CN112426411A - Gastric-soluble tannic acid particles and preparation method thereof - Google Patents
Gastric-soluble tannic acid particles and preparation method thereof Download PDFInfo
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- CN112426411A CN112426411A CN202011524730.3A CN202011524730A CN112426411A CN 112426411 A CN112426411 A CN 112426411A CN 202011524730 A CN202011524730 A CN 202011524730A CN 112426411 A CN112426411 A CN 112426411A
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- tannin
- gastric
- tannic acid
- coating agent
- soluble
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- TUSDEZXZIZRFGC-UHFFFAOYSA-N 1-O-galloyl-3,6-(R)-HHDP-beta-D-glucose Natural products OC1C(O2)COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC1C(O)C2OC(=O)C1=CC(O)=C(O)C(O)=C1 TUSDEZXZIZRFGC-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 239000001263 FEMA 3042 Substances 0.000 title claims abstract description 61
- LRBQNJMCXXYXIU-PPKXGCFTSA-N Penta-digallate-beta-D-glucose Natural products OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-PPKXGCFTSA-N 0.000 title claims abstract description 61
- 229920002258 tannic acid Polymers 0.000 title claims abstract description 61
- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 title claims abstract description 61
- 229940033123 tannic acid Drugs 0.000 title claims abstract description 61
- 235000015523 tannic acid Nutrition 0.000 title claims abstract description 61
- 239000002245 particle Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title description 4
- 239000011248 coating agent Substances 0.000 claims abstract description 74
- 229920001864 tannin Polymers 0.000 claims abstract description 66
- 235000018553 tannin Nutrition 0.000 claims abstract description 66
- 239000001648 tannin Substances 0.000 claims abstract description 66
- 239000000843 powder Substances 0.000 claims abstract description 34
- 238000000576 coating method Methods 0.000 claims abstract description 26
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 15
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 15
- 229920001661 Chitosan Polymers 0.000 claims abstract description 11
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 claims abstract description 11
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 claims abstract description 11
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 claims abstract description 11
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000001856 Ethyl cellulose Substances 0.000 claims abstract description 7
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical group CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims abstract description 7
- 235000019325 ethyl cellulose Nutrition 0.000 claims abstract description 7
- 229920001249 ethyl cellulose Polymers 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 claims abstract description 5
- 239000008187 granular material Substances 0.000 claims description 31
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 24
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 22
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 14
- 229920002261 Corn starch Polymers 0.000 claims description 14
- 239000008120 corn starch Substances 0.000 claims description 14
- 229920000858 Cyclodextrin Polymers 0.000 claims description 13
- 239000001116 FEMA 4028 Substances 0.000 claims description 13
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 claims description 13
- 235000011175 beta-cyclodextrine Nutrition 0.000 claims description 13
- 229960004853 betadex Drugs 0.000 claims description 13
- 239000002904 solvent Substances 0.000 claims description 12
- 239000000377 silicon dioxide Substances 0.000 claims description 11
- 235000012239 silicon dioxide Nutrition 0.000 claims description 11
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 11
- 235000011152 sodium sulphate Nutrition 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 230000002496 gastric effect Effects 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 6
- 239000007779 soft material Substances 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 4
- 238000009835 boiling Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 13
- 241001465754 Metazoa Species 0.000 abstract description 5
- 210000002784 stomach Anatomy 0.000 abstract description 5
- 235000019606 astringent taste Nutrition 0.000 abstract description 4
- 235000013824 polyphenols Nutrition 0.000 abstract description 4
- 150000008442 polyphenolic compounds Chemical class 0.000 abstract description 3
- 230000002378 acidificating effect Effects 0.000 abstract description 2
- 210000003405 ileum Anatomy 0.000 abstract description 2
- 210000001630 jejunum Anatomy 0.000 abstract description 2
- 210000004185 liver Anatomy 0.000 abstract description 2
- 230000004060 metabolic process Effects 0.000 abstract description 2
- 210000003240 portal vein Anatomy 0.000 abstract description 2
- 210000003296 saliva Anatomy 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 25
- 241000287828 Gallus gallus Species 0.000 description 14
- 230000029087 digestion Effects 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 235000021050 feed intake Nutrition 0.000 description 4
- 238000009472 formulation Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000011664 nicotinic acid Substances 0.000 description 4
- 239000012530 fluid Substances 0.000 description 3
- 210000004051 gastric juice Anatomy 0.000 description 3
- 102000057297 Pepsin A Human genes 0.000 description 2
- 108090000284 Pepsin A Proteins 0.000 description 2
