specific steps:

s1, weighing 250kg of sorbitol, 100kg of glycerol, 820 kg of polyethylene glycol, 3kg of cellulose gum, 5kg of guar gum, 50kg of hydroxyapatite, 25kg of potassium nitrate, 0.3kg of tranexamic acid, 6kg of tetrasodium pyrophosphate, 8.3kg of sodium monofluorophosphate, 55kg of clean hydrated silica, 61kg of thickening hydrated silica, 2.5kg of saccharin sodium, 2.3kg of sodium benzoate, 2kg of silicon dioxide, 21kg of sodium lauryl sulfate, 5kg of sodium lauroyl sarcosinate, 6kg of essence and 340kg of water;

s2, adding water into a pre-dispersion pot, and adding a liquid-phase raw material to obtain a liquid-phase mixed solution;

s3, opening vacuum to-0.05 MPa, sucking liquid phase mixed liquor, and opening a scraper and stirring;

s4, feeding powder to a feeding hole, and keeping stirring in the feeding process;

s5, when the vacuum is increased to-0.08 MPa, opening a scraper and double stirring, starting a powder tank for stirring when powder is sucked, continuing stirring for 30 minutes after the powder is sucked, and gradually increasing the vacuum degree (by using no top rushing as a principle);

s6, stopping double stirring and scrapers when the vacuum degree is increased to-0.08 MPa, closing a vacuumizing switch, and sucking essence and foaming agent;

s7, opening double stirring and scraping knives after the essence is fed, opening a vacuum pump switch, and maintaining for 8 min;

s8, stopping double stirring, maintaining the stirring of a scraper, and beginning to degas for at least 27 min;

and S9, when the vacuum degree is equal to-0.012 MPa, deflating until the vacuum degree is zero.

In the preparation process, when the temperature of the paste making machine exceeds 45 ℃, cooling water is started to cool, and the temperature of the paste is maintained to be not more than 45 ℃.

Example 3

This example was carried out in a toothpaste maker, model ZG1300, dedicated to the preparation of toothpaste.

The anti-allergy toothpaste is prepared by the following specific steps:

s1, weighing 300kg of sorbitol, 120kg of glycerol, 825 kg of polyethylene glycol, 7kg of cellulose gum, 7kg of guar gum, 120kg of hydroxyapatite, 50kg of potassium nitrate, 1.5kg of tranexamic acid, 8kg of tetrasodium pyrophosphate, 12.1kg of sodium monofluorophosphate, 100kg of clean hydrated silica, 80kg of thickening hydrated silica, 3.5kg of saccharin sodium, 3kg of sodium benzoate, 3kg of silicon dioxide, 32kg of sodium lauryl sulfate, 7kg of sodium lauroyl sarcosinate, 15kg of essence and 400kg of water;

s2, adding water into a pre-dispersion pot, and adding a liquid-phase raw material to obtain a liquid-phase mixed solution;

s3, opening vacuum to-0.05 MPa, sucking liquid phase mixed liquor, and opening a scraper and stirring;

s4, feeding powder to a feeding hole, and keeping stirring in the feeding process;

s5, when the vacuum is increased to-0.08 MPa, opening a scraper and double stirring, starting a powder tank for stirring when powder is sucked, continuing stirring for 30 minutes after the powder is sucked, and gradually increasing the vacuum degree (by using no top rushing as a principle);

s6, stopping double stirring and scrapers when the vacuum degree is increased to-0.08 MPa, closing a vacuumizing switch, and sucking essence and foaming agent;

s7, opening double stirring and scraping knives after the essence is fed, opening a vacuum pump switch, and maintaining for 10 min;

s8, stopping double stirring, maintaining the stirring of a scraper, and beginning to degas for at least 27 min;

and S9, when the vacuum degree is equal to-0.015 MPa, deflating until the vacuum degree is zero.

In the preparation process, when the temperature of the paste making machine exceeds 45 ℃, cooling water is started to cool, and the temperature of the paste is maintained to be not more than 45 ℃.

Example 4

This example was carried out in a toothpaste maker, model ZG1300, dedicated to the preparation of toothpaste.

The anti-allergy toothpaste is prepared by the following specific steps:

s1, weighing 260kg of sorbitol, 90kg of glycerol, 820 kg of polyethylene glycol, 4.5kg of cellulose gum, 4kg of guar gum, 80kg of hydroxyapatite, 30kg of potassium nitrate, 1kg of tranexamic acid, 5kg of tetrasodium pyrophosphate, 7.6kg of sodium monofluorophosphate, 70kg of clean hydrated silica, 60kg of thickening hydrated silica, 2.2kg of saccharin sodium, 2.5kg of sodium benzoate, 3kg of silicon dioxide, 22kg of sodium lauryl sulfate, 5kg of sodium lauroyl sarcosinate, 1.5kg of essence and 320kg of water;

