A hydrogel with weight loss effect and its preparation method and application

Abstract

The present invention discloses a hydrogel with weight loss efficacy and its preparation method and application, relating to the technical field of hydrogel preparation, wherein the hydrogel is prepared by physical crosslinking of polysaccharide glue, cellulose or its derivatives and fiber powder, and the mixed solution of polysaccharide glue, cellulose or its derivatives and fiber powder is subjected to high-pressure homogenization treatment before physical crosslinking; the weight ratio of the polysaccharide glue, cellulose or its derivatives and fiber powder is 1:100-300:20-50; the polysaccharide glue is high-esterification pectin, and the ratio of its weight average molecular weight to number average molecular weight is 1.5-6; the fiber powder includes apple fiber powder and oat fiber powder, and the weight ratio of the apple fiber powder and oat fiber powder is 1:1-5. The present invention can improve the structural stability of the hydrogel, prevent the degradation or breakage of the hydrogel due to gastric juice and stomach extrusion, prolong the emptying time of the hydrogel in the stomach, and solve the problem of short duration of hydrogel satiety.

Description

Technical Field

[0001] The present invention relates to the technical field of hydrogel preparation, in particular to a hydrogel with weight loss efficacy, a preparation method and an application thereof. Background Art

[0002] The use of hydrogels as gastric fillers for weight loss has recently become a hot topic of research. Hydrogels can increase satiety while remaining undigested and absorbed in the digestive system, while also reducing food intake, ultimately achieving weight loss. Compared to other weight loss methods, such as diet, exercise, medication, and surgery, hydrogels offer advantages such as simplicity, safety, effectiveness, and widespread acceptance.

[0003] Currently, hydrogels are primarily prepared using physical and chemical crosslinking methods. Physical crosslinking, a process that connects hydrogel polymers through physical interactions to form a stable gel network, primarily involves cold-melt crosslinking, ionic crosslinking, and hydrogen bonding. Compared to chemical crosslinking, physical crosslinking offers advantages such as simpler and milder synthesis conditions, the absence of chemical crosslinking agents, and improved safety, making it particularly advantageous for applications in the food and biopharmaceutical sectors.

[0004] CN117179281A discloses a composite gel for weight control, its preparation method, and application. The composite gel comprises a polysaccharide gum comprising pectin and cellulose or its derivatives comprising sodium carboxymethyl cellulose. The composite gel is prepared by dissolving the raw materials in water and drying them at a temperature of 100-120°C for at least 1 hour to obtain the composite gel. The composite gel has a water absorption rate exceeding 50 times, requiring only a small amount to achieve a sense of fullness and enhance weight loss. However, its 30-minute storage modulus is relatively low, ranging from 1240 to 1560 Pa.

[0005] CN119409994A discloses a grease-absorbing hydrogel, its preparation method, and application. The hydrogel preparation method comprises: mixing a polysaccharide gel with water, followed by wet ultrafine grinding to obtain an ultrafine polysaccharide gel solution; using high-shear mixing to uniformly infiltrate the polysaccharide gel into cellulose or its derivatives to form micelles; then using microwave vacuum drying to cause the micelles to form a honeycomb structure; and finally, spraying the honeycomb micelles with high-pressure atomized ultrapure water and drying to obtain the hydrogel. The hydrogel of this invention has a water absorption rate exceeding 100 times, and a 30-minute storage modulus between 1350 Pa and 1570 Pa.

[0006] In summary, the hydrogels prepared by the existing physical cross-linking method generally have problems such as low storage modulus and insufficient structural stability, which leads to short gastric emptying time and poor persistence of satiety, and cannot meet the needs of weight loss. Summary of the Invention

[0007] In order to solve the above technical problems, the present invention provides a hydrogel with weight loss efficacy, a preparation method thereof, and an application thereof. The present invention can improve the structural stability of the hydrogel, prevent the hydrogel from being degraded or broken due to gastric juice and gastric extrusion, prolong the emptying time of the hydrogel in the stomach, and solve the problem of the short duration of satiety caused by the hydrogel.

