CN106083951B - A method of utilizing kasugarnycin broth extraction kasugamycini hydrochloride - Google Patents

A method of utilizing kasugarnycin broth extraction kasugamycini hydrochloride Download PDF

Info

Publication number
CN106083951B
CN106083951B CN201610504642.4A CN201610504642A CN106083951B CN 106083951 B CN106083951 B CN 106083951B CN 201610504642 A CN201610504642 A CN 201610504642A CN 106083951 B CN106083951 B CN 106083951B
Authority
CN
China
Prior art keywords
kasugarnycin
added
kasugamycini
hydrochloride
kasugamycini hydrochloride
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201610504642.4A
Other languages
Chinese (zh)
Other versions
CN106083951A (en
Inventor
任勇
王隽梅
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Ningxia Tairui Pharmaceutical Co Ltd
Original Assignee
Ningxia Tairui Pharmaceutical Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Ningxia Tairui Pharmaceutical Co Ltd filed Critical Ningxia Tairui Pharmaceutical Co Ltd
Priority to CN201610504642.4A priority Critical patent/CN106083951B/en
Publication of CN106083951A publication Critical patent/CN106083951A/en
Application granted granted Critical
Publication of CN106083951B publication Critical patent/CN106083951B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07HSUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
    • C07H15/00Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
    • C07H15/20Carbocyclic rings
    • C07H15/207Cyclohexane rings not substituted by nitrogen atoms, e.g. kasugamycins
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07HSUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
    • C07H1/00Processes for the preparation of sugar derivatives
    • C07H1/06Separation; Purification

Abstract

The present invention relates to a kind of method using kasugarnycin broth extraction kasugamycini hydrochloride, processing step is:Kasugarnycin fermentation liquid is preprocessed, ceramic membrane filter, macroreticular resin decoloration, nanofiltration concentration, crystallizes and dries.It is compared with domestic conventional production process, reduces production cost, improve final product quality, be conducive to the domestic and international market competitiveness for enhancing product.

