Oral cavity blasting bead as well as preparation method and application thereof
By accurately controlling the proportion of each component, oral blast beads with suitable hardness and brittleness were prepared, which solved the problems of poor taste and unstable quality in the prior art, and achieved uniform release of ingredients such as allicin and long-lasting breath freshness.
Patent Information
- Application Number
- CN202411906447.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-23
- Publication Date
- 2025-03-25
AI Technical Summary
The existing oral blast beads have poor taste and unstable quality, easy to leak oil, short shelf life, and difficult to fully play the role of the contained ingredients.
By precisely controlling the proportion of each component, including allicin, excipients, emulsifiers, fillers, flavoring agents and preservatives for core and wall materials, oral blast beads with suitable hardness and brittleness are prepared to ensure the uniform release of ingredients such as allicin.
It has achieved high-quality production of oral blast beads. The product has good hardness and brittleness, bringing a pleasant blasting feeling, improving stability and safety, uniform release of effective ingredients, and a long-lasting breath effect.
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Figure CN119679649A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of oral care, and in particular to an oral explosive bead, a preparation method and application thereof. Background Art
[0002] The human oral cavity is a complex and complete microecological system. The appropriate temperature, pH and humidity provide a suitable environment and conditions for the growth, reproduction and settlement of various microorganisms in the oral cavity. The oral flora and the host are in a dynamic equilibrium. When the microorganisms in the oral cavity grow excessively, the balance of the oral microecology will be broken, which will cause oral problems.
[0003] In the field of daily personal care, oral bursting beads can meet people's needs for keeping fresh breath and maintaining oral health. At the same time, oral bursting beads can also meet the needs of social occasions and are easy to carry, helping people avoid the embarrassment caused by bad breath problems and improve their self-confidence and social image. The market size is large due to the increase in consumers' attention to oral care and their consumption capacity.
[0004] Allicin is a fat-soluble compound with a strong and specific odor, and has many health benefits, such as anti-inflammatory, inhibiting the growth of pathogens, improving intestinal flora, etc. Therefore, how to provide an oral bursting bead with a good taste, antibacterial effect and oral care function is of great significance to further expand the market demand for this product. Summary of the invention
[0005] The main purpose of the present invention is to provide an oral bursting bead, a preparation method and application thereof, so as to solve the problem of poor taste of the oral bursting bead in the prior art.
[0006] In order to achieve the above-mentioned purpose, according to the first aspect of the present invention, there is provided an oral bursting bead, which comprises, by mass fraction, 0.001-2% of allicin, 4-10% of core material excipient, 0.3-30% of wall material excipient, 0.5-1.5% of core material emulsifier, 1-10% of wall material emulsifier, 45-80% of core material filler, 1-10% of wall material filler, 0.1-0.5% of preservative and 1.02%-4.6% of water.
[0007] Further, the oral bursting beads include: allicin 0.001-2%, core material excipient 4-10%, wall material excipient 0.3-30%, core material emulsifier 0.5-1.5%, wall material emulsifier 1-10%, core material filler 45-80%, wall material filler 1-10%, main flavoring agent 0.01-0.3%, auxiliary flavoring agent 0.01-0.3%, preservative 0.1-0.5% and water 1%-4%; preferably, the core material excipient includes: anhydrous calcium chloride; preferably, the core material emulsifier includes: Tween 80; preferably, the core material filler includes: medium chain triglyceride; preferably, the main flavoring agent includes: sucralose; preferably, the auxiliary flavoring agent includes: citric acid, mint flavor, green tea flavor, sweet orange flavor, strawberry flavor, cucumber flavor, passion fruit flavor or strawberry ice cream flavor. One or more.
[0008] Furthermore, the wall material excipient includes: one or more of sodium alginate, pectin, carrageenan, xanthan gum, gelatin or chitosan; preferably, the wall material emulsifier includes: span20; preferably, the wall material filler includes: glycerol; preferably, the preservative includes: one or more of benzoic acid, sodium benzoate, sorbic acid, potassium sorbate, ethyl parahydroxybenzoate or propyl parahydroxybenzoate; preferably, the particle size of the oral bursting beads is 5-8mm; preferably, the hardness of the oral bursting beads is 10N-30N; preferably, the brittleness of the oral bursting beads is 80% to 95%.
[0009] In order to achieve the above-mentioned purpose, according to the second aspect of the present invention, there is provided a method for preparing the above-mentioned oral bursting beads, the preparation method comprising: S1, preparing a core material: adding a core material excipient, a main flavoring agent and a preservative into water, stirring and mixing to obtain a core material water phase, adding allicin, a core material emulsifier and a core material filler into water, stirring and mixing to obtain a core material oil phase; adding the core material water phase into the core material oil phase, performing a first stirring and mixing to obtain a core material; S2, preparing a wall material: adding a wall material excipient into water, stirring and mixing to obtain a wall material initial liquid; adding a wall material emulsifier into a wall material filler, stirring and mixing to obtain a mixed liquid, adding the mixed liquid into the wall material initial liquid, performing a second stirring and mixing to obtain a wall material; S3, preparing the above-mentioned oral bursting beads: dropping the core material into the wall material, performing a third stirring and mixing to obtain a bursting bead primary product; sequentially curing, rinsing, drying and aging the bursting bead primary product to obtain an oral bursting bead.
