Hydrogel composition as well as preparation method and application thereof
By spraying fluidized bed granules, the Pueraria extract-polyethylene glycol dispersed body is distributed on the surface of hydrogel particles to form a hydrogel composition, which solves the low efficiency of the existing alcoholic alcohol-absorbing alcohol and the stomach. The problem of large mucosal stimulation achieves the effect of high -efficiency adsorption of ethanol and protecting gastric mucosa.
Patent Information
- Application Number
- CN202411930095.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-26
- Publication Date
- 2025-01-28
- Estimated Expiration
- Not applicable · inactive patent
AI Technical Summary
The existing alcohol-relieving liver-protecting products have low efficiency in adsorption of alcohol and are highly irritating to the gastric mucosa, which cannot effectively slow down the absorption rate of alcohol and protect the liver.
By spraying fluidized bed granules technology, pueraria extract-polyethylene glycol dispersed body is evenly distributed on the surface of hydrogel particles to form a hydrogel composition to improve the solubility and absorption efficiency of Puerase, delay the stomach empty, and delay the stomach empty. Slowness alcohol absorption and protecting the gastrointestinal mucosa.
It significantly improves the effect of a hydrogel composition in the stomach to adsorb the ethanol aquatic solution. It retains that ethanol is not released, protects the gastric mucosa, reduces the concentration of alcohol in the blood, and has a significant effect of hangover and liver protection.
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Abstract
Description
Technical Field
[0001] The invention belongs to the field of physical methods, and relates to a physical method carried out in the presence of fluid and solid particles, and in particular to a hydrogel composition, a preparation method and an application thereof. Background Art
[0002] China has a long history of winemaking and a prevalent wine culture. With the improvement of economic level, social events, family gatherings, and gatherings with friends are inseparable from wine. However, excessive drinking affects physical health. The World Health Organization points out that alcoholism is still one of the public hazards in the world today. Excessive drinking and diseases and problems caused by alcohol are also increasing. Most of the ethanol that enters the body is metabolized by the liver and has strong toxicity to the liver, such as lipid peroxidation on the surface of the liver cell membrane and damage to the liver cell membrane. Long-term drinking will also damage the microtubules and mitochondria in the liver cells, causing metabolic disorders in the cells, producing cytotoxic metabolites, and causing swelling and necrosis of liver cells. Therefore, the development of alcohol sobering products is very necessary. Patent CN118058405A discloses a sobering and liver-protecting drink with short-chain fatty acids as the core ingredient, which works by accelerating the rate at which the human body metabolizes ethanol and protecting the liver. Patent CN117958369A discloses a solid drink with the function of sobering and liver-protecting with the core of supplementing alcohol dehydrogenase, acetaldehyde dehydrogenase, and medicinal and edible extracts, which works by accelerating the rate at which the human body metabolizes ethanol and protecting the liver. The above methods are all indirect sobering methods, which work slowly and cannot directly reduce the absorption of alcohol. Patent CN113854578 A provides a jelly-like edible hydrogel with sobering and liver-protecting functions, which is prepared in advance with psyllium husk powder premix, konjac flour, carrageenan, xanthan gum, pectin, citric acid, etc. as raw materials, but 1g of hydrogel can only absorb 0.55g of pure ethanol, and the efficiency of alcohol adsorption is low. Patent CN110787185A discloses a hangover-resolving and liver-protecting hydrogel composition with chitosan, sodium alginate, gelatin, calcium carbonate and gallic acid as core ingredients. The composition has chitosan, sodium alginate and calcium carbonate as the inner layer and gelatin and gallic acid as the outer coating. The onset of action is that the gelatin membrane dissolves, gastric acid contacts calcium carbonate to react and produce carbon dioxide gas and calcium ions, and the calcium ions then form a gel with sodium alginate. This process consumes gastric acid and produces carbon dioxide gas, which has a great irritation to the gastric mucosa.
[0003] Therefore, it is necessary to develop products with high alcohol adsorption efficiency and both gastric mucosa protection and liver protection. Traditional Chinese medicine believes that Pueraria root can sober up and protect the liver. Modern medical research has found that the main active ingredient in Pueraria root is puerarin. The literature "Protective effect of isoflavones and triterpenoid saponins from pueraria lobata on liver diseases: A review" reveals that puerarin has a protective effect on liver damage caused by long-term drinking, involving multiple mechanisms: 1) Puerarin can delay gastric emptying, slow down the absorption rate of alcohol, reduce intestinal wall permeability, and protect the gastrointestinal mucosa; 2) Puerarin activates the ethanol metabolic enzymes ADH and ALDH, while selectively inhibiting cytochrome P450 2E1 (CYP2E1), reducing the production of free radicals in the alcohol metabolism process and reducing oxidative stress in the liver. High-purity puerarin has many side effects, so natural Pueraria root extract is a better choice, but Pueraria root extract with a high puerarin content has problems such as low solubility and poor uniformity when mixed with hydrogel. Summary of the invention
[0004] In order to overcome the above-mentioned deficiencies in the prior art, the purpose of the present invention is to provide a hydrogel composition and a preparation method and application thereof, wherein a pueraria extract-polyethylene glycol dispersion is atomized and sprayed on the surface of hydrogel particles, and while the hydrogel particles absorb water and ethanol, the solubility of puerarin in the stomach and intestine is increased, so that puerarin enters the digestive juice and synergistically exerts the effect of sobering up and protecting the liver with the hydrogel particles.
[0005] The purpose of the present invention is achieved by at least one of the following technical solutions.
[0006] The present invention provides a method for preparing a hydrogel composition. The raw materials of the hydrogel composition include, by weight: 80-90 parts of hydrogel particles, 9-18 parts of polyethylene glycol, and 1-4 parts of kudzu root extract; The preparation method comprises the following steps: (1) Preparation of hydrogel particles: crushing the hydrogel into 20-50 meshes to obtain hydrogel particles; (2) Preparation of Pueraria extract-polyethylene glycol dispersion: After heating and melting polyethylene glycol, add Pueraria extract and stir to dissolve to obtain Pueraria extract-polyethylene glycol dispersion, and keep warm for later use; the average molecular weight of the polyethylene glycol is 4000-8000Da; (3) Preparation of hydrogel composition: The kudzu root extract-polyethylene glycol dispersion is sprayed on the surface of the hydrogel particles by high-pressure atomization by a spray fluidized bed granulation technology, and the hydrogel composition is cured by cold air. The process parameters of the spray fluidized bed granulation technology are as follows: inlet air temperature: 2-10°C, outlet air temperature 2-20°C, atomization pressure: 0.1MPa-0.5MPa, fan frequency: 20-50Hz, slurry flow rate 0.5g / min-5g / min; There is no order of precedence for steps (1) and (2).
[0007] Furthermore, in step (1), the hydrogel includes a chemically cross-linked hydrogel and / or a physically cross-linked hydrogel.