Description

A method of utilizing kasugarnycin broth extraction kasugamycini hydrochloride
Technical field
The invention belongs to antibiotic extractive technique fields, utilize kasugarnycin broth extraction hydrochloric acid more particularly to a kind of The method of kasugarnycin.
Background technique
Kasugarnycin is a kind of alkalescent antibiotic generated by small golden streptomysin, which is that dual-purpose antibiotic is cured in agriculture. Currently, Related domestic documents report in kasugarnycin fermentation liquid, addition oxalic acid is pre-processed, macroreticular resin technology extracts the spring The method of thunder mycin.Existing main problem is:
Oxalic acid is added in 1 kasugarnycin fermentation liquor pretreatment technique, improves production cost.
2 pertinent literatures report the method for preparing kasugarnycin, but product effective content is relatively low, are unfavorable for going out for product Mouthful.
3 pertinent literatures, which are reported, prepares kasugarnycin using the method for spray drying, and product is not easy long term storage, transport With use.
Summary of the invention
It is an object of the invention to overcome above-mentioned defect in the prior art, a kind of guarantee yield, extraction process letter are provided Single, product quality meets the method using kasugarnycin broth extraction kasugamycini hydrochloride of relevant regulations.
The technical solution taken to achieve the above object is:
A method of utilizing kasugarnycin broth extraction kasugamycini hydrochloride, it is characterised in that its processing step is:
1)Fermentation liquor pretreatment
It by kasugarnycin fermentation liquid tune pH 4.5-5, is sufficiently stirred and stands, continue to adjust pH to 2.5-3, again sufficiently It stirs and stands;Then polysilicate aluminum chloride calcium is added, is sufficiently stirred and stands;
2)Ceramic membrane filter
By pretreated fermentation liquid, viscosity is brought down below 3000Pas, after be warming up to 50-55 DEG C, then using high speed Cross-current flow carries out ceramic membrane filter, collects filtrate;
In filter process, pressure is controlled in 0.2-0.3MPa, and flow control is in 0.5~0.9m3/m2.h.
When fermentating liquid volume is down to 35%, drinking water is added, control fermentating liquid volume is 35-40%, and total amount is added in drinking water For the 60-70% of fermentating liquid volume.Film filtering terminates, and collects filtrate.
3)Macroreticular resin decoloration
Through process 2)Gained filtrate temperature is controlled at 35-40 DEG C, with macroreticular resin decolorization;
4)Nanofiltration concentration
By process 2)Gained macroreticular resin de-inking solution temperature is controlled at 40-45 DEG C, carries out nanofiltration concentration;
5)Crystallization
Nanofiltration solution temperature is down to 0-5 DEG C, organic solvent is added in speed of agitator control in 30-50r/min, solution, Crystal seed is added when there is crystallization situation in 13-15ml/min in flow control, continues to stir 120-150min, stirring terminates, quiet 150-180min is set, is then filtered, wet solid kasugamycini hydrochloride is obtained;
6)Drying.
The process 1)In, adjustment pH uses mass concentration for the hydrochloric acid solution of 20-30%.
The process 1)In, mixing time 20-30min stands 40-80min.
The process 1)In, polysilicate aluminum chloride calcium dosage is the 0.01-0.03% of fermentating liquid volume.
The process 2)In, during ceramic membrane filter, pressure control in 0.2-0.3MPa, flow control 0.5~ 0.9m3/m2.h;
When fermentating liquid volume is down to 35%, drinking water is added, control fermentating liquid volume is 35-40%, and total amount is added in drinking water For the 60-70% of fermentating liquid volume.
The process 2)In, ceramic membrane is porous ceramic film, and port number 37, material is silica, pore size filter specification It is 0.2 μm.
The process 3)In, macroreticular resin is D941 anion decolorizing resin, and material is divinylbenzene, and resin column is through high ratio It is 1: 6-7, charging rate control is controlled in 2-2.5BV/h, discharging speed in 1.1-1.5BV/h.
The process 4)In, when nanofiltration is concentrated, pressure is controlled in 0.5-1MPa, and solution is concentrated into the 40- of original solution volume 50%, the material of nanofiltration membrane used is polyvinyl alcohol, and nanofiltration membrane component is hollow fiber form.
The process 5)In, organic solvent is acetone or methanol or ethyl alcohol or propyl alcohol or isopropanol, dosage are:V is organic molten Agent:V filtrate=4-6:1.
The process 5)In, crystal seed is kasugamycini hydrochloride sterling, and dosage is the 0.01-0.02% of liquor capacity.
