CN105106164B - A kind of fresh-water fishes coating Enrofloxacin micropill and preparation method thereof - Google Patents
A kind of fresh-water fishes coating Enrofloxacin micropill and preparation method thereof Download PDFInfo
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- CN105106164B CN105106164B CN201510606171.3A CN201510606171A CN105106164B CN 105106164 B CN105106164 B CN 105106164B CN 201510606171 A CN201510606171 A CN 201510606171A CN 105106164 B CN105106164 B CN 105106164B
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Abstract
The invention discloses a kind of fresh-water fishes coating Enrofloxacin micropill and preparation method thereof, solves the problem of medicine of prior art intake is few, and waste is larger, and therapeutic effect is bad.By weight, the present invention is prepared by 5%~20% Enrofloxacin, 60%~75% auxiliary material and 10%~25% coatings.Present invention also offers a kind of preparation method of above-mentioned fresh-water fishes coating Enrofloxacin micropill.Outward appearance of the present invention is in pellets, and particle size is close to fish meal, in water（PH is neutral）The rate of settling is slower, and chance water is insoluble for a long time, will not discharge active ingredient Enrofloxacin into water, after fish search for food it as feed, in its anterior intestine（PH is acid）Outer layer coating material dissolves, and capsule core discharges medicine and plays antibacterial action, and utilization rate is high, and waste is small, will not cause water pollution again.
Description
Technical field
The present invention relates to a kind of fresh-water fishes coating Enrofloxacin micropill and preparation method thereof.
Background technology
In recent years in terms of aquaculture, bacterial infection disease incidence is higher, as septicaemia, stigmatosis, red skin disease,
Fin rot, the especially bacillary enteritis incidence of disease is high, be aquaculture nursery stage most common lethal because.At present,
Had begun in aquaculture using bacterial infection of the various antibacterials for treating fish, due to the special life cycle of fish
Border and feeding are accustomed to, mainly by being fed together with antibacterials are mixed with feed.
At present, in aquaculture, when bacterial infection disease occur in fish, often use antibacterials and feed
The mode fed together is mixed to be administered.It is in powdered mostly due to applying the antibacterials on aquatic products, therefore colony gives
Medicine only has this one kind of spice to feed mode, but the waste of this administering mode is larger, and the medicine that fish can effectively be taken in is very limited,
Optimal therapeutic effect is extremely difficult to, while antibacterial medicament contg is exceeded in water body will also result in water pollution, influences public defend
Raw safety.Therefore, it is badly in need of a kind of administering mode in current aquaculture, drug utilization efficiency high, and meanwhile it is minimum to water pollution
Even without pollution.
The content of the invention
It is an object of the invention to provide a kind of fresh-water fishes coating Enrofloxacin micropill and preparation method thereof, solve existing
The problem of medicine of technology intake is few, and utilization rate is low, and waste is larger, and therapeutic effect is bad.
The present invention is achieved through the following technical solutions：
A kind of fresh-water fishes coating Enrofloxacin micropill, by weight, the micropill be by 5%~20% Enrofloxacin,
60%~75% auxiliary material and 10%~25% coatings are prepared.Wherein, outer layer coating layer is in fresh water（PH is neutral）For a long time
It is insoluble, mainly in the anterior intestine of fish after being taken in by fish（PH is acid）Middle dissolving, capsule core discharge Enrofloxacin, are scattered in enteron aisle.
After Enrofloxacin is absorbed, treated available for general infection, kill various pathogens.Therefore fresh-water fishes coating En Nuosha
Star micropill can be infected oral orally taken for curing fresh water fish bacterial by way of feeding intake, and not interfere with water body safety, utilization rate
It is high.
Further, the auxiliary material is by microcrystalline cellulose, flour, maize cob meal, cornstarch, hydroxypropyl methyl fiber
Element composition.
Further, the coatings are made up of acrylic resin IV, talcum powder and ethanol.
