CN102633641A - Method for extracting pleuromutilin from tiamulin fermentation liquor - Google Patents
Method for extracting pleuromutilin from tiamulin fermentation liquor Download PDFInfo
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- CN102633641A CN102633641A CN2012100759183A CN201210075918A CN102633641A CN 102633641 A CN102633641 A CN 102633641A CN 2012100759183 A CN2012100759183 A CN 2012100759183A CN 201210075918 A CN201210075918 A CN 201210075918A CN 102633641 A CN102633641 A CN 102633641A
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- pleuromutilin
- thiamutilin
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- methyl alcohol
- fermented liquid
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Abstract
A method for extracting pleuromutilin from tiamulin fermentation liquor is characterized by including: firstly, filtering the tiamulin fermentation liquor, leading obtained wet fungus dregs to undergo flash vaporization, then extracting by utilizing methyl alcohol as solvent, and concentrating extraction liquid to obtain pleuromutilin concentrated liquor. The pleuromutilin is extracted from the tiamulin fermentation liquor by utilizing the methyl alcohol as the solvent, and the method has the advantages of small use amount of organic solvent, high extraction yield, low production cost and the like.
Description
Technical field
The invention belongs to biological medicine extractive technique field, particularly relate to a kind of method of from the thiamutilin fermented liquid, extracting pleuromutilin.
Background technology
Pleuromutilin is a kind of diterpene carbapenem antibiotic, from pleuromutilin through the semi-synthetic thiamutilin that obtains.Pleuromutilin and fumaric acid tiamulin are as antibiotics; Be widely used as veterinary drug, use, mainly be used as the fodder additives of poultry and livestock with the fodder additives form; In feed, add this product; Can effectively prevent many transmissible diseases, main effect is anti-gram-bacteria, treponema (helicobacter), leptospira and mycoplasma etc., especially streptococcus aureus, suis, multiple Mycoplasma and some spirochete is had strong germicidal action.
At present, the source of the pleuromutilin raw material that uses in the fumaric acid tiamulin building-up process mainly is the bacterium slag that adopts organic solvent extraction thiamutilin fermented liquid, and the active substance pleuromutilin in the bacterium slag is dissolved in the organic solvent.Organic solvent commonly used at present mainly is industrial spirit, acetone, ether and methyl second butyl ketone (4-methyl-2 pentanone).
Use ether and acetone extraction pleuromutilin, low, the complicated operation of its yield, and also bigger to environment and human health damage, domestic production producer stops using.
Use industrial spirit (quality standard: GB/T394.1-94 number; Concentration: 95.5%) extract pleuromutilin; Its yield only can reach 85～95%; Though the industrial alcohol after the use can adopt distillating method to reclaim and utilize, its maximum concentration can only reach 95.5%, can not further improve purity again; And domestic industry alcohol market value is 6～9 yuan/kg, and its solvent use cost is higher relatively.
Methyl second butyl ketone (quality standard: HG/T 3481-1999) be mainly used in and produce rubber antioxidant 4020 and paint solvent, also as the extraction agent of Multiple Pesticides, medicine and thinner, rare metal extraction agent, lubricating oil dewaxing agent, tensio-active agent etc.Olympic Competition biochemical ltd in domestic Jiangsu adopts this organic solvent to extract pleuromutilin, applies for a patent (the patent No.: 200510122954.0) simultaneously.With methyl second butyl ketone is that solvent mainly exists following defective:
1, the organic solvent cost is high.Domestic methyl second butyl ketone market value is 60～70 yuan/kg.
2, extract yield is low.Adopt methyl second butyl ketone, its extract yield is 80～90%.
3, pollution and cost of sewage disposal have been increased to environment.Adopt methyl second butyl ketone to extract pleuromutilin, after accomplishing the bacterium slag is handled, contain a large amount of methyl second butyl ketones in the waste water of discharging, increased the waste water control cost.
Summary of the invention
The object of the invention is to provide the defective that overcomes above-mentioned prior art, and a kind of employing organic solvent that suits is provided, and extract yield is high, and production cost is relatively low, the method for from the thiamutilin fermented liquid, extracting pleuromutilin easy and simple to handle.