The process 6)In, it is dry to use double conic rotary vacuum dryer, 60~80 DEG C of drying temperature, vacuum degree is- 0.02~-0.08 MPa, 12~15h of drying time.
The technology of the present invention advantage is embodied in:
1 present invention replaces conventional oxalic acid preprocess method using membrane filtering method, effectively improves kasugarnycin fermentation liquid Pretreated yield, reduces production cost.
2 extract kasugarnycin using method of the invention, and effective content has reached 98% or more.
3 extract kasugarnycin using method of the invention, wherein 70% or more kasugarnycin product cut size reaches 50um, product is convenient for storage and long-distance transport.
Specific embodiment
The present invention will be described below by way of examples, it should be understood that example is for illustrating rather than to this The limitation of invention.The scope of the present invention is determined with core content according to claims.
Kasugarnycin fermentation liquid source in following embodiments:
The acquisition of kasugarnycin fermentation liquid:Use proprietary streptomyces microaureus for producing strains, with low temperature soybean cake powder, ferment The raw material such as female powder, glucose are configured to fermentation culture, through three grade fermemtation biosynthesis kasugarnycin.
Ceramic membrane is porous ceramic film, and port number 37, material is silica, and pore size filter specification is 0.2 μm.
Macroreticular resin is D941 anion decolorizing resin, and material is divinylbenzene, and resin column is through height than being 1: 6-7.
The material of nanofiltration membrane is polyvinyl alcohol, and nanofiltration membrane component is hollow fiber form.
Crystal seed is kasugamycini hydrochloride sterling, and dosage is the 0.01-0.02% of liquor capacity.
Embodiment 1
Kasugarnycin fermentation liquid 100m3, chemical titer 15201u/ml.
1)Fermentation liquor pretreatment
Kasugarnycin fermentation liquid pH to 5 is adjusted using 20% hydrochloric acid solution, 20min is stirred, stands 40min;Continue to adjust Kasugarnycin fermentation liquid pH to 3 stirs 20min, stands 40min.
Polysilicate aluminum chloride calcium 100kg is added in fermentation liquid, continues to stir 20min, stands 60min.
2)Ceramic membrane filter
Drinking water is added in pretreated fermentation liquid, viscosity is down to 2943Pas, and fermentation liquid is warming up to 50 DEG C.
In membrane filtration processes, film filtering is carried out using high speed cross-current flow, in filter process, pressure is controlled in 0.2- 0.3MPa, flow control is in 0.5m3/m2.h。
When fermentating liquid volume is down to 35%, drinking water is added, control fermentating liquid volume is 35-40%, and total amount is added in drinking water It is the 60% of fermentating liquid volume.
Film filtering terminates, and collects 150 m of kasugarnycin filtrate3, chemical titer 7150u/ml.
3)Macroreticular resin decoloration
Filtrate temperature is warming up to 35 DEG C, through macroreticular resin decolorization, it is desirable that resin column is 1: 6 through height ratio, charging rate Control is controlled in 2BV/h, discharging speed in 1.1BV/h.
Filtering terminates, and collects 149 m of kasugarnycin filtrate3
4)Nanofiltration concentration
It controls through macroreticular resin de-inking solution temperature at 40 DEG C, carries out nanofiltration, pressure is controlled in 0.5MPa.Nanofiltration terminates, Filtrate volume is 60 m3
5)Crystallization
It is down to 0 DEG C through nanofiltration solution temperature, organic solvent-acetone is added in speed of agitator control in 30r/min, solution 240m3, flow control is in 13ml/min, and when there is crystallization situation, addition crystal seed kasugamycini hydrochloride sterling 6kg continues to stir 120min.Stirring terminates, and stands 150min, then filters, obtain wet solid kasugamycini hydrochloride.
6)It is dry
Wet solid kasugamycini hydrochloride puts into double conic rotary vacuum dryer, and temperature rises to 60 DEG C, and control vacuum degree is- 0.02~-0.08 MPa, dry 15h.It is dry to terminate to obtain kasugamycini hydrochloride 995kg.Through detecting, effective content 98.7%; 74% kasugarnycin product cut size has reached 50um.
Embodiment 2
Kasugarnycin fermentation liquid 100m3, chemical titer 14936u/ml.
1)Fermentation liquor pretreatment
Kasugarnycin fermentation liquid pH to 4.8 is adjusted using 22% hydrochloric acid solution, 22min is stirred, stands 45min;Continue to adjust Kasugarnycin fermentation liquid pH to 2.8 is saved, 22min is stirred, stands 45min.
Polysilicate aluminum chloride calcium 150kg is added in fermentation liquid, continues to stir 22min, stands 65min.
