CN1263097A - Technological process for extracting penicillin from fermented filtrate - Google Patents
Technological process for extracting penicillin from fermented filtrate Download PDFInfo
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- CN1263097A CN1263097A CN 00100114 CN00100114A CN1263097A CN 1263097 A CN1263097 A CN 1263097A CN 00100114 CN00100114 CN 00100114 CN 00100114 A CN00100114 A CN 00100114A CN 1263097 A CN1263097 A CN 1263097A
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Abstract
The technological process for extracting penicillin from fermented filtrate is characterized by using penicillin fermented filtrate as raw material, using sulfuric acid solution to regulate pH value, adding butyl acetate or alcohols solvent to make extraction, then washing extracted organic phase and using centrifuge to make washed organic phase and soda lye undergo the process of three-stage back-extraction, azeotropic crystallizing the back-extract with butyl alcohol and drying so as to obtain the invented product. Said invention is simple in operation, and its yield is raised.
Description
The present invention relates to a kind of technology of from ferment filtrate, extracting penicillin, belong to pharmaceutical chemistry technical field.
From ferment filtrate, extract penicillin, comprise extraction, washing, reextraction and azeotropic crystalization.In leaching process, traditional technology is that ferment filtrate and solvent are extracted and washing with whizzer, and reextraction afterwards then is an intermittent type cross-flow operation of using standing demix in stirred autoclave.Be about to organic phase and in stirred autoclave, carry out the reextraction cross-flow operation of standing demix with buck.The shortcoming of this process is:
1, technological operation complexity.
2, operation pH value is generally higher, causes the penicillin degraded.
3, the batch operation interface thing of standing demix is many, and efficient is low, and yield is low.
4, the fault of operator's people mistake is big, and loss is big.
5, operational condition and environment are poor.
Penicillin is a kind ofly to meet the microbiotic that soda acid is very easily degraded, and leaching process must carry out in soda acid, thereby requires operating process as quickly as possible, and the time is short as far as possible, and operation balance pH is as far as possible near neutral, particularly high more should be like this when dense.And the processing of interface thing bothers and causes damage, and is a disagreeable operation.So quality, yield do not guarantee, total recovery is mostly below about 70%.Thereby, need improve.
The objective of the invention is to propose a kind of technology of from ferment filtrate, extracting penicillin, improve traditional technology and equipment, make it to simplify the operation, improve yield, improve work situation.
The technology of from ferment filtrate, extracting penicillin that the present invention proposes, form by following each step:
(1) be raw material with penicillin fermentation filtrate, transfer pH with sulphuric acid soln, add N-BUTYL ACETATE or alcohols mixed solvent and extract, filtrate is 2～5: 1 with the ratio of solvent phase, and balance pH value is 2～3, and service temperature is 15 ℃～25 ℃;
(2) extracted organic phase of the above-mentioned the first step is at room temperature carried out one-level or secondary washing with whizzer, organic phase is 5～12: 1 with the ratio of water;
(3) organic phase after the above-mentioned washing and buck are at room temperature carried out three grades of continuous countercurrent reextractions with whizzer and get, balance pH value is 6.6～7.2, and organic phase is 5～30: 1 with the ratio of buck;
(4) with above-mentioned anti-stripping agent through crystallization of n-butanol azeotropic, drying, be penicillin salt product of the present invention.
Alcohols mixed solvent in the above-mentioned the first step is an isooctyl alcohol, the mixed solvent of one or more and other solvent composition in secondary octanol, the n-Octanol.Buck in above-mentioned the 3rd step is any aqueous solution in salt of wormwood, saleratus or yellow soda ash, the sodium bicarbonate.
Use preparation method of the present invention,, substitute the intermittent type cross-flow operation process of the standing demix of tradition use owing to carry out the reextraction operation of continuous countercurrent with centrifugal extractor, thereby simplified the origin operation process greatly, improve yield, reduced labour intensity, improved operational condition and work situation.Simultaneously, because under centrifugal action, two are separated better, carry minimizing secretly, have not only reduced solvent loss, and have improved quality product.
