CN1110686A - Extracting and purifying of penicillin - Google Patents
Extracting and purifying of penicillin Download PDFInfo
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- CN1110686A CN1110686A CN 94116070 CN94116070A CN1110686A CN 1110686 A CN1110686 A CN 1110686A CN 94116070 CN94116070 CN 94116070 CN 94116070 A CN94116070 A CN 94116070A CN 1110686 A CN1110686 A CN 1110686A
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- penicillin
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- filtrate
- filtration
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- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
In solvent extracting process of fermented penicillin liquid, surfactant is not used and ultrafilter membrane is used for ultrafiltering of said fermented liquid or filtrate to purfy the filtrate. The purification and concentration of penicillin may be one-pass completed by use of any extracting equipment. The liquid extractant is washed by salt-free water for purifying the extractant further.
Description
The invention belongs to the separation of organic compound.
The purification of penicillin has report in prior art, extract penicillin from fermented liquid, and methods such as active carbon adsorption, the precipitator method, ion exchange method, solvent extraction are arranged.Generally adopting solvent extraction at present, is that the filtrate that organic solvent and penicillin fermentation liquid pre-treatment are filtered is mixed, and makes penicillin change solvent over to by water by regulating pH value, reaches and purifies and spissated purpose.This method has following several: penicillin is extracted into the step of one in solvent extraction process (R.W.Swartz.comprensive Biotchnology.ed.M.Mooyoung.vol.3.P28-29 Pergamon press New York, 1985) by filtrate by one step of Podbielniak extracter; Penicillin is carried into solvent by filtrate, is changed over to damping fluid, again by damping fluid carry into the solvent phase three the step extraction methods (Yu Wen and etc., " microbiotic technology ", Liaoning science tech publishing house, P227(1988); Penicillin is put forward the single extraction azeotropic crystalization method of directly carrying out azeotropic crystalization behind the solvent (Yu Wen and etc., " microbiotic technology ", Liaoning science tech publishing house, P196-197(1988)); Penicillin fermentation liquid is directly used the direx process that decanting vessel extracts (Yu Wen and etc., " microbiotic technology ", Liaoning science tech publishing house, P227(1988)).These extraction processs all can realize purifying purpose of penicillin, but all must could realize the isolating extraction process of solvent and water by means of emulsion splitter, and all need just can carry out the penicillin crystallization through the decoloration process process, so complex technical process, cost height, the use of emulsion splitter cause the pollution of discharge water to environment, have increased the difficulty and the expense of sewage disposal, no matter use which kind of extraction equipment and emulsion splitter, its secondary counter-current extraction yield is far below theoretical yield.
The extraction process that the purpose of this invention is to provide a kind of penicillin of purifying, this technological process are not introduced any surfactivity emulsion splitter, and technology is simple, and the extraction yield is near theoretical yield, and cost is low, improve the quality of products, and overcome the shortcoming of prior art.
The present invention extracts and process to purify penicillin from penicillin fermentation liquid, and the technical process of producing the penicilline g potassium inject salt is:
The technical process of salt is:
Penicillin fermentation liquid carries out ultrafiltration with molecular weight cut off (MWCO) 20000 and following ultra-filtration membrane (organic membrane or mineral membrane) after pre-treatment is filtered (or not filtering), the ultra-filtration process yield is greater than 98%.The bottom product of ultrafiltration is delivered to original fermented solution pre-treatment jar or is used to produce the feed byproduct, sees through liquid with solvent (N-BUTYL ACETATE etc.) and 10%H
2SO
4Transferring pH value is to carry out the secondary counter-current extraction at 2.0～2.2 o'clock, and extraction liquid is with the salt-free water washing of 0.5～1 times of volume, washing water with enter System of Recovery Tower recovery solvent BA after raffinate mixes.Extraction liquid look level after the washing is less than 3, pollute number less than 0.4%, through-10 ℃ of lyophilizations and sterile filtration (manufacture salt then need not to filter), in crystallizer, under 10～20 ℃ of conditions, carry out the potassium penicillin G crystallization with 25% ethanol-liquor kalii acetici, crystal is with 4～6L/
1,000,000,000The butanols and the 1.5～2L/ of amount
1,000,000,000The vinyl acetic monomer of amount carries out filtration washing, obtains purified potassium penicillin G crystal.Crystalline mother solution, washings enter rectifying tower respectively and reclaim solvent.
