A fiber-enriched aerated confectionery and a method for making the same
Patent Information
- Application Number
- CN202611255097.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-08-18
- Publication Date
- 2026-09-25
AI Technical Summary
这种微观结构的破坏会导致最终产品在储存过程中出现密度增大、容积塌陷、表面结晶以及质构硬化等严重的坍塌问题,大幅降低充气糖果特有的绵软弹性与感官品质
(1)本发明利用改性蒲公英花粉微球作为天然微型载体,通过氧化活化提高其亲水性和负载能力,并结合内部凝胶网络实现矿物质补给源和再矿化活性因子的稳定封装,有效改善功能组分在糖果体系中的分散稳定性,降低活性组分在加工及储存过程中的损失。
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Figure CN122804862A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the food industry, and more particularly to a fiber-rich aerated candy and its preparation method. Background Technology
[0002] Aerated candies are a type of food product in which gas is introduced into a syrup matrix through mechanical whipping or foaming, resulting in a textured food with a rich microporous structure and a unique soft, elastic texture. With the increasing health awareness of modern consumers and the growing demand for sugar-free and low-sugar foods, using non-fermentable sugar substitutes like sugar alcohols instead of traditional sucrose and glucose syrup in the preparation of aerated candies can not only significantly reduce the calories and glycemic index of the candies, but also effectively block the pathway of oral microorganisms using fermentable sugars to produce acid, thus helping to maintain a low-acid environment in the mouth. At the same time, dietary fiber, as an important nutrient, can be incorporated into the candy system to increase the dietary fiber content of the product, meeting the dual pursuit of a balanced diet and healthy taste.
[0003] However, significant technical bottlenecks remain in the traditional production and technological development of aerated candies, particularly in the efficient integration of sugar substitutes (sugar alcohols) and dietary fiber while maintaining system stability. Traditional aerated candies primarily rely on water-soluble colloids such as gelatin and pectin, as well as the viscosity of the syrup itself, to maintain the shape of the foaming bubbles. When large or rigid insoluble dietary fiber particles are directly introduced into the syrup matrix, these exogenous particles easily disrupt the force balance at the gas-liquid interface in the aerated system. During the aeration, whipping, and subsequent cooling and solidification stages, rigid fiber particles can easily penetrate the bubble walls, inducing bubble merging, rupture, and droplet discharge from the continuous phase. This disruption of the microstructure leads to severe collapse problems in the final product during storage, such as increased density, volume collapse, surface crystallization, and textural hardening, significantly reducing the unique softness, elasticity, and sensory quality of aerated candies.
[0004] Furthermore, because aerated candies require high-temperature cooking before whipping and are in a highly fluid, hot syrup state after whipping, the directly added insoluble dietary fiber particles and sugar substitute crystals are easily affected by gravity sedimentation in the hot fluid. This not only causes stratification of the syrup during mold pouring or extrusion molding but also results in uneven dispersion of fiber and sugar substitute components within the finished product, severely affecting the consistency of product quality between batches.
[0005] On the other hand, the sugar substitutes and auxiliary ingredients directly dispersed in the syrup matrix dissolve rapidly during the chewing process due to the washing action of saliva and are quickly swallowed. This results in the sugar substitutes having a very short residence time in the oral cavity, making it impossible to form a continuous and stable environmental regulation effect in the oral cavity, thus limiting the full realization of their functional properties.
[0006] Therefore, how to solve the problems of bubble instability and particle sedimentation caused by the introduction of dietary fiber without destroying the porous and soft texture of aerated candies, while optimizing the dissolution and release behavior of active components in the system during chewing, is a technical challenge that urgently needs to be overcome in the field of aerated candy research and development. Summary of the Invention
[0007] The first object of the present invention is to provide an aerated candy, comprising, by weight parts: Oxidative activation of dandelion pollen, 1.0-4.0; Microfiber dietary fiber, 1.5-3.5; Water-soluble colloid, 2.0-6.0; Non-fermentable sugar substitutes, sugar alcohols, 45.0-65.0; Mineral replenishment source, 0.2-1.5; Remineralization activity factor, 0.1-1.0; Water, 8.0-15.0; The oxidized activated dandelion pollen is formed by oxidizing and activating defatted and deproteinized dandelion pollen. It is loaded with at least part of the mineral supply source and / or remineralization active factor. The residual polysaccharides and / or exogenous gelled polysaccharides in the oxidized activated dandelion pollen form an internal gel network with the mineral supply source and / or remineralization active factor. The remineralization active factor is a bioactive inorganic material or a calcium-phosphorus composite active component that provides mineralization active sites, promotes calcium and phosphorus ion deposition, or regulates the calcium and phosphorus mineralization process. The microfibrillated dietary fiber is obtained by physical microfibrillation of insoluble dietary fiber, and its microfibril structure has a length of 60-250μm and an aspect ratio of 35-120. The apparent density of the aerated candy is 0.5-0.8 g / cm³. 3 .
[0008] Preferably, the oxidized and activated dandelion pollen is loaded with a mineral supply source and a remineralization active factor to form modified dandelion pollen microspheres with an internal gel network structure. The modified dandelion pollen microspheres were prepared by the following steps: (1) Oxidative activation: Defatted and deproteinized dandelion pollen was dispersed in a food-grade alkaline peroxide system for oxidative activation treatment, washed and dried to obtain oxidized activated dandelion pollen; (2) Pressure differential loading: The oxidized and activated dandelion pollen is mixed with a composite aqueous solution containing non-fermentable sugar alcohol, mineral replenishment source and remineralization active factor, and the mixture is alternately circulated between vacuum conditions and normal pressure to allow the composite aqueous solution to penetrate into the hollow cavity inside the dandelion pollen. (3) In-situ gel network trapping: Introduce an inducer to induce the formation of a gel network of the water-soluble colloid into the system obtained in step (2) to form a polysaccharide gel network inside the dandelion pollen; (4) Post-processing: The material obtained in step (3) is subjected to solid-liquid separation, washing to remove free components that are not bound to the cavity, and drying to obtain the modified dandelion pollen microspheres; The specific surface area of the oxidized and activated dandelion pollen is 15-45 m². 2 / g, and the static contact angle with water is ≤45°.
