CN106349305A - Extraction and preparation method of streptomycin sulfate - Google Patents
Extraction and preparation method of streptomycin sulfate Download PDFInfo
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- CN106349305A CN106349305A CN201610732913.1A CN201610732913A CN106349305A CN 106349305 A CN106349305 A CN 106349305A CN 201610732913 A CN201610732913 A CN 201610732913A CN 106349305 A CN106349305 A CN 106349305A
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- streptomycin
- streptomycin sulfate
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- molecule polymer
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H15/00—Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
- C07H15/20—Carbocyclic rings
- C07H15/22—Cyclohexane rings, substituted by nitrogen atoms
- C07H15/238—Cyclohexane rings substituted by two guanidine radicals, e.g. streptomycins
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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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- Health & Medical Sciences (AREA)
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- Biotechnology (AREA)
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- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Compounds Of Unknown Constitution (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses an extraction and preparation method of streptomycin sulfate. The extraction and preparation method comprises the steps of acidizing, filtering, adsorbing, pre-washing, eluting, decompression concentrating, salt forming, decoloring, concentrating and spray-drying, thus obtaining a finished product. The extraction and preparation method of the streptomycin sulfate has the beneficial effects that the technical problems in the prior art that the extraction and preparation route is long, the production efficiency is low, the investment cost is high, the yield is low, the product color is poor, and the qualification rate is low are solved and has the advantages that the extraction and preparation process is short, the procedures are simple, the production efficiency is high, the investment cost is low, the consumption of active carbon is small, the yield is high, the product color is good, and the qualification rate is high.
Description
Technical field
The invention belongs to extract drugs field, it is related to a kind of extraction preparation method of pharmaceutical raw material, more particularly to one kind
Streptomycin sulfate extracts preparation method.
Background technology
Streptomycin sulfate is a kind of aminoglycoside antibioticss.This product has powerful antibacterial action to tubercule bacillus, and it is minimum
Mlc (mic) is generally 0.5mg/l.It is to many gram negative bacterias (g-) such as escherichia coli, pneumobacilluses, enterobacteria
Genus, Salmonella, Brucella etc. also have an antibacterial action, poor to gram positive bacteria (g+) antibacterial activity.It is for treatment
Various tuberculosis have significant curative effect, are class drug of first choices for the treatment of pulmonary tuberculosis, are additionally operable to treat the plague and Gram-negative
Microbial urinary tract infection, intestinal infection, tuberculous meningitis, septicemia, pneumonia, peritonitis etc..
At present, the method extracting preparation is the fermentation liquid acidifying of streptomycin, by ceramic membrane filter, sodium form faintly acid sun from
Sub-exchange resin dynamic adsorption, aqueous sulfuric acid desorbing, one time stripping liquid adsorbs through macropore primary amine resins again, aqueous sulfuric acid
Desorbing, secondary stripping liquid carries out desalination neutralization through the mixed bed that resin forms, and then uses activated carbon decolorizing, thin film concentration, ultrafiltration
Remove endotoxin and pigment, be spray-dried and obtain streptomycin sulfate finished product.
In actual production operating process, this extraction preparation method there are following weak point:
Extract preparation process through ion exchange twice, circuit is longer, low production efficiency, high cost, and yield is low；
The streptomycin sulfate finished product color level that extraction prepares is poor, and conforming product rate is low.
Content of the invention
The present invention is to solve problem of the prior art, provides a kind of production efficiency high, input cost is low, eluting liquid hold-up
High, clarity is good, and activated carbon dosage is little, high income, and product color level is good, and the new side of streptomycin sulfate is prepared in the high extraction of qualification rate
Method.
The present invention is to realize its purpose to the technical scheme is that a kind of streptomycin sulfate extracts preparation method, the method
Comprise the steps:
A, filtration: streptomycin sulfate fermentation liquid is carried out being acidified to ph2.0 ~ 4.0, then carries out ceramic membrane filter, obtain filtrate；
B, absorption: with alkali, the filtrate ph that step a obtains is adjusted to 6.0 ~ 8.0, enters action with streptomycin imprint molecule polymer
State is adsorbed；
C, prewashing: prewashing is carried out to the streptomycin imprint molecule polymer in step b with soft water；
D, eluting: with methanol aqueous solution or ethanol water, eluting is carried out to the streptomycin imprint molecule polymer in step c, obtain
To eluent；
E, concentrating under reduced pressure: vacuum distillation is carried out to eluent, obtains concentrated solution；
F, one-tenth salt: concentrated solution addition sulphuric acid is become salt, obtains into saline solution；
G, decolouring: saline solution will be become to add activated carbon, filter, obtain destaining solution；
H, concentration: with NF membrane, destaining solution is concentrated, obtain finished fluid；
I, spray drying: finished fluid is spray-dried, gets product.
