CN105131091A - Method for preparing capreomycin sulfate from capreomycin broth - Google Patents
Method for preparing capreomycin sulfate from capreomycin broth Download PDFInfo
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- CN105131091A CN105131091A CN201510456953.3A CN201510456953A CN105131091A CN 105131091 A CN105131091 A CN 105131091A CN 201510456953 A CN201510456953 A CN 201510456953A CN 105131091 A CN105131091 A CN 105131091A
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Abstract
The invention relates to a method for preparing capreomycin sulfate from capreomycin broth. The method comprises pretreatment on capreomycin broth, plate filtration, dilution, pH adjustment, macroporous resin adsorption decoloring, crystallization and drying. The method realizes stable and high efficiency production of capreomycin sulfate from bulk drugs, improves a capreomycin sulfate extraction yield, shortens a production cycle, reduces a cost and improves a yield.
Description
Technical field
The invention belongs to microbiotic extraction, synthesis technical field, particularly relate to a kind of method utilizing capromycin fermented liquid to prepare capreomycin sulfate.
Background technology
Capromycin (CPM) is the ring type polypeptide class microbiotic produced by curling streptomycete fermentation, by the active compound of 4 structural similitudies---IA, IB, IIA and IIb form, wherein the content of IA and IB accounts for 80% ~ 90%, is the principal constituent playing curative effect.CPM is made generally in vitriol, and clinical application is in tuberculosis field.
At present, according to pertinent literature report, the production technique of domestic raw materials medicine capreomycin sulfate mainly contains two kinds:
Technique one: mainly peracid for capromycin fermentation liquor, ion-exchange, activated carbon decolorizing, thin film concentration, mocromembrane filtration and spraying dry are obtained its esters product, its subject matter existed:
1) extraction cost is high.Employ expensive oxalic acid in leaching process, and have employed membrane filtration technique and ion exchange technique, cause extraction cost high.
2) the extraction process cycle is long, has exceeded 70h.
3) extract yield is low, generally 70 ~ 75%.
Technique two: adopt membrane filtering method to extract capromycin, wherein, microfiltration membrane material is ceramic membrane, for fermentation liquor treatment; Nanofiltration membrane material is rolling poly (ether sulfone) film, concentrates for the exquisite liquid of capromycin; Ultra-filtration membrane material is polysulfone membrane, for removing the bacterial endotoxin in concentrated solution; Drying process with atomizing is adopted to obtain capromycin.Its subject matter existed is that the production cycle is long, and membrane filter plant regularly need carry out care and maintenance, causes production cost high.
Summary of the invention
Object of the present invention is just the defect overcoming above-mentioned prior art, provides one effectively to improve extract yield, reduces costs, and shortens the production cycle, realizes the capromycin fermented liquid that utilizes that is stable, High-efficient Production and prepares the method for capreomycin sulfate.
Technical scheme taked for achieving the above object is:
A kind of method utilizing capromycin fermented liquid to prepare capreomycin sulfate, it is characterized in that its processing step is: first capromycin fermented liquid is carried out pre-treatment, then Plate Filtration, gained filtrate is diluted to tiring of capromycin and adjusts filtrate pH to 5.0 ~ 6.0 after 7000 ~ 8000u/ml, decolour by macroporous resin adsorption, collect the adsorption bleaching filtrate of the > 4000u/ml that tires, crystallization, dry;
Above-mentioned preprocessing process is:
1) under mixing speed 30 ~ 50r/min, first regulate capromycin fermented liquid pH to 5.0 ~ 5.5 with phosphoric acid solution, stir 40 ~ 60min, rear continuation phosphorus acid for adjusting pH to 4.0 ~ 4.5, stir 30 ~ 60min, then regulate pH to 7.5 ~ 8.0 with sodium carbonate solution, stir 20 ~ 40min;
2) under mixing speed 100 ~ 120r/min, add microbial flocculant (JT-613), after stirring 1 ~ 3min, rotating speed is down to 30 ~ 50r/min, after stirring 20 ~ 30min, leave standstill 40 ~ 60min;
3) add flocculating aids, stir 20 ~ 40min.
After Plate Filtration, with filter residue in water cleaning sheet frame, collect water lotion, when potency unit is lower than 500 μ/ml, stop washing, by filtrate and water lotion mixing.
Filtrate concentration after Plate Filtration is the sulfuric acid adjustment pH of 10 ~ 30%.
