Probiotic dietary fiber composite composition for body weight management and preparation method thereof
Through innovative design of materials such as mesoporous silica-magnesium aluminum layered double hydroxide hybrid nanocarrier and zinc-doped calcium phosphate-silica core-shell nanoparticles, a multi-level protection and release system was constructed, which solved the problems of probiotic stability and targeted delivery in the gastric acid environment, and realized the efficient colonization of probiotics and multiple weight management functions.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-01-12
- Publication Date
- 2026-03-31
AI Technical Summary
Existing probiotic products are prone to damage to live bacteria in the acidic environment of the stomach, making it difficult to target and reach the colon. Dietary fiber has a single function and lacks synergistic effects, failing to effectively solve the problems of protecting, controlling release, and targeted delivery of active ingredients.
By employing materials such as mesoporous silica-magnesium aluminum layered double hydroxide hybrid nanocarriers and zinc-doped calcium phosphate-silica core-shell nanoparticles, a multi-layered protection and release system is constructed through precise processes. Combined with cellulose nanofibers and carrageenan to construct a three-dimensional gel network, this system achieves efficient protection of probiotics and multiple weight management functions.
It significantly enhances probiotic activity, enabling efficient targeted delivery and colonization of probiotics, synergistically reducing fat digestion and absorption, providing physical satiety and nutrient proliferation, and achieving a multi-dimensional intervention in weight management through the synergistic effect of multiple mechanisms.
Abstract
Description
Technical Field
[0001] This invention relates to the field of functional food technology, specifically to a probiotic dietary fiber complex composition for weight management and its preparation method. Background Technology
[0002] With the changing lifestyles of modern society, overweight and obesity have become major challenges affecting public health. They are not only related to physical appearance but are also significant risk factors for various chronic metabolic diseases such as diabetes and cardiovascular disease. Traditional weight management methods mainly include dietary control and increased exercise; however, long-term adherence is difficult for many, and the effects are prone to rebound. Therefore, developing safe, effective, and easily adhered weight management aids has become a research hotspot in food science and nutrition. Against this backdrop, the application of theories based on gut microbiota regulation is gradually emerging. Scientific research shows that imbalances in the gut microbiota are closely related to the occurrence and development of obesity, and adjusting the composition of the gut microbiota through dietary intervention is considered a promising new approach. Many existing products attempt to simply combine probiotics with dietary fiber, hoping to aid weight control through the colonization effect of probiotics and the satiety effect of fiber. However, these initial attempts often overlook the stability and targeting issues of active ingredients in the complex environment of the body, resulting in actual efficacy far below theoretical expectations and failing to meet the urgent market demand.
[0003] Currently, probiotic and dietary fiber combination products used in weight management face several key technological bottlenecks. First, most probiotic strains are extremely sensitive to the highly acidic environment of the stomach and bile salts in the intestines. The number of live bacteria decreases significantly during processing, storage, and digestive tract transport after oral administration, resulting in a very low proportion of live bacteria actually reaching the colon and exerting their regulatory effects, severely limiting their efficacy. Second, commonly used dietary fibers or carrier materials have relatively limited functions, either focusing on physical adsorption of fats or increasing satiety, or acting solely as prebiotics, lacking integrated designs that can synergistically enhance effects and target multiple sites. More importantly, existing technologies have failed to effectively address the core issues of protecting, controlling the release of, and targeting the active ingredients. For example, some studies have used conventional microencapsulation technology to encapsulate probiotics, but its protective effect is limited and it cannot achieve intelligent release based on the pH environment of different gastrointestinal segments. Furthermore, how to integrate multiple functions such as mineral supplementation, fat adsorption, and prebiotic delivery into a stable and efficient system, while ensuring the biocompatibility and safety of all components, is a complex problem that current technology has not yet fully solved.
[0004] To overcome the aforementioned limitations, industry and research urgently need a novel design approach and material system. An ideal product composition not only requires scientifically formulated probiotics and prebiotics, but also an innovative carrier system that provides robust protection for probiotics throughout their lifecycle and offers multiple weight management functions. This carrier system should possess excellent biocompatibility, remaining intact in the acidic conditions of the stomach to protect internal active substances, while intelligently responding and releasing probiotics in the neutral intestinal environment to ensure high survival and colonization efficiency. Simultaneously, the carrier itself should ideally contribute additional health benefits, such as adsorbing some dietary fat, slowing sugar absorption, or providing beneficial minerals, thereby creating a synergistic amplification effect with probiotics and dietary fiber. Therefore, developing a composite composition that combines advanced materials science and nutritional principles, achieving efficient delivery of active ingredients and integration of multiple physiological functions through precise formulation design and controllable preparation processes, is crucial for advancing the development of next-generation weight management functional foods. This is precisely the core technical problem and the starting point of this invention. Summary of the Invention
[0005] The purpose of this invention is to provide a probiotic dietary fiber compound composition and preparation method for weight management, which solves the problems of existing probiotic products where live bacteria are easily destroyed by gastric acid and have difficulty reaching the colon, as well as the single weight management mechanism and lack of synergistic effect of ordinary dietary fiber.
[0006] The present invention achieves the above objectives through the following technical solutions: A method for preparing a probiotic dietary fiber complex composition for weight management, comprising the following steps: S1. By weight, 3-15 parts of mesoporous silica-magnesium aluminum layered double hydroxide hybrid nanocarrier are dispersed in sterile phosphate buffer, then mixed with compound probiotic lyophilized powder, shaken and adsorbed at 3-5℃, and freeze-dried to obtain a functional carrier loaded with probiotics; 20-40 parts of cellulose nanofibers and 4-6 parts of carrageenan are mixed in deionized water at 68-72℃, and 3-5 parts of curcumin ethanol solution are added, and homogenized to obtain a composite hydrophobic gel matrix; S2. First, mix the probiotic-loaded functional carrier obtained in step S1 with 5-10 parts by weight of maltodextrin to obtain a premix; then add the premix, 12-16 parts of zinc-doped calcium phosphate-silica core-shell nanoparticles, 10-15 parts of fructooligosaccharides, and 5-15 parts of maltodextrin to the composite hydrophobic gel matrix obtained in step S1, and homogenize at 3000-4000 rpm to obtain a mixture; inject the mixture into a mold for pre-freezing and then freeze-dry to obtain a dry composite powder; mix the dry composite powder with 10-20 parts of steviol glycosides and 3-5 parts of silica, and sieve.
[0007] In this invention, the preparation mechanism of the probiotic dietary fiber composite composition for weight management is a multi-scale, multi-component ordered integration and structural fixation physicochemical process. This process begins with the modular pretreatment of functional components, where probiotics are loaded onto the mesopores and layered structure gaps of a hybrid nanocarrier through physical adsorption. Freeze-drying removes moisture, bringing the bacteria to a dormant and stable state. Simultaneously, cellulose nanofibers and carrageenan are bonded together in hot water through hydrogen bonds, ionic bonds, and molecular chain entanglement, constructing a three-dimensional hydrogel network. Hydrophobic curcumin molecules are embedded within the hydrophobic microregions of this network. The core composite step combines macroscopic homogenization and microscopic structural nesting. The probiotic-loaded carrier, core-shell nanoparticles, prebiotics, and other solid components are homogenized with the gel matrix at high speed. The enormous shear force causes the solid particles to disperse uniformly and embed within the gel network, while maltodextrin and other components fill the gaps, forming a composite "wet material" consisting of a continuous gel phase encapsulating a multifunctional particulate dispersion phase. The final freeze-drying process is crucial for giving the product its final form and structure. Pre-freezing causes the moisture in the material to solidify into ice crystals. The growth of these ice crystals displaces the surrounding solid components, and then, under vacuum conditions, the ice crystals sublimate directly, leaving behind a porous framework structure formed by the ice crystal template. This porous structure maximizes the preservation of the spatial distribution and activity of each component, resulting in a final product with excellent rehydration properties. The entire preparation mechanism is interconnected, from nanoscale surface modification and coating, to microscale particle dispersion and gel encapsulation, and finally to macroscale porous structure formation, ultimately achieving the precise positioning and stabilization of multiple functional components in a stable and easy-to-use solid form.
