CN107441050A - A kind of preparation method of valnemulin hydrochloride premix - Google Patents

A kind of preparation method of valnemulin hydrochloride premix Download PDF

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Publication number
CN107441050A
CN107441050A CN201710754753.5A CN201710754753A CN107441050A CN 107441050 A CN107441050 A CN 107441050A CN 201710754753 A CN201710754753 A CN 201710754753A CN 107441050 A CN107441050 A CN 107441050A
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China
Prior art keywords
valnemulin hydrochloride
preparation
valnemulin
purification
binder liq
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CN201710754753.5A
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Inventor
陈清平
汪敦辉
胡燕琼
王锌睿
郭熙昌
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Hubei Longxiang Pharmaceutical Tech Co Ltd
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Hubei Longxiang Pharmaceutical Tech Co Ltd
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Priority to CN201710754753.5A priority Critical patent/CN107441050A/en
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/14Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
    • A61K9/16Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
    • A61K9/1605Excipients; Inactive ingredients
    • A61K9/1629Organic macromolecular compounds
    • A61K9/1652Polysaccharides, e.g. alginate, cellulose derivatives; Cyclodextrin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K31/00Medicinal preparations containing organic active ingredients
    • A61K31/21Esters, e.g. nitroglycerine, selenocyanates
    • A61K31/215Esters, e.g. nitroglycerine, selenocyanates of carboxylic acids
    • A61K31/22Esters, e.g. nitroglycerine, selenocyanates of carboxylic acids of acyclic acids, e.g. pravastatin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/14Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
    • A61K9/16Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
    • A61K9/1605Excipients; Inactive ingredients
    • A61K9/1617Organic compounds, e.g. phospholipids, fats
    • A61K9/1623Sugars or sugar alcohols, e.g. lactose; Derivatives thereof; Homeopathic globules
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/14Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
    • A61K9/16Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
    • A61K9/1605Excipients; Inactive ingredients
    • A61K9/1629Organic macromolecular compounds
    • A61K9/1635Organic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polyvinyl pyrrolidone, poly(meth)acrylates

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  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Bioinformatics & Cheminformatics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Chemical & Material Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Epidemiology (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Molecular Biology (AREA)
  • Biophysics (AREA)
  • Emergency Medicine (AREA)
  • Medicinal Preparation (AREA)
  • Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)

Abstract

The invention provides a kind of preparation method of valnemulin hydrochloride premix, comprise the following steps:(1), the preparation of binder liq:In the valnemulin hydrochloride bulk drug of synthesis, the purification containing valnemulin hydrochloride is taken, dispersant and adhesive are added in purification, being sufficiently stirred makes both be dissolved in purification, that is, binder liq is made;(2), pelletize:Diluent is thrown into fluid bed, logical hot blast makes fluidized state, then sprayed into after binder liq is atomized in fluid bed, the percentage that diluent accounts for raw material gross weight is respectively 10~84%, continue heating more than 30min after having sprayed under the conditions of less than 45 DEG C, then room temperature is naturally cooled to, that is, obtains granular valnemulin hydrochloride premix.The present invention reduces the drying of valnemulin hydrochloride and crushing, has the advantages that cost is low, reduces excitant of the valnemulin hydrochloride to operating personnel.