- 239000003674 animal food additive Substances 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- 235000010980 cellulose Nutrition 0.000 description 2
- 235000013330 chicken meat Nutrition 0.000 description 2
- 239000003651 drinking water Substances 0.000 description 2
- 235000020188 drinking water Nutrition 0.000 description 2
- 238000000338 in vitro Methods 0.000 description 2
- 229940111202 pepsin Drugs 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 229920000623 Cellulose acetate phthalate Polymers 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- 229920000168 Microcrystalline cellulose Polymers 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 230000000433 anti-nutritional effect Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002301 cellulose acetate Polymers 0.000 description 1
- 229940081734 cellulose acetate phthalate Drugs 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 210000001035 gastrointestinal tract Anatomy 0.000 description 1
- 229920003132 hydroxypropyl methylcellulose phthalate Polymers 0.000 description 1
- 229940031704 hydroxypropyl methylcellulose phthalate Drugs 0.000 description 1
- 230000000968 intestinal effect Effects 0.000 description 1
- 235000013372 meat Nutrition 0.000 description 1
- 229940016286 microcrystalline cellulose Drugs 0.000 description 1
- 235000019813 microcrystalline cellulose Nutrition 0.000 description 1
- 239000008108 microcrystalline cellulose Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 235000019640 taste Nutrition 0.000 description 1
- 125000005591 trimellitate group Chemical group 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
- A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
- A61K9/5005—Wall or coating material
- A61K9/5021—Organic macromolecular compounds
- A61K9/5036—Polysaccharides, e.g. gums, alginate; Cyclodextrin
- A61K9/5042—Cellulose; Cellulose derivatives, e.g. phthalate or acetate succinate esters of hydroxypropyl methylcellulose
- A61K9/5047—Cellulose ethers containing no ester groups, e.g. hydroxypropyl methylcellulose
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/70—Carbohydrates; Sugars; Derivatives thereof
- A61K31/7024—Esters of saccharides
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
- A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
- A61K9/5005—Wall or coating material
- A61K9/5021—Organic macromolecular compounds
- A61K9/5031—Organic macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polyethylene glycol, poly(lactide-co-glycolide)
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
- A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
- A61K9/5005—Wall or coating material
- A61K9/5021—Organic macromolecular compounds
- A61K9/5036—Polysaccharides, e.g. gums, alginate; Cyclodextrin
- A61K9/5042—Cellulose; Cellulose derivatives, e.g. phthalate or acetate succinate esters of hydroxypropyl methylcellulose
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
- A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
- A61K9/5089—Processes
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P1/00—Drugs for disorders of the alimentary tract or the digestive system
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P29/00—Non-central analgesic, antipyretic or antiinflammatory agents, e.g. antirheumatic agents; Non-steroidal antiinflammatory drugs [NSAID]
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P31/00—Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
- A61P31/04—Antibacterial agents
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- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P39/00—General protective or antinoxious agents
- A61P39/06—Free radical scavengers or antioxidants
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P43/00—Drugs for specific purposes, not provided for in groups A61P1/00-A61P41/00
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Abstract
The invention provides gastric-soluble tannic acid particles, which comprise the following components in percentage by mass: 30-50% of tannin powder, 30-60% of a carrier and 10-20% of a coating agent; the coating agent is composed of hydroxypropyl methyl cellulose, chitosan and polyethylene glycol 2000, or the coating agent is ethyl cellulose. The coating material is selected to be dissolved or decomposed under the acidic condition, so that most of the tannin can be released in the stomach and decomposed into small-molecular polyphenol under the low pH environment of the stomach, and the decomposed products are absorbed by the jejunum and ileum and enter the liver through the portal vein for further metabolism without influencing the action effect of the tannin in the animal body; meanwhile, the coating agent isolates the tannic acid from directly contacting with saliva, and avoids the astringent feeling caused by the astringency of the tannic acid.
Description
Technical Field
The invention belongs to the technical field of feed additives, and particularly relates to gastric-soluble tannic acid granules and a preparation method thereof.
Background
Tannic acid is a natural plant polyphenol, also called tannin and tannic acid. It can be divided into two categories: one is condensed tannic acid and the other is hydrolyzed tannic acid. Wherein the condensed tannic acid is an anti-nutritional factor for monogastric animals, and the hydrolyzed tannic acid has antibacterial, antioxidant, anti-inflammatory, intestinal micro-ecological environment improving and animal growth promoting effects due to polyhydric phenolic hydroxyl structure.