Because counter-current operation, the pH value of the first step of stripping at high density penicillin is lower, thus significantly reduced the degraded of penicillin, thus improved yield and quality.
After experiment showed, the employing whizzer, the emulsion layer that has been produced in the reextraction process when having eliminated with standing demix has been eliminated the loss that brings because of emulsification.Simultaneously, make extraction, washing, reextraction form the successive counter-current operation, shortened the operating time, and be that further detection and automatic control lay the foundation automatically.
Introduce embodiments of the invention below:
Embodiment 1
Annulus type centrifugal extractor with 20 millimeters rotary drums of Φ carries out continuous countercurrent extraction, washing, reextraction experiment, and rotating speed is 2600 rev/mins, and temperature is a room temperature.
The penicillin analog material liquid (tire is 20000 units/ml) transfer pH with sulphuric acid soln, is 3 compare with centrifugal extractor carry out 3 grade extractions by filtrate than solvent with the isooctyl alcohol mixed solvent, balance pH is 3, solvent phase concentration is 56400 units/ml, carry out the secondary washing continuously, solvent is 10 with the ratio of washing water, and it is 2450 units/ml that washings is tired, the set out ferment filtrate extraction of this washings.Solvent after the washing carries out three grades of continuous countercurrent reextraction extract operations with wet chemical again, balance pH6.9, and solvent is 12 with the ratio of buck, and anti-stripping agent concentration is 660900 units/ml, and useless organic phase concentration is 624 units/ml.
Anti-stripping agent gets potassium salt of penicillin after crystallization of n-butanol azeotropic, drying, tiring is 1560 units/mg, up-to-standard.
Embodiment 2
Annulus type centrifugal extractor with 20 millimeters rotary drums of Φ carries out continuous extraction, washing, reextraction experiment, and rotating speed is 2600 rev/mins, and temperature is a room temperature.
Penicillin fermentation filtrate (tire is 17500 units/ml) transfer pH with sulphuric acid soln, is 2.5 compare carry out three grade Centrifugical extractions by filtrate than solvent with N-BUTYL ACETATE, balance pH is 2.8, solvent phase concentration is 39800 units/ml, carry out the one-level washing, solvent is 10 with the ratio of washings, and it is 2800 units/ml that washing water are tired, the set out ferment filtrate extraction of this washings.Solvent after the washing carries out three grades of continuous countercurrent reextraction extract operations with potassium bicarbonate aqueous solution again, balance pH7.1, and solvent is 15 with the ratio of buck, and anti-stripping agent concentration is 615000 units/ml, and useless organic phase concentration is 580 units/ml.
Anti-stripping agent is through crystallization of n-butanol azeotropic, the dry potassium salt of penicillin that gets, and tiring is 1545 units/mg, up-to-standard.
Embodiment 3
Annulus type centrifugal extractor with 20 millimeters rotary drums of Φ carries out continuous extraction, washing, reextraction experiment, and rotating speed is 2600 rev/mins, and temperature is a room temperature.
Penicillin fermentation filtrate (tire is 17500 units/ml) transfer pH with sulphuric acid soln, is 2.5 compare carry out three grade Centrifugical extractions by filtrate than solvent with N-BUTYL ACETATE, solvent phase concentration is 39800 units/ml, carry out the secondary washing, solvent is 10 with the ratio of washings, it is 2800 units/ml that washing water are tired, the set out ferment filtrate extraction of this washings.Solvent after the washing carries out three grades of continuous countercurrent reextraction extract operations with saturated aqueous sodium carbonate again, balance pH7.1, and solvent is 15 with the ratio of buck, and anti-stripping agent concentration is 615000 units/ml, and useless organic phase concentration is 580 units/ml.
Anti-stripping agent is through crystallization of n-butanol azeotropic, the dry penicillin sodium salt that gets, and tiring is 1645 units/mg, up-to-standard.