[0008] In order to achieve the above object, the present invention adopts the following technical solutions:

[0009] In a first aspect, the present invention provides a hydrogel with weight loss efficacy, which is prepared by physically cross-linking polysaccharide gum, cellulose or its derivatives and fiber powder.

[0010] In some embodiments, the weight ratio of the polysaccharide gum, cellulose or its derivatives and fiber powder is 1:100-300:20-50; preferably 1:150-250:30-40; further preferably 1:200:30-40.

[0011] In some embodiments, the polysaccharide gum is high-esterification pectin, and the weight average molecular weight (Mw) of the high-esterification pectin is 90,000-180,000; the ratio of the weight average molecular weight (Mw) to the number average molecular weight (Mn) of the high-esterification pectin is 1.5-6; preferably 2-5; more preferably 3-4.

[0012] In some embodiments, the cellulose or its derivative is at least one of sodium carboxymethyl cellulose and hydroxyethyl cellulose; preferably sodium carboxymethyl cellulose.

[0013] In some embodiments, the weight average molecular weight (Mw) of the cellulose or its derivative is 20,000-80,000.

[0014] In some embodiments, the fiber powder includes apple fiber powder and oat fiber powder; preferably, the weight ratio of the apple fiber powder to the oat fiber powder is 1:1-5; more preferably 1:2-4; and even more preferably 1:3-4.

[0015] In a second aspect, the present invention provides a method for preparing the above-mentioned hydrogel, comprising the following steps:

[0016] (1) Dissolving and mixing polysaccharide gum, cellulose or its derivatives and fiber powder, and performing high-pressure homogenization to obtain a mixed solution;

[0017] (2) The mixed solution is concentrated and freeze-dried to obtain a dry product;

[0018] (3) The dried product is dried for a second time to obtain the hydrogel.

[0019] In some embodiments, the pressure of the high-pressure homogenization in step (1) is 10,000 psi-20,000 psi; preferably 15,000 psi-20,000 psi.

[0020] In some embodiments, the concentration in step (2) is to concentrate the mixture until the water content is 30%-40%, preferably 32%-38%, and more preferably 34%-36%.

[0021] In some embodiments, the freeze-drying temperature in step (2) is -20°C to -10°C; preferably -18°C to -12°C; and more preferably -15°C to -13°C.

[0022] In some embodiments, the moisture content of the dried product in step (2) is 15%-20%; preferably 16%-19%; and more preferably 17%-18%.

[0023] In some embodiments, the temperature of the secondary drying in step (3) is 100°C-120°C.

[0024] In some embodiments, the water content of the hydrogel in step (3) is less than 5%.

[0025] In a third aspect, the present invention provides the use of the above-mentioned hydrogel in the preparation of weight-loss foods, health products or medicines.

[0026] The hydrogel of the present invention has good water absorption and provides a good sense of fullness. At the same time, the hydrogel has a high storage modulus and good structural stability, which can prevent the hydrogel from being degraded or broken due to squeezing by gastric juice and gastric movement, effectively prolonging the emptying time of the hydrogel in the stomach, prolonging the fullness time, and achieving a better weight loss effect.

[0027] In a fourth aspect, the present invention provides an edible hydrogel composition comprising the above hydrogel and food additives.

[0028] In some embodiments, the food additive includes at least one of a preservative, a colorant, a flavoring agent, a color treatment agent, and a nutritional enhancer.

[0029] The beneficial effects of the present invention are:

[0030] (1) The hydrogel of the present invention is prepared by the physical entanglement, hydrogen bond crosslinking and cold-melt crosslinking between polysaccharide glue, cellulose or its derivatives and fiber powder, taking into account the water absorption and structural stability of the hydrogel and meeting the weight loss needs.

[0031] (2) The experiment found that the ratio of the weight average molecular weight (Mw) to the number average molecular weight (Mn) of the polysaccharide gum has an important influence on the structural stability of the hydrogel. When the ratio of the weight average molecular weight (Mw) to the number average molecular weight (Mn) is greater than 6 or less than 1.5, the storage modulus of the hydrogel is low, which cannot solve the problem of the short duration of the hydrogel's satiety.