[0009] In step (1), the mass fraction of peroxide in the alkaline peroxide system is 1%-5%, the temperature of the oxidation activation treatment is 30-50℃, and the treatment time is 1-3h; In step (2), the vacuum level is -0.08 MPa to -0.095 MPa. In step (3), the food inducer is a calcium salt that provides gel-inducing ions.
[0010] Preferably, the microfibrillated dietary fiber is prepared by the following steps: S1 Pretreatment: The insoluble dietary fiber raw material is degreased and impurities are removed, and then dispersed in water to form a dietary fiber suspension; S2 Pre-dispersion: The dietary fiber suspension obtained in step S1 is subjected to high shear dispersion to initially dissociate the fiber bundles; S3 High-pressure homogenization and defibrillation: The system obtained in step S2 is subjected to high-pressure homogenization to cause the dietary fiber to dissociate, peel off and refine in size, so as to obtain a microfibrillated dietary fiber suspension. S4 Post-processing: The suspension obtained in step S3 is dried to obtain the microfibrillated dietary fiber.
[0011] In step S3, the material temperature during the homogenization process is controlled below 45 ℃.
[0012] Preferably, the non-fermentable sugar alcohol has a water solubility of ≥30% (W / W) at 20 °C; and the non-fermentable sugar alcohol is a sugar alcohol compound with a polyhydroxy alcohol structure and without free reducing aldehyde or ketone groups.
[0013] Preferably, the mineral source is calcium salt and / or phosphate.
[0014] Preferably, the water-soluble colloid is one or more of hydrophilic natural polysaccharide colloids and hydrophilic proteins.
[0015] A second objective of this invention is to provide a method for preparing the above-mentioned aerated candy, comprising the following steps: a. Matrix compounding: Microfibrillated dietary fiber, water-soluble colloids and water are mixed and sheared and dispersed to form a continuous phase hydrocolloid system; b. Boiling the syrup: Mix non-fermentable sugar substitutes with water and heat to boil. After cooling, mix with the continuous phase aqueous colloidal system obtained in step a to prepare the aerated precursor syrup. c. Microspheres and active factors are combined: Modified dandelion pollen microspheres, mineral replenishment sources and remineralization active factors are added to the aerated precursor syrup obtained in step b, and dispersed to obtain a dispersion containing microspheres. d. Aeration and solidification: The microsphere-containing dispersion obtained in step c is passed through a gas for high-pressure aeration. The aerated material is then injected into a mold, cooled, and solidified to obtain the aerated candy.
[0016] 10. The method for preparing aerated candy according to claim 9, characterized in that: In step b, the heating and cooking process is carried out until the solid content is ≥85% (w / w); In step c, the mixing temperature when adding modified dandelion pollen microspheres is 50-70℃.
[0017] This invention solves the problems of easy aggregation of active components, insufficient processing stability, and difficulty in controlling release behavior in traditional functional aerated candies by constructing a composite structure of "natural microsphere carrier sustained-release system and fiber-reinforced aerated continuous phase".
[0018] Specifically, this invention uses defatted and deproteinized dandelion pollen as a natural microsphere carrier. Oxidative activation treatment improves its surface hydrophilicity and interfacial binding capacity, enabling the hollow cavities and porous structure within the dandelion pollen to form micro-storage spaces suitable for loading functional components. After oxidation activation, the surface polarity of the dandelion pollen is enhanced, facilitating the entry of water-soluble components into its internal cavities and improving the binding stability between mineral replenishment components and remineralization active factors and the carrier.
[0019] During the loading process, pressure difference drives the entry of non-fermentable sugar alcohols, mineral supplements, and remineralization active factors into the internal space of dandelion pollen, transforming the functional components from a traditional free and dispersed state to a microcavity-confined storage state. Subsequently, a gel network is formed using water-soluble colloids to spatially fix the active components inside the microcavities, forming a rigid-flexible composite microsphere structure of "external stable sporophytin structure - internal gel diffusion network". The high mechanical stability of dandelion pollen reduces the loss of active components during processing, while the internal gel network slows down the diffusion process of components after water ingress, resulting in a smoother release of sugars, mineral supplements, and remineralization active factors loaded inside the microspheres.
[0020] Compared to directly adding mineral components and remineralized active agents to the candy matrix, this invention utilizes the spatial confinement effect provided by modified dandelion pollen microspheres to maintain high dispersion stability of active components in the continuous phase of aerated candy, reducing direct contact and aggregation between inorganic active particles and improving the uniformity of distribution of active components in the candy system. Simultaneously, the microsphere structure acts as a protective barrier for active components, reducing the adverse effects of external environments on functional components during cooking, aeration, shearing, and storage.
[0021] Furthermore, the microfibrillated dietary fiber undergoes physical microfibrillation treatment, causing the original fiber bundles to disintegrate and refine in size, forming a microfibril structure with a high aspect ratio. During the aeration process, the microfibrillated dietary fiber is dispersed in the continuous phase of the candy, constructing a three-dimensional reinforcing network through the entanglement between fibers, thereby improving the viscoelasticity and structural support capacity of the continuous phase system. On the one hand, this fiber network can enhance the stability of the bubble walls, reduce liquid drainage and bubble rupture in the aeration system, and enable the candy to form a uniform and stable porous structure; on the other hand, the fiber network increases the yield stress of the continuous phase, allowing the modified dandelion pollen microspheres to be uniformly suspended in the candy matrix, reducing sedimentation and local enrichment during processing and cooling.
[0022] During consumption, the aerated structure gradually breaks down under chewing, allowing moisture to gradually penetrate the modified dandelion pollen microspheres. Due to the diffusion-blocking effect of the internal gel network, the sugar substitutes, sugar alcohols, mineral replenishment sources, and remineralization active factors in the microspheres are gradually released during the water penetration process, achieving a slow-release supply of active components. Among them, the mineral replenishment source provides a source of mineral elements such as calcium and phosphorus, while the remineralization active factors enhance the synergy in the utilization of mineral elements by providing mineralization active sites, promoting calcium and phosphorus ion deposition, or maintaining the calcium and phosphorus mineralization microenvironment.
[0023] Therefore, this invention does not simply involve physically mixing dietary fiber, minerals, and active materials. Instead, it achieves spatial encapsulation of functional components through modified dandelion pollen microspheres and enhances the structure of the aerated candy system through microfibrillated dietary fiber, ultimately forming a composite aerated candy system with a stable porous structure, uniform distribution of active components, and sustained-release characteristics.
