Oral care product compatible with capsule and preparation method of oral care product

Abstract

The invention relates to the technical field of oral care products, in particular to an oral care product compatible with capsules and a preparation method of the oral care product. The invention discloses an oral care composition compatible with capsules. Raw materials of the oral care composition comprise conventional components and skeleton components, the skeleton component is prepared from the following components in parts by weight: 10 to 80 parts of poloxamer, 0.1 to 1 part of carbomer, 0.1 to 1 part of polyvinylpyrrolidone and 5 to 20 parts of glyceryl triacetate; the conventional components comprise 10-30 parts of an abrasive and 1-3 parts of a surfactant. According to the technical scheme, the technical problem that an existing oral care product which is ideal in cleaning effect and fresh and cool in taste is not ideal in compatibility with a capsule shell can be solved. According to the technical scheme, the poloxamer, the polyvinylpyrrolidone, the carbomer and the glyceryl triacetate are jointly used to form a skeleton component, so that the compatibility of the inner material and the capsule shell is improved, and the oral care product which is compatible with the capsule shell, fresh and cool in taste and stable in inner material is formed, so that the satisfaction degree of consumers is improved.

Description

Technical Field

[0001] The invention relates to the technical field of oral care products, and in particular to an oral care product compatible with capsules and a preparation method thereof. Background Art

[0002] With the improvement of people's living standards and the continuous improvement of consumers' pursuit of oral health and appearance, the growth of emerging oral categories has accelerated, and oral care products with diverse functions and high appearance have become more and more popular among consumers. Oral care product form innovation has also begun to break through category boundaries, and the new oral care experience brought by new packaging and new interactions has become a new demand of consumers. At present, traditional oral care products are highly homogenized, and are basically packaged in the form of composite tubes, pump tubes, etc., which are relatively simple in terms of usage, product form, and user experience.

[0003] Soft capsules refer to dosage forms made by sealing a certain amount of raw materials, raw material extracts and appropriate excipients in spherical, elliptical or other shaped soft capsules. Currently, they are mostly used in the pharmaceutical industry. Soft capsules are suitable for extracts and fat-soluble ingredients, and the filling capacity can be adjusted in a wide range. If this packaging form is applied to oral care products, the effective ingredients of oral care products can be used accurately and quantitatively. At the same time, different soft capsule shapes and capsule colors can be used to distinguish different effects and different flavors, so that consumers can carry them with them and perform corresponding oral care according to different oral health needs and usage scenarios. It has a great market economic prospect.

[0004] The commonly used materials for soft capsule shells are glycerol (plasticizer), gelatin and water. Glycerol and water are placed in a gelatin boiling pot for heating, mixed evenly, expanded gelatin is added, stirred, melted, kept warm, vacuumed, filtered, and loaded into an automatic rotary capsule rolling machine for pressing. The soft capsule shell material and soft capsule preparation process have high requirements for the capsule core wrapping liquid, such as the wrapping liquid does not contain water and hydrophilic substances, and the fluidity of the wrapping liquid is good. Patent CN109662953B discloses a vitamin D soft capsule, the capsule inner material is composed of calcium carbonate, soybean oil, corn oil, vitamin D3, butylated hydroxytoluene, and glyceryl monostearate, and the inner material is composed of oily and lipophilic components. However, the moisturizing components of oral care products are all hydrophilic substances, such as glycerol, sorbitol, polyethylene glycol, etc., and conventional oral care products and capsule shells have incompatible technical problems. Patent CN111700825B discloses an oral health care oily composition composed of cold-pressed virgin coconut oil, cold-pressed virgin olive oil, cold-pressed virgin sesame oil, cold-pressed virgin evening primrose oil, cold-pressed virgin rosehip oil, calendula extract oil and a small amount of essential oil. The composition does not contain hydrophilic liquid, abrasive, surfactant, etc. Although the mouthfeel is soft, it is greasy compared with conventional oral care products, has poor cleaning power, and has not been verified for compatibility with capsule shells. Therefore, a new oral care product formula is urgently needed to solve the technical problem of compatibility with capsule shells, and at the same time has good cleaning effect and refreshing taste. Summary of the invention

[0005] The present invention aims to provide an oral care composition that is compatible with capsules, so as to solve the technical problem that the existing oral care products with ideal cleaning effect and refreshing taste are not compatible with the capsule shell. The technical solution improves consumer satisfaction by providing an oral care product that is compatible with the capsule shell, has a refreshing taste, and has stable internal materials.

[0006] In order to achieve the above object, the present invention adopts the following technical scheme:

[0007] An oral care composition compatible with capsules, the raw materials of which include conventional ingredients and skeleton ingredients; in parts by weight, the skeleton ingredients include 10-80 parts of poloxamer, 0.1-1 parts of carbomer, 0.1-1 parts of polyvinyl pyrrolidone and 5-20 parts of triacetin; the conventional ingredients include 10-30 parts of abrasives and 1-3 parts of surfactants.

[0008] The technical solution also provides a method for preparing an oral care composition that is compatible with capsules, comprising the following steps performed in sequence:

[0009] S1: Poloxamer and carbomer are mixed and stirred evenly to obtain system I;

[0010] S2: Add polyvinyl pyrrolidone and triacetin to system I and stir evenly to obtain system II;

[0011] S3: Add a friction agent and a surfactant to system II and stir thoroughly to obtain system III;

[0012] S4: vacuum degassing the system III to obtain the oral care composition.

[0013] The technical solution also provides a capsule product containing an oral care composition compatible with a capsule, comprising a capsule shell; the oral care composition is encapsulated in the capsule shell; in parts by weight, the capsule shell comprises 35-42 parts of a matrix, 15-25 parts of glycerol, and 35-45 parts of water.

