CN102391363B - Method for extracting enramycin - Google Patents
Method for extracting enramycin Download PDFInfo
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- CN102391363B CN102391363B CN2011102880996A CN201110288099A CN102391363B CN 102391363 B CN102391363 B CN 102391363B CN 2011102880996 A CN2011102880996 A CN 2011102880996A CN 201110288099 A CN201110288099 A CN 201110288099A CN 102391363 B CN102391363 B CN 102391363B
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- enramycin
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- extraction agent
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Abstract
The invention relates to a method for extracting enramycin. The method comprises the following steps of: soaking dried enramycin fungus dreg in an extracting agent; heating and refluxing; filtering; concentrating the filtrate under the vacuum condition until the filtrate is dried; dissolving the obtained substance; filtering; drying the filtrate by distillation under reduced pressure; dissolving the obtained solid substance; filtering; collecting filter cakes; and drying to obtain the enramycin. The method has simple steps; in the extracting process, all the organic solvents are easy to recycle; environmental pollution is light; and the obtained enramycin has high content and high reproducibility.
Description
Technical field
The present invention relates to the feed medicated premix and make field, be specifically related to a kind of extracting method of enramycin.
Technical background
Enramycin (Enramycin), have another name called enramycin, enramycin, enramycin, belong to polypeptide antibiotics, by actinomycete fermentation, it is a kind of organic bases by amino acid molecular and molecular composition of fatty acids, wherein amino acid molecular forms the ring-type polypeptide structure, and fatty acid molecule is positioned at the polypeptide structure end., according to the difference of end fatty acid molecule, be divided into enramycin A (C
107H
138Cl
2N
26O
31), enramycin B(C
108H
141Cl
2N
26O
31) two kinds of components, enramycin is the mixture of these two kinds of components.Enramycin is soluble in dilute hydrochloric acid, and dimethyl formamide dissolves in methyl alcohol, ethanol, is insoluble in acetone, is insoluble to acetic acid, benzene, chloroform, is a kind of wide spectrum, efficient, safe, residual extremely low novel fodder additive.
Enramycin, by Japan's research and development,, due to its powerful sterilizing function, is widely used by many countries and regions the earliest, and 1993, China ratified this medicine and registers at home.2005, domestic production enterprise and U.S. Schering Plough animal health-care product company limited started joint production enramycin pre-mixture.Enramycin stability in feed is very high, storage degraded hardly at ambient temperature for a long time, and granulation material stability is higher.Enramycin as fodder additives is to be made by the fermented liquid fermentation, and its fermentation time is long, and it is extremely complicated to extract separating step.
Chinese patent CN101597578A discloses a kind of method with macroporous resin extraction enramycin (being enramycin), the method is extracted 0.5 ~ 4hr with enramycin bacterium slag with the extraction agent concussion, acquisition contains the extracting solution of enramycin, supernatant liquor concentrating under reduced pressure after again extracting solution is centrifugal obtains enramycin and slightly carries product, with dissolution with solvents by macroporous resin adsorption 2 ~ 5hr after, with after eluent gradient elution, concentrate drying the enramycin sterling.The method is used macroporous adsorbent resin in leaching process, product loss is large, and productive rate is low, and resin absorption products obtained therefrom content is not high, as need more the product of high-content also need silica gel or aluminum oxide to process again; On the other hand, this extracting method is strict to resin pre-treatment and regenerative process, operates more complicatedly, and cost is high, and regeneration also can produce a large amount of waste water and organic solvent, and there is larger pollution in environment; In addition, due to the same model resin that same manufacturing enterprise produces, between each batch, specific surface area and functional group content difference are larger, make and use this method to extract enramycin, poor reproducibility.
Summary of the invention
The present invention is directed to prior art and have the problems such as complicated operation, product loss are large, poor reproducibility, provide that a kind of processing step is simple, low production cost, environmental pollution be little, the extracting method of the enramycin of favorable reproducibility.
Above-mentioned technical purpose of the present invention is achieved by the following technical programs: a kind of extracting method of enramycin, and concrete steps are as follows:
(1) lixiviate
1. the enramycin bacterium slag of drying is soaked 20 ~ 40min with extraction agent, then stirring and refluxing 1 ~ 4hr at 50 ℃ ~ 80 ℃ temperature, refilter;
2. with step 1. in the filter cake of gained soak 20 ~ 40min with extraction agent again, the backflow of repeating step in 1., then filter;
3. with step 1. and 2. the filtrate of gained merge to obtain vat liquor;
(2) concentrated
Vat liquor vacuum concentration at 60 ~ 80 ℃ of temperature that step (1) is collected is extremely done;
(3) dissolve
Step (2) gained dissolution of solid in ethanol or methyl alcohol, is filtered;
(4) concentrated
The filtrate of step (3) vacuum concentration at 50 ~ 70 ℃ of temperature is extremely done;
(5) water extraction
Dry-matter in step (4) is dissolved in the water, filters, filter cake is dried to obtain enramycin;
Wherein, the extraction agent in described step (1) is the acidic aqueous solution of organic solvent.
