CN101348508A - Albiotic purification process - Google Patents
Albiotic purification process Download PDFInfo
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- CN101348508A CN101348508A CNA2008102118657A CN200810211865A CN101348508A CN 101348508 A CN101348508 A CN 101348508A CN A2008102118657 A CNA2008102118657 A CN A2008102118657A CN 200810211865 A CN200810211865 A CN 200810211865A CN 101348508 A CN101348508 A CN 101348508A
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- resin column
- lincomycin
- component
- purifying
- butanols
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Abstract
The invention relates to a purification technology for reducing the component B in Lincomycin. The purification technology is to use a resin column to carry out a purification of an extract of butanol. A ferment filtrate of Lincomycin can also be used for extraction and purification of Lincomycin directly.
Description
The present invention relates to the purifying process that a kind of lincomycin reduces the B component, belong to pharmaceutical chemistry technical field.
The extraction of lincomycin fermentation liquid, traditional technology are to extract with butanols.
Use the butyl alcohol extraction lincomycin, its crystalline product B ratio of component is higher.The B component is a kind of toxic ingredient in the lincomycin, needs to remove.Technology described in inventor's patent ZL200510084312.6 and the ZL98100065.7 also is the purifying process that several lincomycins reduce the B component; The shortcoming of these processes is:
1, alcoholic solvent scent of, operational condition and environment are poor.
2, containing pure waste water can't handle, and waste water can't be up to standard.
3, organic acid operation interface thing is many, influences yield.
Thereby, be necessary to improve.
The objective of the invention is to propose the purifying process that a kind of new lincomycin reduces the B component, improve traditional technology and equipment, improve operating environment.
The lincomycin that the present invention proposes reduces the purifying process of B component, by following each step
Form:
1. the sour strip liquor of lincomycin butyl alcohol extraction or the aqueous solution after the dissolving of butyl alcohol extraction coarse-grain product are transferred more than the pH9;
2. the above-mentioned aqueous solution is slowly squeezed into resin column from the adsorption resin column capital by required flow;
3. prepare washing water, slowly squeeze into from the adsorption resin column capital, carry out continuous washing by required flow;
4. the waste water after the washing goes out from the post underflow, and enters the recovery resin column from reclaiming the resin column capital, emits discharging again at the bottom of this post;
5. adsorption resin column with the butanols desorb after directly condensing crystal get product; Or the butanols desorb gets product again after sour back extraction gets strip liquor after the acetone crystallization.
6. do adsorption resin column with above-mentioned recovery resin column again, former adsorption resin column is done the recovery resin column, repeats 1. to arrive process 5..
Above-mentioned described adsorption resin column and reclaim resin column all is a kind of garden column type void tower, potting resin and form, and in the post grid distributor can be installed.
Equally, also can replace the above-mentioned strip liquor or the aqueous solution to carry out the extraction purifying of lincomycin with ferment filtrate.
Use purification process of the present invention, reduced labour intensity, improved operational condition and work situation.
Introduce embodiments of the invention below:
Embodiment 1
Resin column diameter ф 50mm, high 2m; Adsorb under the normal temperature and wash.
The lincomycin butanol crystallizing coarse-grain aqueous solution (8000u/ml that tires, B component 5%) is slowly squeezed into resin column absorption by 1 liter of/hour flow from the adsorption resin column capital, uses the pH10.5 washing water again, carries out drip washing by 1 liter of/hour flow from capital; Washing water then go out from the post underflow, remove to reclaim resin column.Enter from the adsorption column capital with butanols again and carry out desorb, from the post underflow go out the butanols stripping liquid.The butanols stripping liquid gets product behind condensing crystal.Record the butanols stripping liquid 52500u/ml that tires; Crystalline product is qualified, total recovery 85%, and B component 1.3%.
Embodiment 2
Resin column diameter ф 100mm, high 3m; Adsorb under the normal temperature and wash.Be equipped with one deck grid distributor in the tower.
The hydrochloric acid anti-stripping agent of lincomycin butanols liquid (15000u/ml that tires, B component 4.5%) behind the accent pH10, is slowly squeezed into resin column absorption by 3 liters of/hour flows from the adsorption resin column capital, uses the pH10 washing water again, carries out drip washing by 3T/ hour flow from capital; Washing water then go out from the post underflow, remove to reclaim resin column.Enter from the adsorption column capital with butanols again and carry out desorb, from the post underflow go out the butanols stripping liquid.The butanols stripping liquid is stripped through hydrochloric acid, gets product after the acetone crystallization.Record the butanols stripping liquid 105000u/ml that tires; Crystalline product is qualified, total recovery 90%, and B component 0.5%.
Embodiment 3
Resin column diameter ф 100mm, high 3m; Adsorb under the normal temperature and wash.
Fermented filtrate of lincomycin (8000u/ml that tires, B component 5.3%) behind the accent pH10, is slowly squeezed into resin column absorption by 3 liters of/hour flows from capital, uses the pH10 washing water again, carries out drip washing by 3 liters of/hour flows from capital; Washing water then go out from the post underflow.Carry out desorb with butanols from capital again, from the post underflow go out the butanols stripping liquid.The butanols stripping liquid is stripped through hydrochloric acid, gets product after the acetone crystallization.Record the butanols stripping liquid 32000u/ml that tires; Crystalline product is qualified, total recovery 75%, and B component 0.7%.
