阅读说明：本技术 一种增强氟活性的抗敏感牙膏 (Anti-allergy toothpaste capable of enhancing fluorine activity ) 是由 唐伟月 张环 邓全富 董海德 刘莉 邓嵘 于 2021-01-28 设计创作，主要内容包括：本发明涉及口腔护理用品技术领域,具体涉及一种增强氟活性的抗敏感牙膏,原料包括摩擦剂、增稠剂、氟化物和缓冲剂；所述缓冲剂包括碳酸氢钠和碳酸钠。本方案可以解决现有技术中的碳酸钙基质的含氟牙膏中可溶氟不稳定的技术问题,提高了氟在牙膏中的长效活性,进一步推动了含氟牙膏在抗牙敏感和防龋齿上的广泛应用。(The invention relates to the technical field of oral care products, in particular to anti-sensitivity toothpaste for enhancing fluorine activity, which comprises raw materials of an abrasive, a thickening agent, fluoride and a buffering agent; the buffer includes sodium bicarbonate and sodium carbonate. The proposal can solve the technical problem of unstable soluble fluorine in the fluorine-containing toothpaste with calcium carbonate matrix in the prior art, improve the long-acting activity of fluorine in the toothpaste and further promote the wide application of the fluorine-containing toothpaste in tooth sensitivity resistance and dental caries prevention.)

1. An anti-sensitivity toothpaste for enhancing fluorine activity is characterized in that the raw materials comprise an abrasive, a thickening agent, fluoride and a buffering agent; the buffer includes sodium bicarbonate and sodium carbonate.

2. The fluorine activity enhancing anti-sensitivity toothpaste according to claim 1, wherein the abrasive comprises 30 to 45 mass% of calcium carbonate and/or 1 to 3 mass% of hydrated silica.

3. The anti-sensitivity toothpaste for enhancing fluorine activity according to claim 2, wherein the mass fraction of the fluoride is 0.38-1.1%.

4. The anti-sensitivity toothpaste capable of enhancing fluorine activity according to claim 3, wherein the mass fraction of sodium bicarbonate is 0.3-0.6%, and the mass fraction of sodium carbonate is 0.6-1.2%.

5. The anti-sensitivity toothpaste capable of enhancing fluorine activity according to claim 4, wherein the thickening agent comprises sodium carboxymethylcellulose and xanthan gum in a mass ratio of 6-10: 3.

6. The fluorine activity enhancing anti-sensitivity toothpaste according to claim 5, wherein the thickening agent further comprises carbomer.

7. The anti-sensitivity toothpaste capable of enhancing fluorine activity according to claim 6, wherein the raw materials further comprise 0.1-5% by weight of potassium salt.

8. The fluoride-activity-enhancing anti-sensitivity toothpaste as claimed in claim 7, wherein the potassium salt is potassium nitrate and the fluoride compound is sodium monofluorophosphate.

9. The anti-sensitivity toothpaste capable of enhancing fluorine activity according to claim 8, wherein the raw materials further comprise humectant, surfactant, stabilizer, sweetener and essence; the humectant comprises at least one of glycerol, sorbitol, PEG-6, PEG-8 and PEG-32; the surfactant comprises sodium lauryl sulfate and/or N-acyl sarcosine sodium; the stabilizer comprises sodium nitrate and/or sodium pyrophosphate; the sweetener comprises saccharin sodium and/or sucralose; the essence comprises mint and/or menthol.

10. The desensitizing dentifrice of claim 9, wherein said desensitizing dentifrice is prepared by a process comprising:

s1: mixing carbomer with hydrated silicon dioxide to obtain a mixture I;

s2: adding the mixture I into glycerol, and uniformly mixing to obtain a mixture II;

s3: adding the humectant except the glycerin and the thickener except the carbomer into the mixture II, and uniformly stirring to obtain a mixture III;

s4: adding a sweetening agent, potassium salt, fluoride, a buffering agent, a stabilizing agent, calcium carbonate and water into the mixture III, and uniformly stirring to obtain a mixture IV;

s5: and adding a surfactant and the essence into the mixture IV, homogenizing and stirring, and performing vacuum degassing to obtain a paste.