Today, the feed is totally banned, the hydrolyzed tannin is an important anti-substitution additive, but the hydrolyzed tannin has strong astringency, so that the taste is astringent and the feed intake of animals is influenced.
Disclosure of Invention
The object of the present invention is to provide a gastric-soluble tannic acid granule that solves at least some of the drawbacks of the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
a gastric-soluble tannin granule comprises the following components in percentage by mass: 30-50% of tannin powder, 30-60% of a carrier and 10-20% of a coating agent; the coating agent is composed of hydroxypropyl methyl cellulose, chitosan and polyethylene glycol 2000, or the coating agent is ethyl cellulose.
Preferably, the gastric-soluble tannin particles comprise the following components in percentage by mass: 30-50% of tannin powder, 34-56% of a carrier and 14-18% of a coating agent.
Specifically, the tannin powder is hydrolyzed tannin.
Specifically, the carrier consists of the following components in percentage by mass based on the total mass of the gastric-soluble tannic acid particles: 0-10% of anhydrous sodium sulfate, 15-40% of corn starch, 0-20% of light calcium carbonate, 0-8% of silicon dioxide and 0-10% of beta-cyclodextrin.
Preferably, the carrier consists of the following components in percentage by mass based on the total mass of the gastric-soluble tannic acid particles: 5-10% of anhydrous sodium sulphate, 18-31% of corn starch, 0-10% of light calcium carbonate, 0-6% of silicon dioxide and 5-10% of beta-cyclodextrin.
Specifically, the coating agent comprises the following components in percentage by mass of the total mass of the gastric-soluble tannic acid particles: 4-8% of hydroxypropyl methyl cellulose, 5-9% of chitosan and 20001-4% of polyethylene glycol.
Optimally, the content of each component in the coating agent accounts for the total mass percentage of the gastric-soluble tannin particles as follows: 5-7% of hydroxypropyl methyl cellulose, 6-9% of chitosan and 20001-3% of polyethylene glycol.
Specifically, when the coating agent is ethyl cellulose, the solvent is 85% ethanol solution.
In addition, the invention also provides a preparation method of the gastric-soluble tannic acid particles, which comprises the following steps:
1) weighing tannin powder and a carrier according to a formula, and adding the tannin powder and the carrier into a wet mixer;
2) adding a proper amount of water into the wet mixer, and stirring for 30-60 min to prepare a soft material;
3) preparing the soft material prepared in the step 2) into 50-mesh particles through a screw extruder;
4) drying the tannic acid particles prepared in the step 3) in a boiling bed;
5) weighing the coating materials according to the formula and preparing coating liquid;
6) coating the dried granules obtained in the step 4) by using the coating liquid prepared in the step 5) in a fluidized bed.
Compared with the prior art, the invention has the beneficial effects that:
(1) the coating material is selected, so that the gastric-soluble tannic acid particles can be dissolved or decomposed under an acidic condition (the pH value is 1-3), most of tannic acid can be released in the stomach and decomposed into small-molecular polyphenol under the low-pH environment of the stomach, and the decomposition products are absorbed by the jejunum and the ileum and enter the liver through the portal vein for further metabolism, so that the action effect of the tannic acid in an animal body cannot be influenced.
(2) The gastric-soluble tannic acid particles provided by the invention isolate the direct contact of tannic acid and saliva through a coating technology, and avoid the astringent feeling caused by the astringency of tannic acid; meanwhile, the coating can play a role in preventing moisture and air, so that the stability of the product in the production, transportation and storage processes is improved.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the present example provides a gastric-soluble tannin granule, wherein the formula of each 100kg of the granule is as follows: 30kg of tannic acid powder, 40kg of corn starch, 20kg of light calcium carbonate and 10kg of coating agent. Wherein the tannin powder is hydrolyzed tannin; the coating agent comprises the following components: 4kg of hydroxypropyl methyl cellulose, 5kg of chitosan and 20001kg of polyethylene glycol, wherein the coating agent in the embodiment adopts water as a solvent to prepare a coating solution.
Example 2:
the present example provides a gastric-soluble tannin granule, wherein the formula of each 100kg of the granule is as follows: 30kg of tannin powder, 5kg of anhydrous sodium sulphate, 31kg of corn starch, 10kg of light calcium carbonate, 10kg of beta-cyclodextrin and 14kg of coating agent. Wherein the tannin powder is hydrolyzed tannin; the coating agent is ethyl cellulose, and the coating agent adopts ethanol solution with the concentration of 85 percent as solvent to prepare coating liquid.
