CN109260033B

CN109260033B - Solid gargle granule and preparation method thereof

Info

Publication number: CN109260033B
Application number: CN201811153111.0A
Authority: CN
Inventors: 王丽辉; 董明生; 林锦雄
Original assignee: Guangzhou Aibei Biological Technology Co Ltd
Current assignee: Guangzhou Aibei Biological Technology Co Ltd
Priority date: 2018-09-29
Filing date: 2018-09-29
Publication date: 2021-04-16
Anticipated expiration: 2038-09-29
Also published as: CN109260033A

Abstract

The invention discloses a solid gargle granule and a preparation method thereof, wherein the solid gargle granule comprises the following components: the whitening synergist and the anticarious agent are perlite, the anticarious agent comprises sodium monofluorophosphate and sodium fluoride, and the weight ratio of the sodium monofluorophosphate to the sodium fluoride is 1-8: 0.1-5. The solid mouthwash granule can effectively clean teeth, brighten and whiten the teeth, has good sterilization and antibacterial effects, keeps the oral cavity clean, can prevent dental caries, improve the resistance of the teeth, reduces the occurrence of oral diseases, has good oral care effect, and cannot damage enamel and dentin. In addition, the solid gargle particle is solid particle, is different from the dosage forms of toothpaste and gargle water on the market, can quickly clean oral cavity and teeth, has good taste, is convenient to use and carry, and has good market prospect.

Description

Solid gargle granule and preparation method thereof

Technical Field

The invention relates to an oral care product, and in particular relates to a solid gargle granule and a preparation method thereof.

Background

Of the oral care products, toothpastes, toothbrushes, mouthwashes and the like are popular, and such products are also the highest share of the market. The mouthwash is an emerging oral care product in recent years, and along with the maturing of consumer consumption concept and the convenience in use of the mouthwash, in recent years, the mouthwash is the same as toothpaste, so that the mouthwash becomes a necessary product for daily oral care of more and more people, and is particularly favored by urban people with fast pace of life. However, existing mouthwashes and toothpastes suffer from certain drawbacks. Firstly, the toothpaste needs to be matched with a toothbrush for use, and can effectively clean teeth, but the toothpaste is inconvenient to use and carry, long in tooth cleaning time, large in friction, easy to damage gums and teeth, incapable of playing an effective sterilization role, and not ideal in oral care effect. Secondly, some of the existing mouthwashes on the market have a certain sterilization effect, but cannot effectively clean teeth, and the oral care effect is not ideal. Therefore, there is a need to develop a new oral care product that is convenient and quick to use and that has desirable oral care effects.

Disclosure of Invention

The solid mouthwash particle is solid granular, is convenient to use, can effectively clean teeth, kill bacteria in the oral cavity and the teeth, has the efficacy of preventing dental caries, is easy to carry and quick to clean, and has a good oral care effect.

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

a solid mouthwash granule comprising the following components: the whitening synergist and the anticarious agent are perlite, the anticarious agent comprises sodium monofluorophosphate and sodium fluoride, and the weight ratio of the sodium monofluorophosphate to the sodium fluoride is 1-8: 0.1-5.

Preferably, the perlite has a D50 particle size of 19 μm. The perlite with the grain size of 19 mu m has soft friction performance, can effectively remove dirt stains on teeth, cannot damage enamel and dentin, can effectively clean the teeth, and can brighten and whiten the teeth.

Sodium monofluorophosphate is an excellent caries-preventing agent and tooth desensitizer, and its aqueous solution has obvious bactericidal action and obvious inhibiting action for growth and reproduction of aspergillus niger, staphylococcus aureus, salmonella, pseudomonas aeruginosa, catacoccus, etc. The sodium fluoride adopted by the invention is toothpaste-grade sodium fluoride, and has a better effect of preventing dental caries. The inventor finds that the combination of sodium monofluorophosphate and sodium fluoride can generate a synergistic effect, can effectively improve the anti-dental caries effect of the solid mouthwash granule, has a better effect particularly when the solid mouthwash granule is compounded according to the weight ratio, and can reduce the limitation of the solid mouthwash granule on the selection of an abrasive agent.

