Hydrogel composition with enhanced water absorption, and preparation method therefor and use thereof

Abstract

A hydrogel composition with enhanced water absorption, and a preparation method therefor and the use thereof. The raw materials comprise a carboxymethyl cellulose raw material, an alginic acid raw material, a soluble raw material, a calcium source and silicon dioxide. The composition is prepared by means of using the chelation between calcium ions and the alginic acid raw material. On the one hand, the carboxymethyl cellulose raw material is used to reduce the sensitivity of the chelation, thereby preventing a decline in water absorption of the composition; on the other hand, by means of adding the soluble raw material, which is dispersed in a solid hydrogel composition, after the solid hydrogel composition comes into contact with water, the soluble raw material in the composition exhibits a good water absorption capacity, which can improve the ability of water to penetrate the interior of the composition, thereby improving the water absorption performance of the composition. In addition, silicon dioxide can enhance the elastic modulus of the hydrogel.

Description

Hydrogel composition for enhanced water absorption, and preparation method and application thereof

[0001] Cross-reference to related applications

[0002] The present disclosure claims priority to the application with the application number 2024108373526 and the title "Hydrogel composition for enhanced water absorption, and preparation method and application thereof" filed with the China Patent Office on June 26, 2024, the entire content of which is incorporated herein by reference. TECHNICAL FIELD

[0003] The present disclosure relates to the field of food technology, in particular, to a hydrogel composition for enhanced water absorption, and a preparation method and application thereof. BACKGROUND

[0004] With the development of society and the improvement of living standards, obesity and diabetes have become a serious global health problem. At present, the treatment methods for weight loss and diabetes mainly include drug treatment, diet control and surgery, etc. Among them, surgery is an effective treatment method, but the risk of surgery is large and the recovery time is long; and in the process of weight loss by drug treatment, there is often a problem of weight rebound after drug withdrawal, or the drug itself has some side effects; diet control is a safe and effective non-surgical treatment for weight loss, but weight lossers need to have strong self-control, so it is often difficult to achieve long-term and effective weight loss. In order to assist weight lossers in controlling their diet, weight lossers are usually asked to eat some products with strong satiety, so it is of great significance to develop a safe and effective product to assist people in losing weight.

[0005] The prior art proposes some space-occupying gels in the digestive tract to increase satiety and thus achieve the purpose of weight loss. However, in order to ensure that the existing space-occupying gels in the digestive tract have a high crosslinking degree, the concentration of the polymer needs to be strictly controlled, so the precision requirement of the process in the preparation process is high, resulting in difficult quality control of the space-occupying gels in the digestive tract.

[0006] In view of this, the present disclosure is proposed. SUMMARY

[0007] The purpose of the present disclosure is to provide a hydrogel composition for enhanced water absorption, and a preparation method and application thereof.

[0008] The present disclosure is implemented as follows:

[0009] In a first aspect, the present disclosure provides a hydrogel composition for enhanced water absorption, and the raw materials include carboxymethyl cellulose raw materials, alginic acid raw materials, easily soluble raw materials, a calcium source and silicon dioxide, and the mass relationship of each component in the raw materials satisfies:

[0010] W1 = m2 / (m1+m2) x 100%, and 10%≤W1≤70%;

[0011] W2 = m5 / (m1+m2+m5+m6) x 100%, and 0%≤W2≤40%;

[0012] W3 = m6 / (m1+m2+m5+m6) x 100%, and 5%≤W2≤30%;

[0013] W4 = (m1+m2) / (m1+m2+m5+m6) x 100%, and 55%≤W2≤90%;

[0014] f = m4 / m3, and 0.1≤f≤2.0;

[0015] wherein m1 is the mass of the carboxymethyl cellulose raw material, m2 is the mass of the alginic acid raw material, m3 is the mass of the carboxyl in the alginic acid raw material, m4 is the mass of Ca 2+ in the calcium source, m5 is the mass of the silicon dioxide, and m6 is the mass of the easily soluble raw material.

[0016] In a second aspect, the present disclosure provides a preparation method of the composition of any one of the preceding embodiments, comprising dispersing the carboxymethyl cellulose raw material, the alginic acid raw material, and the silicon dioxide in a solution, mixing uniformly, and then drying to obtain A material, and then mixing the A material, the calcium source, and the easily soluble raw material to obtain the composition.

[0017] In a third aspect, the present disclosure provides use of the composition of any one of the preceding embodiments in the preparation of a digestive tract occupying product.

[0018] The present disclosure has the following beneficial effects:

[0019] The present disclosure provides a kind of water-absorbing reinforced hydrogel composition and its preparation method and application, the composition can quickly form hydrogel in water, wherein, alginic acid raw material is physically crosslinked with calcium ion, carboxymethyl cellulose raw material can reduce the sensitivity of alginic acid raw material to calcium ion, so that the prepared hydrogel greatly improves the medium water absorption while retaining certain hydrogel elastic modulus, in addition, the raw material also includes soluble raw material, soluble raw material is dispersed in solid hydrogel composition, when solid hydrogel composition meets water, the soluble raw material in the composition has better water absorption capacity, so it can improve the ability of water into the composition, thereby improving the water absorption performance of the composition, the volume expansion ability of the composition after water absorption is improved, which is more conducive to occupying in the digestive tract, after adding silicon dioxide, the strength of the hydrogel can also be enhanced.The process of forming hydrogel of the composition of the present disclosure is a physical crosslinking method, no chemical reaction occurs, the hydrogel prepared from the composition has high strength, high elastic modulus and excellent water absorption performance, after entering the digestive tract, it can occupy the stomach volume in the stomach, reduce food intake to achieve the purpose of weight loss and blood sugar control. DETAILED DESCRIPTION

[0020] The embodiments of the present disclosure will be described in detail below with examples, but those skilled in the art will understand that the following examples are only for illustration of the present disclosure and should not be regarded as limiting the scope of the present disclosure. If no specific conditions are specified in the examples, the conventional conditions or the conditions recommended by the manufacturer are used. If no manufacturer of the reagent or instrument is specified, it is a conventional product that can be obtained by market purchase.

