CN110897048A - Enteric sodium butyrate microcapsule and preparation method and application thereof - Google Patents
Enteric sodium butyrate microcapsule and preparation method and application thereof Download PDFInfo
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- CN110897048A CN110897048A CN201911389988.4A CN201911389988A CN110897048A CN 110897048 A CN110897048 A CN 110897048A CN 201911389988 A CN201911389988 A CN 201911389988A CN 110897048 A CN110897048 A CN 110897048A
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- sodium butyrate
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- MFBOGIVSZKQAPD-UHFFFAOYSA-M sodium butyrate Chemical compound [Na+].CCCC([O-])=O MFBOGIVSZKQAPD-UHFFFAOYSA-M 0.000 title claims abstract description 126
- 239000003094 microcapsule Substances 0.000 title claims abstract description 77
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 239000000463 material Substances 0.000 claims abstract description 83
- 239000011248 coating agent Substances 0.000 claims abstract description 48
- 238000000576 coating method Methods 0.000 claims abstract description 48
- 239000012792 core layer Substances 0.000 claims abstract description 37
- 239000010410 layer Substances 0.000 claims abstract description 37
- 239000000843 powder Substances 0.000 claims abstract description 19
- 239000003674 animal food additive Substances 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims description 16
- 238000005507 spraying Methods 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 10
- 239000008103 glucose Substances 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 9
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Natural products CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- GLDOVTGHNKAZLK-UHFFFAOYSA-N octadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 claims description 8
- VBICKXHEKHSIBG-UHFFFAOYSA-N 1-monostearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(O)CO VBICKXHEKHSIBG-UHFFFAOYSA-N 0.000 claims description 6
- ZUAAPNNKRHMPKG-UHFFFAOYSA-N acetic acid;butanedioic acid;methanol;propane-1,2-diol Chemical compound OC.CC(O)=O.CC(O)CO.OC(=O)CCC(O)=O ZUAAPNNKRHMPKG-UHFFFAOYSA-N 0.000 claims description 4
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- 108700042778 Antimicrobial Peptides Proteins 0.000 claims description 2
- 102000044503 Antimicrobial Peptides Human genes 0.000 claims description 2
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- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 2
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- 102000057297 Pepsin A Human genes 0.000 description 1
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- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
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- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
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- 238000006243 chemical reaction Methods 0.000 description 1
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- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 description 1
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Images
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K50/00—Feeding-stuffs specially adapted for particular animals
- A23K50/30—Feeding-stuffs specially adapted for particular animals for swines
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K20/00—Accessory food factors for animal feeding-stuffs
- A23K20/10—Organic substances
- A23K20/105—Aliphatic or alicyclic compounds
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K40/00—Shaping or working-up of animal feeding-stuffs
- A23K40/30—Shaping or working-up of animal feeding-stuffs by encapsulating; by coating
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K50/00—Feeding-stuffs specially adapted for particular animals
- A23K50/60—Feeding-stuffs specially adapted for particular animals for weanlings
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Polymers & Plastics (AREA)
- Zoology (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Animal Husbandry (AREA)
- Birds (AREA)
- Medicinal Preparation (AREA)
Abstract
The invention relates to an enteric sodium butyrate microcapsule, a preparation method and application thereof, wherein the enteric sodium butyrate microcapsule comprises an inner core layer and a coating material layer coated on the surface of the inner core layer; the inner nuclear layer comprises a sodium butyrate core and an auxiliary material layer wrapping the sodium butyrate core. The enteric sodium butyrate microcapsule preparation does not have rancidity-like smell, is not easy to absorb moisture, has good fluidity and dispersibility, can be slowly dissolved in intestinal tracts, achieves intestinal tract targeted release, and remarkably improves the absorption effect. Compared with the common sodium butyrate powder, when the sodium butyrate powder is used as a feed additive for feeding animals, the average daily feed intake and daily gain of the animals can be obviously improved, the feed-weight ratio is reduced, and the diarrhea rate is reduced; and can significantly reduce the content of harmful bacteria such as Escherichia coli in animal ileum and colon, and significantly increase beneficial bacteria such as lactobacillus and Bacillus bifidus in colon and cecum.