Preferably, the weight ratio of the sodium monofluorophosphate to the sodium fluoride is 4: 1. Through a series of intensive researches, the inventor discovers that when sodium monofluorophosphate and sodium fluoride are compounded according to the weight ratio, the solid mouthwash granule has the best effect of preventing decayed teeth.

Preferably, the weight percentage content of the brightening and whitening synergist in the solid mouthwash granule is 0.5-5%, the weight percentage content of the sodium monofluorophosphate in the solid mouthwash granule is 0.1-0.8%, and the weight percentage content of the sodium fluoride in the solid mouthwash granule is 0.01-0.5%.

Preferably, the solid mouthwash granule further contains a cleaning agent, wherein the cleaning agent comprises hydroxypropyl methylcellulose, lactose and sodium bicarbonate, the weight percentage of the hydroxypropyl methylcellulose in the solid mouthwash granule is 0.05-2%, the weight percentage of the lactose in the solid mouthwash granule is 1-10%, and the weight percentage of the sodium bicarbonate in the solid mouthwash granule is 1-10%.

The alkalescence of the sodium bicarbonate, commonly called baking soda, can neutralize acidic substances generated by bacterial fermentation in the oral cavity, reduce acid erosion of tooth enamel, reduce the occurrence of oral fungal infection and can also neutralize peculiar smell. At the same time, sodium bicarbonate is a slightly abrasive cleaning agent. The combination of the sodium bicarbonate, the lactose and the hydroxypropyl methylcellulose can generate a synergistic effect in the aspect of cleaning teeth, and can effectively improve the tooth cleaning effect of the solid mouthwash particles.

Preferably, the solid mouthwash granule further contains active additives, wherein the active additives comprise menthol, L-lysine hydrochloride and catechins, the weight percentage of the menthol in the solid mouthwash granule is 0.05-0.5%, the weight percentage of the L-lysine hydrochloride in the solid mouthwash granule is 0.01-1%, and the weight percentage of the catechins in the solid mouthwash granule is 0.05-3%.

The menthol has the functions of perfuming and antibiosis, has the cooling effect, and can effectively improve the use comfort of the solid gargle particles.

L-lysine hydrochloride, also known as L-lysine hydrochloride, which is classified as the "first deficient" amino acid, is particularly important among the 8 essential amino acids that maintain human nitrogen balance. The addition of L-lysine hydrochloride can be used as a nutrition regulator, so that the solid mouthwash granule can provide nutrition for oral cells.

Catechins, INCI tea (CAMELLIASINENSIS) catechins, are available from Sierra Biotech limited. It has antibacterial, antiinflammatory, heat and toxic materials clearing away, tooth resistance enhancing, dental plaque reducing, periodontal disease relieving, and dental yellowing preventing effects, and also has special effects in stopping gingival hemorrhage and preventing halitosis.

Preferably, the solid mouthwash granule further comprises a binder, wherein the binder comprises polyvinyl alcohol and microcrystalline cellulose, the weight percentage of the polyvinyl alcohol in the solid mouthwash granule is 1-10%, and the weight percentage of the microcrystalline cellulose in the solid mouthwash granule is 0.1-2%. The polyvinyl alcohol and microcrystalline cellulose not only act as binders in the formulations of the present invention, but their combination also acts as a thickener.

Preferably, the solid mouthwash granule further comprises 0.1 to 1 weight percent of olive oil. The INCI name of olive oil is olive (OLEA EUROPAEA) fruit oil; the addition of the olive oil can increase the drawability and lubricity of the mixed raw materials in the sugar gum stage and reduce the viscosity of the sugar gum, thereby greatly improving the processing performance of the sugar gum and ensuring that the comprehensive performance of the solid mouthwash particles is better.

Preferably, the solid mouthwash granule consists of the following components in percentage by weight: 5 to 15 percent of sorbitol, 01 to 10 percent of PEG600, 1 to 10 percent of polyvinyl alcohol, 0.1 to 2 percent of microcrystalline cellulose, 0.05 to 2 percent of hydroxypropyl methyl cellulose, 10 to 20 percent of xylitol, 0.1 to 1 percent of olive oil, 0.05 to 0.5 percent of menthol, 0.1 to 0.8 percent of sodium monofluorophosphate, 0.1 to 5 percent of magnesium stearate, 1 to 10 percent of lactose, 0.5 to 5 percent of titanium dioxide, 0.5 to 5 percent of perlite, 0.01 to 0.5 percent of sodium fluoride, 1 to 10 percent of sodium bicarbonate, 0.01 to 1 percent of L-lysine hydrochloride, 0.05 to 3 percent of catechins, 0.01 to 1 percent of essence and the balance of calcium carbonate.