[0008] According to a preferred embodiment of the present invention, in step S1, the compound probiotic freeze-dried powder is prepared by mixing Lactobacillus plantarum, Lactobacillus reuteri, and Bifidobacterium animalis subsp. lactis.
[0009] According to a preferred embodiment of the present invention, in step S2, the homogenization time at 3000-4000 rpm is 5-10 min.
[0010] According to a preferred embodiment of the present invention, the method for preparing the mesoporous silica-magnesium aluminum layered double hydroxide hybrid nanocarrier includes: A1. Dissolve hexadecyltrimethylammonium bromide in an ammonia solution; add tetraethyl orthosilicate, and stir continuously at 38-42℃ to obtain a suspension; collect the precipitate by centrifugation, wash alternately with ethanol and deionized water, and dry under vacuum at 58-62℃ to obtain a mesoporous silica nanoparticle precursor; disperse the mesoporous silica nanoparticle precursor in anhydrous toluene, add 3-aminopropyltriethoxysilane, react under reflux conditions, and wash by centrifugation to obtain aminated mesoporous silica nanoparticles; disperse the aminated mesoporous silica nanoparticles in nitrogen-deoxygenated deionized water, and sonicate to obtain a dispersion; A2. Under nitrogen protection and stirring, a mixed salt solution containing magnesium nitrate and aluminum nitrate is mixed with a mixed alkaline solution containing sodium hydroxide and sodium carbonate to obtain a core slurry. The core slurry is added to the dispersion and crystallized under stirring. The pH value is adjusted to 9.5-10.0 and aged at 64-66℃. After the reaction is completed, the product is collected by centrifugation, washed with deionized water until neutral, and finally vacuum dried at 78-82℃ and ground.
[0011] In this invention, the core of the preparation reaction mechanism of the mesoporous silica-magnesium-aluminum layered double hydroxide hybrid nanocarrier lies in the sequential process of template-guided synthesis, surface chemical modification, and heterogeneous nucleation crystal growth. First, under alkaline conditions, surfactant molecules self-assemble to form a micelle template. Tetraethyl orthosilicate, acting as a silicon source, undergoes hydrolysis and subsequent condensation. Its silanol groups cross-link and polymerize on the surface of the micelle template, forming an amorphous silica framework. After removing the template, mesoporous silica nanoparticles with regular nanopores are obtained. The surface of these particles is rich in silanol groups, laying the foundation for subsequent functionalization. The key modification step involves using a silane coupling agent to undergo a condensation reaction with the surface silanol groups, covalently grafting amino functional groups onto the surface of the mesoporous silica, thereby changing the surface properties from hydrophilic to positively charged. This transformation is crucial for the successful construction of the subsequent hybrid structure. Subsequently, in a strictly pH-controlled alkaline environment, magnesium and aluminum ions co-precipitate on the surface of aminated silica. The positively charged sites provided by the amino groups effectively adsorb negatively charged metal hydroxyl complex ions, inducing preferential heterogeneous nucleation of layered double hydroxide crystal nuclei on their surface rather than homogeneous nucleation in solution. As the crystallization and aging process proceeds, these nuclei preferentially grow along a two-dimensional direction, ultimately resulting in the in-situ growth of vertically aligned magnesium-aluminum layered double hydroxide nanosheets on the surface of the mesoporous silica particles, forming a hybrid structure with mesoporous silica as the core and layered double hydroxide sheets as petal-like structures. This structure achieves a perfect combination of the high loading capacity of mesopores and the pH-responsive dissociation characteristics of layered double hydroxides.
[0012] According to a preferred embodiment of the present invention, in step A1, the reaction is continuously stirred at 38-42°C for 2-4 hours.
[0013] According to a preferred embodiment of the present invention, in step A2, the aging time at 64-66°C is 18-20 hours.
[0014] According to a preferred embodiment of the present invention, the method for preparing the zinc-doped calcium phosphate-silica core-shell nanoparticles includes: B1. Under room temperature and nitrogen protection, disodium hydrogen phosphate was dissolved in deionized water to obtain solution A; a mixed salt containing calcium nitrate and zinc nitrate was dissolved in deionized water, and the pH was adjusted to 8.8-9.2 to obtain solution B; solution A was poured into solution B with stirring to obtain a colloidal precipitate, and the reaction was continued with stirring; the reaction system was then transferred to a high-pressure reactor and hydrothermally reacted at 115-125℃; after natural cooling, the precipitate was collected by centrifugation, washed with deionized water and ethanol respectively, and dried at 58-62℃ to obtain zinc-doped hydroxyapatite nanorod precursor; B2. Zinc-doped hydroxyapatite nanorod precursors were dispersed in a mixed solution of ethanol and water. Vinyltrimethoxysilane was added, and the mixture was sonicated, stirred, and centrifuged to obtain surface-hydrophobic modified nanorods. The surface-hydrophobic modified nanorods were dispersed in a mixed solution of ethanol, deionized water, and concentrated ammonia, and sonicated to obtain a dispersion. Tetraethyl orthosilicate was added dropwise to the dispersion while stirring. After the addition was complete, the reaction was continued at room temperature. After the reaction was completed, the precipitate was collected by centrifugation, washed with ethanol, and dried under vacuum at 60-80℃.
[0015] In this invention, the preparation of zinc-doped calcium phosphate silica core-shell nanoparticles involves three key stages: co-precipitation crystallization, surface hydrophobic modification, and sol-gel encapsulation. The first stage involves the synthesis of a zinc-doped calcium phosphate core via hydrothermal co-precipitation. In an alkaline environment, calcium, zinc, and phosphate ions meet, and based on the principles of heterogeneous nucleation and crystal growth, amorphous precursors are formed through co-precipitation. Subsequently, under high temperature and pressure in a hydrothermal environment, this precursor undergoes dissolution and recrystallization, driving the crystal to transform into the more thermodynamically stable hydroxyapatite phase and grow along a specific crystal orientation into a nanorod-like morphology. Trace amounts of zinc ions enter the calcium phosphate lattice through isomorphic substitution, achieving uniform doping at the atomic scale. The second stage involves surface modification, utilizing a silane coupling agent for chemical grafting onto the nanorod surface. The alkoxy group at one end of the coupling agent molecule undergoes hydrolytic condensation with the hydroxyl groups on the nanorod surface, forming a stable silicon-oxygen bond. This firmly grafts the organic functional groups (such as vinyl groups) at the other end onto the particle surface, significantly reducing the polarity of the particle surface and enhancing its hydrophobicity. The third stage involves the encapsulation of a silica shell using the classic sol-gel method. Under the catalysis of ammonia, tetraethyl orthosilicate hydrolyzes in an aqueous ethanol solution to generate silicic acid. These silicic acid monomers are adsorbed on the hydrophobically modified calcium phosphate nanorod surface and undergo condensation polymerization. Due to the guiding effect of surface modification, the nucleation and growth of silica are confined to the nanorod surface, gradually accumulating and cross-linking to form a uniform, dense amorphous silica shell, ultimately constituting a core-shell structure. The subsequent drying process aims to completely remove organic residues and strengthen the network structure of the silica shell, ensuring its stability.
[0016] According to a preferred embodiment of the present invention, in step B1, the hydrothermal reaction time at 115-125°C is 6-8 hours.
[0017] According to a preferred embodiment of the present invention, in step B2, the vacuum drying time at 60-80°C is 2-3 hours.