Example 3:
the present example provides a gastric-soluble tannin granule, wherein the formula of each 100kg of the granule is as follows: 40kg of tannin powder, 5kg of anhydrous sodium sulphate, 30kg of corn starch, 6kg of silicon dioxide, 5kg of beta-cyclodextrin and 14kg of coating agent. Wherein the tannin powder is hydrolyzed tannin; the coating agent comprises the following components: 6kg of hydroxypropyl methyl cellulose, 6kg of chitosan and 20002kg of polyethylene glycol, wherein the coating agent in the embodiment adopts water as a solvent to prepare a coating solution.
Example 4:
the present example provides a gastric-soluble tannin granule, wherein the formula of each 100kg of the granule is as follows: 40kg of tannin powder, 10kg of anhydrous sodium sulphate, 20kg of corn starch, 4kg of silicon dioxide, 8kg of beta-cyclodextrin and 18kg of coating agent. Wherein the tannin powder is hydrolyzed tannin; the coating agent comprises the following components: 7kg of hydroxypropyl methyl cellulose, 8kg of chitosan and 20003kg of polyethylene glycol, wherein the coating agent in the embodiment adopts water as a solvent to prepare a coating solution.
Example 5:
the present example provides a gastric-soluble tannin granule, wherein the formula of each 100kg of the granule is as follows: 50kg of tannin powder, 5kg of anhydrous sodium sulphate, 18kg of corn starch, 5kg of light calcium carbonate, 6kg of beta-cyclodextrin and 16kg of coating agent. Wherein the tannin powder is hydrolyzed tannin; the coating agent is ethyl cellulose, and the coating agent adopts ethanol solution with the concentration of 85 percent as solvent to prepare coating liquid.
Example 6:
the present example provides a gastric-soluble tannin granule, wherein the formula of each 100kg of the granule is as follows: 50kg of tannin powder, 2kg of anhydrous sodium sulphate, 15kg of corn starch, 8kg of silicon dioxide, 5kg of beta-cyclodextrin and 20kg of coating agent. Wherein the tannin powder is hydrolyzed tannin; the coating agent comprises the following components: 8kg of hydroxypropyl methyl cellulose, 8kg of chitosan and 20004kg of polyethylene glycol, wherein the coating agent in the embodiment adopts water as a solvent to prepare a coating solution.
The method for preparing the gastric-soluble tannic acid particles of embodiments 1 to 6 includes the following steps:
(1) adding the weighed tannin powder and various carriers into a wet mixer;
(2) adding water accounting for 30% of the weight of the powder in the step (1) into a wet mixer, and stirring for 60min to prepare a soft material;
(3) preparing the soft material prepared in the step (2) into 50-mesh particles through a screw extruder;
(4) drying the tannic acid particles prepared in the step (3) in a boiling bed;
(5) preparing a coating solution according to the formula of the coating agent, and spraying the coating solution on the surface of the particles in the step (4) by using a fluidized bed for coating.
In order to further verify the technical effect of the scheme of the invention, the following tests were carried out.
Example 7:
this example was conducted to examine the release effect of gastric-soluble tannic acid particles obtained in the above examples during in vitro digestion
The experimental process comprises the following steps: the release effect of the gastric-soluble tannic acid particles in simulated gastric juice is inspected by adopting a bionic digestion method; the bionic digester adopts SDS-III type equipment of China intelligent company, the addition amount of gastric-soluble tannic acid particles is 1g, the digestion duration is 4h, and the tannic acid release rate is detected by sampling every hour.
Simulated gastric fluid formula: to 20ml of hydrochloric acid solution having a pH of 2.0, 0.01g of pepsin was added and stirred until completely dissolved.
The release effect of the gastric-soluble tannic acid particles prepared in the above examples 2 to 5 in simulated gastric juice is shown in table 1. As can be seen from Table 1, most tannic acid is released in the stomach, and the rest part reaches the intestinal tract to play a role in astringency and anti-inflammation.
