CN108113966B - Preparation method of engshi powder for removing bitter taste - Google Patents
Preparation method of engshi powder for removing bitter taste Download PDFInfo
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- CN108113966B CN108113966B CN201710733038.3A CN201710733038A CN108113966B CN 108113966 B CN108113966 B CN 108113966B CN 201710733038 A CN201710733038 A CN 201710733038A CN 108113966 B CN108113966 B CN 108113966B
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- enrofloxacin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
- A61K9/141—Intimate drug-carrier mixtures characterised by the carrier, e.g. ordered mixtures, adsorbates, solid solutions, eutectica, co-dried, co-solubilised, co-kneaded, co-milled, co-ground products, co-precipitates, co-evaporates, co-extrudates, co-melts; Drug nanoparticles with adsorbed surface modifiers
- A61K9/143—Intimate drug-carrier mixtures characterised by the carrier, e.g. ordered mixtures, adsorbates, solid solutions, eutectica, co-dried, co-solubilised, co-kneaded, co-milled, co-ground products, co-precipitates, co-evaporates, co-extrudates, co-melts; Drug nanoparticles with adsorbed surface modifiers with inorganic compounds
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/33—Heterocyclic compounds
- A61K31/395—Heterocyclic compounds having nitrogen as a ring hetero atom, e.g. guanethidine or rifamycins
- A61K31/495—Heterocyclic compounds having nitrogen as a ring hetero atom, e.g. guanethidine or rifamycins having six-membered rings with two or more nitrogen atoms as the only ring heteroatoms, e.g. piperazine or tetrazines
- A61K31/496—Non-condensed piperazines containing further heterocyclic rings, e.g. rifampin, thiothixene or sparfloxacin
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Engineering & Computer Science (AREA)
- Medicinal Chemistry (AREA)
- Pharmacology & Pharmacy (AREA)
- Epidemiology (AREA)
- Veterinary Medicine (AREA)
- Bioinformatics & Cheminformatics (AREA)
- General Health & Medical Sciences (AREA)
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- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
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Abstract
The invention provides a preparation method of an enrichment powder for removing bitterness, which comprises the following steps: preparing montmorillonite powder and enrofloxacin hydrochloride into suspension with purified water, stirring, standing, taking supernatant for detecting enrofloxacin content, filtering water when the content is less than or equal to 0.02 percent to obtain filter cake, and drying the filter cake to obtain the enrofloxacin montmorillonite powder; the mass parts of the montmorillonite powder and the enrofloxacin hydrochloride are as follows: 3-5:1. After the poultry take the product prepared by the method, the welfare of the animals is greatly improved compared with the current hard marketing.
Description
Technical Field
The invention relates to the field of preparation of enrofloxacin and montmorillonite powder compositions, and in particular relates to a preparation method of enrofloxacin powder for removing bitter taste.
Background
The enrofloxacin veterinary drug preparations comprise enrofloxacin injection, oral solution, soluble powder, tablets and the like, and are widely used for pigs, chickens, ducks, fur animals, dogs, cats and aquatic animals. The oral preparation is mostly used for chicken, and is less applied to pigs due to bitter taste. In order to improve the palatability of enrofloxacin and improve the compliance of pigs in taking medicine, people adopt an embedding method to prepare microcapsules and suspension by using a hydrophobic material; some of the results are too high in cost, and some of the results cannot completely solve the bitter taste of enrofloxacin. Therefore, the process technology is simple, auxiliary materials are easy to obtain, and the preparation cost is low, so that the bitter-free enrofloxacin is particularly important.
Disclosure of Invention
The invention provides a preparation method of an enrichments powder with excellent performance for removing bitterness, aiming at the problem that the bitterness of enrichments powder cannot be removed in the existing method.
A preparation method of an Enshi powder for removing bitterness comprises the following steps:
preparing montmorillonite powder and enrofloxacin hydrochloride into suspension with purified water, stirring, standing, taking supernatant for detecting enrofloxacin content, filtering water when the content is less than or equal to 0.02 percent to obtain filter cake, washing the filter cake with water, and drying to obtain the enrofloxacin montmorillonite powder; the mass parts of the montmorillonite powder and the enrofloxacin hydrochloride are as follows: 3-5:1.