[0024] The beneficial effects of this invention are as follows: (1) This invention utilizes modified dandelion pollen microspheres as natural microcarriers, improves their hydrophilicity and loading capacity through oxidation and activation, and combines them with an internal gel network to achieve stable encapsulation of mineral replenishment sources and remineralized active factors, effectively improving the dispersion stability of functional components in candy systems and reducing the loss of active components during processing and storage.
[0025] (2) The modified dandelion pollen microspheres in this invention have a rigid-flexible composite structure that combines outer wall protection with an internal slow-release network. This structure can spatially confine the encapsulated sugar substitutes, sugar alcohols, mineral replenishment sources and remineralization active factors, allowing the relevant components to be gradually released during consumption and improving the controllability of the functional component release process.
[0026] (3) This invention constructs an enhanced continuous phase network by microfibrillated dietary fiber, which improves the structural stability of the aerated candy system, improves the uniformity of bubbles and storage stability, and at the same time utilizes the spatial support of the fiber network to reduce the sedimentation of modified dandelion pollen microspheres in the candy matrix, thereby improving the uniformity of the internal structure of the product.
[0027] (4) This invention combines the microcavity structure, gel sustained-release mechanism and fiber-reinforced gas-filling structure of natural dandelion pollen to achieve structural synergy between natural carrier materials and food processing system. Compared with the traditional method of simply adding active powder in functional candies, it has better protection of active components and system stability. Attached Figure Description
[0028] Figure 1 The images, from left to right, are scanning electron microscope (SEM) images of natural dandelion pollen (preliminary washing), oxidized and activated dandelion pollen prepared in Example 1 and Example 2, respectively.
[0029] Figure 2 The image shows a scanning electron microscope (SEM) image of the modified dandelion pollen microspheres loaded with calcium citrate and nano-hydroxyapatite prepared in Example 3.
[0030] Figure 3 Scanning electron microscope (SEM) images of the microfibrillated dietary fibers prepared in Examples 9 and 10.
[0031] Figure 4 SEM microstructure and EDS elemental surface scan images of the surfaces of the untreated / demineralized blank control group, the treatment group of Application Example 1, and the treatment group of Application Example 7. Detailed Implementation
[0032] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0033] Unless otherwise specified, the experimental methods used in the specific implementation methods are all conventional methods, and the materials and reagents used are all commercially available unless otherwise specified.
[0034] In this invention, unless otherwise specified, "%" represents a percentage by mass; the raw materials and reagents used are all commercially available products.
[0035] The raw material parameters used in this invention are as follows: The non-fermentable sugar substitutes used in this invention include: Xylitol: purity 99.0%, water solubility 63% at 20℃; Erythritol: purity 99.5%, water solubility 37% at 20℃.
[0036] Both xylitol and erythritol are sugar alcohols with a polyhydroxy alcohol structure and do not contain free reducing aldehyde or ketone groups.
[0037] The mineral supply sources used in this invention include: Calcium citrate: Calcium content is 21.0%; Calcium hydrogen phosphate: calcium content is 23.0%, phosphorus content is 18.0%.
[0038] The water-soluble colloids used in this invention include: Sodium alginate: purity 98.0%, viscosity of 1% aqueous solution at 25℃ is 450 mPa·s; Gelatin: purity 95.0%, gel strength 220 Bloom.
[0039] The remineralization active factors used in this invention include: Nano-hydroxyapatite: average particle size of 50 nm, calcium-to-phosphorus molar ratio of 1.67; Casein phosphopeptide-amorphous calcium phosphate complex (CPP-ACP): calcium-to-phosphorus molar ratio is 1.50.
[0040] The dandelion pollen used in this invention is: Natural dandelion pollen has an average particle size of 42 μm, a moisture content of 6.5%, a crude protein content of 12.3%, and a crude fat content of 4.8%.
[0041] The dietary fiber raw material used in this invention is: Oat insoluble dietary fiber has a dietary fiber content of 88.5%, an average fiber length of 520 μm, and an average fiber diameter of 18 μm.
[0042] Example 1: Preparation of oxidatively activated dandelion pollen This embodiment provides a method for preparing oxidatively activated dandelion pollen, using natural dandelion pollen as the starting material. The specific steps are as follows: 1. Pre-treatment (defatting and deproteinization) Degreasing treatment: Take 100g of natural dandelion pollen, add 500mL of food-grade anhydrous ethanol, stir and defatted at 45℃ for 2h; filter, wash the filter cake twice with anhydrous ethanol, and dry at 50℃ to constant weight to obtain defatted dandelion pollen.
[0043] Protein removal treatment: The defatted dandelion pollen was dispersed in a 0.5% sodium hydroxide aqueous solution at a solid-liquid ratio of 1:10 (g / mL), and extracted with gentle stirring at 40℃ for 1.5 h to dissolve most of the soluble proteins and intracellular contents; centrifuged (4000 r / min, 10 min), the supernatant was discarded, and the precipitate was repeatedly washed with deionized water until the washing liquid was neutral, and dried to obtain the defatted and protein-free dandelion pollen outer wall microscopic natural matrix.
[0044] 2. Oxidation activation treatment A 1.5% hydrogen peroxide aqueous solution was prepared, and the pH of the system was adjusted to 9.5 using sodium hydroxide to construct a food-grade alkaline peroxide activation system.
[0045] The defatted and deproteinized dandelion pollen was added to an alkaline peroxide activation system (solid-liquid ratio of 1:15 g / mL), heated to 35°C, and gently sheared and stirred for 1.5 h to activate the reaction.
[0046] After the reaction was completed, the mixture was rapidly cooled to room temperature and the solid material was collected by filtration. It was then washed successively with deionized water and anhydrous ethanol until the filtrate was neutral and free of peroxide residue. The oxidized and activated dandelion pollen was then dried in a vacuum drying oven at 55°C for 12 hours to obtain the oxidized and activated dandelion pollen.
[0047] 3. Parameter detection and characterization The oxidized and activated dandelion pollen obtained in this embodiment was subjected to physical characterization and detection: Specific surface area (BET method): The specific surface area of oxidized and activated dandelion pollen was determined to be 16.2 m² using a fully automated specific surface area and porosity analyzer (N₂ adsorption-desorption method). 2 / g.
