CN103845306A - Milk fragrance type tilmicosin enteric microcapsule and preparation method thereof - Google Patents
Milk fragrance type tilmicosin enteric microcapsule and preparation method thereof Download PDFInfo
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- CN103845306A CN103845306A CN201210508927.7A CN201210508927A CN103845306A CN 103845306 A CN103845306 A CN 103845306A CN 201210508927 A CN201210508927 A CN 201210508927A CN 103845306 A CN103845306 A CN 103845306A
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- tilmicosin
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Abstract
The invention relates to a milk fragrance type tilmicosin enteric microcapsule, and belongs to the technical filed of veterinary drugs. The tilmicosin enteric microcapsule is composes of a capsule core layer and a capsule coat layer; wherein the capsule core layer is composed of tilmicosin or tilmicosin phosphate and proper auxiliary materials, and the capsule coat layer is composed of a composite enteric material. The milk fragrance type tilmicosin enteric microcapsule can radically cover the bitterness of tilmicosin, and has a high encapsulation rate and a small microcapsule particle size.
Description
Technical field
The invention belongs to veterinary drug technical field, relate in particular to one and contain tilmicosin or phosphoric acid tilmicosin milk flavoured type enteric-coated microcapsule and preparation method thereof.
Background technology
Tilmicosin is that Elanco company of the U.S. is in the special antibiotic of semi-synthetic Macrolide poultry of the exploitation eighties in 20th century, there is very strong antibacterial activity, drug resistance is low, has a broad antifungal spectrum, all gram positive bacterias and part gram negative bacteria, Mycoplasma, spirillum etc. are all had to inhibitory action, especially multiple mycoplasma and spirillum are also had to very strong inhibitory action.This medicine, successively in the clinical application that goes through of the countries such as Australia, Brazil, France, Malaysia, Italy, Spain, the U.S., is used for the treatment of the infectious disease of the animals such as goat, milch cow, pig, chicken.Tilmicosin drug molecule has strong bitterness, the non-constant of palatability when oral administration, and its stomach to animal has certain zest, and this has become the sixty-four dollar question that affects the clinical use of tilmicosin.Patent CN101879141 discloses a kind of taste-masking tilmicosin gastric-soluble particle preparation, but said preparation has zest to the stomach of animal.Patent CN102319181 discloses a kind of coated technique of microcapsule-type animal drug, prepared the animal drug of microcapsule-type by this technique, complex process, cost are high, and the microcapsule of preparation is single coats, its microcrystalline cellulose excipients serves as filler or binding agent, animal easily bites coating into pieces while food and has the bitterness of major ingredient tilmicosin, affects palatability.Patent CN 102688220 discloses a kind of tilmicosin microcapsule formulation preparation method of tasteless, enteric, and the preparation particle diameter that the method provides is larger, and bioavailability is low, and preparation is tasteless type, and animal feed intake is improved and there is no obvious effect.
Summary of the invention
The invention provides a kind of milk flavoured type tilmicosin enteric-coated microcapsule, microcapsule of the present invention is characterized in that, said preparation microcapsule diameter is 50-200 μ m, is preferably 100-150 μ m, and it has unique milk fragrance.
Milk flavoured type tilmicosin enteric-coated microcapsule provided by the invention agent comprises capsule heart layer and capsule clothing layer, capsule heart layer is to be mixed by tilmicosin or phosphoric acid tilmicosin and appropriate carrier, appropriate carrier is one or more in 12 carbon-18 carbon fatty acid, the two mass ratio is 1-2:1-1.5, capsule clothing layer is compound Enteric Materials, described compound enteric material is hydroxypropyl methylcellulose, hydroxypropyl methylcellulose succinic acid acetate, sorbester p17, milk flavor and solvent composition, and solvent is 75%-85% ethanol.The w/v of each component and solvent is: hydroxypropyl methylcellulose 1-5%, hydroxypropyl methylcellulose succinic acid acetate 10-20%, diethyl phthalate 1-5%, sorbester p17 1-3%, milk flavor 1-2%, capsule heart layer and capsule clothing layer w/v are 2-3:1-1.5.
Tilmicosin microcapsule of the present invention is prepared by the following method:
(1) tilmicosin or the phosphoric acid tilmicosin that take recipe quantity carry out micronizing, make its particle diameter reach 30-100 μ m, then add appropriate carrier, and the two mass ratio is 1-2:1-1.5, at 60-100 ℃ by the two mix homogeneously.
