Mouth wash and preparation method thereof
By using starch-coated povidone iodine granules, the poor stability of povidone iodine in dilute solution was solved, and the long-term stability and efficient antibacterial effect of alcohol-free low-concentration povidone iodine mouthwash was achieved.
Patent Information
- Application Number
- CN202411494154.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-24
- Publication Date
- 2025-02-18
AI Technical Summary
The existing povidone iodine mouthwash has poor stability in dilute solutions, low concentration of povidone iodine is difficult to preserve for a long time, and most mouthwash contains alcohol, which poses a risk of carcinogenicity.
Starch-coated povidone iodine granules are used to achieve stable release of povidone iodine through the coating of the starch layer and the decomposition of saliva amylase, and a low-concentration povidone iodine mouthwash is prepared without alcohol.
It effectively solves the problem of poor stability of povidone iodine, extends the service life of mouthwash, ensures efficient antibacterial and antivirus effects, and avoids the risk of carcinogenicity of alcohol.
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Abstract
Description
Technical Field
[0001] The invention relates to an oral care product, in particular to a mouthwash and a preparation method thereof. The mouthwash uses povidone iodine as an antibacterial agent, and a specific composition effectively solves the problem of poor stability of povidone iodine in a dilute solution. The mouthwash does not contain alcohol and can maintain a relatively high effective iodine content even when stored for a long time. Background Art
[0002] Oral diseases are common diseases caused by various pathogenic bacteria in the oral cavity. For a long time, people have mainly used various toothpastes and mouthwashes containing antibacterial agents to clean the oral cavity and prevent the occurrence of oral diseases. Using mouthwash to rinse the mouth is a more convenient and easy way to maintain oral health than brushing teeth or using antibacterial dental floss and tooth powder. It can remove food residues and some soft scales in the mouth, and can also effectively inhibit bacteria in the mouth. Mouthwash, also known as gargle, is mainly used to clean the mouth, inhibit the growth of bacteria in the mouth, cover up bad smells in the mouth, and freshen breath. The market demand for mouthwash is also increasing.
[0003] The main ingredients of mouthwash include functional additives, flavors, moisturizers, surfactants, preservatives and solvents. Functional additives can be antibacterial agents, anti-caries agents, anti-gingivitis compounds and anti-inflammatory agents to achieve the functions of mouthwash in sterilization, anti-inflammation and anti-infection. Surfactants can achieve the function of mouthwash in cleaning the oral cavity. Flavors can achieve the function of mouthwash in covering up bad breath and other odors. Therefore, the role of mouthwash is relatively comprehensive. Common mouthwashes include physiological saline, compound boric acid solution, 1% to 3% hydrogen peroxide solution, 1% to 4% sodium bicarbonate solution, 0.02% chlorhexidine solution, 0.02% furazolidone solution, 0.1% acetic acid solution, 2% to 3% boric acid solution, 0.08% metronidazole solution, iodine solution, etc. Although many mouthwashes contain disinfectant ingredients that can inhibit the growth of bacteria and viruses, long-term use of broad-spectrum antibiotic mouthwashes can easily cause oral flora imbalance and even drug resistance. For example, compound chlorhexidine mouthwash tastes bitter and has a poor taste. Long-term use can easily cause adverse reactions such as tooth staining and yellow tongue coating. Long-term use of chlorhexidine may cause some strains that are not sensitive to it to develop multidrug resistance. 1% to 4% sodium bicarbonate solution can clean the mouth and inhibit bacteria, but the antibacterial effect is single and cannot effectively prevent various complications such as oral infections. In addition, the taste and effect of removing bad breath are not satisfactory. Although hydrogen peroxide mouthwash has a good bactericidal effect, it is extremely unstable, volatile, and has weak penetration. It has a noticeable odor after entering the mouth; metronidazole solution has a strong bactericidal effect, but its therapeutic effect is unstable and long-term use can easily lead to drug resistance.
[0004] Povidone iodine is a loose and complex chemical complex formed by combining polyvinyl pyrrolidone (POVIDONE, PVP) and iodine. After contacting the wound or the affected area, povidone iodine can depolymerize and release active iodine to produce strong antibacterial and antibacterial activity. It is a new type of external disinfectant with high efficiency, broad spectrum and low toxicity. Povidone iodine solution will release active iodine, the stability of iodine is poor, and the concentration of active iodine decreases rapidly over time, but povidone iodine powder or 10% high concentration povidone iodine solution has good stability. Some people use povidone iodine powder as an antibacterial agent raw material to prepare granular povidone iodine mouthwash, which is small in size and has no risk of leakage, and is easy to carry. For example, CN116173067A discloses a povidone iodine, which is composed of polyvinyl pyrrolidone K30 mass proportion of 83% to 85%, iodine powder mass proportion of 14.8% to 17%, and auxiliary agent mass proportion of 0 to 0.2% by mass; the dosage form of the povidone iodine is powder. The water content of polyvinyl pyrrolidone K30 is 6% to 8%, and the povidone iodine aqueous solution prepared by using the raw material has good stability.
