False tooth safety paste and preparation method thereof

Abstract

The invention relates to the technical field of oral medical materials, and particularly provides a false tooth safety paste and a preparation method thereof. The denture safety paste comprises an oil phase matrix, a gel matrix and a microcapsule functional phase, wherein the oil phase matrix is formed by melting and emulsifying beewax and vegetable oil; the gel matrix comprises fenugreek gum, locust bean gum, nano cellulose and modified aluminum metasilicate; the microcapsule functional phase comprises fenugreek gum microcapsules, and the microcapsule functional phase is dispersed in the oil phase matrix and the gel matrix. Through the three-phase synergistic effect of the oil-phase matrix, the gel matrix and the fenugreek gum microcapsule functional phase dispersed in the oil-phase matrix and the gel matrix, the high-temperature stability of the paste without layering and oil separation is realized; the quick-acting initial adhesion of the locust bean gum, the slow-release lasting adhesion of the microcapsules, the mechanical reinforcement of the nano-crystalline cellulose network and the safe antibacterial property of the bacteriostatic agent are integrated, and the problems that the existing safety and consolidation paste is softened at a high temperature, is easy to lose and is poor in biocompatibility are effectively solved.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of oral medical materials, in particular, the present application provides a denture adhesive paste and a preparation method thereof. BACKGROUND

[0002] With the coming of an aging society, the number of denture wearers continues to increase. As an important medical device for assisting in fixing dentures, the performance of the denture adhesive paste directly affects the quality of life of the wearer. The denture adhesive paste on the market at present mostly uses mineral oil and white oil as the base, and is matched with water-soluble polymers (such as carboxymethyl cellulose, polymethyl vinyl ether-maleic anhydride complex salt) to realize the adhesion function. However, such products often have problems such as paste softening and adhesion reduction in a high-temperature environment, which leads to loose dentures and affects the normal chewing and language functions of the user.

[0003] Therefore, it has become an urgent problem in the industry to develop a denture adhesive paste that is stable at high temperatures and has long-lasting adhesion. SUMMARY

[0004] The present application provides a denture adhesive paste and a preparation method thereof. The denture adhesive paste of the present application realizes high-temperature stability without stratification and oil separation through the synergistic effect of the oil phase base, the gel base, and the dispersed fenugreek gum microcapsule functional phase. It has the advantages of quick initial adhesion of locust bean gum, long-lasting adhesion of microcapsule slow release, mechanical reinforcement of nanocellulose network, and safe antibacterial performance of natural antibacterial agent, effectively solving the problems of existing adhesive paste such as high-temperature softening, easy loss, and poor biocompatibility.

[0005] The present application provides a denture adhesive paste, which comprises an oil phase base, a gel base, and a microcapsule functional phase. The oil phase base is formed by melting and emulsifying beeswax and vegetable oil. The gel base comprises fenugreek gum, locust bean gum, nanocellulose, and modified metasilicate aluminum. The microcapsule functional phase comprises fenugreek gum microcapsules, which are dispersed in the oil phase base and the gel base.

[0006] In any of the above technical solutions, the content of each component in the denture adhesive paste is as follows: beeswax: 1.0-5.0 wt.%, vegetable oil: 35.0-40.0 wt.%, fenugreek gum: 5.0-25.0 wt.%, locust bean gum: 25.0-45.0 wt.%, modified metasilicate aluminum: 1.0-3.0 wt.%, nanocellulose: 2.0-5.0 wt.%, and fenugreek gum microcapsules: 7.0-10.0 wt.%.

[0007] In any of the above technical solutions, the fenugreek gum microcapsules comprise a core material and a wall material covering the core material. The core material comprises water-in-oil microdroplets containing antibacterial active ingredients. The wall material comprises a shell material formed by the complex of fenugreek gum and chitosan

[0008] In any of the technical solutions above, the modified metasilicate aluminum is obtained by grafting 3-aminopropyl triethoxysilane on the surface of metasilicate aluminum; and the vegetable oil includes one or more of sunflower oil, coconut oil, and peanut oil.

[0009] The application provides a preparation method of a denture adhesive paste, including the following steps: S100, heating and stirring beeswax and vegetable oil to form an oil phase matrix; S200, adding fenugreek gum and locust bean gum to the oil phase matrix, and then performing first stirring treatment, and then adding modified metasilicate aluminum to perform second stirring treatment to obtain a gel; and S300, adding fenugreek gum microcapsules to the gel, and performing degassing and shaping and cooling to obtain the denture adhesive paste.