Description
Technical Field
The invention belongs to the technical field of feed additives, and particularly relates to an enteric sodium butyrate microcapsule as well as a preparation method and application thereof.
Background
Butyric acid, the most prominent representative of short-chain volatile fatty acids, is the major anion of the colon lumen and the nutrient substance of colon cells, and is the major energy substrate of large intestine cells, and can be rapidly absorbed and oxidized by colon cells to supply energy to the colon cells. Plays an important role in regulating the microecological balance of the gastrointestinal tract, the electrolyte balance and the food calling. Butyric acid has the physiological action of a feed acidifier and can provide animal productivity, so that it is widely used in the breeding process. But because of its freeness and volatility, it is produced as a relatively stable sodium salt, i.e., sodium butyrate.
The sodium butyrate is an important nutrient substance of the intestinal epithelial cells, is used as an energy source of the intestinal epithelial cells, can be directly absorbed by the epithelial cells without digestion, promotes the proliferation and development of the intestinal epithelial cells, maintains the integrity of intestinal mucosa, effectively promotes the proliferation of beneficial bacteria in the intestinal tract, inhibits the growth of harmful bacteria, thereby adjusting the microecological balance of the intestinal tract and finally realizing the health of the intestinal tract.
Because the sodium butyrate has the characteristics of green and pollution-free, and has the characteristics of unique nutrition physiological function, etc., the sodium butyrate is listed in feed additive variety catalog by Ministry of agriculture, can be used as a novel feed additive, and can be used as an antibiotic substitute to reduce the use of part of antibiotics. But the wide application of the feed additive in feed processing and breeding production is limited due to the defects of the feed additive. Specifically, sodium butyrate has a special rancidity-like odor of cheese, influences the approval of feed quality, and has strong irritation to esophagus; sodium butyrate is easy to absorb moisture and has poor fluidity, so that the processing and storage of the feed are not facilitated; sodium butyrate mainly acts in the second half of the intestinal tract, and if the sodium butyrate is not coated, the active ingredients of the sodium butyrate can be absorbed in the stomach and are difficult to enter the intestinal tract. Even if the intestinal tract is entered, the intestinal tract can also absorb the sodium butyrate, so that the requirement of each section of the intestinal tract on the sodium butyrate cannot be met, and the subsequent section of the intestinal tract cannot continuously supply energy.
CN105995192A discloses a preparation method of nano slow-release sodium butyrate for grass carp feed, wherein n-butyric acid is uniformly dripped into a sodium hydroxide solution, reaction is carried out for 1.5-2.0h after the dripping is finished to obtain a sodium butyrate solution, auxiliary materials are added into the sodium butyrate solution, the mass ratio of the auxiliary materials to the sodium butyrate solution is 1-1.5:2, the auxiliary materials comprise 2-3 parts of beeswax, 1-2 parts of palm wax, 0.1-0.5 part of fish oil, 1-4 parts of polyethylene glycol, 0.5-1 part of filler and 1-1.5 parts of nano slow-release carrier, and finally spray drying is carried out to obtain the nano slow-release sodium butyrate, wherein the drying temperature is 200-. The nano embedding technology is adopted to carry out nano embedding on the sodium butyrate, so that the defects that the sodium butyrate has peculiar smell, is easy to deliquesce, is difficult to be utilized by an intestinal tract and cannot continuously provide energy for the intestinal tract are overcome, the health of the intestinal tract of the grass carp is promoted, the absorption of nutrient substances is improved, and the economic benefit of grass carp breeding is improved.
CN102579369A discloses a sodium butyrate enteric-coated sustained-release preparation and a preparation method thereof, wherein the product synthesis is started from a sodium butyrate synthesis process, the synthesized sodium butyrate liquid is subjected to liquid-state inclusion, and the liquid-state inclusion is followed by spray granulation to obtain the sodium butyrate enteric-coated sustained-release preparation. The preparation method reduces production links and production cost, reduces environmental influence in the production process, reduces volatile smell and hygroscopicity of the product, and the prepared sodium butyrate enteric sustained-release preparation is white spherical particles with the particle size of 200-500 mu m. Has good stability and strong moisture resistance, can be slowly released in intestinal tracts, and improves the bioavailability of the product.