Further, by weight, the micropill by 5% Enrofloxacin, 20% microcrystalline cellulose, 10% flour,
5% maize cob meal, 39% cornstarch, 1% hydroxypropyl methyl cellulose, 20% coatings composition；Wherein, micropill particle diameter
For 20~60 mesh；
Or, the micropill by 10% Enrofloxacin, 12.4% microcrystalline cellulose, 12% flour, 15% maize cob meal,
25% cornstarch, 0.6% hydroxypropyl methyl cellulose, 25% coatings composition；Wherein, micropill particle diameter is 20~60 mesh.
In addition, by weight, the coatings by 13.5% acrylic resin IV, 1.5% talcum powder, 85% ethanol
Composition.
In addition, the particle diameter of the talcum powder is 1200 mesh.
The above-mentioned fresh-water fishes preparation method of coating Enrofloxacin micropill, comprises the following steps：
Prepare capsule core：
（1）Enrofloxacin, microcrystalline cellulose, flour, maize cob meal, cornstarch are well mixed, mixture is made；
（2）Compound concentration is the 1.5% hydroxypropyl methyl cellulose aqueous solution, is added in mixture and makes as adhesive
Obtain softwood；
（3）Strip-shaped materials are made in softwood, and pass through shearing and round as a ball obtained capsule core；
（4）Capsule core is dried with fluid bed dryer, it is standby；
Prepare coating solution：
Acrylic resin IV, ethanol are stirred to after being completely dissolved, add talcum powder, be well mixed, being sufficiently stirred makes point
Dissipate uniformly, produce coating solution；
Prepare micropill：
Dry capsule core is added in fluidized-bed coating machine, sprays into coating solution, coating solution becomes after it has sprayed, dried
For coatings, micropill is produced.
Further, the step（3）Middle softwood obtains bar by the extrusion mechanism that rotating speed is 40r/min, aperture is 1.2mm
Shape material；Shearing and round as a ball obtained capsule core, and now turn of the spheronizator are carried out by the spheronizator that blower fan frequency is 25Hz again
Speed is rotating speed 650r/min, duration 15s.
Yet further, the step（4）Middle capsule core use EAT for 70 DEG C, blower fan frequency be 30Hz fluid bed
Dryer is dried, wherein trembling bag delay 6s.
Further, the step（6）During middle penetrating coating solution, capsule core temperature is kept at 33~37 DEG C.
The present invention has advantages below and beneficial effect：
（1）Outward appearance of the present invention is in pellets, and particle size is close to fish meal, in water（PH is neutral）The rate of settling is slower,
It is insoluble for a long time to meet water, active ingredient Enrofloxacin will not be discharged into water, after fish search for food it as feed, at it
Anterior intestine（PH is acid）Outer layer coating material dissolves, and capsule core discharges medicine and plays antibacterial action, and utilization rate is high, and waste is small, again
Water pollution will not be caused.
（2）Raw material of the present invention easily obtains, and formula is reasonable, and production cost is low, and technological process is simple, use easy to spread.
Embodiment
With reference to embodiment, the present invention is further illustrated, but embodiments of the present invention are not limited to this.
Embodiment 1
A kind of fresh-water fishes coating Enrofloxacin micropill, by weight, by 10% Enrofloxacin, 12.4% microcrystalline cellulose
Element, 12% flour, 15% maize cob meal, 25% cornstarch, 0.6% hydroxypropyl methyl cellulose, 25% coatings group
Into.Wherein, coatings by 13.5% acrylic resin IV, 1.5% talcum powder（The mesh of particle diameter 1200）Ethanol with 85% forms.