For realizing that the technical scheme that above-mentioned purpose is taked is:
A kind of method of from the thiamutilin fermented liquid, extracting pleuromutilin; It is characterized in that: at first with the thiamutilin filtering fermentation liquor; The wet bacteria slag expansion drying that obtains carries out lixiviate with methyl alcohol as solvent then, and the gained vat liquor concentrates and obtains the pleuromutilin liquid concentrator.
Above-mentioned filtration is meant filters the thiamutilin fermented liquid with box plate-and-frame filter press, filtered liq is entered waste liquid pool, and the sheet frame feed pressure is increased to 0.45MPa gradually; After treating that the sheet frame material advances to expire, stop charging, water cleans material in the sheet frame; Till treating that the liquid change is limpid, when drying to the outflow of nothing filtrating with pressurized air to sheet frame then, carry out sheet frame and unpick and wash; Obtain wet bacteria slag, wet bacteria slag is placed on specified location.
Above-mentioned expansion drying adopts flash dryer to realize, at first need flash dryer preheating half a hour be opened gas blower, and the control EAT is at 100～120 ℃, and air outlet temperature is controlled at 70～90 ℃; Wet bacteria slag after filtering is constantly dropped into the flash dryer charging opening, collect dried bacterium slag at discharge port, the reinforced rotating speed of control is 50～400r/min, carries out expansion drying; Require dried dried bacterium slag color and luster to be faint yellow or yellow.
Saidly be meant with methyl alcohol (quality standard: GB-338 2004 when carrying out lixiviate as solvent with methyl alcohol; Concentration >=99%) as organic solvent the pleuromutilin in the dried bacterium slag is extracted in the methyl alcohol; Obtain containing the vat liquor of pleuromutilin, be collected in the vat liquor storage tank.Leaching process is under whipped state, to carry out, and mixing speed is controlled at 100～300r/min.Extract the multiple extraction method that adopts, for the first time withdrawal ratio: the ratio of bacterium slag and methyl alcohol is to add 0.9～1.1kg bacterium slag in every 5L methyl alcohol, is extracted into for the second time to extract and finishes, and methyl alcohol extracts usage quantity at every turn and reduces 20%; Each extraction time is controlled at 100～150min.The each extraction finished, and pleuromutilin content in the Detection and Extraction liquid if be higher than 0.6%, extracts once more, and the pleuromutilin amount contains and is lower than 0.6% in methanol solution, stops to extract.
Extract to finish, it is carried out concentration, temperature is controlled at 60～80 ℃, and vacuum tightness be-0.04～-0.08Mpa, be concentrated into till the no methyl alcohol outflow.
The present invention is that solvent extracts pleuromutilin with methyl alcohol from the thiamutilin fermented liquid, has following technical superiority:
1, extract yield is high.
It is solvent that the present invention adopts methyl alcohol, because dissolve with methanol property is high, so the pleuromutilin extract yield can reach more than 95%.
2, the organic solvent cost is low.
At present, domestic industry alcohol market value is 6～9 yuan/kg, and methyl second butyl ketone market value is 60～70 yuan/kg, and the market value of methyl alcohol is merely 1.3～1.5 yuan/kg, thereby adopting methyl alcohol is that solvent can reduce extraction cost greatly.
3, can effectively reduce pollution and cost of sewage disposal to environment.
The present invention adopts the methanol extraction pleuromutilin, utilizes methyl alcohol character soluble in water, can the waste water of cleaning bacterium slag be recycled and reclaim, thereby reduce the loss of methyl alcohol, reduces production costs and to the infringement of environment.
In sum, the method for from the thiamutilin fermented liquid, extracting pleuromutilin of the present invention has advantages such as the organic solvent consumption is little, and extract yield is high, and production cost is low.
Embodiment
With instance the present invention is described below, it should be understood that instance is to be used to explain the present invention rather than limitation of the present invention.Scope of the present invention and core content are confirmed according to claims.