Claims (4)
1, a kind of technology of extracting penicillin from ferment filtrate comprises following each step:
(1) be raw material with penicillin fermentation filtrate, transfer pH with sulphuric acid soln, add N-BUTYL ACETATE or alcohols mixed solvent and extract, filtrate is 2～5: 1 with the ratio of solvent phase, and balance pH value is 2～3, and service temperature is 15 ℃～25 ℃;
(2) extracted organic phase of the above-mentioned the first step is at room temperature carried out one-level or secondary washing with whizzer, organic phase is 5～12: 1 with the ratio of water;
It is characterized in that, also comprise:
(3) organic phase after the above-mentioned washing and buck are at room temperature carried out three grades of continuous countercurrent reextractions with whizzer and get, balance pH value is 6.6～7.2, and organic phase is 5～30: 1 with the ratio of buck;
(4) with above-mentioned anti-stripping agent through crystallization of n-butanol azeotropic, drying, be penicillin salt product of the present invention.
2, technology as claimed in claim 1 is characterized in that, wherein said alcohols mixed solvent is an isooctyl alcohol, the mixed solvent of one or more and other solvent in secondary octanol, the n-Octanol.
3, technology as claimed in claim 1 is characterized in that, wherein said buck is any solution in salt of wormwood, saleratus or yellow soda ash, the sodium bicarbonate.
4, technology as claimed in claim 1 is characterized in that, wherein said whizzer can be annulus type centrifugal extractor, butterfly chip whizzer and other kinds centrifugal extractor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00100114 CN1263097A (en) | 2000-01-11 | 2000-01-11 | Technological process for extracting penicillin from fermented filtrate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00100114 CN1263097A (en) | 2000-01-11 | 2000-01-11 | Technological process for extracting penicillin from fermented filtrate |
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| CN1263097A true CN1263097A (en) | 2000-08-16 |
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| CN 00100114 Pending CN1263097A (en) | 2000-01-11 | 2000-01-11 | Technological process for extracting penicillin from fermented filtrate |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102070682A (en) * | 2011-01-07 | 2011-05-25 | 亓平言 | Novel process for extracting lincomycin by annular space centrifugal extractor |
| US7951555B2 (en) | 2004-05-18 | 2011-05-31 | Australian Nuclear Science And Technology Organisation | Membrane bioreactor |
| CN101487029B (en) * | 2009-02-20 | 2011-10-26 | 广东省微生物研究所 | Method and device for producing n-butyric acid by microbial catalysis |
| CN101747341B (en) * | 2008-12-09 | 2012-06-27 | 华北制药股份有限公司 | Method for producing penicillin V salt |
| CN103159782A (en) * | 2011-12-08 | 2013-06-19 | 胡先念 | Method for extracting penicillin from penicillin aqueous solution and applications thereof, and penicillin extraction method |
-
2000
- 2000-01-11 CN CN 00100114 patent/CN1263097A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7951555B2 (en) | 2004-05-18 | 2011-05-31 | Australian Nuclear Science And Technology Organisation | Membrane bioreactor |
| CN1989236B (en) * | 2004-05-18 | 2012-05-16 | 澳大利亚核科学技术组织 | Membrane bioreactor |
| CN101747341B (en) * | 2008-12-09 | 2012-06-27 | 华北制药股份有限公司 | Method for producing penicillin V salt |
| CN101487029B (en) * | 2009-02-20 | 2011-10-26 | 广东省微生物研究所 | Method and device for producing n-butyric acid by microbial catalysis |
| CN102070682A (en) * | 2011-01-07 | 2011-05-25 | 亓平言 | Novel process for extracting lincomycin by annular space centrifugal extractor |
| CN103159782A (en) * | 2011-12-08 | 2013-06-19 | 胡先念 | Method for extracting penicillin from penicillin aqueous solution and applications thereof, and penicillin extraction method |
| CN103159782B (en) * | 2011-12-08 | 2015-10-21 | 湖南中创化工股份有限公司 | The method of extracting penicillin and the extracting method of application and penicillin thereof from benzylpenicillin sodium solution |
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