Described macroporous resin adsorption decolorization is: first the filtrate of the Plate Filtration of pH5.0 ~ 6.0 is warming up to 30 ~ 35 DEG C, enters macroporous adsorbent resin equipment with 12 ~ 15ml/min flow velocity; Collect the filtrate through macroporous resin adsorption, flow rate control, at 14 ~ 16ml/min, through the > 4000u/ml that tires of macroporous resin adsorption filtrate, starts to collect filtrate.
Blade diameter length ratio 1:5 ~ 10 of described macroporous adsorbent resin equipment.
Described macroporous adsorbent resin material is polyacrylate type polymer, and its consumption is 20 ~ 30 times of activity in filtrate total hundred million.
Described crystallisation process is, under mixing speed 50 ~ 60r/min, temperature 1 ~ 10 DEG C of condition, adds acetone and sterling capreomycin sulfate solid, continues stirring 80 ~ 100min, then leaves standstill 120 ~ 160min, obtains solid matter capreomycin sulfate after filtration.
The consumption of described acetone is 5 ~ 10 times of adsorption bleaching filtrate volume, and sterling capreomycin sulfate solid consumption is 0.01 ~ 0.05% of adsorption bleaching filtrate volume.
Described drying process is, enables bipyramid and mixes powder machine, regulates inlet temperature to 120 ~ 130 DEG C, temperature of outgoing air to 50 ~ 80 DEG C, add wet-milling in charging opening, after 8 ~ 12 order stainless steel meshs, with air-flow to cyclonic separator, arrive powder shifter and obtain capreomycin sulfate through sieving.
Described preprocessing process is, the concentration of phosphoric acid controls 20 ~ 40%; The concentration of sodium carbonate controls 30 ~ 40%; Microbial flocculant (JT-613) consumption controls at 60 ~ 70mg/L; Flocculating aids is diatomite or Mierocrystalline cellulose or perlite, and consumption is 1 ~ 5% of fermentating liquid volume.
Technique effect of the present invention is:
1 compares with technique one, and its yield extracted reaches 85%, and yield improves 13.3%.
2 compare with technique one, adopt phosphoric acid to replace oxalic acid, reduce pre-treatment cost.
3 compare with technique one, adopt macroporous adsorbent resin and crystallization method respectively, replace activated carbon decolorizing, ion-exchange and mocromembrane filtration process, simplify extraction process step, shorten life cycle of the product, reduce production cost, improve the competitiveness of product in market.
4 compare with technique two, simplify capreomycin sulfate preparation technology, reduce equipment maintenance expense, reduce extraction cost.The product yield of this patent is higher than technique two simultaneously, improves product competitiveness in the market.
5 adopt this patent to prepare capreomycin sulfate, and its final product quality meets the regulation of Chinese Pharmacopoeia.
Embodiment
Be explained the present invention with example below, it should be understood that example is for illustration of the present invention instead of limitation of the present invention.Scope of the present invention and core content are determined according to claims.
Capromycin fermented liquid source in following embodiment:
Capromycin adopts curling streptomycete, and obtain capromycin fermented liquid by three grade fermemtation pattern, the carbon source in this fermention medium can be glucose, Testa Tritici or starch, the main soybean cake powder of nitrogenous source, fish meal or dried silkworm chrysalis meal etc.Its fermentation unit is at more than 11000u/ml.
Microbial flocculant JT-613 Hebei Jin Ti lagging material company limited in following embodiment.
Embodiment 1
Capromycin fermented liquid 10m
3, tire as 11896u/ml, total hundred million is 118.96.
1) pre-treatment:
Mixing speed controls at 30r/min, adds 20% phosphoric acid solution, first regulates pH to 5.0, stirs 40min, continues to add 20% phosphoric acid solution, regulates pH to 4.0, stirs 30min, adds 30% sodium carbonate solution, regulates pH to 7.5, stirs 20min.
Mixing speed controls at 100r/min, and add microbial flocculant JT-613600g, after 1min, rotating speed is down to 30r/min, leaves standstill 40min after stirring 20min.
Add flocculating aids diatomite 10kg in fermented liquid, stir 20min.
2) Plate Filtration
Use Plate Filtration fermented liquid, collect clear filtrate 7.7m
3.
3) dilute
After filtration completes, in reply sheet frame, filter residue is washed.Collect water lotion, when potency unit is lower than 500 μ/ml, stop washing.By filtrate and water lotion mixing, the volume of filtrate is 15.9m
3, tiring of capromycin controls at 7052u/ml.