The following methyl alcohol of selecting for use adopts quality standard: GB-338 2004, concentration >=99%.
Embodiment 1 adopts the methanol extraction pleuromutilin
The thiamutilin fermented liquid filters with box plate-and-frame filter press.Filtered liq is entered waste liquid pool, and the sheet frame feed pressure is increased to 0.45MPa gradually, treat the sheet frame material advance full after, stop charging, with tap water material in the sheet frame is cleaned, treat liquid become limpid till.With pressurized air sheet frame is dried, when blowing, carry out sheet frame and unpick and wash to the outflow of nothing filtrating.Wet bacteria slag is placed on specified location.
Flash dryer preheating half a hour, open gas blower, the control EAT is at 100～105 ℃, and air outlet temperature is at 70～75 ℃.Wet bacteria slag after filtering is constantly dropped into the flash dryer charging opening, and with collecting dried bacterium slag, the reinforced rotating speed of control is 50～100r/min, carries out expansion drying at discharge port.Behind dry the end, bacterium slag color and luster is faint yellow.
The dried bacterium slag of weighing 100kg, pleuromutilin content is 19.34%.In the leaching process, mixing speed is controlled at 100r/min, and each extraction time is 100min.Methanol usage is 500L for the first time; Methanol usage is 400L for the second time, and methanol usage is 300L for the third time, and pleuromutilin content is respectively 3.0%, 0.78%, 0.27% in the methanol solution; It is carried out concentration; Temperature is controlled at 60～65 ℃, and vacuum tightness is-0.06～-0.08Mpa, till being concentrated into no methyl alcohol and flowing out.The pleuromutilin extract yield is 97.8%.
Embodiment 2 adopts the methanol extraction pleuromutilin
The thiamutilin fermented liquid filters with box plate-and-frame filter press.Filtered liq is entered waste liquid pool, and the sheet frame feed pressure is increased to 0.45MPa gradually, treat the sheet frame material advance full after, stop charging, with tap water material in the sheet frame is cleaned, treat liquid become limpid till.With pressurized air sheet frame is dried, when blowing, carry out sheet frame and unpick and wash to the outflow of nothing filtrating.Wet bacteria slag is placed on specified location.
Flash dryer preheating half a hour, open gas blower, the control EAT is at 110～115 ℃, and air outlet temperature is controlled at 80～85 ℃.Wet bacteria slag after filtering is constantly dropped into the flash dryer charging opening, collect dried bacterium slag at discharge port, the reinforced rotating speed of control is 200～300r/min, carries out expansion drying.Behind dry the end, it is yellow that bacterium slag color and luster is.
The dried bacterium slag of weighing 100kg, pleuromutilin content is 22.74%.In the leaching process, mixing speed is controlled at 100r/min, and each extraction time is 125min.Methanol usage is 500L for the first time, and methanol usage is 400L for the second time, and pleuromutilin content is respectively 4.09%, 0.56% in the methanol solution; It is carried out concentration; Temperature is controlled at 70～75 ℃, and vacuum tightness is-0.05～-0.06Mpa, till being concentrated into no methyl alcohol and flowing out.The pleuromutilin extract yield is 99.8%.
Embodiment 3 adopts the methanol extraction pleuromutilin
The thiamutilin fermented liquid filters with box plate-and-frame filter press.Filtered liq is entered waste liquid pool, and the sheet frame feed pressure is increased to 0.45MPa gradually, treat the sheet frame material advance full after, stop charging, with tap water material in the sheet frame is cleaned, treat liquid become limpid till.With pressurized air sheet frame is dried, when blowing, carry out sheet frame and unpick and wash to the outflow of nothing filtrating.Wet bacteria slag is placed on specified location.
Flash dryer preheating half a hour, open gas blower, the control EAT is at 115～120 ℃, and air outlet temperature is controlled at 85～90 ℃.Wet bacteria slag after filtering is constantly dropped into the flash dryer charging opening, collect dried bacterium slag at discharge port, the reinforced rotating speed of control is 300～400r/min, carries out expansion drying.Behind dry the end, it is yellow that bacterium slag color and luster is.
