CN108358979A - The purification process of safe ten thousand rhzomorphs - Google Patents
The purification process of safe ten thousand rhzomorphs Download PDFInfo
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- CN108358979A CN108358979A CN201810494053.1A CN201810494053A CN108358979A CN 108358979 A CN108358979 A CN 108358979A CN 201810494053 A CN201810494053 A CN 201810494053A CN 108358979 A CN108358979 A CN 108358979A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H17/00—Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
- C07H17/04—Heterocyclic radicals containing only oxygen as ring hetero atoms
- C07H17/08—Hetero rings containing eight or more ring members, e.g. erythromycins
Abstract
The present invention provides the purification process of safe ten thousand rhzomorphs, and this method is using safe ten thousand rhzomorphs of tartaric acid as raw material after water dissolution, organic solvent to be added, is adjusted to suitable pH value, safe ten thousand rhzomorphs is made to enter organic phase, organic phase stands crystallization after being concentrated under reduced pressure；Dry after separation of solid and liquid, solid is dissolved with organic solvent, adds dissolved agent, controls mixing speed and temperature carries out secondary crystallization to get safe ten thousand rhzomorph fine work.This method can be effectively removed impurity, overcome the problem that product purity is low made from existing safe ten thousand rhzomorphs purifying technique.Using safe ten thousand rhzomorph purity made from the method for the present invention 97% or more.
Description
Technical field
The present invention relates to chemical fields, specifically, being related to the purification process of safe ten thousand rhzomorphs.
Background technology
Safe ten thousand rhzomorphs are also known as super tylosin, chemical entitled 3-O- acetyl -4 "-O- isovaleryl tylosins are livestock and poultry
Special antibiotic.Safe ten thousand rhzomorphs are that tylosin turns through heat-resisting streptomycete (Streptomyces thermotolerans) biology
Change, in the novel macrolide antibiotic that 3 acetylations and 4 " position isoamyls are acylated, makes because its chemical constitution changes
It is in antimicrobial spectrum, antibacterial activity, drug resistance, chemical stability, oral absorptivity and blood concentration etc. and tylosin phase
Compare with apparent advantage.
It is (i.e. safe that CN101381756A discloses a kind of Methods For Purification super tylosin carrying the heavy secondary crystallization of alkali using acid
Ten thousand rhzomorphs) method, since ten thousand rhzomorphs of Thailand contain that the similar substance of structure is more, and acid carry alkali sink secondary crystallization method to knot
Structure analog is selectively low, therefore cannot be removed effectively the similar related substances of structure by this method, therefore this method obtains
Ten thousand rhzomorph purity of Thailand be only 81-83%, purity is relatively low.Similarly, it is different to disclose a kind of tartaric acid acetyl by CN102659882A
The method of purification of valeryl tylosin (i.e. safe ten thousand rhzomorphs), due to also being purified by the way of soda acid displacement, there is also not
The shortcomings that analogue can be efficiently separated, obtained ten thousand rhzomorph purity highest of Thailand are also only 92.1%.
Either safe ten thousand rhzomorphs or safe ten thousand rhzomorphs of tartaric acid that above two method obtains, purity is all relatively low, due to
Impurity is excessively high, it is impossible to be used in the high-quality veterinary products such as injection, and since impurity is excessive, easily causes product quality and is difficult to completely
The problem of foot production needs.
CN104610403A discloses a kind of method using safe ten thousand rhzomorphs of purified on silica, and this method is with column chromatography
Silica gel is separating medium, and 97% or more can be reached by preparing safe ten thousand rhzomorph product purities.But due to the use of the preparation of column chromatography
Method, production technology is complicated, is not easy to industrial production, and production cost is high, product preparative-scale is few, cannot meet extensive life
The needs of production；And be difficult to improve purity due to the means of column chromatography and take into account the yield of purified product simultaneously, city cannot be met
Field application demand.
Invention content
The object of the present invention is to provide a kind of new methods using safe ten thousand rhzomorphs of purified by crystallisation, to overcome existing safe ten thousand bacterium
The too low problem of product purity made from plain purifying technique.
In order to realize that the object of the invention, safe ten thousand rhzomorphs purification process provided by the invention are original with safe ten thousand rhzomorphs of tartaric acid
Material is added organic solvent, is adjusted to suitable pH value after water dissolution, and safe ten thousand rhzomorphs is made to enter organic phase, and organic phase decompression is dense
Crystallization is stood after contracting；Dry after separation of solid and liquid, solid is dissolved with organic solvent, adds dissolved agent, controls mixing speed and temperature
Degree carries out secondary crystallization to get safe ten thousand rhzomorph fine work.