[0048] Static water contact angle: Using an optical contact angle meter, dried oxidized and activated dandelion pollen was pressed into tablets, and 2 μL of deionized water was added. The static contact angle with water was measured to be 38.5°.
[0049] Example 2: Preparation of oxidatively activated dandelion pollen This embodiment provides another method for preparing oxidatively activated dandelion pollen, the specific steps of which are as follows: 1. Pre-treatment (defatting and deproteinization) Degreasing treatment: Take 100g of natural dandelion pollen, add 600mL of food-grade anhydrous ethanol, and reflux extract at 50℃ for 2.5h; filter, wash the filter cake 3 times with anhydrous ethanol, and dry at 50℃ to constant weight to obtain defatted dandelion pollen.
[0050] Protein removal treatment: The defatted dandelion pollen was dispersed in a 0.8% sodium hydroxide aqueous solution at a solid-liquid ratio of 1:15 (g / mL), and extracted by stirring at 45℃ for 2 hours to fully dissolve intracellular proteins and free impurities; centrifuged (4500 r / min, 10 min), the supernatant was discarded, and the precipitate was repeatedly washed with deionized water until the washing liquid was neutral, and dried to obtain defatted and protein-free dandelion pollen.
[0051] 2. Oxidation activation treatment (high specific surface area enhancement process) A 4.8% hydrogen peroxide aqueous solution was prepared, and the pH of the system was adjusted to 10.5 using sodium hydroxide to construct a highly effective alkaline peroxide activation system.
[0052] The defatted and deproteinized dandelion pollen was added to an alkaline peroxide activation system (solid-liquid ratio of 1:20 g / mL), heated to 50°C, and stirred at high shear (800 r / min) for 3 h to activate the reaction, thereby thoroughly opening and clearing the micropores and gaps in the outer wall of the pollen.
[0053] After the reaction was completed, the mixture was quickly cooled to room temperature in an ice bath, and the solid material was collected by filtration. It was then washed with deionized water and anhydrous ethanol until the filtrate was neutral and free of peroxide residue. The mixture was then dried in a vacuum drying oven at 60°C for 10 hours to obtain oxidized and activated dandelion pollen with high specific surface area.
[0054] 3. Parameter detection and characterization The oxidized and activated dandelion pollen obtained in this embodiment was subjected to physical characterization and detection: Specific surface area (BET method): The specific surface area of oxidized activated dandelion pollen, measured using a fully automated specific surface area and porosity analyzer (N2 adsorption-desorption method), was 43.8 m². 2 / g.
[0055] Static water contact angle: Using an optical contact angle meter, dried oxidized and activated dandelion pollen was pressed into tablets, and 2 μL of deionized water was added. The static contact angle with water was measured to be 26.4°. Scanning electron microscopy (SEM) images of natural dandelion pollen (preliminary washing), oxidized and activated dandelion pollen prepared in Examples 1 and 2 are shown below. Figure 1 As shown.
[0056] Example 3: Preparation of modified dandelion pollen microspheres This embodiment provides a method for preparing modified dandelion pollen microspheres, the specific steps of which are as follows: 1. Raw material preparation and formula ratio The raw materials were weighed according to a mass ratio of oxidized activated dandelion pollen to loaded mineral replenishment source and remineralization active factor of 1.0:0.2:0.1. Take 10.0 g of the oxidized and activated dandelion pollen prepared in Example 1; Mineral source: Calcium citrate 2.0g; Remineralization active agent: Nano-hydroxyapatite (nHAp) 1.0g; 100mL of deionized water.
[0057] 2. Differential Pressure Loading Procedure Calcium citrate and nano-hydroxyapatite were added to deionized water and ultrasonically dispersed for 15 minutes to prepare a uniform composite suspension aqueous solution.
[0058] The oxidized and activated dandelion pollen prepared in Example 1 was slowly added to the above composite suspension and gently stirred to fully wet and disperse it.
[0059] The mixture was transferred to a vacuum negative pressure reactor and evacuated to a vacuum level of -0.09 MPa. The vacuum was maintained for 15 minutes to remove residual gas from the hollow cavities and micropores inside the dandelion pollen. Then, the pressure was quickly restored to normal, allowing the composite suspension to penetrate into the hollow cavities inside the dandelion pollen under the action of pressure difference. This vacuum-normal pressure alternating cycle was repeated 3 times.
[0060] 3. In-situ gel trapping procedure Under gentle stirring, a 2.0% (w / w) aqueous solution of calcium lactate (as a calcium salt inducer to provide gel-inducing ions) was added dropwise to the system that had undergone differential pressure loading.
[0061] After continuous stirring for 30 minutes, calcium ions combine and cross-link with the residual polysaccharides on the outer wall of the oxidized and activated dandelion pollen, forming a polysaccharide gel network in situ inside the dandelion pollen, which then traps and solidifies the loaded calcium citrate and nano-hydroxyapatite within the internal cavity of the microspheres.
[0062] 4. Post-processing steps The material was centrifuged to separate solid and liquid components (4500 r / min, 8 min), and the precipitated microspheres were collected.
[0063] Use deionized water to wash quickly away any free components that have not entered the cavity and bound.
[0064] The washed microspheres were dried in a vacuum drying oven at 50℃ for 12 hours until constant weight was obtained, thus obtaining modified dandelion pollen microspheres; SEM results are shown below. Figure 2 As shown.
[0065] Example 4: Preparation of modified dandelion pollen microspheres This embodiment provides another method for preparing modified dandelion pollen microspheres, using activated pollen with high specific surface area and different minerals and active factors. The specific steps are as follows: 1. Raw material preparation and formula ratio The raw materials were weighed according to a mass ratio of oxidized activated dandelion pollen to loaded mineral replenishment source and remineralization active factor of 1.0:0.2:0.1. Take 10.0g of the oxidized and activated dandelion pollen prepared in Example 2; Mineral source: 2.0g of dicalcium phosphate; Remineralization active factor: Casein phosphopeptide-amorphous calcium phosphate complex (CPP-ACP) 1.0g; 100mL of deionized water.