[0014] Furthermore, the molecular weight of poloxamer is 1000-2500, 10≤HLB value≤20; the molecular weight of polyvinyl pyrrolidone is 44000-54000.

[0015] Furthermore, the conventional ingredients also include 0-5 parts of effective ingredients, 1-3 parts of sweeteners and 0.5-1.5 parts of aroma regulators.

[0016] Further, the friction agent includes at least one of silicon dioxide, stone powder and calcium hydrogen phosphate;

[0017] The surfactant comprises at least one of sodium lauryl sulfate, cocamidopropyl betaine, potassium cocoyl glycinate, sodium cocoyl glycinate, sodium lauroyl sarcosinate, sodium laureth sulfate and triethanolamine cocoyl glutamate;

[0018] The sweetener includes at least one of saccharin sodium, aspartame, stevia and sucralose;

[0019] The aroma regulator includes at least one of mint essence, spearmint essence, tea essence, floral essence, fruit essence, etc.;

[0020] The effective ingredients include at least one of an anti-allergic ingredient, a whitening ingredient, an antibacterial ingredient, an ingredient for relieving gum swelling and pain, and a hemostatic ingredient.

[0021] Furthermore, the matrix includes edible starch and / or gelatin; edible starch includes starch from natural sources and / or modified starch; starch from natural sources includes at least one of corn starch, potato starch, cassava starch, wheat starch, mung bean starch and rice starch; modified starch includes at least one of oxidized starch, cationic starch, esterified starch, cross-linked starch and hydroxypropyl starch; gelatin includes at least one of cowhide gelatin, pig skin gelatin, fish skin gelatin, bovine bone gelatin, pig bone gelatin and fish bone gelatin.

[0022] Furthermore, the capsule shell also includes 0.1-2 parts of edible flavor, 0.1-5 parts of sweetener, 0.1-1 parts of colorant, and 0-3 parts of thickener.

[0023] Furthermore, the sweetener includes at least one of saccharin sodium, aspartame, stevia and sucralose; the thickener includes at least one of carrageenan, xanthan gum, sodium carboxymethyl cellulose, gellan gum and propylene glycol alginate; the edible flavor includes at least one of sweet orange flavor, cherry flavor, strawberry flavor, lime flavor, mint essential oil, edible apple flavor, edible mint flavor and edible orange flavor; the colorant includes at least one of carmine, new red, amaranth, allura red, erythrosine, azorubin, lemon yellow, sunset yellow, chlorophyll, brilliant blue, anthocyanin, cocoa shell pigment, iron oxide, caramel color, carbon black and brilliant black.

[0024] Furthermore, the preparation method of the capsule shell is: glycerol, matrix and water are mixed and heated to 55-80°C, and stirred while heating; after reaching 55-80°C, the mixture is boiled for 10 minutes, and then a pre-prepared edible flavor solution, colorant solution, thickener solution and sweetener solution are added; the mixture is boiled for 0-50 minutes under stirring conditions and then vacuum degassed to obtain a capsule shell solution.

[0025] The principle of this technical solution is as follows:

[0026] Glycerol triacetate is an organic compound with the molecular formula C9H 14 O6, colorless oily liquid, with a faint fruity and sweet taste, bitter at low concentrations, mainly used as a fixative in flavor formulations in the field of daily chemicals; Poloxamer is a new type of high molecular non-ionic surfactant, a polyoxyethylene polyoxypropylene ether block copolymer, easily soluble in water or ethanol, with a molecular weight ranging from 1000 to more than 7000, and is a compound with different lipophilic water balance values ​​copolymerized by an appropriate amount of polyoxypropylene and an appropriate amount of polyoxyethylene. It is mainly used as an emulsifier or solubilizer in the field of daily chemicals; Carbomer is a nano-scale acrylic resin, containing The carboxylic acid group (-COOH) should be 56.0%-68.0%. It is a very important rheology regulator. The neutralized carbomer is an excellent gel matrix with important uses such as thickening and suspension. Polyvinylpyrrolidone (PVP), referred to as PVP, is a non-ionic high molecular compound of N-vinylamide polymers. In daily cosmetics, PVP and copolymers have good dispersibility and film-forming properties. PVP has the function of protective colloid in emulsions and can be used in fatty and non-fatty pastes.

[0027] The inventor accidentally discovered during the research and development process that when the capsule skin wraps the hydrophilic inner material, such as when the moisturizer is glycerol, sorbitol, or polyethylene glycol, the capsule will have serious concave, deflated pills, and oily capsule surface at room temperature. After the accelerated test, the inner material is stratified, thickened, or dried up, and the capsule shell surface is thickened and elastic. Triacetin is generally used as a fixative in the flavor formula in the field of daily chemicals. When the amount of triacetin in the formula is increased, the phenomenon of capsule concave and deflated pills is alleviated. However, triacetin has a bitter taste, and for oral care products, mouthfeel is very important, so triacetin is not suitable for large-scale use. This technical solution replaces the glycerol commonly used in toothpaste with triacetin, and simultaneously adds poloxamer, carbomer, and polyvinyl pyrrolidone, which improves the compatibility between the oral care composition (inner material) and the capsule shell and the stability of the inner material. Further solves the technical problem that the compatibility of existing oral care products with ideal cleaning effect and refreshing taste and capsule shells is not ideal. The inventors analyzed that the reason is that the four substances can form a stable skeleton structure under a certain preparation process, thereby improving the stability of the capsule. Poloxamer is a triblock copolymer polymerized by polyoxypropylene (PPO) and polyoxyethylene (PEO). PEO is relatively hydrophilic and PPO is relatively lipophilic. Due to the hydrophobic effect, PPO aggregates with triacetin to form a uniformly mixed macromolecular structure. The carbomer molecular structure contains acidic groups and has hydrophilic properties. It aggregates with PEO in the poloxamer molecule through hydrogen bonds. Polyvinylpyrrolidone is an amphiphilic polymer with a special structure. The CC bond on the main chain is a hydrophobic segment with lipophilicity, and the pyrrolidone group is a hydrophilic group. The CC bond is a hydrophobic segment that aggregates with poloxamer PPO, and the hydrophilic group of the pyrrolidone group aggregates with carbomer. In the macromolecular structure formed by poloxamer, carbomer and triacetin, cross-filling is carried out to form a tightly arranged and stable gel state. The phenomena of stratification, roughening, thickening and thinning of the internal material are all solved, and the capsule shell does not become thicker, lose elasticity or have oil on the surface.