(2) said mixture is put into coating pan and added 30%-50% oligofructose liquid mist projection granulating, adding oligofructose liquid and volume of mixture weight ratio is 1:3-5, and 50-55 ℃ of hot air drying obtains capsule heart layer.
(3) take hydroxypropyl methylcellulose 1-5%, hydroxypropyl methylcellulose succinic acid acetate 10-20%, diethyl phthalate 1-5%, sorbester p17 1-3%, milk flavor 1-2%, 75%-85% ethanol is settled to 100ml, obtains capsule clothing layer.
(4) capsule heart layer is mixed with 2-3:1-1.5 with capsule clothing layer, carry out under the following conditions encapsulation: capsule heart layer amount 100-500g, filtrated air pressure 2-6kg/cm
2, hot air temperature 40-60 ℃, fluid bed flow velocity 0.5-1.5m
2/ minute, nozzle is 0.2-0.8m
2/ minute, capsule clothing flow quantity 30-150ml/ hour, encapsulation time 1-2 hour, the 100-140 order microcapsule of system, to obtain final product.
The specific embodiment
Following examples only elaborate to the present invention, but also limit never in any form the present invention
Embodiment 1
The preparation of capsule heart layer:
Take phosphoric acid tilmicosin 30kg, carry out micronizing, add 30kg 12 carbon fatty acids, mix homogeneously at 60 ℃, puts into coating pan by mixture and adds 20kg 30% oligofructose liquid mist projection granulating, and 50-55 ℃ of hot air drying, obtains capsule heart layer.
Compound enteric capsule clothing layer is prepared 65L according to the following formulation:
Take hydroxypropyl methylcellulose 10g, hydroxypropyl methylcellulose succinic acid acetate 100g, diethyl phthalate 10g, sorbester p17 10g, milk flavor 10g, add 75% ethanol to be settled to 1000ml, to obtain final product.
Encapsulation preparation condition is as follows:
Capsule heart layer is mixed with 2:1 with capsule clothing layer, carry out under the following conditions encapsulation: filtrated air pressure 2kg/cm
2, 40 ℃ of hot air temperatures, fluid bed flow velocity 0.5m
2/ minute, nozzle is 0.2m
2/ minute, capsule clothing flow quantity 30ml/ hour, 1 hour encapsulation time, the 100-140 order microcapsule of system, to obtain final product.
Embodiment 2
The preparation of capsule heart layer:
Take phosphoric acid tilmicosin 40kg, carry out micronizing, add 45kg 15 carbon fatty acids, mix homogeneously at 80 ℃, puts into coating pan by mixture and adds 30kg 40% oligofructose liquid mist projection granulating, and 50-55 ℃ of hot air drying, obtains capsule heart layer.
Compound enteric capsule clothing layer is prepared 50L according to the following formulation:
Take hydroxypropyl methylcellulose 20g, hydroxypropyl methylcellulose succinic acid acetate 150g, diethyl phthalate 15g, sorbester p17 15g, milk flavor 15g, add 80% ethanol to be settled to 1000ml, to obtain final product.
Encapsulation preparation condition is as follows:
Capsule heart layer is mixed with 2:1 with capsule clothing layer, carry out under the following conditions encapsulation: filtrated air pressure 4kg/cm
2, 50 ℃ of hot air temperatures, fluid bed flow velocity 1m
2/ minute, nozzle is 0.4m
2/ minute, capsule clothing flow quantity 80ml/ hour, 1.5 hours encapsulation time, the 100-140 order microcapsule of system, to obtain final product.
Embodiment 3
The preparation of capsule heart layer:
Take phosphoric acid tilmicosin 35kg, carry out micronizing, add 52.5kg 18 carbon fatty acids, mix homogeneously at 100 ℃, puts into coating pan by mixture and adds 17.5kg 50% oligofructose liquid mist projection granulating, and 50-55 ℃ of hot air drying, obtains capsule heart layer.
Compound enteric capsule clothing layer is prepared 50L as follows:
Take hydroxypropyl methylcellulose 50g, hydroxypropyl methylcellulose succinic acid acetate 200g, diethyl phthalate 50g, sorbester p17 30g, milk flavor 20g, add 85% ethanol to be settled to 1000ml, to obtain final product.
