Hydrogel with weight losing effect as well as preparation method and application thereof

Abstract

The invention discloses hydrogel with a weight losing effect and a preparation method and application thereof, and relates to the technical field of hydrogel preparation, the hydrogel is prepared from polysaccharide gum, cellulose or derivatives thereof and fiber powder through physical crosslinking, a mixed solution of the polysaccharide gum, the cellulose or the derivatives thereof and the fiber powder is subjected to high-pressure homogenization treatment before physical crosslinking; the weight ratio of the polysaccharide gum to the cellulose or the derivative thereof to the fiber powder is 1: (100-300): (20-50); the polysaccharide gum is high-esterification-degree pectin, and the ratio of the weight-average molecular weight to the number-average molecular weight of the polysaccharide gum is 1.5-6; the fiber powder comprises apple fiber powder and oat fiber powder, and the weight ratio of the apple fiber powder to the oat fiber powder is 1: (1-5). The structural stability of the hydrogel can be improved, the hydrogel is prevented from being degraded or broken due to gastric juice and stomach extrusion, the emptying time of the hydrogel in the stomach is prolonged, and the problem that the duration of satiety of the hydrogel is short is solved.

Description

Technical Field

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

[0002] The application of hydrogel as a gastric filler in the field of weight loss is a hot topic in recent research. Hydrogel can increase satiety and is not digested and absorbed in the digestive system. It can also reduce the intake of other foods to achieve the purpose of weight loss. Compared with other weight loss methods, such as dieting, exercise, drugs and surgery, it has the advantages of being simple, safe, effective and highly accepted.

[0003] At present, the preparation methods of hydrogel mostly adopt physical cross-linking and chemical cross-linking. Among them, the physical cross-linking method is the process of connecting the polymers of the hydrogel together through physical interaction to form a stable gel network structure, which mainly includes cold-melt cross-linking, ionic cross-linking and hydrogen bond cross-linking. Compared with chemical cross-linking, physical cross-linking has the advantages of relatively simple synthesis conditions, mild conditions, no need for chemical cross-linking agents, good safety, etc., which is more advantageous in the application of food and biomedicine.

[0004] CN117179281A discloses a composite gel for weight control and its preparation method and application, the composite gel comprises polysaccharide gum and cellulose or its derivatives, the polysaccharide gum comprises pectin, the cellulose or its derivatives comprises sodium carboxymethyl cellulose, and the preparation method of the composite gel comprises: dissolving the raw materials in water, drying at a drying temperature of 100-120°C for more than 1h, and obtaining the composite gel. The composite gel of the invention has a water absorption multiple of more than 50 times, and only a small amount of intake is required to obtain a sense of fullness, thereby improving the weight loss effect, but its 30min storage modulus is relatively low, between 1240-1560Pa.

[0005] CN119409994A discloses a hydrogel for absorbing oil and fat, and its preparation method and application. The preparation method of the hydrogel is as follows: a polysaccharide glue is mixed with water and then wet-milled to obtain an ultrafine polysaccharide glue solution, high shear mixing is used to make the polysaccharide glue evenly penetrate into the interior of cellulose or its derivatives to form micelles, microwave vacuum drying is used to promote the micelles to form a honeycomb structure, and finally the honeycomb micelles are sprayed with ultrapure water with high pressure atomization and dried to obtain a hydrogel. The hydrogel of the invention has a water absorption multiple of more than 100 times, and a 30-min storage modulus of between 1350Pa and 1570Pa.

[0006] In summary, the hydrogels prepared by the existing physical cross-linking method generally have the problems of low storage modulus and insufficient structural stability, which leads to a 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 and a preparation method and application thereof. 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 satiety of the hydrogel.

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

[0009] 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.

[0010] 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; and more preferably 3-4.

[0011] In some embodiments, the cellulose or its derivative is at least one of sodium carboxymethyl cellulose and hydroxyethyl cellulose; preferably sodium carboxymethyl cellulose.

[0012] In some embodiments, the weight average molecular weight (Mw) of the cellulose or its derivative is 20,000-80,000.

[0013] 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.

[0014] In a second aspect, the present invention provides a method for preparing the above hydrogel, comprising the following steps: (1) dissolving and mixing polysaccharide gum, cellulose or its derivatives and fiber powder, and subjecting them to high pressure homogenization to obtain a mixed solution; (2) Concentrating the mixed solution and freeze-drying it to obtain a dry product; (3) The dried product is dried again to obtain the hydrogel.

[0015] 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.

[0016] In some embodiments, the concentration in step (2) is to concentrate the mixed solution until the water content is 30%-40%, preferably 32%-38%, and more preferably 34%-36%.

[0017] 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.

[0018] In some embodiments, the moisture content of the dried product in step (2) is 15%-20%, preferably 16%-19%, and more preferably 17%-18%.

[0019] In some embodiments, the secondary drying temperature in step (3) is 100°C-120°C.

[0020] In some embodiments, the water content of the hydrogel in step (3) is less than 5%.