Sorbitol, INCI, is sorbitol. Sorbitol can be used as a humectant in the formula of the invention, so that the inside of the solid mouthwash particle can keep the moisture of the paste, and the solid mouthwash particle is easy to absorb moisture and foam when in use.

Xylitol is a natural sweetener, and the solid mouth wash granules have better taste and are more beneficial to human health by adopting the xylitol to replace saccharides as the sweetener. At normal temperature, the sweetness of xylitol is equal to that of sucrose, and at low temperature, the sweetness of xylitol is 1.2 times that of sucrose. And the xylitol is easy to dissolve in water, and can absorb a large amount of heat when dissolved, thereby increasing the cool mouthfeel of the solid mouthwash particles. Meanwhile, xylitol is not fermented and utilized by bacteria in oral cavity, and can inhibit bacterial growth and acid generation, and prevent dental caries.

More preferably, the solid mouthwash granule consists of the following components in percentage by weight: sorbitol 9%, PEG 60005%, polyvinyl alcohol 5%, microcrystalline cellulose 0.5%, hydroxypropyl methyl cellulose 0.3%, xylitol 15%, olive oil 0.5%, menthol 0.2%, sodium monofluorophosphate 0.4%, magnesium stearate 1%, lactose 5%, titanium dioxide 2%, perlite 2%, sodium fluoride 0.1%, sodium bicarbonate 3%, L-lysine hydrochloride 0.1%, catechins 0.5%, essence 0.5% and calcium carbonate in balance.

Preferably, the preparation method of the solid mouthwash granule comprises the following steps:

(1) preparation of gum base material:

a. mixing sorbitol, PEG6000, polyvinyl alcohol, microcrystalline cellulose and hydroxypropyl methyl cellulose, and uniformly stirring to obtain a mixture A;

b. adding xylitol into the mixture A, and uniformly stirring to obtain a mixture B;

c. uniformly mixing olive oil and menthol, then adding the mixture B, then adding sodium monofluorophosphate, and uniformly stirring to obtain a mixture C;

d. adding magnesium stearate, lactose, titanium dioxide, perlite, sodium fluoride, sodium bicarbonate, L-lysine hydrochloride, calcium carbonate, catechins and essence into the mixture C in sequence, and uniformly stirring to obtain a gum base material;

(2) preparing sugar gum:

melting the gum base material prepared in the step (1) at high temperature, filtering, and stirring until the gum base material forms hard dough-like sugar gum;

(3) preparation of solid mouthwash granules:

and (3) extruding and molding the sugar gum prepared in the step (2) by using an extruder, then calendering the sugar gum into sheets by using a tablet press, cooling, cutting and embossing by using a roller cutting machine, aging and packaging to obtain the solid gargle particles.

Preferably, the high-temperature melting temperature is 75-85 ℃;

preferably, the calendering is carried out at a temperature of 20 ℃ and a relative humidity of 60%. Therefore, the temperature of the sugar gum can be reduced, and the surface of the sugar gum is dry and has certain hardness.

Preferably, the cooling is carried out in an environment with the temperature of 10-15 ℃ and the relative humidity of 40-60%.

Preferably, the aging is carried out in an aging chamber with the temperature of 20-25 ℃ and the relative humidity of 45-55%, and the aging time is 15-25 h.

The cooling and aging environmental conditions of the present invention allow the physical properties of the solid mouthwash particles to change more consistently, thereby improving their packaging flexibility.

The use method of the solid mouthwash granule comprises the following steps: putting 1 granule (1-2 g/granule) of the solid mouthwash granule into the mouth at one time, chewing, then rubbing fragments of the solid mouthwash granule with the tongue and the lips to clean the gums, the teeth and the tongue, spitting out foams, and repeatedly gargling with water for several times.