[0018] The present invention also provides a probiotic dietary fiber complex composition for weight management prepared according to the preparation method of the probiotic dietary fiber complex composition for weight management.
[0019] The beneficial effects of this invention are as follows: This invention provides a probiotic dietary fiber complex composition for weight management and its preparation method. Through innovative material design and precise process integration, it achieves multi-layered synergistic enhancements, significantly surpassing existing single probiotic products or simple physical mixtures of synbiotic preparations. Its core effect is primarily reflected in the revolutionary improvement of probiotic activity and efficacy. The invention's unique mesoporous silica-magnesium-aluminum layered double hydroxide hybrid nanocarrier, through sophisticated surface amination modification and interface growth technology, successfully constructs a micro-nano protective chamber with intelligent responsive characteristics. This carrier maintains structural stability in a simulated highly acidic environment of the stomach, effectively isolating the probiotics loaded within from harsh external conditions, thus achieving highly efficient protection of the strains and greatly reducing the killing of live bacteria by gastric acid and digestive enzymes. When the complex enters the neutral-to-alkaline environment of the intestine, the layered double hydroxide components in the carrier undergo controllable degradation, achieving targeted sustained release of probiotics and ensuring that a large number of highly active probiotics accurately reach the colon for colonization and proliferation. This pH-responsive intelligent delivery system fundamentally solves the traditional industry bottleneck of low survival rate of live bacteria after oral administration of probiotic products, which prevents them from effectively reaching the site of action, laying a solid foundation for probiotics to exert their core function of regulating the gut microbiota.
[0020] Secondly, the technical effect of this invention lies in constructing a multi-dimensional, synergistic, composite functional system that works together to address key aspects of weight management. Zinc-doped calcium phosphate silica core-shell nanoparticles not only serve as a source of mineral supplementation, but their unique core-shell structure and hydrophobic surface modification endow them with excellent adsorption capacity for lipids and bile acids, enabling them to physically intercept some dietary fats in the intestines and reduce their digestion and absorption. These particles work synergistically with a hybrid nanocarrier carrying probiotics and a three-dimensional gel network constructed from cellulose nanofibers and carrageenan. The gel network swells upon contact with water, providing a significant physical feeling of fullness and delaying gastric emptying; while the two inorganic nanomaterials respectively perform the functions of bioactive protective delivery and physical adsorption blocking. Simultaneously, the carefully formulated prebiotics, such as fructooligosaccharides, provide exclusive nutrition for the targeted release of probiotics, stimulating their metabolism to produce beneficial short-chain fatty acids. This multi-mechanism of "physical satiety, intelligent bacterial delivery, targeted lipid inhibition, and nutrient proliferation" is interconnected and reinforces each other. Through the synergistic effect of multiple pathways such as reducing energy intake, regulating energy metabolism, and improving the intestinal environment, it achieves a three-dimensional intervention in the complex physiological process of weight management. Its comprehensive effect is far superior to the simple superposition of any single functional component.
[0021] Finally, this invention, while achieving superior biological functions, also demonstrates excellent process adaptability and product stability, showing clear prospects for industrialization. The entire preparation method is rationally designed, and all selected raw materials are commercially available. Through standardized food processing technologies such as stepwise mixing, homogenization, pre-freezing, and freeze-drying, components with different properties, such as probiotics, inorganic nanomaterials, and dietary fiber, can be stably integrated into a unified product matrix. The freeze-drying process maximizes the preservation of the activity of probiotics and the functions of other heat-sensitive components. The final product is a dry solid powder or pulverized granules with good flowability, facilitating quantitative dispensing, storage, transportation, and consumer consumption. It can be used directly for brewing or further prepared into tablets or capsules. The functional components in the entire system, especially the two inorganic modified compounds, are organically embedded in the gel network and carbohydrate matrix. This not only further ensures its stability during storage and transportation but also effectively reduces the potential bioactivity of nanomaterials during digestion, improving the safety margin from a product engineering perspective. Therefore, this invention not only provides a high-efficiency weight management solution, but also has a solid technical foundation for transforming it into stable, reliable functional foods or health products suitable for large-scale production. Detailed Implementation
[0022] The following detailed embodiments are only used to further illustrate this application and should not be construed as limiting the scope of protection of this application. Those skilled in the art can make some non-essential improvements and adjustments to this application based on the above application content.
[0023] Example 1 Mesoporous silica-magnesium-aluminum layered double hydroxide hybrid nanocarriers were prepared. First, 48 L of deionized water and 2 L of 28% (w / w) concentrated ammonia solution were mixed in a 100 L glass reactor. Stirring was started and the mixture was heated to 40 °C in a water bath. 1.0 kg of cetyltrimethylammonium bromide was added to the solution, and the mixture was stirred at 500 rpm at 40 °C until completely dissolved and clear. Then, using a constant-pressure dropping funnel, 2.0 L of tetraethyl orthosilicate was uniformly added dropwise to the solution over 1 hour. After the addition was complete, the mixture was stirred at 40 °C and 500 rpm for 3 hours. After the reaction, the resulting white suspension was transferred to a continuous flow centrifuge and centrifuged at 10,000 rpm for 10 minutes to collect the solid precipitate. The precipitate was redispersed in 10 L of anhydrous ethanol, sonicated for 15 minutes, and centrifuged again. This ethanol washing step was repeated three times. Subsequently, the same washing procedure was performed three times with 10 L of deionized water. The final washed white solid was transferred to a vacuum drying oven and dried at 60℃ and -0.1MPa for 12 hours to obtain dried mesoporous silica nanoparticle precursor powder. In the second step, 500g of the precursor powder was placed in a 20L three-necked flask, and 10L of anhydrous toluene was added. The mixture was stirred under nitrogen protection to form a suspension. A reflux condenser was installed, and the system was heated to 110℃ in an oil bath. After the temperature stabilized, 50mL of 3-aminopropyltriethoxysilane was added via syringe, and the mixture was refluxed at 110℃ and 300rpm for 8 hours. After the reaction, the system was cooled to room temperature, and the material was transferred to a centrifuge tube. The solid was collected by centrifugation at 8000rpm for 5 minutes. The solid was dispersed in 5L of fresh anhydrous ethanol and washed by centrifugation. This process was repeated three times. Finally, the obtained solid was vacuum dried at 60℃ for 6 hours to obtain aminated mesoporous silica nanoparticles. Third, weigh 200g of the amination-modified particles and add them to 20L of deionized water that has been deoxygenated by bubbling under nitrogen for 30 minutes. Under ice-water bath conditions, sonicate the solution using a 500W ultrasonic cell disruptor for 30 minutes to obtain a uniform dispersion A. In a nitrogen-atmospheric glove box, prepare mixed salt solution B: dissolve 71.79g of magnesium nitrate hexahydrate and 37.51g of aluminum nitrate nonahydrate in 1L of deoxygenated deionized water; prepare mixed alkali solution C: dissolve 32.00g of sodium hydroxide and 21.20g of anhydrous sodium carbonate in 1L of deoxygenated deionized water. Under nitrogen protection and continuous stirring, simultaneously and at the same rate, add solutions B and C to a 1L beaker through two dropping funnels, mixing rapidly within 30 seconds to immediately form a milky white LDH nucleation slurry D. Immediately pour all of slurry D into dispersion A. The mixture was transferred to a 40°C water bath, and the pH was precisely adjusted to 9.8 with 1 mol / L sodium hydroxide solution while stirring. Subsequently, the reactor was transferred to a 65°C constant-temperature water bath, and the crystallization aging reaction was carried out for 19 hours with continuous stirring.After the reaction was completed, the product was collected by centrifugation at 10,000 rpm for 10 minutes and washed repeatedly with deionized water until the conductivity of the supernatant was below 10 μS / cm and the pH was 7. The resulting paste product was spread evenly on a tray and placed in a vacuum drying oven at 80℃ and -0.1 MPa for 24 hours. Finally, the dried block was ground in an agate mortar and passed through a 200-mesh sieve to obtain mesoporous silica-magnesium aluminum layered double hydroxide hybrid nanocarrier powder.
