CN108420796A - A kind of salinomycin particle premix and preparation method thereof - Google Patents
A kind of salinomycin particle premix and preparation method thereof Download PDFInfo
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- CN108420796A CN108420796A CN201810288676.3A CN201810288676A CN108420796A CN 108420796 A CN108420796 A CN 108420796A CN 201810288676 A CN201810288676 A CN 201810288676A CN 108420796 A CN108420796 A CN 108420796A
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- Prior art keywords
- salinomycin
- zymotic fluid
- preparation
- filter cake
- glycine
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- 235000019378 salinomycin Nutrition 0.000 title claims abstract description 128
- KQXDHUJYNAXLNZ-XQSDOZFQSA-N Salinomycin Chemical compound O1[C@@H]([C@@H](CC)C(O)=O)CC[C@H](C)[C@@H]1[C@@H](C)[C@H](O)[C@H](C)C(=O)[C@H](CC)[C@@H]1[C@@H](C)C[C@@H](C)[C@@]2(C=C[C@@H](O)[C@@]3(O[C@@](C)(CC3)[C@@H]3O[C@@H](C)[C@@](O)(CC)CC3)O2)O1 KQXDHUJYNAXLNZ-XQSDOZFQSA-N 0.000 title claims abstract description 115
- 239000004189 Salinomycin Substances 0.000 title claims abstract description 115
- 229960001548 salinomycin Drugs 0.000 title claims abstract description 115
- 239000002245 particle Substances 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title claims abstract description 37
- 239000012530 fluid Substances 0.000 claims abstract description 123
- 239000012065 filter cake Substances 0.000 claims abstract description 69
- 238000002156 mixing Methods 0.000 claims abstract description 21
- 238000005469 granulation Methods 0.000 claims abstract description 7
- 230000003179 granulation Effects 0.000 claims abstract description 7
- 238000007906 compression Methods 0.000 claims abstract description 3
- 230000006835 compression Effects 0.000 claims abstract description 3
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims description 146
- 239000004471 Glycine Substances 0.000 claims description 73
- 239000011734 sodium Substances 0.000 claims description 40
- 229910052708 sodium Inorganic materials 0.000 claims description 40
- 229920002472 Starch Polymers 0.000 claims description 39
- 239000008107 starch Substances 0.000 claims description 39
- 235000019698 starch Nutrition 0.000 claims description 39
- 238000003756 stirring Methods 0.000 claims description 29
- 238000000034 method Methods 0.000 claims description 22
- 238000000855 fermentation Methods 0.000 claims description 20
- 230000004151 fermentation Effects 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 229920002401 polyacrylamide Polymers 0.000 claims description 19
- 230000008569 process Effects 0.000 claims description 18
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 9
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 8
- 125000002091 cationic group Chemical group 0.000 claims description 3
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims 1
- 125000000129 anionic group Chemical group 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 238000005265 energy consumption Methods 0.000 abstract description 5
- 239000003674 animal food additive Substances 0.000 abstract description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 13
- 239000002253 acid Substances 0.000 description 13
- 239000011575 calcium Substances 0.000 description 13
- 229910052791 calcium Inorganic materials 0.000 description 13
- 210000003454 tympanic membrane Anatomy 0.000 description 13
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 12
- 239000003795 chemical substances by application Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- 150000003839 salts Chemical class 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 210000004027 cell Anatomy 0.000 description 4
- 230000006378 damage Effects 0.000 description 4
- 238000000605 extraction Methods 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 238000001694 spray drying Methods 0.000 description 4
- 150000001768 cations Chemical class 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000007127 saponification reaction Methods 0.000 description 3
- 241000224483 Coccidia Species 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 210000000170 cell membrane Anatomy 0.000 description 2
- 235000009508 confectionery Nutrition 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000012010 growth Effects 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 235000011121 sodium hydroxide Nutrition 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 206010012735 Diarrhoea Diseases 0.000 description 1
- 206010059866 Drug resistance Diseases 0.000 description 1
- 241001568757 Elsinoe glycines Species 0.000 description 1
- 241000192125 Firmicutes Species 0.000 description 1
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 206010034133 Pathogen resistance Diseases 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000011260 aqueous acid Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 description 1
- 230000010261 cell growth Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000686 essence Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000029142 excretion Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 230000002147 killing effect Effects 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 150000002763 monocarboxylic acids Chemical class 0.000 description 1
- 210000000633 nuclear envelope Anatomy 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920002338 polyhydroxyethylmethacrylate Polymers 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 238000011045 prefiltration Methods 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 210000001563 schizont Anatomy 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 210000004215 spore Anatomy 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
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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
- A61K9/16—Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
- A61K9/1682—Processes
-
- 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
- A61K31/335—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin
- A61K31/35—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin having six-membered rings with one oxygen as the only ring hetero atom
- A61K31/351—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin having six-membered rings with one oxygen as the only ring hetero atom not condensed with another ring
-
- 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