[0066] 2. Differential pressure loading and in-situ gel trapping Add dicalcium phosphate and CPP-ACP to deionized water and disperse evenly by ultrasonication; add oxidized activated dandelion pollen prepared in Example 2 and stir to mix evenly.
[0067] The mixture was transferred to a vacuum negative pressure reactor and circulated four times between a vacuum of -0.085 MPa and atmospheric pressure to promote the deep penetration of the composite suspension into the internal cavity of the pollen.
[0068] Under gentle stirring, a 1.5% (w / w) calcium chloride aqueous solution (as an inducer) was added dropwise, and the reaction was stirred for 25 min to induce the formation of an internal gel network of pollen residual polysaccharides, thereby trapping and solidifying dicalcium phosphate and CPP-ACP within the internal cavity of the microspheres.
[0069] 3. Post-processing The material was centrifuged, and the free components that were not bound to the cavity were quickly washed with deionized water. The material was then vacuum dried at 50°C to constant weight to obtain modified dandelion pollen microspheres.
[0070] Example 5: Preparation of modified dandelion pollen microspheres (high loading ratio) This embodiment provides a method for preparing modified dandelion pollen microspheres with a high loading ratio. The specific steps are as follows: 1. Raw material preparation and formula ratio The raw materials were weighed according to a mass ratio of oxidized activated dandelion pollen to loaded mineral replenishment source and remineralization active factor of 4.0:1.5:1.0. Take 40.0g of the oxidized and activated dandelion pollen prepared in Example 2; Mineral source: Calcium citrate 15.0g; Remineralization active agent: 10.0g of nano-hydroxyapatite (nHAp); 250mL of deionized water.
[0071] 2. Differential pressure loading and in-situ gel trapping Calcium citrate and nano-hydroxyapatite were dissolved / dispersed in deionized water and ultrasonically dispersed, followed by the addition of oxidized and activated dandelion pollen and mixed well.
[0072] The mixture is transferred to a vacuum reactor and subjected to alternating cycles of -0.095 MPa vacuum and atmospheric pressure five times to achieve high-density differential pressure filling.
[0073] A 3.0% (w / w) aqueous solution of calcium lactate was added dropwise, and the mixture was stirred for 40 min to induce the formation of a gel network that locks in the components within the microcavities.
[0074] 3. Post-processing Centrifugation, washing of free components, and drying yield modified dandelion pollen microspheres with high loading capacity.
[0075] Example 6: Preparation of modified dandelion pollen microspheres (single-loaded mineral supply source) This embodiment provides a method for preparing modified dandelion pollen microspheres loaded only with mineral replenishment sources. The specific steps are as follows: 1. Raw material preparation and formula ratio The raw materials were weighed according to a mass ratio of oxidized activated dandelion pollen to loaded mineral source of 1.0:0.3 (excluding remineralization active factors): Take 10.0 g of the oxidized and activated dandelion pollen prepared in Example 1; Mineral source: Calcium citrate 3.0g; 100mL of deionized water.
[0076] 2. Differential pressure loading and in-situ gel trapping Disperse calcium citrate in water, add oxidized and activated dandelion pollen, and stir well.
[0077] The calcium citrate suspension was injected into the internal cavity of the pollen by three cycles of alternating vacuum and atmospheric pressure at -0.09 MPa.
[0078] A 2.0% (w / w) aqueous solution of calcium lactate was added dropwise, and the reaction was allowed to proceed for 30 minutes. The pollen residual polysaccharides were used to form a gel network embedded with calcium citrate.
[0079] 3. Post-processing Solid-liquid separation was performed, and free calcium citrate outside the chamber was washed away. The mixture was then vacuum dried to obtain modified dandelion pollen microspheres with a single mineral supply source.
[0080] Example 7: Preparation of modified dandelion pollen microspheres (single-loaded remineralization active factor) This embodiment provides a method for preparing modified dandelion pollen microspheres loaded only with remineralization active factors. The specific steps are as follows: 1. Raw material preparation and formula ratio The raw materials were weighed according to a mass ratio of oxidized activated dandelion pollen to loaded remineralization active factor of 1.0:0.3 (excluding mineral replenishment source): Take 10.0 g of the oxidized and activated dandelion pollen prepared in Example 1; Remineralization active agent: Nano-hydroxyapatite 3.0g; 100mL of deionized water.
[0081] 2. Differential pressure loading and in-situ gel trapping Nano-hydroxyapatite was ultrasonically dispersed in water to prepare a suspension, and then oxidatively activated dandelion pollen was added.
[0082] Three cycles of alternating vacuum and atmospheric pressure treatment under -0.09 MPa conditions were performed to promote the infiltration of nano-hydroxyapatite into the pollen cavity.
[0083] A 2.0% (w / w) aqueous solution of calcium lactate was added dropwise, and the reaction was allowed to proceed for 30 minutes, resulting in the formation of a gel network that traps nano-hydroxyapatite within the pollen cavity.
[0084] 3. Post-processing Centrifugation, washing away free active particles on the surface, and drying yield modified dandelion pollen microspheres loaded with remineralized active factors.
[0085] Example 8: Comparative preparation of modified dandelion pollen microspheres (natural dandelion pollen control group) This embodiment provides a comparative preparation method for modified microspheres using natural dandelion pollen as a carrier. The difference from Example 3 is that natural dandelion pollen without oxidation activation treatment is used instead of the oxidized and activated dandelion pollen prepared in Example 1 to obtain natural dandelion pollen loaded microspheres (control sample).
[0086] Example 9: Preparation of Microfibrillated Dietary Fiber This embodiment provides a method for preparing microfibrillated dietary fiber, using oat insoluble dietary fiber as raw material. The specific steps are as follows: S1 Pretreatment (Degreasing and Impurity Removal) Weigh 100g of oat insoluble dietary fiber raw material, add 500mL of 85% ethanol aqueous solution, and gently stir and extract at 50℃ for 1h to defatt and remove water-soluble impurities.
[0087] The filter cake was filtered and rinsed with deionized water until no alcohol odor was detected. The filter cake was then dispersed in deionized water to prepare a dietary fiber suspension with a mass fraction of 2.0%.