Table 1: sample Release Rate
| Example 2 | Example 3 | Example 4 | Example 5 | |
| 1h(％) | 29.35 | 27.61 | 28.34 | 30.18 |
| 2h(％) | 82.36 | 85.19 | 84.51 | 88.44 |
| 3h(％) | 89.59 | 90.47 | 92.94 | 93.27 |
| 4h(％) | 90.03 | 91.83 | 92.34 | 92.49 |
Example 8:
this example examined the effect of gastric-soluble tannic acid granules prepared in the above examples on broiler growth performance.
360 healthy broilers of similar weight were selected for the trial and randomly divided into 3 groups, each group receiving one treatment and each group being four replicates. Test 1 group was a control group, and the feed was fed without tannic acid, test 2 group was prepared by adding 0.1% of commercially available tannic acid powder to the feed, and test 3 to 6 group were prepared by adding 0.1% of the gastric-soluble tannic acid granules prepared in examples 2 to 5 to the feed. The test is carried out for 42 days, the test chicken is raised in cages, is normally raised and managed, is freely eaten, and is fully supplied with clean drinking water, and the test results are shown in a table 2.
Table 2: influence of gastric-soluble tannic acid particles on growth performance of broiler chickens
As can be seen from Table 2, the broiler feed intake of the test group 2 is obviously lower than that of the other two groups at each growth stage of the broilers, but the daily gain and feed-meat ratio is basically equal to that of the control group; the ratio of the daily gain of the broilers to the feed meat of the test groups 3-6 is obviously superior to that of the other two groups. The test result shows that the tannic acid has obvious influence on the feed intake of the broilers, while the gastric-soluble tannic acid granules have no influence on the feed intake of the broilers basically, can promote the growth of the broilers and improve the utilization rate of feed.
The effect of the coated tannic acid particles made with different celluloses and their derivatives as coating agents is illustrated by the following comparative examples.
Comparative example 1:
the present comparative example provides a coated tannic acid granule, the formulation of which per 100kg of granule is: 40kg of tannin powder, 10kg of anhydrous sodium sulphate, 20kg of corn starch, 4kg of silicon dioxide, 8kg of beta-cyclodextrin and 18kg of coating agent. Wherein the tannin powder is hydrolyzed tannin; the coating agent comprises the following components: 15kg of cellulose acetate phthalate and 20003kg of polyethylene glycol, and in the comparative example, water is used as a solvent for preparing a coating solution.
Comparative example 2:
the present comparative example provides a coated tannic acid granule, the formulation of which per 100kg of granule is: 40kg of tannin powder, 10kg of anhydrous sodium sulphate, 20kg of corn starch, 4kg of silicon dioxide, 8kg of beta-cyclodextrin and 18kg of coating agent. Wherein the tannin powder is hydrolyzed tannin; the coating agent comprises the following components: 15kg of hydroxypropyl methyl cellulose phthalate and 20003kg of polyethylene glycol, wherein the coating agent in the comparative example adopts water as a solvent to prepare a coating solution.
Comparative example 3:
the present comparative example provides a coated tannic acid granule, the formulation of which per 100kg of granule is: 40kg of tannin powder, 10kg of anhydrous sodium sulphate, 20kg of corn starch, 4kg of silicon dioxide, 8kg of beta-cyclodextrin and 18kg of coating agent. Wherein the tannin powder is hydrolyzed tannin; the coating agent comprises the following components: 15kg of cellulose acetate trimellitate and 20003kg of polyethylene glycol, and in the comparative example, water is used as a solvent for preparing a coating solution.
Comparative example 4:
the present comparative example provides a coated tannic acid granule, the formulation of which per 100kg of granule is: 40kg of tannin powder, 10kg of anhydrous sodium sulphate, 20kg of corn starch, 4kg of silicon dioxide, 8kg of beta-cyclodextrin and 18kg of coating agent. Wherein the tannin powder is hydrolyzed tannin; the coating agent comprises the following components: 15kg of microcrystalline cellulose and 20003kg of polyethylene glycol, and the coating agent in the comparative example adopts water as a solvent to prepare a coating solution.
Comparative example 5:
this comparative example measured the release effect of the coated tannic acid particles of comparative examples 1 to 4 during in vitro digestion
The experimental process comprises the following steps: the release effect of the gastric-soluble tannic acid particles in simulated gastric juice is inspected by adopting a bionic digestion method; the bionic digester adopts SDS-III type equipment of China intelligent company, the addition amount of gastric-soluble tannic acid particles is 1g, the digestion duration is 4h, and the tannic acid release rate is detected by sampling every hour.
Simulated gastric fluid formula: to 20ml of hydrochloric acid solution having a pH of 2.0, 0.01g of pepsin was added and stirred until completely dissolved.