Pre-treatment yield: 94.1%.
4) pH is regulated
Capromycin filtrate pH to 5.0 is regulated with 10% sulfuric acid.
5) macroporous resin adsorption decolouring
Resin filter equipment adds decolorizing resin 2379.2kg, by capreomycin sulfate solution warms to 30 DEG C, enters macroporous adsorbent resin equipment with 12ml/min flow velocity; Collect the filtrate through macroporous resin adsorption, flow rate control, at 14ml/min, through the > 4000u/ml that tires of macroporous resin adsorption filtrate, starts to collect filtrate, and the volume of filtrate is 15.8m
3, tiring of capromycin controls at 7011u/ml.
The yield of resin absorption decolouring: 98.8%.
6) crystallization
Mixing speed controls at 50r/min, and temperature controls, at 1 DEG C, to add acetone 79m in filtrate
3with sterling capreomycin sulfate solid 1.58kg, continue to stir 80min, then leave standstill 120min, after filtration, obtain solid matter capreomycin sulfate.
7) dry
Enable bipyramid and mix powder machine, regulate inlet temperature to 120 ~ 130 DEG C, temperature of outgoing air to 50 ~ 80 DEG C, add wet-milling in charging opening, after 8 ~ 12 order stainless steel meshs, with air-flow to cyclonic separator, arrive powder shifter and obtain capreomycin sulfate 109.7kg through sieving.
Total recovery: (109.7-1.58) × 0.94/ total hundred million=85.3%.
Embodiment 2
Capromycin fermented liquid 10m
3, tire as 11920u/ml, total hundred million is 119.2.
1) pre-treatment:
Mixing speed controls at 35r/min, adds 25% phosphoric acid solution, first regulates pH to 5.1, stirs 45min, continues to add 25% phosphoric acid solution, regulates pH to 4.1, stirs 40min, adds 33% sodium carbonate solution, regulates pH to 7.6, stirs 25min.
Mixing speed controls at 105r/min, and add microbial flocculant JT-613625g, after 1.5min, rotating speed is down to 35r/min, leaves standstill 45min after stirring 23min.
Add flocculating aids Mierocrystalline cellulose 20kg in fermented liquid, stir 25min.
2) Plate Filtration
Use Plate Filtration fermented liquid, collect clear filtrate 7.5m
3.
3) dilute
After filtration completes, in reply sheet frame, filter residue is washed.Collect water lotion, when potency unit is lower than 500 μ/ml, stop washing.By filtrate and water lotion mixing, the volume of filtrate is 15.4m
3, tiring of capromycin controls at 7361u/ml.
Pre-treatment yield: 95.1%.
4) pH is regulated
Capromycin filtrate pH to 5.3 is regulated with 15% sulfuric acid.
5) macroporous resin adsorption decolouring
Resin filter equipment adds decolorizing resin 2741.6kg, by capreomycin sulfate solution warms to 32 DEG C, enters macroporous adsorbent resin equipment with 13ml/min flow velocity; Collect the filtrate through macroporous resin adsorption, flow rate control, at 14.5ml/min, through the > 4000u/ml that tires of macroporous resin adsorption filtrate, starts to collect filtrate, and the volume of filtrate is 15.3m
3, tiring of capromycin controls at 7298u/ml.
The yield of resin absorption decolouring: 98.5%.
6) crystallization
Mixing speed controls at 52r/min, and temperature controls, at 3 DEG C, to add acetone 91.8m in filtrate
3with sterling capreomycin sulfate solid 3.06kg, continue to stir 85min, then leave standstill 130min, after filtration, obtain solid matter capreomycin sulfate.
7) dry
Enable bipyramid and mix powder machine, regulate inlet temperature to 120 ~ 130 DEG C, temperature of outgoing air to 50 ~ 80 DEG C, add wet-milling in charging opening, after 8 ~ 12 order stainless steel meshs, with air-flow to cyclonic separator, arrive powder shifter and obtain capreomycin sulfate 111.7kg through sieving
Total recovery: (111.76-3.06) × 0.94/ total hundred million=85.7%.
Embodiment 3
Capromycin fermented liquid 10m
3, tire as 12045u/ml, total hundred million is 120.45.
1) pre-treatment:
Mixing speed controls at 40r/min, adds 30% phosphoric acid solution, first regulates pH to 5.3, stirs 50min, continues to add 30% phosphoric acid solution, regulates pH to 4.3, stirs 45min, adds 35% sodium carbonate solution, regulates pH to 7.7, stirs 30min.