[0024] Preparation of Zinc-Doped Calcium Phosphate-Silica Core-Shell Nanoparticles. Step 1: Solution Preparation: Weigh 28.39 g of disodium hydrogen phosphate into a 2 L beaker, add 1.0 L of deionized water, and stir magnetically until completely dissolved. Label this solution A. Weigh 70.86 g of calcium nitrate tetrahydrate and 8.92 g of zinc nitrate hexahydrate into another 2 L beaker, add 1.0 L of deionized water, and stir until dissolved. While stirring, add 25% ammonia solution dropwise to this mixed salt solution until the pH stabilizes at 9.0. Label this solution B. Step 2: Under room temperature and nitrogen protection, rapidly pour solution A into solution B within 10 seconds, immediately forming a white gel-like precipitate. Continuously stir this mixture at 500 rpm for 1 hour. Third, the entire suspension was transferred to a 5L polytetrafluoroethylene-lined high-pressure reactor, sealed, and placed in a forced-air drying oven. The temperature was increased from room temperature to 120°C at a rate of 2°C / min, and maintained at this temperature for 7 hours for hydrothermal reaction. After the reaction, the oven was closed and allowed to cool naturally to room temperature. The reactor was opened, and the contents were transferred to a centrifuge cup. The precipitate was collected by centrifugation at 8000 rpm for 8 minutes. The precipitate was washed three times with 1.5L of deionized water by centrifugation, and then three times with 1.0L of anhydrous ethanol by centrifugation. The washed precipitate was placed in a vacuum drying oven and dried at 60°C for 10 hours to obtain the zinc-doped hydroxyapatite nanorod precursor. Fourth, 100g of the above precursor was taken and dispersed in a mixed solvent consisting of 1.6L of anhydrous ethanol and 0.4L of deionized water in a 3L round-bottom flask and ultrasonically dispersed for 30 minutes. Add 20 mL of vinyltrimethoxysilane to the mixture, and reflux the mixture in a 60°C water bath at 400 rpm for 5 hours. After the reaction, collect the solid by centrifugation and wash it three times with 500 mL of anhydrous ethanol to obtain surface-modified hydrophobic nanorods. In the fifth step, disperse 50 g of the modified nanorods in a mixed solution composed of 800 mL of anhydrous ethanol, 200 mL of deionized water, and 20 mL of concentrated ammonia (28%), and sonicate for 30 minutes to form a uniform dispersion. Under gentle stirring at room temperature and 300 rpm, use a constant pressure dropping funnel to add 50 mL of tetraethyl orthosilicate dropwise to the dispersion at a uniform rate over 1 hour. After the addition is complete, continue stirring at room temperature for 12 hours. After the reaction is complete, collect the solid product by centrifugation and wash it three times with 400 mL of anhydrous ethanol. Place the final product in a vacuum drying oven and dry it at 70°C and -0.1 MPa for 24 hours to obtain white powdery zinc-doped calcium phosphate-silica core-shell nanoparticles.
[0025] A probiotic dietary fiber complex composition for weight management was prepared. The first step involved preparing a functional carrier loaded with probiotics: 10.0 g of the previously prepared mesoporous silica-magnesium-aluminum layered double hydroxide hybrid nanocarrier was accurately weighed and placed in a sterile 500 mL Erlenmeyer flask. 100 mL of sterile phosphate buffer (pH 7.2) was added, and the mixture was vortexed to ensure thorough dispersion. 5.00 g of the compound probiotic lyophilized powder (composed of *Lactobacillus plantarum*, *Lactobacillus reuteri*, and *Bifidobacterium animalis* subsp. *lactobacter* at a dry bacterial powder mass ratio of 2:1:1, with a total viable count of 1.0 × 10⁻⁶) was then weighed. 11(CFU / g) was added to the above suspension. The Erlenmeyer flask was placed in a constant-temperature shaker at 4℃ and shaken at 150 rpm for 4 hours for adsorption. Afterwards, the mixture was transferred to a freeze-drying pan pre-cooled to -40℃ and pre-frozen in an ultra-low temperature freezer at -80℃ for 2 hours, then immediately transferred to a freeze dryer. Under conditions of a cold trap temperature of -50℃ and a vacuum degree below 10 Pa, it was freeze-dried for 24 hours to obtain a dried functional carrier loaded with probiotics. The second step involved preparing the composite hydrophobic gel matrix: 500 mL of deionized water was added to a 2L jacketed heating reaction vessel, and the mixture was stirred and heated to 70℃ using an external circulating water bath. 30.0 g of cellulose nanofibers and 5.00 g of carrageenan powder were slowly added sequentially, maintaining a 70℃ water bath and stirring at 500 rpm until the mixture was completely dissolved and a homogeneous, transparent gel was formed. Separately, 4.00 g of curcumin was dissolved in 40 mL of 75% ethanol solution. After complete dissolution, it was slowly added dropwise to the warm gel solution with stirring. After the addition was complete, the mixture was homogenized at 5000 rpm for 5 minutes using a high-speed homogenizer to obtain an orange-yellow, homogeneous composite hydrophobic gel matrix, which was then kept warm in a 60℃ water bath for later use. The third step, compounding and molding: The probiotic-loaded functional carrier obtained in the first step and 8.00 g of maltodextrin were placed in a V-type mixer and mixed at 30 rpm for 5 minutes to obtain a premix. A 5L container was taken, and the entire warm gel matrix obtained in the second step was transferred into it. While maintaining a basic stirring speed of 500 rpm, the above premix, 14.0 g of zinc-doped calcium phosphate-silica core-shell nanoparticles, 12.0 g of fructooligosaccharides, and 10.0 g of maltodextrin were added sequentially. After all powders are added, switch to a high-shear dispersion emulsifier head and homogenize at 3500 rpm for 8 minutes until a homogeneous, viscous mixture without obvious particles is obtained. Fourth step, freeze drying: Pour the mixture into a flat PTFE mold and gently vibrate the mold to remove large air bubbles. Quickly transfer the mold to an -80°C ultra-low temperature freezer and pre-freeze for 4 hours to allow it to fully solidify. Then, transfer the solidified material block to the freeze dryer shelf and perform primary drying (shelf temperature slowly increased from -40°C to 25°C, taking 40 hours) and desorption drying (maintaining 25°C for 8 hours) under a cold trap temperature of -50°C and a vacuum of 10 Pa, for a total drying time of 48 hours. A fluffy, porous, dried composite solid block is obtained. Fifth step, post-processing: Place the dried solid block in a pulverizer and pulverize at 10000 rpm for 30 seconds to obtain coarse powder. The coarse powder, 15.0g of steviol glycosides, and 4.00g of fumed silica anti-caking agent were added to a three-dimensional motion mixer and mixed at 15 rpm for 20 minutes. Finally, the mixture was passed through an 80-mesh (approximately 180μm) nylon sieve using a vibrating sieve separator, and the sieve-passing material was collected to obtain the final probiotic dietary fiber complex powder product for weight management according to this invention.