Compared with the prior art, the invention has the beneficial effects that: the solid mouthwash granule can effectively clean teeth, brighten and whiten the teeth, has good sterilization and antibacterial effects, keeps the oral cavity clean, can prevent dental caries, improve the resistance of the teeth, reduces the occurrence of oral diseases, has good oral care effect, and cannot damage enamel and dentin. In addition, the solid gargle particle is solid particle, is different from the dosage forms of toothpaste and gargle water on the market, can quickly clean oral cavity and teeth, has good taste, is convenient to use and carry, and has good market prospect.

Detailed Description

The present invention will be further described with reference to specific examples for better illustrating the objects, technical solutions and advantages of the present invention, but the present invention is not limited to the following examples. It is noted that, unless otherwise indicated, the various components used in the present invention are all materials known in the art, and are either commercially available or prepared by known methods.

The formulations of the solid mouth rinse granules of examples 1 to 4 are shown in table 1.

The preparation method of the solid mouthwash granule of embodiment 1 to 4 includes the following steps:

(1) preparation of gum base material:

(2) preparing sugar gum:

putting the gum base material prepared in the step (1) into an oven, melting at a high temperature of 75-85 ℃, filtering by a filtering device, and uniformly stirring the molten gum by a stirrer with a turnover frame until the molten gum forms hard dough-like sugar gum;

(3) preparation of solid mouthwash granules:

extruding the sugar gum prepared in the step (2) by using a screw extruder, rolling the sugar gum into thin and wide sheets by using a tablet press under the environment of 20 ℃ and 60% of relative humidity, cooling the sheet sugar gum by using a cooling cabinet, performing the cooling process under the environment of 10-15 ℃ and 40-60% of relative humidity, cutting and embossing the sheet sugar gum by using a roller cutter in a land preparation manner, aging for 15-25 hours in an aging chamber under the condition of 20-25 ℃ and 45-55% of relative humidity, and finally packaging by using a packaging machine to obtain the solid gargle particles.

Table 1 formulation of solid mouthwash particles of examples 1-4 (weight%/%)

The formulations of the solid mouthwash particles of comparative examples 1-5 are shown in table 2.

TABLE 2 formulation of solid mouthwash particles of comparative examples 1-5 (weight%/%)

The preparation methods of the solid mouthwash particles of comparative examples 1-5 refer to the preparation methods of examples 1-4.

Effect testing

360 volunteers with the age of 20-40 years are extracted as subjects, and the 360 subjects are divided into 9 groups, and the number of the groups is 1-9. Wherein group 1 used the solid mouthwash granule of example 1, group 2 used the solid mouthwash granule of example 2, group 3 used the solid mouthwash granule of example 3, group 4 used the solid mouthwash granule of example 4, group 5 used the solid mouthwash granule of comparative example 1, group 6 used the solid mouthwash granule of comparative example 2, group 7 used the solid mouthwash granule of comparative example 3, group 8 used the solid mouthwash granule of comparative example 4, and group 9 used the solid mouthwash granule of comparative example 5. The test method comprises the following steps: putting the solid mouthwash particles into the mouth, chewing, rubbing the fragments of the solid mouthwash particles with the tongue and lips to clean the gums, teeth and tongue, spitting out foam after 1min, and repeatedly gargling with water for 3 times, 1 time each in the morning and evening, 1 particle each time, continuously using for 30 days, and not using other oral care products during the test period. The effect feedback of the subjects was counted after 30 days, and the results are shown in table 3.

TABLE 3 statistics of the effectiveness of solid mouthwash particles

As can be seen from the results of table 3:

1. the solid mouthwash particles in examples 1 to 4 have good effects in various evaluation items, which shows that the solid mouthwash particles have excellent effects of cleaning teeth and brightening teeth, can prevent dental caries, keep the oral cavity clean, and have good oral care effects.

2. Comparing example 1, comparative example 1 and comparative example 2, it can be seen that the combination of sodium monofluorophosphate and sodium fluoride can generate synergistic effect, which can significantly improve the anti-dental caries efficacy of the solid mouthwash granule and also improve the tooth cleaning effect of the solid mouthwash granule to a certain extent.

3. Comparative example 1 and comparative examples 3 to 5 show that the combination of sodium bicarbonate, lactose and hydroxypropyl methylcellulose can produce a synergistic effect in the aspect of cleaning teeth, can effectively improve the tooth cleaning effect of the solid mouthwash granule, and can also improve the mouth feel of the solid mouthwash granule.

Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.