2)Ceramic membrane filter
Drinking water is added in pretreated fermentation liquid, viscosity is down to 2893Pas, and fermentation liquid is warming up to 52 DEG C.
In membrane filtration processes, film filtering is carried out using high speed cross-current flow, in filter process, pressure is controlled in 0.2- 0.3MPa, flow control is in 0.6m3/m2.h。
When fermentating liquid volume is down to 35%, drinking water is added, control fermentating liquid volume is 35-40%, and total amount is added in drinking water It is the 62% of fermentating liquid volume.
Film filtering terminates, and collects kasugarnycin filtrate 155m3, chemical titer 6893u/ml.
3)Macroreticular resin decoloration
Filtrate temperature is warming up to 36 DEG C, through macroreticular resin decolorization, it is desirable that for resin column through height than being 1: 6.2, charging is fast Degree control is controlled in 2.2BV/h, discharging speed in 1.2BV/h.
Filtering terminates, and collects kasugarnycin filtrate 154m3
4)Nanofiltration concentration
It controls through macroreticular resin de-inking solution temperature at 42 DEG C, carries out nanofiltration, pressure is controlled in 0.6MPa.Nanofiltration terminates, Filtrate volume is 64.7m3
5)Crystallization
2 DEG C are down to through nanofiltration solution temperature, organic solvent methanol is added in speed of agitator control in 35r/min, solution 292m3, flow control is in 13.5ml/min, and when there is crystallization situation, crystal seed kasugamycini hydrochloride sterling 8.4kg, continuation is added Stir 130min.Stirring terminates, and stands 160min, then filters, obtain wet solid kasugamycini hydrochloride.
6)It is dry
Wet solid kasugamycini hydrochloride puts into double conic rotary vacuum dryer, and temperature rises to 65 DEG C, and control vacuum degree is- 0.02~-0.08 MPa, dry 14h.It is dry to terminate to obtain kasugamycini hydrochloride 994kg.Through detecting, effective content 98.9%; 76% kasugarnycin product cut size has reached 50um.
Embodiment 3
Kasugarnycin fermentation liquid 100m3, chemical titer 15106u/ml.
1)Fermentation liquor pretreatment
Kasugarnycin fermentation liquid pH to 4.7 is adjusted using 25% hydrochloric acid solution, 25min is stirred, stands 50min;Continue to adjust Kasugarnycin fermentation liquid pH to 2.7 is saved, 25min is stirred, stands 50min.
Polysilicate aluminum chloride calcium 200kg is added in fermentation liquid, continues to stir 25min, stands 70min.
2)Ceramic membrane filter
Drinking water is added in pretreated fermentation liquid, viscosity is down to 2851Pas, and fermentation liquid is warming up to 53 DEG C.
In membrane filtration processes, film filtering is carried out using high speed cross-current flow, in filter process, pressure is controlled in 0.2- 0.3MPa, flow control is in 0.7m3/m2.h。
When fermentating liquid volume is down to 35%, drinking water is added, control fermentating liquid volume is 35-40%, and total amount is added in drinking water It is the 65% of fermentating liquid volume.
Film filtering terminates, and collects kasugarnycin filtrate 161m3, chemical titer 6746u/ml.
3)Macroreticular resin decoloration
Filtrate temperature is warming up to 37 DEG C, through macroreticular resin decolorization, it is desirable that for resin column through height than being 1: 6.5, charging is fast Degree control is controlled in 2.3BV/h, discharging speed in 1.3BV/h.
Filtering terminates, and collects kasugarnycin filtrate 160m3
4)Nanofiltration concentration
It controls through macroreticular resin de-inking solution temperature at 43 DEG C, carries out nanofiltration, pressure is controlled in 0.5MPa.Nanofiltration terminates, Filtrate volume is 72m3
5)Crystallization
3 DEG C are down to through nanofiltration solution temperature, organic solvent ethyl alcohol is added in speed of agitator control in 40r/min, solution 360m3, flow control is in 14ml/min, and when there is crystallization situation, addition crystal seed kasugamycini hydrochloride sterling 10.8kg continues to stir Mix 135min.Stirring terminates, and stands 165min, then filters, obtain wet solid kasugamycini hydrochloride.
6)It is dry
Wet solid kasugamycini hydrochloride puts into double conic rotary vacuum dryer, and temperature rises to 70 DEG C, and control vacuum degree is- 0.02~-0.08 MPa, dry 13.5h.It is dry to terminate to obtain kasugamycini hydrochloride 994kg.Through detecting, effective content is 99.2%;79% kasugarnycin product cut size has reached 50um.
Embodiment 4
Kasugarnycin fermentation liquid 100m3, chemical titer 15002u/ml.
1)Fermentation liquor pretreatment