Preferably, the stirring device is a stirrer; the time is 20 to 60 minutes; the strength is 800 and 1200 turns per minute.
Preferably, the standing time is 30-80 minutes, and the standing temperature is room temperature.
Preferably, the equipment adopted for filtering is a three-foot centrifuge, and the filter material is canvas; filtering for 40-60 min; the rotation speed is about 1500-.
Preferably, the drying temperature is 70-80 ℃, and the drying time is 2-5 hours.
Preferably, the mass part ratio of the montmorillonite powder to the enrofloxacin hydrochloride is as follows: 4:1.
Preferably, the water washing refers to washing the filter cake with purified water, and the washing time is 30-60 minutes.
Compared with the prior art, the preparation method of the enrofloxacin powder for removing bitter taste can improve the bitter taste characteristic of the special quinolone medicine enrofloxacin for animals, so that the enrofloxacin is orally taken to sensitive animals with taste sense such as pigs, domestic pets, aquatic animals and the like, and the applicable animal spectrum of the enrofloxacin is expanded and prolonged. The adsorption rates of montmorillonite powder, ofloxacin, norfloxacin, lomefloxacin, ciprofloxacin and pefloxacin mesylate in artificial gastric juice are all more than 98-99% in clinical practice. Based on the above, the quinolone medicines are not recommended to be taken together with the montmorillonite powder, so that the incompatibility is avoided, and the antibacterial effect of the quinolone is not influenced. The stirring process brings enrofloxacin and montmorillonite crystals into full collision contact, and creates necessary and sufficient conditions for physical adsorption and chemical adsorption of montmorillonite.
Detailed Description
In order to better illustrate the present invention, the technical solutions in the embodiments of the present invention are clearly and completely described below with reference to the embodiments of the present invention.
Example 1
A preparation method of an Enshi powder for removing bitterness comprises the following steps:
take the production of 100 kg of 20% enrofloxacin montmorillonite powder as an example.
Prescription: enrofloxacin hydrochloride 20 kg
Montmorillonite powder 80 kg
160 kg of purified water.
The method comprises the following steps: putting 160 kg of purified water into a solution preparation tank with a stirrer, starting the stirrer, regulating the speed to 1200 revolutions per minute, slowly adding 80 kg of montmorillonite powder into the solution preparation tank to prepare montmorillonite suspension, slowly adding enrofloxacin hydrochloride under the stirring of the stirrer, and continuously stirring for 45 minutes after the addition, wherein the stirring strength is 800 revolutions per minute; and stopping stirring, standing for 60 minutes at room temperature, taking the supernatant for detecting the enrofloxacin content, and determining the content of the enrofloxacin solution by the detection method according to the content of the enrofloxacin solution in the 'Chinese veterinary pharmacopoeia' of 2015 edition. When the content is less than or equal to 0.02 percent; filtering water by using a three-foot type centrifuge, wherein the filtering time is 40 minutes, and the rotating speed is 2000 revolutions per minute; and the filter cake is rinsed with 50 kg of purified water for 30 minutes to further remove a very small amount of free enrofloxacin. And drying the filter cake at 70 ℃ for 2 hours to obtain the 20 percent enrofloxacin montmorillonite powder (mass percentage).
Example 2
A preparation method of an Enshi powder for removing bitterness comprises the following steps:
take the production of 100 kg of 25% enrofloxacin montmorillonite powder as an example.
Prescription: enrofloxacin hydrochloride 25 kg
Montmorillonite powder 75 kg
160 kg of purified water.
The method comprises the following steps: putting 160 kg of purified water into a solution preparation tank with a stirrer, starting the stirrer, regulating the speed to 1000 revolutions per minute, slowly adding 75 kg of montmorillonite powder into the solution preparation tank to prepare montmorillonite suspension, slowly adding enrofloxacin hydrochloride under the stirring of the stirrer, and continuously stirring for 60 minutes after the addition, wherein the stirring strength is 1000 revolutions per minute; and stopping stirring, standing at room temperature for 30 minutes, taking the supernatant for detecting the enrofloxacin content, and determining the content of the enrofloxacin solution according to the content of the enrofloxacin solution in the Chinese veterinary pharmacopoeia P268 of 2015 edition. When the content is less than or equal to 0.02 percent; filtering water by using a three-foot type centrifuge, wherein the filtering time is 60 minutes, and the rotating speed is 1500 revolutions per minute; and the filter cake is rinsed with 50 kg of purified water for 60 minutes, so that a very small amount of free enrofloxacin is further removed. And drying the filter cake at the temperature of 80 ℃ for 5 hours to obtain 25 percent enrofloxacin montmorillonite powder (mass percentage).
