CN105106164A - Coated enrofloxacin micropills for freshwater fish and preparation method of coated enrofloxacin micropills - Google Patents
Coated enrofloxacin micropills for freshwater fish and preparation method of coated enrofloxacin micropills Download PDFInfo
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- CN105106164A CN105106164A CN201510606171.3A CN201510606171A CN105106164A CN 105106164 A CN105106164 A CN 105106164A CN 201510606171 A CN201510606171 A CN 201510606171A CN 105106164 A CN105106164 A CN 105106164A
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Abstract
The invention discloses coated enrofloxacin micropills for freshwater fish and a preparation method of the coated enrofloxacin micropills, and solves the problems of less drug intake, much waste and poor curative effect in the prior art. The coated enrofloxacin micropills are prepared from 5-20 percent of enrofloxacin, 60-75 percent of auxiliary materials and 10-25 parts of a coating layer in percentage by weight. The invention also provides a preparation method of the coated enrofloxacin micropills for freshwater fish. The coated enrofloxacin micropills are pellets in appearance, have the particle diameters approximate to a fish feed, slowly settle in water (the pH is neutral), are nonsoluble for a long time in water, and therefore, cannot release the active ingredient (enrofloxacin) into water. After fish take the coated enrofloxacin micropills as the feed, the material from which the outer coating layer is made is dissolved at the foregut (the pH is acidic), and the pill cores release medicines to play an antimicrobial role. The coated enrofloxacin micropills are extremely high in utilization ratio and small in waste and avoid water pollution.
Description
Technical field
The present invention relates to a kind of fresh-water fishes bag by enrofloxacin micropill and preparation method thereof.
Background technology
In recent years in aquaculture, bacterial infection disease incidence rate is higher, and as septicemia, stigmatosis, erythroderma, gill rot, especially bacterial enteritis sickness rate is high, be aquaculture nursery stage modal lethal because of.At present, aquaculture has been brought into use various antibacterials be used for the treatment of the bacterial infection of fish, the living environment special due to Fish and custom of searching for food, throw something and feed together with antibacterials being mixed with feedstuff.
At present, on aquaculture, when bacterial infection disease appears in Fish, often adopt the mode administration carrying out together with antibacterials being mixed with feedstuff throwing something and feeding.Because the antibacterials be applied on Aquatic product are Powdered mostly, therefore colony's administration only has this one of spice to throw something and feed mode, but this administering mode waste is larger, the medicine that fish can effectively be taken in is very limited, be difficult to reach best therapeutic effect, in water body, antibacterials content overproof also can cause water pollution simultaneously, affects public health security.Therefore, current aquaculture is badly in need of a kind of administering mode, drug utilization efficiency is high, does not even pollute water pollution is minimum simultaneously.
Summary of the invention
The object of the present invention is to provide a kind of fresh-water fishes bag by enrofloxacin micropill and preparation method thereof, the medicine solving prior art absorption is few, and utilization rate is low, and waste is comparatively large, the problem that therapeutic effect is not good.
The present invention is achieved through the following technical solutions:
A kind of fresh-water fishes with bag by enrofloxacin micropill, by weight, described micropill be by the enrofloxacin of 5% ~ 20%, 60% ~ 75% adjuvant and 10% ~ 25% coatings be prepared from.Wherein, outer coatings (pH is neutral) in fresh water is not dissolved for a long time, and dissolve in the main anterior intestine fish (pH is acid) after being taken in by fish, ball core discharges enrofloxacin, is scattered in intestinal.After enrofloxacin is absorbed, can be used for systemic infection treatment, kill various pathogen.Therefore these fresh-water fishes bag can be infected by the mode per os orally taken for curing fresh water fish bacterial fed intake by enrofloxacin micropill, and can not affect water body safety, utilization rate is high.
Further, described adjuvant is made up of microcrystalline Cellulose, flour, maize cob meal, corn starch, hydroxypropyl emthylcellulose.
Further, described coatings is made up of acrylic resin IV, Pulvis Talci and ethanol.
Further, by weight, described micropill by 5% enrofloxacin, the microcrystalline Cellulose of 20%, flour, the maize cob meal of 5%, corn starch, the hydroxypropyl emthylcellulose of 1%, the coatings of 20% of 39% of 10% form; Wherein, micropill particle diameter is 20 ~ 60 orders;
Or described micropill is made up of enrofloxacin, the microcrystalline Cellulose of 12.4%, flour, the maize cob meal of 15%, corn starch, the hydroxypropyl emthylcellulose of 0.6%, the coatings of 25% of 25% of 12% of 10%; Wherein, micropill particle diameter is 20 ~ 60 orders.