[0088] S2 pre-mixing The dietary fiber suspension prepared in step S1 is placed in a high-shear emulsifier and dispersed under high shear at a speed of 8000 r / min for 15 min, so that the tightly packed dietary fiber bundles undergo initial mechanical dissociation and dispersion.
[0089] S3 High Pressure Homogenization and Defiberization The pre-dispersed suspension obtained in step S2 is fed into a high-pressure homogenizer for high-pressure homogenization.
[0090] The homogenization pressure was set to 60 MPa, and the homogenization cycle was repeated twice to promote the axial peeling, longitudinal cracking, and microfibrillation of dietary fiber.
[0091] During the homogenization process, the outlet of the homogenizer is connected to a shell-and-tube plate heat exchanger and cooled with ice water to keep the material temperature between 38-42℃ throughout the homogenization process.
[0092] S4 Post-processing The microfibrillated dietary fiber suspension obtained in step S3 is spray-dried (inlet air temperature 140℃, outlet air temperature 75℃) to obtain microfibrillated dietary fiber powder.
[0093] 5. Structural parameter characterization The microstructure of the microfibrillated dietary fiber prepared in this embodiment was analyzed using scanning electron microscopy (SEM) and a laser particle size and morphology analyzer. Figure 3 As shown.
[0094] Average length: The length of the microfiber structure is between 60-80 μm, and the aspect ratio is between 35-45.
[0095] Example 10: Preparation of Microfibrillated Dietary Fiber This embodiment provides another method for preparing microfibrillated dietary fiber. By controlling the pretreatment concentration, shear strength, and homogenization pressure, microfibrillated dietary fiber with a large average length and high aspect ratio is obtained. The specific steps are as follows: S1 Pretreatment (Degreasing and Impurity Removal) Weigh 100g of oat insoluble dietary fiber raw material, add 500mL of 85% ethanol aqueous solution, and gently stir and extract at 50℃ for 1h to remove fat and impurities.
[0096] The filter cake was filtered and rinsed with deionized water until no alcohol odor was detected. The filter cake was then dispersed in deionized water to prepare a dietary fiber suspension with a mass fraction of 3.5%.
[0097] S2 pre-mixing The dietary fiber suspension prepared in step S1 was placed in a high-shear emulsifier and gently sheared and dispersed at a speed of 5000 r / min for 8 min (the shearing speed and dispersion time were reduced compared to Example 9 to avoid excessive mechanical chain breakage), so that the dietary fiber bundles would initially dissociate.
[0098] S3 High Pressure Homogenization and Defiberization The pre-dispersed suspension obtained in step S2 is fed into a high-pressure homogenizer for high-pressure homogenization.
[0099] The homogenization pressure was set to 50 MPa, and the homogenization cycle was repeated once.
[0100] During the homogenization process, ice water is introduced into the outlet of the homogenizer to cool the material and control the material temperature at 35-39℃.
[0101] S4 Post-processing After centrifuging and concentrating the microfibrillated dietary fiber suspension obtained in step S3, vacuum freeze-drying is used to obtain microfibrillated dietary fiber powder that maintains a high aspect ratio.
[0102] 5. Structural parameter characterization The microstructure of the microfibrillated dietary fiber prepared in this embodiment was analyzed using scanning electron microscopy (SEM) and a laser particle size and morphology analyzer. Figure 3 As shown.
[0103] Average length: The length of the microfiber structure is between 220 and 250 μm; the aspect ratio is between 110 and 120.
[0104] Application Example 1: Preparation of aerated candy The specific steps of the preparation method in this application embodiment are as follows: 1. Raw material formula Modified dandelion pollen microspheres (prepared according to Example 3): 1.3 parts; Microfiberized dietary fiber (prepared using Example 9): 1.5 parts; Water-soluble colloid (sodium alginate): 2.0 parts; Non-fermented sugar substitute (xylitol): 45.0 parts; Water: 8.0 parts.
[0105] 2. Preparation process steps S1 continuous phase matrix and microfiber network swelling preparation Weigh 2.0 parts of sodium alginate and 1.5 parts of the microfibrillated dietary fiber prepared in Example 9, and mix them evenly.
[0106] The above mixture was slowly added to 8.0 parts of deionized water and stirred at 1200 r / min for 30 min in a 60°C water bath to completely hydrate and dissolve sodium alginate. At the same time, it promoted the full expansion of microfibrillated dietary fiber in the aqueous phase to form a continuous phase colloidal suspension with three-dimensional network cross-linking support potential.
[0107] S2 sugar alcohol melted and mixed syrup cooked Add 45.0 parts xylitol to the above colloidal suspension, heat to 95-100℃ and stir until the xylitol is completely melted and dissolved to prepare a uniform mixed syrup.
[0108] The mixed syrup is transferred to a vacuum cooking pot for preheating under normal pressure and dehydration under slight negative pressure. The cooking temperature is controlled at 110-112℃ to evaporate and remove some of the water, thereby obtaining a high-viscosity concentrated syrup matrix.
[0109] S3 active microsphere compound and pre-inflated Cool the boiled concentrated syrup to 80-85℃ and add 1.3 parts of the modified dandelion pollen microspheres prepared in Example 3.
[0110] Under nitrogen protection, gentle low-speed stirring (300 r / min) was performed to uniformly suspend the modified dandelion pollen microspheres and embed them in the network structure constructed by high-viscosity syrup and microfibrillated dietary fiber, preventing the microspheres from settling or agglomerating.
[0111] S4 Continuous Inflation Foaming and Micropore Curing The material containing microspheres is conveyed to a continuous high-pressure air compressor, where sterile compressed air is introduced for inflation and foaming.
[0112] The inflation head speed was controlled at 450 r / min, the inflation back pressure at 0.25 MPa, and the material outlet temperature at 65-70℃. Microfibrillated dietary fiber and sodium alginate synergistically act at the gas-liquid interface, strengthening the bubble wall membrane and preventing bubble coalescence.
[0113] S5 Forming, Cooling and Packaging The aerated and foamed sugar paste is extruded and poured into the molding mold.
[0114] Cool and solidify in a cooling tunnel with relative humidity <40% and temperature 18-20℃ for 45 minutes, then demold and cut into pieces to obtain the finished inflatable candy.
[0115] 3. Characterization of physical properties and apparent density The density of the prepared aerated candy was determined using the water displacement method. Apparent density: The final aerated candy had an apparent density of 0.52 g / cm³. 3 .