Example 3
A preparation method of an Enshi powder for removing bitterness comprises the following steps:
take the production of 100 kg of 23% enrofloxacin montmorillonite powder as an example.
Prescription: enrofloxacin hydrochloride 23 kg
Montmorillonite powder 77 kg
160 kg of purified water.
The method comprises the following steps: putting 160 kg of purified water into a solution preparation tank with a stirrer, starting the stirrer, regulating the speed to 1200 revolutions per minute, slowly adding 77 kg of montmorillonite powder into the solution preparation tank to prepare montmorillonite suspension, slowly adding enrofloxacin hydrochloride under the stirring of the stirrer, and continuously stirring for 20 minutes after the addition, wherein the stirring strength is 1200 revolutions per minute; and stopping stirring, standing at room temperature for 50 minutes, taking the supernatant for detecting the enrofloxacin content, and determining the content of the enrofloxacin solution according to the content of the enrofloxacin solution in the Chinese veterinary pharmacopoeia P268 of 2015 edition. When the content is less than or equal to 0.02 percent; filtering water by using a three-foot type centrifuge, wherein the filtering time is 50 minutes, and the rotating speed is 1800 revolutions per minute; and the filter cake is rinsed with 50 kg of purified water for 50 minutes, so that a very small amount of free enrofloxacin is further removed. And drying the filter cake at the temperature of 80 ℃ for 4 hours to obtain 23 percent enrofloxacin montmorillonite powder (mass percentage).
Example 4
A preparation method of an Enshi powder for removing bitterness comprises the following steps:
take the production of 100 kg of 18% enrofloxacin montmorillonite powder as an example.
Prescription: enrofloxacin hydrochloride 18 kg
Montmorillonite powder 82 kg
160 kg of purified water.
The method comprises the following steps: putting 160 kg of purified water into a solution preparation tank with a stirrer, starting the stirrer, regulating the speed to 1100 revolutions per minute, then slowly adding 82 kg of montmorillonite powder into the solution preparation tank to prepare montmorillonite suspension, slowly adding enrofloxacin hydrochloride under the stirring of the stirrer, and continuously stirring for 45 minutes after the addition, wherein the stirring strength is 1100 revolutions per minute; and stopping stirring, standing for 60 minutes at room temperature, taking the supernatant for detecting the enrofloxacin content, and determining the content of the enrofloxacin solution by the detection method according to the content of the enrofloxacin solution in the 'Chinese veterinary pharmacopoeia' of 2015 edition. When the content is less than or equal to 0.02 percent; filtering water by using a three-foot type centrifuge, wherein the filtering time is 55 minutes, and the rotating speed is 1600 revolutions per minute; and the filter cake is rinsed with 50 kg of purified water for 45 minutes to further remove a very small amount of free enrofloxacin. And drying the filter cake at the temperature of 80 ℃ for 4 hours to obtain the enrofloxacin montmorillonite powder (the mass percentage content) with the concentration of 18 percent.
Example 5
A preparation method of an Enshi powder for removing bitterness comprises the following steps:
take the production of 100 kg of 20% enrofloxacin montmorillonite powder as an example.
Prescription: enrofloxacin hydrochloride 20 kg
Montmorillonite powder 80 kg
160 kg of purified water.