[0005] CN110799179A discloses a solid composition comprising an iodine reagent and sodium chloride with improved water solubility, wherein the solid composition comprises a mixture of 0.2 to 50 parts by weight of an iodine reagent and 100 parts by weight of sodium chloride, and the dissolution rate in water is less than 30 seconds, and the water solubility is excellent. The iodine reagent is selected from the group consisting of povidone iodine, cadexomer iodine and poloxamer iodine. However, when using powder, the content of povidone iodine per unit solid preparation is very small, and there is also a problem of slow dissolution rate. Others use high-concentration povidone iodine solution as a mouthwash after dilution, but low-concentration povidone iodine is difficult to circulate or store for a long time, wherein the activity of povidone iodine will drop sharply, the product life is short, and it is inconvenient to dilute and use a high-concentration solution, and due to the inaccurate concentration of commercially available high-concentration iodine solution, there is also a problem that the required correct concentration solution cannot be produced. For this reason, stabilizers are widely used in povidone-iodine solutions to improve the stability of the solution. For example, CN114259503A discloses a povidone-iodine solution for human use, which is prepared using the following formula: 5-10 kg povidone-iodine, 0.5-1.0 kg potassium iodide, 6-10 kg betaine, 0.2-0.5 kg D-panthenol, 30-65 kg water, and the balance is glycerol, to prepare a total of 100 L of solution. Promote wound healing while also having a moisturizing effect. A povidone-iodine solution for human use containing 0.5% to 1.0% effective iodine can sterilize and disinfect for a long time. CN110037940A discloses an oral sterilization and disinfection mouthwash, and specifically discloses the following weight percentages of the components: povidone iodine 4.5% to 5.5%; potassium iodate 0 to 0.05%; potassium iodide 0.1% to 0.15%; polyvinyl pyrrolidone 0.5% to 0.8%; sodium lauryl sulfate 0.05% to 0.1%; glycerol 1% to 3%; polyethylene glycol 400
[0006] 0.4% to 0.6%; citric acid 0.15% to 0.25%; auxiliary materials 0% to 0.1%; freshener 0.5% to 1.2%; purified water as the balance. The mouthwash has the characteristics of good sterilization and disinfection effect, low irritation, harmlessness to the human body, good stability and long storage time. CN102885852A discloses a povidone iodine paste, the components and weight percentage of the povidone iodine paste are 10% povidone iodine, 0.1% to 0.5% potassium iodate, 20% to 31% polyethylene glycol-400, 20% to 30% polyethylene glycol-4000, 5% to 15% matrix protective agent xylitol or sorbitol, 15% to 20% glycerol, 0.5% to 2.0% sodium lauryl sulfate, and 7.5% to 15% purified water. The present invention utilizes unique protection methods and means to overcome the technical difficulty that the stability of povidone iodine is not high during product preparation and storage after being compatible with water-soluble matrix polyethylene glycol. However, in povidone iodine mouthwash, active iodine has strong oxidizability, resulting in unstable content of effective iodine. After dilution, the content of its effective ingredient decreases at an accelerated rate, and it needs to be prepared and used immediately, which is inconvenient for patients to use. When there is a wound surface in the oral cavity, it is very easy to reduce its antibacterial performance due to the loss of effective iodine. In addition, most mouthwashes use alcohol, and some mouthwashes containing alcohol may have carcinogenic effects. The level of its risk is closely related to the formula and alcohol concentration of the mouthwash. It can be seen that it is necessary to develop a non-alcoholic, directly usable, stable, long-life mouthwash containing low-concentration povidone iodine solution, which can also maintain a high effective iodine content for a long time. Summary of the invention
[0007] In order to solve the defects in the prior art, the present invention provides a mouthwash and a preparation method thereof. The mouthwash uses starch-coated povidone iodine as an antibacterial agent, does not use alcohol, can directly prepare a low-concentration povidone iodine mouthwash, and can maintain the long-term stability of povidone iodine. When used, it is directly used for gargling. When the mouthwash enters the user's oral cavity, salivary amylase existing in the user's oral cavity or produced by chewing can decompose the starch layer wrapped on the surface of the antibacterial agent, so that the povidone iodine particles quickly escape and contact with solvent water, quickly release active iodine within a safe concentration range and act on various parts of the oral cavity, thereby achieving antibacterial and antiviral effects, and solving the problem of poor stability of low-concentration povidone iodine mouthwashes in the prior art.