- A61K9/16—Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
- A61K9/1605—Excipients; Inactive ingredients
- A61K9/1617—Organic compounds, e.g. phospholipids, fats
-
- 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
- A61K9/16—Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
- A61K9/1605—Excipients; Inactive ingredients
- A61K9/1629—Organic macromolecular compounds
- A61K9/1652—Polysaccharides, e.g. alginate, cellulose derivatives; 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
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P33/00—Antiparasitic agents
- A61P33/02—Antiprotozoals, e.g. for leishmaniasis, trichomoniasis, toxoplasmosis
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Veterinary Medicine (AREA)
- General Health & Medical Sciences (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Medicinal Chemistry (AREA)
- Pharmacology & Pharmacy (AREA)
- Chemical & Material Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Public Health (AREA)
- Engineering & Computer Science (AREA)
- Epidemiology (AREA)
- General Chemical & Material Sciences (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Communicable Diseases (AREA)
- Oncology (AREA)
- Tropical Medicine & Parasitology (AREA)
- Biophysics (AREA)
- Molecular Biology (AREA)
- Fodder In General (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Medicinal Preparation (AREA)
Abstract
The present invention relates to feed additive fields, and in particular to a kind of salinomycin particle premix and preparation method thereof.The preparation method of the salinomycin particle premix, includes the following steps：1) salinomycin zymotic fluid is pre-processed；2) it filters：The pretreated salinomycin zymotic fluid of step 1) is subjected to plate compression, obtains filter cake；3) it squeezes：High-pressure compressing is carried out to filter cake；4) it is granulated：Filter cake through high-pressure compressing in step 3) is subjected to extruding granulation, dry, mixing obtains salinomycin particle premix.The preparation method high income of salinomycin particle premix provided by the invention, low energy consumption, a granulating rate height.
Description
Technical field
The present invention relates to feed additive fields, in particular to a kind of salinomycin particle premix and its preparation side
Method.
Background technology
Salinomycin is monocarboxylic acid polyethers animal specific antibiotic, is had to most of gram-positive bacterias and various coccidias
Stronger inhibition and killing effect are not likely to produce drug resistance and cross-resistance, and excretion is rapid, and residual quantity is extremely low, can be used for preventing
It controls diarrhea, growth promotion, improve survival rate.Salinomycin has particularly ring-shaped structure, and center is constituted by oxygen atom arranged side by side, carries
Negative electrical charge has cation carrier property, is especially all had to potassium, sodium, calcium, magnesium etc. to the cation contained in cell stronger
Affinity, formed complex compound, becomes liposoluble substance, and cation necessary to cell activities is caused to pass through fat on film
The permeability of matter barrier is reinforced, and ion discrepancy cell is freer.The destruction of membrane permeability function causes intraor extracellular ion
Concentration changes greatly, and the normal equilibrium state of ion is destroyed, and the just bulk deposition of the ion in spore and schizont caused
More hydrones penetrates into cell, makes cell expansion, and cell membrane is damaged, and polypide growth, development are inhibited.Development is gone down, coccidia
Cell membrane, nuclear membrane rupture, polypide are dead.
In current technology, in order to solve influence of the zymotic fluid Residual oil height to subsequent production, the granulating rate of salinomycin is improved,
Preparing in bacterium slurries needs that some auxiliary materials are added.Calcium carbonate can improve solid content and disperse Residual oil as a kind of auxiliary material.Salt at present
The extraction process that mycin uses after fermentation is mainly salinomycin zymotic fluid → plus auxiliary material → spray drying → mixing → packaging.It should
In technique, it is spray-dried as a step of salinomycin extraction process key.Due to containing a large amount of greases in zymotic fluid, can not carry out straight
The plate-frame filtering connect, therefore, most producer take spray drying in extraction；But since the zymotic fluid without prefiltration contains
Water is high, and when causing to be concentrated by evaporation, time-consuming, high energy consumption.
Grease is removed using addition soda acid in the prior art, but salinomycin is unstable under acidic condition, adjusts acid that can lead to salt
The destruction of mycin product, product yield are low.Such as lye is used to carry out saponification to zymotic fluid.But since saponification is slow, need pair
Zymotic fluid often adds liquid caustic soda, thorough saponification.
CN105326800A discloses a kind of preparation method of salinomycin particle preparation, includes the following steps：It prepares acid
Zymotic fluid：Salinomycin zymotic fluid acid solution is adjusted into pH to 4.0-5.0；The pretreatment of acid fermentation liquid：The acidity of pH will be mixed up
Zymotic fluid keeps the temperature 3-4 hours at 60 DEG C -65 DEG C；Prepare salinomycin feed liquid：It is added into obtained acid fermentation liquid a certain amount of
Salinomycin feed liquid is made in calcium carbonate；Spray drying：Particle is made to get salt using spray drying process in the salinomycin feed liquid of preparation
Mycin granular preparation.The zymotechnique to salinomycin of the invention uses acid fermentation, improves the speed of zymotic fluid layering, contracting
Time of short layering, and be layered thorough, improve the yield of salinomycin, and the invention passes through spraying granulation and cooperation is added
The spray condition of setting improves the efficiency of spraying.But the invention uses acidification, salinomycin is in acid condition not
Stablize, adjusts acid that the destruction of salinomycin product, product yield can be caused low；It uses in technical process and is being boiled after being spray-dried
It is big to rise energy consumption for drying；It is big with acid amount to adjust salinomycin zymotic fluid, causes salt content in salinomycin pre-mixing agent high.