[0010] In any of the technical solutions above, in step S100, the temperature of the heating and stirring treatment is 70-80℃, and the rotating speed is 100-200 rpm; and the beeswax is melted and filtered at 70-80℃ before being added.

[0011] In any of the technical solutions above, in step S200, the preparation method of the modified metasilicate aluminum includes the following steps: S211, dispersing metasilicate aluminum powder in an ethanol solution, adding 3-aminopropyl triethoxysilane, and performing ultrasonic treatment for 8-12 min to obtain a metasilicate aluminum intermediate; and S212, stirring the metasilicate aluminum intermediate at 60-80℃ under a nitrogen atmosphere for 3-5 h, centrifuging and washing with ethanol for 2-5 times, and drying at 70-90℃ for 5-7 h to obtain the modified metasilicate aluminum.

[0012] In any of the technical solutions above, in step S200, the temperature of the first stirring treatment is 62-68℃, the rotating speed is 200-300 rpm, and the time is 40-50 min; the rotating speed of the second stirring treatment is 250-350 rpm, and the time is 15-25 min; and the fenugreek gum and the locust bean gum are mixed and sieved through a 200-mesh sieve.

[0013] In any of the technical solutions above, the preparation method of the fenugreek gum microcapsules includes the following steps: S311, dissolving fenugreek gum and chitosan in deionized water containing acetic acid at a mass ratio of (3-5) : 1, heating to 40-50℃, and stirring until completely dissolved to obtain a fenugreek gum-chitosan composite solution; S312, dissolving a water-soluble bacteriostatic agent in water, and adding the water-soluble bacteriostatic agent to an oil phase containing an emulsifying agent to obtain a core material; and S313, dropping the core material into the fenugreek gum-chitosan composite solution, adding a crosslinking agent under stirring, and obtaining the fenugreek gum microcapsules through spray drying.

[0014] In any of the technical solutions above, in step S300, the vacuum degree of the degassing treatment is 0.01-0.05 MPa.

[0015] 0.02-0.1 MPa, temperature 40-45℃, time 10-15 min.

[0016] The technical effects that can be achieved after adopting the technical solutions of the present application are as follows:

[0017] 1. The "locking" effect of the semi-solid crystal framework and gel network constructed by beeswax-plant oil ensures that the paste is stable in shape without delamination and oil separation in an environment of 45℃ and above;

[0018] 2. The rapid swelling of locust bean gum provides initial high viscosity; the microcapsule of fenugreek gum-chitosan slowly releases the antibacterial ingredients, achieving sustained adhesion, and the two work together to significantly prolong the holding time;

[0019] 3. The nanocellulose forms a rigid framework in the colloid, greatly improving the structural strength under shear and chewing load; at the same time, the bacteriostatic agent stored in the microcapsule is released in a controlled manner, achieving long-term inhibition of harmful bacteria and being more gentle and safe to normal oral flora. BRIEF DESCRIPTION OF DRAWINGS

[0020] In order to more clearly illustrate the technical solutions of the embodiments of the present application, the following will briefly introduce the drawings to be used in the embodiment description. Obviously, the drawings in the following description are only some embodiments of the present application, and other drawings can also be obtained by those skilled in the art without creative labor on the basis of these drawings:

[0021] Figure 1 is a use state diagram of Example 1;

[0022] Figure 2 is a comparison diagram of Example 1 and Comparative Example 1 before and after 90 days. DETAILED DESCRIPTION

[0023] In order to more clearly illustrate the above-mentioned purposes, features and advantages of the present application, the following will further describe the present application in combination with the drawings and specific embodiments. It should be noted that the embodiments of the present application and the features in the embodiments can be combined with each other without conflict.

[0024] In the following description, many specific details are set forth in order to provide a thorough understanding of the present application, however, the present application can also be implemented in other ways different from those described herein, therefore, the scope of protection of the present application is not limited by the specific embodiments disclosed below.

[0025] In order to make the above-mentioned purposes, features and advantages of the present application more obvious and easy to understand, the following will describe the specific embodiments of the present application in detail.