[0116] Application Example 2: Preparation of aerated candy The difference between this application example and application example 1 is that: Raw material changes: The modified dandelion pollen microspheres were prepared using the method described in Example 4; the microfibrillated dietary fiber was prepared using the method described in Example 10; the water-soluble colloid was gelatin; the non-fermentable sugar substitute was erythritol; the proportions of the remaining raw materials and the preparation process were exactly the same as in Application Example 1; the apparent density of the final aerated candy was 0.55 g / cm³. 3 Application Example 3: Preparation of aerated candy The difference between this application example and application example 1 is that: Raw material formula: Modified dandelion pollen microspheres (prepared according to Example 5): 6.5 parts; Microfiberized dietary fiber (prepared using Example 9): 3.5 parts; Water-soluble colloid (sodium alginate): 6.0 parts; Non-fermented sugar substitute (xylitol): 65.0 parts; Water (deionized water): 15.0 parts; Apparent density control: Adjust the continuous aeration foaming process parameters, reduce the aeration head speed to 300 r / min, and adjust the aeration back pressure to 0.35 MPa, so that the final aerated candy has an apparent density of 0.78 g / cm³. 3 ; The remaining preparation process steps are exactly the same as in Application Example 1.
[0117] Application Example 4: Preparation of aerated candy The difference between this application example and application example 1 is that the modified dandelion pollen microspheres used are those prepared in Example 6 (single-loaded mineral supply source); the apparent density of the final aerated candy is 0.51 g / cm³. 3 The remaining raw material components, dosages, and preparation process steps are exactly the same as in Application Example 1.
[0118] Application Example 5: Preparation of aerated candy The difference between this application example and application example 1 is that the modified dandelion pollen microspheres used are those prepared in Example 7 (single-loaded remineralization active factor); the apparent density of the final aerated candy is 0.52 g / cm³. 3 The remaining raw material components, dosages, and preparation process steps are exactly the same as in Application Example 1.
[0119] Application Example 6: Preparation of aerated candy (Comparative example: microspheres loaded with natural pollen) The difference between this application example and application example 1 is that the modified dandelion pollen microspheres used are those prepared in Example 8 (the control group using microspheres prepared from natural dandelion pollen); the apparent density of the final aerated candy is 0.53 g / cm³. 3 The remaining raw material components, dosages, and preparation process steps are exactly the same as in Application Example 1.
[0120] Application Example 7: Preparation of aerated candy (Comparative Example: Physical Mixing Group 1) The difference between this application example and application example 1 is that the modified dandelion pollen microspheres are not added; instead, 1.0 part of oxidized activated dandelion pollen, 0.2 parts of calcium citrate, and 0.1 parts of nano-hydroxyapatite prepared in example 1 are directly added (the three are physically mixed, and the total mass fraction is maintained at 1.3 parts); the apparent density of the final aerated candy is 0.52 g / cm³. 3 The remaining raw material components, dosages, and preparation process steps are exactly the same as in Application Example 1.
[0121] Application Example 8: Preparation of aerated candy (Comparative Example: Physical Mixing Group 2) The difference between this application example and application example 1 is that the modified dandelion pollen microspheres are not added; instead, 1.0 part of oxidized activated dandelion pollen, 0.2 parts of calcium citrate, and 0.1 parts of nano-hydroxyapatite prepared in example 2 are directly added (the three are physically mixed, and the total mass fraction is maintained at 1.3 parts); the apparent density of the final aerated candy is 0.51 g / cm³. 3 The remaining raw material components, dosages, and preparation process steps are exactly the same as in Application Example 1.
[0122] Application Example 9: Preparation of aerated candy (Comparative Example: Physical Mixing Group 3) The difference between this application example and application example 1 is that: instead of adding modified dandelion pollen microspheres, 1.0 part of natural dandelion pollen, 0.2 parts of calcium citrate, and 0.1 parts of nano-hydroxyapatite are directly added (the three are physically mixed, and the total mass fraction is maintained at 1.3 parts); the apparent density of the final aerated candy is 0.53 g / cm3; the remaining raw material components, dosages, and preparation process steps are exactly the same as in application example 1.
[0123] Application Example 10: Preparation of aerated candy (Comparative Example: Blank carrier group) The difference between this application example and application example 1 is that: no modified dandelion pollen microspheres are added, and no mineral replenishment source or remineralization active factor is added; instead, only 1.3 parts of oxidized activated dandelion pollen prepared in example 1 are added; the apparent density of the final aerated candy is 0.51 g / cm³. 3The remaining raw material components, dosages, and preparation process steps are exactly the same as in Application Example 1.
[0124] Test Example 1: Oral Active Component Release and Remineralization Performance Test The aerated candies prepared in Examples 1-10 were tested for sustained release of oral active components, enamel remineralization, and retention of simulated chewing residues. The specific test methods and results are as follows: 1. Testing Method (1) Dynamic release rate and cumulative release rate of calcium / phosphate ions in artificial saliva in vitro Candy samples (5.0 g) from each application example were placed in 100 mL of dynamic artificial saliva (pH 6.8, 37 °C, rotation speed 100 r / min). Samples were taken at set time points of 1, 3, 5, 10, 15, and 30 min. The Ca2+ concentration in the solution was determined using inductively coupled plasma optical emission spectrometry (ICP-OES). The 5-minute burst release rate (the percentage of the total load released in the first 5 minutes) and the 30-minute cumulative release rate were calculated.
[0125] (2) In vitro demineralized enamel remineralization capacity and deep deposition depth Artificial demineralized enamel slices were prepared using extracted incisors (initial surface microhardness approximately 110-120 HV). The slices were then immersed in the sample leachate for pH-cycled remineralization treatment (37℃, 6 hours of leachate remineralization + 18 hours of demineralization solution treatment daily, for 14 consecutive days). After treatment, the surface hardness recovery rate of the enamel was measured using a microhardness tester; the depth of the remineralized deposit and the surface calcium-to-phosphorus atomic ratio (Ca / P) were analyzed using scanning electron microscopy-energy dispersive spectroscopy (SEM-EDS) and cross-sectional nanoindentation.