CN101884621A discloses a kind of preparation method of salinomycin particle premix, the specific steps are：By salinomycin
Zymotic fluid adjusts pH to 6.5-10.0 with alkali, obtains alkaline broth；Calcium carbonate is added again, obtains salinomycin feed liquid；Obtained by step a
Salinomycin feed liquid is spray-dried to get salinomycin particle premix；Salinomycin particle premix prepared by this method is uniform
Property and stability it is high.But this method uses base extraction to zymotic fluid, and which use a large amount of alkali, and salinomycin is caused to premix
Salt content is high in agent.
Invention content
It is an object of the invention to overcome the deficiencies of existing technologies, provide that a kind of product yield is high, low energy consumption, granulating rate is high
Salinomycin particle premix and preparation method thereof.
To achieve the goals above, the present invention provides a kind of preparation method of salinomycin particle premix, which is characterized in that
Include the following steps：
1) it pre-processes：In salinomycin zymotic fluid, sodium carboxymethyl starch, flocculant and calcium carbonate, stirring, Xiang Fa is added
Glycine solution is added dropwise in zymotic fluid, continues to stir, obtains pretreated salinomycin zymotic fluid；
2) it filters：The pretreated salinomycin zymotic fluid of step 1) is subjected to plate compression, obtains filter cake；
3) it squeezes：High-pressure compressing is carried out to filter cake；
4) it is granulated：Filter cake through high-pressure compressing in step 3) is subjected to extruding granulation, dry, mixing obtains salinomycin
Grain pre-mixing agent.
Further, flocculant described in step 1) is selected from non-ionic polyacrylamide, cationic polyacrylamide, the moon
It is one or more in cationic polyacrylamide；The addition of the flocculant is the 0.3-1.0wt% of zymotic fluid quality；
Further, the addition of calcium carbonate described in step 1) is the 3.0-5.0wt% of zymotic fluid quality.
Further, sodium carboxymethyl starch described in step 1) and the 0.1- that the total addition of glycine is zymotic fluid quality
0.8wt%；The mass ratio of the sodium carboxymethyl starch and glycine is 5-8:1.
In the present invention, individually addition sodium carboxymethyl starch can improve the granulating rate of salinomycin.Carboxymethyl starch is added
Sodium and glycine contain carboxyl and amino in glycine, act synergistically with sodium carboxymethyl starch, pass through hydrogen bond action with salinomycin
It unites combination, the granulating rate of salinomycin particle can be further improved.Meanwhile sodium carboxymethyl starch and sweet ammonia in the present invention
The mass ratio of acid is 5-8:1, the amount of glycine be added it is excessive, the same sodium carboxymethyl starch of glycine, salinomycin combination degree mistake
Greatly, granulation is difficult, and the amount addition of glycine is very few, and it is loose to easily cause salinomycin particle.
Further, in glycine solution described in step 1) glycine a concentration of 0.05-0.2g/ml.
Further, the rate that glycine solution is added dropwise described in step 1) is 0.5-1.5ml/s.
In the present invention, glycine is added to by way of dropwise addition in zymotic fluid, glycine solution it is a concentration of
0.05-0.2g/ml, the rate that glycine solution is added dropwise are 0.5-1.5ml/s.Glycine solution concentration is excessive, dropwise addition
Rate is too fast, and the same sodium carboxymethyl starch of glycine, salinomycin can be caused to unite rapidly, and glycine and sodium carboxymethyl starch, salt are mould
It is also easy to produce larger hole between element, it is uneven to eventually lead to salinomycin particle.Glycine solution concentration is too small, the speed of dropwise addition
Rate is excessively slow, and partial glycine is soluble in water, has little time same sodium carboxymethyl starch, salinomycin effect, causes unnecessary waste.
Further, the fermentation titer of salinomycin zymotic fluid described in step 1) is 3000-3500 μ g/mL.
Further, the pressure of high-pressure compressing described in step 3) is 0.5-3.0MPa, and the squeezing time is 1-5h.
Further, filter cake described in step 4) is 10-28wt% containing water quality.
In the present invention, the water content of the filter cake through high-pressure compressing need to be controlled strictly, and the water content of filter cake is excessively high, squeeze system
The salinomycin particle that grain obtains is easy to unite, and is not easy to disperse.
