A satiety hydrogel and methods of making and using same

Abstract

The present application relates to a kind of satiety hydrogel and its preparation method and application.The satiety hydrogel has interpenetrating double network structure, which is formed by the first network gel with brittle structure and the second network gel with elastic structure penetrating each other and being crosslinked by physics.In order to improve the stability of the hydrogel in digestive tract, the present application adopts physical crosslinking to construct double-layer network structure, the hydrogel enters into gastrointestinal tract, slightly swells by absorbing water, expands the volume of gel, in addition, the dense network structure in satiety hydrogel can delay the penetration of gastrointestinal fluid, the brittle structure can delay the degradation rate of gel, and at the same time has higher elastic modulus, and the undegraded part in the interior can further maintain higher elastic modulus, so as to occupy the volume of digestive tract and exert pressure on the wall of digestive tract to continuously produce satiety.

Description

Technical Field

[0001] This invention belongs to the field of medical technology or food processing technology, specifically relating to a satiating hydrogel, its preparation method and application. Background Technology

[0002] With social development and improved living standards, obesity has become a significant issue affecting people's health and quality of life.

[0003] Currently, emerging weight-loss materials with gastric volume-filling effects, prepared from hydrogels, have become a hot research direction in weight-loss products. Hydrogels are a type of highly hydrophilic three-dimensional network structure gel that can rapidly absorb water and swell fully in the stomach, thereby achieving a physical support effect and producing a feeling of fullness. Such weight-loss products can achieve weight loss goals by reducing appetite and controlling food intake. However, currently commercially available weight-loss hydrogel products (such as Light Diamond Dietary Fiber Solid Beverage, Gelender®, and Full Feeling)... TM (For example, it needs to be mixed with 50-100ml of water, stirred for 3 seconds and taken immediately, followed by drinking 400-500ml of water, which reduces the convenience and compliance of users.)

[0004] CN116731354A discloses a method for covalently cross-linking nanocellulose into a monolithic structure using a chemical cross-linking agent, followed by further reduction of the cross-linked cellulose microspheres through dry cutting and compression processes. The resulting microspheres exhibit rapid water absorption and a high expansion ratio (3000-9000%). However, excessive expansion of stomach contents in a short period can lead to discomfort, pain, reflux, and even physical irritation of the stomach wall or impaired normal peristalsis. Furthermore, due to the disruptive effect of water molecules on the hydrogen bonds of nanocellulose, the material becomes structurally unstable and rapidly disintegrates after swelling upon contact with water, making it difficult to maintain a feeling of fullness.

[0005] CN120092943A discloses a hydrogel with weight-loss effects, its preparation method, and its application. The preparation method involves dissolving and mixing polysaccharide gum, cellulose, and fiber powder, homogenizing under high pressure to obtain a mixture, concentrating the mixture, and performing two freeze-drying processes to obtain the hydrogel. This hydrogel exhibits good water absorption and structural stability, preventing degradation or breakage caused by gastric juice and stomach movement. CN117796533A discloses a potent satiety-enhancing weight-loss hydrogel, which is cross-linked from sodium carboxymethyl cellulose, ethyl cellulose, and citric acid. The sodium carboxymethyl cellulose is obtained by treating commercially available high-viscosity sodium carboxymethyl cellulose with hydrogen peroxide and ethanol, followed by pulverization and sieving to obtain a low-viscosity sample. However, the overall production processes for these two hydrogels are cumbersome and costly, making large-scale production difficult. Furthermore, the chemical reagents such as hydrogen peroxide and ethanol introduced during the preparation process are difficult to remove and may cause harm to the human body.

[0006] CN119857015A discloses a gastric-slimming device and its manufacturing method. The device includes a jelly matrix and hydrogel microspheres encapsulated within the matrix. The hydrogel microspheres consist of a microsphere body derived from sodium alginate emulsification and a waterproof, biodegradable membrane coating the microsphere body. In an acidic gastric environment, the waterproof, biodegradable membrane decomposes, exposing the encapsulated hydrogel microspheres, causing them to absorb water and swell to 10-20 times their original volume, thus filling the stomach and prolonging gastric emptying. However, due to the high density of the microspheres, after ingestion, they absorb water and swell on the outside, forming sticky clumps that adhere to the esophagus and hinder their entry into the stomach. Furthermore, because the microspheres are small, a large quantity needs to be ingested to meet the functional requirements.

[0007] Therefore, existing hydrogel products for weight loss often suffer from poor durability and long-term safety, low nutritional value, and cumbersome production processes. Improving the stability of the gel in the gastrointestinal digestive system and developing a hydrogel that is easy to consume, palatable, nutritious, low in preparation cost, and has a strong satiating effect has become one of the urgent technical problems to be solved. Summary of the Invention

[0008] To address the shortcomings of existing technologies, the present invention aims to provide a saturated hydrogel, its preparation method, and its applications.

[0009] To achieve this objective, the present invention adopts the following technical solution:

[0010] In a first aspect, the present invention provides a saturated hydrogel having an interpenetrating double network structure, which is formed by interpenetrating a first network gel having a brittle structure and a second network gel having an elastic structure through physical cross-linking.

[0011] The raw materials for preparing the first network gel include gelling agent I and cationic crosslinking agent. The first network gel is formed by gelling agent I and cationic crosslinking agent through ionic crosslinking.