Specific preparation method is as follows：
Prepare capsule core：
（1）Enrofloxacin, microcrystalline cellulose, flour, maize cob meal, cornstarch are well mixed, mixture is made；
（2）Compound concentration is the 1.5% hydroxypropyl methyl cellulose aqueous solution, is added in mixture and makes as adhesive
Obtain softwood；
（3）Softwood is added in extruder, now extruder rotating speed 40r/min, aperture 1.2mm, strip-shaped materials is made,
Be then added to blower fan frequency be 25Hz spheronizator carry out shearing and it is round as a ball, now the rotating speed of the spheronizator is rotating speed 650r/
Min, duration 15s, that is, capsule core is made；
（4）Use EAT for 70 DEG C, blower fan frequency be 30Hz fluid bed dryer capsule core is dried to water content
Less than 5%；
Prepare coating solution：
Acrylic resin IV, ethanol are stirred to after being completely dissolved, add talcum powder, be well mixed, being sufficiently stirred makes point
Dissipate uniformly, produce coating solution；
Prepare micropill：
Dry capsule core is added in fluidized-bed coating machine, in the case where medicine is in good fluidized state, keeps capsule core
Temperature slowly sprays into coating solution at 33 DEG C~37 DEG C, gets product micropill after it has sprayed, dried, now micropill particle diameter is 20
~60 mesh.
Embodiment 2
The present embodiment compared with Example 1, only difference is that a kind of proportioning of fresh-water fishes with coating Enrofloxacin micropill
Difference, the proportioning of the present embodiment are as follows：
A kind of fresh-water fishes coating Enrofloxacin micropill, by weight, by 5% Enrofloxacin, 20% microcrystalline cellulose,
10% flour, 5% maize cob meal, 39% cornstarch, 1% hydroxypropyl methyl cellulose, 20% coatings composition.Its
In, coatings by 13.5% acrylic resin IV, 1.5% talcum powder（The mesh of particle diameter 1200）Ethanol with 85% forms.
Embodiment 3
The present embodiment compared with Example 1, only difference is that a kind of proportioning of fresh-water fishes with coating Enrofloxacin micropill
Difference, the proportioning of the present embodiment are as follows：
A kind of fresh-water fishes coating Enrofloxacin micropill, by weight, by 20% Enrofloxacin, 10% microcrystalline cellulose
Element, 9% flour, 19% maize cob meal, 30% cornstarch, 2% hydroxypropyl methyl cellulose, 10% coatings composition.
Wherein, coatings by 13.5% acrylic resin IV, 1.5% talcum powder（The mesh of particle diameter 1200）Ethanol with 85% forms.
Embodiment 4
The present embodiment compared with Example 1, only difference is that a kind of proportioning of fresh-water fishes with coating Enrofloxacin micropill
Difference, the proportioning of the present embodiment are as follows：
A kind of fresh-water fishes coating Enrofloxacin micropill, by weight, by 15% Enrofloxacin, 15% microcrystalline cellulose
Element, 9% flour, 20% maize cob meal, 25% cornstarch, 1% hydroxypropyl methyl cellulose, 15% coatings composition.
Wherein, coatings by 13.5% acrylic resin IV, 1.5% talcum powder（The mesh of particle diameter 1200）Ethanol with 85% forms.
Embodiment 5
The present embodiment compared with Example 1, only difference is that a kind of proportioning of fresh-water fishes with coating Enrofloxacin micropill
Difference, the proportioning of the present embodiment are as follows：
A kind of fresh-water fishes coating Enrofloxacin micropill, by weight, by 13% Enrofloxacin, 12% microcrystalline cellulose
Element, 13% flour, 10.5% maize cob meal, 28% cornstarch, 1.5% hydroxypropyl methyl cellulose, 22% coatings
Composition.Wherein, coatings by 13.5% acrylic resin IV, 1.5% talcum powder（The mesh of particle diameter 1200）With 85% ethanol group
Into.
Embodiment 6
The present embodiment compared with Example 1, only difference is that a kind of proportioning of fresh-water fishes with coating Enrofloxacin micropill
Difference, the proportioning of the present embodiment are as follows：
A kind of fresh-water fishes coating Enrofloxacin micropill, by weight, by 8% Enrofloxacin, 16% microcrystalline cellulose,
7% flour, 11% maize cob meal, 32% cornstarch, 1% hydroxypropyl methyl cellulose, 25% coatings composition.Its
In, coatings by 13.5% acrylic resin IV, 1.5% talcum powder（The mesh of particle diameter 1200）Ethanol with 85% forms.