[0126] (3) Simulated chewing process: flushing and retention rate of active factors Using an oral mastication simulator (with a set biting force of 50N and a flushing frequency of 60 times / min), artificial saliva was used as the flushing medium to simulate the entire process of eating candy and chewing for 5 minutes. After the test, the active components (nHAp / CPP-ACP) remaining on the simulated tooth surface and mucosal adhesion layer were collected, digested with strong acid, and then the marker elements were determined by ICP-OES to calculate the chewing residue retention rate of the active factors.
[0127] 2. Test Results The test results of Application Examples 1-10 are shown in Tables 1 and 2: Table 1
[0128] Table 2
[0129] Figure 4 shows the SEM microstructure and EDS elemental surface scan images of the surfaces of the untreated / demineralized blank control group, the treatment group of Application Example 1, and the treatment group of Application Example 7.
[0130] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and not to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some of the technical features; and these modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims
1. An aerated candy, characterized in that, By weight, including: Oxidative activation of dandelion pollen, 1.0-4.0; Microfiber dietary fiber, 1.5-3.5; Water-soluble colloid, 2.0-6.0; Non-fermentable sugar substitutes, sugar alcohols, 45.0-65.0; Mineral replenishment source, 0.2-1.5; Remineralization activity factor, 0.1-1.0; Water, 8.0-15.0; The oxidized activated dandelion pollen is formed by oxidizing and activating defatted and deproteinized dandelion pollen. It is loaded with at least part of the mineral supply source and / or remineralization active factor. The residual polysaccharides and / or exogenous gelled polysaccharides in the oxidized activated dandelion pollen form an internal gel network with the mineral supply source and / or remineralization active factor. The remineralization active factor is a bioactive inorganic material or a calcium-phosphorus composite active component that provides mineralization active sites, promotes calcium and phosphorus ion deposition, or regulates the calcium and phosphorus mineralization process. The microfibrillated dietary fiber is obtained by physical microfibrillation of insoluble dietary fiber, and its microfibril structure has a length of 60-250μm and an aspect ratio of 35-120. The apparent density of the aerated candy is 0.5-0.8 g / cm³. 3 .
2. The aerated candy according to claim 1, characterized in that, The oxidized and activated dandelion pollen is loaded with mineral supply sources and remineralization active factors to form modified dandelion pollen microspheres with an internal gel network structure. The modified dandelion pollen microspheres were prepared by the following steps: (1) Oxidative activation: Defatted and deproteinized dandelion pollen was dispersed in a food-grade alkaline peroxide system for oxidative activation treatment, washed and dried to obtain oxidized activated dandelion pollen; (2) Pressure differential loading: The oxidized and activated dandelion pollen is mixed with a composite aqueous solution containing non-fermentable sugar alcohol, mineral replenishment source and remineralization active factor, and the mixture is alternately circulated between vacuum conditions and normal pressure to allow the composite aqueous solution to penetrate into the hollow cavity inside the dandelion pollen. (3) In-situ gel network trapping: Introduce an inducer to induce the formation of a gel network of the water-soluble colloid into the system obtained in step (2) to form a polysaccharide gel network inside the dandelion pollen; (4) Post-processing: The material obtained in step (3) is subjected to solid-liquid separation, washing to remove free components that are not bound to the cavity, and drying to obtain the modified dandelion pollen microspheres; The specific surface area of the oxidized and activated dandelion pollen is 15-45 m². 2 / g, and the static contact angle with water is ≤45°.
3. The aerated candy according to claim 2, characterized in that, In step (1), the mass fraction of peroxide in the alkaline peroxide system is 1%-5%, the temperature of the oxidation activation treatment is 30-50℃, and the treatment time is 1-3h; In step (2), the vacuum level is -0.08 MPa to -0.095 MPa. In step (3), the food inducer is a calcium salt that provides gel-inducing ions.
4. The aerated candy according to claim 1, characterized in that, The microfibrillated dietary fiber is prepared by the following steps: S1 Pretreatment: The insoluble dietary fiber raw material is degreased and impurities are removed, and then dispersed in water to form a dietary fiber suspension; S2 Pre-dispersion: The dietary fiber suspension obtained in step S1 is subjected to high shear dispersion to initially dissociate the fiber bundles; S3 High-pressure homogenization and defibrillation: The system obtained in step S2 is subjected to high-pressure homogenization to cause the dietary fiber to dissociate, peel off and refine in size, so as to obtain a microfibrillated dietary fiber suspension. S4 Post-processing: The suspension obtained in step S3 is dried to obtain the microfibrillated dietary fiber.
5. The aerated candy according to claim 4, characterized in that: In step S3, the material temperature during the homogenization process is controlled below 45 ℃.
6. The aerated candy according to claim 1, characterized in that: The non-fermentable sugar alcohol has a water solubility of ≥30% (W / W) at 20 °C; and the non-fermentable sugar alcohol is a sugar alcohol compound with a polyhydroxy alcohol structure and without free reducing aldehyde or ketone groups.
7. The aerated candy according to claim 1, characterized in that: The mineral supply source is calcium salts and / or phosphates.
8. The aerated candy according to claim 1, characterized in that: The water-soluble colloid is one or more of hydrophilic natural polysaccharide colloids and hydrophilic proteins.
9. A method for preparing an aerated candy according to any one of claims 1-8, characterized in that, Includes the following steps: a. Matrix compounding: Microfibrillated dietary fiber, water-soluble colloids and water are mixed and sheared and dispersed to form a continuous phase hydrocolloid system; b. Boiling the syrup: Mix non-fermentable sugar substitutes with water and heat to boil. After cooling, mix with the continuous phase aqueous colloidal system obtained in step a to prepare the aerated precursor syrup. c. Microspheres and active factors are combined: Modified dandelion pollen microspheres, mineral replenishment sources and remineralization active factors are added to the aerated precursor syrup obtained in step b, and dispersed to obtain a dispersion containing microspheres. d. Aeration and solidification: The microsphere-containing dispersion obtained in step c is passed through a gas for high-pressure aeration. The aerated material is then injected into a mold, cooled, and solidified to obtain the aerated candy.
10. The method for preparing aerated candy according to claim 9, characterized in that: In step b, the heating and cooking process is carried out until the solid content is ≥85% (w / w); In step c, the mixing temperature when adding modified dandelion pollen microspheres is 50-70℃.