CN114469866A - Preparation method of tilmicosin soluble powder - Google Patents
Preparation method of tilmicosin soluble powder Download PDFInfo
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- CN114469866A CN114469866A CN202011163108.4A CN202011163108A CN114469866A CN 114469866 A CN114469866 A CN 114469866A CN 202011163108 A CN202011163108 A CN 202011163108A CN 114469866 A CN114469866 A CN 114469866A
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- tilmicosin
- soluble powder
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- JTSDBFGMPLKDCD-XVFHVFLVSA-N tilmicosin Chemical compound O([C@@H]1[C@@H](C)[C@H](O)CC(=O)O[C@@H]([C@H](/C=C(\C)/C=C/C(=O)[C@H](C)C[C@@H]1CCN1C[C@H](C)C[C@H](C)C1)CO[C@H]1[C@@H]([C@H](OC)[C@H](O)[C@@H](C)O1)OC)CC)[C@@H]1O[C@H](C)[C@@H](O)[C@H](N(C)C)[C@H]1O JTSDBFGMPLKDCD-XVFHVFLVSA-N 0.000 title claims abstract description 74
- 229960000223 tilmicosin Drugs 0.000 title claims abstract description 74
- 239000000843 powder Substances 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000003756 stirring Methods 0.000 claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229920000858 Cyclodextrin Polymers 0.000 claims abstract description 10
- 239000001116 FEMA 4028 Substances 0.000 claims abstract description 10
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 claims abstract description 10
- 235000011175 beta-cyclodextrine Nutrition 0.000 claims abstract description 10
- 229960004853 betadex Drugs 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 229920002472 Starch Polymers 0.000 claims abstract description 8
- 235000003599 food sweetener Nutrition 0.000 claims abstract description 8
- 239000008213 purified water Substances 0.000 claims abstract description 8
- 235000019698 starch Nutrition 0.000 claims abstract description 8
- 239000008107 starch Substances 0.000 claims abstract description 8
- 239000003765 sweetening agent Substances 0.000 claims abstract description 8
- 238000001291 vacuum drying Methods 0.000 claims abstract description 8
- 238000007873 sieving Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 7
- 239000012295 chemical reaction liquid Substances 0.000 claims description 6
- 229920003171 Poly (ethylene oxide) Polymers 0.000 abstract description 8
- 239000002244 precipitate Substances 0.000 abstract description 7
- 229920001030 Polyethylene Glycol 4000 Polymers 0.000 abstract description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 abstract description 3
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 9
- 239000000243 solution Substances 0.000 description 8
- 241001465754 Metazoa Species 0.000 description 7
- 239000003814 drug Substances 0.000 description 7
- 229920001223 polyethylene glycol Polymers 0.000 description 6
- 229940079593 drug Drugs 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 244000144972 livestock Species 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 241000283690 Bos taurus Species 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- 208000022362 bacterial infectious disease Diseases 0.000 description 2
- 235000019658 bitter taste Nutrition 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 235000019629 palatability Nutrition 0.000 description 2
- 244000144977 poultry Species 0.000 description 2
- 235000013594 poultry meat Nutrition 0.000 description 2
- 239000000273 veterinary drug Substances 0.000 description 2
- 208000035143 Bacterial infection Diseases 0.000 description 1
- 241000283707 Capra Species 0.000 description 1
- 208000035473 Communicable disease Diseases 0.000 description 1
- 241000192125 Firmicutes Species 0.000 description 1
- 241000287828 Gallus gallus Species 0.000 description 1
- 241001430197 Mollicutes Species 0.000 description 1
- 241001494479 Pecora Species 0.000 description 1
- 206010057190 Respiratory tract infections Diseases 0.000 description 1
- 241000589970 Spirochaetales Species 0.000 description 1
- 241000282887 Suidae Species 0.000 description 1
- 229930194936 Tylosin Natural products 0.000 description 1
- 239000004182 Tylosin Substances 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 235000013330 chicken meat Nutrition 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 230000037406 food intake Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 239000003120 macrolide antibiotic agent Substances 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 210000004400 mucous membrane Anatomy 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229940057838 polyethylene glycol 4000 Drugs 0.000 description 1
- 238000005063 solubilization Methods 0.000 description 1
- 230000007928 solubilization Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- WBPYTXDJUQJLPQ-VMXQISHHSA-N tylosin Chemical compound O([C@@H]1[C@@H](C)O[C@H]([C@@H]([C@H]1N(C)C)O)O[C@@H]1[C@@H](C)[C@H](O)CC(=O)O[C@@H]([C@H](/C=C(\C)/C=C/C(=O)[C@H](C)C[C@@H]1CC=O)CO[C@H]1[C@@H]([C@H](OC)[C@H](O)[C@@H](C)O1)OC)CC)[C@H]1C[C@@](C)(O)[C@@H](O)[C@H](C)O1 WBPYTXDJUQJLPQ-VMXQISHHSA-N 0.000 description 1
- 229960004059 tylosin Drugs 0.000 description 1
- 235000019375 tylosin Nutrition 0.000 description 1
Classifications
-
- 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
- A61K9/146—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 organic macromolecular compounds
-
- 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
- A61K31/70—Carbohydrates; Sugars; Derivatives thereof
- A61K31/7042—Compounds having saccharide radicals and heterocyclic rings