However, the prior art has limited strategies on how to better overcome the defects of the sodium butyrate, such as esophageal irritation, moisture absorption tendency, low fluidity and the like, and therefore, the development of a novel enteric sodium butyrate preparation is very necessary.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide an enteric sodium butyrate microcapsule, a preparation method and application thereof, and particularly provides the enteric sodium butyrate microcapsule, the preparation method thereof, a feed additive and a feed. The enteric sodium butyrate microcapsule preparation is not easy to absorb moisture, has good fluidity and dispersibility, can reach the intestinal part to be slowly released in a targeted manner, and can meet the requirement of each section of the intestinal tract on sodium butyrate.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides an enteric sodium butyrate microcapsule, which comprises an inner core layer and a coating material layer coated on the surface of the inner core layer; the inner nuclear layer comprises a sodium butyrate core and an auxiliary material layer wrapping the sodium butyrate core.
The enteric sodium butyrate microcapsule uses auxiliary materials to wrap sodium butyrate to prepare microcapsule particles, and a layer of coating material is sprayed on the surface of the microcapsule particles to completely isolate the sodium butyrate from the outside; after double-layer coating, the odor of the sodium butyrate is covered, the problem of easy moisture absorption is solved, the fluidity and the dispersibility of the product are improved, and the stability and the quality of the product are improved.
Preferably, the auxiliary materials comprise any one or a combination of at least two of fat powder, auxiliary powder, glucose, antibacterial peptide, stearic acid, glyceryl monostearate, stearyl alcohol, saturated triglyceride, monoglyceride or paraffin; the combination of at least two of the above components, such as the combination of fat powder and auxiliary powder, the combination of glucose and antimicrobial peptide, the combination of stearyl alcohol and saturated triglyceride, and the like, can be selected in any combination manner, and are not described herein.
Preferably, the auxiliary material accounts for 65-80% of the enteric sodium butyrate microcapsule by mass, such as 65%, 68%, 70%, 72%, 75%, 78%, or 80%, and other specific values within the range can be selected, which is not described herein.
The mass percentage of the auxiliary material is specifically selected within the range of 65-80%, because the size of the inner core layer directly influences the grain diameter of the microcapsule and influences the stability and the release rate of the medicine. When the mass fraction of the sodium butyrate is constant, the particle size is too large due to excessive auxiliary materials, the release is too slow, and the entrapment rate of the raw material medicine is low, the release speed is high and the effect is poor due to less auxiliary materials. The controlled release and targeting of the medicament can also be affected by different proportions of a plurality of auxiliary materials.
Preferably, the coating material comprises any one or a combination of at least two of hypromellose phthalate, polyvinyl acetate phthalate, cellulose acetate phthalate, hypromellose acetate succinate or acrylic resin; the combination of at least two of the above-mentioned components, for example, the combination of hypromellose phthalate and polyvinyl acetate phthalate, the combination of cellulose acetate phthalate and hypromellose acetate succinate, the combination of hypromellose acetate succinate and acrylic resin, etc., may be selected in any combination manner, and is not described herein in detail.
The coating layer material is an enteric film coating material, so that the active ingredients of the product can safely pass through the stomach, the dissolution rate in the stomach is less than or equal to 1%, and the active ingredients are slowly dissolved in the intestinal tract, thereby achieving the purposes of intestinal targeted release and slow and sustained release, obviously improving the drug effect and reducing the drug addition.
Preferably, the coating material accounts for 5-10% of the enteric sodium butyrate microcapsules by mass, such as 5%, 6%, 7%, 8%, 9%, 10% or the like.
The mass percentage of the coating material is specifically selected in the range of 5-10% because the mass percentage of the coating material affects the dissolution rate of the capsule wall, as well as the integrity of the microcapsules, avoiding rupture due to pressure, shear force, abrasion, etc., resulting in drug release.
Preferably, the particle size of the enteric sodium butyrate microcapsule is 180-355 μm, such as 180 μm, 190 μm, 200 μm, 220 μm, 230 μm, 250 μm, 260 μm, 280 μm, 300 μm, 320 μm, 340 μm, 350 μm or 355 μm, and other specific values within the range can be selected, which is not described herein again.