Embodiment 7
The present embodiment compared with Example 1, only difference is that a kind of proportioning of fresh-water fishes with coating Enrofloxacin micropill
Difference, the proportioning of the present embodiment are as follows：
A kind of fresh-water fishes coating Enrofloxacin micropill, by weight, by 12% Enrofloxacin, 14.2% microcrystalline cellulose
Element, 10% flour, 20% maize cob meal, 25% cornstarch, 0.8% hydroxypropyl methyl cellulose, 18% coatings group
Into.Wherein, coatings by 13.5% acrylic resin IV, 1.5% talcum powder（The mesh of particle diameter 1200）Ethanol with 85% forms.
The gained micropill of embodiments of the invention 1 is subjected to correlation test, it is specific as follows：
First, the stability in in-vitro simulated fresh water
1st, method summary
Sample is added to fresh water（pH6.8）In, acted on 4 hours under the conditions of 20 DEG C with disintegration time tester, constant volume, mistake
Filter, the content of high effective liquid chromatography for measuring Enrofloxacin, the quality of the Enrofloxacin of dissolution in people's fresh water is calculated, so as to count
Calculate the percentage that Enrofloxacin discharges in fresh water.
2nd, reagent
Acetonitrile：Chromatographically pure；Phosphoric acid：Analyze pure；Enrofloxacin reference substance：Purity >=99.8%；Enrofloxacin standard inventory
Liquid：Enrofloxacin reference substance 2.5mg is taken, it is accurately weighed, it is placed in 50mL measuring bottles, adds flowing phased soln and be simultaneously quantitatively diluted to quarter
Degree, shakes up.Stored under the conditions of 4 DEG C, storage life 3 months.
3rd, instrument
Disintegration time tester；Assay balance：Sensibility reciprocal is 0.0001g；High performance liquid chromatograph（Equipped with UV-detector）.
4th, the measure of Enrofloxacin release rate in fresh water
The hanging basket of aperture 0.25mm screen clothes is selected, hanging basket is hung on metallic support by the stainless steel shaft of upper end, is soaked
In the beaker for entering 1000ml, and adjust hanging basket position, when making its decline screen cloth away from beaker bottom 25mm, toward beaker in add temperature
For 37 DEG C ± 1 DEG C of drinking water, screen cloth is at the 15mm of underwater when the hanging basket is increased.Sample 2.0g is taken, is accurate to 0.0002g,
Put respectively in the glass tube of hanging basket, setting time 4 hours, 37 DEG C of temperature, start disintegration tester reaction, after 4 hours, stop；Take out
Solution in beaker, move into 1000mL volumetric flasks, be diluted with water to scale, shake up, take 5mL with triangular flask, adding mobile phase
25mL ultrasonic dissolutions, detect the content of Enrofloxacin in solution.
5th, the quality of Enrofloxacin in solution is determined
（1）Chromatographic condition
Chromatographic column：C18Post, long 250mm, internal diameter 4.6mm, 5 μm of granularity；Column temperature：30℃；
Mobile phase：Acetonitrile+0.025mol/L phosphoric acid solutions（PH value is adjusted to 3.0 with triethylamine）=17+83（Volume
Than）；
Flow velocity：0.5mL/min；Detection wavelength：278nm；Sample size：10μL.
（2）Specimen Determination
The filtrate after ultrasound is taken, crosses 0.45 μm of filter membrane, filtrate is shone as sample solution（1）Chromatographic condition determines, and separately takes grace
Promise sand star standard reserving solution, is measured in the same method.Go out the quality of citric acid in filtrate with calculated by peak area by external standard method, so as to calculate
The percentage that fresh-water fishes are discharged with coating Enrofloxacin micropill in fresh water.
