CN105111254A - Extraction method of lincomycin - Google Patents
Extraction method of lincomycin Download PDFInfo
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- CN105111254A CN105111254A CN201510668303.5A CN201510668303A CN105111254A CN 105111254 A CN105111254 A CN 105111254A CN 201510668303 A CN201510668303 A CN 201510668303A CN 105111254 A CN105111254 A CN 105111254A
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- lincomycin
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Abstract
The invention discloses an extraction method of lincomycin. A lincomycin fermentation solution is filtered through a ceramic film with pore diameters ranging from 0.01 mu m to 0.1 mu m after the pH (potential of hydrogen) of the lincomycin fermentation solution is adjusted to 2.0-4.5, then an acid aqueous solution with the pH ranging from 2.0 to 4.0 is used for washing the ceramic film repeatedly, filter liquor is discarded, a hydrochloric acid aqueous solution with the pH ranging from 8 to 10 is used for washing the ceramic film repeatedly, purified water is added for dissolution, and a lincomcin aqueous solution is obtained. Clear filter liquor is obtained after filtration of the ceramic film, a destaining solution and a desorbed solution can be both used for production of the next batch of lincomycin, the utilization rate of raw materials can be increased, meanwhile, the ultimate yield of the next batch of products can be further increased, and the extraction method has the advantages that a precipitation method is simple and convenient and a technological process is applicable to large-scale production.
Description
Technical field
The present invention relates to lincomycin intermediate processing technical field, particularly relate to a kind of extracting method of lincomycin.
Background technology
Lincomycin is first product that a class is called cyclic ester Tai Lei new antibiotic family.It is from streptomyces parvus (
streptomycesparvus) the central Cyclic lipopeptide antibiotic extracting the novel structure of 13 the amino acid compositions obtained of fermented liquid, wherein ten Amino acid profile ring texturees, in the outer capric acid of ring and tryptophane generation esterification.It not only has novel chemical structure, and its binding mode is also from arbitrary to have got permission microbiotic different.It can destroy bacterial cell membrane function in many aspects, kills gram positive organism rapidly thus.Lincomycin decapacitation acts on outside most of clinical relevant gram positive organism, the more important thing is in vitro in X-1497 (methicillin), the resistance isolated strains such as vancomycin and Linezolid still has a strong active.
Lincomycin is tunning, the ferment filtrate obtained by fermentation culture, a large amount of pigments can be produced in fermenting process and with the akin by product of lincomycin structure as the lincomycin that dewaters, therefore the extracting and purifying method of lincomycin is more complicated.General lincomycin producing strain, throughput is unstable, and output is lower, fermentation byproduct is more, and impurity is more, causes rear extraction work comparatively complicated, substantially increase the purification difficulty of postorder, be difficult to obtain highly purified final product, thus cannot industrialization produce.
Many reported in literature have been had to the extracting and purifying method of lincomycin postorder, " a kind of preparation method of high-purity lincomycin " of such as Anhui Fengyuan Fermentation Technology Engineering Research Co., Ltd.'s application, disclosed in it, roughly technique is: fermentation liquor ultrafiltration, nanofiltration, resin cation (R.C.) absorption pickling, resin anion(R.A) neutralization, nanofiltration is concentrated, crystallization.Membrane filtration yield reaches 98-99%, and product purity after crystallization also can obtain more than 98.5%.But lincomycin is an amphiprotic substance, iso-electric point is about pH4-5, under different pH conditions, its solvability is different, especially lincomycin has a large amount of homologues, isomer, and these impurity are very similar to lincomycin in nature, therefore, by so simple technique, industrially want separation and purification even crystallization lincomycin be very difficult.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of extracting method of lincomycin is provided.
Technical scheme of the present invention is as follows: the extracting method that the invention provides a kind of lincomycin, comprises the following steps:
A, lincomycin fermentation liquid to be regulated after pH2.0-4.5, filter with the ceramic membrane that membrane pore size is 0.01 μm-0.1 μm, then the acidic aqueous solution circulation cleaning ceramic membrane of pH2.0-4.0 is used, abandon filtrate, use the aqueous hydrochloric acid circulation cleaning ceramic membrane of pH8-10 again, add pure water to dissolve, obtain the lincomycin aqueous solution;
B, the lincomycin aqueous solution obtained is added discoloring agent decolour in step a, decolour after filtering complete, press-in stoste obtains destainer in filling with;
C, the post destainer obtained by step b add saturated propyl carbinol and resolve, and control to resolve flow velocity, and the desorbed solution detecting resin column outlet is tired, and desorbed solution is collected into desorbed solution hold-up vessel, when tiring lower than when resolving terminal of desorbed solution, stop collecting; Continuing to resolve with saturated propyl carbinol, desorbed solution is collected into low liter desorbed solution hold-up vessel, when detecting that desorbed solution is without when tiring, stopping resolving;
The desorbed solution of d, gained carries out concentrating under reduced pressure, adds salt acid crystal after obtaining concentrated solution, obtains hydrochloric acid xln, adds acetone recrystallization, obtain finished product after drying at hydrochloric acid xln.