[0028] The beneficial effects of this technical solution are summarized as follows:

[0029] (1) The oral care products containing the composition have good compatibility with the capsule skin, which innovates the packaging form of oral care products. This product form abandons the traditional tube packaging of toothpaste paste. The shape of the capsule skin can be designed in a variety of ways according to the preferences of consumers, subverting the unchanging use experience of toothpaste.

[0030] (2) The oral care product system containing the composition provided by the present invention is stable and belongs to an anhydrous system. The inner material is wrapped by the capsule skin, and the chance of contamination is reduced, which not only facilitates transportation but also extends the shelf life of the product, is naturally safe, and has quality assurance. Due to the above reasons, no or less preservatives can be used in freeze-dried products. In the prior art, paste toothpaste contains water and nutrients. In order to prevent the growth of microorganisms and reasonably extend the shelf life of the product, some toothpastes usually add preservatives to ensure that the product will not deteriorate during the use period. Because preservatives have potential carcinogenicity, irritation and allergy problems, the use of preservatives in toothpaste is controversial.

[0031] (3) The oral care product system containing the present composition forms a gel system, which avoids the influence of moisture in conventional oral care products on active substances, can ensure the activity of various active substances in the products, and expand the application of active substances in oral cleaning products. For example, the anhydrous system has a good protective effect on active substances such as vitamins, vitamin-like substances, tea polyphenols, grape seed polyphenols, protein peptides, fungi, etc. The above-mentioned active substances are easily inactivated in an aqueous environment, and the water content of conventional oral cleaning products is relatively high, and the efficacy of the active substances cannot be guaranteed. For another example, in the prior art, bioactive glass-ceramic materials release calcium ions and phosphate ions in an aqueous environment to exert their effects. In an aqueous system, the bioactive glass-ceramic materials cannot maintain their activity for a long time, which limits the application of this active ingredient in oral care products. BRIEF DESCRIPTION OF THE DRAWINGS

[0032] Figure 1 This is the typical appearance of oral care capsules of different shapes successfully prepared by this technical solution.

[0033] Figure 2 This is a typical photograph of the conventional oral care capsules containing products in the prior art of Experimental Example 1 after accelerated testing.

[0034] Figure 3 These are typical photographs of the capsule of Example 1 of Experimental Example 1 after the accelerated test (the top is the appearance of the capsule, and the bottom is the state of the capsule after being cut open).

[0035] Figure 4 These are typical photos of the capsule of Comparative Example 1 of Experimental Example 1 after the accelerated test (the top is the appearance of the capsule, and the bottom is the state of the capsule after being cut open).

[0036] Figure 5 These are typical photos of the capsules of Comparative Example 3 of Experimental Example 1 after the accelerated test (the top is the appearance of the capsule, and the bottom is the state of the capsule after being cut open).

[0037] Figure 6These are typical photos of the capsule of Comparative Example 8 of Experimental Example 1 after the accelerated test (the top is the appearance of the capsule, and the bottom is the state of the capsule after being cut open). DETAILED DESCRIPTION

[0038] The present invention is further described in detail below in conjunction with examples, but the embodiments of the present invention are not limited thereto. Unless otherwise specified, the technical means used in the following examples and experimental examples are conventional means well known to those skilled in the art, and the materials, reagents, etc. used can be obtained from commercial sources.

[0039] Embodiment 1:

[0040] (1) Composition ingredients

[0041] An oral care composition compatible with capsules, the raw materials of which include conventional ingredients and skeleton ingredients. In parts by weight, the skeleton ingredients include 10-80 parts of poloxamer, 0.1-1 parts of carbomer, 0.1-1 parts of polyvinyl pyrrolidone, and 5-20 parts of triacetin; the conventional ingredients include 10-30 parts of abrasives and 1-3 parts of surfactants.

[0042] In order to enhance the use experience of the oral care composition, 1-3 parts of a sweetener and 0.5-1.5 parts of an aroma regulator may be added to the conventional ingredients.

[0043] In order to increase the functionality of the oral care composition, 0-5 parts of effective ingredients may be added to the conventional ingredients.

[0044] Among them, poloxamer can be selected with a molecular weight of 1000-2500 and an HLB value of 10≤≤20. The subsequent experiments of this scheme will use poloxamer 105 model (optional supplier: Hai'an Petrochemical Plant, Jiangsu Province); in this scheme, the model of carbomer is 956 (optional supplier: Lubrizol Specialty Chemical Manufacturing (Shanghai) Co., Ltd.); triacetin is a food-grade raw material (optional supplier: Wuhan Lanabai Pharmaceutical Chemical Co., Ltd.); polyvinylpyrrolidone (PVP) can be selected with a molecular weight of 44000-54000, and the specific model selected for subsequent experimental research in this scheme is K30 (optional supplier: Guangdong Yuemei Chemical Co., Ltd.).

