Anti-sticking hydrogel coated particle as well as preparation method and application thereof

Abstract

The invention discloses an anti-sticking nozzle hydrogel coated particle and a preparation method and application thereof, the anti-sticking nozzle hydrogel coated particle comprises hydrogel particles and a coating layer from inside to outside, the mass of the hydrogel particles accounts for 50%-99% of the total mass of the anti-sticking nozzle hydrogel coated particle, and the coating layer accounts for 50%-99% of the total mass of the anti-sticking nozzle hydrogel coated particle. The coating layer accounts for 1%-50% of the total mass of the anti-sticking hydrogel coating particle; the coating layer comprises a film-forming substrate and a plasticizer, the film-forming substrate accounts for 50-100% of the mass of the coating layer, the plasticizer accounts for 0-50% of the mass of the coating layer, and the coating layer of the prepared anti-sticking hydrogel coating particle is insoluble in the oral cavity within a short time. According to the invention, the hydrogel particles are coated by a film coating technology, so that the defects that the hydrogel particles are easy to stick to the mouth when being directly drunk and easy to absorb moisture when being exposed to air for a short time are overcome, the original water swelling performance of the hydrogel particles is not influenced, and the taste of the hydrogel particles is improved.

Description

Technical Field

[0001] The invention belongs to the technical field of weight loss food development, and particularly relates to a mouth-adhesive-resistant hydrogel-coated particle and a preparation method and application thereof. Background Art

[0002] Obesity can cause many chronic diseases, such as diabetes, hypertension, hyperlipidemia, coronary heart disease, fatty liver and endocrine disorders. Health problems caused by obesity must be given enough attention, and weight loss is the main means to deal with obesity-related problems. The basic principle of weight loss is that the calories consumed are less than the calories consumed. At present, the main ways to lose weight are dieting, exercise, drugs, surgery, etc. Dieting and weight loss require tenacious willpower of the person who loses weight, and it is easy to rebound once the diet is resumed; most people cannot persist in weight loss through exercise, and it is difficult to achieve the expected weight loss effect; drug weight loss has great side effects and only treats the symptoms but not the root cause; surgical weight loss has a high risk, and 99% of obese patients do not accept it. When many of the above weight loss methods are not ideal, meal replacement foods were born.

[0003] Among the meal replacement products currently on the market, there are some hydrogel particles made using cellulose cross-linking technology. This type of particle is very easy to absorb water, expands to a high multiple after absorbing water, and has a strong sense of fullness. At the same time, there are also some problems in use, such as sticking to the mouth, difficult to swallow, bland, low in nutritional content, and poor consumer experience. Patent CN115918889A discloses a composite hydrogel obtained by physical cross-linking of polysaccharide gum and cellulose or its derivatives. The water absorption capacity of the composite hydrogel reaches more than 50 times. CN113854567A discloses an edible hydrogel obtained by chemical cross-linking of polysaccharides or polysaccharide derivatives with dibasic acids. It has extremely strong water absorption and water locking capabilities in the gastrointestinal tract and can quickly and continuously fill the gastrointestinal space. The hydrogels disclosed in the above two patents are very easy to absorb water and moisture due to the hydrophilic groups in their molecular structure and the capillary effect of the three-dimensional network structure. When eaten, they easily absorb moisture from the mouth, teeth and palate due to their super water absorption ability, thereby sticking to the mouth, affecting the absorption and filling effect of the hydrogel in the stomach, and the taste is not good when eaten.

[0004] Patent CN118000277A provides a gastric volume-occupying satiety product based on a chocolate matrix. The product uses hydrogel particles wrapped in chocolate fat to achieve the effect of preventing adhesion to the oral cavity. However, the particles wrapped in solid fat need to be stored at 16-18°C, and they feel greasy when eaten directly. They need to be made into chocolate. Therefore, the product form is single and the application scenario is narrow. In addition, due to the characteristics of solid fat and chocolate, cold chain transportation and storage are required in summer, which consumes a lot of energy and is costly. Therefore, it is urgent to explore a low-cost and easy-to-prepare anti-adhesive mouth hydrogel formula. Summary of the invention

[0005] In order to overcome the above-mentioned deficiencies in the prior art, the purpose of the present invention is to provide a mouth-adhering hydrogel-coated granule and a preparation method and application thereof, so as to solve the problems that the current hydrogel granules are easy to stick to the mouth and easy to absorb moisture and swell when eaten. It has been verified that the mouth-adhering hydrogel-coated granules provided by the present invention have the functions of mouth-adhering and moisture-proof, while not affecting the original high water absorption and expansion multiple and large storage modulus characteristics of the hydrogel granules, and can produce a strong sense of fullness at a low dosage, thereby reducing calorie intake.

[0006] The purpose of the present invention is achieved by at least one of the following technical solutions.

[0007] The invention discloses an anti-sticking mouth hydrogel coated granule, which comprises a hydrogel granule and a coating layer from the inside to the outside, wherein the mass of the hydrogel granule accounts for 50%-99% of the total mass of the anti-sticking mouth hydrogel coated granule, and the coating layer accounts for 1%-50% of the total mass of the anti-sticking mouth hydrogel coated granule; the coating layer comprises a film-forming matrix and a plasticizer, wherein the film-forming matrix accounts for 50%-100% of the mass of the coating layer, and the plasticizer accounts for 0-50% of the mass of the coating layer.