[0008] In order to achieve the above-mentioned purpose of the invention, the present application provides a mouthwash, the components and weight percentages of the components are as follows:
[0009]
[0010]
[0011] Furthermore, the mass of the starch layer is 2% to 5% of the mass of the povidone-iodine particles. The mass of the starch layer cannot be too high, otherwise the starch layer on the surface of the povidone-iodine cannot be quickly decomposed by salivary enzymes, making the mouthwash ineffective; when the starch layer content is too low, the povidone-iodine particles cannot be effectively coated and protected. The slow hydrolysis of starch in an aqueous solution may cause the mouthwash to contact the solution before use, decompose and release active iodine, and the effective ingredients gradually decompose and become ineffective, affecting the service life of the mouthwash. Preferably, the mass of the starch layer is 2%, 2.5%, 3%, 3.5%, 3.7%, 4%, 4.2%, 4.4%, 4.6%, 4.8%, 5% of the mass of the povidone-iodine particles.
[0012] Furthermore, the average particle size of the povidone-iodine particles is 1 to 100 μm.
[0013] Further, the preparation method of the povidone iodine particles coated with starch on the surface is as follows: weigh povidone iodine particles and starch powder in proportion; add starch to water according to a solid content of 5% to 10%, continue stirring and gelatinize at 70 to 90°C for 20 to 60 minutes, and the stirring rate is 300 to 800 r / min to obtain a gelatinized starch solution and cool to room temperature; grind the povidone iodine particles to an average particle size of 1 to 100 μm, add the ground povidone iodine particles to the gelatinized starch solution, continue stirring for 30 to 60 minutes, filter, wash with water, and dry to obtain povidone iodine particles coated with a starch layer on the surface. There are more hydroxyl groups on the starch surface, which can form hydrogen bonds with povidone iodine, and the coating is more stable.
[0014] Further, the thickener is selected from one or more of ethyl cellulose, hydroxypropyl methylcellulose, sodium carboxymethyl cellulose, cross-linked sodium polyacrylate, guar gum, sodium alginate, and carrageenan; the surfactant is selected from one or more of sodium dodecyl sulfate, sodium dodecylbenzene sulfonate, sodium lauryl sulfate, sodium lauroyl sarcosinate, sodium cocoyl glycinate, and sodium acyl glutamate; the flavor is selected from one or more of tea flavor, mint flavor, fruit flavor, flower flavor, and bamboo flavor; the sweetener is selected from one or more of saccharin sodium, sucralose, xylitol, sodium cyclamate, aspartame, stevioside, or mogroside. There is no special need for the selection of thickeners, surfactants, flavors, and sweeteners, mainly to meet the market requirements for mouthwashes. There is no special limitation on the composition and content ratio of each material, and it is appropriate to meet the requirements of mouthwashes.
[0015] Further, a mouthwash has the following components and the weight percentages of the components:
[0016]
[0017] The average particle size of the povidone-iodine particles is 50-100 μm, and the surface of the povidone-iodine particles is coated with a starch layer accounting for 2%-5% of the mass of the povidone-iodine particles.
[0018] The present application also provides a method for preparing a mouthwash, comprising the following steps:
[0019] (1) preparing povidone iodine particles coated with starch, the method is as follows: weighing povidone iodine particles and starch powder in proportion; adding starch to water at a solid content of 5% to 10%, stirring continuously and gelatinizing at 70 to 90° C. for 20 to 60 minutes, stirring at a rate of 300 to 800 r / min to obtain a gelatinized starch solution, and cooling to room temperature; grinding the povidone iodine particles to an average particle size of 1 to 100 μm, adding the ground povidone iodine particles to the gelatinized starch solution, stirring continuously for 30 to 60 minutes, filtering, washing with water, and drying to obtain the product;
[0020] (2) Add a thickener, a sweetener, a surfactant, and a flavor to water in sequence, stir and disperse them uniformly, then add the starch-coated povidone-iodine particles obtained in step (1), stir and disperse them, place them in a micro mixer for shear mixing for 30 to 200 minutes, and then take them out to obtain a mouthwash. There is no special restriction on the order of adding the thickener, sweetener, surfactant, and flavor, as long as they can be quickly dissolved and dispersed.