- A61K31/7052—Compounds having saccharide radicals and heterocyclic rings having nitrogen as a ring hetero atom, e.g. nucleosides, nucleotides
- A61K31/706—Compounds having saccharide radicals and heterocyclic rings having nitrogen as a ring hetero atom, e.g. nucleosides, nucleotides containing six-membered rings with nitrogen as a ring hetero atom
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/50—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates
- A61K47/69—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates the conjugate being characterised by physical or galenical forms, e.g. emulsion, particle, inclusion complex, stent or kit
- A61K47/6949—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates the conjugate being characterised by physical or galenical forms, e.g. emulsion, particle, inclusion complex, stent or kit inclusion complexes, e.g. clathrates, cavitates or fullerenes
- A61K47/6951—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates the conjugate being characterised by physical or galenical forms, e.g. emulsion, particle, inclusion complex, stent or kit inclusion complexes, e.g. clathrates, cavitates or fullerenes using cyclodextrin
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P31/00—Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
- A61P31/04—Antibacterial agents
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Public Health (AREA)
- General Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Pharmacology & Pharmacy (AREA)
- Veterinary Medicine (AREA)
- Chemical & Material Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Engineering & Computer Science (AREA)
- Epidemiology (AREA)
- Communicable Diseases (AREA)
- Oncology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Organic Chemistry (AREA)
- Molecular Biology (AREA)
- Medicinal Preparation (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
A preparation method of tilmicosin soluble powder comprises the following steps: adding purified water into a reaction kettle, stirring at 50-70 ℃, adding beta-cyclodextrin, PEO and PEG4000 into the reaction kettle, and dissolving; then, 37.5g of tilmicosin raw powder is slowly added into the reaction solution and stirred to be completely dissolved; after the reaction solution is clarified, continuing stirring for 1h, rapidly cooling to separate out the content in the reaction solution; vacuum drying, physically compacting and crushing the content precipitate to obtain a tilmicosin soluble powder intermediate; sieving the tilmicosin soluble powder intermediate, adding a proper amount of sweetener and soluble starch into a mixer, and uniformly mixing to obtain the tilmicosin soluble powder intermediate; the invention is suitable for clinical application, accords with the relevant regulations of pharmacopoeia, and is suitable for industrial large-scale production, so the invention has very wide application prospect and good practical value.
Description
Technical Field
The invention relates to the technical field of veterinary drug preparations, in particular to a preparation method of tilmicosin soluble powder (37.5%).
Background
Tilmicosin is a semisynthetic macrolide antibiotic special for livestock, is generally prepared by tylosin semisynthesis, has a wide antibacterial spectrum, and has an inhibiting effect on all gram-positive bacteria, partial gram-negative bacteria, mycoplasmas, spirochetes and the like. The traditional Chinese medicine composition is mainly used for treating infectious diseases of animals such as cows, goats, sheep, cows, pigs and chickens caused by sensitive bacteria, and especially has more obvious effect of treating respiratory tract infection of livestock and poultry. Tilmicosin is extremely insoluble in water, has strong bitter taste and low bioavailability. The main formulations of tilmicosin on the market are premix, soluble powder and injection, the tilmicosin injection requires other animals except cattle to be used with caution, the stress reaction of the injected animals is large, and the animals are easy to die. The tilmicosin solution has the problems of inconvenient transportation, difficult storage and the like. The tilmicosin premix is mainly prepared by mixing medicines for administration, is not easy to be uniformly mixed with feed, causes inaccurate dosage and also causes medicine waste. Research shows that after the tilmicosin soluble powder and the tilmicosin solution are orally taken in single dose, the tilmicosin is quickly absorbed and slowly faded, and the tilmicosin soluble powder and the tilmicosin solution can be mutually replaced in treatment according to important judgment indexes of bioequivalence. Soluble powder existing in the market at present seriously influences the ingestion of livestock due to heavy bitter taste, and cannot be used according to the recommended dose.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a preparation method of tilmicosin soluble powder (37.5%), the soluble powder takes tilmicosin as a main drug, is easy to dissolve in water, has strong stability, is used for treating and preventing bacterial infectious diseases of livestock and poultry, has obvious curative effect and convenient administration, can accurately control the administration dosage according to the condition of the animal, can quickly and accurately prevent and treat the diseases, can avoid the waste of the drugs in the administration process, and has good palatability.