[0008] Specifically, the "anti-sticking mouth" of the present invention refers to that the coating layer of the hydrogel-coated particles is not completely dissolved within at least 120 seconds (s) after contacting water to expose the hydrogel.

[0009] Furthermore, the mass of the hydrogel particles accounts for 65%-95% of the total mass of the anti-sticking mouth hydrogel coated particles, and the coating layer accounts for 5%-35% of the total mass of the anti-sticking mouth hydrogel coated particles.

[0010] Furthermore, the film-forming matrix accounts for 60%-100% of the mass of the coating layer, and the plasticizer accounts for 0-40% of the mass of the coating layer.

[0011] Furthermore, the hydrogel particles include chemically cross-linked hydrogel particles and / or physically cross-linked hydrogel particles.

[0012] Furthermore, the chemically cross-linked hydrogel particles include hydrogels obtained by chemically cross-linking cellulose or its derivatives with dibasic acid or polybasic acid, and the physically cross-linked hydrogel particles include hydrogels obtained by physically cross-linking cellulose or its derivatives with polysaccharide gum.

[0013] Preferably, the cellulose or its derivatives include: one or more of carboxymethyl cellulose, methyl cellulose, ethyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, hydroxypropyl methyl cellulose, carboxymethyl hydroxyethyl cellulose, carboxymethyl hydroxypropyl cellulose and carboxymethyl ethyl cellulose or their derivatives.

[0014] Preferably, the dibasic acid or polybasic acid comprises one or more of tartaric acid, malic acid and citric acid.

[0015] Preferably, the polysaccharide gum comprises one or more of pectin, xanthan gum, guar gum, locust bean gum, carrageenan, konjac gum, gellan gum, agar, sachets gum and welan gum.

[0016] Furthermore, the hydrogel particles are formed by physically cross-linking sodium carboxymethyl cellulose and pectin; and / or, the hydrogel particles are formed by chemically cross-linking sodium carboxymethyl cellulose and malic acid.

[0017] Furthermore, the film-forming matrix includes one or more of hydroxypropyl methylcellulose, sodium carboxymethyl cellulose, polyvinyl alcohol, hydroxypropyl cellulose, ethyl cellulose, cellulose acetate phthalate and chitosan.

[0018] Furthermore, the film-forming matrix is ​​a water-soluble film-forming matrix, including one or more of hydroxypropyl methylcellulose, sodium carboxymethyl cellulose, polyvinyl alcohol and hydroxypropyl cellulose.

[0019] Furthermore, the film-forming matrix is ​​a water-insoluble film-forming matrix, including one or more of ethyl cellulose, cellulose acetate phthalate and chitosan.

[0020] Furthermore, the plasticizer includes polyethylene glycol and / or glycerol.

[0021] The present invention also provides a method for preparing the above-mentioned anti-mouth-sticking hydrogel coated particles, comprising the following steps:

[0022] (1) Preparation of hydrogel particles: crushing the hydrogel into 20-50 meshes to obtain hydrogel particles;

[0023] (2) Preparation of coating slurry: dissolve the film-forming matrix and plasticizer and stir them evenly for use;

[0024] (3) Coating: The coating layer slurry is sprayed on the surface of the hydrogel particles by high-pressure atomization using a fluidized bed coating process, and then dried to obtain an anti-sticking hydrogel coated particle.

[0025] Furthermore, the coating process conditions are: air inlet temperature 45-80°C, atomization pressure 0.1-0.4Mpa, fan frequency 10-55Hz, slurry flow rate 5-30g / min.

[0026] Furthermore, the drying process conditions are: inlet air temperature 60-90°C, fan frequency 10-55Hz, and time 10-60min.

[0027] Furthermore, the moisture content of the material after drying is less than 1%, that is, the moisture content of the anti-sticking hydrogel coated particles is less than 1%.

[0028] Furthermore, in step (2), the solvent used to dissolve the film-forming matrix and the plasticizer includes water, ethanol solution, acidic solution or alkaline solution.

[0029] Furthermore, the film-forming matrix is ​​ethyl cellulose and the solvent is an ethanol solution; or, the film-forming matrix is ​​cellulose acetate phthalate and the solvent is an alkaline solution; or, the film-forming matrix is ​​chitosan and the solvent is an acidic solution.

[0030] The present invention also provides the use of the anti-sticking mouth hydrogel coated particles described in the above technical solution or the anti-sticking mouth hydrogel coated particles prepared by the preparation method described in the above technical solution in the preparation of food, medicine or health care products with gastric filling, weight control and blood sugar control effects.

[0031] The present invention also provides a weight control composition, comprising the anti-sticking mouth hydrogel coated particles described in the above technical solution or the anti-sticking mouth hydrogel coated particles prepared by the preparation method described in the above technical solution, and auxiliary materials.