The present invention is preferred, and according in step b, described discoloring agent is gac.
The present invention is preferred, described in have saturated propyl carbinol add-on to be 30%-50%.
The present invention is preferred, and according in steps d, crystallisation process starting temperature is 25 ~ 60 DEG C; Crystallisation process terminal temperature is 0 ~ 30 DEG C; Crystallisation process cooling rate is 0.5 ~ 5 DEG C/min.
Beneficial effect of the present invention is as follows:
Adopt such scheme, the present invention passes through ceramic membrane filter, the clear filtrate obtained, and destainer and desorbed solution all can be used for the production of lower batch, can improve the utilization ratio of raw material, can also improve the ultimate capacity of lower batch product simultaneously; The present invention has the advantage that the easy and technical process of intermediate processing is applicable to produce in enormous quantities.
Accompanying drawing explanation
Fig. 1 is the schema of the extracting method of a kind of lincomycin of the present invention.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
Refer to Fig. 1, the invention provides a kind of extracting method of lincomycin, comprise the following steps:
A, lincomycin fermentation liquid to be regulated after pH2.0-4.5, filter with the ceramic membrane that membrane pore size is 0.01 μm-0.1 μm, then the acidic aqueous solution circulation cleaning ceramic membrane of pH2.0-4.0 is used, abandon filtrate, use the aqueous hydrochloric acid circulation cleaning ceramic membrane of pH8-10 again, add pure water to dissolve, obtain the lincomycin aqueous solution;
B, the lincomycin aqueous solution obtained is added discoloring agent decolour in step a, decolour after filtering complete, during press-in stoste is filled with, obtain destainer, described discoloring agent is gac;
C, the post destainer obtained by step b add saturated propyl carbinol and resolve, and control to resolve flow velocity, and the desorbed solution detecting resin column outlet is tired, and desorbed solution is collected into desorbed solution hold-up vessel, when tiring lower than when resolving terminal of desorbed solution, stop collecting; Continue resolve with saturated propyl carbinol, desorbed solution is collected into low liter desorbed solution hold-up vessel, when detecting that desorbed solution is without when tiring, stop resolve, described in have saturated propyl carbinol add-on to be 30%-50%;
The desorbed solution of d, gained carries out concentrating under reduced pressure, adds salt acid crystal after obtaining concentrated solution, obtains hydrochloric acid xln, adds acetone recrystallization, obtain finished product after drying at hydrochloric acid xln, and crystallisation process starting temperature is 25 ~ 60 DEG C; Crystallisation process terminal temperature is 0 ~ 30 DEG C; Crystallisation process cooling rate is 0.5 ~ 5 DEG C/min.
embodiment one:
The present invention includes following steps:
A, lincomycin fermentation liquid to be regulated after pH3, filter with the ceramic membrane that membrane pore size is 0.05 μm, then use the acidic aqueous solution circulation cleaning ceramic membrane of pH3.0, abandon filtrate, use the aqueous hydrochloric acid circulation cleaning ceramic membrane of pH9 again, add pure water and dissolve, obtain the lincomycin aqueous solution;
B, the lincomycin aqueous solution obtained is added discoloring agent decolour in step a, decolour after filtering complete, during press-in stoste is filled with, obtain destainer, described discoloring agent is gac;
C, the post destainer obtained by step b add saturated propyl carbinol and resolve, and control to resolve flow velocity, and the desorbed solution detecting resin column outlet is tired, and desorbed solution is collected into desorbed solution hold-up vessel, when tiring lower than when resolving terminal of desorbed solution, stop collecting; Continue resolve with saturated propyl carbinol, desorbed solution is collected into low liter desorbed solution hold-up vessel, when detecting that desorbed solution is without when tiring, stop resolve, described in have saturated propyl carbinol add-on to be 40%;
The desorbed solution of d, gained carries out concentrating under reduced pressure, adds salt acid crystal after obtaining concentrated solution, obtains hydrochloric acid xln, adds acetone recrystallization, obtain finished product after drying at hydrochloric acid xln, and crystallisation process starting temperature is 40 DEG C; Crystallisation process terminal temperature is 20 DEG C; Crystallisation process cooling rate is 5 DEG C/min.
In sum, adopt such scheme, the present invention passes through ceramic membrane filter, the clear filtrate obtained, and destainer and desorbed solution all can be used for the production of lower batch, can improve the utilization ratio of raw material, can also improve the ultimate capacity of lower batch product simultaneously; The present invention has the advantage that the easy and technical process of intermediate processing is applicable to produce in enormous quantities.
These are only preferred embodiment of the present invention, be not limited to the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (4)
1. an extracting method for lincomycin, is characterized in that, comprises the following steps:
A, lincomycin fermentation liquid to be regulated after pH2.0-4.5, filter with the ceramic membrane that membrane pore size is 0.01 μm-0.1 μm, then the acidic aqueous solution circulation cleaning ceramic membrane of pH2.0-4.0 is used, abandon filtrate, use the aqueous hydrochloric acid circulation cleaning ceramic membrane of pH8-10 again, add pure water to dissolve, obtain the lincomycin aqueous solution;
B, the lincomycin aqueous solution obtained is added discoloring agent decolour in step a, decolour after filtering complete, press-in stoste obtains destainer in filling with;
C, the post destainer obtained by step b add saturated propyl carbinol and resolve, and control to resolve flow velocity, and the desorbed solution detecting resin column outlet is tired, and desorbed solution is collected into desorbed solution hold-up vessel, when tiring lower than when resolving terminal of desorbed solution, stop collecting; Continuing to resolve with saturated propyl carbinol, desorbed solution is collected into low liter desorbed solution hold-up vessel, when detecting that desorbed solution is without when tiring, stopping resolving;
The desorbed solution of d, gained carries out concentrating under reduced pressure, adds salt acid crystal after obtaining concentrated solution, obtains hydrochloric acid xln, adds acetone recrystallization, obtain finished product after drying at hydrochloric acid xln.
2. the extracting method of a kind of lincomycin according to claim 1, is characterized in that, according in step b, described discoloring agent is gac.
3. the extracting method of a kind of lincomycin according to claim 1, is characterized in that, described in have saturated propyl carbinol add-on to be 30%-50%.
4. the extracting method of a kind of lincomycin according to claim 1, is characterized in that, according in steps d, crystallisation process starting temperature is 25 ~ 60 DEG C; Crystallisation process terminal temperature is 0 ~ 30 DEG C; Crystallisation process cooling rate is 0.5 ~ 5 DEG C/min.
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| CN201510668303.5A CN105111254A (en) | 2015-10-17 | 2015-10-17 | Extraction method of lincomycin |
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| CN201510668303.5A CN105111254A (en) | 2015-10-17 | 2015-10-17 | Extraction method of lincomycin |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106518936A (en) * | 2016-09-24 | 2017-03-22 | 合肥信达膜科技有限公司 | Membrane extraction process for lincomycin |
| CN107474081A (en) * | 2017-08-20 | 2017-12-15 | 合肥信达膜科技有限公司 | A kind of membrane process craft of efficient extraction lincomycin |
| CN108872458A (en) * | 2018-06-26 | 2018-11-23 | 江西国药有限责任公司 | A kind of detection method of lincomycin fermentation liquid |
Citations (3)
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| CN101648981A (en) * | 2009-09-22 | 2010-02-17 | 南阳普康药业有限公司 | Extraction and refinement process of lincomycin |
| 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 |
| CN103724380A (en) * | 2013-12-25 | 2014-04-16 | 江苏久吾高科技股份有限公司 | Extraction method of lincomycin |
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2015
- 2015-10-17 CN CN201510668303.5A patent/CN105111254A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101648981A (en) * | 2009-09-22 | 2010-02-17 | 南阳普康药业有限公司 | Extraction and refinement process of lincomycin |
| 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 |
| CN103724380A (en) * | 2013-12-25 | 2014-04-16 | 江苏久吾高科技股份有限公司 | Extraction method of lincomycin |
Non-Patent Citations (3)
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| 段永平，等: ""林可霉素大孔吸附树脂工艺研究"", 《药品评价》 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106518936A (en) * | 2016-09-24 | 2017-03-22 | 合肥信达膜科技有限公司 | Membrane extraction process for lincomycin |
| CN107474081A (en) * | 2017-08-20 | 2017-12-15 | 合肥信达膜科技有限公司 | A kind of membrane process craft of efficient extraction lincomycin |
| CN108872458A (en) * | 2018-06-26 | 2018-11-23 | 江西国药有限责任公司 | A kind of detection method of lincomycin fermentation liquid |
| CN108872458B (en) * | 2018-06-26 | 2020-06-16 | 江西国药有限责任公司 | Detection method of lincomycin fermentation liquor |
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