[0026] Example 2 The specific implementation method is the same as in Example 1, except that a mesoporous silica-magnesium-aluminum layered double hydroxide hybrid nanocarrier is prepared. 38.4 L of deionized water and 1.6 L of 28% (w / w) concentrated ammonia solution were mixed and heated to 39 °C. 0.80 kg of hexadecyltrimethylammonium bromide was added, and after stirring to dissolve, 1.6 L of tetraethyl orthosilicate was added dropwise over 1.5 hours. The mixture was stirred at 39 °C and 450 rpm for 3.5 hours. The resulting suspension was centrifuged, washed three times with ethanol and three times with water, and the solid was vacuum-dried at 59 °C for 13 hours to obtain the precursor. 400 g of the precursor was dispersed in 8 L of anhydrous toluene, and 40 mL of 3-aminopropyltriethoxysilane was added. The mixture was refluxed at 108 °C for 6 hours under nitrogen protection. After the reaction, the mixture was centrifuged, washed three times with ethanol, and the solid was vacuum-dried at 59 °C for 7 hours to obtain amination-modified particles. Weigh 150g of the amination particles and disperse them in 15L of deoxygenated deionized water. Sonicate in an ice-water bath for 35 minutes to obtain dispersion A. Prepare mixed salt solution B: Dissolve 57.43g of magnesium nitrate hexahydrate and 30.01g of aluminum nitrate nonahydrate in 0.8L of deoxygenated water. Prepare mixed alkali solution C: Dissolve 25.60g of sodium hydroxide and 16.96g of anhydrous sodium carbonate in 0.8L of deoxygenated water. Under nitrogen atmosphere, rapidly mix solutions B and C to form core slurry D, and immediately pour it into dispersion A. Transfer the mixture to a 40℃ water bath, adjust the pH to 9.7 with 1mol / L sodium hydroxide, then transfer to a 64℃ water bath and stir for aging for 20 hours. Centrifuge the product, wash with water until neutral, and vacuum dry the paste at 79℃ for 26 hours. Grind and sieve to obtain the final carrier powder.
[0027] Zinc-doped calcium phosphate-silica core-shell nanoparticles were prepared. 22.71 g of disodium hydrogen phosphate was dissolved in 0.8 L of water to obtain solution A. 56.69 g of calcium nitrate tetrahydrate and 7.14 g of zinc nitrate hexahydrate were dissolved in 0.8 L of water, and the pH was adjusted to 8.9 with 25% ammonia to obtain solution B. Under nitrogen atmosphere at room temperature, solution A was rapidly poured into solution B, and the mixture was stirred for 1 hour. All materials were transferred to a 4 L reactor, and the temperature was increased to 118 °C at 2 °C / min, and the reaction was carried out for 6.5 hours. After natural cooling, the precipitate was collected by centrifugation and washed three times with 1.2 L of water and three times with 0.8 L of ethanol. The solid was vacuum dried at 59 °C for 11 hours to obtain the precursor. 80 g of the precursor was dispersed in a mixture of 1.28 L of ethanol and 0.32 L of water and sonicated for 25 minutes. 16 mL of vinyltrimethoxysilane was added, and the mixture was stirred and refluxed at 59 °C for 4.5 hours. After centrifugation and washing with ethanol, modified nanorods were obtained. 40 g of modified nanorods were dispersed in a mixture of 640 mL ethanol, 160 mL water, and 16 mL concentrated ammonia, and sonicated for 25 minutes. Under stirring at 300 rpm, 40 mL of tetraethyl orthosilicate was added dropwise over 50 minutes, and the reaction was continued at room temperature for 10 hours. After centrifugation, the solid was washed with ethanol and dried under vacuum at 68 °C for 26 hours to obtain the final core-shell nanoparticles.
[0028] A probiotic dietary fiber complex composition for weight management was prepared. 6.00 g of the aforementioned hybrid nanocarrier was weighed and dispersed in 60 mL of sterile pH 7.2 phosphate buffer. 3.00 g of lyophilized probiotic powder (same strain ratio as in Example 1, total viable count 1.0 × 10⁻⁶) was added. 11 The probiotic-loaded carrier was pre-frozen and freeze-dried for 24 hours at 140 rpm in a shaker at 3℃ for 5 hours. 25.0 g of cellulose nanofibers and 4.50 g of carrageenan were added sequentially to 400 mL of 70℃ deionized water and stirred until dissolved. 3.50 g of curcumin was dissolved in 35 mL of 75% ethanol and added dropwise to the gel solution. The mixture was homogenized at 5000 rpm for 4 minutes to obtain a gel matrix, which was then kept warm for later use. The carrier was mixed with 6.00 g of maltodextrin for 5 minutes to obtain a premix. The gel matrix was transferred to a 3L container, and the premix, 13.0 g of core-shell nanoparticles, 11.0 g of fructooligosaccharides, and 8.00 g of maltodextrin were added sequentially while stirring at 500 rpm. A high-shear emulsifier was then used, and the mixture was homogenized at 3200 rpm for 6 minutes to obtain a homogeneous mixture. The mixture was poured into a mold and pre-frozen at -78℃ for 5 hours. Then, it was transferred to a freeze dryer and dried at -50℃ and 10Pa for 50 hours to obtain porous solid blocks. After pulverizing, the blocks were mixed with 12.0g of steviol glycosides and 3.50g of silica in a three-dimensional mixer for 20 minutes and then passed through an 80-mesh sieve to obtain the final product powder.
[0029] Example 3 The specific implementation method is the same as in Example 1, except that a mesoporous silica-magnesium-aluminum layered double hydroxide hybrid nanocarrier is prepared. 57.6 L of deionized water and 2.4 L of 28% (w / w) concentrated ammonia solution were mixed and heated to 41 °C. 1.20 kg of hexadecyltrimethylammonium bromide was added, and after stirring to dissolve, 2.2 L of tetraethyl orthosilicate was added dropwise over 2 hours. The mixture was stirred at 41 °C and 550 rpm for 2.5 hours. The resulting suspension was centrifuged, washed three times with ethanol and three times with water, and the solid was vacuum-dried at 61 °C for 11 hours to obtain the precursor. 600 g of the precursor was dispersed in 12 L of anhydrous toluene, and 60 mL of 3-aminopropyltriethoxysilane was added. The mixture was refluxed at 112 °C for 10 hours under nitrogen protection. After the reaction, the mixture was centrifuged, washed three times with ethanol, and the solid was vacuum-dried at 61 °C for 5 hours to obtain amination-modified particles. Weigh 250g of the amination particles and disperse them in 25L of deoxygenated deionized water. Sonicate in an ice-water bath for 25 minutes to obtain dispersion A. Prepare mixed salt solution B: Dissolve 95.72g of magnesium nitrate hexahydrate and 50.02g of aluminum nitrate nonahydrate in 1.2L of deoxygenated water. Prepare mixed alkali solution C: Dissolve 38.40g of sodium hydroxide and 25.44g of anhydrous sodium carbonate in 1.2L of deoxygenated water. Under nitrogen atmosphere, rapidly mix solutions B and C to form core slurry D, and immediately pour it into dispersion A. Transfer the mixture to a 40℃ water bath, adjust the pH to 10.0 with 1mol / L sodium hydroxide, then transfer to a 66℃ water bath and stir for aging for 18 hours. Centrifuge the product, wash with water until neutral, and vacuum dry the paste at 81℃ for 22 hours. Grind and sieve to obtain the final carrier powder.
[0030] Zinc-doped calcium phosphate-silica core-shell nanoparticles were prepared. 34.06 g of disodium hydrogen phosphate was dissolved in 1.2 L of water to obtain solution A. 85.03 g of calcium nitrate tetrahydrate and 10.70 g of zinc nitrate hexahydrate were dissolved in 1.2 L of water, and the pH was adjusted to 9.1 with 25% ammonia to obtain solution B. Under nitrogen atmosphere at room temperature, solution A was rapidly poured into solution B, and the mixture was stirred for 1 hour. All materials were transferred to a 6 L reactor, and the temperature was increased to 122 °C at 2 °C / min, and the reaction was carried out for 7.5 hours. After natural cooling, the precipitate was collected by centrifugation and washed three times with 1.8 L of water and three times with 1.2 L of ethanol. The solid was vacuum dried at 61 °C for 9 hours to obtain the precursor. 120 g of the precursor was dispersed in a mixture of 1.92 L of ethanol and 0.48 L of water and sonicated for 35 minutes. 24 mL of vinyltrimethoxysilane was added, and the mixture was stirred and refluxed at 61 °C for 5.5 hours. After centrifugation and washing with ethanol, modified nanorods were obtained. 60 g of modified nanorods were dispersed in a mixture of 960 mL ethanol, 240 mL water, and 24 mL concentrated ammonia, and sonicated for 35 minutes. Under stirring at 300 rpm, 60 mL of tetraethyl orthosilicate was added dropwise over 70 minutes, and the reaction was continued at room temperature for 14 hours. After centrifugation, the solid was washed with ethanol and dried under vacuum at 72 °C for 22 hours to obtain the final core-shell nanoparticles.