[0032] Compared with the prior art, the present invention has the following advantages and beneficial effects:

[0033] (1) The present invention provides a mouth-preventing hydrogel-coated particle. Through the film coating technology, a coating material and internal hydrogel particles are mixed in a specific ratio to form a thin film on the surface of the hydrogel particles, covering its three-dimensional network structure, reducing the possibility of contact between the hydrophilic groups of the hydrogel particles and water molecules, and preventing or slowing down the capillary effect of the hydrogel in the oral cavity. The obtained hydrogel-coated particles have the properties of moisture resistance and mouth-preventing adhesion, preventing the hydrogel from absorbing water and swelling in the oral cavity in advance, and solving the problem of poor sensory perception of the hydrogel particles sticking to the mouth when taken.

[0034] (2) The film-forming matrix of the present invention can be a water-soluble material, such as hydroxypropyl methylcellulose and / or polyvinyl alcohol. The film formed after coating will dissolve quickly after entering the oral cavity, but the dissolved macromolecular substances will form intermolecular hydrogen bonds with the internal hydrogel particles, increasing the viscosity. In a short period of time, they will still adhere to the surface of the hydrogel particles and will not dissolve, thereby inhibiting the capillary effect of the three-dimensional network structure, reducing the water absorption capacity of the hydrogel, and achieving the effect of preventing the mouth from sticking.

[0035] (3) The film-forming matrix in the present invention may also be a water-insoluble material, such as ethyl cellulose and / or chitosan. The film formed after coating will not dissolve in a short time, which can prevent the particles from directly contacting with water molecules in saliva, thereby preventing the particles from sticking to the oral cavity when directly swallowed. At the same time, by using a water-insoluble material as the film-forming matrix, the obtained anti-mouth-sticking hydrogel coated particles exhibit more excellent moisture-proof properties.

[0036] (4) The present invention has a specific ratio of the coating layer to the internal hydrogel particles, and there is no need to add additional disintegrants to the coating layer. After the anti-sticking hydrogel coated particles enter the stomach, the coating layer disintegrates within a time limit. The long-term swelling performance of the anti-sticking hydrogel coated particles in gastric juice is similar to that of the uncoated hydrogel particles. The hydrogel particles have extremely strong water absorption and water locking capabilities in the gastrointestinal tract, can quickly and continuously fill the gastrointestinal space, reduce the body's calorie intake, and achieve excellent weight control effects. BRIEF DESCRIPTION OF THE DRAWINGS

[0037] Figure 1 This is a micrograph of the cross section (oblique cut) of the anti-sticking hydrogel coated granules prepared in Example 5.

[0038] Among them, 1 is the hydrogel particles and 2 is the coating layer. DETAILED DESCRIPTION

[0039] The specific implementation of the present invention is further described below in conjunction with examples, but the implementation and protection of the present invention are not limited thereto. It should be noted that if there are processes that are not particularly described in detail below, they can be implemented or understood by those skilled in the art with reference to the prior art. If the manufacturer of the reagents or instruments used is not indicated, they are deemed to be conventional products that can be purchased commercially.

[0040] The present invention provides a kind of anti-sticking mouth hydrogel coated granules, which include hydrogel granules and coating layers from the inside to the outside, wherein the mass of the hydrogel granules accounts for 50%-99% of the total mass of the anti-sticking mouth hydrogel coated granules, and the coating layer accounts for 1%-50% of the total mass of the anti-sticking mouth hydrogel coated granules; the coating layer includes a film-forming matrix and a plasticizer, wherein the film-forming matrix accounts for 50%-100% of the mass of the coating layer, and the plasticizer accounts for 0-50% of the mass of the coating layer; the coating layer of the hydrogel coated granules is not completely dissolved within at least 120 seconds (s) after contacting water, so as to expose the hydrogel. In some embodiments of the present invention, the mass of the hydrogel granules accounts for 65%-95% of the total mass of the anti-sticking mouth hydrogel coated granules, and the coating layer accounts for 5%-35% of the total mass of the anti-sticking mouth hydrogel coated granules. In some embodiments of the present invention, the film-forming matrix accounts for 60%-100% of the mass of the coating layer, and the plasticizer accounts for 0-40% of the mass of the coating layer.

[0041] The coating layer improves the stability of the hydrogel particles. Compared with the uncoated hydrogel particles, the coating layer can effectively isolate the hydrogel particles from the external environment (such as air, moisture, light, etc.), protect the hydrogel particles from moisture absorption, degradation and oxidation, thereby extending the stability and shelf life of the hydrogel particles. The hydrogel particles and the coating layer have a specific mass ratio, which has a synergistic effect. While ensuring the anti-sticking effect, the coating layer does not need to add additional disintegrants to ensure that the coating layer disintegrates smoothly within a suitable time limit in the gastric juice, and does not affect the swelling effect of the hydrogel particles.