Mixing speed controls at 110r/min, and add microbial flocculant JT-613650g, after 2min, rotating speed is down to 40r/min, leaves standstill 50min after stirring 25min.
Add flocculating aids perlite 30kg in fermented liquid, stir 30min.
2) Plate Filtration
Use Plate Filtration fermented liquid, collect clear filtrate 7.6m
3.
3) dilute
After filtration completes, in reply sheet frame, filter residue is washed.Collect water lotion, when potency unit is lower than 500 μ/ml, stop washing.By filtrate and water lotion mixing, the volume of filtrate is 15.3m
3, tiring of capromycin controls at 7516u/ml.
Pre-treatment yield: 95.6%.
4) pH is regulated
Capromycin filtrate pH to 5.5 is regulated with 20% sulfuric acid.
5) macroporous resin adsorption decolouring
Resin filter equipment adds decolorizing resin 3011.25kg, by capreomycin sulfate solution warms to 33 DEG C, enters macroporous adsorbent resin equipment with 13.5ml/min flow velocity; Collect the filtrate through macroporous resin adsorption, flow rate control, at 15ml/min, through the > 4000u/ml that tires of macroporous resin adsorption filtrate, starts to collect filtrate, and the volume of filtrate is 15.1m
3, tiring of capromycin controls at 7486u/ml.
The yield of resin absorption decolouring: 98.3%.
6) crystallization
Mixing speed controls at 55r/min, and temperature controls, at 5 DEG C, to add acetone 113.25m in filtrate
3with sterling capreomycin sulfate solid 4.53kg, continue to stir 90min, then leave standstill 140min, after filtration, obtain solid matter capreomycin sulfate.
7) dry
Enable bipyramid and mix powder machine, regulate inlet temperature to 120 ~ 130 DEG C, temperature of outgoing air to 50 ~ 80 DEG C, add wet-milling in charging opening, after 8 ~ 12 order stainless steel meshs, with air-flow to cyclonic separator, arrive powder shifter and obtain capreomycin sulfate 111.7kg through sieving.
Total recovery: (114.6-4.53) × 0.94/ total hundred million=85.9%.
Embodiment 4
Capromycin fermented liquid 10m
3, tire as 11900u/ml, total hundred million is 119.
1) pre-treatment:
Mixing speed controls at 45r/min, adds 35% phosphoric acid solution, first regulates pH to 5.4, stirs 55min, continues to add 35% phosphoric acid solution, regulates pH to 4.4, stirs 50min, adds 37% sodium carbonate solution, regulates pH to 7.8, stirs 35min.
Mixing speed controls at 115r/min, and add microbial flocculant JT-613675g, after 2.5min, rotating speed is down to 45r/min, leaves standstill 55min after stirring 27min.
Add flocculating aids diatomite 40kg in fermented liquid, stir 35min.
2) Plate Filtration
Use Plate Filtration fermented liquid, collect clear filtrate 7.8m
3.
3) dilute
After filtration completes, in reply sheet frame, filter residue is washed.Collect water lotion, when potency unit is lower than 500 μ/ml, stop washing.By filtrate and water lotion mixing, the volume of filtrate is 14.4m
3, tiring of capromycin controls at 7874u/ml.
Pre-treatment yield: 95.3%.
4) pH is regulated
Capromycin filtrate pH to 5.7 is regulated with 25% sulfuric acid.
5) macroporous resin adsorption decolouring
Resin filter equipment adds decolorizing resin 3213kg, by capreomycin sulfate solution warms to 34 DEG C, enters macroporous adsorbent resin equipment with 14ml/min flow velocity; Collect the filtrate through macroporous resin adsorption, flow rate control, at 15.5ml/min, through the > 4000u/ml that tires of macroporous resin adsorption filtrate, starts to collect filtrate, and the volume of filtrate is 14.2m
3, tiring of capromycin controls at 7825u/ml.
The yield of resin absorption decolouring: 98.0%.
6) crystallization
Mixing speed controls at 57r/min, and temperature controls, at 7 DEG C, to add acetone 127.8m in filtrate
3with sterling capreomycin sulfate solid 5.68kg, continue to stir 95min, then leave standstill 150min, after filtration, obtain solid matter capreomycin sulfate.
7) dry
Enable bipyramid and mix powder machine, regulate inlet temperature to 120 ~ 130 DEG C, temperature of outgoing air to 50 ~ 80 DEG C, add wet-milling in charging opening, after 8 ~ 12 order stainless steel meshs, with air-flow to cyclonic separator, arrive powder shifter and obtain capreomycin sulfate 111.7kg through sieving.