It the described method comprises the following steps：
(1) add 5-20m milliliters of water dissolutions in the safe ten thousand rhzomorph raw materials of m grams of tartaric acid, decolourize, obtain solution I；
(2) 5-20m milliliters of organic solvent is added into solution I, it is quiet after stirring with lye tune system pH to 3.0-5.5
Liquid separation is set, organic phase obtains solution II through being dried；
(3) solution II is concentrated into 1-4m milliliters, is cooled to 0-10 DEG C, stand crystallization 1-16h through filtering；Then it filters, uses
0.5-2m milliliters of cold organic solvent filter wash cakes obtain safe ten thousand rhzomorphs crude product then by filtration cakes torrefaction；
(4) 2-5m milliliter organic solvents are added into safe ten thousand rhzomorph crude products, are heated to 40-60 DEG C, stir to being completely dissolved,
Then 7-10m milliliters of dissolved agent are added, then 0-15 DEG C of stirring and crystallizing filters, agent filter wash cake, filter cake are analysed with 1-2m milliliters of cold cuts
After drying to get safe ten thousand rhzomorph fine work.
Preferably, step (1) is specially：Safe ten thousand rhzomorphs of m grams of tartaric acid add 5-20m milliliters of water dissolutions, and 0.3- is then added
0.5m aluminium oxide filters after stirring 0.5-3h, obtains solution I.
Preferably, step (2) is specially：5-20m milliliters of organic solvent is added into solution I, with 20% sodium hydroxide
Or potassium hydroxide solution tune system pH to 3.0-5.5, stand liquid separation after stirring, take organic phase, into organic phase be added 2-3m without
Aqueous sodium persulfate filters after standing 0.5-1h, obtains solution II.
Preferably, in step (3) and (4), filter cake is dry under the conditions of 40-60 DEG C.
Further, it the described method comprises the following steps：
1) in the safe ten thousand rhzomorph raw materials of m grams of tartaric acid plus 5-20m milliliter water dissolutions, temperature is controlled at 20-60 DEG C, rotating speed 50-
300rpm stirs 0.5-2h；
2) 0.3-0.5m aluminium oxide is added in above-mentioned solution, is filtered after stirring 0.5-3h；
3) 5-20m milliliters of organic solvents are added in above-mentioned filtrate, 20% sodium hydroxide or potassium hydroxide solution tune is added dropwise
System pH to 3.0-5.5, is stirred for 0.5-2h；Liquid separation after standing, take it is organic be added to 2-3m anhydrous sodium sulfates, stand 0.5-1h
After filter；
4) filtrate decompression is concentrated into 1-4m milliliters, is cooled to 0-10 DEG C, is filtered after standing crystallization 1-16h；
5) 0.5-2m milliliters of cold organic solvent filter wash cakes are used, wet cake is obtained；
6) wet cake dry 10-30h under the conditions of 40-60 DEG C, obtains safe ten thousand rhzomorphs crude product；
7) 2-5m milliliters of organic solvents are added into safe ten thousand rhzomorph crude products, are heated to 40-60 DEG C, rotating speed 50-300rpm is stirred
It mixes to being completely dissolved；
8) 7-10m milliliter dissolved agent are added into step 7) acquired solution, temperature is controlled at 0-15 DEG C, rotating speed 50-
300rpm stirring and crystallizing 0.5-6h, then filter；
9) it uses 1-2m milliliters of cold cuts to analyse agent filter wash cake, obtains wet cake；
10) wet cake dries 10-30h to get safe ten thousand rhzomorph fine work under the conditions of 40-60 DEG C.
If without specified otherwise, the condition being concentrated under reduced pressure in the present invention is：- 0.08-0.095MPa, 40-60 DEG C of temperature.
Organic solvent of the present invention is selected from least one of ethyl acetate, butyl acetate, benzene, toluene.
Dissolved agent of the present invention is selected from least one of methyl tertiary butyl ether(MTBE), ether, petroleum ether.
The content of safe ten thousand rhzomorphs of the raw materials used in the present invention mesotartaric acid is 80% or more.Safe ten thousand rhzomorphs of the tartaric acid are resistance to
The tartrate for ten thousand rhzomorph of Thailand that hot streptomycete (Streptomyces thermotolerans) fermenting and producing obtains, related wine
The production method of safe ten thousand rhzomorphs of stone acid is referring to CN201710673410.6 and CN201310265454.7 and US4522919.