[0045] The friction agent includes at least one of silicon dioxide, stone powder and calcium hydrogen phosphate. The friction agent is a conventional component in the prior art and has the advantages of stable properties and safety.

[0046] The surfactant includes at least one of sodium lauryl sulfate, cocamidopropyl betaine, potassium cocoyl glycinate, sodium cocoyl glycinate, sodium lauroyl sarcosinate, sodium laureth sulfate and triethanolamine cocoyl glutamate. The above surfactants are all commonly used substances in the prior art, with suitable prices and easy to obtain.

[0047] The sweetener includes at least one of saccharin sodium, aspartame, stevia and sucralose. The aroma modifier includes at least one of mint flavor, spearmint flavor, tea flavor, flower flavor, fruit flavor, etc. Sweeteners and flavors are added to oral care products to cover up the bad taste of certain ingredients in toothpaste and give the toothpaste a pleasant taste.

[0048] The effective ingredients include at least one of an anti-allergic ingredient (such as potassium nitrate), a whitening ingredient (such as sodium phytate), an antibacterial ingredient (such as zinc lactate), an ingredient for relieving gum swelling and pain (such as zinc citrate) and a hemostatic ingredient (such as tranexamic acid).

[0049] (2) Composition Preparation Method

[0050] A method for preparing an oral care composition compatible with capsules comprises the following steps:

[0051] S1: Poloxamer (specifically, poloxamer 105 type, liquid, having HLB <20 and PO chain (polyoxypropylene chain) <30) and carbomer 956 are mixed and stirred evenly to obtain system I;

[0052] S2: Add polyvinyl pyrrolidone and triacetin to system I and stir evenly to obtain system II;

[0053] S3: Add a friction agent and a surfactant to system II and stir thoroughly to obtain system III;

[0054] S4: Vacuum degassing the system III, and the paste making is completed to obtain an oral care composition (solution state) that is compatible with capsules.

[0055] If it is necessary to selectively add sweeteners, aroma modifiers and functional ingredients to the oral care composition, S3 can be adjusted to:

[0056] S3: Add abrasives, surfactants, sweeteners and functional ingredients to system II and stir thoroughly; then add aroma regulators and stir thoroughly to obtain system III.

[0057] The oral care composition is then loaded into a capsule shell to obtain the oral care capsule of the present invention. The main raw materials of the capsule shell used in the present invention include 35-42 parts of a matrix, 15-25 parts of glycerol, 35-45 parts of water, and according to the needs, the following can be selectively added in appropriate amounts: 0.1-2 parts of edible flavor, 0.1-5 parts of sweetener, 0.1-1 parts of colorant, and 0-3 parts of thickener.

[0058] The matrix includes edible starch and / or gelatin. Edible starch is starch from various natural sources and / or modified starch. Starch from natural sources includes at least one of corn starch, potato starch, cassava starch, wheat starch, mung bean starch and rice starch; modified starch includes at least one of oxidized starch, cationic starch, esterified starch, cross-linked starch and hydroxypropyl starch. Gelatin includes at least one of cowhide gelatin, pig skin gelatin, fish skin gelatin, bovine bone gelatin, pig bone gelatin and fish bone gelatin.

[0059] The sweetener includes at least one of saccharin sodium, aspartame, stevioside and sucralose. The thickener includes at least one of carrageenan, xanthan gum, sodium carboxymethyl cellulose, gellan gum and propylene glycol alginate; the edible flavor includes at least one of sweet orange flavor, cherry flavor, strawberry flavor, lime flavor, mint essential oil, edible apple flavor, edible mint flavor and edible orange flavor; the colorant (edible pigment) includes at least one of carmine, new red, amaranth, allure red, erythrosine, azorubin, lemon yellow, sunset yellow, chlorophyll, brilliant blue, anthocyanin, cocoa shell pigment, iron oxide, caramel color, carbon black and brilliant black.

[0060] The production process of capsule shell: weigh the edible flavor, colorant (edible pigment), thickener and sweetener in the formula amount, dissolve them with purified water respectively, and set aside after they are completely dissolved. Take the glycerin and matrix in the formula amount, and the remaining purified water into the gelling tank, start stirring and heating; when the temperature in the tank reaches the range of 55-80℃ (for the sake of specific examples, the subsequent experiments specifically use 70℃), boil for 10-60min (for the sake of specific examples, the subsequent experiments specifically use 30min). When it is boiled for more than 10min, turn off the stirring and open the lid of the gelling tank, add the edible flavor solution, edible pigment solution and sweetener solution, close the lid, and quickly start stirring until the matrix is ​​completely gelatinized. After the boiling is completed, close the air valves at the lid of the tank, open the vacuum valve and vacuum pump for degassing and defoaming; keep the capsule shell solution warm (the temperature is set to 70℃~90℃) and set aside.

[0061] Next, the oral care composition (inner material) is loaded into the capsule formed according to the conventional method of the prior art by the conventional method of the prior art. The oral care composition solution is poured into the liquid preparation tank; the material conveying pipeline of the glue tank and the glue box, the conveying pipeline of the liquid preparation tank and the oral care composition, and the compressed air pipeline of the molding host and the glue tank are installed; after installation, the compressed air valve and the host power supply are opened, the glue box and the material conveying pipe are heated, and the temperature of the glue box is set to 80°C. When the temperature of the glue box and the material conveying pipe reaches 80°C, the flow regulating valve is opened to adjust the thickness of the wrapping layer (the thickness of the capsule shell is controlled to be about 0.80mm), and the indoor temperature (24°C) and relative humidity (20%) are controlled at the same time; after the thickness of the wrapping layer is qualified, the spray body is put down, adjusted to the appropriate spray body height, and the mold is cast, and the amount of each capsule is detected. When the amount reaches the requirement of ±7.5%, the prepared capsule is passed through the conveyor belt into the rotating cage for cooling and shaping. The above process is the conventional capsule skin production and content canning process of the prior art, which will not be repeated here.