Total recovery: (114-5.68) × 0.94/ total hundred million=85.6%.
Embodiment 5
Capromycin fermented liquid 10m
3, tire as 11843u/ml, total hundred million is 118.43.
1) pre-treatment:
Mixing speed controls at 50r/min, adds 40% phosphoric acid solution, first regulates pH to 5.5, stirs 60min, continues to add 40% phosphoric acid solution, regulates pH to 4.5, stirs 50min, adds 40% sodium carbonate solution, regulates pH to 8.0, stirs 40min.
Mixing speed controls at 120r/min, and add microbial flocculant JT-613700g, after 3min, rotating speed is down to 50r/min, leaves standstill 60min after stirring 30min.
Add flocculating aids Mierocrystalline cellulose 50kg in fermented liquid, stir 40min.
2) Plate Filtration
Use Plate Filtration fermented liquid, collect clear filtrate 7.6m
3.
3) dilute
After filtration completes, in reply sheet frame, filter residue is washed.Collect water lotion, when potency unit is lower than 500 μ/ml, stop washing.By filtrate and water lotion mixing, the volume of filtrate is 14.1m
3, tiring of capromycin controls at 7986u/ml.
Pre-treatment yield: 95.1%.
4) pH is regulated
Capromycin filtrate pH to 6.0 is regulated with 30% sulfuric acid.
5) macroporous resin adsorption decolouring
Resin filter equipment adds decolorizing resin 3553kg, by capreomycin sulfate solution warms to 35 DEG C, enters macroporous adsorbent resin equipment with 15ml/min flow velocity; Collect the filtrate through macroporous resin adsorption, flow rate control, at 16ml/min, through the > 4000u/ml that tires of macroporous resin adsorption filtrate, starts to collect filtrate, and the volume of filtrate is 13.9m
3, tiring of capromycin controls at 7939u/ml.
The yield of resin absorption decolouring: 98.0%.
6) crystallization
Mixing speed controls at 60r/min, and temperature controls, at 10 DEG C, to add acetone 139m in filtrate
3with sterling capreomycin sulfate solid 6.95kg, continue to stir 100min, then leave standstill 160min, after filtration, obtain solid matter capreomycin sulfate.
7) dry
Enable bipyramid and mix powder machine, regulate inlet temperature to 120 ~ 130 DEG C, temperature of outgoing air to 50 ~ 80 DEG C, add wet-milling in charging opening, after 8 ~ 12 order stainless steel meshs, with air-flow to cyclonic separator, arrive powder shifter and obtain capreomycin sulfate 111.7kg through sieving.
Total recovery: (114.3-6.95) × 0.94/ total hundred million=85.2%.
Claims (10)
1. the method utilizing capromycin fermented liquid to prepare capreomycin sulfate, it is characterized in that its processing step is: first capromycin fermented liquid is carried out pre-treatment, then Plate Filtration, gained filtrate is diluted to tiring of capromycin and adjusts filtrate pH to 5.0 ~ 6.0 after 7000 ~ 8000u/ml, decolour by macroporous resin adsorption, collect the adsorption bleaching filtrate of the > 4000u/ml that tires, crystallization, dry;
Above-mentioned preprocessing process is:
1) under mixing speed 30 ~ 50r/min, first regulate capromycin fermented liquid pH to 5.0 ~ 5.5 with phosphoric acid solution, stir 40 ~ 60min, rear continuation phosphorus acid for adjusting pH to 4.0 ~ 4.5, stir 30 ~ 60min, then regulate pH to 7.5 ~ 8.0 with sodium carbonate solution, stir 20 ~ 40min;
2) under mixing speed 100 ~ 120r/min, add microbial flocculant, after stirring 1 ~ 3min, rotating speed is down to 30 ~ 50r/min, after stirring 20 ~ 30min, leave standstill 40 ~ 60min;
3) add flocculating aids, stir 20 ~ 40min.
2. according to the method utilizing capromycin fermented liquid to prepare capreomycin sulfate according to claim 1, it is characterized in that: after Plate Filtration, with filter residue in water cleaning sheet frame, collect water lotion, when potency unit is lower than 500 μ/ml, stop washing, by filtrate and water lotion mixing.