In addition, by weight, described coatings by 13.5% the Pulvis Talci of acrylic resin IV, 1.5%, the ethanol of 85% form.
In addition, described talcous particle diameter is 1200 orders.
Above-mentioned fresh-water fishes, are comprised the following steps by the preparation method of enrofloxacin micropill with bag:
Prepare ball core:
(1) by enrofloxacin, microcrystalline Cellulose, flour, maize cob meal, corn starch mix homogeneously, obtained mixture;
(2) compound concentration is the hydroxypropyl emthylcellulose aqueous solution of 1.5%, joins obtained soft material in mixture as binding agent;
(3) soft material is made strip-shaped materials, and by shearing and round as a ball obtained ball core;
(4) ball core fluid bed dryer is dried, for subsequent use;
Prepare coating solution:
By acrylic resin IV, ethanol, be stirred to after dissolving completely, add Pulvis Talci, mix homogeneously, fully stir and make to be uniformly dispersed, obtain coating solution;
Prepare micropill:
The ball core of drying is joined in fluidized-bed coating machine, sprays into coating solution, sprayed until it, coating solution just becomes coatings after drying, obtains micropill.
Further, in described step (3) soft material by rotating speed be 40r/min, aperture is that the extruder of 1.2mm obtains strip-shaped materials; The spheronizator being 25Hz by blower fan frequency again carries out shearing and round as a ball obtained ball core, and now the rotating speed of this spheronizator is rotating speed 650r/min, duration 15s.
Again further, in described step (4), ball core adopts the fluid bed dryer that inlet temperature is 70 DEG C, blower fan frequency is 30Hz to dry, and wherein trembles a bag time delay 6s.
Further, when spraying into coating solution in described step (6), keep ball core temperature at 33 ~ 37 DEG C.
The present invention has the following advantages and beneficial effect:
(1) outward appearance of the present invention is pellets, size is close to fish meal, in water, (pH is neutral) rate of settling is comparatively slow, and chance water is insoluble for a long time, can not be released in water by effective ingredient enrofloxacin, Fish are treated as after feedstuff searches for food, at its anterior intestine (pH is acid) outer coating material dissolves, ball core discharges medicine and plays antibacterial action, and utilization rate is high, waste little, can not water pollution be caused again.
(2) raw material of the present invention very easily obtains, and formula is reasonable, and production cost is low, and technological process is simple, is easy to promote the use of.
Detailed description of the invention
Below in conjunction with 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 with bag by enrofloxacin micropill, by weight, the enrofloxacin by 10%, the microcrystalline Cellulose of 12.4%, 12% flour, the maize cob meal of 15%, corn starch, the hydroxypropyl emthylcellulose of 0.6%, the coatings of 25% of 25% form.Wherein, coatings by 13.5% the Pulvis Talci (particle diameter 1200 order) of acrylic resin IV, 1.5% and the ethanol of 85% form.
Concrete preparation method is as follows:
Prepare ball core:
(1) by enrofloxacin, microcrystalline Cellulose, flour, maize cob meal, corn starch mix homogeneously, obtained mixture;
(2) compound concentration is the hydroxypropyl emthylcellulose aqueous solution of 1.5%, joins obtained soft material in mixture as binding agent;
(3) add in extruder by soft material, now extruder rotating speed 40r/min, aperture are 1.2mm, obtained strip-shaped materials, joining blower fan frequency is again that the spheronizator of 25Hz carries out shearing and round as a ball, now the rotating speed of this spheronizator is rotating speed 650r/min, duration 15s, i.e. obtained ball core;
(4) adopt the fluid bed dryer that inlet temperature is 70 DEG C, blower fan frequency is 30Hz that the oven dry of ball core is less than 5% to water content;
Prepare coating solution:
By acrylic resin IV, ethanol, be stirred to after dissolving completely, add Pulvis Talci, mix homogeneously, fully stir and make to be uniformly dispersed, obtain coating solution;
Prepare micropill:
Join in fluidized-bed coating machine by the ball core of drying, under medicine is in good fluidized state, keeps ball core temperature at 33 DEG C ~ 37 DEG C, slowly spray into coating solution, sprayed until it, get product after drying micropill, now micropill particle diameter is 20 ~ 60 orders.