The particle size of the enteric sodium butyrate microcapsule is specifically selected to be 180-355 μm, because the particle size of the microcapsule influences the release, bioavailability, drug loading, in-vivo distribution and targeting of the medicament besides the palatability. Above this range the release rate is low, targeting is poor, bioavailability is low, below this range the release rate is high, targeting is poor, bioavailability is low. The particle size is determined by the size of the core layer, the amount of the coating layer, the preparation temperature, the mixing and stirring rate, and the like.
In a second aspect, the present invention provides a preparation method of the enteric sodium butyrate microcapsule, wherein the preparation method comprises:
(1) mixing the sodium butyrate raw material with auxiliary materials, and coating to obtain an inner nuclear layer;
(2) and (2) spraying a coating material on the surface of the inner core layer prepared in the step (1) to obtain the enteric sodium butyrate microcapsule.
The preparation method of the enteric sodium butyrate microcapsule related by the invention is simple, low in cost, easy to operate, less in loss and high in total product yield.
Preferably, the mixing in step (1) comprises stirring.
Preferably, the temperature of the mixing in step (1) is 80-90 ℃, for example, 80 ℃, 82 ℃, 83 ℃, 84 ℃, 85 ℃, 86 ℃, 87 ℃, 88 ℃, 89 ℃ or 90 ℃ and the like, and other specific values in the range can be selected, which is not described in detail herein.
Preferably, the mixing time in step (1) is 30-60min, for example, 30min, 35min, 40min, 45min, 50min, 55min or 60min, and other specific values in the range can be selected, which is not described herein.
Preferably, the temperature of the spraying in the step (2) is 80-90 ℃, for example, 80 ℃, 82 ℃, 83 ℃, 84 ℃, 85 ℃, 86 ℃, 87 ℃, 88 ℃, 89 ℃ or 90 ℃ and the like, and other specific values in the range can be selected, which is not described herein.
Preferably, the spraying time in step (2) is 3-4h, such as 3h, 3.5h or 4h, etc., the speed is 1100-1300r/min, such as 1100r/min, 1200r/min or 1300r/min, etc., and other specific values in the range can be selected, which is not described herein.
Preferably, after the coating material is sprayed in step (2), the product is dried, and the temperature is 80-90 ℃, for example, 80 ℃, 82 ℃, 83 ℃, 84 ℃, 85 ℃, 86 ℃, 87 ℃, 88 ℃, 89 ℃ or 90 ℃, and other specific values in the range can be selected, which is not described herein.
As a preferable technical scheme of the invention, the preparation method of the enteric sodium butyrate microcapsule comprises the following steps:
(1) mixing sodium butyrate and molten auxiliary materials at 80-90 deg.C for 30-60min, and coating to obtain inner core layer;
(2) and (2) spraying a coating material on the surface of the inner core layer prepared in the step (1) at the temperature of 80-90 ℃ for 3-4h at the speed of 1100-1300r/min, and drying at the temperature of 80-90 ℃ to obtain the enteric sodium butyrate microcapsule.
In a third aspect, the invention provides a feed additive comprising sodium enteric butyrate microcapsules as described above.
In a fourth aspect, the present invention provides a feed comprising a feed additive as described above.
Compared with the prior art, the invention has the following beneficial effects:
the enteric sodium butyrate microcapsule preparation does not have rancidity-like smell, is not easy to absorb moisture, has good fluidity and dispersibility, can be slowly dissolved in intestinal tracts, achieves intestinal tract targeted release, and remarkably improves the absorption effect. Compared with the common sodium butyrate powder, when the enteric sodium butyrate microcapsule preparation is used as a feed additive for feeding animals, the average daily feed intake and daily gain of the animals can be obviously improved, the feed-weight ratio is reduced, and the diarrhea rate is reduced; the content of harmful bacteria such as escherichia coli in the ileum and colon of animals can be obviously reduced, and beneficial bacteria such as lactobacillus and bifidobacterium in the colon and cecum can be obviously increased; more importantly, the intestinal tract of the young animal is not well developed, and after weaning, the changes of the intestinal tract forms such as the weight loss of the intestinal mucosa, the intestinal villus atrophy, the epithelial cell shedding and the like seriously affect the digestion capability and the nutrient utilization of the young animal.