Technical Field

The invention relates to the technical field of oral care products, in particular to anti-sensitivity toothpaste capable of enhancing fluorine activity.

Background

According to the authoritative statistics of the world health organization (WTO), more than 70% of people in the world suffer from different oral problems, including caries, dentin sensitivity, gingival bleeding, periodontitis and the like. The dentine sensitivity is a common easy-to-send and multiple disease in oral diseases and is one of the clinically common causes of toothache. Dentine sensitivity is clinically manifested as tooth soreness and pain caused by the action of external temperature and physical and chemical substances.

The fluoride can improve acid resistance of dental tissue in dental treatment, inhibit acid dissolution of dentin, prevent opening of more dentin tubules, and promote remineralization of dentin tubules. Fluoride is used as a common anticarious agent, and fluoride ions can be combined with hydroxyapatite in an enamel structure to promote remineralization of a carious lesion and reduce exposure of dentin. The principle of anti-dentin sensitivity of fluorine-containing toothpaste is to enhance the enamel structure through soluble fluorine/free fluorine in the toothpaste so as to achieve the purpose of reducing dental caries and reducing exposure of dentin. Thus, the amount of soluble/free fluorine content in the toothpaste determines the anti-sensitivity effect. During the long-term storage of the calcium carbonate-based toothpaste, a small amount of calcium ions decomposed from the calcium carbonate are easy to react with fluoride to generate calcium fluoride, so that the fluoride is inactivated. In addition, the carbon dioxide gas generated by the reaction can cause unstable phenomena such as water separation and gas expansion of the paste.

Disclosure of Invention

The invention aims to provide anti-sensitivity toothpaste capable of enhancing fluorine activity so as to solve the technical problem that soluble fluorine in fluorine-containing toothpaste in the prior art is unstable.

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

an anti-allergic toothpaste for enhancing fluorine activity comprises abrasive, thickener, fluoride and buffer; the buffer includes sodium bicarbonate and sodium carbonate.

The principle and the advantages of the scheme are as follows: fluoride has poor long-term stability in calcium carbonate based toothpastes, with a gradual reduction in the soluble/free fluorine in the toothpaste over time, which is critical to achieving anticaries, anti-sensitivity. The inventors have conducted extensive studies on the ingredients of toothpastes and have found that the addition of specific buffering agents to a calcium carbonate based toothpaste maintains the long term stability of soluble fluorine in the toothpaste. While this particular buffer comprises sodium bicarbonate and sodium carbonate, the fluorine-containing species in an environment containing sodium carbonate and sodium bicarbonate, the soluble fluorine does not bind in significant amounts to the calcium ions in calcium carbonate and is available for long term presence and activity in the toothpaste. The inventors have tried other buffering agents (for example, disodium hydrogen phosphate, sodium dihydrogen phosphate, etc.), and found that the addition of other buffering agent pairs does not maintain the long-term stability of soluble fluorine in the toothpaste, and also deteriorates the stability of the appearance of the paste, and causes moisture and oil separation after long-term storage. The inventors further analyzed the occurrence of the above phenomenon in that the use of a buffer consisting of sodium carbonate and sodium bicarbonate reduced the formation of calcium ions in the toothpaste, such that the concentration of calcium and fluoride ions in the toothpaste was less than the solubility product Ksp [ CaF ] required for the formation of calcium fluoride precipitates₂]Therefore, the content of soluble fluorine is maintained to the maximum extent, and the activity of fluoride is further improved.

In conclusion, the toothpaste of the scheme solves the technical problem of unstable soluble fluorine in the fluorine-containing toothpaste in the prior art, improves the long-acting activity of fluorine in the toothpaste, and further promotes the wide application of the fluorine-containing toothpaste in tooth sensitivity resistance and dental caries prevention.

Further, the rubbing agent comprises 30-45% by mass of calcium carbonate and/or 1-3% by mass of hydrated silicon dioxide.

By adopting the technical scheme, the calcium carbonate and the hydrated silicon dioxide are common abrasive agents in the toothpaste, and can be used together with the toothbrush to wipe off tartar on the surface of teeth and relieve tooth stain, dental plaque, dental calculus and the like.

Further, the mass fraction of the fluoride is 0.38% -1.1%.