[0042] In the present invention, the film-forming matrix includes one or more of chitosan, hydroxypropyl methylcellulose, sodium carboxymethyl cellulose, polyvinyl alcohol, hydroxypropyl cellulose, ethyl cellulose, and cellulose acetate phthalate. In some embodiments of the present invention, the film-forming matrix is ​​a water-soluble film-forming matrix, including one or more of hydroxypropyl methylcellulose, sodium carboxymethyl cellulose, polyvinyl alcohol, and hydroxypropyl cellulose. In some preferred embodiments of the present invention, the film-forming matrix is ​​selected from hydroxypropyl methylcellulose and / or polyvinyl alcohol. The film formed after coating will dissolve quickly after entering the oral cavity, but the dissolved macromolecular substances will still adhere to the surface of the hydrogel particles in a short time under the action of intermolecular hydrogen bonds, etc., and will not dissolve, thereby inhibiting the capillary effect of the three-dimensional network structure, reducing the water absorption capacity of the hydrogel, and achieving the effect of preventing the mouth from sticking. In some embodiments of the present invention, the film-forming matrix is ​​a non-water-soluble film-forming matrix, including one or more of ethyl cellulose, cellulose acetate phthalate, and chitosan. In some preferred embodiments of the present invention, the film-forming matrix is ​​selected from ethyl cellulose and / or chitosan. The film formed after coating will not dissolve in a short time, which can prevent the particles from directly contacting the water molecules in the saliva, thereby preventing the particles from sticking to the oral cavity when swallowed directly. At the same time, using ethyl cellulose and / or chitosan as the film-forming matrix, the obtained anti-mouth-sticking hydrogel coated particles show better moisture-proof performance. When ethyl cellulose is used as the film-forming matrix, the good chemical stability of ethyl cellulose and its ability to withstand strong alkali, weak alkali and dilute acid ensures that the coating layer is targeted and dissolved in the gastric juice, so that the hydrogel particles are released smoothly.

[0043] In the present invention, the plasticizer includes polyethylene glycol and / or glycerol.

[0044] In the present invention, the hydrogel particles include chemically cross-linked hydrogel particles and / or physically cross-linked hydrogel particles.

[0045] Chemically cross-linked hydrogel particles include hydrogels obtained by chemically cross-linking cellulose or its derivatives with dibasic acids or polybasic acids. In some embodiments of the present invention, the cellulose or its derivatives include: one or more of carboxymethyl cellulose, methyl cellulose, ethyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, hydroxypropyl methyl cellulose, carboxymethyl hydroxyethyl cellulose, carboxymethyl hydroxypropyl cellulose and carboxymethyl ethyl cellulose or their derivatives, and the dibasic acid or polybasic acid includes: one or more of tartaric acid, malic acid, and citric acid.

[0046] In a specific embodiment of the present invention, the chemically cross-linked hydrogel particles are hydrogels obtained by chemically cross-linking sodium carboxymethyl cellulose and citric acid (tribasic acid), and the synthesis mechanism of the chemically cross-linked hydrogel particles is as follows:

[0047]

[0048] The raw materials of physically cross-linked hydrogel particles include polysaccharide gum and cellulose or its derivatives, wherein the polysaccharide gum is a linear polysaccharide without branches or containing only short branches. In some embodiments of the present invention, the cellulose or its derivatives in the raw materials of physically cross-linked hydrogel particles include, but are not limited to, one or more of carboxymethyl cellulose, methyl cellulose, ethyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, hydroxypropyl methyl cellulose, carboxymethyl hydroxyethyl cellulose, carboxymethyl hydroxypropyl cellulose and carboxymethyl ethyl cellulose. In some specific embodiments of the present invention, the cellulose or its derivatives may be sodium carboxymethyl cellulose.

[0049] Preferably, the hydrogel particles are formed by physically cross-linking sodium carboxymethyl cellulose and pectin; or, the hydrogel particles are formed by chemically cross-linking sodium carboxymethyl cellulose and malic acid.

[0050] The present invention also provides a method for preparing the anti-sticking mouth hydrogel coated particles described in the above technical solution, comprising the following steps:

[0051] (1) Preparation of hydrogel particles: crushing the hydrogel into 20-50 meshes to obtain hydrogel particles;

[0052] (2) Preparation of coating slurry: dissolve the film-forming matrix and plasticizer and stir them evenly for use;

[0053] (3) Coating: The coating layer slurry is sprayed on the surface of the hydrogel particles by high-pressure atomization using a fluidized bed coating process, and then dried to obtain an anti-sticking hydrogel coated particle.

[0054] The hydrogel in step (1) includes a chemically cross-linked hydrogel and / or a physically cross-linked hydrogel; the hydrogel can be a commercially available product or can be prepared by itself, wherein the preparation method of the chemically cross-linked hydrogel refers to Chinese patent CN113854567A; the preparation method of the physically cross-linked hydrogel refers to Chinese patent CN115918889A.

[0055] In some embodiments of the present invention, the solvents that can be used to dissolve the film-forming matrix and the plasticizer include water, ethanol solution, acidic solution or alkaline solution. Preferably, the film-forming matrix is ​​a non-water-soluble film-forming matrix, including one or more of ethyl cellulose, cellulose acetate phthalate and chitosan. The non-water-soluble film-forming matrix is ​​selected, and the solvent used in the coating layer slurry is an ethanol solution, an acidic solution or an alkaline solution. When ethanol is used as a solvent, the moisture content in the coating layer slurry is reduced, so that the hydrogel particles are not easily affected by moisture during the preparation process. While ethanol evaporates and dries, it can take away moisture, thereby improving production efficiency. In a specific embodiment of the present invention, the film-forming matrix is ​​ethyl cellulose, and the solvent is an ethanol solution. In a specific embodiment of the present invention, the film-forming matrix is ​​cellulose acetate phthalate, and the solvent is an alkaline solution. In another specific embodiment of the present invention, the film-forming matrix is ​​chitosan, and the solvent is an acidic solution.