[0008] Furthermore, the chemically cross-linked hydrogel includes a hydrogel obtained by chemically cross-linking cellulose or its derivatives with a dibasic acid or a polybasic acid; and / or, the physically cross-linked hydrogel includes a hydrogel obtained by physically cross-linking cellulose or its derivatives with a 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 or polybasic acid comprises 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.
[0009] More preferably, the hydrogel is formed by physically cross-linking sodium carboxymethyl cellulose and pectin; and / or, the hydrogel is formed by chemically cross-linking sodium carboxymethyl cellulose and malic acid.
[0010] Furthermore, in step (2), the polyethylene glycol is polyethylene glycol 6000.
[0011] Furthermore, in step (2), the puerarin content in the kudzu root extract is greater than or equal to 5%.
[0012] Furthermore, in step (2), the content of puerarin in the kudzu root extract is 5%-20%.
[0013] Furthermore, in step (2), the mass ratio of the polyethylene glycol to the kudzu root extract is 4-9:1.
[0014] Furthermore, in step (2), the mass ratio of polyethylene glycol to kudzu root extract is 9:1.
[0015] Furthermore, in step (2), the heating is water bath heating, and the heating temperature is 70-90°C.
[0016] Furthermore, in step (3), the equipment used in the fluidized bed granulation technology is a boiling granulator.
[0017] Furthermore, in step (3), the content of puerarin in the hydrogel composition is 0.05%-0.8%.
[0018] Furthermore, in step (3), the mass ratio of the kudzu root extract-polyethylene glycol dispersion to the hydrogel particles is 1:4-9.
[0019] Furthermore, in the raw materials of the hydrogel composition, the mass of hydrogel particles: the mass of polyethylene glycol: the mass of puerarin extract = 4000-9000: 800-900: 100-200.
[0020] Furthermore, in the raw materials of the hydrogel composition, the mass of the hydrogel particles: the mass of the polyethylene glycol: the mass of the puerarin extract is 4000:900:100, 9000:900:100 or 4000:800:200.
[0021] The present invention provides a hydrogel composition prepared by any one of the above preparation methods. The raw materials of the hydrogel composition include, by weight: 80-90 parts of hydrogel particles, 9-18 parts of polyethylene glycol, and 1-4 parts of kudzu root extract. The content of puerarin in the hydrogel composition is 0.05%-0.8%.
[0022] The present invention also provides the use of the hydrogel composition prepared by any of the above preparation methods or the above hydrogel composition in the preparation of drugs, foods or health products for sobering up, protecting the liver and / or protecting the gastrointestinal mucosa.
[0023] Compared with the prior art, the present invention has the following advantages and beneficial effects: (1) The present invention uses a spray fluidized bed granulation technology to evenly distribute the pueraria extract-polyethylene glycol dispersion on the surface of the hydrogel particles by spraying, thereby overcoming the problem of poor uniformity when the puerarin extract and the hydrogel particles are directly mixed. The resulting hydrogel composition particles have a regular shape and a smooth appearance.
[0024] (2) The present invention uses hot polyethylene glycol 6000 to mix with kudzu root extract to prepare kudzu root extract-polyethylene glycol dispersion. The kudzu root extract-polyethylene glycol dispersion is combined with hydrogel particles formed by physical crosslinking of sodium carboxymethyl cellulose and pectin or hydrogel particles formed by chemical crosslinking of sodium carboxymethyl cellulose and malic acid, which can effectively improve the solubility of puerarin, so that it can smoothly enter the gastric juice environment, play a role in delaying gastric emptying, slowing down the absorption rate of alcohol, and protecting the gastrointestinal mucosa. Part of puerarin enters the blood circulation with alcohol to activate the ethanol metabolic enzymes ADH and ALDH, further playing a role in sobering up and protecting the liver. DETAILED DESCRIPTION
[0025] The first aspect of the present invention provides a method for preparing a hydrogel composition, wherein the raw materials of the hydrogel composition include, by weight: 80-90 parts of hydrogel particles, 9-18 parts of polyethylene glycol, and 1-4 parts of kudzu root extract; The preparation method comprises the following steps: (1) Preparation of hydrogel particles: crushing the hydrogel into 20-50 meshes to obtain hydrogel particles; (2) Preparation of Pueraria extract-polyethylene glycol dispersion: After heating and melting polyethylene glycol, add Pueraria extract and stir to dissolve to obtain Pueraria extract-polyethylene glycol dispersion, and keep warm for later use; the average molecular weight of the polyethylene glycol is 4000-8000Da; (3) Preparation of hydrogel composition: The kudzu root extract-polyethylene glycol dispersion is sprayed on the surface of the hydrogel particles by high-pressure atomization by a spray fluidized bed granulation technology, and the hydrogel composition is cured by cold air. The process parameters of the spray fluidized bed granulation technology are as follows: inlet air temperature: 2-10°C, outlet air temperature 2-20°C, atomization pressure: 0.1MPa-0.5MPa, fan frequency: 20-50Hz, slurry flow rate 0.5g / min-5g / min; There is no order of precedence for steps (1) and (2).
[0026] The present invention uses a spray fluidized bed granulation technology (boiling granulation technology), adopts fluidized air to make hydrogel particles form a fluidized state and move in a device, and uses a spray method to make a kudzu root extract-polyethylene glycol dispersion evenly distributed on the surface of the hydrogel particles. The operation process has a high degree of automation, and the formed hydrogel composition particles have a regular shape and a smooth appearance. In order to ensure that the dispersion liquid condenses on the surface of the hydrogel particles within an appropriate time and to ensure the temperature difference between the hydrogel particles and the dispersion liquid, the air inlet temperature is set to 2-10°C, and the air outlet temperature is set to 2-20°C, which not only ensures the particle size but also is not easy to stick together, the fan frequency is set to 20-50Hz, the dispersion liquid supply flow rate is 0.5g / min-5g / min, and the spraying is uniform, which not only ensures energy consumption but also is not easy to stick together.
[0027] In some embodiments of the present invention, in step (1), the hydrogel includes a chemically crosslinked hydrogel and / or a physically crosslinked hydrogel. Preferably, the chemically crosslinked hydrogel includes a hydrogel obtained by chemically crosslinking cellulose or its derivatives with a dibasic acid or a polybasic acid; and / or, the physically crosslinked hydrogel includes a hydrogel obtained by physically crosslinking cellulose or its derivatives with a 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, trisammonium gum and welan gum. In some specific embodiments of the present invention, the hydrogel is formed by physically crosslinking sodium carboxymethyl cellulose with pectin; and / or, the hydrogel is formed by chemically crosslinking sodium carboxymethyl cellulose with malic acid.