[0031] A probiotic dietary fiber complex composition for weight management was prepared. 14.0 g of the aforementioned hybrid nanocarrier was weighed and dispersed in 140 mL of sterile pH 7.2 phosphate buffer. 7.00 g of lyophilized probiotic powder (same strain ratio as in Example 1, total viable count 1.0 × 10⁻⁶) was added. 11 The probiotic-loaded carrier was pre-frozen and freeze-dried for 24 hours at 160 rpm in a shaker at 5°C for 3 hours. 35.0 g of cellulose nanofibers and 5.50 g of carrageenan were added sequentially to 600 mL of 70°C deionized water and stirred until dissolved. 4.50 g of curcumin was dissolved in 45 mL of 75% ethanol and added dropwise to the gel solution. The mixture was homogenized at 5000 rpm for 6 minutes to obtain a gel matrix, which was then kept warm for later use. The carrier was mixed with 9.00 g of maltodextrin for 5 minutes to obtain a premix. The gel matrix was transferred to a 6L container, and the premix, 15.0 g of core-shell nanoparticles, 14.0 g of fructooligosaccharides, and 14.0 g of maltodextrin were added sequentially while stirring at 500 rpm. A high-shear emulsifier was then used, and the mixture was homogenized at 3800 rpm for 9 minutes to obtain a homogeneous mixture. The mixture was poured into a mold and pre-frozen at -82℃ for 3 hours. Then, it was transferred to a freeze dryer and dried at -50℃ and 10Pa for 46 hours to obtain porous solid blocks. After pulverizing, the blocks were mixed with 18.0g of steviol glycosides and 4.50g of silica in a three-dimensional mixer for 20 minutes and then passed through an 80-mesh sieve to obtain the final product powder.
[0032] Comparative Example 1 The specific implementation method is the same as in Example 1, except that this comparative example does not include the addition of mesoporous silica-magnesium-aluminum layered double hydroxide hybrid nanocarrier and its loading step. When preparing the composite composition, 5.00g of the composite probiotic freeze-dried powder (same strain ratio and viable count as in Example 1) and 8.00g of maltodextrin were directly weighed and mixed in a V-type mixer at 30 rpm for 5 minutes as a substitute premix. The remaining components and amounts are: 14.0g of zinc-doped calcium phosphate-silica core-shell nanoparticles, 30.0g of cellulose nanofibers, 5.00g of carrageenan, 4.00g of curcumin (dissolved in 40mL of 75% ethanol), 12.0g of fructooligosaccharides, 10.0g of subsequently added maltodextrin, 15.0g of steviol glycosides, and 4.00g of silica. The preparation steps and process parameters were exactly the same as in Example 1: First, a carrageenan-cellulose nanofiber gel matrix without curcumin was prepared, cooled to 60°C, and then a curcumin ethanol solution was added and homogenized; this gel matrix was transferred to a liquid tank, and the above premix and all other powders were added sequentially under stirring; it was homogenized at 3500 rpm for 8 minutes; it was poured into a mold, pre-frozen at -80°C for 4 hours, and then freeze-dried for 48 hours; the obtained porous solid block was crushed, mixed with steviol glycosides and silica for 20 minutes, and passed through an 80-mesh sieve to obtain the product of Comparative Example 1.
[0033] Comparative Example 2 The specific implementation method is the same as in Example 1, except that zinc-doped calcium phosphate-silica core-shell nanoparticles are not added in this comparative example. When preparing the composite composition, except for the omission of this component, the amounts of other components and the preparation steps are exactly the same as in Example 1: 10.0g of mesoporous silica-magnesium aluminum layered double hydroxide hybrid nanocarrier and its loaded 5.00g of probiotic lyophilized powder (adsorbed and lyophilized), 30.0g of cellulose nanofibers, 5.00g of carrageenan, 4.00g of curcumin (dissolved in 40mL 75% ethanol), 12.0g of fructooligosaccharides, 18.0g of maltodextrin (added in two portions), 15.0g of steviol glycosides, and 4.00g of silica. All preparation process parameters, including loading and adsorption conditions, gel preparation temperature and homogenization parameters, composite homogenization speed and time, pre-freezing and freeze-drying conditions, and post-treatment mixing and sieving parameters, are strictly consistent with those in Example 1.
[0034] Comparative Example 3 The specific implementation method is the same as in Example 1, except that this comparative example does not add mesoporous silica-magnesium aluminum layered double hydroxide hybrid nanocarriers and their loading steps, nor does it add zinc-doped calcium phosphate-silica core-shell nanoparticles. When preparing the composite composition, 5.00g of the composite probiotic freeze-dried powder (same strain ratio and viable count as in Example 1) was directly weighed and mixed with 8.00g of maltodextrin as a premix. The system contains only: 30.0g of cellulose nanofibers, 5.00g of carrageenan, 4.00g of curcumin (dissolved in 40mL of 75% ethanol), 12.0g of fructooligosaccharides, 10.0g of subsequently added maltodextrin, 15.0g of steviol glycosides, and 4.00g of silica. The preparation process was exactly the same as in Example 1: a gel matrix was prepared and homogenized with all the powders (i.e., the above premix, fructooligosaccharide, and 10.0 g maltodextrin) at 3500 rpm for 8 minutes; all parameters of the subsequent pre-freezing, freeze-drying, pulverizing, final mixing and sieving steps were consistent with those of Example 1, and the product of Comparative Example 3 was obtained.
[0035] Performance testing The probiotic dietary fiber composite compositions for weight management prepared in Examples 1-3 and Comparative Examples 1-3 were subjected to performance testing according to the following method, which included the following steps: All performance tests were conducted in a sterile operating room, with the ambient temperature controlled at 25℃±1℃ and the relative humidity controlled at 50%±5%. The test samples were the final composite powders prepared in Examples 1, 2, 3, Comparative Examples 1, 2, and 3. All samples were equilibrated in a desiccator for 24 hours before testing.
[0036] Test 1: Probiotic Gastrointestinal Tolerance and Targeted Survival Rate Test The study simulated the human upper digestive tract environment in stages. The first stage simulated gastric juice tolerance: 1.000g of each test sample powder was accurately weighed using an analytical balance and placed in a 250mL sterile Erlenmeyer flask. 100.0mL of sterile simulated gastric juice preheated to 37℃ was added. This simulated gastric juice was prepared as follows: 3.00g of pepsin (enzyme activity 1:10000) and 2.00g of sodium chloride were weighed, dissolved in 1L of deionized water, and the pH was adjusted to 2.00±0.05 with 1.0mol / L hydrochloric acid solution. The solution was then filtered through a 0.22μm sterile filter membrane for sterilization. The Erlenmeyer flask was placed in a 37℃ constant temperature water bath shaker and horizontally shaken at 100rpm. At treatment times of 0min, 60min, and 120min, 1.0mL of the mixture was accurately pipetted using a sterile pipette. Immediately perform a 10-fold serial dilution with pre-cooled sterile phosphate buffer (0.1 mol / L, pH 7.2), selecting 2-3 suitable dilutions. Spread 0.1 mL of each dilution onto an MRS agar plate, with three replicates per dilution. Incubate the plates in a 37°C anaerobic incubator for 48 ± 2 hours, and count the colony-forming units on the plates. The survival rate is calculated as: (number of viable bacteria after treatment / initial number of viable bacteria) × 100%. The second stage simulates intestinal fluid tolerance: After 120 min of gastric fluid treatment, the entire mixture is slowly neutralized to pH 6.80 ± 0.10 with sterile 1.0 mol / L sodium bicarbonate solution. Then, 100.0 mL of sterile simulated intestinal fluid preheated to 37°C was added. This intestinal fluid was prepared as follows: 10.00 g of trypsin and 3.00 g of ox bile salt were weighed and dissolved in 1 L of phosphate buffer (0.1 mol / L, pH 6.8), and then filtered through a 0.22 μm sterile filter for sterilization. The mixture was then shaken at 37°C and 100 rpm. Samples were taken again at 0 min, 60 min, and 120 min of intestinal fluid treatment, and diluted, spread, cultured, and counted using the same method described above. The overall survival rate after undergoing complete simulated gastrointestinal digestion was calculated.