[0012] The raw materials for preparing the second network gel include gelling agent II, which is hydrophilic, and the second network gel is formed by the physical interaction between molecular chains of gelling agent II;

[0013] The gelling agent I includes gellan gum.

[0014] The gelling agent II comprises a combination of konjac gum and carrageenan.

[0015] This invention demonstrates that hydrogels prepared from konjac gum or carrageenan alone degrade rapidly in the acidic environment of the stomach, proving that the combination of konjac gum and carrageenan to prepare a second network gel has a significant synergistic effect in improving the stability and elasticity of the prepared hydrogel.

[0016] The dual-network gel is formed by the physical cross-linking of a first network gel with a brittle structure and a second network gel with an elastic structure, creating an interpenetrating dual-network structure. Here, "brittle" refers to the high rigidity of the network, which tends to undergo localized structural failure under stress. When a gel with a dual-network structure is subjected to external force, the first network gel (with a brittle structure) breaks down to dissipate energy. During this process, the second network gel (with an elastic structure) maintains the integrity of the gel. Therefore, the brittle first network gel and the elastic second network gel work together to leverage their respective excellent properties, thereby ensuring a harmonious balance between rigidity and toughness.

[0017] To improve the stability of hydrogels in the digestive tract, this invention employs a physical cross-linking structure to construct a dual-network structure. The first network gel is formed by gellan gum through metal ion cross-linking, creating a brittle network. At low temperatures, its molecules transform from random coils into double helices and aggregate, forming a highly rigid but easily fractured structure, primarily responsible for providing initial strength and delaying degradation. The second network gel is formed by carrageenan and konjac gum through hydrogen bonding and other interactions, creating an elastic network. The long-chain entanglement of konjac gum provides high water retention and a continuous elastic framework, while carrageenan forms reversible ionic bonding regions with metal ions. During the formation of the dual network, the mutual inhibition between gellan gum and carrageenan molecules promotes a tighter connection at the interface, thereby significantly improving the overall elastic modulus and structural robustness. When subjected to external force, the brittle first network breaks and dissipates energy first; then the ionic bonding regions of carrageenan in the elastic network break preferentially as "reversible sacrificial bonds", dissipating a large amount of energy to prevent crack propagation, while the elastic skeleton of konjac gum remains continuous, storing potential energy and maintaining overall integrity, so that the gel has both high strength, high toughness and excellent water absorption capacity.

[0018] Once inside the gastrointestinal tract, this dual-network gel absorbs water and expands moderately to increase its volume. Its dense dual-network structure effectively slows down the penetration and erosion of digestive juices. The brittle first network slows down the overall degradation rate, resulting in a gradient degradation of the gel from the surface inwards: while the outer layer gradually degrades, the inner layer maintains a high elastic modulus due to the synergistic effect of the dual networks. This stable volume maintenance and structural strength allow the gel to continuously occupy space in the digestive tract and exert pressure on the intestinal wall, thus producing a lasting feeling of fullness.

[0019] Preferably, the gelling agent I further includes sodium alginate.

[0020] Gellan gum and sodium alginate, when used together as gelling agents, have a significant synergistic effect in improving the stability of the prepared hydrogel.

[0021] Preferably, the mass ratio of gellan gum to sodium alginate is 10:1 to 10:5, for example, it can be 10:1, 10:1.5, 10:2, 10:2.5, 10:3, 10:3.5, 10:4, 10:4.5, 10:5, etc.

[0022] And / or, the gelling agent I further includes chitosan and / or pectin.

[0023] Preferably, the cation in the cationic crosslinking agent includes any one or a combination of at least two of calcium ions, magnesium ions, potassium ions, and sodium ions, with calcium ions being the most preferred.

[0024] Compared to other cations, calcium ion crosslinking agents can better complex with gelling agent I, forming a more compact network structure, thereby improving the stability of the gel.

[0025] Preferably, the source of the calcium ions includes any one or a combination of at least two of calcium lactate, calcium chloride, calcium carbonate, calcium hydroxide, calcium sulfate, and calcium ascorbate.

[0026] Preferably, the source of the magnesium ions includes any one or a combination of at least two of magnesium sulfate, magnesium chloride, magnesium carbonate, and magnesium silicate.

[0027] Preferably, the potassium ion source includes any one or a combination of at least two of potassium chloride, potassium citrate, potassium hydroxide, potassium lactate, potassium carbonate, potassium stearate, potassium bicarbonate, potassium hydrogen tartrate, potassium dihydrogen phosphate, potassium copper chlorophyllin, potassium sorbate, potassium alginate, potassium glycyrrhizate, and potassium polyaspartate.

[0028] Preferably, the source of the sodium ions includes any one or a combination of at least two of sodium sulfate, sodium hydroxide, sodium carbonate, sodium bicarbonate, sodium malate, and sodium acetate.

[0029] Preferably, the mass ratio of gelling agent I to cationic crosslinking agent is 10:1-200:1, for example, it can be 10:1, 30:1, 60:1, 90:1, 120:1, 150:1, 180:1, 200:1, etc.

[0030] The present invention controls the ratio of gelling agent I and cationic crosslinking agent within the above range, which can better balance the swelling effect and elastic modulus of the prepared hydrogel in the gastrointestinal tract.

[0031] Preferably, the gellan gum is a low-acyl gellan gum.