[0056] In some embodiments of the present invention, the coating process conditions are: inlet air temperature 45-80°C, atomization pressure 0.1-0.4Mpa, fan frequency 10-55Hz, slurry flow rate 5-30g / min.

[0057] In some embodiments of the present invention, the drying process conditions are: air inlet temperature 60-90°C, fan frequency 10-55Hz, time 10-60min. Preferably, the moisture content of the material after drying is less than 1%, that is, the moisture content of the anti-sticking hydrogel coated particles is less than 1%.

[0058] The present invention also provides the use of the above-mentioned anti-sticking mouth hydrogel coated particles or the anti-sticking mouth hydrogel coated particles prepared by the above-mentioned preparation method in the preparation of food, medicine or health care products with gastric filling, weight control and blood sugar control.

[0059] The present invention also provides a weight control composition, comprising the above-mentioned anti-sticking mouth hydrogel coated particles or the anti-sticking mouth hydrogel coated particles prepared by the above-mentioned preparation method, and auxiliary materials.

[0060] Example 1

[0061] The invention discloses a mouth-adhesive-resistant hydrogel coated granule, which consists of 95 parts of hydrogel granules and 5 parts of coating layer (3 parts of hydroxypropyl methylcellulose and 2 parts of polyethylene glycol 4000) by weight.

[0062] ① Preparation of hydrogel particles: as described in Example 2 of patent CN115918889A, by weight, 67 parts of sodium carboxymethyl cellulose and 1 part of pectin were dissolved in 1111 parts of water and stirred for 2 hours, dried at a drying temperature of 110°C for 8 hours, crushed and sieved, and 20-50 mesh hydrogel particles were taken for use;

[0063] ② Preparation of coating slurry: Add 3 parts of Hydroxypropyl Methylcellulose and 2 parts of Macrogol 4000 into 50 parts of purified water and stir for use;

[0064] ③ Coating: Place the hydrogel particles in a fluidized bed, spray the coating slurry on the surface of the hydrogel particles and dry them to obtain moisture-proof and anti-sticking hydrogel coated particles. The coating process conditions are: inlet air temperature 45-80°C, atomization pressure 0.1-0.4Mpa, fan frequency 10-55Hz, slurry flow rate 5-30g / min. The drying process conditions are: inlet air temperature 60-90°C, fan frequency 10-55Hz, time 10-60min, and the moisture content of the material after drying is <1%.

[0065] Example 2

[0066] The invention discloses a mouth-adhesive-resistant hydrogel coated granule, which consists of 65 parts of hydrogel granules and 35 parts of coating layer (28 parts of polyvinyl alcohol and 7 parts of polyethylene glycol 4000) by weight.

[0067] ① Preparation of hydrogel particles: as described in Example 1 of patent CN113854567A, 64 parts of sodium carboxymethyl cellulose and 0.19 parts of malic acid were dissolved in 1000 parts of water and stirred for 6 hours, dried at 50°C for 72 hours, crushed and sieved, and 20-50 mesh hydrogel particles were taken, cross-linked at a drying temperature of 110°C for 2 hours, and then used;

[0068] ② Preparation of coating slurry: Add 28 parts of polyvinyl alcohol and 7 parts of polyethylene glycol 4000 into 350 parts of purified water and stir for standby use;

[0069] ③ Coating: Place the hydrogel particles in a fluidized bed, spray the coating slurry on the surface of the hydrogel particles and dry them to obtain moisture-proof and anti-sticking hydrogel coated particles. The coating process conditions are: inlet air temperature 45-80℃, atomization pressure 0.1-0.4Mpa, fan frequency 10-55Hz, slurry flow rate 5-30g / min. The drying process conditions are: inlet air temperature 60-90℃, fan frequency 10-55Hz, time 10-60min, and the moisture content of the material after drying is <1%.

[0070] Embodiment 3:

[0071] The invention discloses a mouth-adhesive-proof hydrogel coated granule, which consists of 90 parts of hydrogel granules and 10 parts of coating layer (8 parts of ethyl cellulose and 2 parts of glycerol) by weight.

[0072] ① Preparation of hydrogel particles: as described in Example 2 of patent CN115918889A, by weight, 67 parts of sodium carboxymethyl cellulose and 1 part of pectin were dissolved in 1111 parts of water and stirred for 2 hours, dried at a drying temperature of 110°C for 8 hours, crushed and sieved, and 20-50 mesh hydrogel particles were taken for use;

[0073] ② Preparation of coating layer slurry: add 8 parts of ethyl cellulose and 2 parts of glycerol into 120 parts of 75% ethanol solution and stir for standby use;

[0074] ③ Coating: Place the hydrogel particles in a fluidized bed, spray the coating slurry on the surface of the hydrogel particles and dry them to obtain moisture-proof and anti-sticking hydrogel coated particles. The coating process conditions are: inlet air temperature 45-80℃, atomization pressure 0.1-0.4Mpa, fan frequency 10-55Hz, slurry flow rate 5-30g / min. The drying process conditions are: inlet air temperature 60-90℃, fan frequency 10-55Hz, time 10-60min, and the moisture content of the material after drying is <1%.