Description

A kind of preparation method of valnemulin hydrochloride premix
Technical field
The invention provides a kind of preparation side of animal specific pleuromulins antibiotic valnemulin hydrochloride premix Method, belong to veterinary antibiotic formulation art.
Background technology
Valnemulin hydrochloride belongs to pleuromulins semisynthetic antibiotics of new generation, belongs to two terpenes, with Tiamulin category Same class medicine, it is animal specific antibiotic.
Valnemulin hydrochloride is to utilize Pleuromutilin by BernerH of Sandoz companies etc. as original first in 1984 Material synthesis.Thereafter, pre-mixing agent is made by Switzerland Norvatis companies, in 1999 with trade nameListed in Europe, Valnemulin hydrochloride category pleuromulins semisynthetic antibiotics, ratify to be used to prevent and treat by swine dysentery by European Union within 1999 Swine dysentery and the porcine enzootic pneumonia as caused by mycoplasma pneumoniae infection caused by Brachyspira infection, it is first all Europe The medicine pre-mixing agent of approval, China has valnemulin hydrochloride raw material at present and its preparation lists, and exploitation this product is more beneficial for The preventing and treating of livestock and poultry infectious diseases.
Valnemulin hydrochloride is used to prevent swine dysentery, region pneumonia, hog middle conveyor screw mainly as feed preblending agent Sick (colitis), pig proliferative enteropathy (enteritis) etc..With the characteristics of off-drug period is short, residual is small, toxicity is low.Pre-mixing agent is livestock and poultry The main formulation being administered orally, compared with injection, convenient drug administration, save aquaculture cost.Valnemulin hydrochloride salt bulk drug has Draw moist, powder excitant it is strong, to photo-labile, the deficiencies of easily being decomposed with contacts such as feeds.Therefore, valnemulin hydrochloride premixes Agent preparation process must cover raw material excitant by preparation process, improve the stability of medicine, the purpose taken in favor of animal.
The content of the invention
It is an object of the invention to make up directly to prepare valnemulin hydrochloride premix tool with valnemulin hydrochloride bulk drug The deficiencies of having that cost is high, excitant is strong etc., there is provided a kind of directly with the purification preparation of synthetic hydrochloric acid valnemulin bulk drug The method of pre-mixing agent, reduce the drying and crushing of valnemulin hydrochloride, have cost it is low, reduce valnemulin hydrochloride to operation The advantages that excitant of personnel.
Technical scheme is used by realizing above-mentioned purpose of the present invention:
A kind of preparation method of valnemulin hydrochloride premix, comprises the following steps:
(1), the preparation of binder liq:
In the valnemulin hydrochloride bulk drug of synthesis, the purification containing valnemulin hydrochloride is taken, in purification Middle addition dispersant and adhesive, being sufficiently stirred makes both be dissolved in purification, that is, binder liq, adhesive liquid is made Mass percent in body shared by each component is:Valnemulin hydrochloride 5~40%, dispersant 10~40%, adhesive 1~ 10%, surplus is solvent;
(2), pelletize:
Diluent is thrown into fluid bed, logical hot blast makes fluidized state, is sprayed after then binder liq is atomized In fluidized bed, the percentage that diluent accounts for raw material gross weight is respectively 10~84%, after having sprayed under the conditions of less than 45 DEG C after Continuous heating more than 30min, then naturally cools to room temperature, that is, obtains granular valnemulin hydrochloride premix.
In step (1), described dispersant is more than one or both of sucrose, lactose, glucose, mannitol mixed Compound.
In step (1), described adhesive is hydroxypropyl methyl cellulose, polyvinylpyrrolidone, carboxymethyl cellulose Mixture more than one or both of sodium.
In step (2), described diluent is one kind in starch, sucrose, lactose, glucose, mannitol, beta-schardinger dextrin Or two or more mixture.
In step (2), the EAT of the hot blast is 70~75 DEG C, and air quantity frequency is 30~50HZ.
In step (2), after using peristaltic pump, binder liq is atomized spray into fluid bed in, wriggling revolution speed be 200~ 400rpm, atomisation pressure are 2.0~3.0bar.
Compared with prior art, the advantage of the invention is that:
The invention provides a kind of preparation method of valnemulin hydrochloride premix, and it is wonderful to irrigate Buddhist nun with synthetic hydrochloric acid by directly Pre-mixing agent, which is made, in the purification of woods bulk drug can effectively reach taste masking purpose.Shown by study on the stability, valnemulin salt Under acceleration by light experiment condition be stable after microencapsulation, can effectively make up the cost having with valnemulin hydrochloride bulk drug it is high, Powder excitant is strong, to photo-labile, the deficiencies of easily being decomposed with contacts such as feeds, taken beneficial to animal, and manufacture craft is simple.