[0021] The endpoints of the ranges and any values disclosed in the present disclosure are not limited to the precise values stated. The ranges and values should be interpreted as being approximate. Values that are near to the endpoints of the ranges and values are to be interpreted as being within the scope of the ranges. The endpoints of the ranges and values are not to be construed as being required.

[0022] The inventors found that the prior art uses citric acid to chemically crosslink low molecular weight sodium carboxymethyl cellulose to obtain a hydrogel with certain strength and water absorption performance, which can increase satiety in the stomach and achieve the purpose of weight loss. However, the preparation process of this hydrogel uses chemical crosslinking, which utilizes the hydroxyl groups in sodium carboxymethyl cellulose to react with citric acid to form ester bonds, thereby achieving the connection between molecules and obtaining a hydrogel product. However, in order to ensure the crosslinking density, the concentration of carboxymethyl cellulose in the reaction process needs to be strictly controlled, resulting in a complex preparation process, low yield and high cost.

[0023] Based on existing chemical cross-linking methods, the inventors have discovered a key issue in the practical application of gastric volume-carrying hydrogels: the water absorption rate and elastic modulus of the hydrogel are often contradictory. Generally, when the water absorption rate of the medium increases, the hydrogel becomes softer, resulting in a lower elastic modulus and poorer mechanical properties. Under the peristalsis and pressure of the digestive tract, the satiating sensation produced by the hydrogel is easily lost. Conversely, when the water absorption rate decreases, the hydrogel becomes harder, resulting in a higher elastic modulus and better mechanical properties. However, the reduced water absorption rate leads to a smaller volume, which also reduces the satiating sensation.

[0024] In addition, existing hydrogels can generally only provide good volume filling effect in the stomach. When the hydrogel reaches the intestines, the high pH value of the intestinal fluid will cause the gel to expand further and lose a large part of its strength. It will also be unable to exert pressure on the intestines, ultimately leading to a shortened duration of satiety.

[0025] Therefore, this disclosure not only requires the development of a simple process, but also the simultaneous improvement of the hydrogel's medium water absorption rate and elastic modulus, as well as the improvement of the hydrogel's tolerance under different pH and pressure conditions. Based on this, the inventors propose the following solution.

[0026] In a first aspect, this disclosure provides a hydrogel composition for enhanced water absorption, the raw materials of which include carboxymethyl cellulose raw materials, alginate raw materials, readily soluble raw materials, calcium source and silica, and the mass relationship of each component in the raw materials satisfies the following:

[0027] W1 = m2 / (m1+m2)×100%, and 10%≤W1≤70%;

[0028] W2 = m5 / (m1+m2+m5+m6)×100%, and 0%≤W2≤40%;

[0029] W3 = m6 / (m1+m2+m5+m6)×100%, and 5%≤W2≤30%;

[0030] W4 = (m1 + m2) / (m1 + m2 + m5 + m6) × 100%, and 55% ≤ W2 ≤ 90%;

[0031] f = m⁴ / m³, and 0.1 ≤ f ≤ 2.0;

[0032] Where m1 is the mass of carboxymethyl cellulose raw material, m2 is the mass of alginic acid raw material, m3 is the mass of carboxyl groups in alginic acid raw material, and m4 is the mass of Ca in calcium source. 2+m1 is the mass of the alginate raw material, m2 is the mass of the calcium source, m3 is the mass of the carboxymethyl cellulose raw material, m4 is the mass of the silicon dioxide, m5 is the mass of the silicon dioxide, and m6 is the mass of the easily soluble raw material. The units of m1, m2, m3, m4, m5, and m6 are the same and can be g or kg.

[0033] The composition of the present disclosure is dispersed in water, and the composition can be gelled to form a hydrogel. Specifically, the alginate raw material in the composition can chelate with calcium ions in a solution state to form a hydrogel and undergo physical crosslinking. However, because the alginate raw material has high sensitivity to calcium ions, after the alginate raw material and the calcium source are directly mixed, the alginate raw material rapidly chelates with calcium ions in a solution state, the formed hydrogel has high strength and poor water absorption capacity, and cannot meet the requirements of occupying a space in the digestive tract.

[0034] Therefore, the applicant proposes, on the one hand, adding a carboxymethyl cellulose raw material to the system of the alginate raw material and the calcium source. The carboxymethyl cellulose raw material can reduce the sensitivity of the alginate raw material to calcium ions, avoid the formation of a hydrogel with excessively high strength and poor water absorption, and thus, by controlling the values of W1 and f, the chelating ability of the alginate raw material and calcium ions can be controlled, the water absorption performance of the composition can be controlled, and the water absorption capacity and the elastic modulus of the composition during the gelling process can be controllably adjusted. The hydrogel formed by the composition provided by the present disclosure not only has good water absorption capacity, but also has high elastic modulus.