Further, extruding granulation is carried out to filter cake using SET series twin-screw extruder comminutors in step 4).
The present invention also provides a kind of salinomycin particle premixes prepared by above-mentioned preparation method.
What the present invention reached has the beneficial effect that：
1) high degree of automation, whole flow process is easy to automate, and personnel labor intensity is low.
2) present invention is added without acid during preparing salinomycin particle premix, avoid acid condition cause it is mould to salt
The destruction of plain product, product yield are high.
3) that salinomycin zymotic fluid is all not dry during the present invention prepares salinomycin particle premix, only
It squeezes filter cake and removes partial moisture, greatly reduce energy consumption.
4) it in the present invention, is flocculated with non-ionic polyacrylamide, glycine and sodium carboxymethyl starch collaboration are made
With being united combination by hydrogen bond action with salinomycin, substantially increase the granulating rate of salinomycin particle.
Specific implementation mode
Embodiment 1
A kind of preparation method of salinomycin particle premix, includes the following steps：
1) it pre-processes：In 1000L salinomycins zymotic fluid (fermentation titer is 3000 μ g/mL), addition accounts for zymotic fluid quality
The carbonic acid of 0.1% sodium carboxymethyl starch, the non-ionic polyacrylamide of zymotic fluid quality 0.3%, zymotic fluid quality 3%
Calcium stirs 10 minutes, and glycine solution (a concentration of 0.05g/ of glycine in glycine solution is added dropwise into zymotic fluid
The mass ratio of ml, quality and sodium carboxymethyl starch that glycine is added are 1:5), drop rate 1.5ml/s continues to stir,
Obtain pretreated salinomycin zymotic fluid；
2) it filters：The pretreated salinomycin zymotic fluid of step 1) is squeezed plate and frame filter press by eardrum formula hydraulic pressure to carry out
Filter, obtains filter cake；
3) it squeezes：High-pressure compressing is carried out to filter cake, the pressure of high-pressure compressing is 0.5MPa, and the squeezing time is 5h, control filter
Cake is 28wt% containing water quality；
4) it is granulated：Filter cake through high-pressure compressing in step 3) is transported to SET series pair by auger and belt conveyor
Screw extruder pelletizer is pelletized, and particle obtained is dried by vibrated fluidized bed, controls 120 DEG C of inlet air temperature, row
Then 60 DEG C of air temperature is uniformly mixed by two-dimensional mixing machine, obtains salinomycin particle premix.
Embodiment 2
A kind of preparation method of salinomycin particle premix, includes the following steps：
1) it pre-processes：In 1000L salinomycins zymotic fluid (fermentation titer is 3500 μ g/mL), addition accounts for zymotic fluid quality
The carbonic acid of 0.5% sodium carboxymethyl starch, the non-ionic polyacrylamide of zymotic fluid quality 1.0%, zymotic fluid quality 5%
Calcium stirs 15 minutes, be added dropwise into zymotic fluid glycine solution (a concentration of 0.2g/ml of glycine in glycine solution,
The mass ratio of quality and sodium carboxymethyl starch that glycine is added is 1:8), drop rate 0.5ml/s continues to stir, obtain
Pretreated salinomycin zymotic fluid；
2) it filters：The pretreated salinomycin zymotic fluid of step 1) is squeezed plate and frame filter press by eardrum formula hydraulic pressure to carry out
Filter, obtains filter cake；
3) it squeezes：High-pressure compressing is carried out to filter cake, the pressure of high-pressure compressing is 3.0MPa, and the squeezing time is 1h, control filter
Cake is 10wt% containing water quality；
4) it is granulated：Filter cake through high-pressure compressing in step 3) is transported to SET series pair by auger and belt conveyor
Screw extruder pelletizer is pelletized, and particle obtained is dried by vibrated fluidized bed, controls 110 DEG C of inlet air temperature, row
Then 70 DEG C of air temperature is uniformly mixed by two-dimensional mixing machine, obtains salinomycin particle premix.
Embodiment 3
A kind of preparation method of salinomycin particle premix, includes the following steps：
1) it pre-processes：In 1000L salinomycins zymotic fluid (fermentation titer is 3200 μ g/mL), addition accounts for zymotic fluid quality
The carbonic acid of 0.4% sodium carboxymethyl starch, the non-ionic polyacrylamide of zymotic fluid quality 0.5%, zymotic fluid quality 4%
Calcium stirs 15 minutes, be added dropwise into zymotic fluid glycine solution (a concentration of 0.1g/ml of glycine in glycine solution,
The mass ratio of quality and sodium carboxymethyl starch that glycine is added is 1:5), drop rate 0.8ml/s continues to stir, obtain
Pretreated salinomycin zymotic fluid；
2) it filters：The pretreated salinomycin zymotic fluid of step 1) is squeezed plate and frame filter press by eardrum formula hydraulic pressure to carry out
Filter, obtains filter cake；
3) it squeezes：High-pressure compressing is carried out to filter cake, the pressure of high-pressure compressing is 2.0MPa, and the squeezing time is 2h, control filter
Cake is 25wt% containing water quality；
4) it is granulated：Filter cake through high-pressure compressing in step 3) is transported to SET series pair by auger and belt conveyor
Screw extruder pelletizer is pelletized, and particle obtained is dried by vibrated fluidized bed, controls 120 DEG C of inlet air temperature, row
Then 60 DEG C of air temperature is uniformly mixed by two-dimensional mixing machine, obtains salinomycin particle premix.