[0021] Furthermore, the shear energy of the shear mixing of the micro mixer is 300 to 1000 KJ / L. The micro mixer is a mixing device that delivers the slurry into the nozzle part through a pump and mixes it through the shear energy generated when it flows through the nozzle part. In the manufacturing method of the mouthwash of the present application, the shear energy of the mixing part of the micro mixer is preferably in the range of 300 to 1000 KJ / L. There are a large number of hydroxyl groups on the surface of starch-coated povidone-iodine particles. When the particles are dispersed in an aqueous solvent, the hydroxyl groups between different particles will preferentially form hydrogen bonds with the solvent, generating a solvation force, which promotes the dispersion and stability of the povidone-iodine particles. At the same time, with the rapid shearing of the micro mixer, under the action of a sufficiently high speed shear force, the starch-coated particles will continue to form hydrogen bonds with the solvent, preventing the hydroxyl groups inside the particles from combining to produce flocculation, resulting in the possibility of particles agglomerating in water to form precipitation. The entire system forms a non-flocculated stable dispersion system under the specific preparation method of the present application. With thickeners, surfactants and other mouthwash compositions, the antibacterial ingredient starch-coated povidone-iodine particles can be stably dispersed in water for a long time. Starch can protect the contact between povidone-iodine and water, effectively protect the active iodine, and reduce the loss of active ingredients before use. If the shear energy of the micro mixer is low, such as less than 300kJ / L, the agglomeration caused by the internal force of the starch-coated povidone-iodine is not easy to dissolve, and sometimes the dispersion is insufficient; if the shear force is too large, it will lead to energy waste and may cause the starch-coated povidone-iodine to break, such as the starch layer is damaged or the povidone-iodine particles are crushed and reduced, making the coating protection ineffective, and active iodine is produced and continuously consumed.
[0022] The present application also provides a method for using a mouthwash. Compared with conventional high-povidone-iodine concentration solution systems, the mouthwash of the present application can be used directly without diluting with water first, and is safe and convenient. When using, gargle for 60 to 100 seconds and then spit it out, and gargle multiple times.
[0023] Compared with the prior art, the technical solution of this application has the following beneficial effects:
[0024] 1. The present application uses povidone iodine as an antibacterial agent. Povidone iodine is a broad-spectrum bactericidal agent that effectively kills pathogenic microorganisms such as bacteria, viruses and fungi. It is low-toxic and non-irritating to the oral mucosa, thereby maintaining the comfort of using the mouthwash and achieving a good bactericidal effect; the mouthwash of the present application is alcohol-free and does not contain other irritating raw materials. The mouthwash is safe and hygienic and has a good antibacterial and disinfecting effect;
[0025] 2. The present application ingeniously uses starch to coat the povidone-iodine particles, and isolates the povidone-iodine before contacting with water. The specific treatment method of the present application firstly ensures the long-term stable dispersion of the starch-coated particles in the mouthwash system, and secondly, when the mouthwash is used, the amylase in the oral cavity can quickly destroy the starch layer, so that the povidone-iodine particles quickly come into contact with water, producing a large amount of active iodine, and achieving antibacterial and antiviral effects. Before the mouthwash is used, the starch will keep the povidone-iodine separated from the water, protecting the antibacterial agent, effectively solving the problem of poor stability of low-concentration povidone-iodine solutions with high antibacterial activity, and extending the service life of the mouthwash;
[0026] 3. The mouthwash of the present application has simple raw materials, a relatively easy preparation method, low cost, good antibacterial effect, and good economic value. DETAILED DESCRIPTION
[0027] In order to make the technical problems solved by the present invention, the technical solutions adopted and the technical effects achieved clearer, the technical solutions of the embodiments of the present invention are further described in detail below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative work are within the scope of protection of the present invention.
[0028] It should be noted that the reference to "embodiment" in this document means that the specific features, structures or characteristics described in conjunction with the embodiment may be included in at least one embodiment of the present application. The appearance of this phrase in various places in the specification does not necessarily refer to the same embodiment, nor is it an independent or alternative embodiment that is mutually exclusive with other embodiments. It is explicitly and implicitly understood by those skilled in the art that the embodiments described herein may be combined with other embodiments.
[0029] The experimental methods in the following examples are conventional methods unless otherwise specified. The materials, reagents, etc. used in the following examples are commercially available unless otherwise specified.
[0030] The bactericidal effect of povidone-iodine mainly depends on its effective iodine content, and the effective iodine reduction rate is an important indicator for measuring the quality of povidone-iodine. The prepared mouthwash is tested using the following method:
[0031] 1. Heat stability: Pour 25 μL of the sample into a stoppered colorimetric tube, place it in a constant temperature incubator at 50°C for 24 hours, then take it out, return it to room temperature, and observe visually.