[0035] On the other hand, by adding an easily soluble raw material to the system of the alginate raw material and the calcium source, when the composition is in a particulate solid state, the easily soluble raw material forms a physical space in the composition. When the composition forms a hydrogel after being exposed to water, the easily soluble raw material inside the composition has good water absorption capacity, and thus, the external water can be promoted to enter the interior of the composition, thereby improving the water absorption performance of the composition and increasing the volume expansion rate of the composition after water absorption, which is more conducive to realizing the occupation of a space in the digestive tract and improving the weight loss effect. Therefore, the water absorption capacity and the elastic modulus of the composition during the gelling process can also be controllably adjusted by adjusting the value of W3. The hydrogel formed by the composition provided by the present disclosure not only has good water absorption capacity, but also has high elastic modulus.

[0036] Further, after the composition of the present disclosure is added with silicon dioxide in the above system, the elastic modulus of the hydrogel formed by the composition can also be adjusted. By controlling the value of W2, the hydrogel formed by the composition of the present disclosure also has high strength.

[0037] Further, the composition of the present disclosure does not undergo chemical reactions during preparation, and is a physical cross-linking process. The main molecular chain is formed by chelation of the alginate raw material and the calcium source. Compared with the chemical cross-linking process, the water absorption capacity and elastic modulus of the hydrogel can be controlled by strictly controlling the molecular weight of the cross-linked molecules. The composition provided by the present disclosure can achieve controllable adjustment of the water absorption capacity and elastic modulus of the hydrogel by controlling the ratio of the raw materials. The preparation is more convenient, the yield is higher, and the development cost is lower.

[0038] The composition of the present disclosure is dispersed in water, and the composition rapidly absorbs water and swells to form a gel-like hydrogel. After swallowing the hydrogel, the hydrogel enters the stomach through the esophagus. Because the hydrogel prepared from the composition of the present disclosure has high strength, high elastic modulus, and excellent water absorption performance, it can occupy the gastric volume in the stomach, reduce food intake, and thus achieve the purposes of weight loss and blood glucose control. When the hydrogel reaches the small intestine, the hydrogel swells again in the high-pH environment of the small intestine, and the hydroxide at high pH reacts with the silicon dioxide to form a microgel locally, which enhances the elastic modulus at high pH and thus occupies the volume of the small intestine and / or exerts pressure on the small intestine wall to continuously produce satiety, thereby more favorably managing body weight.

[0039] In optional embodiments, W1 can be 10%, 20%, 30%, 40%, 50%, 60%, or 70%, and a range value between any two of the above values.

[0040] W2 can be 0%, 5%, 10%, 15%, 20%, 25%, 30%, 35%, or 40%, and a range value between any two of the above values.

[0041] W3 can be 5%, 7%, 10%, 12%, 15%, 17%, 20%, 22%, 25%, 27%, or 30%, and a range value between any two of the above values.

[0042] W4 can be 55%, 60%, 65%, 70%, 75%, 80%, 85%, or 90%, and a range value between any two of the above values.

[0043] f can be 0.1, 0.5, 1.0, 1.5, or 2.0, and a range value between any two of the above values.

[0044] To further optimize the strength, water absorption, and elastic modulus of the hydrogel formed after the composition provided by the present disclosure gels, the parameter ranges of W1, W2, W3, W4, and f can be further controlled.

[0045] Specifically, W1 satisfies: 10%≤W1≤70%, W2 satisfies: 5%≤W2≤30%, W3 satisfies: 5%≤W3≤25%, W4 satisfies: 65%≤W4≤90%, and f satisfies: 0.2≤f≤2.0;

[0046] More preferably, W1 satisfies: 12%≤W1≤25%, W2 satisfies: 9%≤W2≤25%, W3 satisfies: 5%≤W3≤20%, W4 satisfies: 70%≤W4≤90%, and f satisfies: 0.4≤f≤2.00.

[0047] Further, the selection of the source of the raw material is also another factor for improving the performance of the hydrogel formed by the composition. For example, some literatures report that sodium alginate can form a gel at the pH in the stomach, which can prolong the emptying time of the stomach, thereby reducing food intake and preventing obesity. However, due to the limitations of different sources of alginate, molecular weight and molecular structure (ratio between mannuronic acid and guluronic acid), the weight loss effect varies greatly in different literature reports, which greatly limits the application of alginate in the field of weight loss.

[0048] In order to further improve the performance of the hydrogel, in an optional embodiment, the viscosity of the alginate raw material in the solution is ≥2000 mPa·S when the concentration of the alginate raw material in the solution is 2%; preferably, the viscosity of the alginate raw material in the solution is ≥3000 mPa·S when the concentration of the alginate raw material in the solution is 2%; more preferably, the viscosity of the alginate raw material in the solution is 3000-20000 mPa·S when the concentration of the alginate raw material in the solution is 2%.

[0049] The viscosity of the carboxymethyl cellulose raw material in the solution is ≥4000 mPa·S when the concentration of the carboxymethyl cellulose raw material in the solution is 2%; preferably, the viscosity of the carboxymethyl cellulose raw material in the solution is ≥8000 mPa·S when the concentration of the carboxymethyl cellulose raw material in the solution is 2%; more preferably, the viscosity of the carboxymethyl cellulose raw material in the solution is 8000-60000 mPa·S when the concentration of the carboxymethyl cellulose raw material in the solution is 2%.