Kasugarnycin fermentation liquid pH to 4.6 is adjusted using 27% hydrochloric acid solution, 27min is stirred, stands 55min;Continue to adjust Kasugarnycin fermentation liquid pH to 2.6 is saved, 27min is stirred, stands 55min.
Polysilicate aluminum chloride calcium 250kg is added in fermentation liquid, continues to stir 28min, stands 75min.
2)Ceramic membrane filter
Drinking water is added in pretreated fermentation liquid, viscosity is down to 2830Pas, and fermentation liquid is warming up to 54 DEG C.
In membrane filtration processes, film filtering is carried out using high speed cross-current flow, in filter process, pressure is controlled in 0.2- 0.3MPa, flow control is in 0.8m3/m2.h。
When fermentating liquid volume is down to 35%, drinking water is added, control fermentating liquid volume is 35-40%, and total amount is added in drinking water It is the 67% of fermentating liquid volume.
Film filtering terminates, and collects kasugarnycin filtrate 164m3, chemical titer 6494u/ml.
3)Macroreticular resin decoloration
Filtrate temperature is warming up to 38 DEG C, through macroreticular resin decolorization, it is desirable that for resin column through height than being 1: 6.8, charging is fast Degree control is controlled in 2.4BV/h, discharging speed in 1.4BV/h.
Filtering terminates, and collects kasugarnycin filtrate 163m3
4)Nanofiltration concentration
It controls through macroreticular resin de-inking solution temperature at 44 DEG C, carries out nanofiltration, pressure is controlled in 0.5MPa.Nanofiltration terminates, Filtrate volume is 78m3
5)Crystallization
4 DEG C are down to through nanofiltration solution temperature, organic solvent propyl alcohol is added in speed of agitator control in 45r/min, solution 430m3, flow control is in 14.5ml/min, and when there is crystallization situation, addition crystal seed kasugamycini hydrochloride sterling 14kg continues to stir Mix 145min.Stirring terminates, and stands 175min, then filters, obtain wet solid kasugamycini hydrochloride.
6)It is dry
Wet solid kasugamycini hydrochloride puts into double conic rotary vacuum dryer, and temperature rises to 75 DEG C, and control vacuum degree is- 0.02~-0.08 MPa, dry 13h.It is dry to terminate to obtain kasugamycini hydrochloride 987kg.Through detecting, effective content 99.0%; 78% kasugarnycin product cut size has reached 50um.
Embodiment 5
Kasugarnycin fermentation liquid 100m3, chemical titer 14926u/ml.
1)Fermentation liquor pretreatment
Kasugarnycin fermentation liquid pH to 4.5 is adjusted using 30% hydrochloric acid solution, 30min is stirred, stands 60min;Continue to adjust Kasugarnycin fermentation liquid pH to 2.5 is saved, 30min is stirred, stands 60min.
Polysilicate aluminum chloride calcium 300kg is added in fermentation liquid, continues to stir 30min, stands 80min.
2)Ceramic membrane filter
Drinking water is added in pretreated fermentation liquid, viscosity is down to 2816Pas, and fermentation liquid is warming up to 55 DEG C.
In membrane filtration processes, film filtering is carried out using high speed cross-current flow, in filter process, pressure is controlled in 0.2- 0.3MPa, flow control is in 0.9m3/m2.h。
When fermentating liquid volume is down to 35%, drinking water is added, control fermentating liquid volume is 35-40%, and total amount is added in drinking water It is the 70% of fermentating liquid volume.
Film filtering terminates, and collects kasugarnycin filtrate 167m3, chemical titer 6338u/ml.
4)Macroreticular resin decoloration
Filtrate temperature is warming up to 40 DEG C, through macroreticular resin decolorization, it is desirable that resin column is 1: 7 through height ratio, charging rate Control is controlled in 2.5BV/h, discharging speed in 1.5BV/h.
Filtering terminates, and collects kasugarnycin filtrate 166m3
4)Nanofiltration concentration
It controls through macroreticular resin de-inking solution temperature at 45 DEG C, carries out nanofiltration, pressure is controlled in 0.5MPa.Nanofiltration terminates, Filtrate volume is 83m3
5)Crystallization
5 DEG C are down to through nanofiltration solution temperature, organic solvent isopropanol is added in speed of agitator control in 50r/min, solution 498m3, flow control is in 15ml/min, and when there is crystallization situation, addition crystal seed kasugamycini hydrochloride sterling 16.6kg continues to stir Mix 150min.Stirring terminates, and stands 180min, then filters, obtain wet solid kasugamycini hydrochloride.
6)It is dry
Wet solid kasugamycini hydrochloride puts into double conic rotary vacuum dryer, and temperature rises to 80 DEG C, and control vacuum degree is- 0.02~-0.08 MPa, dry 12h.It is dry to terminate to obtain kasugamycini hydrochloride 980kg.Through detecting, effective content 98.9%; 77% kasugarnycin product cut size has reached 50um.