The dried bacterium slag of weighing 100kg, pleuromutilin content is 23.16%.In the leaching process, mixing speed is controlled at 100r/min, and each extraction time is 150min.Methanol usage is 500L for the first time, and methanol usage is 400L for the second time, and pleuromutilin content is respectively 4.2%, 0.51% in the methanol solution; It is carried out concentration; Temperature is controlled at 70～75 ℃, and vacuum tightness is-0.04～-0.05Mpa, till being concentrated into no methyl alcohol and flowing out.The pleuromutilin extract yield is 99.5%.
Comparative Examples adopts industrial spirit (concentration: 95%) extract pleuromutilin
The thiamutilin fermented liquid filters with box plate-and-frame filter press.Filtered liq is entered waste liquid pool, and the sheet frame feed pressure is increased to 0.45MPa gradually, treat the sheet frame material advance full after, stop charging, with tap water material in the sheet frame is cleaned, treat liquid become limpid till.With pressurized air sheet frame is dried, when blowing, carry out sheet frame and unpick and wash to the outflow of nothing filtrating.Wet bacteria slag is placed on specified location.
Flash dryer preheating half a hour, open gas blower, the control EAT is at 110～115 ℃, and air outlet temperature is controlled at 80～85 ℃.Wet bacteria slag after filtering is constantly dropped into the flash dryer charging opening, collect dried bacterium slag at discharge port, the reinforced rotating speed of control is 200～300r/min, carries out expansion drying.Behind dry the end, it is yellow that bacterium slag color and luster is.
The dried bacterium slag of weighing 100kg, pleuromutilin content is 21.86%.In the leaching process, mixing speed is controlled at 100r/min, and each extraction time is 125min.The industrial spirit consumption is 500L for the first time, and pure consumption is 500L for the second time, and pleuromutilin content is respectively 3.5%, 0.52% in the methanol solution; It is carried out concentration; Temperature is controlled at 70～75 ℃, and vacuum tightness is-0.05～-0.06Mpa, till being concentrated into no methyl alcohol and flowing out.The pleuromutilin extract yield is 91.9%.
Claims (8)
1. method of from the thiamutilin fermented liquid, extracting pleuromutilin; It is characterized in that: at first with the thiamutilin filtering fermentation liquor; The wet bacteria slag expansion drying that obtains carries out lixiviate with methyl alcohol as solvent then, and the gained vat liquor concentrates and obtains the pleuromutilin liquid concentrator.
2. according to the described method of from the thiamutilin fermented liquid, extracting pleuromutilin of claim 1, it is characterized in that: above-mentioned filtration is meant filters the thiamutilin fermented liquid with box plate-and-frame filter press, the sheet frame feed pressure is increased to 0.45MPa gradually; After treating that the sheet frame material advances to expire, stop charging, water cleans material in the sheet frame; Till treating that the liquid change is limpid; When drying to the outflow of nothing filtrating with pressurized air to sheet frame then, carry out sheet frame and unpick and wash, obtain wet bacteria slag.
3. according to the described method of from the thiamutilin fermented liquid, extracting pleuromutilin of claim 1; It is characterized in that: above-mentioned expansion drying adopts flash dryer to realize; 100～120 ℃ of control EATs, 70～90 ℃ of air outlet temperatures, reinforced rotating speed are 50～400r/min.
4. according to the described method of from the thiamutilin fermented liquid, extracting pleuromutilin of claim 1; It is characterized in that: said when carrying out lixiviate as solvent with methyl alcohol; The ratio of bacterium slag and methyl alcohol is to add 0.9～1.1kg bacterium slag, extraction time: 100～150min in every 5L methyl alcohol.
5. according to claim 1 or the 4 described methods of from the thiamutilin fermented liquid, extracting pleuromutilin, it is characterized in that: above-mentioned to carry out lixiviate with methyl alcohol as solvent be under whipped state, to carry out, and mixing speed is controlled at 100～300r/min.