Embodiment 4
A kind of preparation method of salinomycin particle premix, includes the following steps：
1) it pre-processes：In 1000L salinomycins zymotic fluid (fermentation titer is 3200 μ g/mL), addition accounts for zymotic fluid quality
The carbonic acid of 0.4% sodium carboxymethyl starch, the non-ionic polyacrylamide of zymotic fluid quality 0.5%, zymotic fluid quality 4%
Calcium stirs 15 minutes, be added dropwise into zymotic fluid glycine solution (a concentration of 0.1g/ml of glycine in glycine solution,
The mass ratio of quality and sodium carboxymethyl starch that glycine is added is 1:8), drop rate 0.8ml/s continues to stir, obtain
Pretreated salinomycin zymotic fluid；
2) it filters：The pretreated salinomycin zymotic fluid of step 1) is squeezed plate and frame filter press by eardrum formula hydraulic pressure to carry out
Filter, obtains filter cake；
3) it squeezes：High-pressure compressing is carried out to filter cake, the pressure of high-pressure compressing is 2.0MPa, and the squeezing time is 2h, control filter
Cake is 25wt% containing water quality；
4) it is granulated：Filter cake through high-pressure compressing in step 3) is transported to SET series pair by auger and belt conveyor
Screw extruder pelletizer is pelletized, and particle obtained is dried by vibrated fluidized bed, controls 120 DEG C of inlet air temperature, row
Then 60 DEG C of air temperature is uniformly mixed by two-dimensional mixing machine, obtains salinomycin particle premix.
Embodiment 5
A kind of preparation method of salinomycin particle premix, includes the following steps：
1) it pre-processes：In 1000L salinomycins zymotic fluid (fermentation titer is 3200 μ g/mL), addition accounts for zymotic fluid quality
The carbonic acid of 0.4% sodium carboxymethyl starch, the non-ionic polyacrylamide of zymotic fluid quality 0.5%, zymotic fluid quality 4%
Calcium stirs 15 minutes, and glycine solution (a concentration of 0.05g/ of glycine in glycine solution is added dropwise into zymotic fluid
The mass ratio of ml, quality and sodium carboxymethyl starch that glycine is added are 1:5), drop rate 0.8ml/s continues to stir,
Obtain pretreated salinomycin zymotic fluid；
2) it filters：The pretreated salinomycin zymotic fluid of step 1) is squeezed plate and frame filter press by eardrum formula hydraulic pressure to carry out
Filter, obtains filter cake；
3) it squeezes：High-pressure compressing is carried out to filter cake, the pressure of high-pressure compressing is 2.0MPa, and the squeezing time is 2h, control filter
Cake is 25wt% containing water quality；
4) it is granulated：Filter cake through high-pressure compressing in step 3) is transported to SET series pair by auger and belt conveyor
Screw extruder pelletizer is pelletized, and particle obtained is dried by vibrated fluidized bed, controls 120 DEG C of inlet air temperature, row
Then 60 DEG C of air temperature is uniformly mixed by two-dimensional mixing machine, obtains salinomycin particle premix.
Embodiment 6
A kind of preparation method of salinomycin particle premix, includes the following steps：
1) it pre-processes：In 1000L salinomycins zymotic fluid (fermentation titer is 3200 μ g/mL), addition accounts for zymotic fluid quality
The carbonic acid of 0.4% sodium carboxymethyl starch, the non-ionic polyacrylamide of zymotic fluid quality 0.5%, zymotic fluid quality 4%
Calcium stirs 15 minutes, be added dropwise into zymotic fluid glycine solution (a concentration of 0.2g/ml of glycine in glycine solution,
The mass ratio of quality and sodium carboxymethyl starch that glycine is added is 1:5), drop rate 0.8ml/s continues to stir, obtain
Pretreated salinomycin zymotic fluid；
2) it filters：The pretreated salinomycin zymotic fluid of step 1) is squeezed plate and frame filter press by eardrum formula hydraulic pressure to carry out
Filter, obtains filter cake；
3) it squeezes：High-pressure compressing is carried out to filter cake, the pressure of high-pressure compressing is 2.0MPa, and the squeezing time is 2h, control filter
Cake is 25wt% containing water quality；
4) it is granulated：Filter cake through high-pressure compressing in step 3) is transported to SET series pair by auger and belt conveyor
Screw extruder pelletizer is pelletized, and particle obtained is dried by vibrated fluidized bed, controls 120 DEG C of inlet air temperature, row
Then 60 DEG C of air temperature is uniformly mixed by two-dimensional mixing machine, obtains salinomycin particle premix.