[0010] Furthermore, the rotation speed of the first stirring and mixing is 3000-4000r / min; preferably, the time of the first stirring and mixing is 3-10min; preferably, the temperature of the first stirring and mixing is 80-90°C; preferably, S1 also includes cooling to 50-45°C after the first stirring and mixing, adding auxiliary flavoring agents, stirring and mixing, and obtaining the core material.
[0011] Furthermore, the rotation speed of the second stirring and mixing is 3000-5000 r / min; preferably, the time of the second stirring and mixing is 3-10 min; preferably, the rotation speed of the third stirring and mixing is 20-50 r / min.
[0012] Furthermore, the solidification includes: immersing the primary blasting beads in a strengthening liquid for solidification after an initial rinse; preferably, the strengthening liquid includes a chitosan solution with a mass fraction of 5-10%; preferably, the solidification time is 10-20 minutes; preferably, the rinsing solution is purified water; preferably, the rinsing time is 10-20 minutes.
[0013] Furthermore, the drying temperature is 20-30° C.; preferably, the aging includes: aging at room temperature for 18-24 hours.
[0014] In order to achieve the above-mentioned purpose, according to the third aspect of the present invention, there is provided an oral bursting bead prepared by the above-mentioned preparation method, wherein the particle size of the oral bursting bead is 5-8mm; preferably, the hardness of the oral bursting bead is 10N-30N; preferably, the brittleness of the oral bursting bead is 80% to 95%.
[0015] In order to achieve the above-mentioned object, according to a fourth aspect of the present invention, there is provided an application of the above-mentioned oral bursting beads or the oral bursting beads prepared by the above-mentioned preparation method in oral care.
[0016] By applying the technical solution of the present invention, the oral blasting beads of the present application have suitable hardness and brittleness, can bring a pleasant bursting feeling in the eating experience, have stable quality and no oil leakage, are easy to carry, and at the same time, the effective ingredients inside are evenly released, making the breath freshening effect more lasting and more comprehensive. In addition, the oral blasting beads of the present application contain allicin, which can better exert its function, have a strong antibacterial effect on oral Staphylococcus aureus, Escherichia coli, and Candida albicans, can regulate the balance of oral flora, prevent oral diseases, and are beneficial to oral health. BRIEF DESCRIPTION OF THE DRAWINGS
[0017] The drawings constituting a part of the present application are used to provide a further understanding of the present invention. The exemplary embodiments of the present invention and their descriptions are used to explain the present invention and do not constitute an improper limitation of the present invention. In the drawings:
[0018] Figure 1 A schematic diagram of the oral explosive beads prepared in the present application is shown;
[0019] Figure 2 The graph shows the experimental results of the antibacterial effect of the oral bursting beads of the present application on Escherichia coli in the detection experiment 1 of the present application.
[0020] Figure 3The graph shows the experimental results of the antibacterial effect of the oral bursting beads of the present application on Staphylococcus aureus in the detection experiment 2 of the present application.
[0021] Figure 4 The graph shows the experimental results of the antibacterial effect of the oral explosive beads of the present application on Candida albicans in the detection experiment 3 of the present application. DETAILED DESCRIPTION
[0022] It should be noted that, in the absence of conflict, the embodiments and features in the embodiments of the present application can be combined with each other. The present invention will be described in detail below with reference to the accompanying drawings and in combination with the embodiments.
[0023] As mentioned in the background technology, oral bursting beads are a relatively new type of oral care product, and the development of their quality and efficacy is not yet mature. The taste of existing oral bursting beads, such as hardness and brittleness, is poor for users, and has a more obvious taste of chemical reagents; and due to unstable quality, they are prone to oil leakage during storage and have a short shelf life (1-1.5 years); due to the texture characteristics of the core material in the bursting beads, the ingredients with oral care efficacy are difficult to fully exert their effects after bursting. Therefore, the present application intends to provide an oral bursting bead with better taste and better care efficacy.
[0024] In a first typical embodiment of the present application, an oral bursting bead is provided, which includes, by mass fraction, 0.001-2% allicin, 4-10% core material excipient, 0.3-30% wall material excipient, 0.5-1.5% core material emulsifier, 1-10% wall material emulsifier, 45-80% core material filler, 1-10% wall material filler, 0.1-0.5% preservative and 1.02%-4.6% water.
[0025] By precisely controlling the proportions of the various components in the oral popping beads of the present application, the antibacterial properties of allicin and the protective effects of the core material and wall material can be effectively combined to extend the shelf life of the oral popping beads, thereby obtaining oral popping beads with better hardness and brittleness (the hardness of existing popping bead products is 1250-1500 and the brittleness is 500-700). This can provide users with a better popping taste and can achieve a lasting care effect in the oral environment, and is suitable for daily oral cleaning, elimination of oral odor, and maintenance of gum health.
[0026] In order to further improve the palatability of the oral bursting beads, an appropriate amount of flavoring agent is added. In a preferred embodiment, the oral bursting beads include: 0.001-2% allicin, 4-10% core material excipient, 0.3-30% wall material excipient, 0.5-1.5% core material emulsifier, 1-10% wall material emulsifier, 45-80% core material filler, 1-10% wall material filler, 0.01-0.3% main flavoring agent, 0.01-0.3% auxiliary flavoring agent, 0.1-0.5% preservative and 1%-4% water.