[0032] Low-acyl gellan gum forms a hard, brittle, and transparent gel with irreversible thermal properties; high-acyl gellan gum forms a soft, elastic gel with reversible thermal properties. In this invention, the gel formed by low-acyl gellan gum has high strength and a more stable structure, and can better maintain its structural integrity during in vivo digestion.

[0033] Preferably, the molecular weight of the gellan gum is 200-300 kDa, for example, it can be 200 kDa, 220 kDa, 240 kDa, 260 kDa, 280 kDa, 300 kDa, etc.

[0034] This invention creatively discovers that by controlling the molecular weight of gellan gum within the above-mentioned range, the stability of the prepared hydrogel can be further improved, the volume occupied in the digestive tract can be increased, and the consumer is more likely to experience a feeling of fullness.

[0035] Preferably, the mass ratio of konjac gum to carrageenan is 1:10-10:1, for example, it can be 1:10, 3:10, 5:10, 7:10, 9:10, 1:1, 3:1, 5:1, 7:1, 9:1, 10:1, etc.

[0036] Preferably, the mass ratio of gelling agent I to gelling agent II is 1:10-10:1, for example, it can be 1:10, 3:10, 5:10, 7:10, 9:10, 1:1, 3:1, 5:1, 7:1, 9:1, 10:1, etc.

[0037] Preferably, the raw materials for preparing the first network gel also include water.

[0038] Preferably, the raw materials for preparing the first network gel further include an acidity regulator.

[0039] Preferably, the acidity regulator includes any one or a combination of at least two of the following: citric acid, sodium citrate, potassium citrate, monosodium citrate, sodium DL-malate, L-malic acid, sodium L-malate, fumaric acid, lactic acid, tartaric acid, acetic acid, phosphoric acid, adipic acid, metatartaric acid, and hydrochloric acid.

[0040] Preferably, the raw materials for preparing the second network gel also include water.

[0041] In a second aspect, the present invention provides a method for preparing the satiated hydrogel as described in the first aspect, the method comprising the following steps:

[0042] (1) Mix gelling agent I and gelling agent II with water, heat to 50-100℃, and stir until gelling agent I and gelling agent II dissolve to obtain a compound adhesive solution.

[0043] (2) After the compound adhesive solution is cooled, it is mixed with a cationic crosslinking agent to obtain a saturated hydrogel.

[0044] The specific point values ​​within the 50-100℃ range can be selected as 50℃, 60℃, 70℃, 80℃, 90℃, 100℃, etc.

[0045] As described in the first aspect, the formation of gellan gum occurs during the cooling process of the solution, where disordered gellan gum molecular chains aggregate with each other through intermolecular forces to form a double helix structure.

[0046] In this invention, by controlling the heating temperature at 50-100℃, gelling agent I and gelling agent II can be better dissolved, giving full play to the gelling effect of the gelling agents, thereby forming a more stable gel structure.

[0047] Preferably, the stirring time in step (1) is 2-6 hours, for example, 2 hours, 3 hours, 4 hours, 5 hours, 6 hours, etc.

[0048] Preferably, after the gelling agent I and gelling agent II are dissolved in step (1), the solution is further subjected to heating sterilization treatment.

[0049] Preferably, the temperature of the heat sterilization treatment is above 80°C (e.g., 80°C, 85°C, 90°C, 95°C, 100°C, etc.), and the time is above 5 minutes (e.g., 5 minutes, 7 minutes, 9 minutes, 11 minutes, 13 minutes, 15 minutes, etc.).

[0050] Preferably, the temperature after cooling in step (2) is 50-70℃, for example, it can be 50℃, 55℃, 60℃, 65℃, 70℃, etc.

[0051] Preferably, in the solution after cooling the compound adhesive solution in step (2) and mixing it with the cationic crosslinking agent, the mass percentage of gelling agent I is 0.03-0.5% (e.g., 0.03%, 0.05%, 0.1%, 0.15%, 0.2%, 0.25%, 0.3%, 0.35%, 0.4%, 0.45%, 0.5%, etc.), preferably 0.2-0.5% (e.g., 0.2%, 0.22%, 0.24%, 0.26%, 0.28%, 0.3%, 0.32%, 0.34%, 0.36%, 0.38%, 0.4%, 0.42%, 0.44%, 0.46%, 0.48%, 0.5%, etc.).

[0052] In this invention, if the mass percentage of gelling agent I is too low, the resulting gel will have weak stability and will degrade rapidly due to gastric acid; if the mass percentage of gelling agent I is too high, the hydrogel jelly prepared further will have a hard texture and poor palatability.

[0053] Preferably, after the compound adhesive solution is cooled and mixed with the cationic crosslinking agent in step (2), the pH value of the solution is adjusted to 3.0-6.9, for example, it can be 3.0, 3.1, 3.5, 4.0, 4.5, 5.0, 5.5, 6.0, 6.5, 6.9, etc.

[0054] In this invention, controlling the pH value within the above-mentioned range can improve the stability of the hydrogel while ensuring that the prepared hydrogel jelly has appropriate hardness, sweetness, and acidity, resulting in excellent palatability.

[0055] Preferably, the pH value of the solution in step (2) is adjusted by an acidity regulator.