[0062] The typical appearance of oral care capsules of different shapes successfully prepared by this technical solution can be seen in Figure 1 .

[0063] According to the culture in Table 1, the oral care composition (inner material) and the corresponding capsule of the example were prepared.

[0064] Table 1: Formula composition of the embodiment

[0065]

[0066]

[0067] The preparation of the oral care capsules of the comparative examples is basically the same as that of Example 1, except for the composition and dosage of the skeleton components. For specific differences, see Table 2. In the preparation process of each comparative example, if a certain material is missing, the material is not added in the process step, and the preparation process is carried out with reference to the preparation process of Example 1. In addition, for the formula of Example 1, a portion of the capsules is added with carmine colorant, and the other portion of the capsules is not added with colorant in order to accelerate the experiment and facilitate observation. And for the sake of observation, all comparative examples are carried out with reference to the case where no colorant is added in Example 1.

[0068] Table 2: Comparative Example Formulation

[0069] raw material Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 Comparative Example 5 Comparative Example 6 Comparative Example 7 Poloxamer 50 servings 0 copies 50 servings 0 copies 0 copies 50 servings 50 servings Carbomer 0.5 serving 0 copies 0 copies 0 copies 0.5 serving 0.5 serving 0 copies PVP 0.5 serving 0 copies 0 copies 0.5 serving 0 copies 0 copies 0.5 serving Triacetin other* 10 servings 10 servings 10 servings 10 servings 10 servings 10 servings

[0070] *Indicates that triacetin is not used, but 10 parts of glycerol is used instead of triacetin, i.e.: a traditional toothpaste moisturizer is used.

[0071] Comparative Example 8

[0072] This comparative example is basically the same as Example 1, except that the preparation method of the oral care composition comprises the following steps:

[0073] S1: Poloxamer, carbomer, polyvinyl pyrrolidone and triacetin are mixed and stirred to obtain system I;

[0074] S3: Add abrasive, surfactant, and sweetener to system I and stir thoroughly; then add aroma regulator and stir thoroughly to obtain system II;

[0075] S3: Vacuum degassing the system II, and the paste preparation is completed to obtain an oral care composition.

[0076] In this comparative example, poloxamer, carbomer, polyvinyl pyrrolidone and triacetin are mixed in one step. The above oral care composition is used to prepare capsules. The preparation method is shown in Example 1.

[0077] Comparative Example 9

[0078] This comparative example is basically the same as Example 1, except that the preparation method of the oral care composition comprises the following steps:

[0079] S1: mixing poloxamer and triacetin, and stirring evenly to obtain system I;

[0080] S2: Add polyvinyl pyrrolidone and carbomer to system I and stir evenly to obtain system II;

[0081] S3: Add abrasives, surfactants, and sweeteners to system II and stir thoroughly; then add aroma regulators and stir thoroughly to obtain system III.

[0082] S4: vacuum degassing the system III, and the paste making is completed to obtain an oral care composition that is compatible with capsules.

[0083] The above oral care composition is used to prepare capsules. The preparation method is shown in Example 1.

[0084] Comparative Example 10

[0085] This comparative example is basically the same as Example 1, except that the preparation method of the oral care composition comprises the following steps:

[0086] S1: mixing poloxamer and polyvinyl pyrrolidone, and stirring evenly to obtain system I;

[0087] S2: Add carbomer and triacetin to system I and stir evenly to obtain system II;

[0088] S3: Add abrasives, surfactants, and sweeteners to system II and stir thoroughly; then add aroma regulators and stir thoroughly to obtain system III.

[0089] S4: vacuum degassing the system III, and the paste making is completed to obtain an oral care composition that is compatible with capsules.

[0090] The above oral care composition is used to prepare capsules. The preparation method is shown in Example 1.

[0091] Experimental Example 1: Capsule Evaluation

[0092] The capsules prepared in the examples and comparative examples were scored. The problems with the capsules were mainly manifested in: whether the capsule shell leaked oil, whether the capsule contents (i.e., the oral care composition filled in the capsule shell) were layered, whether the capsule appearance was concave, and the capsule elasticity effect. The prepared capsule products were placed in an environment with a temperature of 40°C ± 2°C and a relative humidity of 75% ± 5% for an accelerated experiment for 3 months, and then the capsules were observed and scored. The accelerated stability experiment was conducted with 3 batches of test products. The test products should be products of the enlarged test, and the packaging of the test products should be consistent with the marketed products. The scoring criteria are as follows:

[0093] Whether the capsule is dented or oily: 1-10 points; 1 point is very serious, the capsule shell has oil (the oil can be observed on the capsule surface), the capsule is obviously dented, and the volume of the capsule is reduced by more than half (after the capsule is cut open, the inner material becomes dry and powdery); 10 points means no dents, the capsule is full, and the capsule skin is dry and oil-free. The pass mark for this item is a score ≥8.

[0094] Capsule elasticity: 1-10 points; 1 point means very poor elasticity, after the capsule is cut open, the capsule skin is pulled and there is basically no deformation; 10 points means good elasticity, no difference compared with the blank capsule skin. The pass mark for this item is a score ≥8.