The method comprises the following steps: putting 160 kg of purified water into a solution preparation tank with a stirrer, starting the stirrer, regulating the speed to 1000 revolutions per minute, slowly adding 80 kg of montmorillonite powder into the solution preparation tank to prepare montmorillonite suspension, slowly adding enrofloxacin hydrochloride under the stirring of the stirrer, and continuously stirring for 45 minutes after the addition, wherein the stirring strength is 1000 revolutions per minute; and stopping stirring, standing for 45 minutes at room temperature, taking the supernatant for detecting the enrofloxacin content, and determining the content of the enrofloxacin solution by the detection method according to the content of the enrofloxacin solution in the 'Chinese veterinary pharmacopoeia' of 2015 edition. When the content is less than or equal to 0.02 percent; filtering water by using a three-foot type centrifuge, wherein the filtering time is 55 minutes, and the rotating speed is 1800 revolutions per minute; and the filter cake is rinsed with 50 kg of purified water for 55 minutes to further remove a very small amount of free enrofloxacin. And drying the filter cake at 70 ℃ for 5 hours to obtain the 20 percent enrofloxacin montmorillonite powder (mass percentage).
The raw materials are preferably used in edible specifications and then in medicinal specifications. Through more than three years of clinical trials, the 20 percent enrofloxacin montmorillonite powder is used for treating white scour (colibacillosis) of piglets, 1 gram of the enrofloxacin montmorillonite powder is used for each suckling pig, is cooled to be white and boiled into paste, and is smeared on the tongue surface of the piglet for healing once. The biological method is used for trial eating of healthy fattening pigs, the content of the feed is 20%, the feed is used for 10 g per kg, the pigs have no feeling, and the feed intake time and the feed intake are not influenced. Free enrofloxacin molecules could not be obtained by water extraction using a 2W ultrasonic oscillator.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention.
Claims (1)
1. A preparation method of an Enshi powder for removing bitterness is characterized by comprising the following steps:
preparing montmorillonite powder and enrofloxacin hydrochloride into suspension with purified water, stirring, standing, taking supernatant for detecting enrofloxacin content, filtering water when the content is less than or equal to 0.02 percent to obtain filter cake, washing the filter cake with water, and drying to obtain the enrofloxacin montmorillonite powder;
the stirring equipment is a stirrer; the time is 20 to 60 minutes; the strength is 800-;
the standing time is 30-80 minutes, and the standing temperature is room temperature;
the filtering device is a three-leg centrifuge, and the filter material is canvas; filtering for 40-60 min; the rotation speed is about 1500-;
the drying temperature is 70-80 ℃, and the drying time is 2-5 hours;
the mass parts of the montmorillonite powder and the enrofloxacin hydrochloride are as follows: 4: 1;
the water washing refers to washing the filter cake by using purified water, and the washing time is 30-60 minutes.
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| CN201710733038.3A CN108113966B (en) | 2017-08-24 | 2017-08-24 | Preparation method of engshi powder for removing bitter taste |
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| CN108113966B true CN108113966B (en) | 2021-03-16 |
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| CN110559367A (en) * | 2019-08-28 | 2019-12-13 | 内蒙古新开元动物药业发展有限公司 | Medicinal preparation for treating livestock diarrhea |
| CN113717101A (en) * | 2021-08-30 | 2021-11-30 | 深圳市博林达科技有限公司 | Purification process for enrofloxacin |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105726477A (en) * | 2016-03-01 | 2016-07-06 | 山东司邦得制药有限公司 | Pediatric domperidone suspension and preparation method thereof |
| CN106727333A (en) * | 2016-11-24 | 2017-05-31 | 山东滨州智源生物科技有限公司 | A kind of Enrofloxacin water solube powder and preparation method thereof |
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| CN1475556A (en) * | 2002-08-17 | 2004-02-18 | 陈宏基 | Gingko wine and its preparation method |
| SG10201602047QA (en) * | 2009-04-24 | 2016-05-30 | Iceutica Pty Ltd | Method for the production of commercial nanoparticle and microparticle powders |
| CN106539822A (en) * | 2016-12-29 | 2017-03-29 | 重庆金邦动物药业有限公司 | Florfenicol powder and preparation method thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105726477A (en) * | 2016-03-01 | 2016-07-06 | 山东司邦得制药有限公司 | Pediatric domperidone suspension and preparation method thereof |
| CN106727333A (en) * | 2016-11-24 | 2017-05-31 | 山东滨州智源生物科技有限公司 | A kind of Enrofloxacin water solube powder and preparation method thereof |
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