6. according to the described method of from the thiamutilin fermented liquid, extracting pleuromutilin of claim 5, it is characterized in that: above-mentionedly carry out lixiviate repeatedly with methyl alcohol as solvent, the pleuromutilin amount contains and is lower than 0.6% to the methanol solution, stops to extract.
7. according to the described method of from the thiamutilin fermented liquid, extracting pleuromutilin of claim 6, it is characterized in that: finish from being extracted into for the second time to extract, methyl alcohol extracts usage quantity at every turn and reduces 20%.
8. according to the described method of from the thiamutilin fermented liquid, extracting pleuromutilin of claim 1, it is characterized in that: said concentrate be meant in vacuum tightness be-0.04～-0.08MPa, be concentrated under 60～80 ℃ of conditions of temperature till the no methyl alcohol outflow.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2012100759183A CN102633641A (en) | 2012-03-21 | 2012-03-21 | Method for extracting pleuromutilin from tiamulin fermentation liquor |
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| CN2012100759183A CN102633641A (en) | 2012-03-21 | 2012-03-21 | Method for extracting pleuromutilin from tiamulin fermentation liquor |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104592023A (en) * | 2015-01-20 | 2015-05-06 | 山西新源华康化工股份有限公司 | Refining technology of pleuromutilin |
| CN106631796A (en) * | 2016-12-22 | 2017-05-10 | 宁夏泰瑞制药股份有限公司 | Organic solvent and extraction method for extracting crude product of pleuromutilin |
| CN107235841A (en) * | 2017-07-26 | 2017-10-10 | 新疆和生物有限责任公司 | A kind of extracting method of pleuromutilin |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4089891A (en) * | 1975-07-23 | 1978-05-16 | Biochemie | Pleuromutilin solvates |
| CN1775755A (en) * | 2005-12-06 | 2006-05-24 | 江苏赛奥生化有限公司 | Method for preparing raw material of pleuromutilin for use in tiamulin synthesizing process |
| CN101481308A (en) * | 2009-01-20 | 2009-07-15 | 河北瑞通美邦工程有限公司 | Process for extracting pleuromulin |
| CN101676257A (en) * | 2008-09-17 | 2010-03-24 | 大英九合生物化工股份有限公司 | Method for fermenting, extracting and preparing high purity pleuromutilin raw material |
| CN102050737A (en) * | 2010-12-10 | 2011-05-11 | 山东胜利股份有限公司 | Method for extracting and purifying pleuromutilin |
-
2012
- 2012-03-21 CN CN2012100759183A patent/CN102633641A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4089891A (en) * | 1975-07-23 | 1978-05-16 | Biochemie | Pleuromutilin solvates |
| CN1775755A (en) * | 2005-12-06 | 2006-05-24 | 江苏赛奥生化有限公司 | Method for preparing raw material of pleuromutilin for use in tiamulin synthesizing process |
| CN101676257A (en) * | 2008-09-17 | 2010-03-24 | 大英九合生物化工股份有限公司 | Method for fermenting, extracting and preparing high purity pleuromutilin raw material |
| CN101481308A (en) * | 2009-01-20 | 2009-07-15 | 河北瑞通美邦工程有限公司 | Process for extracting pleuromulin |
| CN102050737A (en) * | 2010-12-10 | 2011-05-11 | 山东胜利股份有限公司 | Method for extracting and purifying pleuromutilin |
Non-Patent Citations (1)
| Title |
|---|
| 吴春丽等: "菌渣中截短侧耳素含量的高效液相色谱法测定", 《郑州大学学报医学版》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104592023A (en) * | 2015-01-20 | 2015-05-06 | 山西新源华康化工股份有限公司 | Refining technology of pleuromutilin |
| CN106631796A (en) * | 2016-12-22 | 2017-05-10 | 宁夏泰瑞制药股份有限公司 | Organic solvent and extraction method for extracting crude product of pleuromutilin |
| CN107235841A (en) * | 2017-07-26 | 2017-10-10 | 新疆和生物有限责任公司 | A kind of extracting method of pleuromutilin |
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Application publication date: 20120815 |