By adopting the technical scheme, after the fluoride is added, when the oral cavity anti-caries anti-allergy liquid is used, the content of soluble fluorine/free fluorine in the oral cavity is 500 ppm-1000 ppm, and the anti-caries and anti-allergy effects can be effectively realized.

Further, the mass fraction of the sodium bicarbonate is 0.3-0.6%, and the mass fraction of the sodium carbonate is 0.6-1.2%.

By adopting the technical scheme, the mass fraction of the sodium bicarbonate is maintained at 0.3-0.6%, the mass fraction of the sodium carbonate is maintained at 0.6-1.2%, and the stability and the activity of the soluble fluorine can be maintained to the maximum extent. Although the buffer pair formed by sodium bicarbonate and sodium carbonate can improve the stability of fluoride ions, the selection of the content of the two substances also has a great influence on the toothpaste. The concentration of the sodium bicarbonate and the sodium carbonate is too low, although the effect of stabilizing the appearance of the paste can be achieved, the factors influencing the activity of the fluoride ions cannot be eliminated sufficiently, and the effect of stabilizing the soluble fluorine can be achieved only if the content of the two substances exceeds a certain threshold. If the contents of the two substances are too high, the pH value of the paste body is too high, which exceeds the requirement of the national standard GB 8372-2017 of the toothpaste that the pH value range of the toothpaste is 5.5-10.5.

Further, the thickening agent comprises sodium carboxymethylcellulose and xanthan gum in a mass ratio of 6-10: 3.

By adopting the technical scheme, the sodium carboxymethylcellulose and the xanthan gum in the proportion are used as the thickening agents, so that the activity of soluble fluorine can be prevented from being reduced, and the appearance stability of the whole paste can be maintained.

Further, the thickener also comprises carbomer.

By adopting the technical scheme, the carbomer can improve the residence of fluorine in the oral cavity and enhance the anti-sensitivity effect of the fluorine.

Furthermore, the raw materials of the anti-allergy toothpaste also comprise 0.1 to 5 mass percent of potassium salt.

By adopting the technical scheme, the potassium ions can depolarize the exposed dental pulp nerves, reduce the excitability of the dental pulp nerve fibers and relieve the dentin sensitivity symptom. The anti-allergy functional ingredients with different mechanisms are combined and added with better anti-allergy synergistic effect. In most anti-sensitivity toothpastes, the two special anti-sensitivity ingredients widely used are mainly potassium nitrate and strontium chloride. The inventor combines fluoride and potassium salt, and utilizes the synergistic effect of the two desensitizing components to more effectively reduce and prevent the tooth sensitivity of patients.

Further, the potassium salt is potassium nitrate, and the fluoride is sodium monofluorophosphate.

By adopting the technical scheme, the potassium nitrate and the sodium monofluorophosphate are common substances in the toothpaste, and have stable property and good safety.

Furthermore, the raw materials of the anti-sensitive toothpaste also comprise a humectant, a surfactant, a stabilizer, a sweetening agent and essence; the humectant comprises at least one of glycerol, sorbitol, PEG-6, PEG-8 and PEG-32; the surfactant comprises sodium lauryl sulfate and/or N-acyl sarcosine sodium; the stabilizer comprises sodium nitrate and/or sodium pyrophosphate; the sweetener comprises saccharin sodium and/or sucralose; the essence comprises mint and/or menthol.

By adopting the technical scheme, the humectant, the surfactant, the stabilizer, the sweetener and the essence are all common substances in toothpaste, and can be used as raw materials to be added into the toothpaste, so that the quality of the toothpaste can be improved.

Further, the anti-sensitivity toothpaste is prepared by the following method:

s1: mixing carbomer with hydrated silicon dioxide to obtain a mixture I;

s2: adding the mixture I into glycerol, and uniformly mixing to obtain a mixture II;

s3: adding the humectant except the glycerin and the thickener except the carbomer into the mixture II, and uniformly stirring to obtain a mixture III;

s4: adding a sweetening agent, potassium salt, fluoride, a buffering agent, a stabilizing agent, calcium carbonate and water into the mixture III, and uniformly stirring to obtain a mixture IV;

s5: and adding a surfactant and the essence into the mixture IV, homogenizing and stirring, and performing vacuum degassing to obtain a paste.