Encapsulation preparation condition is as follows:
Capsule heart layer is mixed with 3:1 with capsule clothing layer, carry out under the following conditions encapsulation: filtrated air pressure 6kg/cm
2, 60 ℃ of hot air temperatures, fluid bed flow velocity 1.5m
2/ minute, nozzle is 0.8m
2/ minute, capsule clothing flow quantity 150ml/ hour, encapsulation time 2 h, the 100-140 order microcapsule of system, to obtain final product.
Experimental example 1: entrapment efficiency determination
Entrapment efficiency determination method: precision takes sample 0.5g, is placed in 10ml volumetric flask, is diluted with water to scale, and the ultrafiltration of ultrafiltration instrument discards just filtrate, and getting continuous filtrate is need testing solution.Draw respectively need testing solution, reference substance solution is carried out content detection, measures content value and is designated as W, measures this product medicine total content, measured value is designated as W1.Be calculated as follows sample envelop rate:
Envelop rate En=(W1-W)/W1*100%
Measure as stated above the envelop rate of embodiment 1-3 sample, each embodiment gets three batch samples and measures, and measured value is averaged, measurement result table 1:
Table 1 entrapment efficiency determination result
| Embodiment title | Envelop rate |
| Embodiment 1 | 92.1% |
| Embodiment 2 | 98.3% |
| Embodiment 3 | 95.2% |
Conclusion: result of the test shows, microcapsule envelop rate of the present invention is good
Experimental example 2: microcapsule prepared by embodiment 2 of the present invention and commercially available common tilmicosin pre-mixing agent, the comparison of commercially available tilmicosin microcapsule palatability
Experimental technique: choose 40 healthy market pigs, body weight 40-50kg, is divided into 4 groups at random, 10 every group, first three groups feed respectively tilmicosin microcapsule of the present invention, commercially available tilmicosin pre-mixing agent, commercially available tilmicosin microcapsule, dosage is in tilmicosin, 200g/ ton feedstuff, and the 4th group is matched group, do not add any medicine, the examination phase is one week, records every group of per day feed intake of test group, tests data in table 2:
Table 2 feed intake contrast test data
| Experimental group | Add medicine | Per day feed intake |
| First group | Tilmicosin microcapsule of the present invention | 2.85kg |
| Second group | Commercially available tilmicosin microcapsule | 2.14kg |
| The 3rd group | Commercially available common tilmicosin pre-mixing agent | 1.78kg |
| The 4th group | ----- | 1.99kg |
Conclusion: tilmicosin enteric-coated microcapsule agent palatability of the present invention is good, can obviously improve animal feed intake.
Claims (7)
1. a milk flavoured type tilmicosin enteric-coated microcapsule agent, is characterized in that described microcapsule is made up of capsule heart layer and capsule clothing layer.
2. a kind of milk flavoured type tilmicosin enteric-coated microcapsule according to claim 1 agent, is characterized in that said preparation microcapsule diameter is 50-200 μ m.
3. a kind of milk flavoured type tilmicosin enteric-coated microcapsule according to claim 1 and 2 agent, is characterized in that said preparation microcapsule diameter is 100-150 μ m.
4. a kind of milk flavoured type tilmicosin enteric-coated microcapsule according to claim 1 agent, it is characterized in that capsule heart layer is to be mixed by tilmicosin or phosphoric acid tilmicosin and appropriate carrier, appropriate carrier is one or more in 12 carbon-18 carbon fatty acid, and the two mass ratio is 1-2:1-1.5.
5. a kind of milk flavoured type tilmicosin enteric-coated microcapsule according to claim 1 agent, it is characterized in that capsule clothing layer is compound Enteric Materials, described compound enteric material is hydroxypropyl methylcellulose, hydroxypropyl methylcellulose succinic acid acetate, sorbester p17, milk flavor and solvent composition, and solvent is 75%-85% ethanol.
6. a kind of milk flavoured type tilmicosin enteric-coated microcapsule according to claim 1 agent, the w/v that it is characterized in that the each component of compound Enteric Materials and solvent is: hydroxypropyl methylcellulose 1-5%, hydroxypropyl methylcellulose succinic acid acetate 10-20%, diethyl phthalate 1-5%, sorbester p17 1-3%, milk flavor 1-2%, capsule heart layer and capsule clothing layer w/v are 2-3:1-1.5.