Embodiment 7
A kind of preparation method of salinomycin particle premix, includes the following steps：
1) it pre-processes：In 1000L salinomycins zymotic fluid (fermentation titer is 3200 μ g/mL), addition accounts for zymotic fluid quality
The carbonic acid of 0.4% sodium carboxymethyl starch, the non-ionic polyacrylamide of zymotic fluid quality 0.5%, zymotic fluid quality 4%
Calcium stirs 15 minutes, be added dropwise into zymotic fluid glycine solution (a concentration of 0.1g/ml of glycine in glycine solution,
The mass ratio of quality and sodium carboxymethyl starch that glycine is added is 1:5), drop rate 0.5ml/s continues to stir, obtain
Pretreated salinomycin zymotic fluid；
2) it filters：The pretreated salinomycin zymotic fluid of step 1) is squeezed plate and frame filter press by eardrum formula hydraulic pressure to carry out
Filter, obtains filter cake；
3) it squeezes：High-pressure compressing is carried out to filter cake, the pressure of high-pressure compressing is 2.0MPa, and the squeezing time is 2h, control filter
Cake is 25wt% containing water quality；
4) it is granulated：Filter cake through high-pressure compressing in step 3) is transported to SET series pair by auger and belt conveyor
Screw extruder pelletizer is pelletized, and particle obtained is dried by vibrated fluidized bed, controls 120 DEG C of inlet air temperature, row
Then 60 DEG C of air temperature is uniformly mixed by two-dimensional mixing machine, obtains salinomycin particle premix.
Embodiment 8
A kind of preparation method of salinomycin particle premix, includes the following steps：
1) it pre-processes：In 1000L salinomycins zymotic fluid (fermentation titer is 3200 μ g/mL), addition accounts for zymotic fluid quality
The carbonic acid of 0.4% sodium carboxymethyl starch, the non-ionic polyacrylamide of zymotic fluid quality 0.5%, zymotic fluid quality 4%
Calcium stirs 15 minutes, be added dropwise into zymotic fluid glycine solution (a concentration of 0.1g/ml of glycine in glycine solution,
The mass ratio of quality and sodium carboxymethyl starch that glycine is added is 1:5), drop rate 1.5ml/s continues to stir, obtain
Pretreated salinomycin zymotic fluid；
2) it filters：The pretreated salinomycin zymotic fluid of step 1) is squeezed plate and frame filter press by eardrum formula hydraulic pressure to carry out
Filter, obtains filter cake；
3) it squeezes：High-pressure compressing is carried out to filter cake, the pressure of high-pressure compressing is 2.0MPa, and the squeezing time is 2h, control filter
Cake is 25wt% containing water quality；
4) it is granulated：Filter cake through high-pressure compressing in step 3) is transported to SET series pair by auger and belt conveyor
Screw extruder pelletizer is pelletized, and particle obtained is dried by vibrated fluidized bed, controls 120 DEG C of inlet air temperature, row
Then 60 DEG C of air temperature is uniformly mixed by two-dimensional mixing machine, obtains salinomycin particle premix.
Comparative example 1
A kind of preparation method of salinomycin particle premix, includes the following steps：
1) it pre-processes：In 1000L salinomycins zymotic fluid (fermentation titer is 3200 μ g/mL), addition accounts for zymotic fluid quality
The carbonic acid of 0.4% sodium carboxymethyl starch, the non-ionic polyacrylamide of zymotic fluid quality 0.5%, zymotic fluid quality 4%
Calcium stirs 15 minutes, be added dropwise into zymotic fluid glycine solution (a concentration of 0.1g/ml of glycine in glycine solution,
The mass ratio of quality and sodium carboxymethyl starch that glycine is added is 1:1), drop rate 0.8ml/s continues to stir, obtain
Pretreated salinomycin zymotic fluid；
2) it filters：The pretreated salinomycin zymotic fluid of step 1) is squeezed plate and frame filter press by eardrum formula hydraulic pressure to carry out
Filter, obtains filter cake；
3) it squeezes：High-pressure compressing is carried out to filter cake, the pressure of high-pressure compressing is 2.0MPa, and the squeezing time is 2h, control filter
Cake is 25wt% containing water quality；
4) it is granulated：Filter cake through high-pressure compressing in step 3) is transported to SET series pair by auger and belt conveyor
Screw extruder pelletizer is pelletized, and particle obtained is dried by vibrated fluidized bed, controls 120 DEG C of inlet air temperature, row
Then 60 DEG C of air temperature is uniformly mixed by two-dimensional mixing machine, obtains salinomycin particle premix.