[0027] In order to further improve the taste and antibacterial effect of the oral popping beads, in a preferred embodiment, the core material excipient includes: anhydrous calcium chloride; preferably, the core material emulsifier includes: Tween 80; preferably, the core material filler includes: medium chain triglycerides; preferably, the main flavoring agent includes: sucralose; preferably, the auxiliary flavoring agent includes: one or more of citric acid, mint flavor, green tea flavor, sweet orange flavor, strawberry flavor, cucumber flavor, passion fruit flavor or strawberry ice cream flavor. These preferred ingredients not only improve the taste of the oral popping beads, making them more refreshing and natural, but also enhance the stability and safety of the product.
[0028] In order to further improve the hardness and brittleness of the oral bursting beads and wrap the core material without oil leakage, in a preferred embodiment, the wall material excipient includes: one or more of sodium alginate, pectin, carrageenan, xanthan gum, gelatin or chitosan; preferably, the wall material emulsifier includes: span20; preferably, the wall material filler includes: glycerol; preferably, the preservative includes: one or more of benzoic acid, sodium benzoate, sorbic acid, potassium sorbate, ethyl paraben or propyl paraben. The selection of these wall material components can not only effectively protect the effective ingredients such as allicin, medium-chain triglycerides, and flavoring agents from leakage to ensure that the oral bursting beads still maintain good shape and function after long-term storage, but also increase the bursting experience of the beads, improve the appearance, and make it more convenient to carry around, providing users with oral care anytime and anywhere.
[0029] Among them, since the core material is wrapped by the wall material to form a bursting bead, the total mass of the core material must be greater than the total mass of the wall material, otherwise the core material will float on the wall material, resulting in the bursting bead not being completely wrapped. Therefore, the molecular weight of the excipients, emulsifiers and fillers used in the core material must be greater than the molecular weight of the excipients, emulsifiers and fillers used in the wall material. The molecular weight of span20 used in the wall material emulsifier is 346.459, and the molecular weight of Tween 80 used in the core material emulsifier is 428.6. The larger the molecular weight, the greater the mass.
[0030] In addition, anhydrous calcium chloride is used as the core material excipient to maintain the stability of the core material water-oil system and to play the role of a nutritional enhancer; various gums such as sodium alginate, pectin, and carrageenan are used as wall material excipients to form the shell of the popping beads, and the hardness and brittleness of the shell of the popping beads are improved by mixing different types of gums. The molecular weight of the medium-chain triglyceride used in the core material filler is 639.001, and the molecular weight of the glycerol used in the wall material filler is 92.09. At the same time, medium-chain triglycerides added to the core material can increase the taste and stability of the core material, and glycerol added to the wall material is used to increase the sealing of the shell and enhance the glossiness of the appearance.
[0031] In a preferred embodiment, the particle size of the oral bursting beads is 5-8 mm; preferably, the hardness of the oral bursting beads is 10N-30N; preferably, the brittleness of the oral bursting beads is 80% to 95%.
[0032] In a second typical embodiment of the present application, a method for preparing the above-mentioned oral bursting beads is provided, and the preparation method comprises: S1, preparing a core material: adding a core material excipient, a main flavoring agent and a preservative into water, stirring and mixing to obtain a core material water phase, adding allicin, a core material emulsifier and a core material filler into water, stirring and mixing to obtain a core material oil phase; adding the core material water phase into the core material oil phase, performing a first stirring and mixing to obtain a core material; S2, preparing a wall material: adding a wall material excipient into water, stirring and mixing to obtain a wall material initial liquid; adding a wall material emulsifier into a wall material filler, stirring and mixing to obtain a mixed liquid, adding the mixed liquid into the wall material initial liquid, performing a second stirring and mixing to obtain a wall material; S3, preparing the above-mentioned oral bursting beads: dropping the core material into the wall material, performing a third stirring and mixing to obtain a bursting bead primary product; sequentially curing, rinsing, drying and aging the bursting bead primary product to obtain an oral bursting bead.
[0033] The core material prepared by this method can evenly wrap allicin, medium-chain triglycerides, flavor enhancers and other effective ingredients to ensure their effective release in the oral cavity. It is suitable for oral care scenarios that require deep cleaning and antibacterial properties.
[0034] In order to further mix the various substances in the core material more completely, in a preferred embodiment, the speed of the first stirring and mixing is 3000-4000r / min; preferably, the time of the first stirring and mixing is 3-10min; preferably, the temperature of the first stirring and mixing is 80-90℃; preferably, S1 also includes cooling to 50-45℃ after the first stirring and mixing, adding auxiliary flavoring agents, stirring and mixing, and obtaining the core material. Among them, the addition of auxiliary flavoring agents further improves the taste of the product, making it more comfortable when used, and is suitable for care scenarios that need to improve oral odor.
[0035] In order to further mix the various substances in the wall material more completely, in a preferred embodiment, the second stirring and mixing speed is 3000-5000r / min; preferably, the second stirring and mixing time is 3-10min. In order to further ensure the uniform wrapping of the wall material and avoid the damage of the core material, in a preferred embodiment, the third stirring and mixing speed is 20-50r / min; preferably, the third stirring starts from the time when the core material drips into the wall material until the burst beads are fully formed, and the stirring is stopped during this period, during which the core material drips into the wall material at a speed of 16-20 drops / minute.