[0032] (3) The use of high-pressure homogenization in the preparation process of the hydrogel of the present invention can make the raw materials more evenly dispersed, improve the uniformity of cross-linking, and expose more active sites, thereby promoting the occurrence of cross-linking reactions; the use of freeze-drying can cause free water to crystallize, thereby promoting the aggregation of polymer chains, reducing the distance between chains, and facilitating the interaction and cross-linking of polymer chains to form a stable three-dimensional network structure of the hydrogel. At the same time, freeze-drying can form a porous structure and increase the water absorption performance of the hydrogel; the use of high-temperature drying can enhance the cross-linking effect, forming a denser hydrogel network structure, and further improving the structural stability of the hydrogel.

[0033] (4) The experiment found that the homogeneous mixed liquid obtained by conventional mechanical stirring easily produces foam during the freeze-drying process after concentration, which cannot meet the subsequent production of the product. However, the present invention uses high-pressure homogenization to treat the mixed liquid, which can avoid the generation of foam during the subsequent freeze-drying process.

[0034] (5) The hydrogel of the present invention has good water absorption and provides a good sense of fullness. At the same time, the hydrogel has a high storage modulus and good structural stability, which can prevent the hydrogel from being degraded or broken due to squeezing by gastric juice and gastric movement, effectively prolonging the emptying time of the hydrogel in the stomach, prolonging the fullness time, and achieving a better weight loss effect. DETAILED DESCRIPTION

[0035] The following examples are only intended to help understand the method and core concepts of the present invention. It should be noted that those skilled in the art may make various improvements and modifications to the present invention without departing from the principles of the present invention, and such improvements and modifications also fall within the scope of protection of the claims of the present invention.

[0036] Therefore, the present invention will not be limited to the embodiments shown herein, but may be applied in a wider range consistent with the principles and novel features disclosed herein. Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which the present invention belongs.

[0037] As used in the specification and claims, the singular forms "a," "an," and "the" include plural referents unless the context clearly dictates otherwise.

[0038] All numerical values ​​or expressions used in this invention relating to component amounts, process conditions, etc. should be understood to be modified by "about" in all cases. The term "about" when referring to an amount or a numerical range means that the amount or numerical range referred to is an approximate value within the experimental variability (or within the statistical experimental error). In the present invention, the term "about" should have the meaning of within 10% of the specified value or range, preferably within 5%.

[0039] All ranges relating to the same component or property include endpoints, which can be independently combined. Since these ranges are continuous, they include every numerical value between the minimum and maximum values. It should also be understood that any numerical range cited herein is intended to include all subranges within that range.

[0040] The present invention does not limit the sources of the raw materials used. Unless otherwise specified, the raw materials used in the present invention are all common commercial products in the field of this technology. For example, the cellulose or its derivatives are purchased from Aladdin; the apple fiber powder is purchased from Pingdingshan Jinjing Biotechnology Co., Ltd., model AF-100, and the oat fiber powder is purchased from Jiangsu Yongrui Biological Co., Ltd., batch number 20240308-1; the polysaccharide gum is high-esterification pectin, and the weight average molecular weight and number average molecular weight of high-esterification pectin are determined by gel permeation chromatography of HPLC. The specific information is shown in Table 1 below.

[0041] Table 1

[0042]

[0043] Example 1 A hydrogel with weight loss efficacy

[0044] The hydrogel was prepared according to the formula in Table 2 using the following preparation method.

[0045] Table 2

[0046]

[0047] The preparation method is:

[0048] (1) Dissolve polysaccharide gum in water to obtain a 5% polysaccharide gum solution, dissolve cellulose or its derivatives in water to obtain a 10% cellulose solution, dissolve fiber powder in water, filter, and obtain a 2% fiber solution. Mix the three in proportion, and homogenize once under high pressure at 10,000 psi to obtain a mixed solution;

[0049] (2) The mixed solution is stirred and concentrated until the water content of the mixed solution is 30%, and then freeze-dried at -20°C to obtain a dry product with a water content of 15%;

[0050] (3) The dried product was dried again at 100°C to obtain a hydrogel with a water content of less than 5%.