Further, the acid being acidified in described step a is oxalic acid, and the alkali in step c is sodium hydroxide.
Further, the flow velocity of the dynamic adsorption in described step c is 0.5 ~ 2.0bv/h, and streptomycin imprint molecule is polymerized
The adsorbance of thing is 100 ~ 150g/l.
Further, the prewashing flow velocity in described step c is 1.0 ~ 2.0bv/h, and the wherein consumption of soft water prints for streptomycin
1.0 ~ 4.0 times of sub- polymer volume of scoring.
Further, in described step d, elution flow rate is 0.1-1.0bv/h, the body of methanol and water in methanol aqueous solution
Long-pending ratio is 0.5 ~ 4.0:1, and in ethanol water, ethanol and the volume ratio of water are 0.5 ~ 4.0:1.
Further, in described step e, the temperature of vacuum distillation is 30 ~ 40 DEG C.
Further, adding sulphuric acid to adjust ph in described step f is 4.5 ~ 6.0.
Further, in described step f, the molecular weight of sodium filter membrane is 200 ~ 500da.
Have the beneficial effects that using produced by technique scheme: the invention reside in by improving original sulphuric acid strepto-
Plain extraction and preparation technique, obtains meeting the streptomycin sulfate of usp and cp standard, by using streptomycin imprint molecule polymer pair
Streptomycin in fermentation liquid carries out being enriched with, purification, removes most albumen, pigment and other impurities, in the eluent obtaining
Content of streptomycin is high, changes existing ion exchange extraction preparation production technology, improves production efficiency, reduce and put into into
This, activated carbon dosage is little, high income, and product color level is good, and qualification rate is high.Streptomycin sulfate total recovery more than 95%, higher than mesh
The level of front yield 80% about.
Specific embodiment
Below the embodiment it is clear that described is clearly and completely described to the technical scheme in the embodiment of the present invention
It is only a part of embodiment of the present invention, rather than whole embodiments.Based on the embodiment in the present invention, this area is common
The every other embodiment that technical staff is obtained under the premise of not making creative work, broadly falls into the model of present invention protection
Enclose.
Embodiment 1
A, filtration: by streptomycin fermentation liquid 60l, potency 28550u/ml, product weight 1.713 kg.Adjust ph with oxalic acid to arrive
2.0, then filtered through ceramic membrane, obtained filtrate；
B, absorption: with sodium hydroxide, filtrate ph is adjusted to 6.0, then with streptomycin imprint molecule polymer, action is entered to filtrate
State is adsorbed, and is squeezed into peristaltic pump in the pillar installing streptomycin imprint molecule polymer, and flow velocity is 0.5bv/h, strepto-
Plain imprint molecule Polymer adsorption amount is 100g/l；
C, prewashing: with soft water, prewashing is carried out to the streptomycin imprint molecule polymer after adsorbing in step b, flow velocity is 1.0bv/h,
The consumption of soft water is 1.0 times of streptomycin imprint molecule polymer volume；
D, eluting: with methanol aqueous solution, the streptomycin imprint molecule polymer after prewashing is carried out with eluting, the volume of methanol and water
For 0.5:1, flow velocity is 0.1bv/h to ratio, obtains eluent；
E, concentrating under reduced pressure: eluent is added in vacuum distillation apparatus and is concentrated, temperature is 30 DEG C, obtains concentrated solution；
F, one-tenth salt: adding sulphuric acid to adjust ph in concentrated solution is 4.5, obtains into saline solution；
G, decolouring: to becoming to add the stirring decolouring of 200g activated carbon in saline solution, filter, obtain destaining solution；
H, concentration: with the NF membrane that molecular weight is 300da, destaining solution is concentrated, obtain finished fluid；
I, spray drying: finished fluid is spray-dried, obtains the streptomycin sulfate finished product 1.88kg meeting cp and usp standard, receive
Rate 95.4%.
Embodiment 2
A, filtration: by streptomycin fermentation liquid 50l, potency 28000u/ml, product weight 1.4 kg.Adjust ph to 4.0 with oxalic acid,
Then filtered through ceramic membrane, obtained filtrate；
B, absorption: with sodium hydroxide, filtrate ph is adjusted to 7.2, then with streptomycin imprint molecule polymer, action is entered to filtrate
State is adsorbed, and is squeezed into peristaltic pump in the pillar installing streptomycin imprint molecule polymer, and flow velocity is 2.0bv/h, strepto-
Plain imprint molecule Polymer adsorption amount is 150g/l；
C, prewashing: with soft water, prewashing is carried out to the streptomycin imprint molecule polymer after adsorbing in step b, flow velocity is 1.0bv/h,
The consumption of soft water is 4.0 times of streptomycin imprint molecule polymer volume；
D, eluting: with methanol aqueous solution, the streptomycin imprint molecule polymer after prewashing is carried out with eluting, the volume of methanol and water
For 4.0:1, flow velocity is 1.0bv/h to ratio, obtains eluent；
E, concentrating under reduced pressure: eluent is added in vacuum distillation apparatus and is concentrated, temperature is 40 DEG C, obtains concentrated solution；
F, one-tenth salt: adding sulphuric acid to adjust ph in concentrated solution is 6.0, obtains into saline solution；
G, decolouring: to becoming to add the stirring decolouring of 210g activated carbon in saline solution, filter, obtain destaining solution；
H, concentration: with the NF membrane that molecular weight is 500da, destaining solution is concentrated, obtain finished fluid；
I, spray drying: finished fluid is spray-dried, obtains the streptomycin sulfate finished product 1.61kg meeting cp and usp standard, receive
Rate 96%.