[0026] Denture adhesive cream is an important product for assisting the stability of dentures in the oral cavity. In daily use, the denture adhesive cream needs to have good stability to ensure the fixing effect of the denture and the comfort of the user. However, such products have obvious defects:

[0027] 1. Insufficient high-temperature stability: traditional oil phase matrix (such as mineral oil, white oil) is easily converted from semi-solid to liquid at high temperature (> 40℃), resulting in the precipitation of solid phase and the stratification of cream body, which cannot guarantee uniformity;

[0028] 2. Short bonding time: natural water-soluble polymers are easily lost in the saliva secretion environment, and the action time is usually short. The effect is more easily attenuated when drinking water or eating liquid food;

[0029] 3. Defects of naturalness: the biocompatibility of synthetic polymer (such as carboxymethyl cellulose) and petroleum-based grease is limited, and long-term use may cause oral mucosa irritation and vomiting;

[0030] Therefore, the present embodiment provides a denture adhesive cream and a preparation method thereof. The denture adhesive cream of the present embodiment comprises an oil phase matrix, a gel matrix and a microcapsule functional phase; wherein the oil phase matrix is formed by melting and emulsifying beeswax and vegetable oil; the gel matrix comprises fenugreek gum, locust bean gum, nanocellulose and modified metasilicate aluminum; the microcapsule functional phase comprises fenugreek gum microcapsules, and the microcapsule functional phase is dispersed in the oil phase matrix and the gel matrix.

[0031] Specifically, the formula of the denture adhesive cream of the present embodiment realizes excellent high-temperature stability, bonding strength and long-acting antibacterial function through the synergistic effect of the three phases: the ordered crystal framework formed after the oil phase matrix is heated and melted gives the cream body the structural stability of maintaining semi-solid state; the three-dimensional network gel constructed by hydrogen bonding and physical block interaction of the gel matrix not only enhances the adhesion and shear resistance of the cream body, but also makes it have good adhesion and flexibility in the oral environment; the microcapsule functional phase realizes the controlled release of the antibacterial active ingredient, ensures the balance of oral microecology and prolongs the protection time. Thus, the three advantages of high-temperature stability, excellent bonding and sustained antibacterial function are taken into account, providing a safe, durable and temperature-responsive solution for natural denture fixation.

[0032] Preferably, the denture adhesive paste contains the following components in the range of 1.0-5.0wt.% of beeswax, 35.0-40.0wt.% of vegetable oil, 5.0-25.0wt.% of fenugreek gum, 25.0-45.0wt.% of locust bean gum, 1.0-3.0wt.% of modified metasilicate, 2.0-5.0wt.% of nanocellulose, and 7.0-10.0wt.% of fenugreek gum microcapsules. The base formed by beeswax and vegetable oil not only avoids the potential irritation of oil-based raw materials, but also gives the paste suitable thixotropy, making it smooth and easy to spread. The complex network of fenugreek gum and locust bean gum swells stably in a moist oral environment, not only improving the initial adhesion speed, but also

[0033] It remains durable and does not fall off under chewing and saliva flushing; the addition of modified metasilicate and nanocellulose further optimizes the rheological properties and storage stability, ensuring that the product can be stored for a long time at room temperature without delamination; the entire preparation process is directly compatible with existing vacuum emulsification equipment, and is simple to operate and easy to mass-produce.

[0034] Furthermore, the fenugreek gum microcapsules include a core material and a wall material covering the core material; the core material includes water-in-oil microdroplets containing antibacterial active ingredients; the wall material includes a shell material formed by the complex of fenugreek gum and chitosan. Through the organic combination of the water-in-oil microdroplet core material and the fenugreek gum-chitosan complex wall material, efficient encapsulation and intelligent controlled release of the antibacterial ingredients are achieved. The water-in-oil microdroplets stably encapsulate the active antibacterial agent in the oil phase, avoiding its failure due to hydrolysis or photooxidation during preparation and storage. The complex shell material gives the microcapsules good mechanical strength and shear resistance, allowing them to remain intact under the pressure of application and chewing, while slowly swelling and opening the shell under the action of oral temperature and saliva enzymes, releasing the antibacterial ingredients on demand, prolonging the antibacterial duration and reducing the impact on normal oral flora. In addition, the natural polymer wall material itself has biocompatibility and adhesion ability, which can also assist the overall adhesion performance of the paste, further improving the comfort and safety of use.

[0035] Furthermore, the modified metasilicate is obtained by grafting 3-aminopropyl triethoxysilane onto the surface of metasilicate; the vegetable oil includes one or more of sunflower oil, coconut oil, and peanut oil.