[0075] Embodiment 4:

[0076] The invention discloses a mouth-adhesive-resistant hydrogel coated granule, which consists of 80 parts of hydrogel granules and 20 parts of chitosan by weight.

[0077] ① Preparation of hydrogel particles: as described in Example 2 of patent CN115918889A, by weight, 67 parts of sodium carboxymethyl cellulose and 1 part of pectin were dissolved in 1111 parts of water and stirred for 2 hours, dried at a drying temperature of 110°C for 8 hours, crushed and sieved, and 20-50 mesh hydrogel particles were taken for use;

[0078] ② Preparation of coating slurry: Add 20 parts of chitosan into 200 parts of 0.1% acetic acid solution and stir for standby use;

[0079] ③ Coating: Place the hydrogel particles in a fluidized bed, spray the coating slurry on the surface of the hydrogel particles and dry them to obtain moisture-proof and anti-sticking hydrogel coated particles. The coating process conditions are: inlet air temperature 45-80℃, atomization pressure 0.1-0.4Mpa, fan frequency 10-55Hz, slurry flow rate 5-30g / min. The drying process conditions are: inlet air temperature 60-90℃, fan frequency 10-55Hz, time 10-60min, and the moisture content of the material after drying is <1%.

[0080] Example 5

[0081] The invention discloses a mouth-adhesive-resistant hydrogel coated granule, which consists of 95 parts of hydrogel granules and 5 parts of coating layer (3 parts of hydroxypropyl methylcellulose, 1.9 parts of polyethylene glycol 4000 and 0.1 part of amaranth) by weight.

[0082] ① Preparation of hydrogel particles: as described in Example 2 of patent CN115918889A, by weight, 67 parts of sodium carboxymethyl cellulose and 1 part of pectin were dissolved in 1111 parts of water and stirred for 2 hours, dried at a drying temperature of 110°C for 8 hours, crushed and sieved, and 20-50 mesh hydrogel particles were taken for use;

[0083] ② Preparation of coating layer slurry: Add 3 parts of hypromellose, 1.9 parts of polyethylene glycol 4000, and 0.1 parts of amaranth to 50 parts of purified water and stir for use;

[0084] ③ Coating: Place the hydrogel particles in a fluidized bed, spray the coating slurry on the surface of the hydrogel particles and dry them to obtain moisture-proof and anti-sticking hydrogel coated particles. The coating process conditions are: inlet air temperature 45-80°C, atomization pressure 0.1-0.4Mpa, fan frequency 10-55Hz, slurry flow rate 5-30g / min. The drying process conditions are: inlet air temperature 60-90°C, fan frequency 10-55Hz, time 10-60min, and the moisture content of the material after drying is <1%.

[0085] In this embodiment, amaranth is used as a dye to make the coating layer red.

[0086] Comparative Example 1:

[0087] ① Preparation of hydrogel particles: by weight, take 67 parts of sodium carboxymethyl cellulose and 1 part of pectin, dissolve them in 1111 parts of water and stir for 2 hours, dry them at a drying temperature of 110°C for 8 hours, crush and sieve, and take 20-50 mesh hydrogel particles for use.

[0088] Comparative Example 2:

[0089] ① Preparation of hydrogel particles: Take 64 parts of sodium carboxymethyl cellulose and 0.19 parts of malic acid, dissolve them in 1000 parts of water and stir for 6 hours, dry them at 50°C for 72 hours, crush and sieve, take 20-50 mesh hydrogel particles, cross-link them at a drying temperature of 110°C for 2 hours, and set aside.

[0090] Analysis and Conclusion

[0091] 1. Sample evaluation:

[0092] Sample: the anti-sticking mouth hydrogel coated particles obtained in Examples 1-4 and the hydrogel particles obtained in Comparative Examples 1-2

[0093] a. Mouth stickiness sensory test: 20 testers were selected to conduct oral sensory evaluation tests on each sample. The evaluation criteria were divided into four levels:

[0094] Table 1 Test level of sticky mouth sensory evaluation

[0095] grade Sensory description A All of them stick to the mouth and are difficult to swallow. Even after drinking water, most of the particles are still stuck in the mouth. B Half of them stick to the mouth and are difficult to swallow. After drinking water, more particles stick to the mouth. C A small amount sticks to the mouth, can be swallowed, and a small amount of particles adhere to the mouth after drinking water D No sticking to the mouth, easy to swallow, no particles sticking to the mouth after drinking water

[0096] b. Short-time expansion multiple test: Take samples according to the content of 1g hydrogel particles in the sample (calculated as pure hydrogel particles), put each sample into a clean beaker filled with 100ml purified water, place it in a constant temperature water bath at 37℃, and observe and measure the expansion multiples at 10s, 20s, 30s, 60s, and 120s.

[0097] c. Long-term expansion multiple test: Samples (based on pure hydrogel particles) were taken according to the content of 1g hydrogel particles in the sample and placed in a clean beaker containing 200ml simulated gastric juice (artificial gastric juice: water = 1:8), placed in a 37°C constant temperature water bath for 30min or 60min, then poured into a 40-mesh stainless steel sieve (weight M1) and allowed to stand for 10 minutes, weighed M2, and the water absorption multiple was calculated according to the following formula:

[0098] Expansion multiple = (M2-M1-1) / 1.