[0021] In a third aspect, the present invention provides the use of the above hydrogel in the preparation of weight loss foods, health products or medicines.

[0022] The hydrogel of the present invention has good water absorption and 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.

[0023] In a fourth aspect, the present invention provides an edible hydrogel composition, comprising the above hydrogel and a food additive.

[0024] In some embodiments, the food additive includes at least one of a preservative, a colorant, a flavoring agent, a color treatment agent, and a nutrition enhancer.

[0025] The beneficial effects of the present invention are: (1) The hydrogel of the present invention is prepared by 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 needs of weight loss.

[0026] (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 satiety of the hydrogel.

[0027] (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 to promote the occurrence of cross-linking reactions; 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; high-temperature drying can enhance the cross-linking effect, forming a denser hydrogel network structure, and further improving the structural stability of the hydrogel.

[0028] (4) The experiment found that the homogenous mixed liquid obtained by conventional mechanical stirring is prone to foaming during the freeze-drying process after concentration, which cannot meet the subsequent production of the product. 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.

[0029] (5) The hydrogel of the present invention has good water absorption and 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

[0030] The following examples are only used to help understand the method of the present invention and its core concept. It should be noted that, for those skilled in the art, without departing from the principles of the present invention, several improvements and modifications may be made to the present invention, and these improvements and modifications also fall within the scope of protection of the claims of the present invention.

[0031] Therefore, the present invention will not be limited to these embodiments shown in this article, but can be applied to 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 those of ordinary skill in the art to which the present invention belongs.

[0032] As used in the specification and claims, the singular forms "a", "an", and "the" include plural referents unless the context clearly dictates otherwise.

[0033] All numerical values ​​or expressions used in the present 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 indicated amount or numerical range 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%, preferably within 5% of the specified value or range.

[0034] All ranges involving 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 in the present invention is intended to include all subranges within the range.

[0035] The present invention does not limit the source 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. Exemplarily, 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.

[0036] Table 1

[0037] Example 1 A hydrogel with weight loss effect The hydrogel was prepared according to the formula in Table 2 using the following preparation method.

[0038] Table 2

[0039] The preparation method is: (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 to obtain a 2% fiber solution, mix the three in proportion, and perform high-pressure homogenization treatment at 10,000 psi once to obtain a mixed solution; (2) The mixed solution is stirred and concentrated until the water content of the mixed solution is 30%, and freeze-dried at -20°C to obtain a dry product with a water content of 15%; (3) The dried product is secondary dried at 100°C to obtain a hydrogel with a water content of less than 5%.

[0040] Example 2 A hydrogel with weight loss effect The hydrogel was prepared according to the formulation in Table 3 using the following preparation method.

[0041] Table 3

[0042] The preparation method is: (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 to obtain a 2% fiber solution, mix the three in proportion, and perform high-pressure homogenization treatment at 20,000 psi once to obtain a mixed solution; (2) The mixed solution is stirred and concentrated until the water content of the mixed solution is 40%, and freeze-dried at -10°C to obtain a dry product with a water content of 20%; (3) The dried product is secondary dried at 120°C to obtain a hydrogel with a water content of less than 5%.

[0043] Example 3 A hydrogel with weight loss effect The hydrogel was prepared according to the formulation in Table 4 using the following preparation method.

[0044] Table 4

[0045] The preparation method is: (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 to obtain a 2% fiber solution, mix the three in proportion, and perform high pressure homogenization treatment at 15000 psi once to obtain a mixed solution; (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%; (3) The dried product was secondary dried at 110°C to obtain a hydrogel with a water content of less than 5%.

[0046] Example 4 A hydrogel with weight loss effect The hydrogel was prepared according to the formulation in Table 5 using the following preparation method.

[0047] Table 5

[0048] The preparation method is: (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 to obtain a 2% fiber solution, mix the three in proportion, and perform high pressure homogenization treatment at 15000 psi once to obtain a mixed solution; (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%; (3) The dried product was secondary dried at 110°C to obtain a hydrogel with a water content of less than 5%.

[0049] Example 5 A hydrogel with weight loss effect The hydrogel was prepared according to the formulation in Table 6 using the following preparation method.

[0050] Table 6

[0051] The preparation method is: (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 to obtain a 2% fiber solution, mix the three in proportion, and perform high pressure homogenization treatment at 15000 psi once to obtain a mixed solution; (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%; (3) The dried product was secondary dried at 110°C to obtain a hydrogel with a water content of less than 5%.

[0052] Comparative Example 1 A hydrogel with weight loss effect 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.

[0053] Table 7

[0054] The preparation method is basically the same as that of Example 3.

[0055] Comparative Example 2 A hydrogel with weight loss effect 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.

[0056] Table 8

[0057] The preparation method is basically the same as that of Example 3.

[0058] Comparative Example 3 A hydrogel with weight loss effect 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.

[0059] Table 9

[0060] The specific preparation method is: (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 to obtain a 2% fiber solution, mix the three in proportion, and perform high pressure homogenization treatment at 15000 psi once to obtain a mixed solution; (2) The mixed solution is stirred and concentrated until the water content of the mixed solution is 35%, and freeze-dried at -30°C to obtain a dry product with a water content of 25%; (3) The dried product was secondary dried at 110°C to obtain a hydrogel with a water content of less than 5%.