In order to realize the purpose, the invention is realized by the following technical scheme:
the invention relates to a method for preparing tilmicosin soluble powder (37.5%), which comprises the following steps:
a. putting 500mL of purified water into a reaction kettle, stirring at 50-70 ℃, adding 35-40 g of beta-cyclodextrin, PEO2g and PEG 40002-6 g into the reaction kettle, and dissolving;
b. slowly adding 37.5g of tilmicosin raw powder into the reaction liquid in the step a, and stirring until the tilmicosin raw powder is completely dissolved;
c. after the reaction liquid in the step b is completely clarified, continuously stirring for 1h, rapidly cooling to separate out the content in the reaction liquid;
d. vacuum drying, physically compacting and crushing the content precipitate to obtain a tilmicosin soluble powder intermediate;
e. and (3) sieving the tilmicosin soluble powder intermediate, adding 2g of sweetening agent and a proper amount of soluble starch to 100g of mixer, and uniformly mixing to obtain the tilmicosin soluble powder preparation.
Preferably, the cooling speed in the step c is 10-20 ℃/min, and the temperature is reduced to 0-5 ℃.
Preferably, the stirring speed in the step a is 300-600 r/min.
The preparation method has the advantages of simple process, cheap and easily-obtained raw materials, reduction in the use of organic solvents, and stable performance and high solubility of the prepared tilmicosin soluble powder. The PEG4000 mainly plays roles of solubilization and emulsification, the PEG4000 has good intermiscibility and water solubility, does not participate in the metabolism of animals, does not form any stimulation to skin, mucous membrane, eyes and the like, and is safe to use. When tilmicosin, polyethylene glycol 4000 and beta-cyclodextrin are mixed and stirred for reaction, the solubility of tilmicosin is fully improved due to the strong dispersion effect of PEO, so that the soluble powder can be quickly dissolved. Meanwhile, the beta-cyclodextrin has the dissolution promotion effect of physical inclusion in the stirring process, the solubility of the tilmicosin in water can be greatly improved under the double effects, and the PEO has strong oxidation resistance and moisture resistance, can prevent the tilmicosin soluble powder from being oxidized and deteriorated, and is convenient to store.
The invention has the advantages that: by adopting the preparation method of the tilmicosin soluble powder, the raw materials are all commercially available raw materials, the raw materials are cheap and easy to obtain, the compound preparation has stable performance and good solubility, on one hand, the soluble powder solves the problems of poor stability and difficult water solubility of tilmicosin raw material medicines, on the other hand, the soluble powder is convenient to administer, the administration dosage can be accurately controlled according to the condition of the livestock, the sensitive bacterial infection of the animals can be quickly, conveniently and accurately prevented and treated, the waste of the medicines in the administration process can be avoided, and the palatability is improved. Is suitable for clinical application, accords with the relevant regulations of pharmacopoeia, and is suitable for industrial large-scale production, so the application prospect is very wide, and the practical value is good.
Detailed Description
The present invention is further illustrated by the following examples, but the present invention is not limited to the following examples.
Example 1
The preparation method of the tilmicosin soluble powder (37.5%) of the embodiment comprises the following steps: 500mL of purified water was put into a reaction vessel, and 30g of beta-cyclodextrin, 2g of polyethylene oxide and PEG 40002 g were added to the mixture at 55 ℃ and 300r/min with stirring to dissolve the mixture. And slowly adding 37.5g of tilmicosin raw powder into the reaction solution, stirring until the tilmicosin raw powder is completely dissolved, continuing stirring for 1h, and rapidly cooling at 15 ℃/min until the content is separated out at 0 ℃. And (3) physically compacting the precipitate after vacuum drying, crushing to obtain a tilmicosin soluble powder intermediate, mixing the tilmicosin soluble powder intermediate with 2g of a sweetening agent and 100g of soluble starch, and uniformly mixing to obtain the tilmicosin soluble powder.
Example 2
The preparation method of the tilmicosin soluble powder (37.5%) of the embodiment comprises the following steps: 500mL of purified water was put into a reaction vessel, and 40g of β -cyclodextrin, 2g of polyethylene oxide and PEG 40004 g were added to the reaction vessel at 50 ℃ under stirring at a speed of 400r/min to dissolve the mixture. And slowly adding 37.5g of tilmicosin raw powder into the reaction solution, stirring until the tilmicosin raw powder is completely dissolved, continuing stirring for 1h, and rapidly cooling at the speed of 10 ℃/min until the content is separated out at the temperature of 0 ℃. And (3) physically compacting the precipitate after vacuum drying, crushing to obtain a tilmicosin soluble powder intermediate, and uniformly mixing the tilmicosin soluble powder intermediate, 2g of a sweetening agent and soluble starch to prepare 37.5% tilmicosin soluble powder.