Embodiment
The present invention is described further with reference to embodiments, but the protection content of the present invention is not limited to following reality Apply example.
Embodiment 1
(1) preparation of binder liq
The purification containing valnemulin hydrochloride of synthetic hydrochloric acid valnemulin bulk drug is taken, adds sucrose and hydroxypropyl Methylcellulose is dissolved in purification, and the percentage that the dosage of each raw material accounts for raw material gross weight is respectively:In purification Valnemulin hydrochloride 5%, sucrose 10%, hydroxypropyl methyl cellulose 1%, binder liq is obtained after stirring and dissolving.
(2) pelletize
Starch is thrown into fluid bed, logical hot blast makes fluidized state, sets EAT as 70 DEG C, air quantity frequency For 30HZ, wriggling revolution speed 200rpm, atomisation pressure 2.0bar, fluidisation is sprayed into after binder liq is atomized with peristaltic pump In bed.The percentage that starch accounts for raw material gross weight is respectively 84%, continues heating more than 30min after having sprayed below 45 DEG C, so After naturally cool to room temperature, obtain valnemulin hydrochloride premix.
Embodiment 2
(1) preparation of binder liq
The purification containing valnemulin hydrochloride of synthetic hydrochloric acid valnemulin bulk drug is taken, adds lactose and polyethylene Pyrrolidones is dissolved in purification, and the percentage that the dosage of each raw material accounts for raw material gross weight is respectively:Salt in purification Sour valnemulin 40%, lactose 40%, polyvinylpyrrolidone 10%, binder liq is obtained after stirring and dissolving.
(2) pelletize
Sucrose is thrown into fluid bed, logical hot blast makes fluidized state, sets EAT as 75 DEG C, air quantity frequency For 50HZ, wriggling revolution speed 300rpm, atomisation pressure 3.0bar, fluidisation is sprayed into after binder liq is atomized with peristaltic pump In bed.The percentage that sucrose accounts for raw material gross weight is respectively 10%, continues heating more than 30min after having sprayed below 45 DEG C, so After naturally cool to room temperature, obtain valnemulin hydrochloride premix.
Embodiment 3
(1) preparation of binder liq
The purification containing valnemulin hydrochloride of synthetic hydrochloric acid valnemulin bulk drug is taken, adds glucose and carboxylic first Base sodium cellulosate is dissolved in purification, and the percentage that the dosage of each raw material accounts for raw material gross weight is respectively:In purification Valnemulin hydrochloride 20%, glucose 20%, sodium carboxymethylcellulose 5%, binder liq is obtained after stirring and dissolving.
(2) pelletize
Dextrin is thrown into fluid bed, logical hot blast makes fluidized state, sets EAT as 72 DEG C, air quantity frequency For 40HZ, wriggling revolution speed 250rpm, atomisation pressure 2.5bar, fluidisation is sprayed into after binder liq is atomized with peristaltic pump In bed.The percentage that dextrin accounts for raw material gross weight is respectively 55%, continues heating more than 30min after having sprayed below 45 DEG C, so After naturally cool to room temperature, obtain valnemulin hydrochloride premix.
Embodiment 4
(1) preparation of binder liq
The purification containing valnemulin hydrochloride of synthetic hydrochloric acid valnemulin bulk drug is taken, adds mannitol and carboxylic first Base sodium cellulosate is dissolved in purification, and the percentage that the dosage of each raw material accounts for raw material gross weight is respectively:In purification Valnemulin hydrochloride 5%, mannitol 40%, sodium carboxymethylcellulose 1%, binder liq is obtained after stirring and dissolving.
(2) pelletize
Lactose is thrown into fluid bed, logical hot blast makes fluidized state, sets EAT as 70 DEG C, air quantity frequency For 50HZ, wriggling revolution speed 300rpm, atomisation pressure 2.0bar, fluidisation is sprayed into after binder liq is atomized with peristaltic pump In bed.The percentage that lactose accounts for raw material gross weight is respectively 54%, continues heating more than 30min after having sprayed below 45 DEG C, so After naturally cool to room temperature, obtain valnemulin hydrochloride premix.
Embodiment 5
(1) preparation of binder liq
The purification containing valnemulin hydrochloride of synthetic hydrochloric acid valnemulin bulk drug is taken, adds sucrose and carboxymethyl Sodium cellulosate is dissolved in purification, and the percentage that the dosage of each raw material accounts for raw material gross weight is respectively:Salt in purification Sour valnemulin 10%, sucrose 10%, sodium carboxymethylcellulose 10%, binder liq is obtained after stirring and dissolving.
(2) pelletize