Using above-mentioned method of purification, obtained ten thousand rhzomorph product purity of Thailand is 97% or more.
By above-mentioned technical proposal, the present invention at least has following advantages and advantageous effect：
Compared with the prior art, safe ten thousand rhzomorphs purification process provided by the invention does not use silica gel column chromatography purification process,
Operation is simpler, it is easier to meet the needs of large-scale production, while the product purity for solving prior art preparation low is asked
Topic, 97% or more, the purity than existing purification process is significantly improved ten thousand rhzomorph purity of Thailand after purification.
Specific implementation mode
The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..Unless otherwise specified, embodiment
Used in the conventional means that are well known to those skilled in the art of technological means, raw materials used is commercial goods.
The purification process of safe ten thousand rhzomorphs of embodiment 1
It is 84.1% tartaric acid Thailand, ten thousand rhzomorph 100g to weigh purity, and 2000mL water is added, and keeps 25 DEG C of temperature, is with speed
80 revs/min of mechanical agitation is at the uniform velocity stirred, mixing time 1 hour.30g aluminium oxide is added, system is muddy, is in light brown Huang
Color.After stirring decoloration 1 hour, filters, obtain light yellow transparent solution.2000mL butyl acetates are added, it is molten with 20% sodium hydroxide
It is stirred 0.5 hour after liquid tune pH=4.6, pH stabilization, stands liquid separation.300g anhydrous sodium sulfates are added in butyl acetate phase, it is dry
It is filtered after 0.5 hour, filtrate is concentrated under reduced pressure into 400mL in vacuum degree 0.085-0.090Mpa, 45 DEG C, is transferred in refrigerator (4 DEG C of left sides
It is right) it stands overnight.Filter, wash filter cake with 4 DEG C or so of butyl acetates of 50mL, be transferred in vacuum drying chamber dry (-
0.1Mpa, 60 DEG C, 20 hours), obtain white ten thousand rhzomorph crude product 40.2g of Thailand.
White crystal 40.2g is added in 300mL butyl acetates, stirring and dissolving at 40 DEG C.700mL methyl tertbutyls are added
Ether is transferred in constant-temperature circulating device, -5 DEG C of outer temperature, at the uniform velocity mechanical agitation is carried out with 80 revs/min of speed, after stirring 2 hours
Filter, with 4 DEG C or so cold methyl tertiary butyl ether(MTBE) filter wash cakes of 100mL, wet cake be transferred in vacuum drying chamber it is dry (- 0.1Mpa,
60 DEG C, 10 hours), white crystal 30.9g is obtained, safe ten thousand rhzomorph purity are 97.5%.
The purification process of safe ten thousand rhzomorphs of embodiment 2
The ten thousand rhzomorph 300g of tartaric acid Thailand that purity is 84.5% are weighed, 5600mL water is added, keeps 25 DEG C of temperature, uses speed
Mechanical agitation for 100 revs/min is at the uniform velocity stirred, mixing time 1.5 hours.150g aluminium oxide is added, system is muddy, is in
Light brown yellow.After stirring decoloration 1 hour, filters, obtain yellow transparent solution.6000mL toluene is added, it is molten with 20% sodium hydroxide
It is stirred 0.5 hour after liquid tune pH=3.7, pH stabilization, stands liquid separation.600g anhydrous sodium sulfates are added in toluene phase, dry 0.5 is small
When after filter, filtrate is concentrated under reduced pressure into 800mL in vacuum degree 0.085-0.090Mpa, 50 DEG C, and it is quiet to be transferred in refrigerator (4 DEG C or so)
It sets overnight.Filter, wash filter cake with 4 DEG C or so of toluene of 150mL, be transferred in vacuum drying chamber dry (- 0.1Mpa, 60 DEG C,
26 hours), obtain white ten thousand rhzomorph crude product 147.7g of Thailand.
White crystal 147.7g is added in 700mL toluene, stirring and dissolving at 60 DEG C.2500mL petroleum ethers are added, are transferred to
In constant-temperature circulating device, -2 DEG C of outer temperature carries out at the uniform velocity mechanical agitation with 110 revs/min of speed, and stirring filters after 3.5 hours,
With 4 DEG C or so petroleum ether filter wash cakes of 300mL, wet cake is transferred in vacuum drying chamber dry (- 0.1Mpa, 55 DEG C, 16 hours),
White crystal 104.3g is obtained, safe ten thousand rhzomorph purity are 97.9%.