[0028] In some embodiments of the present invention, in step (2), the polyethylene glycol is polyethylene glycol 6000. The inventors have found that by mixing hot polyethylene glycol 6000 with kudzu root extract, a kudzu root extract-polyethylene glycol dispersion can be prepared, in which the kudzu root extract is evenly distributed. When the kudzu root extract-polyethylene glycol dispersion is sprayed on the surface of hydrogel particles formed by physical crosslinking of sodium carboxymethyl cellulose and pectin or by chemical crosslinking of sodium carboxymethyl cellulose and malic acid, in a water / gastric fluid environment, the hydrogel particles absorb a large amount of water and swell to form a three-dimensional network structure, locking water molecules inside the hydrogel, and intensifying the collision / contact between the kudzu root extract-polyethylene glycol dispersion and water molecules, the solubility of puerarin can be effectively improved, so that it can smoothly enter the gastric fluid environment, delaying gastric emptying, slowing down the absorption rate of alcohol, and protecting the gastrointestinal mucosa.
[0029] In some embodiments of the present invention, in step (2), the puerarin content in the kudzu root extract is greater than or equal to 5%. Preferably, in step (2), the puerarin content in the kudzu root extract is 5%-20%. When the puerarin content is too high, cytotoxicity will occur.
[0030] In some embodiments of the present invention, in step (2), the mass ratio of the polyethylene glycol to the kudzu root extract is 4-9:1. Preferably, in step (2), the mass ratio of the polyethylene glycol to the kudzu root extract is 9:1.
[0031] In some embodiments of the present invention, in step (2), the heating is water bath heating, and the heating temperature is 70-90°C.
[0032] In some embodiments of the present invention, in step (3), the equipment used in the fluidized bed granulation technology is a boiling granulator.
[0033] In some embodiments of the present invention, in step (3), the content of puerarin in the hydrogel composition is 0.05%-0.8%.
[0034] In some embodiments of the present invention, in step (3), the mass ratio of the kudzu root extract-polyethylene glycol dispersion to the hydrogel particles is 1:4-9.
[0035] In some embodiments of the present invention, in the raw materials of the hydrogel composition, the mass of hydrogel particles: the mass of polyethylene glycol: the mass of puerarin extract = 4000-9000: 800-900: 100-200. Preferably, in the raw materials of the hydrogel composition, the mass of hydrogel particles: the mass of polyethylene glycol: the mass of puerarin extract is 4000: 900: 100, 9000: 900: 100 or 4000: 800: 200.
[0036] A second aspect of the present invention provides a hydrogel composition prepared by any of the above preparation methods, wherein the raw materials of the hydrogel composition include, by weight: 80-90 parts of hydrogel particles, 9-18 parts of polyethylene glycol, and 1-4 parts of kudzu root extract, and the content of puerarin in the hydrogel composition is 0.05%-0.8%.
[0037] The third aspect of the present invention provides the use of the hydrogel composition prepared by any of the above preparation methods in the preparation of drugs, foods or health products for sobering up, protecting the liver and / or protecting the gastrointestinal mucosa.
[0038] 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.
[0039] Among them, Pueraria extract was purchased from Nanjing Zhenweikang Biotechnology Co., Ltd. (puerarin content 5%, 20%), puerarin (purity > 98%) was purchased from Shanghai Saiyi Biotechnology Co., Ltd., and polyethylene glycol was purchased from Shandong Ruisheng Pharmaceutical Excipients Co., Ltd. (type 2000, type 4000, type 6000, type 8000, type 10000). Example 1: Physically cross-linked hydrogel composition containing 0.4% puerarin
[0040] This example is a composition of sodium carboxymethylcellulose and pectin physically cross-linked hydrogel, kudzu root extract, and polyethylene glycol, with a puerarin content of 0.4%.
[0041] (1) Preparation of hydrogel particles: 300 g of pectin was placed in 333 L of ultrapure water and stirred to dissolve. 20 kg of sodium carboxymethyl cellulose was added to the pectin solution and stirred for 2 h. The solution was then dried in a forced air drying oven at 110 °C for 8 h. After drying, the solution was crushed into particles of 20-50 mesh to obtain hydrogel particles. 4 kg of the solution was taken for later use.
[0042] (2) Preparation of Pueraria extract-polyethylene glycol dispersion: 900 g of polyethylene glycol 4000 was placed in a water bath at 80°C and heated. After melting, 100 g of Pueraria extract (20% puerarin content) was added and stirred to dissolve to obtain Pueraria extract-polyethylene glycol dispersion, which was kept warm at 80°C for later use; (3) Preparation of hydrogel composition: 4 kg of sodium carboxymethyl cellulose-pectin physically cross-linked hydrogel particles were placed in a boiling granulator, and the kudzu root extract-polyethylene glycol dispersion was atomized and sprayed on the surface of the hydrogel particles. The hydrogel particles were cured by cold air to obtain sample 1. The preparation parameters were: inlet air temperature: 2-10°C, outlet air temperature 2-20°C, atomization pressure: 0.2 MPa, fan frequency: 20-50 Hz, and slurry flow rate 1.5 g / min-5 g / min. Example 2: Chemically cross-linked hydrogel composition containing 0.4% puerarin
[0043] This embodiment is a composition of sodium carboxymethylcellulose and malic acid chemically cross-linked hydrogel, kudzu root extract, and polyethylene glycol, and the puerarin content is 0.4%.
[0044] (1) Preparation of hydrogel particles: 30 g of malic acid was placed in 157 L of ultrapure water and stirred to dissolve. 10 kg of sodium carboxymethyl cellulose was added to the malic acid solution and stirred for 6 h to obtain a composite solution (malic acid: sodium carboxymethyl cellulose (wt / wt) = 3:1000, sodium carboxymethyl cellulose concentration is 63.69 g / L). The composite solution was placed in a forced air drying oven and dried at 50 °C for 72 h. After drying, it was crushed into 20-50 mesh particles and cross-linked at 110 °C for 2 h to obtain hydrogel particles. 4 kg of hydrogel particles were taken for later use.
[0045] (2) Preparation of Pueraria extract-polyethylene glycol dispersion: 900 g of polyethylene glycol 6000 was placed in a 90°C water bath and heated. After melting, 100 g of Pueraria extract (20% puerarin content) was added and stirred to dissolve to obtain Pueraria extract-polyethylene glycol dispersion, which was kept warm at 90°C for later use; (3) Preparation of hydrogel composition: 4 kg of sodium carboxymethyl cellulose-malic acid chemically cross-linked hydrogel particles were placed in a boiling granulator, and the kudzu root extract-polyethylene glycol dispersion was atomized and sprayed on the surface of the hydrogel particles. The hydrogel particles were cured by cold air to obtain sample 2. The preparation parameters were as follows: inlet air temperature: 2-10°C, outlet air temperature 2-20°C, atomization pressure: 0.2 MPa, fan frequency: 20-50 Hz, and slurry flow rate 1.5 g / min-5 g / min. Example 3: Physically cross-linked hydrogel composition with 0.05% puerarin content
[0046] This example is a composition of sodium carboxymethylcellulose and pectin physically cross-linked hydrogel, kudzu root extract, and polyethylene glycol, with a puerarin content of 0.05%.