[0036] The modified metasilicate aluminum surface is introduced with 3-aminopropyl triethoxysilane, so that it has an amino-functionalized surface, which significantly improves the compatibility and interfacial bonding force with the organic colloidal network and the oil phase matrix; the amino group can form hydrogen bonds and electrostatic interactions with the colloidal phase, thereby enhancing the mechanical strength and thermal stability of the overall gel structure, and the lamellar structure of metasilicate aluminum can be physically embedded in the network pores, further inhibiting phase separation at high temperatures. The selected plant oils include at least one of sunflower oil, coconut oil, and peanut oil, preferably sunflower oil, which is rich in linoleic acid, giving the paste good fluidity and thixotropy; coconut oil has a small molecular weight, which can quickly dissolve beeswax and promote the dispersion of microcapsules; peanut oil has a moderate viscosity, which improves the lubrication and persistence during application. The compounding of various plant oils not only regulates the viscosity and melting point range of the paste, but also brings excellent biocompatibility and comfortable smell.

[0037] In general, the oil phase formed by the melting emulsification of beeswax and plant oil is semi-solid at a temperature lower than the melting point of its crystal framework, which provides the paste with basic shape retention and prevents it from flowing; when the temperature rises, this framework can partially loosen to adapt to the temperature fluctuations in the oral cavity, but it still does not completely lose support, thereby ensuring that the paste does not soften and ooze in summer or high-temperature environments; the three-dimensional network gel composed of fenugreek gum, locust bean gum, nanocellulose, and modified metasilicate aluminum "locks" the oil phase firmly in the network pores through hydrogen bonds, electrostatic interactions, and physical blocks, which greatly improves the shear resistance and centrifugal mechanical strength of the paste, ensuring that it does not fall off under dynamic loads such as chewing and brushing; on the other hand, its water phase affinity and swelling properties give the paste rapid initial adhesion and long-lasting adhesion, making the adhesive force both fast and stable; finally, the water-in-oil microemulsion droplets coated with fenugreek gum-chitosan composite wall material efficiently store the antibacterial active ingredients, which not only protect their stability during preparation and storage, but also slowly swell and open the shell under the stimulation of oral temperature and salivary enzymes, realizing sustained low-concentration release, long-term inhibition of harmful bacteria with less impact on normal flora, and providing additional adhesion and mechanical stability to the paste as a whole.

[0038] In general, the oil phase formed by the melting emulsification of beeswax and plant oil is semi-solid at a temperature lower than the melting point of its crystal framework, which provides the paste with basic shape retention and prevents it from flowing; when the temperature rises, this framework can partially loosen to adapt to the temperature fluctuations in the oral cavity, but it still does not completely lose support, thereby ensuring that the paste does not soften and ooze in summer or high-temperature environments; the three-dimensional network gel composed of fenugreek gum, locust bean gum, nanocellulose, and modified metasilicate aluminum "locks" the oil phase firmly in the network pores through hydrogen bonds, electrostatic interactions, and physical blocks, which greatly improves the shear resistance and centrifugal mechanical strength of the paste, ensuring that it does not fall off under dynamic loads such as chewing and brushing; on the other hand, its water phase affinity and swelling properties give the paste rapid initial adhesion and long-lasting adhesion, making the adhesive force both fast and stable; finally, the water-in-oil microemulsion droplets coated with fenugreek gum-chitosan composite wall material efficiently store the antibacterial active ingredients, which not only protect their stability during preparation and storage, but also slowly swell and open the shell under the stimulation of oral temperature and salivary enzymes, realizing sustained low-concentration release, long-term inhibition of harmful bacteria with less impact on normal flora, and providing additional adhesion and mechanical stability to the paste as a whole.

[0039] Specifically, the embodiment provides a preparation method of a denture adhesive paste, including the following steps:

[0040] S100, heating and stirring beeswax and plant oil to form an oil phase matrix;

[0041] S200, after adding fenugreek gum, locust bean gum, and nanocellulose to the oil phase matrix, performing first stirring treatment, and then adding modified metasilicate aluminum to perform second stirring treatment, to obtain a gel;

[0042] S300, adding fenugreek gum microcapsules in the colloid, and degassing and forming, cooling to obtain the denture adhesive paste.

[0043] Preferably, in step S100, the temperature of the heating and stirring treatment is 70-80℃. By heating the beeswax to its melting point and fully stirring with the vegetable oil, the two are uniformly mixed in the liquid phase state, and then during the cooling process, the beeswax molecules recrystallize to form an interconnected crystal framework, which "locks" the vegetable oil in its pores; this temperature-controlled responsive oil phase matrix can maintain a semi-solid state at oral temperature to prevent oil phase loss, and slightly soften at higher temperatures to adapt to chewing activities, thus achieving good form retention, thixotropy, and easy spreadability at the same time.