[0056] Preferably, the acidity regulator includes any one or a combination of at least two of the following: citric acid, sodium citrate, potassium citrate, monosodium citrate, sodium DL-malate, L-malic acid, sodium L-malate, fumaric acid, lactic acid, tartaric acid, acetic acid, phosphoric acid, adipic acid, metatartaric acid, and hydrochloric acid.

[0057] Preferably, after cooling the compound adhesive solution to 50-70°C in step (2), it is further cooled to 20-40°C.

[0058] The specific point values ​​within the 20-40℃ range can be selected as 20℃, 25℃, 30℃, 35℃, 40℃, etc.

[0059] By further reducing the temperature to 20-40℃, the crosslinking agent binds to the carboxyl groups on the outer side of the double helix chain, causing it to further aggregate and form a "linkage region," thus forming a three-dimensional gel network structure.

[0060] Thirdly, the present invention provides a product with weight management function, the product with weight management function including the satiety hydrogel described in the first aspect.

[0061] The types of products with weight management effects include any one of jelly, beverage, or meal replacement powder.

[0062] The beverage is a liquid drink containing the satiating hydrogel described in the first aspect.

[0063] The present invention relates to a satiating hydrogel with stable structure, excellent taste and strong compatibility. Nutritional additives and other components can be added during the preparation process to further improve the nutritional value and palatability of the composition while ensuring the weight loss effect.

[0064] Preferably, the composition further includes any one or a combination of at least two of sweeteners, nutritional additives, colorings, flavorings, fruit juices, and dairy products.

[0065] Preferably, the sweetener includes any one or a combination of at least two of erythritol, steviol glycosides, sucralose, or mogrosides.

[0066] Preferably, the nutritional additive includes any one or a combination of at least two of vitamins, polypeptides, active ions, prebiotics, or amino acids.

[0067] Preferably, the vitamins include any one or a combination of at least two of vitamin A, B vitamins, vitamin C, or vitamin E.

[0068] Preferably, the polypeptide includes any one or a combination of at least two of collagen peptides, elastin peptides, oligopeptides, oat peptides, or collagen tripeptides.

[0069] Preferably, the active ions include any one or a combination of at least two of iron ions, zinc ions, or calcium ions.

[0070] The numerical range described in this invention includes not only the point values ​​listed above, but also any point values ​​within the numerical ranges not listed above. Due to space limitations and for the sake of brevity, this invention will not exhaustively list all the specific point values ​​included in the range.

[0071] Compared with the prior art, the present invention has the following beneficial effects:

[0072] The satiety hydrogel involved in this invention overcomes the problems of short residence time and short disintegration time that occur with physical single cross-linking. It can occupy and remain in the gastric juice and small intestine environment for a long time without disintegrating. The elastic modulus is controlled at >13kPa (pressure applied by gastric peristalsis), achieving a long satiety support time and strong palatability. The technical solution of this invention has a simple process and low production cost.

[0073] The raw materials used in the preparation of the satiety hydrogel involved in this invention do not contain the relevant digestive enzymes in the human body. Therefore, none of its components can be absorbed by the human body and will not generate heat, thus further ensuring the purpose of meal replacement and weight loss.

[0074] The saturated hydrogel involved in this invention does not require the addition of chemical cross-linking substances during the preparation process, thus avoiding the toxic effects caused by chemical cross-linking agents.

[0075] The present invention relates to a satiating hydrogel with stable structure, excellent taste and strong compatibility. Nutritional additives and other components can be added during the preparation process to further improve the nutritional value and palatability of the composition while ensuring the weight loss effect. Attached Figure Description

[0076] Figure 1 This is a comparison chart of the weight change trends of volunteers in the experimental group and the control group in test example 3. Detailed Implementation

[0077] The technical solution of the present invention will be further illustrated below through specific embodiments. Those skilled in the art should understand that the embodiments described are merely illustrative of the present invention and should not be construed as limiting the invention in any way.

[0078] The sources of each component / raw material in the following embodiments are shown in Table 1.

[0079] Table 1

[0080]

[0081] Example 1

[0082] This embodiment provides a saturated hydrogel, the preparation method of which includes:

[0083] (1) Weigh 0.26 g gelling agent I (the mass ratio of gellan gum and sodium alginate is 10:3, where the molecular weight of gellan gum is 250 kDa) and 0.87 g gelling agent II (the mass ratio of konjac gum and carrageenan is 1.5:1) and mix them evenly to prepare a compound powder. Heat 90 g of water to 70°C and add the compound powder to it while stirring. Stir for 3 h until completely dissolved. Then raise the temperature to 100°C and maintain it for 5 min for sterilization. Filter to remove insoluble matter and obtain the compound gel solution.

[0084] (2) After the compound adhesive solution is cooled to 70°C, 10 mL of 0.1% calcium lactate aqueous solution is added to the compound adhesive solution to carry out cross-linking reaction. Then, citric acid is added to adjust the pH of the solution to 4.0 and cooled to 25°C to obtain saturated hydrogel.

[0085] Example 2

[0086] This embodiment provides a saturated hydrogel, the preparation method of which includes:

[0087] (1) Weigh 0.2 g gelling agent I (the mass ratio of gellan gum and sodium alginate is 10:2, of which the molecular weight of gellan gum is 230 kDa) and 0.87 g gelling agent II (the mass ratio of konjac gum and carrageenan is 2:1) and mix them evenly to prepare a compound powder. Heat 90 g of water to 50°C and add the compound powder to it while stirring. Stir for 6 h until completely dissolved. Then raise the temperature to 90°C and maintain it for 10 min for sterilization. Filter to remove insoluble matter and obtain the compound gel solution.