[0061] Comparative Example 4 A hydrogel with weight loss effect 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: (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 to obtain a 2% fiber solution, mix the three in proportion, and perform high pressure homogenization treatment at 15000 psi once to obtain a mixed solution; (2) The mixed solution was dried at 30°C to obtain a dry product with a water content of 17%; (3) The dried product was secondary dried at 110°C to obtain a hydrogel with a water content of less than 5%.

[0062] Comparative Example 5 A hydrogel with weight loss effect 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: (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 to obtain a 2% fiber solution, mix the three in proportion, and perform high pressure homogenization treatment at 15000 psi once to obtain a mixed solution; (2) The mixed solution was freeze-dried at -15°C to obtain a dry product with a water content of 17%; (3) The dried product was secondary dried at 110°C to obtain a hydrogel with a water content of less than 5%.

[0063] Comparative Example 6 A hydrogel with weight loss effect 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: (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, and mix the three in proportion to obtain a mixed solution; (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%; (3) The dried product was secondary dried at 110°C to obtain a hydrogel with a water content of less than 5%.

[0064] Effect Example 1 Determination of water absorption multiple The hydrogel prepared in the embodiment or comparative example was crushed into 20-50 meshes, 1 g was placed in a medium (the mass ratio of artificial gastric juice: water was 1:8, and the artificial gastric juice was prepared according to the Chinese Pharmacopoeia 2020 edition), kept warm at 37°C for 0.5 h, filtered out the water with a stainless steel sieve, and weighed to obtain the weight of the hydrogel after absorption: m 1 , calculate the water absorption multiple, water absorption multiple = (m 1 -1) / 1.

[0065] The results are shown in Table 10.

[0066] Table 10

[0067] Note: Comparative Examples 5 and 6 do not need to be tested because a large amount of foam is produced during the freeze-drying process and does not meet the subsequent processing requirements.

[0068] Effect Example 2 Storage modulus measurement The hydrogel prepared in the embodiment or comparative example was crushed to a size between 20 and 50 meshes, 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 value corresponding to the frequency of 10 rad / s was taken as the storage modulus of the sample.

[0069] The results are shown in Table 11.

[0070] Table 11

[0071] The above is a further description of the present invention in conjunction with specific embodiments, but 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 solution of the present invention may be modified or replaced without departing from the spirit and scope of the present invention, but these modifications and replacements all fall within the scope of protection of the present invention.

Claims

1. A hydrogel with weight loss effect, characterized in that: The polysaccharide gum, cellulose or its derivatives and fiber powder are prepared by physical cross-linking, and before the physical cross-linking, the mixed liquid of the polysaccharide gum, cellulose or its derivatives and fiber powder is subjected to high-pressure homogenization treatment; The weight ratio of the polysaccharide gum, cellulose or its derivatives and fiber powder is 1:100-300:20-50; The polysaccharide gum is high-esterification degree pectin, and the ratio of the weight average molecular weight to the number average molecular weight of the high-esterification degree pectin is 1.5-6; The fiber powder includes apple fiber powder and oat fiber powder, and the weight ratio of the apple fiber powder to the oat fiber powder is 1:1-5.

2. The hydrogel according to claim 1, characterized in that The cellulose or its derivative is at least one of sodium carboxymethyl cellulose and hydroxyethyl cellulose.

3. The hydrogel according to claim 1, characterized in that The weight ratio of the polysaccharide gum, cellulose or its derivatives and fiber powder is 1:150-250:30-40; the weight ratio of the apple fiber powder and oat fiber powder is 1:2-4.

4. The method for preparing the hydrogel according to any one of claims 1 to 3, characterized in that: The steps include: (1) dissolving and mixing polysaccharide gum, cellulose or its derivatives and fiber powder, and subjecting them to high pressure homogenization to obtain a mixed solution; (2) Concentrating the mixed solution and freeze-drying it to obtain a dry product; (3) The dried product is dried again to obtain the hydrogel.

5. The preparation method according to claim 4, characterized in that: The pressure of the high-pressure homogenization in step (1) is 10000psi-20000psi.

6. The preparation method according to claim 4, characterized in that: 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 in step (2) is 15%-20%.

7. The preparation method according to claim 4, characterized in that: The secondary drying temperature in step (3) is 100°C-120°C.

8. Use of the hydrogel according to any one of claims 1 to 3 or the hydrogel prepared by the preparation method according to any one of claims 4 to 7 in the preparation of weight-loss foods, health products or medicines.

9. An edible hydrogel composition, characterized in that The invention comprises the hydrogel according to any one of claims 1 to 3 or the hydrogel prepared by the preparation method according to any one of claims 4 to 7 and a food additive.

10. The edible hydrogel composition according to claim 9, characterized in that The food additives include at least one of preservatives, colorants, flavoring agents, color treatment agents and nutrition enhancers.

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