The purification process of safe ten thousand rhzomorphs of embodiment 3
It is 83.4% tartaric acid Thailand, ten thousand rhzomorph 150g to weigh purity, and 2700mL water is added, and keeps 20 DEG C of temperature, is with speed
200 revs/min of mechanical agitation is at the uniform velocity stirred, mixing time 1.5 hours.50g aluminium oxide is added, system is muddy, in palm fibre
Yellow.After stirring 1 hour, filters, obtain yellow transparent solution.2500mL toluene is added, with 20% sodium hydroxide solution tune pH=
It is stirred 1.5 hours after 4.2, pH stabilizations, stands liquid separation.400g anhydrous sodium sulfates are added in toluene phase, are taken out after 0.5 hour dry
Filter, filtrate are concentrated under reduced pressure into 600mL in vacuum degree 0.085-0.090Mpa, 55 DEG C, are transferred in refrigerator (4 DEG C or so) and stood
Night.It filters, filter cake is washed with 4 DEG C or so of toluene of 75mL, being transferred to drying in vacuum drying chamber, (- 0.1Mpa, 60 DEG C, 18 is small
When), obtain white ten thousand rhzomorph crude product 61.6g of Thailand.
White crystal 61.6g is added in 500mL butyl acetates, stirring and dissolving at 40 DEG C.1100mL ether is added, is transferred to
In constant-temperature circulating device, -12 DEG C of outer temperature carries out at the uniform velocity mechanical agitation with 170 revs/min of speed, and stirring filters after 3 hours,
With 4 DEG C or so ether filter wash cakes of 150mL, wet cake is transferred in vacuum drying chamber dry (- 0.1Mpa, 60 DEG C, 27 hours), obtains
To white crystal 49.8g, safe ten thousand rhzomorph purity are 97.2%.
The purification process of safe ten thousand rhzomorphs of embodiment 4
Ten thousand rhzomorph 100g (purity 81.5%) of tartaric acid Thailand are weighed, 1800mL water is added, temperature 50 C is kept, is with speed
150 revs/min of mechanical agitation is at the uniform velocity stirred, mixing time 1 hour.50g aluminium oxide is added, system is muddy, is in brown.
After stirring 3 hours, filters, obtain light yellow transparent solution.2000mL ethyl acetate is added, with 20% sodium hydroxide solution tune pH=
It is stirred 1.5 hours after 5.0, pH stabilizations, stands liquid separation.200g anhydrous sodium sulfates are added in ethyl acetate phase, after 0.5 hour dry
It filters, filtrate is concentrated under reduced pressure into 400mL in vacuum degree 0.085-0.090Mpa, 40 DEG C, is transferred in refrigerator (4 DEG C or so) and stood
Night.Filter, wash filter cake with 4 DEG C or so of ethyl acetate of 50mL, be transferred in vacuum drying chamber dry (- 0.1Mpa, 40 DEG C, 15
Hour), obtain white ten thousand rhzomorph crude product 45.5g of Thailand.
Crude product 45.5g is added in 400mL toluene, stirring and dissolving at 50 DEG C.800mL ether is added, is transferred to constant temperature circulating
In device, -10 DEG C of outer temperature carries out at the uniform velocity mechanical agitation with 150 revs/min of speed, and stirring filters after 2.5 hours, uses 100mL
4 DEG C or so ether filter wash cakes, wet cake are transferred in vacuum drying chamber dry (- 0.1Mpa, 40 DEG C, 21 hours), obtain white crystalline substance
Body 32.3g, safe ten thousand rhzomorph purity are 97.0%.
The purification process of safe ten thousand rhzomorphs of embodiment 5
It is 82.3% tartaric acid Thailand, ten thousand rhzomorph 300kg to weigh product purity, and 5600L water is added, and 25 DEG C of temperature is kept, with speed
Degree is at the uniform velocity stirred for 45 revs/min of mechanical agitation, mixing time 1.5 hours.150kg aluminium oxide is added, system is muddy,
In light brown yellow.After stirring decoloration 1 hour, filters, obtain yellow transparent solution.6500L toluene is added, it is molten with 20% sodium hydroxide
It is stirred 1 hour after liquid tune pH=3.65, pH stabilization, stands liquid separation.600kg anhydrous sodium sulfates are added in toluene phase, dry 1.5 is small
When after filter, filtrate is concentrated under reduced pressure into 850L in vacuum degree 0.085-0.090Mpa, 40 DEG C, cools to 4 DEG C, 10rpm stirrings 24
Hour.Filter, wash filter cake with 150L4 DEG C or so of toluene, be transferred in double cone dryer be dried in vacuo (- 0.1Mpa, 60 DEG C,
35 hours), obtain white ten thousand rhzomorph crude product 157.6kg of Thailand.