[0032] 2. Determination of effective iodine content in mouthwash: seal the mouthwash solution in a white plastic bottle, store it at room temperature away from light, take samples on time, and measure the effective iodine content of the mouthwash after normal storage and adding salivary amylase and stirring for 20 seconds. The concentration test method is as follows: take 5mL of the solution to be tested, place it in a beaker, add water to 50mL, titrate the sample solution to the end point with 0.01M sodium thiosulfate titration solution, add 2mL of 5% starch indicator, continue to titrate until the blue disappears, and record the volume of sodium thiosulfate lost at the titration end point. 1mL of sodium thiosulfate is equivalent to 1.269mg of effective iodine. Record the effective iodine content on the 30th and 60th days.
[0033] Example 1
[0034] A mouthwash, the components and weight percentages of the components are as follows:
[0035] Povidone-iodine granules 1%; sodium carboxymethylcellulose 0.5%; sodium lauryl sulfate 0.1%;
[0036] 0.01% mint flavor; 0.01% saccharin sodium; the balance is water, and the surface of the povidone-iodine particles is coated with a starch layer.
[0037] The preparation method of the mouthwash is as follows: (1) preparing povidone iodine particles coated with starch on the surface: weighing povidone iodine particles and starch powder at a mass ratio of 100:2; adding starch into water at a solid content of 5%, stirring continuously and gelatinizing at 70° C. for 20 minutes at a stirring rate of 300 r / min to obtain a gelatinized starch solution, and cooling to room temperature; grinding the povidone iodine particles to an average particle size of 1 to 50 μm, adding the ground povidone iodine particles into the gelatinized starch solution, stirring continuously for 30 minutes, filtering, washing with water, and drying to obtain the mouthwash;
[0038] (2) Add a thickener, a sweetener, a surfactant, and a flavor to water in sequence, stir and disperse them uniformly, then add the starch-coated povidone-iodine particles obtained in step (1), stir and disperse them, place them in a micro mixer, shear and mix them at a shear energy of 300 KJ / L for 30 minutes, and then take them out to obtain a mouthwash. After testing, the mouthwash has no stratification or precipitation, and the appearance of the mouthwash is stable and uniform after being placed for 60 days. No effective iodine is detected in the mouthwash on the 30th and 60th days. After adding salivary amylase, the effective iodine on the 30th day is 0.095 mg / mL, and the effective iodine on the 60th day is 0.096 mg / mL.
[0039] Example 2
[0040] A mouthwash, the components and weight percentages of the components are as follows:
[0041] Povidone-iodine granules 5%; sodium carboxymethylcellulose 1%; sodium lauryl sulfate 0.5%;
[0042] 0.1% mint flavor; 0.1% saccharin sodium; the balance is water, and the surface of the povidone iodine particles is coated with a starch layer.
[0043] The preparation method of the mouthwash is as follows: (1) preparing povidone iodine particles coated with starch on the surface: weighing povidone iodine particles and starch powder at a mass ratio of 100:5; adding starch into water at a solid content of 10%, stirring continuously and gelatinizing at 90° C. for 60 minutes at a stirring rate of 800 r / min to obtain a gelatinized starch solution, and cooling to room temperature; grinding the povidone iodine particles to an average particle size of 50 to 100 μm, adding the ground povidone iodine particles into the gelatinized starch solution, stirring continuously for 60 minutes, filtering, washing with water, and drying to obtain the mouthwash;
[0044] (2) Add a thickener, a sweetener, a surfactant, and a flavor to water in sequence, stir and disperse them uniformly, then add the starch-coated povidone-iodine particles obtained in step (1), stir and disperse them, place them in a micro mixer and shear and knead them for 200 minutes at a shear energy of 1000 KJ / L, and then take them out to obtain a mouthwash. After testing, the mouthwash has no stratification or precipitation, and the appearance of the mouthwash is stable and uniform after being placed for 60 days. No effective iodine is detected on the 30th and 60th days of the mouthwash. After adding salivary amylase, the effective iodine on the 30th day is 0.498 mg / mL, and the effective iodine on the 60th day is 0.497 mg / mL.
[0045] Example 3
[0046] A mouthwash, the components and weight percentages of the components are as follows:
[0047] Povidone-iodine granules 3%; sodium carboxymethylcellulose 1%; sodium lauryl sulfate 0.2%;
[0048] 0.01% mint flavor; 0.01% saccharin sodium; the balance is water, and the surface of the povidone-iodine particles is coated with a starch layer.