By adopting the technical scheme, the anti-allergy toothpaste of the scheme can be prepared. Since silica is not readily dispersible, it needs to be mixed and dispersed with carbomer and glycerin first. The anti-allergic toothpaste can be prepared by the sequential adding and mixing processes and vacuum degassing.

Detailed Description

The following is further detailed by way of specific embodiments:

the overall situation of the technical scheme is as follows:

the anti-sensitivity toothpaste capable of enhancing the fluorine activity comprises the following raw material components: abrasives, thickeners, fluorides, potassium salts, buffering agents, humectants, surfactants, stabilizers, sweeteners, and flavors.

The potassium salt is preferably potassium nitrate, and the weight percentage of the potassium salt in the whole paste component is preferably 0.1-5%.

The fluoride is sodium monofluorophosphate, and the weight percentage of the fluoride in the whole paste component is preferably 0.38-1.1%.

The humectant is at least one of glycerol, sorbitol, PEG-6, PEG-8 and PEG-32. As a preferred technical scheme, the humectant comprises glycerin, sorbitol and PEG-6 components; the weight percentage of glycerin in the whole toothpaste is preferably 1-10%, the weight percentage of sorbitol in the whole toothpaste is preferably 15-45%, and the weight percentage of PEG-6 in the whole toothpaste is preferably 0.5-2%.

The abrasive is calcium carbonate and/or hydrated silica. The calcium carbonate is preferably present in an amount of 30% to 45% by weight of the overall toothpaste, and the hydrated silica is preferably present in an amount of 1% to 3% by weight of the overall toothpaste.

The thickener is at least one of sodium carboxymethylcellulose, xanthan gum and carbomer. As a preferable technical scheme, the thickening agent comprises two types of sodium carboxymethyl cellulose and xanthan gum, and the weight ratio of the sodium carboxymethyl cellulose to the xanthan gum is 6-10: 3. As a preferable technical scheme, the thickening agent comprises carbomer, sodium carboxymethylcellulose and xanthan gum, wherein the weight ratio of the sodium carboxymethylcellulose to the xanthan gum is 6-10: 3. The weight percentage of the thickening agent in the whole toothpaste is preferably 0.8-1.5%.

Surfactants include anionic and nonionic surfactants such as sodium lauryl sulfate, sodium N-acyl sarcosinate. The preferred weight percentage of surfactant in the overall toothpaste is 3%.

The essence can be herba Menthae, Mentholum, etc. The weight percentage of the essence in the whole toothpaste is preferably 0.8-1.5%.

The buffer is sodium carbonate and sodium bicarbonate. The buffer sodium carbonate is preferably used in an amount of 0.6 to 1.2% by weight of the entire toothpaste, and the buffer sodium bicarbonate is preferably used in an amount of 0.3 to 0.6% by weight of the entire toothpaste.

According to the formula, the method for preparing the anti-sensitivity toothpaste for enhancing the fluorine activity comprises the following steps:

s1: mixing carbomer with silicon dioxide to obtain a mixture I;

s2: adding the mixture I into glycerol, and uniformly mixing to obtain a mixture II;

s3: adding the humectant except the glycerin and the thickener except the carbomer into the mixture II, and uniformly stirring to obtain a mixture III;

s4: adding a sweetening agent, potassium salt, fluoride, a buffering agent, a stabilizing agent, calcium carbonate and water into the mixture III, and uniformly stirring to obtain a mixture IV;

s5: and adding a surfactant and the essence into the mixture IV, homogenizing and stirring, and performing vacuum degassing to obtain a paste.

Examples and comparative examples

The scheme of the present invention will now be described and verified by referring to specific examples and comparative examples, which are as follows: examples 1 to 4, comparative examples 1 to 12 were prepared according to the above-described protocol, and the formulations of examples 1 to 4 and comparative examples 1 to 12 are shown in tables 1 to 3.