2nd, in-vitro simulated fresh-water fishes anterior intestine disintegration time mensuration
1st, method summary
Sample is added to intestinal juice before appropriate in-vitro simulated fresh-water fishes（PH3.5 hydrochloric acid solution）In, use disintegration time limited
Instrument detects under the conditions of 20 DEG C, and fresh-water fishes must not with complete disintegration time of the coating Enrofloxacin micropill before fresh-water fishes in intestinal juice
More than 1 hour.
2. reagent
Watery hydrochloric acid.
3rd, instrument
Disintegration time tester.
4th, the preparation of in-vitro simulated preceding intestinal juice
Fetch water about 1000ml, and dropwise addition watery hydrochloric acid is appropriate, and regulation pH is 3.5, is produced.
5th, detection method
The hanging basket of aperture 0.25mm screen clothes is selected, hanging basket is hung on metallic support by the stainless steel shaft of upper end, is soaked
In the beaker for entering 1000ml, and adjust hanging basket position, when making its decline screen cloth away from beaker bottom 25mm, toward beaker in add temperature
For 37 DEG C ± 1 DEG C of preceding intestinal juice, screen cloth is at the 15mm of underwater when the hanging basket is increased.Sample 2.0g is taken, puts the glass of hanging basket respectively
In glass pipe, setting time 1 hour, 37 DEG C of temperature, start disintegration tester measure, after 1 hour, fresh-water fishes coating Enrofloxacin micropill
It should all be disintegrated and leach by screen cloth, if any not leaching on a small quantity, but soften and can be by meeting regulation opinion without hard-core person.
3rd, result and analysis
The micropill of the present invention, is handled 4 hours, well-tended appearance does not leach, release rate 0.26% in fresh water；And in anterior intestine
Overwhelming majority disintegration in 50 minutes or so leaches in liquid, by screen cloth, has on a small quantity not by screen cloth, but softened no hard-core.Therefore
Fresh-water fishes coating Enrofloxacin micropill, complies fully with requirement, i.e., is not discharged substantially in fresh water, be most of in the anterior intestine of fish
Release, antibacterial action is played after absorption.Treatment fresh water fish bacterial infection is thus be accordingly used in, small utilization rate height is wasted, does not influence water
Body environment.
According to above-described embodiment, the present invention can be realized well.What deserves to be explained is the premise based on above-mentioned design
Under, to solve same technical problem, some made in the present invention are used without substantial change or polishing
The essence of technical scheme is still as the present invention, therefore it should also be as within the scope of the present invention.
Claims (8)
1. a kind of fresh-water fishes coating Enrofloxacin micropill, it is characterised in that by weight, the micropill is by 5%~20%
Enrofloxacin, 60%~75% auxiliary material and 10%~25% coatings are prepared；
The auxiliary material is made up of microcrystalline cellulose, flour, maize cob meal, cornstarch, hydroxypropyl methyl cellulose；
The coatings are made up of acrylic resin IV, talcum powder and ethanol.
2. a kind of fresh-water fishes coating Enrofloxacin micropill according to right wants 1, it is characterised in that by weight, described
Micropill is by 5% Enrofloxacin, 20% microcrystalline cellulose, 10% flour, 5% maize cob meal, 39% cornstarch, 1%
Hydroxypropyl methyl cellulose, 20% coatings composition；Wherein, micropill particle diameter is 20~60 mesh；
Or, the micropill is by 10% Enrofloxacin, 12.4% microcrystalline cellulose, 12% flour, 15% maize cob meal, 25%
Cornstarch, 0.6% hydroxypropyl methyl cellulose, 25% coatings composition；Wherein, micropill particle diameter is 20~60 mesh.
A kind of 3. fresh-water fishes according to claim 1 coating Enrofloxacin micropill, it is characterised in that by weight, institute
Coatings are stated to be made up of talcum powder, 85% ethanol of 13.5% acrylic resin IV, 1.5%.
4. a kind of fresh-water fishes according to claim 3 coating Enrofloxacin micropill, it is characterised in that the talcum powder
Particle diameter is 1200 mesh.