[0050] Since the molecular weight and molecular structure of the carboxymethyl cellulose raw material and the alginate raw material are different, they will exhibit different performances. The present disclosure controls the viscosity range of the carboxymethyl cellulose raw material and the alginate raw material, thereby controlling the molecular weight and molecular structure of the carboxymethyl cellulose raw material and the alginate raw material, and further improving the water absorption and elastic modulus of the hydrogel formed by the composition.

[0051] Preferably, the carboxymethyl cellulose raw material includes but is not limited to carboxymethyl cellulose and its salts, and the salts of carboxymethyl cellulose include any one of sodium carboxymethyl cellulose, potassium carboxymethyl cellulose and ammonium carboxymethyl cellulose. Any raw material having the structure of carboxymethyl cellulose can be used as a raw material for reducing the sensitivity of sodium alginate and calcium source.

[0052] Preferably, the alginate raw material includes, but is not limited to, alginic acid and its salts, and the salts of alginic acid include any one of sodium alginate, potassium alginate and ammonium alginate, and any raw material having the structure of alginic acid and its carboxyl group can be used as the raw material for chelation with the calcium source and physical cross-linking.

[0053] Preferably, the calcium source includes, but is not limited to, at least one of calcium carbonate, calcium chloride, calcium citrate, calcium lactate, calcium gluconate, calcium acetate or calcium phosphate; and all products capable of providing calcium can be used as the calcium source of the present disclosure. More preferably, the calcium source is a low-solubility calcium source; and more preferably, the low-solubility calcium source is one of calcium lactate, calcium carbonate and calcium phosphate.

[0054] In an optional embodiment, the solubility of the easily soluble raw material is greater than the solubility of at least one of the carboxymethyl cellulose raw material and the alginate raw material.

[0055] Preferably, the solubility of the easily soluble raw material is greater than the solubility of the raw material with the greatest solubility among the carboxymethyl cellulose raw material and the alginate raw material, so as to improve the water absorption performance of the composition.

[0056] Preferably, the solubility of the easily soluble raw material is greater than or equal to 100 g / L.

[0057] Preferably, the easily soluble raw material includes, but is not limited to, at least one of polyvinyl alcohol, polyethylene glycol, cyclodextrin and sucrose. As long as it is a substance containing a hydroxyl group capable of forming a hydrogen bond with water, it can be used as the easily soluble raw material of the present disclosure.

[0058] It should be noted that, since the composition provided by the present disclosure needs to enter the digestive tract after forming a hydrogel to achieve digestive tract occupation, thereby providing satiety and achieving the effect of weight loss, it can be understood that each component in the raw material of the composition of the present disclosure is a food-grade component, so as to ensure that the hydrogel formed by the composition is edible.

[0059] In an optional embodiment, the particle size of the composition is 0.1 mm to 3 mm, more preferably 0.3 mm to 2.5 mm, and more preferably 0.3 mm to 1 mm.

[0060] In a second aspect, the present disclosure provides a preparation method of the hydrogel composition according to any one of the preceding embodiments, including dispersing the carboxymethyl cellulose raw material, the alginate raw material, the easily soluble raw material and the silicon dioxide in a solution, mixing uniformly and then drying to obtain A material, and then mixing the A material and the calcium source to obtain the hydrogel composition.

[0061] By pre-preparing A material, carboxymethyl cellulose raw materials, easily soluble raw materials and silicon dioxide can be added to alginic acid raw materials in advance to occupy space, which is conducive to the carboxymethyl cellulose to reduce the sensitivity of alginic acid raw materials to calcium ions, the easily soluble raw materials to improve the water absorption capacity, and the silicon dioxide to improve the strength of the composition.

[0062] The carboxymethyl cellulose raw materials, alginic acid raw materials, easily soluble raw materials and silicon dioxide in A material are uniformly dispersed in the solution, and then uniformly mixed solid A material is obtained by drying, and then A material is physically mixed with calcium source to obtain the composition product. When the composition encounters water, the calcium source will quickly chelate with the alginic acid raw materials to form long-chain molecules, but due to the pre-dispersing effect of the carboxymethyl cellulose raw materials, the chelating ability of the calcium source is easy to control, avoiding the decrease of the water absorption of the composition. In addition, the easily soluble raw materials can also play an excellent water absorption performance in the composition, promoting the water to enter the inside of the composition, thereby improving the water absorption capacity of the composition, and the silicon dioxide improves the strength of the composition, so that the volume and strength of the hydrogel are easy to control during the process of the composition absorbing water to become a hydrogel.

[0063] Preferably, during the preparation of A material, the polymer concentration in the solution is 4% to 10%, and the drying temperature is 45°C to 100°C; preferably, the drying temperature is 45°C to 80°C.

[0064] The polymer in the solution refers to the total concentration of carboxymethyl cellulose raw materials and alginic acid raw materials.

[0065] The hydrogel composition provided by the present disclosure is in a solid state before gelation, and can quickly gel to obtain a hydrogel after being added to water. After eating the hydrogel, the hydrogel can occupy the digestive tract, provide satiety, reduce the number of meals and the amount of food, thereby achieving weight loss and improving the symptoms of diabetes.