Claims (10)

1. a kind of method using kasugarnycin broth extraction kasugamycini hydrochloride, it is characterised in that its processing step is:
1)Fermentation liquor pretreatment
With mass concentration it is 20-30% hydrochloric acid solution tune pH 4.5-5 by kasugarnycin fermentation liquid, is sufficiently stirred and stands, continues It is 20-30% hydrochloric acid solution adjustment pH to 2.5-3 with mass concentration, is sufficiently stirred and stands again;Then polysilicate aluminum chloride is added Calcium is sufficiently stirred and stands;
2)Ceramic membrane filter
By pretreated fermentation liquid, viscosity is brought down below 3000Pas, after be warming up to 50-55 DEG C, then use high speed cross-flow Mode carries out ceramic membrane filter, collects filtrate;
In filter process, pressure is controlled in 0.2-0.3MPa, and flow control is in 0.5~0.9m3/m2.h;
When fermentating liquid volume is down to 35%, drinking water is added, control fermentating liquid volume is 35-40%, and it is hair that total amount, which is added, in drinking water The 60-70% of zymotic fluid volume, film filtering terminate, and collect filtrate;
3)Macroreticular resin decoloration
Through process 2)Gained filtrate temperature is controlled at 35-40 DEG C, with macroreticular resin decolorization;
4)Nanofiltration concentration
By process 3)Gained macroreticular resin de-inking solution temperature is controlled at 40-45 DEG C, carries out nanofiltration concentration;
5)Crystallization
Nanofiltration solution temperature is down to 0-5 DEG C, organic solvent, flow velocity is added in speed of agitator control in 30-50r/min, solution Crystal seed is added when there is crystallization situation in 13-15ml/min in control, continues to stir 120-150min, and stirring terminates, and stands Then 150-180min is filtered, obtain wet solid kasugamycini hydrochloride;
6)Drying.
2. the method described in accordance with the claim 1 using kasugarnycin broth extraction kasugamycini hydrochloride, it is characterised in that The process 1)In, mixing time 20-30min stands 40-80min.
3. the method described in accordance with the claim 1 using kasugarnycin broth extraction kasugamycini hydrochloride, it is characterised in that The process 1)In, polysilicate aluminum chloride calcium dosage is the 0.01-0.03% of fermentating liquid volume.
4. the method described in accordance with the claim 1 using kasugarnycin broth extraction kasugamycini hydrochloride, it is characterised in that The process 2)In, during ceramic membrane filter, pressure is controlled in 0.2-0.3MPa, and flow control is in 0.5~0.9m3/m2.h;
When fermentating liquid volume is down to 35%, drinking water is added, control fermentating liquid volume is 35-40%, and it is hair that total amount, which is added, in drinking water The 60-70% of zymotic fluid volume.
5. according to, using the method for kasugarnycin broth extraction kasugamycini hydrochloride, feature exists described in claim 1 or 4 In the process 2)In, ceramic membrane is porous ceramic film, and port number 37, material is silica, and pore size filter specification is 0.2 μ m。
6. the method described in accordance with the claim 1 using kasugarnycin broth extraction kasugamycini hydrochloride, it is characterised in that The process 3)In, macroreticular resin is D941 anion decolorizing resin, and material is divinylbenzene, and it is 1: 6-7 that resin column diameter height, which compares, Charging rate control is controlled in 2-2.5BV/h, discharging speed in 1.1-1.5BV/h.
7. the method described in accordance with the claim 1 using kasugarnycin broth extraction kasugamycini hydrochloride, it is characterised in that The process 4)In, when nanofiltration is concentrated, pressure is controlled in 0.5-1MPa, and solution is concentrated into the 40-50% of original solution volume, used The material of nanofiltration membrane is polyvinyl alcohol, and nanofiltration membrane component is hollow fiber form.
8. the method described in accordance with the claim 1 using kasugarnycin broth extraction kasugamycini hydrochloride, it is characterised in that The process 5)In, organic solvent is acetone or methanol or ethyl alcohol or propyl alcohol or isopropanol, dosage are:V organic solvent:V filtrate= 4-6:1。
9. the method described in accordance with the claim 1 using kasugarnycin broth extraction kasugamycini hydrochloride, it is characterised in that The process 5)In, crystal seed is kasugamycini hydrochloride sterling, and dosage is the 0.01-0.02% of liquor capacity.
10. the method described in accordance with the claim 1 using kasugarnycin broth extraction kasugamycini hydrochloride, it is characterised in that The process 6)In, dry to use double conic rotary vacuum dryer, 60~80 DEG C of drying temperature, vacuum degree is -0.02~-0.08 MPa, 12~15h of drying time.
CN201610504642.4A 2016-07-01 2016-07-01 A method of utilizing kasugarnycin broth extraction kasugamycini hydrochloride Active CN106083951B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610504642.4A CN106083951B (en) 2016-07-01 2016-07-01 A method of utilizing kasugarnycin broth extraction kasugamycini hydrochloride