[0051] Example 2 A hydrogel with weight loss efficacy

[0052] The hydrogel was prepared according to the formula in Table 3 using the following preparation method.

[0053] Table 3

[0054]

[0055] The preparation method is:

[0056] (1) Dissolve polysaccharide gum in water to obtain a 5% polysaccharide gum solution, dissolve cellulose or its derivative in water to obtain a 10% cellulose solution, dissolve fiber powder in water, filter, and obtain a 2% fiber solution. Mix the three in proportion, and homogenize once under high pressure at 20,000 psi to obtain a mixed solution;

[0057] (2) The mixed solution is stirred and concentrated until the water content of the mixed solution is 40%, and then freeze-dried at -10°C to obtain a dry product with a water content of 20%;

[0058] (3) The dried product was dried again at 120°C to obtain a hydrogel with a water content of less than 5%.

[0059] Example 3 A hydrogel with weight loss efficacy

[0060] The hydrogel was prepared according to the formula in Table 4 using the following preparation method.

[0061] Table 4

[0062]

[0063] The preparation method is:

[0064] (1) Dissolve polysaccharide gum in water to obtain a 5% polysaccharide gum solution, dissolve cellulose or its derivatives in water to obtain a 10% cellulose solution, dissolve fiber powder in water, filter, and obtain a 2% fiber solution. Mix the three in proportion, and homogenize once under high pressure at 15,000 psi to obtain a mixed solution;

[0065] (2) The mixed solution was stirred and concentrated until the water content of the mixed solution was 35%, and freeze-dried at -15°C to obtain a dry product with a water content of 17%;

[0066] (3) The dried product was dried again at 110°C to obtain a hydrogel with a water content of less than 5%.

[0067] Example 4 A hydrogel with weight loss efficacy

[0068] The hydrogel was prepared according to the formula in Table 5 using the following preparation method.

[0069] Table 5

[0070]

[0071] The preparation method is:

[0072] (1) Dissolve polysaccharide gum in water to obtain a 5% polysaccharide gum solution, dissolve cellulose or its derivatives in water to obtain a 10% cellulose solution, dissolve fiber powder in water, filter, and obtain a 2% fiber solution. Mix the three in proportion, and homogenize once under high pressure at 15,000 psi to obtain a mixed solution;

[0073] (2) The mixed solution was stirred and concentrated until the water content of the mixed solution was 32%, and freeze-dried at -18°C to obtain a dry product with a water content of 16%;

[0074] (3) The dried product was dried again at 110°C to obtain a hydrogel with a water content of less than 5%.

[0075] Example 5 A hydrogel with weight loss efficacy

[0076] The hydrogel was prepared according to the formula in Table 6 using the following preparation method.

[0077] Table 6

[0078]

[0079] The preparation method is:

[0080] (1) Dissolve polysaccharide gum in water to obtain a 5% polysaccharide gum solution, dissolve cellulose or its derivatives in water to obtain a 10% cellulose solution, dissolve fiber powder in water, filter, and obtain a 2% fiber solution. Mix the three in proportion, and homogenize once under high pressure at 15,000 psi to obtain a mixed solution;

[0081] (2) The mixed solution was stirred and concentrated until the water content of the mixed solution was 38%, and freeze-dried at -12°C to obtain a dry product with a water content of 19%;

[0082] (3) The dried product was dried again at 110°C to obtain a hydrogel with a water content of less than 5%.

[0083] Comparative Example 1 A hydrogel with weight loss effect

[0084] The difference between this comparative example and Example 3 is that the formula of the hydrogel is different. The specific formula is shown in Table 7.

[0085] Table 7

[0086]

[0087] The preparation method is basically the same as that of Example 3.

[0088] Comparative Example 2 A hydrogel with weight loss effect

[0089] The difference between this comparative example and Example 3 is that the formula of the hydrogel is different. The specific formula is shown in Table 8.

[0090] Table 8

[0091]

[0092] The preparation method is basically the same as that of Example 3.