Table 1: examples 1 to 4 technical parameters

Table 2: comparative examples 1 to 6 technical parameters

Table 3: comparative examples 7 to 12 technical parameters

The raw material of example 1 contains carbomer, and the specific process for preparing it is: dispersing and mixing a thickening agent carbomer and hydrated silicon dioxide to obtain a mixture for later use; adding glycerol into a container, adding the mixture, and uniformly stirring; adding the rest humectant and other thickening agents into a container and uniformly stirring; then adding a sweetening agent, potassium nitrate, sodium monofluorophosphate, sodium pyrophosphate, sodium carbonate, sodium bicarbonate, sodium nitrate, calcium carbonate and water, and uniformly stirring; adding surfactant and essence, homogenizing, stirring, vacuum degassing, and making into ointment. The raw material of example 2 does not contain carbomer, and the specific process for preparing the carbomer is as follows: adding glycerol and hydrated silicon dioxide into a container, and uniformly stirring; adding the rest humectant and thickener into the container, and stirring uniformly; then adding a sweetening agent, potassium nitrate, sodium monofluorophosphate, sodium pyrophosphate, sodium carbonate, sodium bicarbonate, sodium nitrate, calcium carbonate and water, and uniformly stirring; adding surfactant and essence, homogenizing, stirring, vacuum degassing, and making into ointment. The preparation processes of the remaining examples and comparative examples were carried out with reference to example 1 and example 2.

Experimental example 1: stability observation of anti-allergic toothpaste with enhanced fluorine activity

The stability of the examples and comparative examples was observed at room temperature and 45 ℃ and the results are shown in tables 4 and 5. The toothpaste pastes prepared in examples 1-4 were good in stability. According to the observation results of the comparative examples 1-4 and the comparative examples 1-6, the thickening agent used for the fluorine-active anti-sensitivity toothpaste is the sodium carboxymethyl cellulose and the xanthan gum which are compounded, and when the weight percentage of the sodium carboxymethyl cellulose to the xanthan gum is 6-10: 3, the appearance quality stability of the paste is normal, and the phenomenon of water and oil separation does not occur. According to the observation results of comparative examples 7 to 12, when the types of buffers used in the anti-sensitivity toothpaste for enhancing fluorine activity were sodium carbonate and sodium bicarbonate, the stability of the appearance quality of the paste was normal and no phenomenon of moisture and oil separation occurred.

Table 4: observation record of paste appearance stability

Table 5: observation record of appearance abnormality of paste

Experimental example 2: fluorine activity and stability test

The experimental method comprises the following steps: the soluble fluorine content of the examples and the comparative examples is determined by using the national standard GB/T8372-2017 toothpaste 5.8, and the total fluorine content of the examples and the comparative examples is determined according to the national standard GB/T8372-2017 toothpaste 5.9. Referring to Table 6, it can be seen that the soluble fluorine content of examples 1-4 did not decay over time, while the presence of elemental fluorine in the form of soluble fluorine in the toothpaste was the optimal active form, indicating that the fluoride in the experimental group 1-4 toothpastes retained fluorine activity in the form of soluble fluorine.

In terms of the buffer, comparative example 7 and comparative example 9 did not use sodium carbonate and sodium bicarbonate as the buffer, the content of sodium carbonate was too low in comparative example 8, the content of sodium bicarbonate was too low in comparative example 10, the contents of sodium carbonate and sodium bicarbonate were both low in comparative example 11, and the contents of sodium carbonate and sodium bicarbonate were too high in comparative example 12. The soluble fluorine content of the toothpastes prepared in the comparative examples 7 to 11 is attenuated to a certain extent along with the change of time, and the activity of fluoride is reduced along with the passage of time, so that the buffer consisting of sodium bicarbonate and sodium carbonate plays an important role in maintaining the fluorine activity and the soluble fluorine content, the soluble fluorine content of the toothpaste prepared in the comparative example 12 is not attenuated along with the change of time, but the pH value of the prepared toothpaste is too high to meet the requirement of the national standard GB 8372 and 2017 of the toothpaste. Therefore, the combination of 0.3 to 0.6 mass percent of sodium bicarbonate and 0.6 to 1.2 mass percent of sodium carbonate can obtain the best effect of stabilizing the fluorine activity and meet the requirement of the national standard GB 8372-2017 of toothpaste.