[0066] In a third aspect, the present disclosure provides a use of the composition according to any one of the preceding embodiments in the preparation of a digestive tract occupying product.

[0067] In an optional embodiment, the method for using the hydrogel composition provided by the present disclosure includes adding the entire solid composition into water and stirring, or first adding A material into water and stirring to obtain a pre-gel suspension, and then adding the remaining raw materials into the pre-gel suspension and stirring to obtain the hydrogel composition.

[0068] Example 1

[0069] The embodiment provides a water-absorption-enhanced hydrogel composition which is composed of A material and B material, the A material is sodium carboxymethyl cellulose, sodium alginate, polyethylene glycol and silicon dioxide, and the B material is calcium lactate. Wherein, W1=23%, W2=10%, W3=10%, W4=80%, and f=0.9.

[0070] Specifically, in the embodiment, the mass of the sodium carboxymethyl cellulose is 60.00g, and the viscosity is 12000mPa·S when the concentration in the solution is 2%.

[0071] The mass of the sodium alginate is 17.92g, and the viscosity is 4000mPa·S when the concentration in the solution is 2%.

[0072] The mass of the silicon dioxide is 9.74g, and the mass of the polyethylene glycol is 9.74g.

[0073] The embodiment further provides a preparation method of the composition, which comprises the following steps.

[0074] The sodium alginate is added into 1500mL water in proportion and is dispersed and dissolved under mechanical stirring at 1000rpm, then the polyethylene glycol is added thereto until stirring and dissolving, then the sodium carboxymethyl cellulose and the silicon dioxide are added and stirred under mechanical stirring at 1000rpm until a uniform suspension is formed, and no large blocks are observed. The suspension is transferred into a metal tray, the thickness of the suspension in the metal tray is controlled to be below 1cm, then the metal tray is placed in an oven at 50℃ and dried for 72h to obtain solid A material. The solid A material is crushed in a crusher, and is sieved through 10-mesh and 120-mesh screens to obtain granular A material with a particle size of 0.1-2mm.

[0075] The calcium lactate is encapsulated as B material, and the mass of the calcium lactate in the B material and the mass of the sodium alginate in the A material satisfy f=0.9.

[0076] Embodiment 2

[0077] The embodiment provides a water-absorption-enhanced hydrogel composition which is composed of A material and B material, the A material is sodium carboxymethyl cellulose, sodium alginate, alpha-cyclodextrin and silicon dioxide, and the B material is calcium lactate. Wherein, W1=23%, W2=10%, W3=10%, W4=80%, and f=0.9.

[0078] Specifically, in the embodiment, the mass of the sodium carboxymethyl cellulose is 60.00g, and the viscosity is 12000mPa·S when the concentration in the solution is 2%.

[0079] The mass of the sodium alginate is 17.92g, and the viscosity is 5000mPa·S when the concentration in the solution is 2%.

[0080] The mass of the silica is 9.74 g, and the mass of the α-cyclodextrin is 9.74 g.

[0081] The embodiment also provides a preparation method of the composition, which is similar to that of the embodiment 1, except that the mass of the substances is different, and the drying temperature is 80 °C.

[0082] Embodiment 3

[0083] The embodiment provides a water-absorption-enhanced hydrogel composition, which is composed of A material and B material, the A material is sodium carboxymethyl cellulose, sodium alginate, sucrose and silica, and the B material is calcium lactate, wherein W1=23%, W2=10%, W3=8%, W4=82%, and f=0.9.

[0084] Specifically, in the embodiment, the mass of the sodium carboxymethyl cellulose is 60.00 g, and the viscosity is 16000 mPa·S when the concentration in the solution is 2%.

[0085] The mass of the sodium alginate is 17.92 g, and the viscosity is 5000 mPa·S when the concentration in the solution is 2%.

[0086] The mass of the silica is 9.50 g, and the mass of the sucrose is 7.60 g.

[0087] The embodiment also provides a preparation method of the composition, which is similar to that of the embodiment 1, except that the mass of the substances is different, and the drying temperature is 85 °C.

[0088] Embodiment 4

[0089] The embodiment provides a water-absorption-enhanced hydrogel composition, which is composed of A material and B material, the A material is sodium carboxymethyl cellulose, sodium alginate, sucrose and silica, and the B material is calcium lactate, wherein W1=23%, W2=10%, W3=8%, W4=82%, and f=0.9.

[0090] Specifically, in the embodiment, the mass of the sodium carboxymethyl cellulose is 60.00 g, and the viscosity is 16000 mPa·S when the concentration in the solution is 2%.

[0091] The mass of the sodium alginate is 17.92 g, and the viscosity is 5000 mPa·S when the concentration in the solution is 2%.

[0092] The mass of the silica is 9.50 g, and the mass of the sucrose is 7.60 g.

[0093] The embodiment also provides a preparation method of the composition, which is similar to that of the embodiment 1, except that the mass of the substances is different, and the drying temperature is 85 °C.

[0094] Example 5

[0095] The present example provides a water-absorbing hydrogel composition for enhancing water absorption, which is composed of A material and B material, the A material being potassium carboxymethyl cellulose, sodium alginate, polyvinyl alcohol and silicon dioxide; the B material being calcium lactate. Among them, W1 = 17%, W2 = 10%, W3 = 10%, W4 = 80%, f = 0.9.