[0093] Comparative Example 3 A hydrogel with weight loss effect

[0094] The difference between this comparative example and Example 3 is that the formula and preparation method of the hydrogel are different. The specific formula is shown in Table 9.

[0095] Table 9

[0096]

[0097] The specific preparation method is:

[0098] (1) Dissolve polysaccharide gum in water to obtain a 5% polysaccharide gum solution, dissolve cellulose or its derivatives in water to obtain a 10% cellulose solution, dissolve fiber powder in water, filter, and obtain a 2% fiber solution. Mix the three in proportion, and homogenize once under high pressure at 15,000 psi to obtain a mixed solution;

[0099] (2) The mixed solution is stirred and concentrated until the water content of the mixed solution is 35%, and then freeze-dried at -30°C to obtain a dry product with a water content of 25%;

[0100] (3) The dried product was dried again at 110°C to obtain a hydrogel with a water content of less than 5%.

[0101] Comparative Example 4: A hydrogel with weight loss efficacy

[0102] This comparative example has the same formula as that of Example 3, except that the preparation method is different. The specific preparation method is as follows:

[0103] (1) Dissolve polysaccharide gum in water to obtain a 5% polysaccharide gum solution, dissolve cellulose or its derivatives in water to obtain a 10% cellulose solution, dissolve fiber powder in water, filter, and obtain a 2% fiber solution. Mix the three in proportion, and homogenize once under high pressure at 15,000 psi to obtain a mixed solution;

[0104] (2) The mixed solution was dried at 30°C to obtain a dry product with a water content of 17%;

[0105] (3) The dried product was dried again at 110°C to obtain a hydrogel with a water content of less than 5%.

[0106] Comparative Example 5 A hydrogel with weight loss effect

[0107] This comparative example has the same formula as that of Example 3, except that the preparation method is different. The specific preparation method is as follows:

[0108] (1) Dissolve polysaccharide gum in water to obtain a 5% polysaccharide gum solution, dissolve cellulose or its derivatives in water to obtain a 10% cellulose solution, dissolve fiber powder in water, filter, and obtain a 2% fiber solution. Mix the three in proportion, and homogenize once under high pressure at 15,000 psi to obtain a mixed solution;

[0109] (2) The mixture was freeze-dried at -15°C to obtain a dry product with a water content of 17%;

[0110] (3) The dried product was dried again at 110°C to obtain a hydrogel with a water content of less than 5%.

[0111] Comparative Example 6 A hydrogel with weight loss effect

[0112] This comparative example has the same formula as that of Example 3, except that the preparation method is different. The specific preparation method is as follows:

[0113] (1) Dissolve polysaccharide gum in water to obtain a 5% polysaccharide gum solution, dissolve cellulose or its derivative in water to obtain a 10% cellulose solution, dissolve fiber powder in water, filter, and obtain a 2% fiber solution. Mix the three in proportion and stir to obtain a mixed solution;

[0114] (2) The mixed solution was stirred and concentrated until the water content of the mixed solution was 35%, and freeze-dried at -15°C to obtain a dry product with a water content of 17%;

[0115] (3) The dried product was dried again at 110°C to obtain a hydrogel with a water content of less than 5%.

[0116] Effect Example 1: Determination of water absorption multiple

[0117] The hydrogel prepared in the example or comparative example was crushed into a size of 20-50 mesh, 1 g was placed in a medium (the mass ratio of artificial gastric juice: water was 1:8, and the artificial gastric juice was configured according to the 2020 edition of the Chinese Pharmacopoeia), and kept warm at 37°C for 0.5 h. The water was filtered out with a stainless steel sieve and then weighed to obtain the weight m1 of the hydrogel after absorption. The water absorption multiple was calculated, and the water absorption multiple = (m1-1) / 1.

[0118] The results are shown in Table 10.

[0119] Table 10

[0120]

[0121] Note: Comparative Examples 5 and 6 produced a large amount of foam during the freeze-drying process, which did not meet the subsequent processing requirements and did not require testing.