Comparative example 2
A kind of preparation method of salinomycin particle premix, includes the following steps：
1) it pre-processes：In 1000L salinomycins zymotic fluid (fermentation titer is 3200 μ g/mL), addition accounts for zymotic fluid quality
The carbonic acid of 0.4% sodium carboxymethyl starch, the non-ionic polyacrylamide of zymotic fluid quality 0.5%, zymotic fluid quality 4%
Calcium stirs 15 minutes, be added dropwise into zymotic fluid glycine solution (a concentration of 0.1g/ml of glycine in glycine solution,
The mass ratio of quality and sodium carboxymethyl starch that glycine is added is 1:5), drop rate 10ml/s continues to stir, and obtains pre-
Treated salinomycin zymotic fluid；
2) it filters：The pretreated salinomycin zymotic fluid of step 1) is squeezed plate and frame filter press by eardrum formula hydraulic pressure to carry out
Filter, obtains filter cake；
3) it squeezes：High-pressure compressing is carried out to filter cake, the pressure of high-pressure compressing is 2.0MPa, and the squeezing time is 2h, control filter
Cake is 25wt% containing water quality；
4) it is granulated：Filter cake through high-pressure compressing in step 3) is transported to SET series pair by auger and belt conveyor
Screw extruder pelletizer is pelletized, and particle obtained is dried by vibrated fluidized bed, controls 120 DEG C of inlet air temperature, row
Then 60 DEG C of air temperature is uniformly mixed by two-dimensional mixing machine, obtains salinomycin particle premix.
Comparative example 3
A kind of preparation method of salinomycin particle premix, includes the following steps：
1) it pre-processes：In 1000L salinomycins zymotic fluid (fermentation titer is 3200 μ g/mL), addition accounts for zymotic fluid quality
The carbonic acid of 0.4% sodium carboxymethyl starch, the non-ionic polyacrylamide of zymotic fluid quality 0.5%, zymotic fluid quality 4%
Calcium stirs 15 minutes, be added dropwise into zymotic fluid glycine solution (a concentration of 0.1g/ml of glycine in glycine solution,
The mass ratio of quality and sodium carboxymethyl starch that glycine is added is 1:5), drop rate 0.8ml/s continues to stir, obtain
Pretreated salinomycin zymotic fluid；
2) it filters：The pretreated salinomycin zymotic fluid of step 1) is squeezed plate and frame filter press by eardrum formula hydraulic pressure to carry out
Filter, obtains filter cake；
3) it squeezes：High-pressure compressing is carried out to filter cake, the pressure of high-pressure compressing is 2.0MPa, and the squeezing time is 10h, control filter
Cake is 2wt% containing water quality；
4) it is granulated：Filter cake through high-pressure compressing in step 3) is transported to SET series pair by auger and belt conveyor
Screw extruder pelletizer is pelletized, and particle obtained is dried by vibrated fluidized bed, controls 120 DEG C of inlet air temperature, row
Then 60 DEG C of air temperature is uniformly mixed by two-dimensional mixing machine, obtains salinomycin particle premix.
Comparative example 4
1) it pre-processes：In 1000L salinomycins zymotic fluid (fermentation titer is 3200 μ g/mL), addition accounts for zymotic fluid quality
0.5% non-ionic polyacrylamide, the calcium carbonate of zymotic fluid quality 4% stir 15 minutes, sweet ammonia are added dropwise into zymotic fluid
(a concentration of 0.1g/ml of glycine, the quality that glycine is added account for zymotic fluid quality to aqueous acid in glycine solution
0.48%), drop rate 0.8ml/s continues to stir, and obtains pretreated salinomycin zymotic fluid；
2) it filters：The pretreated salinomycin zymotic fluid of step 1) is squeezed plate and frame filter press by eardrum formula hydraulic pressure to carry out
Filter, obtains filter cake；
3) it squeezes：High-pressure compressing is carried out to filter cake, the pressure of high-pressure compressing is 2.0MPa, and the squeezing time is 2h, control filter
Cake is 25wt% containing water quality；
4) it is granulated：Filter cake through high-pressure compressing in step 3) is transported to SET series pair by auger and belt conveyor
Screw extruder pelletizer is pelletized, and particle obtained is dried by vibrated fluidized bed, controls 120 DEG C of inlet air temperature, row
Then 60 DEG C of air temperature is uniformly mixed by two-dimensional mixing machine, obtains salinomycin particle premix.