Embodiment 2
The present embodiment is compared with embodiment 1, and difference is only that a kind of fresh-water fishes are different by the proportioning of enrofloxacin micropill with bag, and the proportioning of the present embodiment is as follows:
A kind of fresh-water fishes with bag by enrofloxacin micropill, by weight, the enrofloxacin by 5%, the microcrystalline Cellulose of 20%, 10% flour, the maize cob meal of 5%, corn starch, the hydroxypropyl emthylcellulose of 1%, the coatings of 20% of 39% form.Wherein, coatings by 13.5% the Pulvis Talci (particle diameter 1200 order) of acrylic resin IV, 1.5% and the ethanol of 85% form.
Embodiment 3
The present embodiment is compared with embodiment 1, and difference is only that a kind of fresh-water fishes are different by the proportioning of enrofloxacin micropill with bag, and the proportioning of the present embodiment is as follows:
A kind of fresh-water fishes with bag by enrofloxacin micropill, by weight, the enrofloxacin by 20%, the microcrystalline Cellulose of 10%, 9% flour, the maize cob meal of 19%, corn starch, the hydroxypropyl emthylcellulose of 2%, the coatings of 10% of 30% form.Wherein, coatings by 13.5% the Pulvis Talci (particle diameter 1200 order) of acrylic resin IV, 1.5% and the ethanol of 85% form.
Embodiment 4
The present embodiment is compared with embodiment 1, and difference is only that a kind of fresh-water fishes are different by the proportioning of enrofloxacin micropill with bag, and the proportioning of the present embodiment is as follows:
A kind of fresh-water fishes with bag by enrofloxacin micropill, by weight, the enrofloxacin by 15%, the microcrystalline Cellulose of 15%, 9% flour, the maize cob meal of 20%, corn starch, the hydroxypropyl emthylcellulose of 1%, the coatings of 15% of 25% form.Wherein, coatings by 13.5% the Pulvis Talci (particle diameter 1200 order) of acrylic resin IV, 1.5% and the ethanol of 85% form.
Embodiment 5
The present embodiment is compared with embodiment 1, and difference is only that a kind of fresh-water fishes are different by the proportioning of enrofloxacin micropill with bag, and the proportioning of the present embodiment is as follows:
A kind of fresh-water fishes with bag by enrofloxacin micropill, by weight, the enrofloxacin by 13%, the microcrystalline Cellulose of 12%, 13% flour, the maize cob meal of 10.5%, corn starch, the hydroxypropyl emthylcellulose of 1.5%, the coatings of 22% of 28% form.Wherein, coatings by 13.5% the Pulvis Talci (particle diameter 1200 order) of acrylic resin IV, 1.5% and the ethanol of 85% form.
Embodiment 6
The present embodiment is compared with embodiment 1, and difference is only that a kind of fresh-water fishes are different by the proportioning of enrofloxacin micropill with bag, and the proportioning of the present embodiment is as follows:
A kind of fresh-water fishes with bag by enrofloxacin micropill, by weight, the enrofloxacin by 8%, the microcrystalline Cellulose of 16%, 7% flour, the maize cob meal of 11%, corn starch, the hydroxypropyl emthylcellulose of 1%, the coatings of 25% of 32% form.Wherein, coatings by 13.5% the Pulvis Talci (particle diameter 1200 order) of acrylic resin IV, 1.5% and the ethanol of 85% form.
Embodiment 7
The present embodiment is compared with embodiment 1, and difference is only that a kind of fresh-water fishes are different by the proportioning of enrofloxacin micropill with bag, and the proportioning of the present embodiment is as follows:
A kind of fresh-water fishes with bag by enrofloxacin micropill, by weight, the enrofloxacin by 12%, the microcrystalline Cellulose of 14.2%, 10% flour, the maize cob meal of 20%, corn starch, the hydroxypropyl emthylcellulose of 0.8%, the coatings of 18% of 25% form.Wherein, coatings by 13.5% the Pulvis Talci (particle diameter 1200 order) of acrylic resin IV, 1.5% and the ethanol of 85% form.
Embodiments of the invention 1 gained micropill is carried out correlation test, specific as follows:
One, the stability in in-vitro simulated fresh water
1, method summary
Sample is joined in fresh water (pH6.8), under 20 DEG C of conditions, 4 hours are acted on disintegration time tester, standardize solution, filtration, the content of high effective liquid chromatography for measuring enrofloxacin, calculate the quality of the enrofloxacin of stripping in people's fresh water, thus calculate the percentage ratio that enrofloxacin discharges in fresh water.