The release effect of the coated tannic acid particles prepared in comparative examples 1 to 4 in simulated gastric fluid is shown in table 3. As can be seen from Table 3, all the coated tannins showed much lower gastric release rates than the above examples, and the release was poor.
Table 3: sample Release Rate
| Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | |
| 1h(％) | 0.56 | 0.84 | 0.48 | 5.61 |
| 2h(％) | 2.33 | 3.02 | 1.89 | 9.15 |
| 3h(％) | 4.36 | 5.48 | 3.65 | 16.77 |
| 4h(％) | 7.41 | 8.63 | 9.26 | 27.92 |
Comparative example 6:
the test selected 480 healthy broilers of similar weight, randomly divided into 6 groups, each group received one treatment, each group was replicated four times. Test groups 1 to 4 were prepared by adding the coated tannic acid products prepared in comparative examples 1 to 4 to feed in an amount of 0.1% respectively. The test is carried out for 42 days, the test chicken is raised in cages, is normally raised and managed, is freely eaten, and is fully supplied with clean drinking water, and the test results are shown in a table 4.
Table 4: influence of coated tannic acid particles on growth performance of broiler chickens
Comparing the data in tables 4 and 2, it can be seen that the effect of the coated tannic acid granules prepared in comparative examples 1 to 4 as a feed additive is not significantly different from that of the feed without tannic acid (i.e. test group 1) in example 8, which indicates that the coated tannic acid prepared in comparative examples 1 to 4 has no significant effect on the growth performance of broiler chicken, and further indicates that not all the coating materials of cellulose and derivatives thereof can play the same role.
The above examples are merely illustrative of the present invention and should not be construed as limiting the scope of the invention, which is intended to be covered by the claims and any design similar or equivalent to the scope of the invention.
Claims (9)
1. The gastric-soluble tannin particles are characterized by comprising the following components in percentage by mass: 30-50% of tannin powder, 30-60% of a carrier and 10-20% of a coating agent; the coating agent is composed of hydroxypropyl methyl cellulose, chitosan and polyethylene glycol 2000, or the coating agent is ethyl cellulose.
2. The gastric-soluble tannic acid granules of claim 1, comprising in mass%: 30-50% of tannin powder, 34-56% of a carrier and 14-18% of a coating agent.
3. The gastric-soluble tannic acid of claim 1 wherein said tannic acid powder is hydrolyzed tannic acid.
4. The gastric tannin particles of claim 1, wherein the carrier comprises, in percent by weight of the total mass of the gastric tannin particles: 0-10% of anhydrous sodium sulfate, 15-40% of corn starch, 0-20% of light calcium carbonate, 0-8% of silicon dioxide and 0-10% of beta-cyclodextrin.
5. The gastric tannin particles of claim 4, wherein the carrier comprises, in percent by weight of the total mass of the gastric tannin particles: 5-10% of anhydrous sodium sulphate, 18-31% of corn starch, 0-10% of light calcium carbonate, 0-6% of silicon dioxide and 5-10% of beta-cyclodextrin.
6. The gastric-soluble tannin particle of claim 1, wherein the coating agent comprises the following components in percentage by weight of the total mass of the gastric-soluble tannin particle: 4-8% of hydroxypropyl methyl cellulose, 5-9% of chitosan and 20001-4% of polyethylene glycol.
7. The gastric-soluble tannin particle of claim 6, wherein the coating agent comprises the following components in percentage by weight of the total mass of the gastric-soluble tannin particle: 5-7% of hydroxypropyl methyl cellulose, 6-9% of chitosan and 20001-3% of polyethylene glycol.
8. The gastric tannin granule of claim 1, wherein the coating agent is ethyl cellulose, and the solvent is 85% ethanol solution.
9. The method for producing the gastric-soluble tannic acid particles of any one of claims 1 to 8, comprising the steps of:
1) weighing tannin powder and a carrier according to a formula, and adding the tannin powder and the carrier into a wet mixer;
2) adding a proper amount of water into the wet mixer, and stirring for 30-60 min to prepare a soft material;
3) preparing the soft material prepared in the step 2) into 50-mesh particles through a screw extruder;
4) drying the tannic acid particles prepared in the step 3) in a boiling bed;
5) weighing the coating materials according to the formula and preparing coating liquid;
6) coating the dried granules obtained in the step 4) by using the coating liquid prepared in the step 5) in a fluidized bed.
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