[0047] (1) Preparation of hydrogel particles: 300 g of pectin was placed in 333 L of ultrapure water and stirred to dissolve. 20 kg of sodium carboxymethyl cellulose was added to the pectin solution and stirred for 2 h. The solution was then placed in a forced air drying oven at 110 °C and dried for 8 h. After drying, the solution was crushed into particles of 20-50 mesh to obtain hydrogel particles. 9 kg of the solution was set aside.
[0048] (2) Preparation of Pueraria extract-polyethylene glycol dispersion: 900 g of polyethylene glycol 8000 was placed in a water bath at 80°C and heated. After melting, 100 g of Pueraria extract (5% puerarin content) was added and stirred to dissolve to obtain Pueraria extract-polyethylene glycol dispersion, which was kept warm at 80°C for later use. (3) Preparation of hydrogel composition: 9 kg of sodium carboxymethyl cellulose-pectin physically cross-linked hydrogel particles were placed in a boiling granulator, and the kudzu root extract-polyethylene glycol dispersion was atomized and sprayed on the surface of the hydrogel particles. The hydrogel particles were cured by cold air to obtain sample 3. The preparation parameters were as follows: inlet air temperature: 2-10°C, outlet air temperature 2-20°C, atomization pressure: 0.1 MPa, fan frequency: 20-50 Hz, and slurry flow rate 0.5 g / min-3 g / min. Example 4: Physically cross-linked hydrogel composition with 0.8% puerarin content
[0049] This example is a composition of sodium carboxymethylcellulose and pectin physically cross-linked hydrogel, kudzu root extract, and polyethylene glycol, with a puerarin content of 0.8%.
[0050] (1) Preparation of hydrogel particles: 300 g of pectin was placed in 333 L of ultrapure water and stirred to dissolve. 20 kg of sodium carboxymethyl cellulose was added to the pectin solution and stirred for 2 h. The solution was then dried in a forced air drying oven at 110 °C for 8 h. After drying, the solution was crushed into particles of 20-50 mesh to obtain hydrogel particles. 4 kg of the solution was taken for later use.
[0051] (2) Preparation of Pueraria extract-polyethylene glycol dispersion: 800 g of polyethylene glycol 6000 was placed in a water bath at 80°C and heated. After melting, 200 g of Pueraria extract (20% puerarin content) was added and stirred to dissolve to obtain Pueraria extract-polyethylene glycol dispersion, which was kept warm at 80°C for later use; (3) Preparation of hydrogel composition: 4 kg of sodium carboxymethyl cellulose-pectin physically cross-linked hydrogel particles were placed in a boiling granulator, and the kudzu root extract-polyethylene glycol dispersion was atomized and sprayed on the surface of the hydrogel particles. The hydrogel particles were cured by cold air to obtain sample 3. The preparation parameters were as follows: inlet air temperature: 2-10°C, outlet air temperature 2-20°C, atomization pressure: 0.5 MPa, fan frequency: 30-50 Hz, and slurry flow rate 1.5 g / min-5 g / min. Comparative Example 1
[0052] In this comparative example, sodium carboxymethyl cellulose was directly mixed with 4 kg of pectin physically cross-linked hydrogel, 900 g of polyethylene glycol 4000 and 100 g of kudzu root extract (with a puerarin content of 20%).
[0053] (1) Preparation of hydrogel particles: 300 g of pectin was placed in 333 L of ultrapure water and stirred to dissolve. 20 kg of sodium carboxymethyl cellulose was added to the pectin solution and stirred for 2 h. The solution was then dried in a forced air drying oven at 110 °C for 8 h. After drying, the solution was crushed into particles of 20-50 mesh to obtain hydrogel particles. 4 kg of the solution was taken for later use.
[0054] (2) Mixing: Put 100 g of Pueraria root extract, 900 g of polyethylene glycol 4000 and 4 kg of sodium carboxymethyl cellulose pectin particles into a small three-dimensional mixer and mix for 30 minutes to obtain control sample 1. Comparative Example 2
[0055] This comparative example uses hydrogel particles of 50-80 mesh, and the rest is the same as Example 1.
[0056] (1) Preparation of hydrogel particles: 300 g of pectin was placed in 333 L of ultrapure water and stirred to dissolve. 20 kg of sodium carboxymethyl cellulose was added to the pectin solution and stirred for 2 h. The solution was then placed in a forced air drying oven at 110 °C and dried for 8 h. After drying, the solution was crushed to obtain particles of 50-80 mesh. Hydrogel particles were obtained and 4 kg was reserved.
[0057] (2) Preparation of Pueraria extract-polyethylene glycol dispersion: Take 900 g of polyethylene glycol 4000 and place it in a water bath at 80°C for heating. After melting, add 100 g of Pueraria extract (20% puerarin content) and stir to dissolve to obtain Pueraria extract-polyethylene glycol dispersion. Keep it warm at 80°C for later use.
[0058] (3) Preparation of hydrogel composition: 4 kg of sodium carboxymethyl cellulose-pectin physically cross-linked hydrogel particles were placed in a boiling granulator, and the kudzu root extract-polyethylene glycol dispersion was atomized and sprayed on the surface of the hydrogel particles. The sample was cured by cold air to obtain comparative sample 2. The preparation parameters were as follows: inlet air temperature: 2-10°C, outlet air temperature 2-20°C, atomization pressure: 0.2 MPa, fan frequency: 20-50 Hz, and slurry flow rate 1.5 g / min-5 g / min. Comparative Example 3
[0059] In this comparative example, polyethylene glycol 10000 is used to prepare the composite hydrogel, and the rest is the same as in Example 1. Blockage is very likely to occur during the spraying process, the production is difficult, and continuous production is impossible.
[0060] (1) Preparation of hydrogel particles: 300 g of pectin was placed in 333 L of ultrapure water and stirred to dissolve. 20 kg of sodium carboxymethyl cellulose was added to the pectin solution and stirred for 2 h. The solution was then placed in a forced air drying oven at 110 °C and dried for 8 h. After drying, the solution was crushed to obtain particles of 20-50 mesh. Hydrogel particles were obtained and 4 kg was reserved.
[0061] (2) Preparation of Pueraria extract-polyethylene glycol dispersion: Take 900 g of polyethylene glycol 10000 and place it in a water bath at 80°C for heating. After melting, add 100 g of Pueraria extract (20% puerarin content) and stir to dissolve to obtain Pueraria extract-polyethylene glycol dispersion. Keep it warm at 80°C for later use.