2, reagent
Acetonitrile: chromatographically pure; Phosphoric acid: analytical pure; Enrofloxacin reference substance: purity >=99.8%; Enrofloxacin standard reserving solution: get enrofloxacin reference substance 2.5mg, accurately weighed, be placed in 50mL measuring bottle, add mobile phase and dissolve and be quantitatively diluted to scale, shake up.Store under 4 DEG C of conditions, storage life 3 months.
3, instrument
Disintegration time tester; Analytical balance: sensibility reciprocal is 0.0001g; High performance liquid chromatograph (being furnished with UV-detector).
4, the mensuration of enrofloxacin release rate in fresh water
Select the hanging basket of aperture 0.25mm screen cloth, hanging basket is hung on metal rack by the stainless steel shaft of upper end, immerse in the beaker of 1000ml, and regulate hanging basket position, when making it decline, screen cloth is apart from beaker bottom 25mm, in beaker, add the drinking water that temperature is 37 DEG C ± 1 DEG C, when making hanging basket increase, screen cloth is at 15mm place, underwater.Sample thief 2.0g, is accurate to 0.0002g, puts in the glass tubing of hanging basket respectively, setting-up time 4 hours, temperature 37 DEG C, starts disintegration tester reaction, after 4 hours, stops; Take out the solution in beaker, move in 1000mL volumetric flask, be diluted with water to scale, shake up, get in 5mL and triangular flask, add mobile phase 25mL ultrasonic dissolution, detect the content of enrofloxacin in solution.
5, the quality of enrofloxacin in solution is measured
(1) chromatographic condition
Chromatographic column: C
18post, long 250mm, internal diameter 4.6mm, granularity 5 μm; Column temperature: 30 DEG C;
Mobile phase: acetonitrile+0.025mol/L phosphoric acid solution (regulating pH value to 3.0 with triethylamine)=17+83(volume ratio);
Flow velocity: 0.5mL/min; Determined wavelength: 278nm; Sample size: 10 μ L.
(2) Specimen Determination
Get ultrasonic after filtrate, cross 0.45 μm of filter membrane, filtrate as sample solution, according to (1) chromatographic condition measure, separately get enrofloxacin standard reserving solution, be measured in the same method.Go out the quality of citric acid in filtrate by external standard method with calculated by peak area, thus calculate fresh-water fishes with wrapping the percentage ratio discharged in fresh water by enrofloxacin micropill.
Two, in-vitro simulated fresh-water fishes anterior intestine disintegration time mensuration
1, method summary
Joined by sample before appropriate in-vitro simulated fresh-water fishes in intestinal juice (hydrochloric acid solution of pH3.5), detect under 20 DEG C of conditions with disintegration time tester, fresh-water fishes bag must not be greater than 1 hour by the complete disintegration time of enrofloxacin micropill before fresh-water fishes in intestinal juice.
2. reagent
Dilute hydrochloric acid.
3, instrument
Disintegration time tester.
4, the preparation of in-vitro simulated front intestinal juice
Fetch water about 1000ml, drips dilute hydrochloric acid appropriate, regulates pH to be 3.5, to obtain final product.
5, detection method
Select the hanging basket of aperture 0.25mm screen cloth, hanging basket is hung on metal rack by the stainless steel shaft of upper end, immerse in the beaker of 1000ml, and regulate hanging basket position, when making it decline, screen cloth is apart from beaker bottom 25mm, in beaker, add the front intestinal juice that temperature is 37 DEG C ± 1 DEG C, when making hanging basket increase, screen cloth is at 15mm place, underwater.Sample thief 2.0g, puts in the glass tubing of hanging basket respectively, setting-up time 1 hour, temperature 37 DEG C, starts disintegration tester and measures, after 1 hour, fresh-water fishes with bag should all disintegrate be leached by screen cloth by enrofloxacin micropill, if any not leaching on a small quantity, but softened and can by the opinion that conforms with the regulations without hard-core person.
Three, result and analysis
Micropill of the present invention, in fresh water, process 4 hours, well-tended appearance does not leach, and release rate is 0.26%; And most disintegrate in about 50 minutes leaches in front intestinal juice, by screen cloth, have a small amount of not by screen cloth, but softening without hard-core.Therefore fresh-water fishes are with bag by enrofloxacin micropill, meet the requirements completely, namely substantially do not discharge in fresh water, major part discharges in the anterior intestine of fish, plays antibacterial action after absorption.Therefore be used for the treatment of fresh water fish bacterial to infect, it is high to waste little utilization rate, does not affect water body environment.