[0037] Test 2: In vitro fat adsorption capacity test Prepare a 50.0 mmol / L sodium oleate stock solution: Weigh 16.12 g of sodium oleate, dissolve it in 1 L of deionized water preheated to 60 °C, stir until completely clear, and cool to room temperature. For testing, accurately weigh 0.500 g of each test sample powder using an analytical balance and place it in a 150 mL stoppered Erlenmeyer flask. Accurately add 50.0 mL of the above sodium oleate stock solution using a pipette. After sealing the Erlenmeyer flask, place it in a 37 °C constant temperature shaking incubator and shake at 150 rpm for 3.0 hours. Immediately after the time is up, take 10.0 mL of the supernatant suspension from each Erlenmeyer flask, filter it through a 0.45 μm aqueous microporous membrane, and collect the clear filtrate. Determine the concentration of residual sodium oleate in the filtrate by titration: Accurately transfer 10.00 mL of the filtrate to a 250 mL Erlenmeyer flask and add 3 drops of 1% phenolphthalein indicator ethanol solution. Titrate with 0.0100 mol / L standard hydrochloric acid solution until the pink color of the solution just fades and remains unchanged for 15 seconds, recording the volume of hydrochloric acid consumed (V, mL). Simultaneously perform a blank control titration (using sodium oleate stock solution without the sample). The formula for calculating the amount of fat adsorbed per unit mass of sample (Q, mg / g) is: Q = [C0 × (V0 - V) × M] / (m × 10⁻¹⁰) -3 Where C0 is the standard hydrochloric acid concentration (0.0100 mol / L), V0 is the volume of hydrochloric acid consumed in the blank titration (mL), V is the volume of hydrochloric acid consumed in the sample titration (mL), M is the molar mass of sodium oleate (304.45 g / mol), and m is the sample mass (0.500 g). Each sample was measured in triplicate.
[0038] Test 3: Gel matrix swelling and water retention test Swelling test: Accurately weigh 1.000 g of each test sample powder and slowly pour it into a 500 mL graduated glass cylinder containing 200.0 mL of preheated (37°C) simulated gastric fluid (pH 2.0, enzyme-free). Disperse the powder evenly on the liquid surface during pouring. Let stand, and read the total volume occupied by the sample in the solution (including the interface between the gel phase and the supernatant) at 5 min, 30 min, 60 min, and 120 min. The swelling volume is expressed in mL / g, i.e., the total volume divided by the sample mass. Water-holding capacity test: Accurately weigh 0.500 g of sample into a 50 mL centrifuge tube, add 5.00 g of deionized water (25°C), stir with a glass rod for 2 min to mix thoroughly, and let stand for 30 min to swell. Place the mixture, along with the centrifuge tube, into a centrifuge and centrifuge at 4000 rpm for 20 min. Carefully pour off the upper layer of free water, blot dry any remaining water droplets on the tube wall with filter paper, and weigh the total mass of the centrifuge tube and the wet gel. The water-holding capacity is calculated using the formula: [(Wet gel mass - Centrifuge tube mass - Dry sample mass) / Dry sample mass] × 100%. Perform three parallel measurements for each sample.
[0039] Test 4: Storage Stability Test Each sample powder was packaged into aluminum-plastic composite film bags with the same water vapor permeability, 5.00g per bag, and sealed by heat pressing. Four different accelerated storage conditions were set up: Condition A was refrigeration at 4℃ (humidity uncontrolled); Condition B was a constant temperature incubator at 25℃ (relative humidity 60%); Condition C was a constant temperature incubator at 37℃ (relative humidity 60%); and Condition D was a constant temperature and humidity incubator at 37℃ (relative humidity 75%±3%). Under each storage condition, three bags of samples were randomly taken on days 0, 30, 60, and 90. Moisture content was determined: using a rapid moisture analyzer, 1.00g of sample was measured at 105℃ until constant weight. Viable cell count was determined: following the method in Test 1, the sample was reconstituted in sterile buffer, diluted, spread, and anaerobic incubated for counting. The viable cell survival rate at different time points was calculated using the formula: (number of viable cells after storage / number of viable cells at initial storage) × 100%.
[0040] Test 5: Flowability and reconstitution properties of composite powder Flowability Test: The angle of repose was determined using the fixed funnel method. The funnel was fixed above a horizontally placed graph paper, with the bottom opening 50 mm from the plane of the graph paper. Excess sample powder was slowly poured into the funnel, allowing it to flow freely from the bottom opening and accumulate on the graph paper to form a cone. After the powder had completely flowed out, the radius (R, mm) and height (H, mm) of the cone's base were measured using a ruler. The formula for calculating the angle of repose (θ) is: θ = arctan(H / R). Bulk Density Determination: Sample powder was slowly poured into a 100 mL graduated cylinder of known mass (m0, g) until it slightly exceeded the 100 mL mark. Excess powder was gently scraped off along the rim of the graduated cylinder with a scraper, and the total mass of the graduated cylinder and powder (m1, g) was weighed. The formula for calculating the loose bulk density (ρb, g / mL) is: ρb = (m1 - m0) / 100. The graduated cylinder is dropped vertically from a height of 10 mm onto a rubber pad, vibrating once per second for a total of 100 vibrations. The volume of the compacted powder (Vt, mL) is recorded, and the tapped density (ρt, g / mL) is calculated. The compressibility (C, %) is calculated using the formula: C = [(ρt - ρb) / ρt] × 100%. For the reconstitution test: 200 mL of preheated purified water (40℃ ± 1℃) is added to a 250 mL transparent glass beaker. 5.00 g of sample powder is weighed and poured into the water at once. The magnetic stirrer is immediately started and stirred at a fixed speed (200 rpm) for 30 seconds. The time required from the start of stirring until no obvious particles or clumps are visible to the naked eye is recorded as the "complete dissolution time". After stopping stirring, the solution is allowed to stand for 2 minutes. The state of the solution (whether there is layering, clumping, or floating powder) and the height of the sediment at the bottom of the beaker (mm) are observed and recorded.
[0041] Test results: Table 1: Test results of each embodiment and comparative example ; As can be seen from Table 1, the complete technical solutions provided in Examples 1-3, through the systematic contrast of Examples 1-3, clearly and powerfully demonstrate that they have successfully solved the two major technical problems of live bacteria in existing probiotic products being easily destroyed by gastric acid and the simple mechanism of ordinary dietary fiber.