[0096] Specifically, in the present example, the mass of sodium carboxymethyl cellulose is 60.00 g, and the viscosity is 12000 mPa·S when the concentration in the solution is 2%.

[0097] The mass of sodium alginate is 12.30 g, and the viscosity is 6000 mPa·S when the concentration in the solution is 2%.

[0098] The mass of silicon dioxide is 9.00 g, and the mass of polyvinyl alcohol is 9.00 g.

[0099] The present example also provides a preparation method of the above-mentioned composition, which is similar to that of Example 1, and the only difference is that the amounts of the substances are different, and the screen meshes used are 20 mesh and 50 mesh, respectively.

[0100] Example 6

[0101] The present example provides a water-absorbing hydrogel composition for enhancing water absorption, which is composed of A material and B material, the A material being potassium carboxymethyl cellulose, sodium alginate, polyvinyl alcohol and silicon dioxide; the B material being calcium lactate. Among them, W1 = 17%, W2 = 10%, W3 = 10%, W4 = 80%, f = 0.9.

[0102] Specifically, in the present example, the mass of sodium carboxymethyl cellulose is 60.00 g, and the viscosity is 12000 mPa·S when the concentration in the solution is 2%.

[0103] The mass of sodium alginate is 17.92 g, and the viscosity is 3200 mPa·S when the concentration in the solution is 2%.

[0104] The mass of silicon dioxide is 30.00 g, and the mass of polyvinyl alcohol is 12.00 g.

[0105] The present example also provides a preparation method of the above-mentioned composition, which is similar to that of Example 1, and the only difference is that the amounts of the substances are different, and the screen meshes used are 20 mesh and 50 mesh, respectively, and the drying temperature is 85°C.

[0106] Example 7

[0107] The embodiment provides a water-absorption-enhanced hydrogel composition which is composed of A material and B material, the A material is potassium carboxymethyl cellulose, alpha-cyclodextrin and sodium alginate, and the B material is calcium lactate. Wherein, W1=23%, W2=0%, W3=10%, W4=90%, and f=0.9.

[0108] Specifically, in the embodiment, the mass of the sodium carboxymethyl cellulose is 60.00g, and the viscosity is 12000mPa·S when the concentration in the solution is 2%.

[0109] The mass of the sodium alginate is 17.92g, and the viscosity is 4000mPa·S when the concentration in the solution is 2%.

[0110] The mass of the alpha-cyclodextrin is 8.66g.

[0111] The embodiment also provides a preparation method of the composition, and the preparation method is similar to that in the embodiment 1, and the difference is that the use amount of the substances is different, and the drying temperature is 90 DEG C.

[0112] Embodiment 8

[0113] The embodiment provides a water-absorption-enhanced hydrogel composition which is composed of A material and B material, the A material is potassium carboxymethyl cellulose, alpha-cyclodextrin and sodium alginate, and the B material is calcium lactate. Wherein, W1=23%, W2=0%, W3=10%, W4=90%, and f=0.9.

[0114] Specifically, in the embodiment, the mass of the sodium carboxymethyl cellulose is 60.00g, and the viscosity is 12000mPa·S when the concentration in the solution is 2%.

[0115] The mass of the sodium alginate is 17.92g, and the viscosity is 4000mPa·S when the concentration in the solution is 2%.

[0116] The mass of the alpha-cyclodextrin is 8.66g.

[0117] The embodiment also provides a preparation method of the composition, and the preparation method is similar to that in the embodiment 1, and the difference is that the use amount of the substances is different, and the drying temperature is 90 DEG C.

[0118] Comparative Example 1

[0119] The comparative example 1 provides a hydrogel composition, which is prepared by mixing carboxymethyl cellulose sodium having a concentration of 6% (by weight of water) with citric acid having a concentration of 0.3% (by weight of carboxymethyl cellulose). The mixture is dried in an oven at 45°C, and then ground to form particles having a particle size of 100 μm to 1000 μm. The particles are crosslinked at 120°C for 4 hours to obtain the hydrogel composition.

[0120] Comparative Example 2

[0121] The comparative example 2 provides a hydrogel composition, which is prepared by washing the heat-treated crosslinked hydrogel composition obtained in the comparative example 1 with deionized water 3 times, and then drying to obtain the hydrogel composition of the comparative example 2.

[0122] Comparative Example 3

[0123] The comparative example 3 provides a hydrogel composition, which is prepared in the same manner as in the example 1, except that the raw materials do not contain polyethylene glycol and silicon dioxide.

[0124] Comparative Example 4

[0125] The comparative example 4 provides a hydrogel composition, which is prepared in the same manner as in the example 7, except that the α-cyclodextrin is not contained.

[0126] Comparative Example 5

[0127] The comparative example 5 provides a hydrogel composition, which is prepared by mixing 10 g of water-absorbing polymer fibers (COOH:OH = 3.5:1 in PAA and PVA), 20 g of a 3% carboxymethyl cellulose solution, 30 g of a 3% sodium alginate solution, 8 g of α-cyclodextrin, 1 g of citric acid, 0.5 g of silicon dioxide, and 0.5 g of titanium dioxide to form a homogeneous solution, and then crosslinking the homogeneous solution at 120°C for 3 hours. The product after the crosslinking reaction is dried and ground to obtain a sample having a particle size of 200 to 5000 μm. The sample is washed with purified water 5 times at normal temperature and pressure, dried and ground after the washing is completed, and sieved to obtain a water-absorbing hydrogel having a particle size of 200 to 4000 μm.