Drawings
Fig. 1 is an appearance pattern of the enteric sodium butyrate microcapsules according to the present invention.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
The sodium butyrate raw material related to the following examples is feed additive sodium butyrate, the content of which is 98%, and the sodium butyrate raw material is purchased from Jiangxi Conbai farming-grazing development company Limited.
Example 1
The embodiment provides an enteric sodium butyrate microcapsule, which comprises an inner core layer and a coating material layer coated on the surface of the inner core layer; the inner nuclear layer comprises a sodium butyrate core and an auxiliary material layer wrapping the sodium butyrate core. The auxiliary materials are a mixture of hardened oil, glucose and fat powder, and respectively account for 40%, 15% and 20% of the total mass of the microcapsule. The coating material is hydroxypropyl methyl cellulose acetate succinate, and accounts for 10% of the total mass of the microcapsule.
The preparation method comprises the following steps:
(1) mixing sodium butyrate and molten auxiliary materials at 85 deg.C for 40min, and coating to obtain inner core layer;
(2) and (2) spraying a coating material on the surface of the inner core layer prepared in the step (1) at 85 ℃ for 4 hours, and drying at 85 ℃ to obtain the enteric sodium butyrate microcapsule.
Example 2
The embodiment provides an enteric sodium butyrate microcapsule, which comprises an inner core layer and a coating material layer coated on the surface of the inner core layer; the inner nuclear layer comprises a sodium butyrate core and an auxiliary material layer wrapping the sodium butyrate core. The auxiliary materials are a mixture of glyceryl monostearate, stearyl alcohol and glucose, and respectively account for 40%, 30% and 10% of the total mass of the microcapsule. The coating material is a mixture of hydroxypropyl methylcellulose phthalate and polyvinyl acetate phthalate, and respectively accounts for 2% and 3% of the total mass of the microcapsule.
The preparation method comprises the following steps:
(1) mixing sodium butyrate and molten auxiliary materials at 80 deg.C for 50min, and coating to obtain inner core layer;
(2) and (2) spraying a coating material on the surface of the inner core layer prepared in the step (1) at 80 ℃ for 4 hours, and drying at 80 ℃ to obtain the enteric sodium butyrate microcapsule.
Example 3
The embodiment provides an enteric sodium butyrate microcapsule, which comprises an inner core layer and a coating material layer coated on the surface of the inner core layer; the inner nuclear layer comprises a sodium butyrate core and an auxiliary material layer wrapping the sodium butyrate core. The auxiliary material is a mixture of fat powder and auxiliary powder, and respectively accounts for 50% and 25% of the total mass of the microcapsule. The coating material is a mixture of cellulose acetate and hydroxypropyl methylcellulose acetate succinate, and respectively accounts for 5% and 5% of the total mass of the microcapsule.
The preparation method comprises the following steps:
(1) mixing sodium butyrate and molten auxiliary materials at 90 deg.C for 30min, and coating to obtain inner core layer;
(2) and (2) spraying a coating material on the surface of the inner core layer prepared in the step (1) at 90 ℃ for 3 hours, and drying at 90 ℃ to obtain the enteric sodium butyrate microcapsule.
Example 4
The embodiment provides an enteric sodium butyrate microcapsule, which comprises an inner core layer and a coating material layer coated on the surface of the inner core layer; the inner nuclear layer comprises a sodium butyrate core and an auxiliary material layer wrapping the sodium butyrate core. The difference between the product of the embodiment 1 and the auxiliary materials is that the mass ratio of the auxiliary materials is as follows: the auxiliary materials are a mixture of hardened oil, glucose and fat powder, and respectively account for 35%, 5% and 15% of the total mass of the microcapsule. The coating material is hydroxypropyl methyl cellulose acetate succinate, and accounts for 30% of the total mass of the microcapsule.
The preparation process is as in example 1.