[0044] Further, pretreatment of the raw materials before preparation can significantly improve the purity and stability of the finished paste: melt the beeswax at 70-80℃ and filter it to remove plant impurities, propolis residues, and small particles, avoiding the formation of uneven particles or precipitates during subsequent emulsification and gelation, thus ensuring the transparency and smoothness of the oil phase matrix.

[0045] Further, activated carbon adsorption and decolorization and deodorization treatment of the vegetable oil, using the high specific surface area and rich pore structure of activated carbon, strongly adsorbs and removes pigment molecules and volatile aromatic compounds, keeping the oil phase nearly colorless and low in irritating odor, improving the appearance and smell of the paste, and reducing potential oxidation catalyst centers, prolonging the shelf life and improving the comfort of the user; preferably cold-pressed sunflower seed oil is used.

[0046] Preferably, in step S200, first add fenugreek gum, locust bean gum, and nanocellulose to the high-temperature liquid oil phase, use stirring to make the natural polysaccharides quickly absorb oil and swell and intertwine with each other, forming a preliminary three-dimensional network, the fenugreek gum and locust bean gum interact with the hydroxyl and fatty acid residues in the oil phase through hydrogen bonding and hydrophobic interaction, and the nanocellulose acts as a rigid skeleton, cross-linking with the polysaccharide chains through its long fibers, significantly improving the initial viscosity and shear strength of the colloid; the addition of modified metasilicate aluminum, whose amino-functionalized layers are electrostatically adsorbed and hydrogen-bonded to the polysaccharide network under stirring, further fills the network voids and enhances the interfacial bonding force, thus constructing a high-strength, reversible shear-responsive water-in-oil colloid that effectively traps the oil phase from flowing with shear and gives the paste good thixotropy and structure recovery.

[0047] Furthermore, in step S200, the colloidal precursor is stirred at 62–68°C and 200–300 rpm for 40–50 min, allowing fenugreek gum and locust bean gum to fully swell and disperse the nanocellulose uniformly at the appropriate temperature. Simultaneously, gentle shear force promotes the formation of hydrogen bonds and hydrophobic interactions between polymer chains, thus initially constructing a continuous and stable three-dimensional network. Subsequently, stirring at 250–350 rpm for 15–25 min further disperses the modified aluminosilicate sheets and embeds them into the existing network voids through stronger shear force, filling micropores and strengthening interfacial bonding, resulting in optimal homogeneity and mechanical strength of the colloid. Sieving through a 200-mesh sieve ensures consistent particle size of the fenugreek gum and locust bean gum, avoiding localized network defects caused by large particles, ultimately yielding a water-in-oil colloid with a compact structure, good thixotropic properties, and excellent shear resistance.

[0048] Furthermore, the preparation method of modified aluminum metasilicate includes the following steps:

[0049] S211. Disperse aluminum metasilicate powder in an ethanol solution, add 3-aminopropyltriethoxysilane, and sonicate for 8-12 min to obtain an aluminum metasilicate intermediate.

[0050] S212. Under a nitrogen atmosphere, the aluminum metasilicate intermediate is stirred at 60-80℃ for 3-5 hours, centrifuged and washed with ethanol 2-5 times, and dried at 70-90℃ for 5-7 hours to obtain modified aluminum metasilicate.

[0051] Preferably, through sol-gel in-situ grafting modification, 3-aminopropyltriethoxysilane is hydrolyzed in ethanol solution to generate silanol, which, under ultrasonication, fully contacts the surface of aluminosilicate powder to form Si-O-Al covalent bonds, anchoring the organic amino functional groups to the inorganic framework. Subsequently, further polycondensation and crosslinking are carried out in an inert nitrogen atmosphere at 60–80 °C to remove residual ethanol, and unreacted components are removed by multiple centrifugal washing.

[0052] Silane and byproducts were dried at 70–90 °C to obtain modified aluminum metasilicate with an amino-rich surface. This modified aluminum metasilicate not only significantly improved the dispersibility and interfacial compatibility of inorganic powders in the oil phase and polysaccharide network, but also enhanced the mechanical strength and thermal stability of the overall gel skeleton by forming hydrogen bonds and electrostatic adsorption with hydroxyl and carboxyl groups in the colloidal phase system through amino groups. Simultaneously, it reduced the risk of powder agglomeration and precipitation, ensuring the stability of the rheological properties and long-term storage stability of the paste.