[0128] Experimental Example 1

[0129] 1) Test in simulated gastric juice:

[0130] The artificial gastric juice is prepared according to the fourth part of the Pharmacopoeia of the People's Republic of China 2020, and then diluted 8 times to adjust the pH to 2.1 to serve as the artificial gastric juice simulating the half hour before a meal (hereinafter referred to as simulated gastric juice).

[0131] Take 40±1 mL of simulated gastric juice on a magnetic stirrer, the stirring speed is 100 rpm, respectively, 0.25±0.002 g of examples 1-8 and comparative examples 1-5 are weighed, and the calcium source is mixed according to the corresponding f calculation, and then added to the simulated gastric juice and continue to stir (no vortex is generated), the stirring time is 30±2 min, which is used for the treatment process of simulated gastric juice.

[0132] Take a piece of 150 mesh gauze and weigh it, record it as g1, then filter the above mixed mixture with 150 mesh gauze to remove the unabsorbed simulated gastric juice (when filtering, pay attention to scrape the liquid on the surface of the gauze with your hand gently until there is no liquid on your hand visible to the naked eye, then end), weigh the mixture and gauze together and record it as g2, and observe the state of the hydrogel obtained after filtration.

[0133] Calculate the medium water absorption rate MUR of the composition in the simulated gastric juice=(g2-g1) / (0.25×W4). The elastic modulus G1' of the filtered hydrogel is determined by rheometer (the corresponding value at a uniform angular frequency of 10 rad / s), and the results are shown in Table 1.

[0134] 2) Detection in simulated intestinal fluid:

[0135] According to the fourth part of the People's Republic of China Pharmacopoeia, artificial intestinal fluid is prepared as simulated small intestinal fluid (hereinafter referred to as simulated intestinal fluid).

[0136] The hydrogel weighed and recorded as g0 after the detection in 1) simulated gastric fluid is then added to a 200 mL beaker of simulated intestinal fluid, and the beaker is transferred to a shaking bed for treatment at 37°C and 60 rpm / min for 120 min, which is used for the treatment process of simulated intestinal fluid.

[0137] Take a piece of 150 mesh gauze and weigh it, record it as g3, then filter the above treated mixture with 150 mesh gauze to remove the unabsorbed simulated intestinal fluid (when filtering, pay attention to scrape the liquid on the surface of the gauze with your hand gently until there is no liquid on your hand visible to the naked eye, then end), weigh the mixture and gauze together and record it as g4, and observe the state of the hydrogel obtained after filtration.

[0138] The elastic modulus G2' of the filtered hydrogel is determined by rheometer (the corresponding value at a uniform angular frequency of 10 rad / s), and the results are shown in Table 1.

[0139] Table 1 Properties of the composition and hydrogel

[0140] Note: N.A represents not applicable; Comparative Example 1 has poor occupation effect due to low MUR, so subsequent tests are not performed.

[0141] As can be seen from Table 1, the composition provided by the embodiment of the present disclosure can reach a maximum of 85.8 times the original weight after becoming a hydrogel, and still maintains a high elastic modulus (greater than 900 Pa) after absorbing water in the simulated gastric fluid, indicating that the composition provided by the embodiment of the present disclosure can balance the water absorption performance and strength, and is beneficial to assisting in enhancing the weight loss effect.

[0142] Comparative Examples 1, 2 and 5 are all chemical cross-linking, and the preparation process is complex. The hydrogel obtained in Comparative Example 1 has poor water absorption performance and high strength, resulting in insufficient swelling volume of the hydrogel, which is difficult to achieve effective space occupation in the digestive tract. Although the hydrogel obtained in Comparative Example 2 has improved water absorption performance compared with Comparative Example 1, the elastic modulus is reduced, and repeated deionized water washing is required, which is time-consuming and has low preparation yield. Comparative Examples 3 and 4 obtain hydrogel compositions by using a similar physical cross-linking method as the present disclosure, but Comparative Example 3 does not add easily soluble raw materials and silicon dioxide, and the medium water absorption rate and elastic modulus are significantly lower than those of Example 1. Comparative Example 4 does not add easily soluble raw materials, and the medium water absorption rate is significantly lower than that of Example 7.

[0143] Experimental Example 2

[0144] Twenty volunteers were randomly divided into two groups, and the control group took the same amount of sucrose, and the experimental group took 3g of the hydrogel composition with enhanced water absorption of Example 3 for two meals per day. The drinking time is 30 minutes before meals, twice a day, at noon and dinner in the afternoon. At the same time, the volunteers were given nutritional intervention, and the daily caloric intake was reduced by 300kcal. The body weight of the volunteers was recorded at the 2nd month and the 6th month, and the average body weight was calculated as shown in Table 2.

[0145] Table 2 Body weight change table

[0146] Note: n represents the number of people.

[0147] As can be seen from Table 2, through nutritional intervention and the use of the composition provided by the present disclosure, a good weight loss effect is achieved. Within 24 weeks, the body weight of the volunteers in the experimental group decreased by 6.71kg, while the body weight of the volunteers in the control group decreased by only 2.54kg, indicating that the hydrogel composition provided by the embodiment of the present disclosure has a good weight loss effect.