Example 5
The embodiment provides an enteric sodium butyrate microcapsule, which comprises an inner core layer and a coating material layer coated on the surface of the inner core layer; the inner nuclear layer comprises a sodium butyrate core and an auxiliary material layer wrapping the sodium butyrate core. The difference between the product of the embodiment 1 and the auxiliary materials is that the mass ratio of the auxiliary materials is as follows: the auxiliary materials are a mixture of hardened oil, glucose and fat powder, and respectively account for 50%, 3% and 30% of the total mass of the microcapsule. The coating material is hydroxypropyl methyl cellulose acetate succinate, and accounts for 2% of the total mass of the microcapsule.
The preparation process is as in example 1.
Example 6
The embodiment provides an enteric sodium butyrate microcapsule, which comprises an inner core layer and a coating material layer coated on the surface of the inner core layer; the inner nuclear layer comprises a sodium butyrate core and an auxiliary material layer wrapping the sodium butyrate core. The difference between the coating material and the product of the embodiment 1 is that the mass ratio of the coating material is as follows: the auxiliary materials are a mixture of hardened oil, glucose and fat powder, and respectively account for 40%, 22% and 20% of the total mass of the microcapsule. The coating material is hydroxypropyl methyl cellulose acetate succinate, and accounts for 3% of the total mass of the microcapsule.
The preparation process is as in example 1.
Example 7
The embodiment provides an enteric sodium butyrate microcapsule, which comprises an inner core layer and a coating material layer coated on the surface of the inner core layer; the inner nuclear layer comprises a sodium butyrate core and an auxiliary material layer wrapping the sodium butyrate core. The difference between the coating material and the product of the embodiment 1 is that the mass ratio of the coating material is as follows: the auxiliary materials are a mixture of hardened oil, glucose and fat powder, and respectively account for 40%, 10% and 20% of the total mass of the microcapsule. The coating material is hydroxypropyl methyl cellulose acetate succinate, and accounts for 15% of the total mass of the microcapsule.
The preparation process is as in example 1.
Comparative example 1
The comparative example provides an enteric sodium butyrate microcapsule, which only has an inner core layer and does not have a coating material layer coated on the surface of the inner core layer; the inner nuclear layer comprises a sodium butyrate core and an auxiliary material layer wrapping the sodium butyrate core. The auxiliary materials are a mixture of hardened oil, glucose and fat powder, and respectively account for 40%, 25% and 20% of the total mass of the microcapsule.
The preparation method comprises the following steps:
(1) mixing the sodium butyrate raw material and the auxiliary material in a molten state at 85 ℃ for 40min, and coating to obtain an inner nuclear layer, namely the enteric sodium butyrate microcapsule.
Evaluation test:
the enteric sodium butyrate microcapsule products obtained in examples 1 to 7 and comparative example 1 were evaluated as follows, while a commercially available sodium butyrate powder product (feed additive sodium butyrate, content 98%, incorporated by the manufacturer, jiang xi conifer farming-grazing development co., ltd.) was used as a control.
The test operation method comprises the following steps: selecting 60 weaned pigs (28-day-old weaning) with similar body weight, randomly dividing into 10 groups, namely test groups 1-9 and control groups, and feeding the weaned pigs with different daily rations for 6 groups, and performing production performance evaluation, intestinal bacteria evaluation and small intestine length and weight evaluation 28 days later. Wherein test group 1 was basal diet +1kg/t of the product of example 1; test group 2 was basal diet +1kg/t of the product of example 2; test group 3 was basal diet +1kg/t of the product of example 3; test group 4 was basal diet +1kg/t of the product of example 4; test group 5 was basal diet +1kg/t of the product of example 5; test group 6 was basal diet +1kg/t of the product of example 6; test group 7 was basal diet +1kg/t of the product of example 7; test group 8 was basal diet +1kg/t comparative example 1 product; test group 9 was basal diet +1kg/t of commercially available powder; the control group was basal diet group.
(1) Evaluation of production Properties
The operation method comprises the following steps: piglets were weighed on an empty stomach on day 28 of the trial and the Average Daily Feed Intake (ADFI), Average Daily Gain (ADG), feed-to-weight ratio (F/G) and diarrhea rate were calculated and the results are shown in table 1.