[0088] (2) After the compound adhesive solution is cooled to 50°C, 10 mL of 0.2% calcium lactate aqueous solution is added to the compound adhesive solution to carry out cross-linking reaction. Then, citric acid is added to adjust the pH of the solution to 3.1 and cooled to 25°C to obtain saturated hydrogel.

[0089] Example 3

[0090] This embodiment provides a saturated hydrogel, the preparation method of which includes:

[0091] (1) Weigh 0.3 g gelling agent I (the mass ratio of gellan gum and sodium alginate is 10:5, of which the molecular weight of gellan gum is 270 kDa) and 0.87 g gelling agent II (the mass ratio of konjac gum and carrageenan is 1:1.5) and mix them evenly to prepare a compound powder. Heat 90 g of water to 90°C and add the compound powder to it while stirring. Stir for 2 h until completely dissolved. Then raise the temperature to 100°C and maintain it for 8 min for sterilization. Filter to remove insoluble matter and obtain the compound gel solution.

[0092] (2) After the compound adhesive solution is cooled to 60°C, 10 mL of 0.02% calcium lactate aqueous solution is added to the compound adhesive solution to carry out cross-linking reaction. Then, citric acid is added to adjust the pH of the solution to 5, and the solution is cooled to 25°C to obtain saturated hydrogel.

[0093] Example 4

[0094] This embodiment provides a saturated hydrogel, the preparation method of which differs from that of Example 1 only in that the mass ratio of gellan gum and sodium alginate remains unchanged at 10:3 in step (1), and the total mass of gelling agent I is adjusted to 0.13 g. The remaining steps are consistent with those of Example 1.

[0095] Example 5

[0096] This embodiment provides a saturated hydrogel, the preparation method of which differs from that of Example 1 only in that the mass ratio of gellan gum and sodium alginate remains unchanged at 10:3 in step (1), and the total mass of gelling agent I is adjusted to 0.6 g. The remaining steps are consistent with those of Example 1.

[0097] Example 6

[0098] This embodiment provides a saturated hydrogel, the preparation method of which differs from that of Example 1 only in that the total mass of gelling agent I is kept constant in step (1), and gelling agent I is adjusted to a single gellan gel, while the other steps are consistent with those of Example 1.

[0099] Example 7

[0100] This embodiment provides a saturated hydrogel, the preparation method of which differs from that of Example 1 only in that the total mass of gelling agent I is kept constant in step (1), and the mass ratio of gellan gum and sodium alginate is adjusted to 3:10. The remaining steps are consistent with those of Example 1.

[0101] Example 8

[0102] This embodiment provides a saturated hydrogel, the preparation method of which differs from that of Example 1 only in that the total mass of gelling agent II is kept constant in step (1), and gelling agent II is adjusted to be a single konjac gum. The remaining steps are consistent with those of Example 1.

[0103] Example 9

[0104] This embodiment provides a saturated hydrogel, the preparation method of which differs from that of Example 1 only in that the total mass of gelling agent II is kept constant in step (1), and gelling agent II is adjusted to a single carrageenan. The remaining steps are consistent with those of Example 1.

[0105] Example 10

[0106] This embodiment provides a saturated hydrogel, the preparation method of which differs from that of Example 1 only in that the total volume of calcium lactate aqueous solution is kept constant at 10 mL in step (2), and the concentration of calcium lactate aqueous solution is adjusted to 0.01%, while the remaining steps are consistent with those of Example 1.

[0107] Example 11

[0108] This embodiment provides a saturated hydrogel, the preparation method of which differs from that of Example 1 only in that the total volume of calcium lactate aqueous solution is kept constant at 10 mL in step (2), and the concentration of calcium lactate aqueous solution is adjusted to 0.5%. The remaining steps are consistent with those of Example 1.

[0109] Example 12

[0110] This embodiment provides a saturated hydrogel, the preparation method of which differs from that of Example 1 only in that the calcium lactate aqueous solution is replaced with an equal volume and concentration of potassium chloride aqueous solution in step (2), and the remaining steps are consistent with those of Example 1.

[0111] Example 13

[0112] This embodiment provides a saturated hydrogel, the preparation method of which differs from that of Example 1 only in that citric acid is added in step (2) to adjust the pH of the solution to 3, and the remaining steps are consistent with those of Example 1.

[0113] Example 14

[0114] This embodiment provides a saturated hydrogel, the preparation method of which differs from that of Example 1 only in that citric acid is added in step (2) to adjust the pH of the solution to 7, and the remaining steps are consistent with those of Example 1.

[0115] Comparative Example 1

[0116] This comparative example provides a saturated hydrogel, which differs from Example 1 only in that the total mass of gelling agent II is kept constant in step (1), and gelling agent II is adjusted to konjac gum and xanthan gum (the mass ratio of konjac gum and xanthan gum is 1.5:1). The remaining steps are consistent with Example 1.

[0117] Comparative Example 2

[0118] This comparative example provides a saturated hydrogel, which differs from Example 1 only in that the total mass of gelling agent I is kept constant in step (1), and gelling agent I is adjusted to a single sodium alginate. All other steps are consistent with Example 1.