Glucose is thrown into fluid bed, logical hot blast makes fluidized state, sets EAT as 75 DEG C, air quantity frequency Rate is 50HZ, wriggling revolution speed 200rpm, atomisation pressure 2.0bar, and stream is sprayed into after binder liq is atomized with peristaltic pump Change in bed.The percentage that glucose accounts for raw material gross weight is respectively 70%, continue below 45 DEG C to heat after having sprayed 30min with On, room temperature is then naturally cooled to, obtains valnemulin hydrochloride premix.
Embodiment 6
(1) preparation of binder liq
The purification containing valnemulin hydrochloride of synthetic hydrochloric acid valnemulin bulk drug is taken, adds sucrose and polyethylene Pyrrolidones is dissolved in purification, and the percentage that the dosage of each raw material accounts for raw material gross weight is respectively:Salt in purification Sour valnemulin 10%, sucrose 10%, polyvinylpyrrolidone 1%, binder liq is obtained after stirring and dissolving.
(2) pelletize
Mannitol is thrown into fluid bed, logical hot blast makes fluidized state, sets EAT as 75 DEG C, air quantity frequency Rate is 30HZ, wriggling revolution speed 300rpm, atomisation pressure 2.0bar, and stream is sprayed into after binder liq is atomized with peristaltic pump Change in bed.The percentage that mannitol accounts for raw material gross weight is respectively 79%, continue below 45 DEG C to heat after having sprayed 30min with On, room temperature is then naturally cooled to, obtains valnemulin hydrochloride premix.
Embodiment 7
(1) preparation of binder liq
The purification containing valnemulin hydrochloride of synthetic hydrochloric acid valnemulin bulk drug is taken, adds lactose and polyethylene Pyrrolidones is dissolved in purification, and the percentage that the dosage of each raw material accounts for raw material gross weight is respectively:Salt in purification Sour valnemulin 5%, lactose 40%, polyvinylpyrrolidone 10%, binder liq is obtained after stirring and dissolving.
(2) pelletize
Betadex is thrown into fluid bed, logical hot blast makes fluidized state, sets EAT as 70 DEG C, wind Amount frequency is 50HZ, wriggling revolution speed 300rpm, atomisation pressure 3.0bar, is sprayed after with peristaltic pump, binder liq is atomized In fluidized bed.The percentage that betadex accounts for raw material gross weight is respectively 45%, continues to heat below 45 DEG C after having sprayed More than 30min, room temperature is then naturally cooled to, obtain valnemulin hydrochloride premix.
Valnemulin hydrochloride premix clinical test:
152 pigs of nature outburst swine dysentery are selected to investigate clinical efficacy of the valnemulin hydrochloride premix to swine dysentery; 240 health pigs of selection are respectively adopted porcine contagious pleuropneumonia defence line bacillus and establish pleuropneumonia model and mycoplasma foundation branch Pneumonias model, carry out verifying that 10% valnemulin hydrochloride premix faces porcine contagious pleuropneumonia and region pneumonia Bed curative effect.
As a result:Each test group of 10% valnemulin hydrochloride premix is compared with positive controls, to pig transmissible pleura lung Inflammation, porcine enzootic pneumonia, swine dysentery have the effect of notable (P < 0.05), wherein the ratio with 200mg/kg and 300mg/kg There was no significant difference (P > 0.05) for the effect of being added in feed respectively to porcine contagious pleuropneumonia, porcine enzootic pneumonia, with The effect of 75mg/kg and 100mg/kg ratio is added in feed to swine dysentery with there was no significant difference (P > 0.05).
Conclusion:It is recommended that porcine contagious pleuropneumonia, pig place are treated in 10% valnemulin hydrochloride premix clinical practice Property pneumonia when feed in adding proportion be 200mg/kg, the medicine is used to treat adding proportion of the swine dysentery in feed and be 75mg/kg。
Valnemulin hydrochloride premix residual eliminating is tested:
In medicament residue research, mixed valnemulin hydrochloride premix is continuously raised to the pig tons of the 200g/ in terms of valnemulin feed After agent 21 days is discontinued, after last time is administered 0,6,12,18,24,36h collections blood plasma, muscle, fat, liver and kidney Sample carries out analysis measure.As a result show, remained in muscle and fat at least, elimination is very fast, and 24h is in muscle and fat after drug withdrawal 0.07 μ g/g and 0.08 μ g/g can be detected in fat respectively, 36h is not detected by;More in liver, 24h can be detected after drug withdrawal It is less than the μ g/g of quantitative limit 0.1 (being far below MRL0.5 μ g/g) after to 0.15 μ g/g, 36h;Residual is taken second place in kidney, but is eliminated relative Relatively slow, 36h can detect 0.11 μ g/g after drug withdrawal, and blood supersession rate is similar to liver, and 0.09 μ g/ can be detected after drug withdrawal 24h Ml, content are relatively low.Compared with its hetero-organization, medicine eliminates most slow in kidney, it is proposed that as valnemulin hydrochloride in pig body Interior residual target tissue.If using kidney as target tissue, the dosage to the pig ton feeds of the 200g/ in terms of valnemulin continuously raises mixed salt After sour valnemulin pre-mixing agent 21, off-drug period 1d.