Example 3
The preparation method of the tilmicosin soluble powder (37.5%) of the embodiment comprises the following steps: 500mL of purified water was put into a reaction vessel, and 37.5g of beta-cyclodextrin, 2g of polyethylene oxide and PEG 40004 g were added to the mixture at 50 ℃ at a rate of 600r/min with stirring to dissolve the mixture. And slowly adding 37.5g of tilmicosin raw powder into the reaction solution, stirring until the tilmicosin raw powder is completely dissolved, continuing stirring for 1h, and rapidly cooling at 15 ℃/min until the content is separated out at 0 ℃. And (3) after vacuum drying, physically compacting the precipitate, crushing to obtain a tilmicosin soluble powder intermediate, and uniformly mixing the tilmicosin soluble powder intermediate with 2g of a sweetening agent and soluble starch to prepare 37.5% tilmicosin soluble powder.
Example 4
The preparation method of the tilmicosin soluble powder (37.5%) of the embodiment comprises the following steps: 500mL of purified water was put into a reaction vessel, and 35g of beta-cyclodextrin, 2g of polyethylene oxide and PEG 40006 g were added to the reaction vessel at 60 ℃ at a rotation speed of 600r/min to dissolve the mixture. And slowly adding 37.5g of tilmicosin raw powder into the reaction solution, stirring until the tilmicosin raw powder is completely dissolved, continuing stirring for 1h, and rapidly cooling at the speed of 20 ℃/min to 5 ℃ to separate out contents. And (3) physically compacting the precipitate after vacuum drying, crushing to obtain a tilmicosin soluble powder intermediate, and uniformly mixing the tilmicosin soluble powder intermediate, 2g of a sweetening agent and soluble starch to prepare 37.5% tilmicosin soluble powder.
Example 5
The preparation method of the tilmicosin soluble powder (37.5%) of the embodiment comprises the following steps: 500mL of purified water was put into a reaction vessel, and 35g of beta-cyclodextrin, 2g of polyethylene oxide and PEG 40006 g were added to the reaction vessel at 70 ℃ and 600r/min with stirring to dissolve the mixture. And slowly adding 37.5g of tilmicosin raw powder into the reaction solution, stirring until the tilmicosin raw powder is completely dissolved, continuing stirring for 1h, and rapidly cooling at the speed of 20 ℃/min to 5 ℃ to separate out contents. And (3) physically compacting the precipitate after vacuum drying, crushing to obtain a tilmicosin soluble powder intermediate, and uniformly mixing the tilmicosin soluble powder intermediate, 2g of a sweetening agent and soluble starch to prepare 37.5% tilmicosin soluble powder.
The tilmicosin soluble powder prepared in the embodiments 1 to 5 of the invention is detected according to the specified content, and the specific results are shown in the following table:
the results in the table show that all indexes of the tilmicosin soluble powder prepared by the invention meet the requirements of the national veterinary drug code.
Claims (3)
1. A preparation method of tilmicosin soluble powder is characterized by comprising the following steps:
a. putting 500mL of purified water into a reaction kettle, stirring at 50-70 ℃, adding 35-40 g of beta-cyclodextrin, PEO2g and PEG 40002-6 g into the reaction kettle, and dissolving;
b. slowly adding 37.5g of tilmicosin raw powder into the reaction liquid in the step a, and stirring until the tilmicosin raw powder is completely dissolved;
c. after the reaction liquid in the step b is completely clarified, continuously stirring for 1h, rapidly cooling to separate out the content in the reaction liquid;
d. vacuum drying, physically compacting and crushing the content educt to obtain a tilmicosin soluble powder intermediate;
e. and (3) sieving the tilmicosin soluble powder intermediate, adding 2g of sweetening agent and a proper amount of soluble starch to 100g of mixer, and uniformly mixing to obtain the tilmicosin soluble powder preparation.
2. The method for preparing tilmicosin soluble powder according to claim 1, which is characterized in that: and c, cooling in the step c at a speed of 10-20 ℃/min to 0-5 ℃.
3. The method for preparing tilmicosin soluble powder according to claim 1, which is characterized in that: the stirring speed in the step a is 300-600 r/min.
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CN202011163108.4A CN114469866A (en) | 2020-10-27 | 2020-10-27 | Preparation method of tilmicosin soluble powder |
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Application publication date: 20220513 |