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610504642.4A CN106083951B (en) 2016-07-01 2016-07-01 A method of utilizing kasugarnycin broth extraction kasugamycini hydrochloride

Publications (2)

Publication Number Publication Date
CN106083951A CN106083951A (en) 2016-11-09
CN106083951B true CN106083951B (en) 2018-11-27

Family

ID=57214725

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610504642.4A Active CN106083951B (en) 2016-07-01 2016-07-01 A method of utilizing kasugarnycin broth extraction kasugamycini hydrochloride

Country Status (1)

Country Link
CN (1) CN106083951B (en)

Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107033199A (en) * 2017-06-02 2017-08-11 浙江省桐庐汇丰生物科技有限公司 A kind of solid-liquid separating method of kasugarnycin zymotic fluid
CN107459542A (en) * 2017-10-10 2017-12-12 宁夏泰瑞制药股份有限公司 A kind of method that gentamicinC is produced using gentamicinC zymotic fluid
CN107987110A (en) * 2017-12-15 2018-05-04 陕西麦可罗生物科技有限公司 A kind of desalination process of kasugarnycin concentrate
CN108822167A (en) * 2018-07-24 2018-11-16 陕西麦可罗生物科技有限公司 A kind of raising kasugarnycin content method
CN110357934A (en) * 2019-07-31 2019-10-22 陕西麦可罗生物科技有限公司 A kind of process reducing kasugarnycin production process sewage quantity
CN110452275B (en) * 2019-09-17 2023-04-07 陕西绿盾环境工程研究院有限公司 Preparation method of high-purity kasugamycin
CN117645640A (en) * 2023-08-03 2024-03-05 陕西麦可罗生物科技有限公司 Compound hydrochloride crystal form and application thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3607657A (en) * 1963-12-28 1971-09-21 Hamao Umezawa Process for the production of kasugamycin
CN102250165A (en) * 2011-06-03 2011-11-23 陕西绿盾生物制品有限责任公司 Preparation method of technical grade kasumin
CN104770369A (en) * 2015-04-23 2015-07-15 山西新源华康化工股份有限公司 Kasugamycin water-aqua extracting process

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3607657A (en) * 1963-12-28 1971-09-21 Hamao Umezawa Process for the production of kasugamycin
CN102250165A (en) * 2011-06-03 2011-11-23 陕西绿盾生物制品有限责任公司 Preparation method of technical grade kasumin
CN104770369A (en) * 2015-04-23 2015-07-15 山西新源华康化工股份有限公司 Kasugamycin water-aqua extracting process

Also Published As

Publication number Publication date
CN106083951A (en) 2016-11-09

Similar Documents

Publication Publication Date Title
CN106083951B (en) A method of utilizing kasugarnycin broth extraction kasugamycini hydrochloride
CN103923140B (en) The preparation method of a kind of tartrate acetylisovaleryl tylosin
US9708356B2 (en) Method for manufacturing monosaccharides, oligosaccharides, and furfurals from biomass
CN110396188B (en) Post-extraction method for producing epsilon-polylysine by fermentation method
CN102040476B (en) Method for separating and purifying 1,3-propylene glycol from fermentation liquor
CN109081844B (en) Method for extracting spectinomycin from fermentation culture
EP4299578A1 (en) Method for co-producing erythritol and arabinose from xylose mother liquor
CN102675172A (en) Preparation method of tiamulin base
CN112158865A (en) Method for recycling lithium element in lithium precipitation mother liquor
CN108947809B (en) Method for extracting and refining long-chain dicarboxylic acid from fermentation liquor
CN104263793A (en) Method for treating crystalline dextrose mother liquid
CN103361385B (en) Technology for preparation of succinic acid finished product by bioconversion of cassava raw material
CN105131091A (en) Method for preparing capreomycin sulfate from capreomycin broth
CN103804173B (en) A kind of process for purification of fermentation organic acid
CN109553645B (en) Method for extracting low-content erythromycin A in fermentation solution
CN103420826A (en) Method for extracting succinic acid from fermentation broth
CN103343147B (en) Method for preparing dibutyl succinate from cassava raw materials
CN104789607A (en) Method for preparing lactic acid and/or lactate through fermentation-separation coupling
CN115231990A (en) Preparation method of high-purity dipentaerythritol
CN101492366B (en) Method for extracting allomaleic acid from fermentation liquor
CN107586310B (en) Extraction process of flavomycin
CN107459542A (en) A kind of method that gentamicinC is produced using gentamicinC zymotic fluid
CN112430634A (en) Process for preparing L-tryptophan by fermentation method
CN102060688B (en) Continuous thermal crystallization extraction method of itaconic acid
CN106008625B (en) A method of preparing Maduramicin Ammonium using Madumycin zymotic fluid

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant