CN101648981A - Extraction and refinement process of lincomycin - Google Patents
Extraction and refinement process of lincomycin Download PDFInfo
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- CN101648981A CN101648981A CN200910307487A CN200910307487A CN101648981A CN 101648981 A CN101648981 A CN 101648981A CN 200910307487 A CN200910307487 A CN 200910307487A CN 200910307487 A CN200910307487 A CN 200910307487A CN 101648981 A CN101648981 A CN 101648981A
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Abstract
The invention discloses an extraction and refinement process of lincomycin for reducing the content of a component B. In the extraction and refinement process, the pH of a water dissolution liquid ofa lincomycin crude product extracted by a a lincomycin fermented filtering liquid or a solvent or a water solution for recycling the crude product by using active carbon particle column through NaOH for adsorption, and deabsorption is adopted by using n-butyl alcohol. By adopting the new extraction and refinement process of lincomycin for reducing the content of the component B, to the invention improves the traditional technology or the apparatus, reduces the environmental pollution, is beneficial for biochemical performance of waste water, increases the absorption volume of the lincomycin, saves two procedures of regeneration of acid-alkali, greatly reduces the labor intensity and the production cost, and is beneficial for large scale industrial production.
Description
Affiliated technical field
The invention belongs to pharmaceutical chemistry technical field, particularly relate to the extraction and purification process that a kind of lincomycin reduces the B component concentration.
Background technology
The extraction traditional handicraft of fermented filtrate of lincomycin is to extract with solvent.The B constituent content of finished product is relatively higher when wherein extracting lincomycin with butanols, and the clinical practice of its derivative is had very big side effect, and is particularly bigger to renal function; When extracting with higher alcohols, though reduce certain B constituent content, yield instability, and working condition and environmental condition are all relatively poor, and so that process the activated sludge of its waste water and poison and lost efficacy; When extracting with resin method, though reduce the B constituent content, because resin need to be processed with the regeneration of soda acid two procedures, simultaneously, the capacity of the absorption of resin is littler, and desorb unit is concentrated, makes the production cost increase bigger.
Summary of the invention
For above-mentioned situation, for overcoming the defective of prior art, the objective of the invention is to propose the extraction and purification process that a kind of new lincomycin reduces the B constituent content, improved traditional technology or equipment; Reduced the pollution of environment, be conducive to waste water can be biochemical performance; Increased the adsorption capacity to lincomycin, and desorb unit is concentrated, simultaneously, also saves with the regeneration of soda acid two procedures and process, reduced widely labour intensity and production cost, be conducive to big industrial scale.
For achieving the above object, lincomycin extraction and purification process of the present invention, this technology be with the activated carbon granule pillar to lincomycin fermentation liquid through oxalic acid acidifying, filtration, get acidifying filtrate; Or the lincomycin crude product that extracts with solvent or reclaim crude product all after the purified water-soluble solution, get the lincomycin lysate; Above-mentioned lincomycin acidifying filtrate or lysate after NaOH transfers pH, directly be adsorbed to the active carbon pillar saturated, and with the extraction process of n-butanol parsing.
Lincomycin extraction and purification process of the present invention specifically may further comprise the steps:
1., will transfer the pH2.0-3.5 after-filtration through the oxalic acid acidifying to lincomycin fermentation liquid, its filtrate transfers PH between 8.5-10.0 with 8mol/LNaOH again, alkaline solution;
2., above-mentioned alkaline solution is pumped into the pillar that activated carbon granule is housed, according to required flow 1-2BV control, and it is saturated to reach activated carbon granule absorption;
3., be that the alkaline detergent solution of 10-11.5 carries out continuous washing to adsorbing saturated activated carbon granule pillar with PH, and in time detect the content of scrub raffinate B component with HPLC;
4., contain in the waste liquid in the time of will adsorbing and should in time go here and there post absorption after the optically-active unit, and detect the discharging that unit controls tandem post waste liquid by polarimeter; Also can detect the height that the tandem post flows out the B constituent content of waste liquid by HPLC and control discharging;
5., will adsorb saturated active carbon pillar and carry out directly concentrating the decolouring crystallization after the desorb with neutral or alkaline n-butanol, get lincomycin; Maybe will adsorb saturated active carbon pillar and carry out azeotropic crystalization after the desorb, decolouring, acetone recrystallization with neutral or alkaline n-butanol, and lincomycin; After maybe will adsorbing saturated active carbon pillar and carrying out desorb with neutral or alkaline n-butanol, hydrochloric acid is stripped, and gets anti-stripping agent, concentrate again, decolouring, acetone crystallization, and lincomycin;
6., the activated carbon granule pillar after the desorb, be that the 4.0-5.5 acidic aqueous solution enters from the bottom with HClpH, the top effluxes the transition of carrying out gac, with standby;
7., again use above-mentioned tandem post as adsorption column, simultaneously, the former adsorption column after transition is become the tandem post, and repeat 1. to arrive operating procedure 6..
Adsorption column described above and tandem post can be the void towers of a kind of column type or square, and its inside can be the activated carbon granule of filling same model activated carbon granule or different model, also distribution grid can be set in the post, and distribution grid can be set.
Simultaneously, the lincomycin crude product that also can extract with solvent or reclaim crude product all with after the purified water dissolving gets the lincomycin lysate; Directly refining with extracting of active carbon pillar absorption lincomycin after NaOH transfers pH above-mentioned lincomycin lysate.
Extraction and purification process according to the invention provides new lincomycin reduction B constituent content has improved traditional technology or equipment; Reduced the pollution of environment, be conducive to waste water can be biochemical performance; Increased the adsorption capacity to lincomycin, and desorb unit is concentrated, simultaneously, also saves with the regeneration of soda acid two procedures and process, reduced widely labour intensity and production cost, be conducive to big industrial scale.
Embodiment
Lincomycin extraction and purification process of the present invention, this technology be with the activated carbon granule pillar to lincomycin fermentation liquid through oxalic acid acidifying, filtration, get acidifying filtrate; Or the lincomycin crude product that extracts with solvent or reclaim crude product all after the purified water-soluble solution, get the lincomycin lysate; Above-mentioned lincomycin acidifying filtrate or lysate after NaOH transfers pH, directly be adsorbed to the active carbon pillar saturated, and with the extraction process of n-butanol parsing.
Lincomycin extraction and purification process of the present invention specifically may further comprise the steps:
1., will transfer the pH2.0-3.5 after-filtration through the oxalic acid acidifying to lincomycin fermentation liquid, its filtrate transfers PH between 8.5-10.0 with 8mol/LNaOH again, alkaline solution;
2., above-mentioned alkaline solution is pumped into the pillar that activated carbon granule is housed, according to required flow 1-2BV control, and it is saturated to reach activated carbon granule absorption;
3., be that the alkaline detergent solution of 10-11.5 carries out continuous washing to adsorbing saturated activated carbon granule pillar with PH, and in time detect the content of scrub raffinate B component with HPLC;
4., contain in the waste liquid in the time of will adsorbing and should in time go here and there post absorption after the optically-active unit, and detect the discharging that unit controls tandem post waste liquid by polarimeter; Also can detect the height that the tandem post flows out the B constituent content of waste liquid by HPLC and control discharging;
5., will adsorb saturated active carbon pillar and carry out directly concentrating the decolouring crystallization after the desorb with neutral or alkaline n-butanol, get lincomycin; Maybe will adsorb saturated active carbon pillar and carry out azeotropic crystalization after the desorb, decolouring, acetone recrystallization with neutral or alkaline n-butanol, and lincomycin; After maybe will adsorbing saturated active carbon pillar and carrying out desorb with neutral or alkaline n-butanol, hydrochloric acid is stripped, and gets anti-stripping agent, concentrate again, decolouring, acetone crystallization, and lincomycin;
6., the activated carbon granule pillar after the desorb, be that the 4.0-5.5 acidic aqueous solution enters from the bottom with HClpH, the top effluxes the transition of carrying out gac, with standby;
7., again use above-mentioned tandem post as adsorption column, simultaneously, the former adsorption column after transition is become the tandem post, and repeat 1. to arrive operating procedure 6..
Adsorption column described above and tandem post can be the void towers of a kind of column type or square, and its inside can be the activated carbon granule of filling same model activated carbon granule or different model, also distribution grid can be set in the post, and distribution grid can be set.
Simultaneously, the lincomycin crude product that also can extract with solvent or reclaim crude product all with after the purified water dissolving gets the lincomycin lysate; Directly refining with extracting of active carbon pillar absorption lincomycin after NaOH transfers pH above-mentioned lincomycin lysate.
Extraction and purification process according to the invention provides new lincomycin reduction B constituent content has improved traditional technology or equipment; Reduced the pollution of environment, be conducive to waste water can be biochemical performance; Increased the adsorption capacity to lincomycin, and desorb unit is concentrated, simultaneously, also saves with the regeneration of soda acid two procedures and process, reduced widely labour intensity and production cost, be conducive to big industrial scale.
Claims (3)
1. lincomycin extraction and purification process, this technology be with the activated carbon granule pillar to lincomycin fermentation liquid through oxalic acid acidifying, filtration, get acidifying filtrate; Or the lincomycin crude product that extracts with solvent or reclaim crude product all after the purified water-soluble solution, get the lincomycin lysate; Above-mentioned lincomycin acidifying filtrate or lysate after NaOH transfers pH, directly be adsorbed to the active carbon pillar saturated, and with the extraction process of n-butanol parsing.
2. lincomycin extraction and purification process according to claim 1 is characterized in that this extraction and purification process specifically may further comprise the steps:
1., will transfer the pH2.0-3.5 after-filtration through the oxalic acid acidifying to lincomycin fermentation liquid, its filtrate transfers PH between 8.5-10.0 with 8mol/LNaOH again, alkaline solution;
2., above-mentioned alkaline solution is pumped into the pillar that activated carbon granule is housed, according to required flow 1-2BV control, and it is saturated to reach activated carbon granule absorption;
3., be that the alkaline detergent solution of 10-11.5 carries out continuous washing to adsorbing saturated activated carbon granule pillar with PH, and in time detect the content of scrub raffinate B component with HPLC;
4., contain in the waste liquid in the time of will adsorbing and should in time go here and there post absorption after the optically-active unit, and detect the discharging that unit controls tandem post waste liquid by polarimeter; Also can detect the height that the tandem post flows out the B constituent content of waste liquid by HPLC and control discharging;
5., will adsorb saturated active carbon pillar and carry out directly concentrating the decolouring crystallization after the desorb with neutral or alkaline n-butanol, get lincomycin; Maybe will adsorb saturated active carbon pillar and carry out azeotropic crystalization after the desorb, decolouring, acetone recrystallization with neutral or alkaline n-butanol, and lincomycin; After maybe will adsorbing saturated active carbon pillar and carrying out desorb with neutral or alkaline n-butanol, hydrochloric acid is stripped, and gets anti-stripping agent, concentrate again, decolouring, acetone crystallization, and lincomycin;
6., the activated carbon granule pillar after the desorb, be that the 4.0-5.5 acidic aqueous solution enters from the bottom with HClpH, the top effluxes the transition of carrying out gac, with standby;
7., again use above-mentioned tandem post as adsorption column, simultaneously, the former adsorption column after transition is become the tandem post, and repeat 1. to arrive operating procedure 6..
3. lincomycin extraction and purification process according to claim 2 is characterized in that described adsorption column and tandem post, is the void tower of a kind of cylinder shape or square, the inner activated carbon granule of filling.
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| CN200910307487A CN101648981A (en) | 2009-09-22 | 2009-09-22 | Extraction and refinement process of lincomycin |
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| CN200910307487A CN101648981A (en) | 2009-09-22 | 2009-09-22 | Extraction and refinement process of lincomycin |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102746348A (en) * | 2011-04-19 | 2012-10-24 | 上海医药工业研究院 | Method for separation of lincomycin |
| CN104910324A (en) * | 2015-07-03 | 2015-09-16 | 武汉工程大学 | Method for producing lincomycin molecularly imprinted polymer |
| CN105111254A (en) * | 2015-10-17 | 2015-12-02 | 霍进铭 | Extraction method of lincomycin |
| CN105237593A (en) * | 2015-11-17 | 2016-01-13 | 宁夏泰益欣生物科技有限公司 | Lincomycin hydrochloride extraction method |
| 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 |
-
2009
- 2009-09-22 CN CN200910307487A patent/CN101648981A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104910324A (en) * | 2015-07-03 | 2015-09-16 | 武汉工程大学 | Method for producing lincomycin molecularly imprinted polymer |
| CN105111254A (en) * | 2015-10-17 | 2015-12-02 | 霍进铭 | Extraction method of lincomycin |
| CN105237593A (en) * | 2015-11-17 | 2016-01-13 | 宁夏泰益欣生物科技有限公司 | Lincomycin hydrochloride extraction method |
| CN105237593B (en) * | 2015-11-17 | 2019-05-24 | 宁夏泰益欣生物科技有限公司 | Lincomycin Hydrochloride extracting method |
| 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 |
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Application publication date: 20100217 |