[0099] Prepare artificial gastric juice according to the Chinese Pharmacopoeia 2010 edition as follows: Take 16.4 ml of dilute hydrochloric acid, add about 800 ml of water and 10 g of pepsin, shake well, and dilute with water to 1000 ml.

[0100] d. Moisture-proof performance test: Place each sample in a constant temperature and humidity chamber, set the temperature to 30°C and the humidity to 65%. Take 3g of sample every 2h, 6h, 12h, 24h, and 48h and place it in a rapid moisture analyzer to measure the moisture content. The test temperature is 105°C and the constant weight time is 50s.

[0101] 2. Results and analysis:

[0102] Table 2 Sticky mouth sensory evaluation test results

[0103]

[0104]

[0105] Table 3 Short-time expansion multiple test results

[0106]

[0107] Table 4 Long-term expansion multiple test results

[0108] project 30min expansion multiple 60min expansion multiple The anti-sticking mouth hydrogel coated granules obtained in Example 1 100.9 103.6 Anti-sticking mouth hydrogel coated granules obtained in Example 2 108.2 109.1 Example 3 Anti-sticking mouth hydrogel coated particles 101.5 103.9 Example 4 Anti-sticking mouth hydrogel coated particles 102.4 104.6 Hydrogel particles obtained in Comparative Example 1 104.6 105.8 Hydrogel particles obtained in Comparative Example 2 110.2 110.6

[0109] Table 5 Moisture test results (water content, %)

[0110]

[0111]

[0112] Figure 1 This is a microscopic photograph of the cross section of the anti-sticking hydrogel coated particles prepared in Example 5, wherein 1 is the hydrogel particles (the yellow substance in the inner layer) and 2 is the coating layer (the red substance in the outer layer), indicating that through the coating process, the hydrogel particles can be well coated in the coating layer.

[0113] The test results in Table 2 and Table 3 show that the samples of Examples 1, 2, 3, and 4 all have good anti-sticking mouth performance, and the anti-sticking mouth performance of the samples of Examples 3 and 4 is better. The reason is that the coating layer of the samples of Examples 1 and 2 is a water-soluble film-forming matrix such as hydroxypropyl methylcellulose and polyvinyl alcohol. The film formed after coating will dissolve quickly after entering the oral cavity, but the melted macromolecular substances will still adhere to the surface of the hydrogel particles in a short time, thereby inhibiting the capillary effect of the three-dimensional network structure, reducing the water absorption capacity of the hydrogel, and achieving the effect of anti-sticking mouth. While Examples 3 and 4 use non-water-soluble film-forming matrices such as ethyl cellulose and chitosan. The film formed after coating will not dissolve in a short time, which can prevent the particles from directly contacting the water molecules in the saliva, thereby preventing the phenomenon of adhering to the oral cavity when the particles are swallowed directly. The samples of Comparative Examples 1 and 2 are uncoated hydrogel particles, so the hydrophilic effect and capillary effect of the particles cannot be suppressed, and water can be quickly absorbed in the oral cavity, thereby causing sticking mouth.

[0114] The long-term swelling multiple test results in Table 4 show that the samples of Examples 1, 2, 3, and 4 can reach the water absorption swelling multiples of Comparative Examples 1 and 2 at 30 min and 60 min in simulated gastric juice. The reason is that the coating layer matrix can be disintegrated in acidic gastric juice and does not affect the final water absorption swelling multiple of the hydrogel particles.

[0115] The moisture test results in Table 5 show that the samples of Examples 1, 2, 3, and 4 all have good moisture resistance, and the moisture resistance of the samples of Examples 3 and 4 is better, and the reason is consistent with the reason for its anti-sticking mouth. Since the hydrogel particles are in contact with water vapor in the air in the constant temperature and humidity chamber, rather than directly in contact with water like in the oral cavity, even if the coating layer of Examples 1 and 2 is a water-soluble film-forming matrix, the water absorption speed in the constant temperature and humidity chamber is still slow, and it can still play a good moisture-proof effect (based on the water content of the hydrogel particles being less than 5% in 6 hours). Due to the presence of the non-water-soluble film-forming matrix, the moisture-proof time of Examples 3 and 4 in the constant temperature and humidity chamber can reach more than 48 hours.

[0116] In summary, the present invention utilizes the characteristics of each film-forming material and the characteristics of short-time dissolution to inhibit the capillary effect of hydrogel, and creatively covers it on the hydrogel particles through thin film coating technology, thereby solving the defects of hydrogel particles being easy to stick to the mouth when drinking directly and being easy to absorb moisture when exposed to air for a short period of time, and does not affect its original water absorption and expansion performance, improves the taste of hydrogel particles, and enriches its application scenarios; because hydrogel particles have strong water absorption characteristics, specific coating layer materials are selected, and the optimal coating process is explored accordingly, so that the hydrogel particles will not be disturbed by the water in the coating layer slurry during the preparation process, and the final anti-sticking mouth hydrogel coated particles have excellent finished product performance.

[0117] The above embodiments are only preferred implementation modes of the present invention and are only used to explain the present invention rather than to limit the present invention. Any changes, substitutions, modifications, etc. made by those skilled in the art without departing from the spirit of the present invention should fall within the scope of protection of the present invention.