[0053] Preferably, in step S300, after the pre-prepared Fenugreek gum microcapsules are added to the homogeneous colloid, degassing is performed, which can remove the air bubbles brought in during the mixing and stirring process by vacuum removal at a vacuum degree (absolute pressure) of 0.02 MPa to 0.1 MPa, a temperature of 40 to 45°C, and a time of 10 to 15 min, to avoid the occurrence of internal cavities or oxidation "hot spots" in the finished paste; then in the shaping and cooling stage, the oil phase, the colloid network, and the microcapsules are collectively solidified and shaped during the temperature drop, and the microcapsules are firmly "locked" into the gel-oil phase matrix. In this way, the paste is ensured to be smooth and free of pores on the surface, the structural uniformity and mechanical strength are improved, and the microcapsules can gradually swell or break at the expected rate at the temperature of the oral cavity, accurately releasing the antibacterial active ingredients, achieving long-acting antibacterial without affecting the initial adhesion.

[0054] Further, the preparation method of the Fenugreek gum microcapsules comprises the following steps:

[0055] S311, dissolving Fenugreek gum and chitosan in deionized water containing acetic acid at a mass ratio of (3-5):1, heating to 40-50°C and stirring until completely dissolved to obtain a Fenugreek gum-chitosan complex solution;

[0056] S312, dissolving the water-soluble antibacterial agent in water and adding it to the oil phase containing the emulsifier to obtain the core material;

[0057] S313, dropping the core material into the Fenugreek gum-chitosan complex solution, while adding a crosslinking agent under stirring, and obtaining Fenugreek gum microcapsules by spray drying.

[0058] Preferably, the preparation of the Fenugreek gum microcapsules is carried out by compounding Fenugreek gum and chitosan at a ratio of 3-5:1 at 40-50°C, using the electrostatic complex between the anionic and cationic polysaccharides to form a tough shell layer, and synchronously introducing a crosslinking agent when adding the oil phase "core material" containing the emulsifier, to further reinforce the shell structure microscopically; finally, the microcapsules obtained by spray drying not only can efficiently embed the antibacterial agent in the oil phase, but also can slowly release the active ingredients through the controlled permeation and degradation of the shell layer under the action of chewing and oral temperature, thereby enhancing the adhesion of the paste in the initial stage, achieving long-acting antibacterial and sustained adhesion, and significantly improving the use durability and oral safety of the adhesive paste.

[0059] Further, the active ingredients in the antibacterial oil phase include at least one of tea polyphenols, thymol, and cinnamaldehyde, and the carrier oil includes at least one of medium-chain triglyceride, sunflower seed oil, and coconut oil,

[0060] The emulsifying aid includes at least one of octyl glucoside and Tween-80; the crosslinking agent includes at least one of lemon, camphor, and procyanidin, and the carboxyl group of citric acid is subjected to amidation reaction with the amino group of chitosan, and the phenolic hydroxyl group of procyanidin is subjected to hydrogen bond network formation with fenugreek gum, so as to synergistically build a dense interpenetrating network wall material.

[0061] In addition, essential oils such as peppermint oil or menthol can be added to the denture adhesive paste, which not only masks the natural odor of beeswax, vegetable oil and polysaccharide, but also improves the olfactory comfort and experience of the user, and relieves the slight irritation and discomfort of the oral mucosa; in addition, peppermint oil and menthol itself has certain antibacterial and analgesic effect, which can synergize with the bacteriostatic ingredients in the microcapsule, further improve the oral environment, and enhance the subjective satisfaction of the wearer.

[0062] Embodiment 1

[0063] The present embodiment provides a denture adhesive paste, which is used as shown in Figure 1 The denture adhesive paste comprises the following components in percentage by weight:

[0064] Beeswax: 3.0wt.%, sunflower seed oil: 35.0wt.%, fenugreek gum: 15wt.%, locust bean gum: 32.0wt.%, modified metasilicate: 2.0wt.%, nanocellulose: 4.0wt.%, peppermint oil: 0.5wt.%; fenugreek gum microcapsule: 8.5wt.%.

[0065] The preparation method comprises the following steps:

[0066] S100, the beeswax and sunflower seed oil are subjected to heating and stirring treatment at 75℃ and 150rpm to form a molten oil phase matrix;

[0067] S211, the metasilicate powder is dispersed in an ethanol solution, 3-aminopropyl triethoxysilane is added, and ultrasonic treatment is performed for 10min to obtain a metasilicate intermediate;

[0068] S212, the metasilicate intermediate is subjected to stirring at 70℃ for 4h under a nitrogen atmosphere, centrifugal washing with ethanol is performed for 3 times, and drying is performed at 80℃ for 6h to obtain the modified metasilicate;

[0069] S200, after the fenugreek gum, locust bean gum and nanocellulose are added to the oil phase matrix, first stirring treatment is performed at 65℃ and 250rpm for 45min, then the modified metasilicate is added, and second stirring treatment is performed at 300rpm for 20min to obtain a gel;