[0042] First, regarding the issues of probiotic destruction by gastric acid and targeted delivery, the data revealed a decisive difference: Examples 1-3 and Comparative Example 2, containing mesoporous silica-magnesium-aluminum layered double hydroxide hybrid nanocarriers, maintained a probiotic survival rate of over 83% after 120 minutes of rigorous simulated gastric fluid treatment. In contrast, Comparative Examples 1 and 3, lacking this crucial carrier, saw their survival rates plummet to only about 12%. This directly confirms that the hybrid nanocarrier effectively isolates gastric acid and digestive enzymes, playing a key role in ensuring the safe arrival of probiotics in a highly active state in the intestines. Upon entering the simulated intestinal fluid stage, this gap widened further; Examples 1-3 maintained a final survival rate of over 72%, while Comparative Examples 1 and 3 showed a live bacteria survival rate of less than 3%.
[0043] Meanwhile, in addressing the issue of a single weight management mechanism and a lack of synergistic effects, Examples 1-3 and Comparative Example 1, containing zinc-doped calcium phosphate-silica core-shell nanoparticles, exhibited strong in vitro fat adsorption capacity, reaching over 65 mg / g. Conversely, Comparative Examples 2 and 3, without these nanoparticles, showed a sharp decrease in adsorption capacity to only around 12 mg / g. This indicates that the core-shell nanoparticles are the core component that endows the product with the crucial function of physically intercepting dietary fat, rather than the gel matrix or other ingredients. More importantly, Examples 1-3, with the best overall performance, successfully combined the two core effects of high gastric acid tolerance (survival rate >83%) and high fat adsorption (adsorption amount >65 mg / g), which none of the comparative examples could achieve: Comparative Example 1 had high adsorption capacity but the probiotics were almost inactivated; Comparative Example 2 protected the probiotics but had no fat adsorption function; and Comparative Example 3 lost both. This fully demonstrates that the invention, through the ingenious combination of two innovative inorganic modified compounds and dietary fiber matrix, does not simply add up the functions, but produces a synergistic effect of "1+1>2". Ultimately, it constructs a three-dimensional, multi-target weight management system that can intelligently deliver and protect probiotics, actively intervene in lipid absorption, and provide a feeling of fullness through the gel matrix, thus completely solving the technical problem it addresses.
[0044] The embodiments described above are merely examples of several implementations of the present invention, and while the descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the present invention. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of the present invention, and these modifications and improvements all fall within the scope of protection of the present invention.
Claims
1. A process for the preparation of a probiotic dietary fiber composite composition for weight management, characterized by the steps of Comprise: S1, 3-15 parts of mesoporous silica-magnesium aluminum layered double hydroxide hybrid nanocarriers were dispersed in sterile phosphate buffer, then mixed with composite probiotic freeze-dried powder, adsorbed under oscillation at 3-5℃, freeze-dried to obtain functional carriers loaded with probiotics; 20-40 parts of cellulose nanofiber was mixed with 4-6 parts of carrageenan in 68-72℃ deionized water, and 3-5 parts of curcumin ethanol solution was added, and homogenized to obtain a composite hydrophobic gel matrix; S2, the functional carriers loaded with probiotics obtained in step S1 were mixed with 5-10 parts of malt dextrin to obtain a premix; then the premix, 12-16 parts of zinc-doped calcium phosphate-silica core-shell nanoparticles, 10-15 parts of oligofructose and 5-15 parts of malt dextrin were added to the composite hydrophobic gel matrix obtained in step S1, and homogenized at 3000-4000 rpm to obtain a mixture; the mixture was injected into a mold and pre-frozen to form a shape, and then freeze-dried to obtain a dry composite powder; the dry composite powder was mixed with 10-20 parts of steviol glycoside and 3-5 parts of silicon dioxide, and sieved.
2. The process for the preparation of probiotic dietary fiber composite composition for weight management as claimed in claim 1, wherein, In step S1, the composite probiotic freeze-dried powder is prepared by mixing Lactobacillus plantarum, Lactobacillus reuteri and Bifidobacterium animalis lactis.
3. The method for preparing the probiotic dietary fiber composite composition for weight management according to claim 1, characterized by, In step S2, the homogenization time at 3000-4000 rpm is 5-10 min.
4. The process for the preparation of probiotic dietary fiber composite composition for weight management as claimed in claim 1, wherein, The preparation method of the mesoporous silica-magnesium aluminum layered double hydroxide hybrid nanocarriers comprises: A1, cetyltrimethylammonium bromide was dissolved in an aqueous ammonia solution; tetraethyl orthosilicate was added, and continuous stirring reaction was carried out at 38-42℃ to obtain a suspension; the precipitate was collected by centrifugation and washed with ethanol and deionized water alternately, and vacuum dried at 58-62℃ to obtain mesoporous silica nanoparticle precursors; the mesoporous silica nanoparticle precursors were dispersed in anhydrous toluene, 3-aminopropyltriethoxysilane was added, and reaction was carried out under reflux conditions, and the product was washed by centrifugation to obtain amin-modified mesoporous silica nanoparticles; the amin-modified mesoporous silica nanoparticles were dispersed in deionized water deoxygenated by nitrogen, and ultrasonic treatment was carried out to obtain a dispersion liquid; A2, under nitrogen protection and stirring, a mixed salt solution containing magnesium nitrate and aluminum nitrate was mixed with a mixed alkali solution containing sodium hydroxide and sodium carbonate to obtain a core slurry, and the core slurry was added to the dispersion liquid and crystallized under stirring; the pH value was adjusted to 9.5-10.0, and aging was carried out at 64-66℃; after the reaction was completed, the product was collected by centrifugation, washed with deionized water until neutral, and finally vacuum dried at 78-82℃ and ground.
5. The process for the preparation of probiotic dietary fiber composite composition for weight management as claimed in claim 4, wherein, In step A1, the continuous stirring reaction time at 38-42℃ is 2-4h.
6. The process for the preparation of probiotic dietary fiber composite composition for weight management as claimed in claim 4, wherein, In step A2, the aging time at 64-66℃ is 18-20h.
7. The process for the preparation of probiotic dietary fiber composite composition for weight management as claimed in claim 1, wherein, The preparation method of the zinc-doped calcium phosphate-silica core-shell nanoparticles comprises: B1, at room temperature and under nitrogen protection, dissolve disodium hydrogen phosphate in deionized water to obtain solution A; dissolve the mixed salt containing calcium nitrate and zinc nitrate in deionized water, adjust the pH to 8.8-9.2 to obtain solution B; under stirring, pour solution A into solution B to obtain a colloidal precipitate, continue to stir the reaction; then transfer the reaction system to a high-pressure reaction kettle, hydrothermal reaction at 115-125℃; after natural cooling, centrifugal collect the precipitate, wash with deionized water and ethanol, dry at 58-62℃ to obtain zinc-doped hydroxyapatite nanorod precursor; B2, disperse the zinc-doped hydroxyapatite nanorod precursor in a mixed solution of ethanol and water, add vinyltrimethoxysilane, ultrasonic treatment, stirring, centrifugal washing to obtain surface hydrophobic modified nanorods; disperse the surface hydrophobic modified nanorods in a mixed solution composed of ethanol, deionized water and concentrated ammonia water, ultrasonic dispersion to obtain a dispersion liquid; under stirring, add tetraethyl orthosilicate dropwise into the dispersion liquid, after the dropwise addition is completed, continue to react at room temperature; after the reaction is completed, collect the precipitate by centrifugation, wash the precipitate with ethanol, vacuum drying at 60-80℃.
8. The process for the preparation of probiotic dietary fiber composite composition for weight management as claimed in claim 7, wherein, In step B1, the hydrothermal reaction at 115-125℃ is performed for 6-8h.
9. The process for the preparation of probiotic dietary fiber composite composition for weight management as claimed in claim 7, wherein, In step B2, the vacuum drying at 60-80℃ is performed for 2-3h.
10. A probiotic dietary fiber composite composition for weight management, characterized by, The probiotic dietary fiber composite composition for weight management is prepared according to the preparation method of the probiotic dietary fiber composite composition for weight management of any one of claims 1-9.