White crystal 157.6kg is added in 750L toluene, stirring and dissolving at 60 DEG C.2500L petroleum ethers, cooling is added
To -2 DEG C or so, at the uniform velocity mechanical agitation is carried out with 110 revs/min of speed, stirring filters after 3.5 hours, with 330L4 DEG C or so
Petroleum ether filter wash cake, wet cake is transferred to -0.1Mpa in vacuum double cone dryer, 55-60 DEG C, 16 hours dry, obtains white crystalline substance
Body 107.4kg, safe ten thousand rhzomorph purity are 97.1% safe ten thousand rhzomorphs.
Although above the present invention is described in detail with a general description of the specific embodiments,
On the basis of the present invention, it can be modified or is improved, this will be apparent to those skilled in the art.Cause
This, these modifications or improvements, belong to the scope of protection of present invention without departing from theon the basis of the spirit of the present invention.
Claims (10)
1. the purification process of safe ten thousand rhzomorphs, which is characterized in that using safe ten thousand rhzomorphs of tartaric acid as raw material, after water dissolution, addition has
Solvent is adjusted to suitable pH value, and safe ten thousand rhzomorphs is made to enter organic phase, and organic phase stands crystallization after being concentrated under reduced pressure；Solid-liquid point
From rear drying, solid is dissolved with organic solvent, adds dissolved agent, control mixing speed and temperature carry out secondary crystallization to get
Safe ten thousand rhzomorph fine work.
2. according to the method described in claim 1, it is characterized by comprising the following steps：
(1) add 5-20m milliliters of water dissolutions in the safe ten thousand rhzomorph raw materials of m grams of tartaric acid, decolourize, obtain solution I；
(2) 5-20m milliliters of organic solvent is added into solution I, with lye tune system pH to 3.0-5.5, stands and divides after stirring
Liquid, organic phase obtain solution II through being dried；
(3) solution II is concentrated into 1-4m milliliters, is cooled to 0-10 DEG C, stand crystallization 1-16h through filtering；Then it filters, uses 0.5-
2m milliliters of cold organic solvent filter wash cakes obtain safe ten thousand rhzomorphs crude product then by filtration cakes torrefaction；
(4) 2-5m milliliters of organic solvents are added into safe ten thousand rhzomorph crude products, are heated to 40-60 DEG C, stir to being completely dissolved, then
7-10m milliliters of dissolved agent are added, then 0-15 DEG C of stirring and crystallizing filters, analyse agent filter wash cake with 1-2m milliliters of cold cuts, filter cake is through dry
To get safe ten thousand rhzomorph fine work after dry.
3. according to the method described in claim 2, it is characterized in that, step (1) is specially：Safe ten thousand rhzomorphs of m grams of tartaric acid add 5-
Then 0.3-0.5m aluminium oxide is added in 20m milliliters of water dissolutions, filtered after stirring 0.5-3h, obtain solution I.
4. according to the method described in claim 2, it is characterized in that, step (2) is specially：5-20m milliliters are added into solution I
Organic solvent stood liquid separation with 20% sodium hydroxide or potassium hydroxide solution tune system pH to 3.0-5.5 after stirring, taken
2-3m anhydrous sodium sulfates are added into organic phase for machine phase, are filtered after standing 0.5-1h, obtain solution II.
5. according to the method described in claim 2, it is characterized in that, in step (3) and (4), filter cake is done under the conditions of 40-60 DEG C
It is dry.