7. a kind of milk flavoured type tilmicosin enteric-coated microcapsule according to claim 2 agent, is characterized in that being prepared from by the following method:
(1) tilmicosin or the phosphoric acid tilmicosin that take recipe quantity carry out micronizing, make its particle diameter reach 30-100 μ m, then add 12 carbon-18 carbon fatty acid, and the two mass ratio is 1-2:1-1.5, at 60-100 ℃ by the two mix homogeneously;
(2) said mixture is put into coating pan and added 30%-50% oligofructose liquid mist projection granulating, adding oligofructose liquid and volume of mixture weight ratio is 1:3-5, and 50-55 ℃ of hot air drying obtains capsule heart layer;
(3) take hydroxypropyl methylcellulose 1-5%, hydroxypropyl methylcellulose succinic acid acetate 10-20%, diethyl phthalate 1-5%, sorbester p17 1-3%, milk flavor 1-2%, 75%-85% ethanol is settled to 100%, obtains capsule clothing layer.
(4) capsule heart layer is mixed with 2-3:1-1.5 with capsule clothing layer, carry out under the following conditions encapsulation: capsule heart amount 100-500g, filtrated air pressure 2-6kg/cm2, hot air temperature 40-60 ℃, fluid bed flow velocity 0.5-1.5m2/ minute, nozzle is 0.2-0.8m2/ minute, capsule clothing flow quantity 30-150ml/ hour, encapsulation time 1-2 hour, the 100-140 order microcapsule of system, to obtain final product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201210508927.7A CN103845306A (en) | 2012-11-30 | 2012-11-30 | Milk fragrance type tilmicosin enteric microcapsule and preparation method thereof |
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| CN201210508927.7A CN103845306A (en) | 2012-11-30 | 2012-11-30 | Milk fragrance type tilmicosin enteric microcapsule and preparation method thereof |
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| CN103845306A true CN103845306A (en) | 2014-06-11 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105418704A (en) * | 2015-11-11 | 2016-03-23 | 郑州后羿制药有限公司 | Tilmicosin-saccharin compound and preparation method thereof |
| CN106822034A (en) * | 2016-12-02 | 2017-06-13 | 北京科百大科技有限责任公司 | The capsule core material or micro-capsule of drug containing are prepared as capsule core material with maize cob meal |
| CN106924189A (en) * | 2017-04-28 | 2017-07-07 | 华南农业大学 | A kind of Tilmicosin enteric-coated sustained release powder and its preparation method and application |
| CN108210480A (en) * | 2016-12-13 | 2018-06-29 | 河南后羿实业集团有限公司 | A kind of preparation method of Tilmicosin micro-capsule |
| CN112494460A (en) * | 2020-12-10 | 2021-03-16 | 浙江大飞龙动物保健品股份有限公司 | Tilmicosin powder and preparation method thereof |
-
2012
- 2012-11-30 CN CN201210508927.7A patent/CN103845306A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105418704A (en) * | 2015-11-11 | 2016-03-23 | 郑州后羿制药有限公司 | Tilmicosin-saccharin compound and preparation method thereof |
| CN105418704B (en) * | 2015-11-11 | 2018-08-31 | 河南后羿实业集团有限公司 | A kind of Tilmicosin-saccharin compound and preparation method thereof |
| CN106822034A (en) * | 2016-12-02 | 2017-06-13 | 北京科百大科技有限责任公司 | The capsule core material or micro-capsule of drug containing are prepared as capsule core material with maize cob meal |
| CN108210480A (en) * | 2016-12-13 | 2018-06-29 | 河南后羿实业集团有限公司 | A kind of preparation method of Tilmicosin micro-capsule |
| CN106924189A (en) * | 2017-04-28 | 2017-07-07 | 华南农业大学 | A kind of Tilmicosin enteric-coated sustained release powder and its preparation method and application |
| CN106924189B (en) * | 2017-04-28 | 2021-08-24 | 华南农业大学 | Tilmicosin sustained-release enteric-coated powder and preparation method and application thereof |
| CN112494460A (en) * | 2020-12-10 | 2021-03-16 | 浙江大飞龙动物保健品股份有限公司 | Tilmicosin powder and preparation method thereof |
| CN112494460B (en) * | 2020-12-10 | 2022-03-11 | 浙江大飞龙动物保健品股份有限公司 | Tilmicosin powder and preparation method thereof |
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Application publication date: 20140611 |