Claims

1. A mouth-adhesive hydrogel-coated granule, characterized in that: From the inside to the outside, it includes hydrogel particles and a coating layer, wherein the mass of the hydrogel particles accounts for 50%-99% of the total mass of the anti-sticking nozzle hydrogel coated particles, and the coating layer accounts for 1%-50% of the total mass of the anti-sticking nozzle hydrogel coated particles; The coating layer comprises a film-forming matrix and a plasticizer, wherein the film-forming matrix accounts for 50%-100% of the mass of the coating layer, and the plasticizer accounts for 0-50% of the mass of the coating layer.

2. The anti-sticking mouth hydrogel coated granules according to claim 1, characterized in that: The mass of the hydrogel particles accounts for 65%-95% of the total mass of the anti-sticking mouth hydrogel coated particles, and the coating layer accounts for 5%-35% of the total mass of the anti-sticking mouth hydrogel coated particles; and / or, The film-forming matrix accounts for 60%-100% of the coating layer's mass, and the plasticizer accounts for 0-40% of the coating layer's mass.

3. The anti-sticking mouth hydrogel coated granules according to claim 1, characterized in that: The film-forming matrix comprises one or more of hydroxypropyl methylcellulose, sodium carboxymethyl cellulose, polyvinyl alcohol, hydroxypropyl cellulose, ethyl cellulose, cellulose acetate phthalate and chitosan; and / or, The plasticizer includes polyethylene glycol and / or glycerol.

4. The anti-mouth-sticking hydrogel coated granules according to claim 1 or 3, characterized in that: The film-forming matrix is ​​a water-soluble film-forming matrix, including one or more of hydroxypropyl methylcellulose, sodium carboxymethyl cellulose, polyvinyl alcohol and hydroxypropyl cellulose.

5. The anti-mouth-sticking hydrogel coated granules according to claim 1 or 3, characterized in that: The film-forming matrix is ​​a water-insoluble film-forming matrix, which includes one or more of ethyl cellulose, cellulose acetate phthalate and chitosan.

6. The anti-sticking mouth hydrogel coated granules according to claim 1, characterized in that: The hydrogel particles include chemically cross-linked hydrogel particles and / or physically cross-linked hydrogel particles.

7. The anti-mouth-sticking hydrogel coated granules according to claim 6, characterized in that: The chemically cross-linked hydrogel particles include hydrogels obtained by chemically cross-linking cellulose or its derivatives with dibasic acid or polybasic acid; and / or, the physically cross-linked hydrogel particles include hydrogels obtained by physically cross-linking cellulose or its derivatives with polysaccharide gum; The cellulose or its derivatives include one or more of carboxymethyl cellulose, methyl cellulose, ethyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, hydroxypropyl methyl cellulose, carboxymethyl hydroxyethyl cellulose, carboxymethyl hydroxypropyl cellulose and carboxymethyl ethyl cellulose or their derivatives; The dibasic acid or polybasic acid includes one or more of tartaric acid, malic acid, and citric acid; The polysaccharide gum includes one or more of pectin, xanthan gum, guar gum, locust bean gum, carrageenan, konjac gum, gellan gum, agar, sachets gum and welan gum.

8. The method for preparing the anti-sticking mouth hydrogel coated particles according to any one of claims 1 to 7, characterized in that: The following steps are involved: (1) Preparation of hydrogel particles: crushing the hydrogel into 20-50 meshes to obtain hydrogel particles; (2) Preparation of coating slurry: dissolve the film-forming matrix and plasticizer and stir them evenly for use; (3) Coating: The coating layer slurry is sprayed on the surface of the hydrogel particles by high-pressure atomization using a fluidized bed coating process, and then dried to obtain an anti-sticking hydrogel coated particle.

9. The preparation method according to claim 8, characterized in that: The coating process conditions are: inlet air temperature 45-80°C, atomization pressure 0.1-0.4Mpa, fan frequency 10-55Hz, slurry flow rate 5-30g / min; and / or, the drying process conditions are: inlet air temperature 60-90°C, fan frequency 10-55Hz, time 10-60min.

10. The preparation method according to claim 8, characterized in that: In step (2), the solvent used to dissolve the film-forming matrix and the plasticizer includes water, ethanol solution, acidic solution or alkaline solution.

11. The preparation method according to claim 10, characterized in that: The film-forming matrix is ​​ethyl cellulose, and the solvent is ethanol solution; or, The film-forming matrix is ​​cellulose acetate phthalate, and the solvent is an alkaline solution; or, The film-forming matrix is ​​chitosan, and the solvent is an acidic solution.

12. Use of the anti-sticking mouth hydrogel coated granules according to any one of claims 1 to 7 or the anti-sticking mouth hydrogel coated granules prepared by the preparation method according to any one of claims 8 to 11 in preparing food, medicine or health care products with stomach filling, weight control and blood sugar control effects.

13. A weight control composition, characterized in that: The invention comprises the anti-sticking mouth hydrogel coated granules according to any one of claims 1 to 7 or the anti-sticking mouth hydrogel coated granules prepared by the preparation method according to any one of claims 8 to 11, and auxiliary materials.

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