[0049] The preparation method of the mouthwash is as follows: (1) preparing povidone iodine particles coated with starch on the surface: weighing povidone iodine particles and starch powder at a mass ratio of 100:3; adding starch into water at a solid content of 5%, stirring continuously and gelatinizing at 70° C. for 20 minutes, with a stirring rate of 500 r / min to obtain a gelatinized starch solution, and cooling to room temperature; grinding the povidone iodine particles to an average particle size of 20 to 80 μm, adding the ground povidone iodine particles into the gelatinized starch solution, stirring continuously for 40 minutes, filtering, washing with water, and drying to obtain the mouthwash;
[0050] (2) Add a thickener, a sweetener, a surfactant, and a flavor to water in sequence, stir and disperse them uniformly, then add the starch-coated povidone-iodine particles obtained in step (1), stir and disperse them, place them in a micro mixer, shear and mix them at a shear energy of 800 KJ / L for 40 minutes, and then take them out to obtain a mouthwash. After testing, the mouthwash has no stratification or precipitation, and the appearance of the mouthwash is stable and uniform after being placed for 60 days. No effective iodine is detected on the 30th and 60th days of the mouthwash. After adding salivary amylase, the effective iodine on the 30th day is 0.302 mg / mL, and the effective iodine on the 60th day is 0.299 mg / mL.
[0051] Example 4
[0052] A mouthwash, the components and weight percentages of the components are as follows:
[0053] Povidone-iodine granules 3%; sodium alginate 1%; sodium lauryl sulfate 0.2%;
[0054] 0.01% fruit essence; 0.01% xylitol; the balance is water, and the surface of the povidone-iodine particles is coated with a starch layer.
[0055] The preparation method of the mouthwash is as follows: (1) preparing povidone iodine particles coated with starch on the surface: weighing povidone iodine particles and starch powder at a mass ratio of 100:3; adding starch into water at a solid content of 5%, stirring continuously and gelatinizing at 70° C. for 20 minutes, with a stirring rate of 500 r / min to obtain a gelatinized starch solution, and cooling to room temperature; grinding the povidone iodine particles to an average particle size of 20 to 80 μm, adding the ground povidone iodine particles into the gelatinized starch solution, stirring continuously for 40 minutes, filtering, washing with water, and drying to obtain the mouthwash;
[0056] (2) Add a thickener, a sweetener, a surfactant, and a flavor to water in sequence, stir and disperse them uniformly, then add the starch-coated povidone-iodine particles obtained in step (1), stir and disperse them, place them in a micro mixer, shear and mix them at a shear energy of 800 KJ / L for 40 minutes, and then take them out to obtain a mouthwash. After testing, the mouthwash has no stratification or precipitation, and the appearance of the mouthwash is stable and uniform after being placed for 60 days. No effective iodine is detected on the 30th and 60th days of the mouthwash. After adding salivary amylase, the effective iodine on the 30th day is 0.298 mg / mL, and the effective iodine on the 60th day is 0.300 mg / mL.
[0057] Comparative Example 1
[0058] A mouthwash, the components and weight percentages of the components are as follows:
[0059] Povidone-iodine granules 3%; sodium alginate 1%; sodium lauryl sulfate 0.2%;
[0060] Fruit flavor 0.01%; xylitol 0.01%; water, balance
[0061] The preparation method of the mouthwash is as follows: (1) grinding povidone iodine particles to an average particle size of 20 to 80 μm;
[0062] (2) Add a thickener, a sweetener, a surfactant, and a flavor to water in sequence, stir and disperse them uniformly, then add the povidone-iodine particles treated in step (1), stir and disperse them, place them in a micro mixer, shear and mix them at a shear energy of 800 KJ / L for 40 minutes, and then take them out to obtain a mouthwash. After testing, the mouthwash has no stratification or precipitation, and the appearance of the mouthwash is stable and uniform after being placed for 60 days. The effective iodine content of the mouthwash is 0.24 mg / mL on the 30th day and 0.17 mg / mL on the 60th day.
[0063] Comparative Example 2
[0064] A mouthwash, the components and weight percentages of the components are as follows:
[0065] Povidone-iodine granules 3%; sodium alginate 1%; sodium lauryl sulfate 0.2%;
[0066] 0.01% fruit essence; 0.01% xylitol; the balance is water, and the surface of the povidone-iodine particles is coated with a starch layer.