Embodiment 3
A, filtration: by streptomycin fermentation liquid 52l, potency 28600u/ml, product weight 1.487 kg.Adjust ph with oxalic acid to arrive
2.0, then filtered through ceramic membrane, obtained filtrate；
B, absorption: with sodium hydroxide, filtrate ph is adjusted to 6.8, then with streptomycin imprint molecule polymer, action is entered to filtrate
State is adsorbed, and is squeezed into peristaltic pump in the pillar installing streptomycin imprint molecule polymer, and flow velocity is 1.25bv/h, strepto-
Plain imprint molecule Polymer adsorption amount is 125g/l；
C, prewashing: with soft water, prewashing is carried out to the streptomycin imprint molecule polymer after adsorbing in step b, flow velocity is 1.5bv/h,
The consumption of soft water is 2.5 times of streptomycin imprint molecule polymer volume；
D, eluting: with methanol aqueous solution, the streptomycin imprint molecule polymer after prewashing is carried out with eluting, the volume of methanol and water
For 2.25:1, flow velocity is 0.55bv/h to ratio, obtains eluent；
E, concentrating under reduced pressure: eluent is added in vacuum distillation apparatus and is concentrated, temperature is 35 DEG C, obtains concentrated solution；
F, one-tenth salt: adding sulphuric acid to adjust ph in concentrated solution is 5.25, obtains into saline solution；
G, decolouring: to becoming to add the stirring decolouring of 205g activated carbon in saline solution, filter, obtain destaining solution；
H, concentration: with the NF membrane that molecular weight is 400da, destaining solution is concentrated, obtain finished fluid；
I, spray drying: finished fluid is spray-dried, obtains the streptomycin sulfate finished product 1.74kg meeting cp and usp standard, receive
Rate 96.6%.
Embodiment 4
A, filtration: by streptomycin fermentation liquid 46l, potency 29000u/ml, product weight 1.334 kg.Adjust ph with oxalic acid to arrive
3.1, then filtered through ceramic membrane, obtained filtrate；
B, absorption: with sodium hydroxide, filtrate ph is adjusted to 7.5, then with streptomycin imprint molecule polymer, action is entered to filtrate
State is adsorbed, and is squeezed into peristaltic pump in the pillar installing streptomycin imprint molecule polymer, and flow velocity is 0.9bv/h, strepto-
Plain imprint molecule Polymer adsorption amount is 110g/l；
C, prewashing: with soft water, prewashing is carried out to the streptomycin imprint molecule polymer after adsorbing in step b, flow velocity is 1.2bv/h,
The consumption of soft water is 1.5 times of streptomycin imprint molecule polymer volume；
D, eluting: with methanol aqueous solution, the streptomycin imprint molecule polymer after prewashing is carried out with eluting, the volume of methanol and water
For 3.2:1, flow velocity is 0.3bv/h to ratio, obtains eluent；
E, concentrating under reduced pressure: eluent is added in vacuum distillation apparatus and is concentrated, temperature is 36 DEG C, obtains concentrated solution；
F, one-tenth salt: adding sulphuric acid to adjust ph in concentrated solution is 5.7, obtains into saline solution；
G, decolouring: to becoming to add the stirring decolouring of 250g activated carbon in saline solution, filter, obtain destaining solution；
H, concentration: with the NF membrane that molecular weight is 300da, destaining solution is concentrated, obtain finished fluid；
I, spray drying: finished fluid is spray-dried, obtains the streptomycin sulfate finished product 1.6kg meeting cp and usp standard, yield
96.4%.