5. a kind of fresh-water fishes preparation method of coating Enrofloxacin micropill, it is characterised in that comprise the following steps：
Prepare capsule core：
（1）Enrofloxacin, microcrystalline cellulose, flour, maize cob meal, cornstarch are well mixed, mixture is made；
（2）Compound concentration is the 1.5% hydroxypropyl methyl cellulose aqueous solution, is added to as adhesive in mixture and is made soft
Material；
（3）Strip-shaped materials are made in softwood, and pass through shearing and round as a ball obtained capsule core；
（4）Capsule core is dried with fluid bed dryer, it is standby；
Prepare coating solution：
Acrylic resin IV, ethanol are stirred to after being completely dissolved, add talcum powder, be well mixed, being sufficiently stirred makes to disperse
It is even, produce coating solution；
Prepare micropill：
Dry capsule core is added in fluidized-bed coating machine, sprays into coating solution, coating solution is become as bag after it has sprayed, dried
Clothing layer, produces micropill.
A kind of 6. preparation method of fresh-water fishes coating Enrofloxacin micropill according to claim 5, it is characterised in that institute
State step（3）Middle softwood obtains strip-shaped materials by the extrusion mechanism that rotating speed is 40r/min, aperture is 1.2mm；Pass through blower fan frequency again
Rate is that 25Hz spheronizator carries out shearing and round as a ball obtained capsule core, and now the rotating speed of the spheronizator is rotating speed 650r/min, when
Long 15s.
A kind of 7. preparation method of fresh-water fishes coating Enrofloxacin micropill according to claim 6, it is characterised in that institute
State step（4）Middle capsule core use EAT for 70 DEG C, blower fan frequency be 30Hz fluid bed dryer dried, wherein trembling
Bag delay 6s.
A kind of 8. preparation method of fresh-water fishes coating Enrofloxacin micropill according to claim 7, it is characterised in that institute
State step（6）During middle penetrating coating solution, capsule core temperature is kept at 33~37 DEG C.
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| CN108740361B (en) * | 2018-04-26 | 2022-06-28 | 江西派尼生物药业有限公司 | Coated multivitamin and preparation method and application thereof |
| CN110075082B (en) * | 2019-04-12 | 2021-05-18 | 瑞普（天津）生物药业有限公司 | Enrofloxacin quick-release pellet and preparation method thereof |
| CN113960187A (en) * | 2021-09-06 | 2022-01-21 | 新昌和宝生物科技有限公司 | Method for evaluating palatability of coated enrofloxacin by determining encapsulation efficiency |
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| CN102526054A (en) * | 2012-02-23 | 2012-07-04 | 广东大华农动物保健品股份有限公司 | Compound enrofloxacin pellets and preparation method thereof |
| CN102648896A (en) * | 2011-02-28 | 2012-08-29 | 郑州福源动物药业有限公司 | Enrofloxacin slow-release micropill for livestocks, and preparation method of same |
| CN103191064A (en) * | 2012-01-05 | 2013-07-10 | 佳木斯大学 | Animal-use enrofloxacin stomach-positioning pellets, and preparation method thereof |
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| US20050136114A1 (en) * | 2003-12-19 | 2005-06-23 | Council Of Scientific And Industrial Research | Taste masked pharmaceutical compositions comprising bitter drug and pH sensitive polymer |
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| CN102648896A (en) * | 2011-02-28 | 2012-08-29 | 郑州福源动物药业有限公司 | Enrofloxacin slow-release micropill for livestocks, and preparation method of same |
| CN103191064A (en) * | 2012-01-05 | 2013-07-10 | 佳木斯大学 | Animal-use enrofloxacin stomach-positioning pellets, and preparation method thereof |
| CN102526054A (en) * | 2012-02-23 | 2012-07-04 | 广东大华农动物保健品股份有限公司 | Compound enrofloxacin pellets and preparation method thereof |
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