Claims (6)

1. a kind of preparation method of valnemulin hydrochloride premix, it is characterised in that comprise the following steps:
(1), the preparation of binder liq:
In the valnemulin hydrochloride bulk drug of synthesis, the purification containing valnemulin hydrochloride is taken, is added in purification Enter dispersant and adhesive, being sufficiently stirred makes both be dissolved in purification, i.e., obtained binder liq, in binder liq Mass percent shared by each component is:Valnemulin hydrochloride 5~40%, dispersant 10~40%, adhesive 1~10%, it is remaining Measure as solvent;
(2), pelletize:
Diluent is thrown into fluid bed, logical hot blast makes fluidized state, and stream is sprayed into after then binder liq is atomized Change in bed, the percentage that diluent accounts for raw material gross weight is respectively 10~84%, continues to add under the conditions of less than 45 DEG C after having sprayed Hot more than 30min, then naturally cools to room temperature, that is, obtains granular valnemulin hydrochloride premix.
2. the preparation method of valnemulin hydrochloride premix according to claim 1, it is characterised in that:In step (1), institute The dispersant stated is mixture more than one or both of sucrose, lactose, glucose, mannitol.
3. the preparation method of valnemulin hydrochloride premix according to claim 1, it is characterised in that:In step (1), institute The adhesive stated is more than one or both of hydroxypropyl methyl cellulose, polyvinylpyrrolidone, sodium carboxymethylcellulose Mixture.
4. the preparation method of valnemulin hydrochloride premix according to claim 1, it is characterised in that:In step (2), institute The diluent stated is mixture more than one or both of starch, sucrose, lactose, glucose, mannitol, beta-schardinger dextrin.
5. the preparation method of valnemulin hydrochloride premix according to claim 1, it is characterised in that:In step (2), institute The EAT for stating hot blast is 70~75 DEG C, and air quantity frequency is 30~50HZ.
6. the preparation method of valnemulin hydrochloride premix according to claim 1, it is characterised in that:In step (2), adopt Sprayed into after with peristaltic pump, binder liq is atomized in fluid bed, wriggling revolution speed is 200~400rpm, atomisation pressure 2.0 ~3.0bar.
CN201710754753.5A 2017-08-29 2017-08-29 A kind of preparation method of valnemulin hydrochloride premix Pending CN107441050A (en)

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