[0095] Open the capsule to observe the state of the inner material: the ideal inner material should be fine, smooth, and without stratification. If the inner material is slightly thin or thick, or slightly rough or slightly stratified, it is acceptable as long as the situation is not serious. However, if the inner material is obviously stratified (for example, liquid and powder are separated), the inner material is too viscous and rough, or even becomes dry powder, such products will be judged as unqualified products.

[0096] The thickness of the capsule skin was tested. The thickness of the capsule skin prepared in this scheme was about 0.8 mm. After the accelerated experiment, the thickness of the capsule skin needed to be controlled between 0.75 mm and 0.85 mm.

[0097] Take several capsules from the same batch after accelerated testing, extrude and mix the inner materials to test the viscosity and consistency of the inner materials (a certain amount of samples is required for testing). The test results are the average of three parallel tests. The qualified standard for the viscosity of the inner materials is 40-90 kPa.s (T = 25 ° C), and the qualified standard for the consistency of the inner materials is 3-12 (T = 25 ° C).

[0098] The results of the accelerated test on the capsules obtained in the examples and comparative examples are shown in Table 3. Figure 2 The figure shows typical photos of capsules obtained after accelerated testing using conventional oral care products in the prior art as inner materials. Figure 2 Glycerin and PEG, which are commonly used in toothpaste, were added to the inner material of the capsule, causing the inner material of the capsule to dry out after the accelerated experiment, the surface of the capsule to dent, and the capsule to age to a certain extent.

[0099] Figure 3 The typical conditions of the capsules of Example 1 after the accelerated test are shown. The capsule surface is not oily and not concave. After the capsule is cut open, the inner material is fine and smooth with appropriate consistency and viscosity.

[0100] Figure 4 The following shows the typical conditions of the capsules of Comparative Example 1 after the accelerated test. The capsule shell surface is seriously oily, seriously concave, and the elasticity of the capsule shell is seriously deteriorated. After the capsule is opened, it is found that the inner material is thickened.

[0101] Figure 5 The following is a typical example of the capsules of Comparative Example 3 after the accelerated test. The capsule shell surface is seriously oily and concave, and after the capsule is cut open, it is found that the inner material is thick and very rough.

[0102] Figure 6 The following is a typical example of the capsule of Comparative Example 8 after the accelerated test. The capsule shell surface is oily, and after the capsule is cut open, it is found that the inner material is thinner, and further observation shows that the inner material has a certain granular feel.

[0103] Table 3: Acceleration test results

[0104]

[0105]

[0106] The experimental results in the above table are analyzed as follows:

[0107] (1) Observation results of capsule properties of the examples

[0108] It can be seen from the above experimental data that Example 1 of this scheme is the best implementation method. After the accelerated experiment, the capsule did not show oil discharge and concavity, and the capsule shell did not show thickening phenomenon and had ideal elasticity. The inner material of the capsule (the oral care composition filled in the capsule shell) is fine and smooth, and the viscosity and consistency meet the requirements. This shows that the compatibility between the oral care composition and the capsule shell of this embodiment is good, and the stability of the oral care composition is relatively ideal. The amount of poloxamer in Example 2 is increased, and the components of other capsule shells and oral care compositions have certain changes relative to Example 1.

[0109] The capsule of Example 2 has a slight oily surface and is slightly thicker, and the inner material is slightly stratified and thin, but the capsule appearance score, capsule shell thickness, capsule elasticity score, inner material viscosity, consistency and other indicators meet the requirements. Therefore, the product of Example 2 still meets the requirements.

[0110] In Example 3, the amount of poloxamer used is relatively reduced, and the components of other capsule shells and oral care compositions are somewhat different from those of Example 1. The capsules of Example 3 have a slight oily surface and are slightly thicker, and the inner material is slightly thicker, but the overall indicators of the capsules meet the requirements.

[0111] The friction agent in Example 4 is calcium hydrogen phosphate, and the amount of the friction agent is relatively increased, and the components of other capsule shells and oral care compositions are somewhat different from those in Example 1. The product of Example 4, except that the inner material has a slightly rough feel, meets the requirements in terms of overall indicators.

[0112] The friction agent in Example 5 is calcium hydrogen phosphate, and the amount of friction agent used is relatively reduced, and the components of other capsule shells and oral care compositions are somewhat different from those in Example 1. The capsule shell of Example 5 is slightly thicker, and the inner material is slightly layered and thin, and the overall indicators meet the requirements.

[0113] (2) Analysis of the effects of triacetin

[0114] Conventional toothpaste and other oral care products usually contain moisturizers (such as hydroxyl-containing substances such as glycerol). However, the purpose of this technical solution is to put oral care products into capsules. Since the components of the capsules include hydrophilic substances such as glycerol, it is necessary to avoid the presence of substances containing alcohol matrix in the inner material, otherwise the alcohol substances will migrate back and forth in the capsule shell, resulting in concave, deflated pills and other phenomena. For example, in Comparative Example 1, the inventors used glycerol (triacetin was not used), and the prepared capsules showed very serious concave phenomena. After the accelerated test, the inner material showed stratification, thickening or drying, and the surface of the capsule shell showed thickening, poor elasticity, concave and oily phenomena.

[0115] At the beginning of the research and development, the inventors conducted a lot of research and screening on moisturizers containing hydroxyl groups that can replace glycerol, and found that triacetin can effectively solve the problem of capsule concavity. The inventors used triacetin to prepare oral care products (toothpaste) for the first time, solving the problem of unsatisfactory compatibility between the contents and the capsule shell. Therefore, one of the key technical points for realizing the preparation of oral care capsules is to use triacetin to replace traditional moisturizers such as glycerol. The inventors further speculated on the technical principle of using triacetin: triacetin is an ester substance, which is not easy to migrate in the capsule shell, so the phenomenon of capsule concavity and deflated pills is alleviated.

[0116] (3) Use of skeleton components

[0117] Glyceryl triacetate is slightly soluble in water and has a small molecular polarity. The addition of glyceryl triacetate alone (without other skeleton components) will cause oiling. And after adding insoluble components such as abrasives to glyceryl triacetate, the suspension performance of glyceryl triacetate is poor, and the inner material shows stratification and thickening. Referring to the experimental results of Comparative Example 2, glyceryl triacetate is mixed with conventional ingredients to prepare the inner material (without adding poloxamer, carbomer, PVP), and the inner material shows thickening and roughening, and the surface of the capsule shell shows thickening, severe concave, and oiling of the capsule surface. It can be seen that the use of glyceryl triacetate alone cannot form a product with ideal performance in all aspects, and it needs to be used in combination with other materials.

[0118] In order to solve the above problems, the inventors have tried to add amphiphilic substances (such as poloxamer, polyvinyl pyrrolidone, etc.) and hydrophilic substances (such as carbomer, etc.) to the inner material formula. Poloxamer is often used as a solubilizer and surfactant in oral care products, while polyvinyl pyrrolidone and carbomer are often used as thickeners for oral care products. See Comparative Examples 3-5. In Comparative Example 3, triacetin and poloxamer are used in combination; in Comparative Example 4, triacetin and PVP are used in combination; in Comparative Example 5, triacetin and carbomer are used in combination, and there will be a serious oil discharge on the surface of the capsule shell, the capsule shell becomes thicker and the elasticity becomes worse, and the viscosity and consistency of the inner material are also increased. Therefore, the use of triacetin with poloxamer, polyvinyl pyrrolidone, and carbomer respectively is difficult to solve the problems of compatibility between the oral care composition and the capsule shell, and stability of the inner material of the oral care composition.

[0119] Comparative Example 6 uses poloxamer and carbomer together, and no polyvinyl pyrrolidone is added. The capsule shell surface oiling, thickening, and deterioration of the capsule shell elasticity are not alleviated, and the inner material is layered and thinned. Comparing Comparative Example 6 (containing poloxamer and carbomer), Comparative Example 4 (containing polyvinyl pyrrolidone) and Example 1, it can be seen that the combined use of poloxamer, carbomer and polyvinyl pyrrolidone can solve the problem of poor stability of the inner material. After the accelerated test, the viscosity, consistency, and state of the inner material meet the requirements. In particular, after the combined use of the three, the capsule shell oiling, unsatisfactory elasticity, and thickening of Comparative Example 6 and Comparative Example 4 disappeared, and the compatibility of the inner material and the capsule shell was improved.

[0120] Comparative Example 7 uses poloxamer and polyvinyl pyrrolidone in combination, without adding carbomer. The capsule shell surface oiling, thickening and deterioration of the capsule shell elasticity are not alleviated, and the inner material is stratified, and the viscosity and consistency are reduced. Comparing Comparative Example 7 (containing poloxamer and polyvinyl pyrrolidone), Comparative Example 5 (containing carbomer) and Example 1, it can be seen that the combined use of poloxamer, carbomer and polyvinyl pyrrolidone can solve the problem of poor stability of the inner material. After the accelerated test, the viscosity, consistency and state of the inner material meet the requirements. In particular, after the combined use of the three, the capsule shell oiling, unsatisfactory elasticity and thickening of Comparative Example 7 and Comparative Example 5 disappeared, and the compatibility of the inner material and the capsule shell was improved.

[0121] It can be seen that the effects of different amphiphilic substances and hydrophilic substances on the use of triacetin are very different, and it is necessary to use poloxamer, carbomer and polyvinyl pyrrolidone in combination. The inventor further analyzed the reasons for the excellent effect of the above-mentioned poloxamer, carbomer, polyvinyl pyrrolidone and triacetin in combination: poloxamer is a triblock copolymer polymerized by polyoxypropylene (PPO) and polyoxyethylene (PEO), PEO has relative hydrophilicity, PPO has relative lipophilicity, and PPO is aggregated with triacetin due to hydrophobic effect to form a uniformly mixed macromolecular structure. The carbomer molecular structure contains acidic groups and has hydrophilic properties, and is aggregated with PEO in the poloxamer molecule through hydrogen bonds. Polyvinyl pyrrolidone is an amphiphilic polymer with a special structure, and the CC bond on the main chain is a hydrophobic segment with lipophilicity, and the pyrrolidone group is a hydrophilic group. The CC bond is a hydrophobic segment that aggregates with poloxamer PPO, and the hydrophilic group of the pyrrolidone group aggregates with carbomer. In the macromolecular structure formed by poloxamer, carbomer, and triacetin, cross-filling is performed to form a tightly arranged, stable gel state. The phenomena of stratification, roughening, thickening, and thinning of the inner material are all solved, and the capsule shell does not become thicker, lose elasticity, or have oil on the surface. If the above four substances are not used together, the above stable structure will not appear.

[0122] In summary, the combined use of poloxamer, carbomer and polyvinyl pyrrolidone has a very significant benefit effect on the overall stability of capsules containing triacetin as the inner ingredient, which is specifically manifested in the stability of the inner material itself (no stratification, thickening, thinning, or roughening), and the stability of the capsule shell (no depression, maintenance of shell elasticity and thickness, and no surface oiling).

[0123] (4) The impact of production technology on the efficacy of skeleton structure

[0124] In the technical scheme, the preparation process of the oral care composition (inner material) is: firstly mix poloxamer and carbomer, then add polyvinyl pyrrolidone and triacetin and stir evenly, and finally add other conventional toothpaste ingredients. The above process sequence is critical for the efficacy of the skeleton structure.

[0125] In Comparative Example 8, poloxamer, carbomer, and polyvinyl pyrrolidone are mixed in one step, and other conventional toothpaste ingredients are added at last. In Comparative Example 9, poloxamer and triacetin are first mixed, and then polyvinyl pyrrolidone and carbomer are added and stirred evenly, and finally other conventional toothpaste ingredients are added. In Comparative Example 10, poloxamer and polyvinyl pyrrolidone are first mixed, and then carbomer and triacetin are added, and finally other conventional toothpaste ingredients are added. The above treatment methods will cause the inner material to become slightly thinner, and there will be a certain amount of oil on the surface of the capsule shell. The inventor speculates that only the preparation process adopted in this scheme can obtain the aforementioned "stable structure", thereby ensuring the compatibility between the inner material and the capsule shell, and ensuring the stability of the inner material and the capsule as a whole, thereby improving the product quality.

[0126] The above is only an embodiment of the present invention, and the common knowledge such as the known specific technical solutions and / or characteristics in the solution is not described in detail here. It should be pointed out that for those skilled in the art, without departing from the technical solution of the present invention, several modifications and improvements 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 practicality of the patent. The scope of protection required by this application shall be based on the content of its claims, and the specific implementation methods and other records in the specification can be used to interpret the content of the claims.

Claims

1. An oral care composition compatible with capsules, characterized in that: The raw materials include conventional ingredients and skeleton ingredients; in parts by weight, the skeleton ingredients include 10-80 parts of poloxamer, 0.1-1 parts of carbomer, 0.1-1 parts of polyvinyl pyrrolidone and 5-20 parts of triacetin; the conventional ingredients include 10-30 parts of abrasives and 1-3 parts of surfactants.

2. An oral care composition compatible with capsules according to claim 1, characterized in that: The molecular weight of poloxamer is 1000-2500, 10≤HLB value≤20; the molecular weight of polyvinylpyrrolidone is 44000-54000.

3. An oral care composition compatible with capsules according to claim 2, characterized in that: The conventional ingredients also include 0-10 parts of effective ingredients, 1-3 parts of sweeteners and 0.5-1.5 parts of aroma regulators.

4. An oral care composition compatible with capsules according to claim 3, characterized in that: The friction agent includes at least one of silicon dioxide, stone powder and calcium hydrogen phosphate; The surfactant includes at least one of sodium lauryl sulfate, cocamidopropyl betaine, potassium cocoyl glycinate, sodium cocoyl glycinate, sodium lauroyl sarcosinate, sodium laureth sulfate and triethanolamine cocoyl glutamate.

5. An oral care composition compatible with capsules according to claim 4, characterized in that: The sweetener includes at least one of saccharin sodium, aspartame, stevia and sucralose; The aroma regulator includes at least one of mint essence, spearmint essence, tea essence, floral essence, fruit essence, etc.; The effective ingredients include at least one of an anti-allergic ingredient, a whitening ingredient, an antibacterial ingredient, an ingredient for relieving gum swelling and pain, and a hemostatic ingredient.

6. A method for preparing a capsule-compatible oral care composition according to any one of claims 1 to 5, characterized in that: The method includes the following steps: S1: Poloxamer and carbomer are mixed and stirred evenly to obtain system I; S2: Add polyvinyl pyrrolidone and triacetin to system I and stir evenly to obtain system II; S3: Add a friction agent and a surfactant to system II and stir thoroughly to obtain system III; S4: vacuum degassing the system III to obtain the oral care composition.

7. A capsule product containing an oral care composition compatible with a capsule according to any one of claims 1 to 4, characterized in that: It comprises a capsule shell; the capsule shell contains the oral care composition; In parts by weight, the capsule shell comprises 35-42 parts of matrix, 15-25 parts of glycerol and 35-45 parts of water.

8. The capsule product according to claim 7, characterized in that: The matrix includes edible starch and / or gelatin; edible starch includes starch from natural sources and / or modified starch; starch from natural sources includes at least one of corn starch, potato starch, cassava starch, wheat starch, mung bean starch and rice starch; modified starch includes at least one of oxidized starch, cationic starch, esterified starch, cross-linked starch and hydroxypropyl starch; gelatin includes at least one of cowhide gelatin, pig skin gelatin, fish skin gelatin, bovine bone gelatin, pig bone gelatin and fish bone gelatin.

9. The capsule product according to claim 8, characterized in that: In parts by weight, the capsule shell further comprises 0.1-2 parts of edible flavor, 0.1-5 parts of sweetener, 0.1-1 parts of colorant and 0-3 parts of thickener.

10. The capsule product according to claim 8, characterized in that: The sweetener includes at least one of saccharin sodium, aspartame, stevia and sucralose; the thickener includes at least one of carrageenan, xanthan gum, sodium carboxymethyl cellulose, gellan gum and propylene glycol alginate; the edible flavor includes at least one of sweet orange flavor, cherry flavor, strawberry flavor, lime flavor, mint essential oil, edible apple flavor, edible mint flavor and edible orange flavor; the colorant includes at least one of carmine, new red, amaranth, allura red, erythrosine, azorubin, lemon yellow, sunset yellow, chlorophyll, brilliant blue, anthocyanin, cocoa shell pigment, iron oxide, caramel color, carbon black and brilliant black.

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