[0036] In order to further improve the structural strength of the oral popping beads and remove impurities that may remain during the preparation process, in a preferred embodiment, the solidification includes: after the initial rinsing of the popping beads, immersing them in a strengthening liquid for solidification; preferably, the strengthening liquid includes a chitosan solution with a mass fraction of 5-10%; preferably, the solidification time is 10-20 minutes; preferably, the rinsing solution is purified water; preferably, the rinsing time is 10-20 minutes.
[0037] In order to further improve the hardness and brittleness of the oral bursting beads so that they can quickly release effective ingredients in the oral cavity, in a preferred embodiment, the drying temperature is 20-30°C; preferably, the aging includes: aging at room temperature for 18-24 hours.
[0038] In the third typical embodiment of the present application, an oral bursting bead prepared by the above-mentioned preparation method is provided, the particle size of the oral bursting bead is 5-8mm; preferably, the hardness of the oral bursting bead is 10N-30N; preferably, the brittleness of the oral bursting bead is 80% to 95%. The optimization of these physical properties not only makes the oral bursting bead easy to use, but also can be quickly broken in the mouth to release effective ingredients such as allicin, which is suitable for various oral care needs, such as preventing oral diseases, improving oral hygiene and enhancing breath freshness.
[0039] In a fourth typical embodiment of the present application, there is provided an application of the oral bursting beads mentioned above or the oral bursting beads prepared by the above preparation method in oral care.
[0040] The present application is further described in detail below in conjunction with specific embodiments. These embodiments should not be construed as limiting the scope of protection claimed in the present application.
[0041] Detection experiment
[0042] 1. Testing of physical and chemical indicators: Use a texture analyzer to test the hardness and brittleness of the prepared oral popping beads.
[0043] 2. Sensory index detection: 10 healthy volunteers were selected to conduct trial scoring on the prepared oral bursting beads. The scoring criteria are shown in Table 1:
[0044] Table 1 Allicin oral burst score table
[0045]
[0046]
[0047] Example 1
[0048] The mass fractions of the components of the oral bursting beads in this embodiment are as follows: 0.001% allicin, 4% anhydrous calcium chloride, 0.01% sucralose, 0.5% Tween 80, 80% medium chain triglycerides, 0.01% strawberry ice cream flavor, 0.01% mint flavor, 10% sodium alginate, 0.1% pectin, 0.3% carrageenan, 1% span20, 1% glycerol, 0.3% sodium benzoate and 2.769% water.
[0049] The preparation method of the oral explosive beads in this embodiment is as follows:
[0050] S1, preparing a core material: adding anhydrous calcium chloride, sucralose and sodium benzoate to water, stirring until completely dissolved, and mixing evenly to obtain a core material water phase; adding allicin, Tween 80 and medium chain triglycerides to water, stirring until completely dissolved, and mixing evenly to obtain a core material oil phase;
[0051] The core material water phase and the core material oil phase are heated to 80°C respectively, the core material water phase is added to the core material oil phase, and the first stirring and mixing is performed at a speed of 3500r / min for 8min. After the first stirring and mixing, the temperature is lowered to 50°C, strawberry ice cream flavor and mint flavor are added, and the mixture is stirred and mixed to obtain the core material.
[0052] S2, preparing wall material: adding sodium alginate, pectin and carrageenan into water, stirring and mixing to obtain an initial wall material solution;
[0053] Span 20 was added to glycerol, stirred and mixed, and the obtained mixed solution was added to the initial liquid of the wall material, and a second stirring and mixing was performed at a speed of 3500 r / min for 5 minutes to obtain the wall material.
[0054] S3, preparing the above-mentioned oral popping beads: dripping the core material into the wall material, performing a third stirring and mixing, the speed is 28r / min, and continuously stirring until the initial popping beads are obtained;
[0055] After the first batch of popping beads was rinsed with purified water, they were immersed in 8% chitosan solution for curing for 15 minutes and rinsed with purified water for 15 minutes.
[0056] Place the rinsed popping beads in a drying oven for drying, set the temperature to 25°C, turn the popping beads regularly to avoid sticking, and dry at low temperature until there is no water on the surface. Then place them at room temperature for aging for 22 hours to obtain oral popping beads. Subsequently, the finished products can be screened according to the particle integrity, core liquid filling, color and diameter of the oral popping beads, and packaged according to the required specifications to obtain the finished oral popping beads.
[0057] The results of the hardness and brittleness of the oral popping beads obtained in this example are shown in Table 2, and the scores of color, appearance, smell, taste, impurities and particle size evaluated by volunteers are shown in Table 3.