[0122] Effect Example 2 Storage Modulus Measurement

[0123] The hydrogel prepared in the embodiment or comparative example was crushed into a size of 20-50 mesh, 1 g was placed in a medium (the mass ratio of artificial gastric juice: water was 1:8, and the artificial gastric juice was configured according to the 2020 edition of the Chinese Pharmacopoeia), and kept warm at 37°C for 4 h. After filtering out the water with a stainless steel sieve, the water on the surface of the sample was wiped clean and placed between the parallel plates (25 mm) of a rotational rheometer. The tension was fixed at 0.5%, the frequency range was fixed at 1 rad / s-50 rad / s, and the storage modulus corresponding to a frequency of 10 rad / s was taken as the storage modulus of the sample.

[0124] The results are shown in Table 11.

[0125] Table 11

[0126]

[0127] The above further describes the present invention in conjunction with specific embodiments. However, these embodiments are merely exemplary and do not constitute any limitation on the scope of the present invention. It should be understood by those skilled in the art that the details and forms of the technical solutions of the present invention may be modified or replaced without departing from the spirit and scope of the present invention, and such modifications and replacements shall fall within the scope of protection of the present invention.

Claims

1. A hydrogel with weight loss effect, characterized in that: It is prepared by physically cross-linking polysaccharide gum, cellulose derivatives and fiber powder, and before the physical cross-linking, the mixed liquid of polysaccharide gum, cellulose derivatives and fiber powder is subjected to high-pressure homogenization treatment; The weight ratio of the polysaccharide gum, cellulose derivative and fiber powder is 1:100-300:20-50; The polysaccharide gum is high-esterification pectin, and the ratio of the weight average molecular weight to the number average molecular weight of the high-esterification pectin is 1.5-6; The cellulose derivative is at least one of sodium carboxymethyl cellulose and hydroxyethyl cellulose; The fiber powder comprises apple fiber powder and oat fiber powder, wherein the weight ratio of the apple fiber powder to the oat fiber powder is 1:1-5; The preparation method of the hydrogel comprises the following steps: (1) Dissolving and mixing polysaccharide gum, cellulose derivatives and fiber powder, and homogenizing under high pressure to obtain a mixed solution; (2) The mixed solution is concentrated and freeze-dried to obtain a dry product; (3) secondary drying of the dried product to obtain the hydrogel; The concentration in step (2) is to concentrate the mixed solution until the water content is 30%-40%, the freeze-drying temperature is -20°C to -10°C, and the water content of the dried product is 15%-20%; The temperature of the secondary drying in step (3) is 100°C-120°C.

2. The hydrogel according to claim 1, wherein The weight ratio of the polysaccharide gum, the cellulose derivative and the fiber powder is 1:150-250:30-40; the weight ratio of the apple fiber powder and the oat fiber powder is 1:2-4.

3. The method for preparing the hydrogel according to any one of claims 1 to 2, characterized in that: The steps include: (1) Dissolving and mixing polysaccharide gum, cellulose derivatives and fiber powder, and homogenizing under high pressure to obtain a mixed solution; (2) The mixed solution is concentrated and freeze-dried to obtain a dry product; (3) The dried product is dried for a second time to obtain the hydrogel.

4. The preparation method according to claim 3, characterized in that The pressure of the high-pressure homogenization in step (1) is 10,000 psi-20,000 psi.

5. The preparation method according to claim 3, characterized in that The concentration in step (2) is to concentrate the mixture until the water content is 30%-40%, the freeze-drying temperature is -20°C to -10°C, and the water content of the dried product is 15%-20%.

6. The preparation method according to claim 3, characterized in that The temperature of the secondary drying in step (3) is 100°C-120°C.

7. Use of the hydrogel according to any one of claims 1 to 2 or the hydrogel prepared by the preparation method according to any one of claims 3 to 6 in the preparation of weight-loss foods, health products or medicines.

8. An edible hydrogel composition, characterized in that The invention comprises the hydrogel according to any one of claims 1 to 2 or the hydrogel prepared by the preparation method according to any one of claims 3 to 6 and a food additive.

9. The edible hydrogel composition according to claim 8, wherein The food additives include at least one of preservatives, colorants, flavorings, color treatment agents and nutrition enhancers.

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