s2, adding water into a pre-dispersion pot, and adding a liquid-phase raw material to obtain a liquid-phase mixed solution;

s3, opening vacuum to-0.05 MPa, sucking liquid phase mixed liquor, and opening a scraper and stirring;

s4, feeding powder to a feeding hole, and keeping stirring in the feeding process;

s5, when the vacuum is increased to-0.08 MPa, opening a scraper and double stirring, starting a powder tank for stirring when powder is sucked, continuing stirring for 30 minutes after the powder is sucked, and gradually increasing the vacuum degree (by using no top rushing as a principle);

s6, stopping double stirring and scrapers when the vacuum degree is increased to-0.08 MPa, closing a vacuumizing switch, and sucking essence and foaming agent;

s7, opening double stirring and scraping knives after the essence is fed, opening a vacuum pump switch, and maintaining for 10 min;

s8, stopping double stirring, maintaining the stirring of a scraper, and beginning to degas for at least 27 min;

and S9, when the vacuum degree is equal to-0.015 MPa, deflating until the vacuum degree is zero.

In the preparation process, when the temperature of the paste making machine exceeds 45 ℃, cooling water is started to cool, and the temperature of the paste is maintained to be not more than 45 ℃.

Comparative example 1

In comparison to example 4, the comparative example lacks hydroxyapatite and is otherwise identical.

The anti-sensitivity toothpastes prepared in example 4 and comparative example 1 were evaluated for the occlusion effect of the tubules, as follows.

1. Stadium sample

Test subjects (experimental group): example 4 anti-sensitivity toothpaste prepared

Control (control group): comparative example 1

2. Experimental methods

1) Preparing a dentin sample: fresh extracted bovine incisors are cut and polished to prepare 12 dentin blocks with the size of about 5mm multiplied by 5mmx2mm, the dentin blocks are corroded for 20 minutes by 40% orthophosphoric acid, then corroded for 5 minutes by 5% sodium hypochlorite after being washed, and finally ultrasonically cleaned for 20 minutes by deionized water. Observation under a polarized light microscope ensured adequate exposure of the dentinal tubules.

2) Grouping: 12 dentin samples were randomly assigned to the negative control group and the experimental group, with 6 samples per group.

3) Partitioning: one half of the area (about 5mmx2.5mm) of the dentin sample was taped as a non-treated area, and the other half (about 5mmx2.5mm) was used as an experimental treated area.

4) Preparation of test anti-sensitivity toothpaste: weighing toothpaste and deionized water at a certain weight ratio of 1:1.6 (anti-allergic toothpaste: water), stirring with a glass rod to disperse toothpaste, and stirring with a magnetic stirrer to obtain homogenate for use.

5) And (3) dentin circulation treatment: the negative control group was treated with a control and the experimental group was treated with a test substance. Brushing teeth for 3 min by using a tooth brushing machine, then fully cleaning with deionized water, then soaking in artificial saliva, and preserving heat at 37 ℃ for 55 min. Brushing was repeated for 3 minutes, followed by thorough rinsing with deionized water, followed by immersion in artificial saliva at 37 ℃ overnight. The experiment was repeated for 3 days.

6) And (3) drying: the dentin samples after the circulation treatment were dried in an oven at 25 ℃ for 24 h.

7) Observation by a scanning electron microscope: the dried dentin was sprayed with gold, and then observed under a scanning electron microscope, and three visual fields (2000 times) were respectively taken in each of the treated area and the non-treated area, and the exposed dentin tubules were counted C.

8) Calculate each group dentinal tubule plugging rate R (%):

3. laboratory apparatus

Low Speed precision cutting machine (ISOMET Low Speed Saw), grinding and polishing machine (Metaserv 250), automatic mechanical tooth brushing machine (V-8), Low vacuum thermal field emission scanning electron microscope (GeminiSEM 300)

4. Evaluation method

The independent sample 1 is adopted for testing, the plugging rate R (%) of the dentinal tubules of the experimental group and the negative control group is compared, the test level a-0.05 experimental group is compared with the negative control group, the P value is less than 0.05, the obvious difference exists, and the effect of plugging the dentinal tubules by the test object is considered to be better than that of the negative control group.

5 test data and statistical results

FIG. 1 shows the under-mirror image of the non-treated region of the control group, FIG. 2 shows the under-mirror image of the treated region of the control group, FIG. 3 shows the under-mirror image of the non-treated region of the experimental group, and FIG. 4 shows the under-mirror image of the treated region of the experimental group; the statistical results are shown in table 1.

TABLE 1 dentinal tubule occlusion Rate R (%)

6. Conclusion

As can be seen from table 1 and fig. 1-4, the anti-sensitivity toothpaste prepared in example 4 has a higher plugging rate for dentinal tubules than the control group, and has significant difference (P <0.05), which indicates that the anti-sensitivity toothpaste prepared in example 4 has significant plugging effect for dentinal tubules.

Finally, it should be noted that: the above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.