TABLE 1
Note: the test results are all expressed as mean value + -standard deviation, with the same lower case letters on the shoulder marked with no significant difference (P > 0.05) and the different lower case letters with significant difference (P <0.05)
As can be seen from the data in Table 1: the daily ration added with the enteric sodium butyrate microcapsule product can obviously increase the daily feed intake and daily gain of weaned piglets; significantly reduces the feed-to-weight ratio and the diarrhea rate of piglets (P < 0.05).
(2) Evaluation of intestinal bacteria
The operation method comprises the following steps: after 28 days, the cecum contents of the pigs were slaughtered and accurately weighed, and diluted with sterile physiological saline to a final concentration of 10mg/mL bacterial suspension, which was a 100-fold dilution of the mother liquor. Accurately sucking 0.1mL of bacterial suspension by using a 0.2mL sterile pipette, putting the bacterial suspension into a clean sterilized test tube containing 0.9mL of normal saline, and uniformly mixing the suspension in the test tube to obtain 10-1Diluting the bacterial liquid by times. Another suction tube 10-1Sucking 0.1mL of the test tube, placing the test tube into a test tube containing 0.9mL of physiological saline, and repeating the rest steps to obtain 10-1、10-2、10-3、10-4、10-5、10-6Diluted bacterial liquid. And (3) respectively inoculating 0.01mL of diluent into 3 culture media for carrying out isolated culture on escherichia coli, lactobacillus and bifidobacterium, and detecting each diluent for 3 times. At the same time, physiological saline was added to the sterile plate as a blank. And (3) taking out the culture dish after 24-48h of culture, calculating the average number of colonies at the same dilution, and calculating the total viable count per milliliter according to the average number of the colonies at three times of the same dilution multiplied by 10. The data were analyzed using JMP10 statistical software and the results are shown in table 2.
TABLE 2
Note: the test results are all expressed as mean value + -standard deviation, with the same lower case letters on the shoulder marked with no significant difference (P > 0.05) and the different lower case letters with significant difference (P <0.05)
As can be seen from the data in Table 2: the addition of the enteric sodium butyrate microcapsule related to the invention into daily ration can remarkably promote the number of beneficial intestinal flora such as bifidobacteria and the number of lactobacillus (P <0.05), and can remarkably inhibit the number of harmful intestinal flora such as escherichia coli (P < 0.05).
(3) Small intestine Length and weight evaluation
The operation method comprises the following steps: after 28 days, the duodenum, jejunum and ileum were slaughtered and taken for length and weight measurements. The results are shown in Table 3.
TABLE 3
Note: the test results are all expressed as mean value + -standard deviation, with the same lower case letters on the shoulder marked with no significant difference (P > 0.05) and the different lower case letters with significant difference (P <0.05)
As can be seen from the data in Table 3: the addition of the enteric sodium butyrate microcapsules in daily ration can remarkably promote the length and weight (P is less than 0.05) of duodenum, jejunum and ileum, remarkably promote the growth of small intestine epithelial cells and be more beneficial to the absorption of nutrient substances by the small intestine.
(4) Evaluation of dissolution Effect
The operation method comprises the following steps: the effect is tested by an in vitro dissolution test simulating artificial gastric juice and intestinal juice.
Preparing artificial gastric juice: taking 16.4mL of dilute hydrochloric acid, adding about 800mL of water, adding 10g of pepsin, shaking up, adding water and fixing the volume to 1000mL to obtain the compound preparation;
preparing artificial intestinal juice: 6.8g of potassium dihydrogen phosphate was taken and dissolved in 500mL of water. Dissolving pancreatin 10g in water, mixing the two solutions, adjusting pH to 6.8 with 0.1mol/L sodium hydroxide solution, and adding water to a constant volume of 1000 mL.
And (3) determining the dissolution rate of gastric juice: 250mL of degassed artificial gastric juice is measured and injected into each operation container, the temperature of the solvent is kept at (37 +/-0.5) DEG C by heating, and the rotating speed can be adjusted at (60 +/-1) r/min. Respectively weighing 6 samples to be tested, each sample is 10g, putting the samples into 6 operating containers, immediately starting rotation and starting timing, respectively taking out one sample in 0.5, 1, 2, 4, 6 and 8 hours, filtering the sample by filter paper, drying the sample at a low temperature to constant weight, measuring the content of sodium butyrate by a hydrochloric acid titration method, and calculating the dissolution amount of each sample. The results are shown in Table 4.