6. according to the method described in claim 2, it is characterized by comprising the following steps：
1) in the safe ten thousand rhzomorph raw materials of m grams of tartaric acid plus 5-20m milliliter water dissolutions, temperature is controlled at 20-60 DEG C, rotating speed 50-
300rpm stirs 0.5-2h；
2) 0.3-0.5m aluminium oxide is added in above-mentioned solution, is filtered after stirring 0.5-3h；
3) 5-20m milliliters of organic solvents are added in above-mentioned filtrate, 20% sodium hydroxide or potassium hydroxide solution tune system is added dropwise
PH to 3.0-5.5, is stirred for 0.5-2h；Liquid separation after standing, take it is organic be added to 2-3m anhydrous sodium sulfates, stand mistake after 0.5-1h
Filter；
4) filtrate decompression is concentrated into 1-4m milliliters, is cooled to 0-10 DEG C, is filtered after standing crystallization 1-16h；
5) 0.5-2m milliliters of cold organic solvent filter wash cakes are used, wet cake is obtained；
6) wet cake dry 10-30h under the conditions of 40-60 DEG C, obtains safe ten thousand rhzomorphs crude product；
7) 2-5m milliliters of organic solvents are added into safe ten thousand rhzomorph crude products, are heated to 40-60 DEG C, rotating speed 50-300rpm stir to
It is completely dissolved；
8) 7-10m milliliters of dissolved agent are added into step 7) acquired solution, temperature is controlled at 0-15 DEG C, and rotating speed 50-300rpm is stirred
Crystallization 0.5-6h is mixed, is then filtered；
9) it uses 1-2m milliliters of cold cuts to analyse agent filter wash cake, obtains wet cake；
10) wet cake dries 10-30h to get safe ten thousand rhzomorph fine work under the conditions of 40-60 DEG C.
7. according to claim 1-6 any one of them methods, which is characterized in that the organic solvent is selected from ethyl acetate, second
At least one of acid butyl ester, benzene, toluene.
8. according to claim 1-6 any one of them methods, which is characterized in that the dissolved agent be selected from methyl tertiary butyl ether(MTBE),
At least one of ether, petroleum ether.
9. according to claim 1-6 any one of them methods, which is characterized in that the content of safe ten thousand rhzomorphs of raw material mesotartaric acid exists
80% or more.
10. according to the method described in claim 9, it is characterized in that, ten thousand rhzomorphs of tartaric acid Thailand are heat-resisting streptomycetes
The tartrate for ten thousand rhzomorph of Thailand that (Streptomyces thermotolerans) fermenting and producing obtains.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112094305A (en) * | 2020-10-30 | 2020-12-18 | 内蒙古中牧生物药业有限公司 | Preparation process of tylosin alkali |
| CN113546155A (en) * | 2021-08-02 | 2021-10-26 | 四川成康动物药业有限公司 | Chinese and western medicine compound preparation containing tulathromycin and preparation method thereof |
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| US4092473A (en) * | 1975-08-01 | 1978-05-30 | Sanraku Ocean Co., Ltd. | Tylosin derivatives and their manufacturing process |
| CN103276031A (en) * | 2013-06-28 | 2013-09-04 | 宁夏泰瑞制药股份有限公司 | Culture medium for producing acetylisovaleryltylosin by fermenting streptomyces thermotolerans and fermentation method |
| CN103275154A (en) * | 2013-06-28 | 2013-09-04 | 宁夏泰瑞制药股份有限公司 | Preparation method of crystalline particles of acetyl isovaleryl tylosin salt |
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2018
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| US4092473A (en) * | 1975-08-01 | 1978-05-30 | Sanraku Ocean Co., Ltd. | Tylosin derivatives and their manufacturing process |
| CN103276031A (en) * | 2013-06-28 | 2013-09-04 | 宁夏泰瑞制药股份有限公司 | Culture medium for producing acetylisovaleryltylosin by fermenting streptomyces thermotolerans and fermentation method |
| CN103275154A (en) * | 2013-06-28 | 2013-09-04 | 宁夏泰瑞制药股份有限公司 | Preparation method of crystalline particles of acetyl isovaleryl tylosin salt |
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| 姬竹玲: "泰万菌素颗粒剂的研制及其在猪体内的药动学研究", 《中国优秀硕士学位论文全文数据库（电子期刊）》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112094305A (en) * | 2020-10-30 | 2020-12-18 | 内蒙古中牧生物药业有限公司 | Preparation process of tylosin alkali |
| CN112094305B (en) * | 2020-10-30 | 2022-03-11 | 内蒙古中牧生物药业有限公司 | Preparation process of tylosin alkali |
| CN113546155A (en) * | 2021-08-02 | 2021-10-26 | 四川成康动物药业有限公司 | Chinese and western medicine compound preparation containing tulathromycin and preparation method thereof |
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| CN108358979B (en) | 2020-08-25 |
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