Embodiment 5
A, filtration: by streptomycin fermentation liquid 65l, potency 28930u/ml, product weight 1.88 kg.Adjust ph to 2.6 with oxalic acid,
Then filtered through ceramic membrane, obtained filtrate；
B, absorption: with sodium hydroxide, filtrate ph is adjusted to 6.4, then with streptomycin imprint molecule polymer, action is entered to filtrate
State is adsorbed, and is squeezed into peristaltic pump in the pillar installing streptomycin imprint molecule polymer, and flow velocity is 1.8bv/h, strepto-
Plain imprint molecule Polymer adsorption amount is 144g/l；
C, prewashing: with soft water, prewashing is carried out to the streptomycin imprint molecule polymer after adsorbing in step b, flow velocity is 1.7bv/h,
The consumption of soft water is 2.3 times of streptomycin imprint molecule polymer volume；
D, eluting: with methanol aqueous solution, the streptomycin imprint molecule polymer after prewashing is carried out with eluting, the volume of methanol and water
For 3.3:1, flow velocity is 0.6bv/h to ratio, obtains eluent；
E, concentrating under reduced pressure: eluent is added in vacuum distillation apparatus and is concentrated, temperature is 34 DEG C, obtains concentrated solution；
F, one-tenth salt: adding sulphuric acid to adjust ph in concentrated solution is 5.0, obtains into saline solution；
G, decolouring: to becoming to add the stirring decolouring of 220g activated carbon in saline solution, filter, obtain destaining solution；
H, concentration: with the NF membrane that molecular weight is 420da, destaining solution is concentrated, obtain finished fluid；
I, spray drying: finished fluid is spray-dried, obtains the streptomycin sulfate finished product 2.2kg meeting cp and usp standard, yield
96.2%.
Claims (8)
1. a kind of streptomycin sulfate extract preparation method it is characterised in that: the method comprises the steps:
A, filtration: streptomycin sulfate fermentation liquid is carried out being acidified to ph2.0 ~ 4.0, then carries out ceramic membrane filter, obtain filtrate；
B, absorption: with alkali, the filtrate ph that step a obtains is adjusted to 6.0 ~ 8.0, enters action with streptomycin imprint molecule polymer
State is adsorbed；
C, prewashing: prewashing is carried out to the streptomycin imprint molecule polymer after absorption with soft water；
D, eluting: the streptomycin imprint molecule polymer after prewashing in step c is carried out with methanol aqueous solution or ethanol water
Eluting, obtains eluent；
E, concentrating under reduced pressure: vacuum distillation is carried out to eluent, obtains concentrated solution；
F, one-tenth salt: concentrated solution addition sulphuric acid is become salt, obtains into saline solution；
G, decolouring: saline solution will be become to add activated carbon, filter, obtain destaining solution；
H, concentration: with NF membrane, destaining solution is concentrated, obtain finished fluid；
I, spray drying: finished fluid is spray-dried, gets product.
2. a kind of streptomycin sulfate according to claim 1 extracts preparation method it is characterised in that acid in described step a
The acid changed is oxalic acid, and the alkali in step c is sodium hydroxide.
3. a kind of streptomycin sulfate according to claim 1 extracts preparation method it is characterised in that in described step c
The flow velocity of dynamic adsorption is 0.5 ~ 2.0bv/h, and the adsorbance of streptomycin imprint molecule polymer is 100 ~ 150g/l.
4. a kind of streptomycin sulfate according to claim 1 extracts preparation method it is characterised in that in described step c
Prewashing flow velocity is 1.0 ~ 2.0bv/h, and the wherein consumption of soft water is 1.0 ~ 4.0 times of streptomycin imprint molecule polymer volume.
5. a kind of streptomycin sulfate according to claim 1 extracts preparation method it is characterised in that in described step d
Elution flow rate is 0.1 ~ 1.0bv/h, and in methanol aqueous solution, methanol and the volume ratio of water are 0.5 ~ 4.0:1, second in ethanol water
Alcohol is 0.5 ~ 4.0:1 with the volume ratio of water.
6. a kind of streptomycin sulfate according to claim 1 extracts preparation method it is characterised in that in described step e
The temperature of vacuum distillation is 30 ~ 40 DEG C.
7. a kind of streptomycin sulfate according to claim 1 extracts preparation method it is characterised in that in described step f
Adding sulphuric acid to adjust ph is 4.5 ~ 6.0.
8. a kind of streptomycin sulfate according to claim 1 extracts preparation method it is characterised in that in described step f
The molecular weight of sodium filter membrane is 200 ~ 500da.
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| CN201610732913.1A CN106349305A (en) | 2016-08-27 | 2016-08-27 | Extraction and preparation method of streptomycin sulfate |
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| CN201610732913.1A CN106349305A (en) | 2016-08-27 | 2016-08-27 | Extraction and preparation method of streptomycin sulfate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN117259383A (en) * | 2023-10-30 | 2023-12-22 | 河南理工大学 | Organic solid waste treatment process |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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| CN117259383B (en) * | 2023-10-30 | 2024-05-17 | 河南理工大学 | Organic solid waste treatment process |
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Application publication date: 20170125 |