The present invention's outstanding advantage compared with the prior art is, owing to removed biopolymer materials such as influencing penicillin g extract and crystalline protein in the ultra-filtration process, just can once not finish penicillin is changed over to the solvent phase by water purification concentration process so in the penicillin g extract process, need not add any tensio-active agent, and need not decolour and just can meet and exceed the requirement of crystalline look level, quality product height, yield height, production cost reduce work simplification.Adopt this technology to being that the product yield and the quality of the semisynthetic penicillin (as cephalosporin) of raw material all is significantly improved than existing technology with penicillin.
Embodiment:
Penicillin thread fungus fermented liquid 5000L, 49580u/mL tires, behind pre-treatment and Plate Filtration, get filtrate 9600L, 22567u/mL tires, after ultrafiltration under 20 ℃ of 0.2MPa working pressures, obtain seeing through liquid 9600L with molecular weight cut off (MWCO) 20000 and following ultra-filtration membrane, the 22116u/mL that tires, ultra-filtration process yield 98%.Use the 2400L N-BUTYL ACETATE, 10%H
2SO
4It is 2.0 that 108L transfers pH value, and the penicillin fermentation liquid after the ultrafiltration is carried out the secondary counter-current extraction in butterfly chip centrifugal extractor, obtains 2350L penicillin g extract liquid, and 85810u/mL tires; With this extraction liquid and the salt-free water washing of 1500L, again through lyophilization below-10 ℃, again through in crystallizer, under 15 ℃ of conditions, carrying out the potassium penicillin G crystallization after the sterile filtration with 25% ethanol-liquor kalii acetici.Crystal carries out washing and filtering with 1016L and 608L propyl carbinol and 1016L vinyl acetic monomer respectively, crystal again through press-powder, sieve, make penicillin g potassium for inj salt 110.7kg after the drying, 1598u/mL tires, the look level is less than 0.5,280nm light absorption value 0.015, clarity and trichobothrium are less than 5, and specific volume 4.5mL/g, pH value are 5.9.
Claims (2)
1, a kind of separating technology of organic compound, the invention is characterized in the filtrate of using after molecular weight cut off (MWCO) 20000 and following ultra-filtration membrane filter the penicillin fermentation liquid pre-treatment, or directly fermented liquid is carried out super filtration, purifying filtrate, see through purification and the concentration process of once finishing penicillin in any extraction equipment that the penicillin g extract process of liquid can use aborning, the salt-free water washing of extraction liquid is further purified extraction liquid.
2, Separation of Organic Compounds technology according to claim 1 is characterized in that super filtration is at 5～30 ℃, carries out under the condition of 0.1～0.5MPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94116070 CN1052727C (en) | 1994-09-22 | 1994-09-22 | Extracting and purifying of penicillin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94116070 CN1052727C (en) | 1994-09-22 | 1994-09-22 | Extracting and purifying of penicillin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1110686A true CN1110686A (en) | 1995-10-25 |
| CN1052727C CN1052727C (en) | 2000-05-24 |
Family
ID=5037779
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 94116070 Expired - Fee Related CN1052727C (en) | 1994-09-22 | 1994-09-22 | Extracting and purifying of penicillin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1052727C (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1997035029A1 (en) * | 1996-03-15 | 1997-09-25 | Antibioticos, S.A. | Alternative process for producing 6-amino-penicillanic acid (6-apa) |
| CN103214498A (en) * | 2013-04-20 | 2013-07-24 | 河北美邦工程科技有限公司 | Penicillin fermentation broth treating technology |
-
1994
- 1994-09-22 CN CN 94116070 patent/CN1052727C/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1997035029A1 (en) * | 1996-03-15 | 1997-09-25 | Antibioticos, S.A. | Alternative process for producing 6-amino-penicillanic acid (6-apa) |
| US6110699A (en) * | 1996-03-15 | 2000-08-29 | Antibioticos, S.A. | Process for producing 6-amino-penicillanic acid and phenylacetic acid |
| CN103214498A (en) * | 2013-04-20 | 2013-07-24 | 河北美邦工程科技有限公司 | Penicillin fermentation broth treating technology |
| CN103214498B (en) * | 2013-04-20 | 2015-03-11 | 河北美邦工程科技有限公司 | Penicillin fermentation broth treating technology |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1052727C (en) | 2000-05-24 |
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| CF01 | Termination of patent right due to non-payment of annual fee |