Comparative example 5
A kind of preparation method of salinomycin particle premix, includes the following steps：
1) it pre-processes：In 1000L salinomycins zymotic fluid (fermentation titer is 3200 μ g/mL), addition accounts for zymotic fluid quality
The carbonic acid of 0.48% sodium carboxymethyl starch, the non-ionic polyacrylamide of zymotic fluid quality 0.5%, zymotic fluid quality 4%
Calcium stirs 15 minutes, obtains pretreated salinomycin zymotic fluid；
2) it filters：The pretreated salinomycin zymotic fluid of step 1) is squeezed plate and frame filter press by eardrum formula hydraulic pressure to carry out
Filter, obtains filter cake；
3) it squeezes：High-pressure compressing is carried out to filter cake, the pressure of high-pressure compressing is 2.0MPa, and the squeezing time is 2h, control filter
Cake is 25wt% containing water quality；
4) it is granulated：Filter cake through high-pressure compressing in step 3) is transported to SET series pair by auger and belt conveyor
Screw extruder pelletizer is pelletized, and particle obtained is dried by vibrated fluidized bed, controls 120 DEG C of inlet air temperature, row
Then 60 DEG C of air temperature is uniformly mixed by two-dimensional mixing machine, obtains salinomycin particle premix.
Quality requirement according to pharmacopeia about granular preparation, to being premixed made from 3-8 of the embodiment of the present invention and comparative example 1-5
Agent carries out appearance, a granulating rate and yield and is detected respectively, as a result see the table below：
Wherein, salinomycin content × 100% in salinomycin content/zymotic fluid in yield=particle premix
As seen from the above table, pre-mixing agent appearance made from 3-8 of the embodiment of the present invention and comparative example 1-5 meets the requirements, once
Granulating rate reaches 98% or more, and yield reaches 97% or more.Change the mass ratio of sodium carboxymethyl starch and glycine, glycine
The conditions such as the water content of rate of addition, filter cake have apparent influence to the appearance of pre-mixing agent, granulating rate, a yield, premix
Agent particle occurs that caking, particle be uneven, situations, a granulating rate and the yield such as loose are decreased obviously.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
With within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention god.
Claims (10)
1. a kind of preparation method of salinomycin particle premix, which is characterized in that include the following steps：
1) it pre-processes：In salinomycin zymotic fluid, sodium carboxymethyl starch, flocculant and calcium carbonate, stirring, to zymotic fluid is added
Middle dropwise addition glycine solution, continues to stir, and obtains pretreated salinomycin zymotic fluid；
2) it filters：The pretreated salinomycin zymotic fluid of step 1) is subjected to plate compression, obtains filter cake；
3) it squeezes：High-pressure compressing is carried out to filter cake；
4) it is granulated：Filter cake through high-pressure compressing in step 3) is subjected to extruding granulation, dry, it is pre- to obtain salinomycin particle for mixing
Mixture.
2. preparation method according to claim 1, which is characterized in that flocculant described in step 1) is poly- selected from nonionic
It is one or more in acrylamide, cationic polyacrylamide, anionic polyacrylamide；The addition of the flocculant is
The 0.3-1.0wt% of zymotic fluid quality.
3. preparation method according to claim 1, which is characterized in that the addition of calcium carbonate described in step 1) is fermentation
The 3.0-5.0wt% of liquid quality.
4. preparation method according to claim 1, which is characterized in that sodium carboxymethyl starch described in step 1) and glycine
Total addition is the 0.1-0.8wt% of zymotic fluid quality；The mass ratio of the sodium carboxymethyl starch and glycine is 5-8:1.
5. preparation method according to claim 1, which is characterized in that glycine in glycine solution described in step 1)
A concentration of 0.05-0.2g/ml.
6. preparation method according to claim 1, which is characterized in that the fermentation of salinomycin zymotic fluid described in step 1) is imitated
Valence is 3000-3500 μ g/mL.
7. preparation method according to claim 1, which is characterized in that the pressure of high-pressure compressing described in step 3) is 0.5-
3.0MPa, squeezing time are 1-5h.
8. preparation method according to claim 1, which is characterized in that filter cake described in step 4) is 10- containing water quality
28wt%.
9. preparation method according to claim 1, which is characterized in that made using SET series twin-screw extruders in step 4)
Grain machine carries out extruding granulation to filter cake.
10. a kind of salinomycin particle premix prepared according to preparation method described in any one of claim 1-9.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1631365A (en) * | 2004-04-14 | 2005-06-29 | 山东鲁抗舍里乐药业有限公司 | Sodium salinomycin powder and its preparation |
| CN101884621A (en) * | 2010-06-29 | 2010-11-17 | 金河生物科技股份有限公司 | Method for preparing salinomycin particle premix |
| CN105326797A (en) * | 2015-11-10 | 2016-02-17 | 成都中牧生物药业有限公司 | Processing process for salinomycin granular preparation |
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2018
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1631365A (en) * | 2004-04-14 | 2005-06-29 | 山东鲁抗舍里乐药业有限公司 | Sodium salinomycin powder and its preparation |
| CN101884621A (en) * | 2010-06-29 | 2010-11-17 | 金河生物科技股份有限公司 | Method for preparing salinomycin particle premix |
| CN105326797A (en) * | 2015-11-10 | 2016-02-17 | 成都中牧生物药业有限公司 | Processing process for salinomycin granular preparation |
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