3. according to the method utilizing capromycin fermented liquid to prepare capreomycin sulfate according to claim 1, it is characterized in that: the filtrate concentration after Plate Filtration is the sulfuric acid adjustment pH of 10 ~ 30%.
4. according to the method utilizing capromycin fermented liquid to prepare capreomycin sulfate according to claim 1, it is characterized in that described macroporous resin adsorption decolorization is: first the filtrate of the Plate Filtration of pH5.0 ~ 6.0 is warming up to 30 ~ 35 DEG C, enters macroporous adsorbent resin equipment with 12 ~ 15ml/min flow velocity; Collect the filtrate through macroporous resin adsorption, flow rate control, at 14 ~ 16ml/min, through the > 4000u/ml that tires of macroporous resin adsorption filtrate, starts to collect filtrate.
5., according to the method utilizing capromycin fermented liquid to prepare capreomycin sulfate according to claim 4, it is characterized in that blade diameter length ratio 1:5 ~ 10 of described macroporous adsorbent resin equipment.
6. prepare the method for capreomycin sulfate according to the capromycin fermented liquid that utilizes described in claim 1 or 4, it is characterized in that described macroporous adsorbent resin material is polyacrylate type polymer, its consumption is 20 ~ 30 times of activity in filtrate total hundred million.
7. according to the method utilizing capromycin fermented liquid to prepare capreomycin sulfate according to claim 1, it is characterized in that described crystallisation process is, under mixing speed 50 ~ 60r/min, temperature 1 ~ 10 DEG C of condition, add acetone and sterling capreomycin sulfate solid, continue stirring 80 ~ 100min, then leave standstill 120 ~ 160min, after filtration, obtain solid matter capreomycin sulfate.
8. according to the method utilizing capromycin fermented liquid to prepare capreomycin sulfate according to claim 7, it is characterized in that the consumption of described acetone is 5 ~ 10 times of adsorption bleaching filtrate volume, sterling capreomycin sulfate solid consumption is 0.01 ~ 0.05% of adsorption bleaching filtrate volume.
9. according to the method utilizing capromycin fermented liquid to prepare capreomycin sulfate according to claim 1, it is characterized in that described drying process is, enable bipyramid and mix powder machine, regulate inlet temperature to 120 ~ 130 DEG C, temperature of outgoing air to 50 ~ 80 DEG C, add wet-milling in charging opening, after 8 ~ 12 order stainless steel meshs, with air-flow to cyclonic separator, arrive powder shifter and obtain capreomycin sulfate through sieving.
10., according to the method utilizing capromycin fermented liquid to prepare capreomycin sulfate according to claim 1, it is characterized in that described preprocessing process is, the concentration of phosphoric acid controls 20 ~ 40%; The concentration of sodium carbonate controls 30 ~ 40%; Microbial flocculant consumption controls at 60 ~ 70mg/L; Flocculating aids is diatomite or Mierocrystalline cellulose or perlite, and consumption is 1 ~ 5% of fermentating liquid volume.
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| CN105506042A (en) * | 2016-02-23 | 2016-04-20 | 华北制药集团新药研究开发有限责任公司 | Method for producing capreomycin by fermentation |
| CN105504023A (en) * | 2016-02-23 | 2016-04-20 | 华北制药集团新药研究开发有限责任公司 | Capreomycin preparation method |
| CN105622593A (en) * | 2016-02-25 | 2016-06-01 | 中国农业科学院蜜蜂研究所 | Extraction method of fumagillin |
| CN110483617A (en) * | 2019-09-17 | 2019-11-22 | 陕西绿盾环境工程研究院有限公司 | A kind of preparation method of high-content polyoxin original powder |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105506042A (en) * | 2016-02-23 | 2016-04-20 | 华北制药集团新药研究开发有限责任公司 | Method for producing capreomycin by fermentation |
| CN105504023A (en) * | 2016-02-23 | 2016-04-20 | 华北制药集团新药研究开发有限责任公司 | Capreomycin preparation method |
| CN105622593A (en) * | 2016-02-25 | 2016-06-01 | 中国农业科学院蜜蜂研究所 | Extraction method of fumagillin |
| CN105622593B (en) * | 2016-02-25 | 2018-06-26 | 中国农业科学院蜜蜂研究所 | A kind of extracting method of fumidil |
| CN110483617A (en) * | 2019-09-17 | 2019-11-22 | 陕西绿盾环境工程研究院有限公司 | A kind of preparation method of high-content polyoxin original powder |
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| CN105131091B (en) | 2018-09-11 |
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