[0058] Table 2 Allicin oral burst beads hardness and brittleness test results
[0059] Explosion bead number 1 2 3 4 5 6 7 8 9 10 average Brittleness / g 800 825 789 800 820 810 826 800 810 810 809 Hardness / g 1525 1605 1508 1526 1608 1486 1512 1525 1609 1500 1540.4
[0060] Table 3 Allicin oral burst bead scoring results
[0061] Volunteer Number 1 2 3 4 5 6 7 8 9 10 average Color 7 8 8 9 10 9 10 8 9 9 8.7 Appearance 8 8 9 10 8 9 8 10 10 9 8.9 odor 8 9 7 10 9 8 9 10 10 8 8.8 Taste 9 9 10 8 9 10 10 9 9 8 9.1 Impurities 10 10 10 9 10 10 9 10 9 10 9.7 Particle size 10 10 10 10 9 10 10 10 10 10 9.9 Oil phase leakage 10 10 10 10 10 10 10 10 10 10 10
[0062] Example 2
[0063] The mass fractions of the components of the oral bursting beads in this embodiment are as follows: 10% anhydrous calcium chloride, 0.3% sucralose, 2% allicin, 1.1% Tween 80, 45% medium chain triglycerides, 0.1% strawberry ice cream flavor, 0.1% mint flavor, 18% sodium alginate, 3% pectin, 9% carrageenan, 5% span20, 5% glycerol, 0.1% sodium benzoate, and 1.3% water.
[0064] The preparation method of the oral explosive beads in this embodiment is as follows:
[0065] S1, preparing a core material: adding anhydrous calcium chloride, sucralose and sodium benzoate to water, stirring until completely dissolved, and mixing evenly to obtain a core material water phase; adding allicin, Tween 80 and medium chain triglycerides to water, stirring until completely dissolved, and mixing evenly to obtain a core material oil phase;
[0066] The core material water phase and the core material oil phase are heated to 80°C respectively, the core material water phase is added to the core material oil phase, and the first stirring and mixing is performed at a speed of 4000r / min for 6min. After the first stirring and mixing, the temperature is lowered to 50°C, strawberry ice cream flavor and mint flavor are added, and the mixture is stirred and mixed to obtain the core material.
[0067] S2, preparing wall material: adding sodium alginate, pectin and carrageenan into water, stirring and mixing to obtain an initial wall material solution;
[0068] Span 20 was added to glycerol, stirred and mixed, and the obtained mixed solution was added to the initial liquid of the wall material, and a second stirring and mixing was performed at a speed of 3500 r / min and a time of 7 minutes to obtain the wall material.
[0069] S3, preparing the above-mentioned oral popping beads: dripping the core material into the wall material, performing a third stirring and mixing, the speed is 25r / min, and continuously stirring until the initial popping beads are obtained;
[0070] After the first batch of popping beads was rinsed with purified water, they were immersed in 8% chitosan solution for curing for 10 minutes and rinsed with purified water for 10 minutes.
[0071] Place the rinsed popping beads in a drying oven for drying, set the temperature to 28°C, turn the popping beads regularly to avoid sticking, and dry at low temperature until there is no water on the surface. Then place them at room temperature for aging for 23 hours to obtain oral popping beads. Subsequently, the finished products can be screened according to the particle integrity, core liquid filling, color and diameter of the oral popping beads, and packaged according to the required specifications to obtain the finished oral popping beads.
[0072] The results of the hardness and brittleness of the oral popping beads obtained in this example are shown in Table 4, and the scores of color, appearance, smell, taste, impurities and particle size evaluated by volunteers are shown in Table 5.
[0073] Table 4 Allicin oral burst beads hardness and brittleness test results
[0074] Explosion bead number 1 2 3 4 5 6 7 8 9 10 average Brittleness / g 815 820 800 780 820 788 855 780 810 800 806.8 Hardness / g 1580 1600 1586 1500 1548 1502 1500 1503 1505 1500 1532.4
[0075] Table 5 Allicin oral bursting beads scoring results
[0076] Volunteer Number 1 2 3 4 5 6 7 8 9 10 average Color 8 10 9 9 10 9 10 9 10 9 9.3 Appearance 9 10 9 10 9 9 8 9 10 9 9.2 odor 10 9 8 10 8 10 9 10 9 8 9.1 Taste 8 10 10 8 9 10 10 9 9 8 9.1 Impurities 10 10 9 10 10 9 10 9 9 10 9.6 Particle size 10 9 9 10 10 10 10 10 10 10 9.8 Oil phase leakage 10 10 10 10 10 10 10 10 10 10 10
[0077] Example 3
[0078] The mass fractions of the components of the oral bursting beads in this embodiment are as follows: 6% anhydrous calcium chloride, 0.05% sucralose, 1% allicin, 1% Tween 80, 65% medium chain triglycerides, 0.04% strawberry ice cream flavor, 0.04% mint flavor, 14% sodium alginate, 1% pectin, 3% carrageenan, 3% span20, 3% glycerol, 0.1% sodium benzoate, and 2.77% water.
[0079] The preparation method of the oral explosive beads in this embodiment is as follows:
[0080] S1, preparing a core material: adding anhydrous calcium chloride, sucralose and sodium benzoate to water, stirring until completely dissolved, and mixing evenly to obtain a core material water phase; adding allicin, Tween 80 and medium chain triglycerides to water, stirring until completely dissolved, and mixing evenly to obtain a core material oil phase;
[0081] The core material water phase and the core material oil phase are heated to 80°C respectively, the core material water phase is added to the core material oil phase, and the first stirring and mixing is performed at a speed of 4000r / min for 6min. After the first stirring and mixing, the temperature is lowered to 50°C, strawberry ice cream flavor and mint flavor are added, and the mixture is stirred and mixed to obtain the core material.
[0082] S2, preparing wall material: adding sodium alginate, pectin and carrageenan into water, stirring and mixing to obtain an initial wall material solution;
[0083] Span 20 was added to glycerol, stirred and mixed, and the obtained mixed solution was added to the initial liquid of the wall material, and a second stirring and mixing was performed at a speed of 3500 r / min and a time of 7 minutes to obtain the wall material.
[0084] S3, preparing the above-mentioned oral popping beads: dripping the core material into the wall material, performing a third stirring and mixing, the speed is 25r / min, and continuously stirring until the initial popping beads are obtained;
[0085] After the first batch of popping beads was rinsed with purified water, they were immersed in 8% chitosan solution for curing for 10 minutes and rinsed with purified water for 10 minutes.
[0086] Place the rinsed popping beads in a drying oven for drying, set the temperature to 28°C, turn the popping beads regularly to avoid sticking, and dry at low temperature until there is no water on the surface. Then place them at room temperature for aging for 23 hours to obtain oral popping beads. Subsequently, the finished products can be screened according to the particle integrity, core liquid filling, color and diameter of the oral popping beads, and packaged according to the required specifications to obtain the finished oral popping beads.
[0087] The results of the hardness and brittleness of the oral popping beads obtained in this example are shown in Table 6, and the scores of color, appearance, smell, taste, impurities and particle size evaluated by volunteers are shown in Table 7.
[0088] Table 6 Allicin oral burst beads hardness and brittleness test results
[0089] Explosion bead number 1 2 3 4 5 6 7 8 9 10 average Brittleness / g 825 820 790 785 815 820 805 790 810 820 808 Hardness / g 1550 1550 1546 1480 1498 1420 1510 1493 1495 1505 1504.7
[0090] Table 7 Allicin oral burst bead scoring results
[0091]
[0092]
[0093] Comparative Example 1
[0094] This comparative example is the same as Example 1 except that the core material filler is different. The core material filler in this comparative example is sesame oil. When the core material prepared by sesame oil is mixed with the wall material, it is impossible to obtain a formed oral popping bead.
[0095] Comparative Example 2
[0096] Except for step S3 of the preparation method, the other operations of this comparative example are the same. The operation of S3 in this comparative example is as follows: dripping the wall material into the core material, and performing a third stirring and mixing. However, due to the different order of adding the two phases, formed oral bursting beads cannot be obtained.
[0097] Comparative Example 3
[0098] This comparative example is the same as Example 1 except that the wall material excipient is different, and the other operations are the same. The wall material excipient of this comparative example is guar gum, agar locust bean gum or konjac gum. The hardness of oral popping beads 1, oral popping beads 2 and oral popping beads 3 obtained by the same preparation method as Example 1 is significantly reduced. Among them, the average hardness of the popping beads prepared by guar gum, agar locust bean gum or konjac gum is 1325, 1251, and 1262 respectively.
[0099] Comparative Example 4
[0100] This comparative example is the same as Example 3 except for allicin. In this comparative example, allicin is not added, and medium-chain triglycerides are used instead of allicin. The antibacterial activity of the prepared oral bursting beads against Staphylococcus aureus, Escherichia coli, and Candida albicans is about 90%.
[0101] Detection experiment 1
[0102] According to the Art Standards for Disinfectant Products (2002 Edition), the oral explosive beads (shaped as shown in FIG. 3 ) obtained in Example 3 were Figure 1 coli (ATCC 8099) was tested for bacteriostasis.
[0103] (1) Preparation of bacterial suspension: Pick up activated single colonies and add them to 10 mL PBS phosphate buffer, mix well, and make 3 × 10 4 cfu / mL to 4×10 4 cfu / mL bacterial suspension;
[0104] (2) Pipette 5 mL of PBS control sample and oral bead sample (crushed) into sterile EP tubes, add 0.1 mL of bacterial suspension, mix well and start timing. When the reaction time is 2, 5, 10, and 20 min, pipette 500 μL of control sample and sample solution into test tubes containing 5 mL of PBS, mix well, and then take 0.1 mL for dilution gradient. -1 , 10 -2 Pipette 0.1 mL of each dilution onto nutrient agar medium, make 2 plates for each dilution gradient, invert and culture at 35°C for 48 h, and observe the results.
[0105] like Figure 2 As shown, the four columns on the left are the culture effects of Escherichia coli coated on blank plates, and the four columns on the right are the culture effects of Escherichia coli coated on plates with different concentrations of oral bursting beads solution. From top to bottom, each row represents a different culture time, which is 2 minutes, 5 minutes, 10 minutes and 20 minutes. The total number of colonies and the antibacterial rate are statistically analyzed, and the results are shown in Table 8. It can be seen that the oral bursting beads of the present application have a strong antibacterial effect on Escherichia coli, and the antibacterial effect can reach more than 99%.
[0106] Table 8:
[0107]
[0108] Detection experiment 2
[0109] According to the Artistic Standards for Disinfectant Products (2002 Edition), the antibacterial test of the oral explosive beads obtained in Example 3 against Staphylococcus aureus (ATCC 6538) was carried out.
[0110] (1) Preparation of bacterial suspension: Pick up activated single colonies and add them to 10 mL PBS phosphate buffer, mix well, and make 3 × 10 4 cfu / mL to 4×10 4 cfu / mL bacterial suspension;
[0111] (2) Pipette 5 mL of PBS control sample and oral bead sample (crushed) into sterile EP tubes, add 0.1 mL of bacterial suspension, mix well and start timing. When the reaction time is 2, 5, 10, and 20 min, pipette 500 μL of control sample and sample solution into test tubes containing 5 mL of PBS, mix well, and then take 0.1 mL for dilution gradient. -1 , 10 -2 Pipette 0.1 mL of each dilution onto nutrient agar medium, make 2 plates for each dilution gradient, invert and culture at 35°C for 48 h, and observe the results.
[0112] like Figure 3 As shown, the four columns on the left are the culture effects of Staphylococcus aureus coated on blank plates, and the four columns on the right are the culture effects of Staphylococcus aureus coated on plates with different concentrations of oral bursting beads solution. From top to bottom, each row represents a different culture time, which is 2 minutes, 5 minutes, 10 minutes and 20 minutes. The total colony count and the antibacterial rate are statistically analyzed, and the results are shown in Table 9. It can be seen that the oral bursting beads of the present application have a strong antibacterial property against Staphylococcus aureus, and the antibacterial property can reach more than 99%.
[0113] Table 9:
[0114]
[0115]
[0116] Detection experiment 3
[0117] According to the Artistic Standards for Disinfectant Products (2002 Edition), the oral explosive beads obtained in Example 3 were tested for antibacterial activity against Candida albicans (ATCC 10231).
[0118] (1) Preparation of bacterial suspension: Pick up activated single colonies and add them to 10 mL PBS phosphate buffer, mix well, and make 3 × 10 4 cfu / mL to 4×10 4 cfu / mL bacterial suspension;
[0119] (2) Pipette 5 mL of PBS control sample and oral bead sample (crushed) into sterile EP tubes, add 0.1 mL of bacterial suspension, mix well and start timing. When the reaction time is 2, 5, 10, and 20 min, pipette 500 μL of control sample and sample solution into test tubes containing 5 mL of PBS, mix well, and then take 0.1 mL for dilution gradient. -1 , 10 -2 Pipette 0.1 mL of each dilution onto Sabouraud glucose agar medium. Make 2 plates for each dilution gradient. Incubate at 35°C upside down for 48 h and observe the results.
[0120] like Figure 4 As shown, the four columns on the left are the culture effects of Candida albicans coated on blank plates, and the four columns on the right are the culture effects of Candida albicans coated on plates with different concentrations of oral bursting beads solution. From top to bottom, each row represents a different culture time, which is 2 minutes, 5 minutes, 10 minutes and 20 minutes. The total colony count and the antibacterial rate are statistically analyzed, and the results are shown in Table 10. It can be seen that the oral bursting beads of the present application have a strong antibacterial property against Candida albicans, and the antibacterial property can reach more than 99%.
[0121] Table 10:
[0122]
[0123] Detection experiment 4
[0124] The drug sensitivity paper multiple dilution method was used to detect the minimum inhibitory concentration of the oral bursting beads obtained in Example 3 against Staphylococcus aureus, Escherichia coli, Candida albicans, Streptococcus mutans, Bacillus subtilis, Pseudomonas aeruginosa, Lactobacillus acidophilus, and Helicobacter pylori.
[0125] (1) Preparation of bacterial suspension: Pick up activated single colonies and add them to 10 mL of PBS phosphate buffer, mix well, and measure the concentration of the bacterial suspension using a bacterial turbidity meter. The number of recovered colonies is 3 × 10 4cfu / mL~4×10 4 cfu / mL.
[0126] (2) Take an appropriate amount of oral explosive beads, crush them and dissolve them in 10 mL of sterile purified water, add 0.05% Tween 80 and mix well, and use the serial dilution method to prepare the sample solutions with concentrations of 2296.064, 1148.032, 574.016, 287.008, 143.504, 71.752, 35.876, 17.938, 8.969, 4.485, and 2.242 mg / mL for later use. Use sterile distilled water as the blank control.
[0127] (3) Pipette 10 μL of bacterial suspension into 20 mL of sterilized culture medium cooled to 50°C, shake well, pour into a plate and wait for it to solidify for later use. Take sterile and dry drug-sensitive sheets, add 20 μL of the sample solution to be tested to each sheet, and place them to dry naturally at room temperature. Place 3 test sheets and 1 blank control sheet (add 20 μL of sterile distilled water to each sheet) on each plate. The distance between the centers of each sheet should be more than 25 mm, and the distance from the edge of the plate should be more than 15 mm. Incubate at 37°C for 16-18 hours. The lowest solution concentration that produces an antibacterial zone around the sample is the minimum inhibitory concentration of the gallic acid extract.
[0128] The minimum inhibitory concentrations of the oral bursting beads of the present application against Staphylococcus aureus, Escherichia coli, Candida albicans, Streptococcus mutans, Bacillus subtilis, Pseudomonas aeruginosa, Lactobacillus acidophilus, and Helicobacter pylori are 35.875 mg / mL, 287 mg / mL, 8.969 mg / mL, 71.75 mg / mL, 8.969 mg / mL, 35.875 mg / mL, 1148 mg / mL, and 1148 mg / mL, respectively.