[0119] Comparative Example 3

[0120] This comparative example provides a saturated hydrogel, which differs from Example 1 only in that the total mass of gelling agent I is kept constant in step (1), and gelling agent I is adjusted to xanthan gum. All other steps are consistent with Example 1.

[0121] Comparative Example 4

[0122] This comparative example provides a saturated hydrogel, which differs from Example 1 only in that the heating temperature of the water in step (1) is adjusted from 70°C to 40°C, while the remaining steps are consistent with Example 1.

[0123] Application Example 1

[0124] This application example provides a satiating hydrogel jelly, the preparation method of which includes:

[0125] (1) Weigh 0.26 g gelling agent I (the mass ratio of gellan gum and sodium alginate is 10:3, of which the molecular weight of gellan gum is 250 kDa), 0.87 g gelling agent II (the mass ratio of konjac gum and carrageenan is 1.5:1), and 10 g erythritol and mix them evenly to prepare a compound powder. Heat 70 g of water to 70°C and add the compound powder to it while stirring. Stir for 3 h until completely dissolved. Then raise the temperature to 100°C and maintain it for 5 min for sterilization. Filter to remove insoluble matter and obtain the compound gel solution.

[0126] (2) After the compound gel solution is cooled to 70°C, 10 mL of 0.1% calcium lactate aqueous solution, 10 mL of grape juice, 0.02 g of fish collagen peptide, 0.03 g of bonito elastin peptide, 0.02 g of vitamin C, 0.0001 g of vitamin A and 0.002 g of vitamin E are added to the compound gel solution. Then, citric acid is added to adjust the pH of the solution to 4.0 and the solution is cooled to 25°C to obtain a saturated hydrogel jelly.

[0127] Application Example 2

[0128] This application example provides a satiating hydrogel jelly, which differs from application example 1 only in that the mass ratio of gellan gum and sodium alginate remains unchanged at 10:3 in step (1), and the total mass of gelling agent I is adjusted to 0.6 g. The remaining steps are consistent with application example 1.

[0129] Application Example 3

[0130] This application example provides a saturated hydrogel jelly, which differs from application example 1 only in that the total mass of gelling agent I is kept constant in step (1), and gelling agent I is adjusted to a single gellan gel. The remaining steps are consistent with application example 1.

[0131] Application Example 4

[0132] This application example provides a satiating hydrogel jelly, which differs from application example 1 only in that the total volume of the calcium lactate aqueous solution remains unchanged at 10 mL in step (2), and the concentration of the calcium lactate aqueous solution is adjusted to 0.5%. The remaining steps are consistent with application example 1.

[0133] Application Example 5

[0134] This application example provides a satiating hydrogel jelly, which differs from application example 1 only in that citric acid is added in step (2) to adjust the pH of the solution to 7, while the rest of the steps are consistent with application example 1.

[0135] Comparative Application Example 1

[0136] This comparative application example provides a satiating hydrogel jelly, which differs from application example 1 only in that the total mass of gelling agent I is kept constant in step (1), and gelling agent I is adjusted to a single sodium alginate. All other steps are consistent with application example 1.

[0137] Comparative Application Example 2

[0138] This comparative application example provides a commercially available zero-calorie konjac jelly from the brand "Xizhilang".

[0139] Test Example 1

[0140] Hydrogel swelling effect test:

[0141] (1) Samples to be tested: hydrogels obtained from each example and comparative example and commercially available jelly from comparative application example 2.

[0142] (2) Test method:

[0143] (2.1) Preparation of simulated gastric / intestinal fluid:

[0144] Simulated gastric juice: 0.35 g pepsin was dissolved in 100 mL of an aqueous solution containing 0.2% NaCl, and the pH was adjusted to 2 using 1 mol / L hydrochloric acid;

[0145] Simulated intestinal fluid: 0.1 g trypsin and 0.5 g bovine bile salts were dissolved in 100 mL of aqueous solution containing 0.5% NaCl, and the pH was adjusted to 8 using 1 mol / L NaOH aqueous solution.

[0146] (2.2) Simulated gastric juice test:

[0147] 300 mL of simulated gastric fluid was measured into a 500 mL beaker. The hydrogels obtained in each example and comparative example were cut into gel particles and wrapped with 500-mesh nylon mesh at 37°C and 100 rpm, secured with cable ties, and weighed (recorded as m0). The particles were then immersed in the simulated gastric fluid and stirred for 4 hours to simulate the gastric fluid treatment process. The gel particles were removed at 1, 2, 3, and 4 hours of stirring and allowed to stand for 5 minutes. The surface moisture was wiped dry with paper, and the particles were weighed (recorded as m). t (m) t After processing the gel particles in artificial gastric fluid (to measure the mass of the gel particles), they are returned to the artificial gastric fluid for further processing.

[0148] Calculate the mass change rate of the hydrogel at each time period: a t =(m0-m t ) / m0×100% (where a) t The mass change rate of gel particles treated in artificial gastric fluid (the result is shown in Table 2).

[0149] The elastic modulus G of the hydrogel after treatment in simulated gastric fluid for 4 h was determined using a rheometer. 胃 (The values ​​corresponding to an angular frequency of 10 rad / s were uniformly taken), and the results are shown in Table 2.