[0067] The preparation method of the mouthwash is as follows: (1) preparing povidone iodine particles coated with starch on the surface: weighing povidone iodine particles and starch powder at a mass ratio of 100:1; adding starch to water at a solid content of 5%, stirring continuously and gelatinizing at 60° C. for 20 minutes, and stirring at a rate of 500 r / min to obtain a gelatinized starch solution; grinding the povidone iodine particles to an average particle size of 20 to 80 μm, adding the ground povidone iodine particles to the gelatinized starch solution, stirring continuously for 40 minutes, filtering, washing with water, and drying to obtain the mouthwash;
[0068] (2) Add a thickener, a sweetener, a surfactant, and a flavor to water in sequence, stir and disperse them evenly, then add the starch-coated povidone-iodine particles obtained in step (1), stir and disperse them, place them in a micro mixer, and shear and mix them for 40 minutes at a shear energy of 800 KJ / L, and then take them out to obtain a mouthwash. After testing, the mouthwash has no stratification or precipitation, and the appearance of the mouthwash is stable and uniform after being placed for 60 days. The effective iodine content of the mouthwash is 0.03 mg / mL on the 30th day and 0.07 mg / mL on the 60th day. After adding salivary amylase, the effective iodine content is 0.28 mg / mL on the 30th day and 0.25 mg / mL on the 60th day.
[0069] Comparative Example 3
[0070] A mouthwash, the components and weight percentages of the components are as follows:
[0071] Povidone-iodine granules 3%; sodium alginate 1%; sodium lauryl sulfate 0.2%;
[0072] 0.01% fruit essence; 0.01% xylitol; the balance is water, and the surface of the povidone-iodine particles is coated with a starch layer.
[0073] The preparation method of the mouthwash is as follows: (1) preparing povidone iodine particles coated with starch on the surface: weighing povidone iodine particles and starch powder at a mass ratio of 100:3; adding starch into water at a solid content of 5%, stirring continuously and gelatinizing at 70° C. for 20 minutes, with a stirring rate of 500 r / min to obtain a gelatinized starch solution, and cooling to room temperature; grinding the povidone iodine particles to an average particle size of 20 to 80 μm, adding the ground povidone iodine particles into the gelatinized starch solution, stirring continuously for 40 minutes, filtering, washing with water, and drying to obtain the mouthwash;
[0074] (2) Add a thickener, a sweetener, a surfactant, and a flavor to water in sequence, stir and disperse them uniformly, then add the starch-coated povidone-iodine particles obtained in step (1), stir and disperse them, and then take them out to obtain a mouthwash. After testing, the mouthwash has no stratification or precipitation within 30 days, a small amount of white matter precipitates at the bottom of the mouthwash after 60 days of storage, no effective iodine is detected on the 30th and 60th days of the mouthwash, and after adding salivary amylase, the effective iodine on the 30th day is 0.295 mg / mL, and the effective iodine on the 60th day is 0.27 mg / mL.
[0075] Comparative Example 4
[0076] A mouthwash, the components and weight percentages of the components are as follows:
[0077] Povidone-iodine granules 3%; sodium alginate 1%; sodium lauryl sulfate 0.2%;
[0078] 0.01% fruit essence; 0.01% xylitol; the balance is water, and the surface of the povidone-iodine particles is coated with β-cyclodextrin.
[0079] The preparation method of the mouthwash is as follows: (1) preparing povidone iodine particles coated with β-cyclodextrin on the surface: weighing povidone iodine particles and β-cyclodextrin powder in a mass ratio of 100:3; grinding the povidone iodine particles to an average particle size of 20 to 80 μm, mixing the ground povidone iodine particles with β-cyclodextrin, stirring for 40 minutes and then drying to obtain the mouthwash;
[0080] (2) Add a thickener, a sweetener, a surfactant, and a flavor to water in sequence, stir and disperse them uniformly, then add the surface-coated povidone-iodine particles obtained in step (1), stir and disperse them, place them in a micro mixer, shear and mix them at a shear energy of 800 KJ / L for 40 minutes, and then take them out to obtain a mouthwash. After testing, the mouthwash has no stratification or precipitation, and the appearance of the mouthwash is stable and uniform after being placed for 60 days. No effective iodine is detected in the mouthwash on the 30th and 60th days. After adding salivary amylase, the effective iodine on the 30th day is 0.158 mg / mL, and the effective iodine on the 60th day is 0.163 mg / mL.
[0081] From the test results in the above embodiments and comparative examples, it can be seen that the starch-coated povidone iodine mouthwash prepared by the specific method of the present application has good heat stability, and the effective iodine content of the povidone iodine mouthwash not coated with a starch layer decreases significantly after 60 days, mainly because the active iodine has poor stability. As the active iodine decreases, the povidone iodine continues to release elemental iodine and is continuously consumed, resulting in a continued decrease in the effective iodine content in the mouthwash and reduced antibacterial performance. Although cyclodextrin coating can also improve the stability of low-concentration povidone iodine solutions, β-cyclodextrin has good stability, and its coated povidone iodine is not easy to contact with water to release active iodine. Using it as a mouthwash cannot release active iodine in time for antibacterial and antiviral disinfection, and the effect of an antibacterial mouthwash cannot be obtained. At the same time, it was found that the starch-coated povidone-iodine particles have a large number of hydroxyl groups on their surface. Some of the hydroxyl groups on the starch surface will form hydrogen bonds in the mouthwash, causing the particles to precipitate, affecting the content of the antibacterial agent in the mouthwash. If the starch ratio is low, the povidone-iodine cannot be completely coated. When the prepared mouthwash antibacterial agent comes into contact with water, the povidone-iodine will begin to release iodine, causing the mouthwash to gradually become ineffective, affecting the product life.