[0062] (3) Preparation of hydrogel composition: 4 kg of sodium carboxymethyl cellulose-pectin physically cross-linked hydrogel particles were placed in a boiling granulator, and the kudzu root extract-polyethylene glycol dispersion was atomized and sprayed on the surface of the hydrogel particles. The hydrogel particles were cured by cold air to obtain comparative sample 3. The preparation parameters were as follows: inlet air temperature: 2-10°C, outlet air temperature 2-20°C, atomization pressure: 0.2 MPa, fan frequency: 20-50 Hz, and slurry flow rate 1.5 g / min-5 g / min. Comparative Example 4
[0063] In this comparative example, polyethylene glycol 2000 is used to prepare the composite hydrogel, and the rest is the same as that of Example 1. However, the melting temperature of polyethylene glycol 2000 is between 49-53° C., and it is easy to cause adhesion in hot weather, which is not conducive to transportation.
[0064] (1) Preparation of hydrogel particles: 300 g of pectin was placed in 333 L of ultrapure water and stirred to dissolve. 20 kg of sodium carboxymethyl cellulose was added to the pectin solution and stirred for 2 h. The solution was then placed in a forced air drying oven at 110 °C and dried for 8 h. After drying, the solution was crushed to obtain particles of 20-50 mesh. Hydrogel particles were obtained and 4 kg was reserved.
[0065] (2) Preparation of Pueraria extract-polyethylene glycol dispersion: Take 900 g of polyethylene glycol 2000 and place it in a water bath at 80°C for heating. After melting, add 100 g of Pueraria extract (20% puerarin content) and stir to dissolve to obtain Pueraria extract-polyethylene glycol dispersion. Keep it warm at 80°C for later use.
[0066] (3) Preparation of hydrogel composition: 4 kg of sodium carboxymethyl cellulose-pectin physically cross-linked hydrogel particles were placed in a boiling granulator, and the kudzu root extract-polyethylene glycol dispersion was atomized and sprayed on the surface of the hydrogel particles. The sample was cured by cold air to obtain comparative sample 4. The preparation parameters were as follows: inlet air temperature: 2-10°C, outlet air temperature 2-20°C, atomization pressure: 0.2 MPa, fan frequency: 20-50 Hz, and slurry flow rate 1.5 g / min-5 g / min. Comparative Example 5
[0067] The content of the hydrogel particles in this comparative example is 70%, the content of the kudzu root extract-polyethylene glycol dispersion is 30%, and the rest is the same as in Example 1.
[0068] (1) Preparation of hydrogel particles: 300 g of pectin was placed in 333 L of ultrapure water and stirred to dissolve. 20 kg of sodium carboxymethyl cellulose was added to the pectin solution and stirred for 2 h. The solution was then dried in a forced air drying oven at 110 °C for 8 h. After drying, the solution was crushed to obtain 20-50 mesh particles to obtain hydrogel particles. 3.5 kg of the particles were reserved.
[0069] (2) Preparation of Pueraria extract-polyethylene glycol dispersion: Take 1350g of polyethylene glycol 4000 and heat it in a water bath at 80°C. After it melts, add 150g of Pueraria extract (20% puerarin content) and stir to dissolve to obtain Pueraria extract-polyethylene glycol dispersion. Keep it warm at 80°C for later use.
[0070] (3) Preparation of hydrogel composition: 3.5 kg of sodium carboxymethyl cellulose-pectin physically cross-linked hydrogel particles were placed in a boiling granulator, and the kudzu root extract-polyethylene glycol dispersion was atomized and sprayed on the surface of the hydrogel particles. The sample was cured by cold air to obtain comparative sample 5. The preparation parameters were as follows: inlet air temperature: 2-10°C, outlet air temperature 2-20°C, atomization pressure: 0.2 MPa, fan frequency: 20-50 Hz, and slurry flow rate 1.5 g / min-5 g / min. Comparative Example 6
[0071] The material ratio of this comparative example is the same as that of Example 1, except for the inlet air temperature and the outlet air temperature. Under this parameter, due to the small temperature difference between the solid and the liquid, the liquid condensation time is too long, and then adhesion and agglomeration occur, making production impossible.
[0072] (1) Preparation of hydrogel particles: 300 g of pectin was placed in 333 L of ultrapure water and stirred to dissolve. 20 kg of sodium carboxymethyl cellulose was added to the pectin solution and stirred for 2 h. The solution was then placed in a forced air drying oven at 110 °C and dried for 8 h. After drying, the solution was crushed to obtain particles of 20-50 mesh. Hydrogel particles were obtained and 4 kg was reserved.
[0073] (2) Preparation of Pueraria extract-polyethylene glycol dispersion: Take 900 g of polyethylene glycol 4000 and place it in a water bath at 80°C for heating. After melting, add 100 g of Pueraria extract (20% puerarin content) and stir to dissolve to obtain Pueraria extract-polyethylene glycol dispersion. Keep it warm at 80°C for later use.
[0074] (3) Preparation of hydrogel composition: 4 kg of sodium carboxymethyl cellulose-pectin physically cross-linked hydrogel particles were placed in a boiling granulator, and the kudzu root extract-polyethylene glycol dispersion was atomized and sprayed on the surface of the hydrogel particles. The sample was cured by cold air to obtain comparative sample 6. The preparation parameters were as follows: inlet air temperature: 11-20°C, outlet air temperature 11-30°C, atomization pressure: 0.2 MPa, fan frequency: 20-50 Hz, and slurry flow rate 1.5 g / min-5 g / min. Comparative Example 7
[0075] This comparative example uses hydrogel particles of 10-20 mesh, and the rest are the same as Example 1. Since the particle size is too coarse, the fluidization state of the particles is poor and the bottom is seriously adhered and agglomerated.
[0076] (1) Preparation of hydrogel particles: 300 g of pectin was placed in 333 L of ultrapure water and stirred to dissolve. 20 kg of sodium carboxymethyl cellulose was added to the pectin solution and stirred for 2 h. The solution was then placed in a forced air drying oven at 110 °C and dried for 8 h. After drying, the solution was crushed to obtain 10-20 mesh particles to obtain hydrogel particles. 4 kg of the particles were reserved.
[0077] (2) Preparation of Pueraria extract-polyethylene glycol dispersion: Take 900 g of polyethylene glycol 4000 and place it in a water bath at 80°C for heating. After melting, add 100 g of Pueraria extract (20% puerarin content) and stir to dissolve to obtain Pueraria extract-polyethylene glycol dispersion. Keep it warm at 80°C for later use.
[0078] (3) Preparation of hydrogel composition: 4 kg of sodium carboxymethyl cellulose-pectin physically cross-linked hydrogel particles were placed in a boiling granulator, and the kudzu root extract-polyethylene glycol dispersion was atomized and sprayed on the surface of the hydrogel particles. The hydrogel particles were cured by cold air to obtain comparative sample 7. The preparation parameters were as follows: inlet air temperature: 2-10°C, outlet air temperature 2-20°C, atomization pressure: 0.2 MPa, fan frequency: 20-50 Hz, and slurry flow rate 1.5 g / min-5 g / min. Comparative Example 8
[0079] The material ratio of this comparative example is the same as that of Example 1, except that the fan frequency is too small. Under this parameter, the fan frequency is too small and the air volume is insufficient, resulting in poor fluidization of the particles, and then serious agglomeration occurs, making production impossible.