[0150] (2.3) Tests in simulated intestinal fluid:

[0151] Take the hydrogel tested in the simulated gastric fluid in step (2.2) and add it to a beaker containing 300 mL of simulated intestinal fluid. Continue stirring for 2 hours in a 37°C water bath at 100 rpm to simulate the intestinal fluid treatment process. At 5 hours and 6 hours (i.e., 1 hour and 2 hours after treatment in the intestinal fluid), remove the gel particles and let them stand for 5 minutes. Wipe the surface of the gel dry with paper and weigh it, recording the weight as m. t (m) t To determine the mass of gel particles co-processed in simulated gastric and intestinal fluids.

[0152] Calculate the mass change rate of the hydrogel at each time period: a t =(m0-m t) / m0×100% (where at is the mass change rate of gel particles treated with artificial gastric fluid and artificial intestinal fluid), the results are shown in Table 2;

[0153] The elastic modulus G of the hydrogel after treatment in artificial intestinal fluid for 2 h was determined using a rheometer. 肠 (The values ​​corresponding to an angular frequency of 10 rad / s were uniformly taken), and the results are shown in Table 2.

[0154] Table 2

[0155]

[0156] Note: NA indicates that the gel degrades rapidly in simulated gastric fluid and has poor occupancy; therefore, subsequent mass change tests and elastic modulus tests in simulated intestinal fluid were not performed.

[0157] As shown in Table 2, the complex obtained in Comparative Example 1 exhibited extremely poor stability in simulated gastric fluid, with a mass loss rate (a2) reaching as high as 94.62% after 2 hours of treatment. Furthermore, it failed to maintain its intact gel morphology (a3 and a4 are denoted as NA), therefore, simulated intestinal fluid testing was not conducted. This indicates that although replacing carrageenan with xanthan gum in the second network gel allows for cross-linking with calcium ions, the resulting network structure lacks sufficient mechanical strength and rapidly disintegrates in the acidic environment of the stomach, completely failing to meet the sustained occupancy requirements for long-lasting satiety. This result, compared with the data from Example 1, demonstrates that the combination of konjac gum and carrageenan is indispensable for constructing a second network with suitable elasticity and stability.

[0158] A comparison of the data from Example 1 with Comparative Examples 1-3 and Example 6 shows that, compared with hydrogels prepared using other polysaccharide molecules as raw materials (such as xanthan gum), the hydrogels prepared with gellan gum have better stability, can remain stable in gastrointestinal fluids, and have a higher elastic modulus. In addition, gellan gum and sodium alginate have a significant synergistic effect in improving the stability of the prepared hydrogels.

[0159] A comparison of the data from Examples 1 and 4-5 shows that when the content of gelling agent I is too high, the gel strength increases; when the content of gelling agent I is too low, the number of effective "connecting regions" in the gel network decreases, the hydrogel degrades rapidly in the digestive tract, and its mechanical properties are difficult to maintain.

[0160] A comparison of the data from Example 1 and Example 7 shows that when the mass ratio of gellan gum to sodium alginate is controlled within the range of 10:1 to 10:5, the prepared hydrogel has better stability and a higher elastic modulus.

[0161] A comparison of the data from Examples 1 and 8-9 shows that the combination of konjac knots and carrageenan to prepare the second network gel has a significant synergistic effect in improving the stability and elasticity of the prepared hydrogel.

[0162] A comparison of the data from Examples 1 and 10-12 shows that, compared to other cations, calcium ion crosslinking agents can better complex with gelling agent I, forming a more compact network structure and thus improving gel stability. Furthermore, excessively high crosslinking agent content reduces the gel's water absorption capacity and its swelling effect in gastric juice; conversely, excessively low crosslinking agent content leads to a significant decrease in the elastic modulus of the hydrogel in the gastrointestinal tract.

[0163] A comparison of the data from Example 1 and Examples 13-14 shows that the saturated hydrogel prepared under pH conditions of 3.5-6.5 can better maintain relative stability in the gastrointestinal fluid environment and has excellent elasticity.

[0164] A comparison of the data from Example 1 and Comparative Example 4 shows that when the heating temperature of gelling agent I, gelling agent II and water is controlled at 50-100℃, the prepared hydrogel has better stability, can remain stable in gastrointestinal fluid, and has a higher elastic modulus.

[0165] As can be seen from the data comparison between Example 1 and Comparative Application Example 2, the satiating hydrogel involved in this invention has significantly better stability compared to commercially available jelly products.

[0166] Test Example 2

[0167] Sensory evaluation test:

[0168] (1) Test samples: hydrogel jelly obtained from each application example and the comparative application example.

[0169] (2) Test method:

[0170] A panel of 20 sensory evaluators was invited to conduct sensory evaluations of the products. A double-blind method was used to score each sample, with each sample being scored three times. Sensory scoring criteria were developed based on the product’s color, flavor, taste, and texture. Overall acceptance was used as the overall evaluation index. The specific scoring criteria are shown in Table 3, and the test results are shown in Table 4.

[0171] Table 3

[0172]

[0173] Table 4

[0174]

[0175] As can be seen from the above data, the hydrogel jelly of the present invention has color, flavor, texture and consistency comparable to commercially available jelly products.