[0129] From the above description, it can be seen that the above-mentioned embodiments of the present invention achieve the following technical effects: by accurately controlling the ratio of each component and each parameter condition in the preparation process, allicin, medium-chain triglycerides, flavoring agents and other ingredients can be effectively wrapped without oil leakage, and their functions can be better exerted, and they have good antibacterial effects on Staphylococcus aureus, Escherichia coli, and Candida albicans, and the structural stability of the oral bursting beads is enhanced to ensure their high efficiency and safety when released in the oral cavity. In addition, the preparation method of the present application is relatively simple, and the obtained oral bursting beads are not easy to deform or break during storage and transportation, and are easy to carry, and can ensure the integrity of the oral bursting beads. At the same time, by adding the main flavoring agent and the auxiliary flavoring agent, the taste of the oral bursting beads is improved, so that it can provide a good user experience while providing the oral care function.
[0130] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. For those skilled in the art, the present invention may have various modifications and variations. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.
Claims
1. An oral explosive bead, characterized in that: Calculated by mass fraction, the oral explosive beads include: 0.001-2% of allicin, 4-10% of core material excipients, 0.3-30% of wall material excipients, 0.5-1.5% of core material emulsifiers, 1-10% of wall material emulsifiers, 45-80% of core material fillers, 1-10% of wall material fillers, 0.1-0.5% of preservatives and 1.02%-4.6% of water.
2. The oral explosive beads according to claim 1, characterized in that: The oral explosive beads include: 0.001-2% of the allicin, 4-10% of the core material excipient, 0.3-30% of the wall material excipient, 0.5-1.5% of the core material emulsifier, 1-10% of the wall material emulsifier, 45-80% of the core material filler, 1-10% of the wall material filler, 0.01-0.3% of the main flavoring agent, 0.01-0.3% of the auxiliary flavoring agent, 0.1-0.5% of the preservative and 1%-4% of the water; Preferably, the core material excipient comprises: anhydrous calcium chloride; Preferably, the core material emulsifier comprises: Tween 80; Preferably, the core filler comprises: medium chain triglycerides; Preferably, the main flavoring agent includes: sucralose; Preferably, the auxiliary flavoring agent includes one or more of citric acid, mint flavor, green tea flavor, sweet orange flavor, strawberry flavor, cucumber flavor, passion fruit flavor or strawberry ice cream flavor.
3. The oral explosive beads according to claim 1, characterized in that: The wall material excipients include: one or more of sodium alginate, pectin, carrageenan, xanthan gum, gelatin or chitosan; Preferably, the wall material emulsifier comprises: span20; Preferably, the wall material filler includes: glycerol; Preferably, the preservative comprises: one or more of benzoic acid, sodium benzoate, sorbic acid, potassium sorbate, ethyl p-hydroxybenzoate or propyl p-hydroxybenzoate; Preferably, the particle size of the oral bursting beads is 5-8 mm; Preferably, the hardness of the oral explosive beads is 10N-30N; Preferably, the crispness of the oral popping beads is 80% to 95%.
4. A method for preparing oral explosive beads according to any one of claims 1 to 3, characterized in that: The preparation method comprises: S1, preparing the core material: adding the core material excipient, the main flavoring agent and the preservative into water, stirring and mixing to obtain a core material water phase, adding the allicin, the core material emulsifier and the core material filler into water, stirring and mixing to obtain a core material oil phase; Adding the core material water phase into the core material oil phase, performing a first stirring and mixing process to obtain the core material; S2, preparing the wall material: adding the wall material excipient into water, stirring and mixing, to obtain an initial wall material solution; Adding the wall material emulsifier to the wall material filler, stirring and mixing, and adding the obtained mixed liquid to the wall material initial liquid, performing a second stirring and mixing to obtain the wall material; S3, preparing the oral popping beads: dripping the core material into the wall material, performing a third stirring and mixing, and obtaining a primary popping bead product; The primary popping beads are solidified, rinsed, dried and aged in sequence to obtain the oral popping beads.
5. The preparation method according to claim 4, characterized in that: The first stirring and mixing speed is 3000-4000r / min; Preferably, the first stirring and mixing time is 3-10 min; Preferably, the temperature of the first stirring and mixing is 80-90°C; Preferably, the S1 further comprises, after the first stirring and mixing, cooling the mixture to 50-45° C., adding an auxiliary flavoring agent, stirring and mixing, to obtain the core material.
6. The preparation method according to claim 4, characterized in that: The second stirring and mixing speed is 3000-5000r / min; Preferably, the second stirring and mixing time is 3-10 min; Preferably, the rotation speed of the third stirring and mixing is 20-50 r / min.
7. The preparation method according to claim 4, characterized in that: The curing comprises: immersing the primary popping beads in a strengthening liquid after initial rinsing to perform the curing; Preferably, the strengthening liquid comprises a chitosan solution with a mass fraction of 5-10%; Preferably, the curing time is 10-20 minutes; Preferably, the solution for rinsing is purified water; Preferably, the rinsing time is 10-20 minutes.
8. The preparation method according to claim 4, characterized in that: The drying temperature is 20-30°C; Preferably, the aging comprises: performing the aging at room temperature for 18-24 hours.
9. The oral explosive beads prepared by the preparation method according to any one of claims 4 to 8, characterized in that: The particle size of the oral explosive beads is 5-8mm; Preferably, the hardness of the oral explosive beads is 10N-30N; Preferably, the crispness of the oral popping beads is 80% to 95%.
10. Use of the oral bursting beads according to any one of claims 1 to 3 or the oral bursting beads prepared by the preparation method according to any one of claims 4 to 8 in oral care.