[0070] S311, the fenugreek gum and chitosan are dissolved in deionized water containing acetic acid at a mass ratio of 4:1, heated to 45℃ and stirred until completely dissolved to obtain a fenugreek gum-chitosan composite solution;

[0071] S312, dissolving tea polyphenol in sunflower oil to form a bacteriostatic oil phase containing 10% tea polyphenol, obtaining

[0072] the core material;

[0073] S312, slowly dripping the core material into the fenugreek gum-chitosan composite solution, while adding citric acid under stirring, and performing spray drying by an inlet air temperature of 150℃, an outlet air temperature of 70℃, and an atomizer rotating speed of 20000rpm, to obtain fenugreek gum microcapsules;

[0074] S300, adding the fenugreek gum microcapsules and peppermint oil into the gel, and performing stirring treatment at 100rpm, degassing treatment at a vacuum degree (absolute pressure) of 0.05MPa for 15min, hot filling into an aluminum plastic tube, and sealing and cooling to form at room temperature, to obtain the denture adhesive paste;

[0075] In step S100, the beeswax is melted and filtered at 75℃ before being added; in step S200, the fenugreek gum is mixed with locust bean gum, and sieved through a 200-mesh sieve.

[0076] Example 2

[0077] This example provides a denture adhesive paste, and the specific steps refer to Example 1, and the difference lies in different component contents, and the specific component contents refer to Table 1:

[0078] Table 1

[0079]

[0080]

[0081] Example 3

[0082] This example provides a denture adhesive paste, and the specific steps refer to Example 1, and the difference lies in the selection of various process parameters, and the specific process parameters refer to Table 2:

[0083] Table 2

[0084]

[0085]

[0086] Comparative Example 1

[0087] This comparative example provides a denture adhesive paste, which is obtained by outsourcing.

[0088] Physical and chemical performance test

[0089] The performance determinations such as high temperature stability test, adhesive strength test, endurance test, biocompatibility test, etc. of Examples 1-3 and Comparative Example 1 were carried out, and the test methods are shown as follows, and the results are shown in Table 3.

[0090] (1) High temperature stability test: the denture adhesive paste samples prepared from Examples 1-3 and Comparative Example 1 were taken, and were loaded into transparent glass bottles and sealed; the samples were placed in a 45℃ constant temperature box with a humidity of 75%, and were continuously observed for 90 days, and the comparison chart before and after 90 days is shown as Figure 2 ;

[0091] (2) Adhesive strength test: according to EN ISO 10873:2021, on-machine sample testing was carried out using a servo material machine; after soaking in a 37℃ water bath for 1 min, after 30 s under the action of a 9.8N load, the maximum resistance of the pressure sensitive shaft was recorded, the adhesive strength per unit area was calculated, and this test was repeated, 3 test results were obtained for one sample, and the average value was taken.

[0092] (3) Endurance test: simulate the oral environment, evenly coat the specially prepared mold, immerse it in 36℃ artificial saliva (pH 6.8), and pass in CO2 gas, apply a 4.9N upward tension, connect a stress sensing device, and record the stress change curve, and the time of mold separation and detachment;

[0093] (4) Biocompatibility test: 20 volunteers wearing dentures were selected, and the denture adhesive pastes of Examples 1-3 and Comparative Example 1 were used respectively.

[0094] Table 3

[0095]

[0096]

[0097] Based on the tests of Examples 1-3 and Comparative Example 1, the denture adhesive paste of the present application realizes the excellent performance of no delamination at 45℃ for 90 days, strong stability, good adhesive effect, endurance improvement, and no pathological stimulation and foreign body sensation through the three-phase synergy of oil phase skeleton-interpenetrating gel network-microcapsule slow release and the ratio of locust bean gum and fenugreek gum. Compared with the commercially available comparative product, the high temperature stability, adhesion and endurance are significantly enhanced, and through the reinforcement of nanocellulose and the sustained 12h antibacterial and slow release of chitosan-fenugreek gum composite wall material microcapsules, the technical difficulties of traditional adhesive paste softening at high temperature, easy loss and poor biocompatibility are solved.

[0098] In the description of the specification, the description of the terms "one embodiment", "some embodiments", "certain embodiments", and the like are intended to indicate that the described implementation, feature, structure, material or characteristic is included in at least one embodiment or example of the application. The above described terms are not necessarily indicative of the same embodiment or example. Moreover, the described implementation, feature, structure, material or characteristic can be combined in any one or more embodiments or examples in a suitable manner.