Intestinal juice dissolution determination: 250mL of degassed artificial intestinal juice is measured and injected into each operation container, the temperature of the solvent is kept at (37 +/-0.5) DEG C by heating, and the rotating speed can be adjusted at (60 +/-1) r/min. Respectively weighing 6 samples to be tested, each sample is 5g, putting the samples into 6 operating containers, immediately starting rotation and starting timing, respectively taking 1 sample out after 1, 2, 4, 8, 16 and 32 hours, filtering the samples by filter paper, drying the samples at a low temperature to constant weight, measuring the content of sodium butyrate by a hydrochloric acid titration method, and calculating the dissolution amount of each sample. The results are shown in Table 5.
TABLE 4
TABLE 5
As can be seen from the data in tables 4 and 5: the enteric sodium butyrate microcapsule provided by the invention can realize the effect of protecting sodium butyrate from passing the stomach and enabling the sodium butyrate to be slowly released in intestinal tracts.
The applicant states that the invention is illustrated by the above examples to provide an enteric sodium butyrate microcapsule, a preparation method and application thereof, but the invention is not limited to the above examples, that is, the invention is not limited to the above examples. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
Claims (10)
1. The enteric sodium butyrate microcapsule is characterized by comprising an inner core layer and a coating material layer coated on the surface of the inner core layer; the inner nuclear layer comprises a sodium butyrate core and an auxiliary material layer wrapping the sodium butyrate core.
2. The enteric sodium butyrate microcapsule according to claim 1, wherein the auxiliary material comprises any one or a combination of at least two of fat powder, auxiliary powder, glucose, antimicrobial peptide, stearic acid, glyceryl monostearate, stearyl alcohol, saturated triglyceride, monoglyceride or paraffin;
preferably, the auxiliary material accounts for 65-80% of the enteric sodium butyrate microcapsule by mass.
3. The enteric sodium butyrate microcapsule according to claim 1 or 2, wherein the coating material comprises any one or a combination of at least two of hypromellose phthalate, polyvinyl acetate phthalate, cellulose acetate phthalate, hypromellose acetate succinate or acrylic resin;
preferably, the coating material accounts for 5-10% of the enteric sodium butyrate microcapsule by mass.
4. The enteric sodium butyrate microcapsules of any one of claims 1-3, wherein the particle size of said enteric sodium butyrate microcapsules is 180-355 μm.
5. The process for the preparation of enteric sodium butyrate microcapsules according to any one of claims 1 to 4, characterized in that it comprises:
(1) adding sodium butyrate into molten auxiliary materials, performing primary coating, and passing through a 80-mesh screen to prepare microcapsule granules serving as an inner core layer;
(2) and (2) spraying a coating material on the surface of the inner core layer prepared in the step (1) to obtain the enteric sodium butyrate microcapsule.
6. The method for preparing enteric sodium butyrate microcapsules according to claim 5, wherein the mixing means of step (1) includes stirring;
preferably, the temperature of the mixing in the step (1) is 80-90 ℃;
preferably, the time for mixing the coating in the step (1) is 30-60 min.
7. The method for preparing enteric sodium butyrate microcapsules according to claim 5 or 6, wherein the spraying temperature in the step (2) is 80-90 ℃;
preferably, the spraying time in the step (2) is 3-4h, and the speed is 1100-1300 r/min;
preferably, after the spraying of the coating material in the step (2) is finished, the product is dried at the temperature of 80-90 ℃.
8. The process for the preparation of enteric sodium butyrate microcapsules according to any one of claims 5 to 7, characterized in that it comprises:
(1) mixing sodium butyrate and molten auxiliary materials at 80-90 deg.C for 30-60min, and coating to obtain inner core layer;
(2) and (2) spraying a coating material on the surface of the inner core layer prepared in the step (1) at the temperature of 80-90 ℃ for 3-4h at the speed of 1100-1300r/min, and drying at the temperature of 80-90 ℃ to obtain the enteric sodium butyrate microcapsule.
9. Feed additive, characterized in that it comprises sodium enteric butyrate microcapsules according to any one of claims 1 to 4.
10. A feed comprising the feed additive of claim 9.
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