[0148] The hydrogel composition with enhanced water absorption provided by the embodiment of the present disclosure, and the preparation method and application thereof, have at least the following advantages:

[0149] 1) The composition provided by the present disclosure is prepared by physical action of food-grade raw materials, and can be directly used as food.

[0150] 2) The present disclosure adopts seaweed acid raw materials and calcium source to prepare the composition and form hydrogel by physical cross-linking, which has simpler preparation process and higher yield than the hydrogel prepared by chemical cross-linking method, and is conducive to large-scale production.

[0151] 3) By controlling the content of carboxymethyl cellulose raw materials, easily soluble raw materials and silicon dioxide, the water absorption performance and strength of the hydrogel formed by the composition can be directly regulated, so as to ensure that the composition can rapidly expand by absorbing water, form a space with a larger volume, and ensure its mechanical strength, thereby ensuring the long-acting satiety effect of the hydrogel in the digestive tract.

[0152] The above is only a preferred embodiment of the present disclosure and is not intended to limit the present disclosure. For those skilled in the art, the present disclosure can have various modifications and changes. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present disclosure shall be included in the protection scope of the present disclosure. Industrial applicability

[0153] The present disclosure provides a hydrogel composition with enhanced water absorption and its preparation method and application. The composition is prepared by physical action of food-grade raw materials and can be directly used as food, has simpler preparation process, higher yield, and is conducive to large-scale production.

Claims

1. A hydrogel composition for enhanced water absorption, characterized in that, The raw materials include carboxymethyl cellulose, alginate, easily soluble materials, calcium source, and silicon dioxide, and the mass relationships of the components in the raw materials satisfy the following: W1 = m2 / (m1+m2)×100%, and 10%≤W1≤70%; W2 = m5 / (m1+m2+m5+m6)×100%, and 0%≤W2≤40%; W3 = m6 / (m1+m2+m5+m6)×100%, and 5%≤W2≤30%; W4 = (m1+m2) / (m1+m2+m5+m6)×100%, and 55%≤W2≤90%; f = m4 / m3, and 0.1≤f≤2.0; Where m1 is the mass of carboxymethyl cellulose raw material, m2 is the mass of alginic acid raw material, m3 is the mass of carboxyl groups in alginic acid raw material, and m4 is the mass of Ca in calcium source. 2+ The mass of m5 is the mass of silicon dioxide, and the mass of m6 is the mass of easily soluble raw materials.

2. The composition according to claim 1, characterized in that, The following conditions must be met: W1 satisfies: 10% ≤ W1 ≤ 70%; W2 satisfies: 5% ≤ W2 ≤ 30%; W3 satisfies: 5% ≤ W3 ≤ 25%; W4 satisfies: 65% ≤ W4 ≤ 90%; and f satisfies: 0.2 ≤ f ≤ 2.

0. More preferably, W1 satisfies: 12% ≤ W1 ≤ 25%, W2 satisfies: 9% ≤ W2 ≤ 25%, W3 satisfies: 5% ≤ W3 ≤ 20%, W4 satisfies: 70% ≤ W4 ≤ 90%, and f satisfies: 0.4 ≤ f ≤ 2.

0.

3. The composition according to claim 1 or 2, characterized in that, The solubility of the readily soluble raw material is greater than that of at least one of the carboxymethyl cellulose raw materials and alginate raw materials; Preferably, the solubility of the readily soluble raw material is greater than or equal to 100 g / L; Preferably, the readily soluble raw material includes at least one of polyvinyl alcohol, polyethylene glycol, cyclodextrin, and sucrose.

4. The composition according to claim 1, characterized in that, The carboxymethyl cellulose raw material has a viscosity ≥ 4000 mPa·s when the concentration in the solution is 2%; Preferably, the carboxymethyl cellulose raw material includes carboxymethyl cellulose and its salts, wherein the carboxymethyl cellulose salts include any one of sodium carboxymethyl cellulose, potassium carboxymethyl cellulose, and ammonium carboxymethyl cellulose.

5. The composition according to claim 1, characterized in that, The alginate raw material has a viscosity ≥2000 mPa·s when the concentration of the solution is 2%; Preferably, the alginate raw material includes alginate and its salts, wherein the alginate salts include any one of sodium alginate, potassium alginate, and ammonium alginate.

6. The composition according to claim 1, characterized in that, The calcium source includes at least one of calcium carbonate, calcium chloride, calcium citrate, calcium lactate, calcium gluconate, calcium acetate, or calcium phosphate; more preferably, the calcium source is a calcium source with low solubility; even more preferably, the calcium source with low solubility is one of calcium lactate, calcium carbonate, and calcium phosphate.

7. The composition according to claim 1, characterized in that, The particle size of the composition is 0.1 mm to 3 mm, more preferably 0.3 mm to 2.5 mm, and even more preferably 0.3 mm to 1 mm.

8. A method for preparing the composition according to any one of claims 1 to 7, characterized in that, The process involves dispersing carboxymethyl cellulose raw materials, alginate raw materials, and silica in a solution, mixing them evenly, and then drying them to obtain material A. Then, material A, calcium source, and easily soluble raw materials are mixed to obtain the final product.

9. The preparation method according to claim 8, characterized in that, During the preparation of material A, the polymer concentration in the solution is 4% to 10%, and the drying temperature is 45°C to 100°C; preferably, the drying temperature is 45°C to 80°C.

10. The use of the composition according to any one of claims 1 to 7 in the preparation of a digestive tract occupant product.

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