[0080] (1) Preparation of hydrogel particles: 300 g of pectin was placed in 333 L of ultrapure water and stirred to dissolve. 20 kg of sodium carboxymethyl cellulose was added to the pectin solution and stirred for 2 h. The solution was then placed in a forced air drying oven at 110 °C and dried for 8 h. After drying, the solution was crushed to obtain particles of 20-50 mesh. Hydrogel particles were obtained and 4 kg was reserved.
[0081] (2) Preparation of Pueraria extract-polyethylene glycol dispersion: Take 900 g of polyethylene glycol 4000 and place it in a water bath at 80°C for heating. After melting, add 100 g of Pueraria extract (20% puerarin content) and stir to dissolve to obtain Pueraria extract-polyethylene glycol dispersion. Keep it warm at 80°C for later use.
[0082] (3) Preparation of hydrogel composition: 4 kg of sodium carboxymethyl cellulose-pectin physically cross-linked hydrogel particles were placed in a boiling granulator, and the kudzu root extract-polyethylene glycol dispersion was atomized and sprayed on the surface of the hydrogel particles. The sample was cured by cold air to obtain comparative sample 8. The preparation parameters were as follows: inlet air temperature: 2-10°C, outlet air temperature 2-20°C, atomization pressure: 0.2 MPa, fan frequency: 10-19 Hz, and slurry flow rate 1.5 g / min-5 g / min. Comparative Example 9
[0083] The material ratio of this comparative example is the same as that of Example 1, except that the fan frequency is too large. Under this parameter, due to the excessive fan frequency, most of the particles are concentrated in the middle and upper parts, and the dispersion condenses on the sides and bottom of the cavity, making production impossible.
[0084] (1) Preparation of hydrogel particles: 300 g of pectin was placed in 333 L of ultrapure water and stirred to dissolve. 20 kg of sodium carboxymethyl cellulose was added to the pectin solution and stirred for 2 h. The solution was then placed in a forced air drying oven at 110 °C and dried for 8 h. After drying, the solution was crushed to obtain particles of 20-50 mesh. Hydrogel particles were obtained and 4 kg was reserved.
[0085] (2) Preparation of Pueraria extract-polyethylene glycol dispersion: Take 900 g of polyethylene glycol 4000 and place it in a water bath at 80°C for heating. After melting, add 100 g of Pueraria extract (20% puerarin content) and stir to dissolve to obtain Pueraria extract-polyethylene glycol dispersion. Keep it warm at 80°C for later use.
[0086] (3) Preparation of hydrogel composition: 4 kg of sodium carboxymethyl cellulose-pectin physically cross-linked hydrogel particles were placed in a boiling granulator, and the kudzu root extract-polyethylene glycol dispersion was atomized and sprayed on the surface of the hydrogel particles. The hydrogel particles were cured by cold air to obtain comparative sample 9. The preparation parameters were as follows: inlet air temperature: 2-10°C, outlet air temperature 2-20°C, atomization pressure: 0.2 MPa, fan frequency: 51-60 Hz, and slurry flow rate 1.5 g / min-5 g / min. Comparative Example 10
[0087] The material ratio of this comparative example is the same as that of Example 1, except that the slurry flow rate is too high. Under this parameter, due to the excessively fast flow rate, serious adhesion and agglomeration occur, making production impossible.
[0088] (1) Preparation of hydrogel particles: 300 g of pectin was placed in 333 L of ultrapure water and stirred to dissolve. 20 kg of sodium carboxymethyl cellulose was added to the pectin solution and stirred for 2 h. The solution was then placed in a forced air drying oven at 110 °C and dried for 8 h. After drying, the solution was crushed to obtain particles of 20-50 mesh. Hydrogel particles were obtained and 4 kg was reserved.
[0089] (2) Preparation of Pueraria extract-polyethylene glycol dispersion: Take 900 g of polyethylene glycol 4000 and place it in a water bath at 80°C for heating. After melting, add 100 g of Pueraria extract (20% puerarin content) and stir to dissolve to obtain Pueraria extract-polyethylene glycol dispersion. Keep it warm at 80°C for later use.
[0090] (3) Preparation of hydrogel composition: 4 kg of sodium carboxymethyl cellulose-pectin physically cross-linked hydrogel particles were placed in a boiling granulator, and the kudzu root extract-polyethylene glycol dispersion was atomized and sprayed on the surface of the hydrogel particles. The hydrogel particles were cured by cold air to obtain comparative sample 10. The preparation parameters were as follows: inlet air temperature: 2-10°C, outlet air temperature 2-20°C, atomization pressure: 0.2 MPa, fan frequency: 20-50 Hz, and slurry flow rate 5.1 g / min-6 g / min. Comparative Example 11
[0091] The material ratio of this comparative example is the same as that of Example 1, except that the slurry flow rate is smaller. Under this parameter, the production time is too long and the energy consumption is too high due to the slow flow rate, and there is no industrial value.
[0092] (1) Preparation of hydrogel particles: 300 g of pectin was placed in 333 L of ultrapure water and stirred to dissolve. 20 kg of sodium carboxymethyl cellulose was added to the pectin solution and stirred for 2 h. The solution was then placed in a forced air drying oven at 110 °C and dried for 8 h. After drying, the solution was crushed to obtain particles of 20-50 mesh. Hydrogel particles were obtained and 4 kg was reserved.
[0093] (2) Preparation of Pueraria extract-polyethylene glycol dispersion: Take 900 g of polyethylene glycol 4000 and place it in a water bath at 80°C for heating. After melting, add 100 g of Pueraria extract (20% puerarin content) and stir to dissolve to obtain Pueraria extract-polyethylene glycol dispersion. Keep it warm at 80°C for later use.