[0176] A comparison of the data from Application Example 1 and Application Example 2 shows that an excessively high content of gelling agent I will cause the prepared hydrogel jelly to become hard and will also have a significant impact on the flavor of the hydrogel jelly.

[0177] A comparison of the data from Application Example 1 and Application Example 4 shows that an excessively high content of crosslinking agent will cause the prepared hydrogel jelly to harden, collapse in shape, deteriorate in texture, and reduce flavor.

[0178] A comparison of the data from Application Example 1 and Application Example 5 shows that a pH value above 6.5 will result in a hydrogel jelly with an overly hard texture, an overly sweet taste, an unbalanced sourness, and an increased grainy texture.

[0179] The data from Application Example 1 and Comparative Application Example 1 show that when gelling agent I is sodium alginate alone, the prepared hydrogel jelly has a poor taste, increased astringency, poor stability, and collapses in shape.

[0180] As can be seen, the hydrogel jelly of this invention can greatly improve the satiety effect while still maintaining excellent color, flavor, texture and structure.

[0181] Test Example 3

[0182] Weight loss effect test:

[0183] (1) Samples to be tested: hydrogel jelly obtained by application example 1 and commercially available Xizhilang zero-calorie konjac jelly of comparison application example 2.

[0184] (2) Test method:

[0185] Twenty volunteers were recruited and randomly divided into two groups of 10 each. The experimental group consumed the hydrogel jelly (Example 1) 30 minutes before each of their two daily meals (lunch and dinner), while the control group consumed an equal amount of the zero-calorie konjac jelly (Example 2) at the same time.

[0186] Volunteers' weight was recorded every 15 days for 60 days, and the weight loss rate was calculated: TWL (%) = (initial weight - weight at follow-up) / initial weight × 100%.

[0187] Test results are as follows Figure 1 As shown, the satiating hydrogel jelly of this invention achieves a weight loss of approximately 8% within 60 days, demonstrating a good weight loss effect that is significantly superior to the weight loss capabilities of commercially available products.

[0188] The applicant declares that the technical solution of this invention is illustrated by the above embodiments, but this invention is not limited to the above embodiments, that is, it does not mean that this invention must rely on the above embodiments to be implemented. Those skilled in the art should understand that any improvements to this invention, equivalent substitutions of raw materials for the products of this invention, addition of auxiliary components, selection of specific methods, etc., all fall within the protection scope and disclosure scope of this invention.

[0189] The preferred embodiments of the present invention have been described in detail above. However, the present invention is not limited to the specific details in the above embodiments. Within the scope of the technical concept of the present invention, various simple modifications can be made to the technical solution of the present invention, and these simple modifications all fall within the protection scope of the present invention.

[0190] It should also be noted that the various specific technical features described in the above specific embodiments can be combined in any suitable manner without contradiction. In order to avoid unnecessary repetition, the present invention will not describe the various possible combinations separately.

Claims

1. A saturated hydrogel, characterized in that, The saturated hydrogel has an interpenetrating double network structure, which is formed by the interpenetration of a first network gel with a brittle structure and a second network gel with an elastic structure through physical cross-linking. The raw materials for preparing the first network gel include gelling agent I and cationic crosslinking agent. The first network gel is formed by gelling agent I and cationic crosslinking agent through ionic crosslinking. The mass ratio of gelling agent I to cationic crosslinking agent is 10:1-200:1, and the cationic crosslinking agent is a calcium ion crosslinking agent. The raw materials for preparing the second network gel include gelling agent II, which is hydrophilic, and the second network gel is formed by the physical interaction between molecular chains of gelling agent II; The gelling agent I includes gellan gum and sodium alginate, wherein the mass ratio of gellan gum to sodium alginate is 10:1-10:5; the gelling agent II includes a combination of konjac gum and carrageenan. The gellan gum is a low-acyl gellan gum with a molecular weight of 200-300 kDa; the saturated hydrogel is prepared by the following method, which includes the following steps: (1) Mix gelling agent I and gelling agent II with water, heat to 50-100℃ and stir until gelling agent I and gelling agent II dissolve to obtain a compound adhesive solution; (2) After the compound gel solution is cooled, it is mixed with a cationic crosslinking agent and the pH value of the solution is adjusted to 3.1-6.9 to obtain a saturated hydrogel.

2. The satiating hydrogel according to claim 1, characterized in that, The gelling agent I also includes chitosan and / or pectin.

3. The satiating hydrogel according to claim 1, characterized in that, The mass ratio of gelling agent I to gelling agent II is 1:10-10:

1.

4. A method for preparing a saturated hydrogel as described in any one of claims 1-3, characterized in that, The preparation method includes the following steps: (1) Mix gelling agent I and gelling agent II with water, heat to 50-100℃ and stir until gelling agent I and gelling agent II dissolve to obtain a compound adhesive solution; (2) After the compound gel solution is cooled, it is mixed with a cationic crosslinking agent and the pH value of the solution is adjusted to 3.1-6.9 to obtain a saturated hydrogel.

5. The preparation method according to claim 4, characterized in that, In step (2), after the compound adhesive solution is cooled and mixed with the cationic crosslinking agent, the mass percentage of gelling agent I is 0.03-0.5%.

6. A product with weight management effects, characterized in that, The product with weight management function includes the satiety hydrogel as described in any one of claims 1-3; The types of products with weight management effects include any one of jelly, beverage, or meal replacement powder.

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