[0099] Although the present application has been disclosed in its currently best embodiment with reference to the drawings, it will be understood that it is not limited to the details of the specific embodiment, which can be varied in many ways. It is therefore desired that the present application be construed as not limited to the specific embodiment set forth above, but rather only by the appended claims.

Claims

1. A denture securing paste, characterized in that, The denture fixation paste comprises an oil phase matrix, a gel matrix, and a microcapsule functional phase; The oil phase matrix is ​​formed by the melt emulsification of beeswax and vegetable oil; The gel matrix includes fenugreek gum, locust bean gum, nanocellulose, and modified aluminum metasilicate; The microcapsule functional phase includes fenugreek gum microcapsules, and the microcapsule functional phase is dispersed in the oil phase matrix and the gel matrix.

2. The denture securing paste according to claim 1, characterized in that, The content range of each component of the denture bonding paste, by weight, is as follows: The beeswax: 1.0–5.0 wt.%, the vegetable oil: 35.0–40.0 wt.%, the fenugreek gum: 5.0–25.0 wt.%, the locust bean gum: 25.0–45.0 wt.%, the modified aluminum metasilicate: 1.0–3.0 wt.%, the nanocellulose: 2.0–5.0 wt.%, and the fenugreek gum microcapsules: 7.0–10.0 wt.%.

3. The denture securing paste according to claim 1, characterized in that, The fenugreek microcapsule includes a core material and a wall material covering the core material; The core material comprises water-in-oil microemulsion droplets containing antibacterial active ingredients; The wall material comprises a shell material formed by a composite of fenugreek gum and chitosan.

4. The denture securing paste according to claim 1, characterized in that, The modified aluminum metasilicate is obtained by grafting 3-aminopropyltriethoxysilane onto the surface of aluminum metasilicate; The vegetable oils include one or more of sunflower seed oil, coconut oil, and peanut oil.

5. A method for preparing a denture bonding paste, characterized in that, The preparation method is used to prepare the denture adhesive as described in any one of claims 1 to 4, and includes the following steps: S100. Beeswax and vegetable oil are heated and stirred to melt and form an oil phase matrix; S200: After adding the fenugreek gum, the locust bean gum and the nanocellulose to the oil phase matrix, a first stirring treatment is performed, and then the modified aluminum metasilicate is added and a second stirring treatment is performed to obtain a gel. S300: Add the fenugreek gum microcapsules to the gel, and degas, shape, and cool to obtain the denture fixation paste.

6. The preparation method according to claim 5, characterized in that, In step S100, The heating and stirring process is carried out at a temperature of 70–80°C and a rotation speed of 100–200 rpm. The beeswax is melted and filtered at 70-80°C before being added.

7. The preparation method according to claim 5, characterized in that, In step S200, the method for preparing the modified aluminum metasilicate includes the following steps: S211. Disperse aluminum metasilicate powder in an ethanol solution, add 3-aminopropyltriethoxysilane, and sonicate for 8-12 min to obtain an aluminum metasilicate intermediate. S212. Under a nitrogen atmosphere, the aluminum metasilicate intermediate is stirred at 60-80°C for 3-5 hours, centrifuged and washed with ethanol 2-5 times, and dried at 70-90°C for 5-7 hours to obtain the modified aluminum metasilicate.

8. The preparation method according to claim 5, characterized in that, In step S200, The temperature of the first stirring treatment is 62-68℃, the speed is 200-300 rpm, and the time is 40-50 min; The second stirring process is carried out at a rate of 250–350 rpm for 15–25 min. The fenugreek gum and the locust bean gum are mixed and sieved through a 200-mesh sieve.

9. The preparation method according to claim 5, characterized in that, The preparation method of the fenugreek gelatin microcapsules includes the following steps: S311. Dissolve the fenugreek gum and chitosan in deionized water containing acetic acid at a mass ratio of (3-5):1, heat to 40-50℃ and stir until completely dissolved to obtain a fenugreek gum-chitosan composite solution. S312. Dissolve the water-soluble antibacterial agent in water and add it to the oil phase containing the emulsifier to obtain the core material; S313. The core material is dropped into the fenugreek gum-chitosan composite solution, and a crosslinking agent is added while stirring. The fenugreek gum microcapsules are obtained by spray drying.

10. The preparation method according to claim 5, characterized in that, In step S300, The degassing process is carried out at a vacuum of 0.02–0.1 MPa, a temperature of 40–45 °C, and a time of 10–15 min.

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