Claims

1. A solid mouthwash granule, characterized by comprising the following components: the whitening synergist and the anticarious agent are perlite, the anticarious agent comprises sodium monofluorophosphate and sodium fluoride, and the weight ratio of the sodium monofluorophosphate to the sodium fluoride is 1-8: 0.1-5; the solid mouthwash particle also contains a cleaning agent, wherein the cleaning agent comprises 0.05-2 wt% of hydroxypropyl methyl cellulose, 1-10 wt% of lactose and 1-10 wt% of sodium bicarbonate.

2. The solid mouthwash of claim 1, wherein the perlite has a D50 particle size of 19 μ ι η; the weight ratio of the sodium monofluorophosphate to the sodium fluoride is 4: 1.

3. The solid mouthwash granule according to claim 1 or 2, wherein the whitening synergist is present in the solid mouthwash granule in an amount of 0.5 to 5% by weight, the sodium monofluorophosphate is present in the solid mouthwash granule in an amount of 0.1 to 0.8% by weight, and the sodium fluoride is present in the solid mouthwash granule in an amount of 0.01 to 0.5% by weight.

4. The solid mouthwash granule according to claim 3, further comprising active additives, wherein the active additives comprise menthol, L-lysine hydrochloride and catechins, the menthol is 0.05% to 0.5% by weight of the solid mouthwash granule, the L-lysine hydrochloride is 0.01% to 1% by weight of the solid mouthwash granule, and the catechins are 0.05% to 3% by weight of the solid mouthwash granule.

5. The solid mouthwash granule according to claim 3, further comprising a binder, wherein the binder comprises polyvinyl alcohol in an amount of 1% to 10% by weight of the solid mouthwash granule and microcrystalline cellulose in an amount of 0.1% to 2% by weight of the solid mouthwash granule.

6. The solid mouthwash granule according to claim 3, further comprising 0.1 to 1 weight percent of olive oil.

7. The solid mouthwash granule is characterized by comprising the following components in percentage by weight: 5-15% of sorbitol, 01-10% of PEG600, 1-10% of polyvinyl alcohol, 0.1-2% of microcrystalline cellulose, 0.05-2% of hydroxypropyl methyl cellulose, 10-20% of xylitol, 0.1-1% of olive oil, 0.05-0.5% of menthol, 0.1-0.8% of sodium monofluorophosphate, 0.1-5% of magnesium stearate, 1-10% of lactose, 0.5-5% of titanium dioxide, 0.5-5% of perlite, 0.01-0.5% of sodium fluoride, 1-10% of sodium bicarbonate, 0.01-1% of L-lysine hydrochloride, 0.05-3% of catechins, 0.01-1% of essence and the balance of calcium carbonate; the perlite had a D50 particle size of 19 μm.

8. The solid mouthwash granule according to claim 7, consisting of the following components in weight percent: sorbitol 9%, PEG 60005%, polyvinyl alcohol 5%, microcrystalline cellulose 0.5%, hydroxypropyl methyl cellulose 0.3%, xylitol 15%, olive oil 0.5%, menthol 0.2%, sodium monofluorophosphate 0.4%, magnesium stearate 1%, lactose 5%, titanium dioxide 2%, perlite 2%, sodium fluoride 0.1%, sodium bicarbonate 3%, L-lysine hydrochloride 0.1%, catechins 0.5%, essence 0.5% and calcium carbonate in balance.

9. A process for the preparation of a solid mouthwash according to claim 7 or 8, comprising the following steps:

(1) preparation of gum base material:

(2) preparing sugar gum:

(3) preparation of solid mouthwash granules:

10. The method of preparing a solid mouthwash granule according to claim 9, wherein the temperature of the high temperature melting is 75-85 ℃.

11. The method of making a solid mouthwash according to claim 9, wherein the calendering is performed at a temperature of 20 ℃ and a relative humidity of 60%.

12. The method of preparing a solid mouthwash granule according to claim 9, wherein the cooling is performed in an environment with a temperature of 10 to 15 ℃ and a relative humidity of 40 to 60%.

13. The method of preparing a solid mouthwash granule according to claim 9, wherein the aging is performed in an aging chamber at a temperature of 20 to 25 ℃ and a relative humidity of 45 to 55% for a period of 15 to 25 hours.