Claims (4)
1. the purifying process of a lincomycin reduction B component is characterized in that this technology is the purifying that carries out the butyl alcohol extraction product with resin column.
2. lincomycin according to claim 1 reduces the purifying process of B component, it is characterized in that its technology is as follows:
1. the sour strip liquor of lincomycin butyl alcohol extraction or the aqueous solution after the dissolving of butyl alcohol extraction coarse-grain product are transferred more than the pH9;
2. the above-mentioned aqueous solution is slowly squeezed into resin column from the adsorption resin column capital by required flow;
3. prepare washing water, slowly squeeze into from the adsorption resin column capital, carry out continuous washing by required flow;
4. the waste water after the washing goes out from the post underflow, and enters the recovery resin column from reclaiming the resin column capital, emits discharging again at the bottom of this post;
5. adsorption resin column with the butanols desorb after directly condensing crystal get product; Or the butanols desorb gets product again after sour back extraction gets strip liquor after the acetone crystallization.
6. do adsorption resin column with above-mentioned recovery resin column again, former adsorption resin column is done the recovery resin column, repeats 1. to arrive process 5..
3. lincomycin according to claim 1 reduces the purifying process of B component, it is characterized in that can filling polymeric adsorbent in the post of this resin column, also can filling ion-exchange resin; Can be empty, also can add various grid distributors.
4. lincomycin according to claim 1 reduces the purifying process of B component, it is characterized in that also can replacing the above-mentioned strip liquor or the aqueous solution to carry out the extraction purifying of lincomycin with ferment filtrate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008102118657A CN101348508A (en) | 2008-09-11 | 2008-09-11 | Albiotic purification process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008102118657A CN101348508A (en) | 2008-09-11 | 2008-09-11 | Albiotic purification process |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101348508A true CN101348508A (en) | 2009-01-21 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2008102118657A Pending CN101348508A (en) | 2008-09-11 | 2008-09-11 | Albiotic purification process |
Country Status (1)
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102002079A (en) * | 2010-05-21 | 2011-04-06 | 北京华致信诚科技有限公司 | Production process for reducing component B content of lincomycin |
| CN102633846A (en) * | 2012-04-09 | 2012-08-15 | 南阳普康药业有限公司 | Lincomycin purification method |
| CN102746348A (en) * | 2011-04-19 | 2012-10-24 | 上海医药工业研究院 | Method for separation of lincomycin |
| CN104356179A (en) * | 2014-10-15 | 2015-02-18 | 江西国药有限责任公司 | Lincomycin hydrochloride purification technology |
| CN108801725A (en) * | 2018-04-03 | 2018-11-13 | 新宇药业股份有限公司 | The preparation method of B component reference substance in a kind of Lincomycin Hydrochloride |
| CN110746473A (en) * | 2018-07-10 | 2020-02-04 | 浙江华谱新创科技有限公司 | Purification process for reducing content of lincomycin B component |
| CN111116686A (en) * | 2019-12-17 | 2020-05-08 | 丽珠集团新北江制药股份有限公司 | Preparation method of lincomycin hydrochloride component B |
-
2008
- 2008-09-11 CN CNA2008102118657A patent/CN101348508A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102002079A (en) * | 2010-05-21 | 2011-04-06 | 北京华致信诚科技有限公司 | Production process for reducing component B content of lincomycin |
| CN102002079B (en) * | 2010-05-21 | 2013-01-30 | 北京华致信诚科技有限公司 | Production process for reducing component B content of lincomycin |
| CN102746348A (en) * | 2011-04-19 | 2012-10-24 | 上海医药工业研究院 | Method for separation of lincomycin |
| CN102746348B (en) * | 2011-04-19 | 2016-04-20 | 上海医药工业研究院 | A kind of separation method of lincomycin |
| CN102633846A (en) * | 2012-04-09 | 2012-08-15 | 南阳普康药业有限公司 | Lincomycin purification method |
| CN104356179A (en) * | 2014-10-15 | 2015-02-18 | 江西国药有限责任公司 | Lincomycin hydrochloride purification technology |
| CN104356179B (en) * | 2014-10-15 | 2017-11-21 | 江西国药有限责任公司 | A kind of Lincomycin Hydrochloride purifying technique |
| CN108801725A (en) * | 2018-04-03 | 2018-11-13 | 新宇药业股份有限公司 | The preparation method of B component reference substance in a kind of Lincomycin Hydrochloride |
| CN110746473A (en) * | 2018-07-10 | 2020-02-04 | 浙江华谱新创科技有限公司 | Purification process for reducing content of lincomycin B component |
| CN110746473B (en) * | 2018-07-10 | 2021-08-24 | 浙江华谱新创科技有限公司 | Purification process for reducing content of lincomycin B component |
| CN111116686A (en) * | 2019-12-17 | 2020-05-08 | 丽珠集团新北江制药股份有限公司 | Preparation method of lincomycin hydrochloride component B |
| CN111116686B (en) * | 2019-12-17 | 2022-12-20 | 丽珠集团新北江制药股份有限公司 | Preparation method of lincomycin hydrochloride component B |
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Application publication date: 20090121 |