According to above-described embodiment, just the present invention can be realized well.What deserves to be explained is; under prerequisite based on above-mentioned design, for solving same technical problem, even if some making on the invention are without substantial change or polishing; the essence of the technical scheme adopted is still the same with the present invention, therefore it also should in protection scope of the present invention.
Claims (10)
1. fresh-water fishes with bag by an enrofloxacin micropill, it is characterized in that, by weight, described micropill be by the enrofloxacin of 5% ~ 20%, 60% ~ 75% adjuvant and 10% ~ 25% coatings be prepared from.
2. a kind of fresh-water fishes according to claim 1 are with bag by enrofloxacin micropill, and it is characterized in that, described adjuvant is made up of microcrystalline Cellulose, flour, maize cob meal, corn starch, hydroxypropyl emthylcellulose.
3. a kind of fresh-water fishes according to claim 2 are with bag by enrofloxacin micropill, and it is characterized in that, described coatings is made up of acrylic resin IV, Pulvis Talci and ethanol.
4. want a kind of fresh-water fishes described in 2 or 3 with wrapping by enrofloxacin micropill according to right, it is characterized in that, by weight, described micropill by 5% enrofloxacin, the microcrystalline Cellulose of 20%, flour, the maize cob meal of 5%, corn starch, the hydroxypropyl emthylcellulose of 1%, the coatings of 20% of 39% of 10% form; Wherein, micropill particle diameter is 20 ~ 60 orders;
Or described micropill is made up of enrofloxacin, the microcrystalline Cellulose of 12.4%, flour, the maize cob meal of 15%, corn starch, the hydroxypropyl emthylcellulose of 0.6%, the coatings of 25% of 25% of 12% of 10%; Wherein, micropill particle diameter is 20 ~ 60 orders.
5. a kind of fresh-water fishes according to claim 3 are with bag by enrofloxacin micropill, it is characterized in that, by weight, described coatings is made up of the Pulvis Talci of acrylic resin IV, 1.5%, the ethanol of 85% of 13.5%.
6. a kind of fresh-water fishes according to claim 5 are with bag by enrofloxacin micropill, and it is characterized in that, described talcous particle diameter is 1200 orders.
7. fresh-water fishes are with bag by a preparation method for enrofloxacin micropill, it is characterized in that, comprise the following steps:
Prepare ball core:
(1) by enrofloxacin, microcrystalline Cellulose, flour, maize cob meal, corn starch mix homogeneously, obtained mixture;
(2) compound concentration is the hydroxypropyl emthylcellulose aqueous solution of 1.5%, joins obtained soft material in mixture as binding agent;
(3) soft material is made strip-shaped materials, and by shearing and round as a ball obtained ball core;
(4) ball core fluid bed dryer is dried, for subsequent use;
Prepare coating solution:
By acrylic resin IV, ethanol, be stirred to after dissolving completely, add Pulvis Talci, mix homogeneously, fully stir and make to be uniformly dispersed, obtain coating solution;
Prepare micropill:
The ball core of drying is joined in fluidized-bed coating machine, sprays into coating solution, sprayed until it, coating solution just becomes coatings after drying, obtains micropill.
8. a kind of fresh-water fishes according to claim 7 are with bag by the preparation method of enrofloxacin micropill, it is characterized in that, in described step (3) soft material by rotating speed be 40r/min, aperture is that the extruder of 1.2mm obtains strip-shaped materials; The spheronizator being 25Hz by blower fan frequency again carries out shearing and round as a ball obtained ball core, and now the rotating speed of this spheronizator is rotating speed 650r/min, duration 15s.
9. a kind of fresh-water fishes according to claim 8 are with wrapping by the preparation method of enrofloxacin micropill, it is characterized in that, in described step (4), ball core adopts the fluid bed dryer that inlet temperature is 70 DEG C, blower fan frequency is 30Hz to dry, and wherein trembles a bag time delay 6s.
10. a kind of fresh-water fishes according to claim 9 are with bag by the preparation method of enrofloxacin micropill, it is characterized in that, when spraying into coating solution in described step (6), keep ball core temperature at 33 ~ 37 DEG C.
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| 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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| CN105106164B (en) | 2017-12-12 |
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