[0094] (3) Preparation of hydrogel composition: 4 kg of sodium carboxymethyl cellulose-pectin physically cross-linked hydrogel particles were placed in a boiling granulator, and the kudzu root extract-polyethylene glycol dispersion was atomized and sprayed on the surface of the hydrogel particles. The hydrogel particles were cured by cold air to obtain control sample 11. The preparation parameters were as follows: inlet air temperature: 2-10°C, outlet air temperature 2-20°C, atomization pressure: 0.2 MPa, fan frequency: 20-50 Hz, and slurry flow rate 0.1 g / min-0.4 g / min. Analysis and Conclusion
[0095] 1. Sample evaluation: a. Sample uniformity test: Take out 2 samples of implementation 1 from the upper layer, middle layer and lower layer of the boiling granulator, and take out 2 samples of comparison 1 from the upper layer, middle layer and lower layer of the three-stage mixer, respectively. Take 5g of each sample, and test the puerarin content of the sample according to GB / T22251-2008 Determination of Puerarin in Health Foods; b. Sample adsorption test of ethanol-water solution: prepare artificial gastric juice according to the Pharmacopoeia of the People's Republic of China, take 49 portions (50 ml each) of artificial gastric juice and place them in 49 stoppered conical bottles, then take 7 portions (1 g each) of sample 1, 7 portions (1 g each) of sample 2, 7 portions (1 g each) of sample 3, 7 portions (1 g each) of sample 4, 7 portions (1 g each) of sample 2, 7 portions (1 g each) of sample 4, 7 portions (1 g each) of sample 2, 7 portions (1 g each) of sample 4 and 7 portions (1 g each) of sample 4. g) Comparative sample 5 was placed in 49 stoppered conical flasks containing 50 ml of artificial gastric juice, and then 200 ml of 0.5% ethanol aqueous solution (v / v), 12% ethanol aqueous solution (v / v), 32% ethanol aqueous solution (v / v), 42% ethanol aqueous solution (v / v), 53% ethanol aqueous solution (v / v), 68% ethanol aqueous solution (v / v) and 75% ethanol aqueous solution (v / v) were added to 7 stoppered conical flasks containing implementation sample 1, 7 stoppered conical flasks containing implementation sample 2, 7 stoppered conical flasks containing implementation sample 3, 7 stoppered conical flasks containing implementation sample 4, 7 stoppered conical flasks containing comparison sample 2, 7 stoppered conical flasks containing comparison sample 4 and 7 stoppered conical flasks containing comparison sample 5, respectively. After plugging the bottle, keep warm at 37°C for 30 minutes, filter with a stainless steel mesh to obtain filtrate 1, record the volume of filtrate 1 and measure the ethanol content c1 in filtrate 1 by gas chromatography according to the third method of GB 5009.225 National Food Safety Standard Determination of Ethanol Concentration in Wines and Edible Alcohol.
[0096] Ethanol adsorption rate = (200*concentration of ethanol solution-volume of filtrate 1*c1) / 200*concentration of ethanol solution*100%; Pure ethanol adsorption amount = (200*concentration of ethanol solution-volume of filtrate 1*c1)*0.789; The unit of pure ethanol adsorption is g, and 0.789 (g / ml) is the density of ethanol.
[0097] c. Sample ethanol retention rate: Artificial gastric juice and simulated small intestinal juice were prepared according to the Pharmacopoeia of the People's Republic of China. 35 portions (50 ml each) of artificial gastric juice were taken and placed in 35 stoppered conical bottles respectively. Then 5 portions (1 g each) of Example 1 sample, 5 portions (1 g each) of Example 2, 5 portions (1 g each) of Example 3, 5 portions (1 g each) of Example 4, 5 portions (1 g each) of Comparative Sample 2, 5 portions (1 g each) of Comparative Sample 4 and 5 portions (1 g each) of Comparative Sample 5 were taken and placed in stoppered conical bottles containing 50 ml of artificial gastric juice respectively. Then 200 ml of 53% ethanol aqueous solution (v / v) were added to each of them. Put a stopper on the bottle and keep it warm at 37°C for 30 minutes. Filter with a stainless steel mesh to obtain filtrate 2 and filter residue, record the volume of filtrate 2 and measure the ethanol content c2 in filtrate 2 by gas chromatography according to the third method of "GB 5009.225 National Food Safety Standard Determination of Ethanol Concentration in Wine and Edible Alcohol"; quickly transfer the above-mentioned filter residues to 35 stoppered conical bottles filled with 200 ml simulated small intestinal fluid, plug the bottle stopper, and place 5 stoppered conical bottles filled with sample 1 filter residue, 5 sample 2 filter residues, 5 sample 3 filter residues, 5 sample 4 filter residues, 5 comparison sample 2 filter residues, 5 comparison sample 4 filter residues and 5 comparison sample 5 filter residues at 37°C for 0.5h, 1h, 2h, 5h, 9h respectively, filter with a stainless steel mesh to obtain filtrate 3, record the volume of filtrate 3 and measure the ethanol content c2 in filtrate 2 according to "GB 5009.225 National Food Safety Standard - Determination of Ethanol Concentration in Wine and Edible Alcohol - Method 3 - Measure the ethanol content c3 in filtrate 3 by gas chromatography.
[0098] Ethanol retention rate = ((200*53%-volume of filtrate 2*c2)-volume of filtrate 3*c3) / (200*53%-volume of filtrate 2*c2)*100%; d. Preparation of puerarin-polyethylene glycol 6000 solid dispersion: 9 parts of polyethylene glycol 6000 were placed in a water bath at 80°C for heating, and after melting, 1 part of puerarin (purity ≥ 98%) was added, and after stirring and dissolving, the mixture was quickly transferred to a stainless steel plate precooled to 5°C, and after solidification, the mixture was crushed to obtain puerarin-polyethylene glycol 6000 solid dispersion (puerarin: polyethylene glycol 6000 = 1:9); Solubility test: Take 1g puerarin (purity ≥98%) and 20g puerarin-polyethylene glycol 6000 solid dispersion (puerarin: polyethylene glycol 6000=1:9) respectively, put them in a 50 mL stoppered conical flask, add 25 mL (25g) of pure water that has been boiled and cooled to room temperature, put it on a magnetic stirrer, adjust the temperature to 25 ℃ and stir to make a supersaturated solution. When the dissolution reaches equilibrium, take the supernatant and test the puerarin content in the supernatant according to "GB / T 22251-2008 Determination of Puerarin in Health Foods"; the puerarin content in the supernatant is the solubility.
[0099] e. Dissolution test: Take 2 beakers, place them in a 37℃ water bath, add 500ml (500g) pure water, weigh 5.0000g puerarin and 50.0000g puerarin-polyethylene glycol 6000 solid dispersion (puerarin: polyethylene glycol 6000 = 1:9, containing 5g puerarin) respectively, put them into the above beakers, start the stirrer when in contact with the medium and record the time, the stirring speed is 100rpm, take samples at 5min, and test the puerarin content of the sample according to GB / T 22251-2008 Determination of Puerarin in Health Foods; dissolution percentage = puerarin content * 500 / (1000 * 5) * 100%, the unit of puerarin content is g / kg, and 1000 is the unit conversion factor; 2. Results and analysis: Table 1 Puerarin content of samples at different locations (g / kg)
[0100] Table 2 Ethanol adsorption rate of samples after 30 min treatment in simulated gastric fluid (%)
[0101] Table 3 Pure ethanol adsorption of samples after 30 min of treatment with simulated gastric fluid (g)
[0102] Table 4 Ethanol retention rate of samples after being treated with small intestinal fluid for different time periods (%)
[0103] Table 5 Solubility ( / g / kg) and dissolution percentage (%) of puerarin and puerarin-polyethylene glycol solid dispersion
[0104] Table 1 shows that the puerarin content in the upper, middle and lower layers of the implementation sample 1 is between 3.8-3.9 g / kg, with good uniformity; the puerarin content in the comparison sample 1 is between 0.9-8.6 g / kg, with a large deviation, and the puerarin content in the lower layer > the middle layer > the upper layer, indicating that the pueraria extract is not directly mixed with the hydrogel particles. The uniformity tends to be enriched in the lower layer.