Table 6: stability test data of paste fluorine activity

The results of experiments in experimental example 1 and experimental example 2 were comprehensively analyzed, and in combination with the data of tables 4 to 6, the inventors added soluble fluorine to the calcium carbonate-based toothpaste during the development thereof to prepare a toothpaste having caries preventing and anti-sensitivity functions. However, in toothpastes based on calcium carbonate as the main base, the soluble fluorine is very unstable, so that the quality of such toothpastes is severely affected. To solve this problem, the inventors tried various methods such as changing the composition and ratio of ingredients in the toothpaste and finally found that the buffer is a key factor affecting the stability of soluble fluorine in the toothpaste based on calcium carbonate. The inventors have also tried various buffers, and found that only a buffer consisting of sodium carbonate and sodium bicarbonate can promote the maintenance of the stability of soluble fluorine, and that the above effects cannot be achieved by replacing other kinds of buffers (for example, disodium hydrogen phosphate and sodium dihydrogen phosphate, comparative examples 7 and 9).

Although the use of a suitable buffer pair solves the problem of free fluorine stability, a new problem arises in that the stability of the toothpaste itself is difficult to maintain with the addition of the buffer. The inventors have also attempted to modify the composition and proportions of the ingredients in the toothpaste to solve the above problems. Finally, it was surprisingly found that the choice of thickener is very important to improve the stability of the paste (toothpaste using sodium carbonate and sodium bicarbonate as buffering agents). The weight percentage of the sodium carboxymethylcellulose to the xanthan gum is 6-10: 3, so that the stabilizing effect on the paste can be realized. The paste stability cannot be effectively improved by using the thickening agent consisting of sodium carboxymethylcellulose and carrageenan (comparative example 1), the thickening agent content is too low (comparative example 2), the ratio of sodium carboxymethylcellulose is too high (comparative example 3), the thickening agent consisting of xanthan gum and carrageenan (comparative example 4), the ratio of carboxyl cellulose is too low (comparative example 5) and only carrageenan (comparative example 6), and the paste stability can be well maintained only when 6-10: 3 of sodium carboxymethylcellulose and xanthan gum are used. In addition, the conditions of 6-10: 3 of sodium carboxymethyl cellulose and xanthan gum are only effective for the toothpaste containing the buffer solution of sodium carbonate and sodium bicarbonate, and do not improve the efficacy of paste stability for the toothpaste containing other types of buffer solutions (see comparative examples 7 and 9). Therefore, we can see that the thickener combination of this protocol has a specific effect on maintaining paste stability for the toothpaste of this protocol. The toothpaste in the scheme is toothpaste taking sodium carbonate and sodium bicarbonate as buffer solutions.

Experimental example 3: clinical effect observation of anti-sensitive toothpaste for enhancing fluorine activity and resisting dentin sensitivity

The experimental method comprises the following steps:

1. subjects were healthy adult males and females meeting inclusion and exclusion criteria. A total of 82 eligible subjects participated in the baseline examination and 80 subjects completed the entire study for 8 weeks.

2. Inclusion criteria were: the age is 18-72 years old; the health condition of the whole body is good; the examination can be carried out at any time during 8 weeks of the test; firstly, the condition of teeth and gum is checked, and at least two teeth which are suitable for the research standard are required; has no allergic reaction to toothpaste and its components; no other anti-allergic toothpaste was used; no colleagues participated in other similar trial studies; no drug was used one month prior to study participation.

Referring to tables 7 and 8, there was no statistical difference between the groups of example 1 and example 4 compared to four and eight weeks regardless of the visit sensitivity index or the cold air blowing sensitivity index. However, the probing sensitivity index or the cold air blowing sensitivity index of the two groups of four weeks and eight weeks are statistically different from the baseline test, which shows that the two groups of toothpastes have obvious dentin sensitivity resisting effect in four weeks and eight weeks.

Table 7: summary of assessment of visit sensitivity

Table 8: cold air blowing sensitivity evaluation summary

The foregoing is merely an example of the present invention and common general knowledge in the art of designing and/or characterizing particular aspects and/or features is not described in any greater detail herein. It should be noted that, for those skilled in the art, without departing from the technical solution of the present invention, several variations and modifications can be made, which should also be regarded as the protection scope of the present invention, and these will not affect the effect of the implementation of the present invention and the practicability of the patent. The scope of the claims of the present application shall be determined by the contents of the claims, and the description of the embodiments and the like in the specification shall be used to explain the contents of the claims.