[0082] A mouthwash and its preparation method are described in detail above. The above content is a further detailed description of the present invention in combination with specific preferred embodiments. It cannot be determined that the specific implementation of the present invention is limited to these descriptions. For ordinary technicians in the technical field to which the present invention belongs, without departing from the concept of the present invention, its architecture can be flexible and can derive a series of products. Just making a few simple deductions or substitutions should be regarded as belonging to the scope of patent protection of the present invention determined by the submitted claims.
Claims
1. A mouthwash, characterized in that: Its components and the weight percentage of each component are as follows: The surface of the povidone-iodine particles is coated with a starch layer.
2. The mouthwash according to claim 1, characterized in that The mass of the starch layer is 2% to 5% of the mass of the povidone-iodine particles.
3. The mouthwash according to claim 1, characterized in that The average particle size of the povidone-iodine particles is 1 to 100 μm.
4. The mouthwash according to claim 1, characterized in that The preparation method of the povidone iodine particles coated with starch on the surface is as follows: weigh povidone iodine particles and starch powder in proportion; add starch into water at a solid content of 5% to 10%, continuously stir and gelatinize at 70 to 90° C. for 20 to 60 minutes, and the stirring rate is 300 to 800 r / min to obtain a gelatinized starch solution, and cool to room temperature; grind the povidone iodine particles to an average particle size of 1 to 100 μm, add the ground povidone iodine particles into the gelatinized starch solution, continuously stir for 30 to 60 minutes, filter, wash with water, and dry to obtain povidone iodine particles coated with a starch layer on the surface.
5. The mouthwash according to claim 4, characterized in that The mass ratio of the povidone-iodine particles to the starch is 100:2-5.
6. The mouthwash according to claim 1, characterized in that The thickener is selected from one or more of ethyl cellulose, hydroxypropyl methylcellulose, sodium carboxymethyl cellulose, cross-linked sodium polyacrylate, guar gum, sodium alginate, and carrageenan; the surfactant is selected from one or more of sodium dodecyl sulfate, sodium dodecylbenzene sulfonate, sodium lauryl sulfate, sodium lauroyl sarcosinate, sodium cocoyl glycinate, and sodium acyl glutamate; the flavor is selected from one or more of tea flavor, mint flavor, fruit flavor, flower flavor, and bamboo flavor; the sweetener is selected from one or more of saccharin sodium, sucralose, xylitol, sodium cyclamate, aspartame, stevioside, or mogroside.
7. The mouthwash according to claim 1, characterized in that Its components and the weight percentage of each component are as follows: The average particle size of the povidone-iodine particles is 50-100 μm, and the surface of the povidone-iodine particles is coated with a starch layer accounting for 2%-5% of the mass of the povidone-iodine particles.
8. A method for preparing the mouthwash according to any one of claims 1 to 7, characterized in that: The following steps are involved: (1) preparing povidone iodine particles coated with starch, the method is as follows: weighing povidone iodine particles and starch powder in proportion; adding starch to water at a solid content of 5% to 10%, stirring continuously and gelatinizing at 70 to 90° C. for 20 to 60 minutes, stirring at a rate of 300 to 800 r / min to obtain a gelatinized starch solution, and cooling to room temperature; grinding the povidone iodine particles to an average particle size of 1 to 100 μm, adding the ground povidone iodine particles to the gelatinized starch solution, stirring continuously for 30 to 60 minutes, filtering, washing with water, and drying to obtain the product; (2) Add a thickener, a sweetener, a surfactant, and a flavor to water in sequence, stir and disperse them evenly, then add the starch-coated povidone-iodine particles obtained in step (1), stir and disperse them, place them in a micro mixer for shear mixing for 30 to 200 minutes, and then take them out to obtain a mouthwash.
9. The preparation method according to claim 8, characterized in that: The shear energy of the micro mixer during shear mixing is 300-1000 KJ / L.
10. A method for using the mouthwash according to any one of claims 1 to 7, characterized in that: There is no need to dilute with water when using. Just rinse your mouth for 60 to 100 seconds and then spit it out.
Citation Information
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