[0105] Table 2 shows that the hydrogel composition can adsorb ethanol aqueous solution, and the adsorbed ethanol aqueous solution is locked inside the hydrogel, which greatly reduces the contact between ethanol and gastric mucosa, thereby reducing the stimulation of ethanol on gastric mucosa. The effect of adsorbing ethanol aqueous solution by the hydrogel composition of the embodiment is better than that of the comparative example, indicating that the particle size and content of the hydrogel affect the effect of adsorbing ethanol aqueous solution.
[0106] Table 3 shows that the amount of pure ethanol adsorbed by the hydrogel composition increases first and then decreases with the increase of the concentration of the ethanol solution, and the adsorption amount reaches the highest at 53% ethanol concentration, reaching 35.96g of pure ethanol; the ethanol adsorption amount of the hydrogel described in patent CN113854578 A is 0.55g, and the pure ethanol adsorption amount per unit weight of the embodiment is 65.3 times that of the control sample, indicating that the efficiency of the embodiment in adsorbing ethanol is extremely high.
[0107] Table 4 shows that the hydrogel compositions (Examples 1-4, Comparative Example 4) that absorb ethanol aqueous solution can retain more than 50% of ethanol in the simulated small intestinal fluid, and ethanol is absorbed mainly in the stomach and small intestine in the human body. It can be seen that the hydrogel composition can not only reduce the irritation to the intestinal mucosa but also reduce the concentration of ethanol in the blood. The retention rate of Comparative Example 2 is lower than 50%, indicating that the particle size selection of the hydrogel particles will significantly affect the ethanol retention rate.
[0108] Due to the strong water absorption properties of hydrogel particles, puerarin-polyethylene glycol 6000 solid dispersion was used to determine the solubility and dissolution rate of puerarin. Table 5 shows that after the introduction of polyethylene glycol 6000, the dissolution percentage of puerarin increased from 22.68% to 89.98%, an increase of 396%; the solubility increased from 3.74 g / kg to 66.37 g / kg, an increase of 1774%, indicating that the introduction of polyethylene glycol 6000 resulted in significant synergistic effects.
[0109] Comparative sample 1 has poor uniformity, and comparative examples 3, 6, 7, 8, 9, 10, and 11 are extremely difficult to produce and have no significance for comparative testing. The melting point of polyethylene glycol 2000 used in comparative example 4 is within the range of 49-53°C, and adhesion is likely to occur when the temperature is high, which is not conducive to storage and transportation.
[0110] In summary, the hydrogel composition provided by the present invention has a significant effect on adsorbing ethanol aqueous solution in the stomach, and can retain most of the ethanol in the small intestine without being released, which can protect the gastric mucosa and reduce the alcohol concentration in the blood during drinking. Therefore, it can be developed into a drug, food or health product for sobering up, protecting the liver and / or protecting the gastric mucosa.
[0111] 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 method for preparing a hydrogel composition, characterized in that: The raw materials of the hydrogel composition include, by weight: 80-90 parts of hydrogel particles, 9-18 parts of polyethylene glycol, and 1-4 parts of kudzu root extract; The preparation method comprises the following steps: (1) Preparation of hydrogel particles: crushing the hydrogel into 20-50 meshes to obtain hydrogel particles; (2) Preparation of Pueraria extract-polyethylene glycol dispersion: After heating and melting polyethylene glycol, add Pueraria extract and stir to dissolve to obtain Pueraria extract-polyethylene glycol dispersion, and keep warm for later use; the average molecular weight of the polyethylene glycol is 4000-8000Da; (3) Preparation of hydrogel composition: The kudzu root extract-polyethylene glycol dispersion is sprayed on the surface of the hydrogel particles by high-pressure atomization by a spray fluidized bed granulation technology, and the hydrogel composition is cured by cold air. The process parameters of the spray fluidized bed granulation technology are as follows: inlet air temperature: 2-10°C, outlet air temperature 2-20°C, atomization pressure: 0.1MPa-0.5MPa, fan frequency: 20-50Hz, slurry flow rate 0.5g / min-5g / min; There is no order of precedence for steps (1) and (2).
2. The preparation method according to claim 1, characterized in that: In step (1), the hydrogel includes a chemically cross-linked hydrogel and / or a physically cross-linked hydrogel; The chemically cross-linked hydrogel includes a hydrogel obtained by chemically cross-linking cellulose or its derivatives with a dibasic acid or a polybasic acid; and / or, the physically cross-linked hydrogel includes a hydrogel obtained by physically cross-linking cellulose or its derivatives with a 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 or polybasic acid comprises 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.
3. The preparation method according to claim 2, characterized in that: The hydrogel is formed by physically cross-linking sodium carboxymethyl cellulose and pectin; and / or, the hydrogel is formed by chemically cross-linking sodium carboxymethyl cellulose and malic acid.
4. The preparation method according to claim 1, characterized in that: In step (2), the polyethylene glycol is polyethylene glycol 6000.
5. The preparation method according to claim 1, characterized in that: In step (2), the puerarin content in the kudzu root extract is greater than or equal to 5%.
6. The preparation method according to claim 1, characterized in that: In step (2), the heating is water bath heating, and the heating temperature is 70-90°C.
7. The preparation method according to any one of claims 1 to 6, characterized in that: In step (2), the mass ratio of the polyethylene glycol to the kudzu root extract is 4-9:
1.
8. The preparation method according to claim 1, characterized in that: In step (3), the content of puerarin in the hydrogel composition is 0.05%-0.8%.
9. The preparation method according to claim 1 or 8, characterized in that: In step (3), the mass ratio of the kudzu root extract-polyethylene glycol dispersion to the hydrogel particles is 1:4-9.
10. The preparation method according to claim 1, characterized in that: In the raw materials of the hydrogel composition, the mass of hydrogel particles: the mass of polyethylene glycol: the mass of puerarin extract = 4000-9000: 800-900: 100-200.
11. The hydrogel composition prepared by the preparation method according to any one of claims 1 to 10, characterized in that: The raw materials of the hydrogel composition include, by weight: 80-90 parts of hydrogel particles, 9-18 parts of polyethylene glycol, and 1-4 parts of kudzu root extract. The content of puerarin in the hydrogel composition is 0.05%-0.8%.
12. Use of the hydrogel composition prepared by the preparation method according to any one of claims 1 to 10 or the hydrogel composition according to claim 10 in the preparation of drugs, foods or health products for sobering up, protecting the liver and / or protecting the gastrointestinal mucosa.
Citation Information
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