As preferably, described organic solvent is a kind of in acetone, methyl alcohol, ethanol, and its volume fraction that accounts for extraction agent is 40 ~ 60%.
As preferably, the acid in described acidic aqueous solution is one or more of hydrochloric acid, sulfuric acid, acetic acid, formic acid.
As preferably, described step (1) 1. in the consumption of every Kern's mycin bacterium slag extraction agent be 2 ~ 10mL.
As preferably, the pH value of described extraction agent is 4 ~ 6.
As preferably, in step (1), 1. temperature is 60 ~ 70 ℃.
As preferably, the temperature in step (2) is 70 ~ 80 ℃.
As preferably, the ethanol of every Kern's mycin bacterium slag or the consumption 1 ~ 5mL of methyl alcohol in described step (3).
As preferably, the temperature in step (4) is 60 ~ 70 ℃.
As preferably, the ethanol in step (3) or the consumption of methyl alcohol are every Kern's mycin bacterium slag 1 ~ 5mL; Water in described step (5) is pure water, and its consumption is every Kern's mycin bacterium slag 1 ~ 3mL.
In sum, the present invention compared with prior art, has following outstanding advantages and beneficial effect:
1, preparation process step of the present invention is simple, and organic solvent used all is easy to recycle, and the wastewater flow rate of generation is few, and environmental pollution is little, the high and favorable reproducibility of gained enramycin content;
2, after testing, its content, uniformity coefficient all reach the requirement of import veterinary drug quality standard to products obtained therefrom of the present invention, and product stability is good.
Embodiment
In order to be illustrated more clearly in the present invention, the present invention will be further described below in conjunction with the embodiment of indefiniteness, but be not limited to this.
Embodiment 1
(1) lixiviate
1. the enramycin bacterium slag of 250g drying is soaked 20min with the extraction agent that volume is 500mL, extraction agent used is the ethanol of 200mL and the acidic aqueous solution that hydrochloric acid forms, and its pH is 4.0,, at 50 ℃ of lower stirring and refluxing 1hr, then filters;
2. with step the filter cake in 1. use with step 1. the same extraction agent of same amount soak 30min,, at 50 ℃ of lower stirring and refluxing 1hr, refilter;
3. with step 1. and the filtrate 2. merge to obtain vat liquor, lixiviate step total recovery is 98.3%;
(2) concentrated
The vat liquor that step (1) is collected is extremely done at 60 ℃ of lower vacuum concentration;
(3) dissolve
Gained solid in step (2) is dissolved in the 250mL dissolve with ethanol, filters;
(4) concentrated
Filtrate in step (3) is extremely done at 50 ℃ of vacuum concentration;
(5) water extraction
Dry-matter in step (4) is dissolved in 250mL water, filter, filter cake is dried to obtain enramycin, the total recovery of leaching process is 82%, and enramycin content is 80%.
Embodiment 2
(1) lixiviate
1. the enramycin bacterium slag of 250g drying is soaked 40min with the extraction agent of volume 2500mL, extraction agent used is the methyl alcohol of 1500mL and the acidic aqueous solution that sulfuric acid forms, and its pH is 5.0,, at 80 ℃ of lower stirring and refluxing 4hr, then filters;
2. with step the filter cake in 1. use with step 1. the same extraction agent of same amount soak 30min,, at 80 ℃ of lower stirring and refluxing 4hr, refilter;
3. with step 1. and the filtrate 2. merge to obtain vat liquor, lixiviate step total recovery is 98.5%;
(2) concentrated
Vat liquor in step (1) is extremely done at 80 ℃ of vacuum concentration;
(3) dissolve
Step (2) gained solid matter is dissolved in 1250mL methyl alcohol, filters;
(4) concentrated
Filtrate in step (3) is extremely done at 70 ℃ of vacuum concentration;
(5) water extraction
Dry-matter in step (4) is dissolved in 500mL water, filters, filter cake is dried to obtain enramycin, the total recovery of leaching process is 81%, and enramycin content is 85%.
Embodiment 3
(1) lixiviate
1. the enramycin bacterium slag of 250g oven dry is soaked 30min with the extraction agent that volume is 1000mL, extraction agent used is the acetone of 500mL and the acidic aqueous solution that acetic acid forms, and its pH is 6.0,, at 75 ℃ of lower stirring and refluxing 2hr, refilters;
2. with step 1. in the gained filter cake use with step 1. the same extraction agent of same amount soak 30min,, at 75 ℃ of lower stirring and refluxing 2hr, then filter;
3. with step 1. and the filtrate 2. merge to obtain vat liquor, lixiviate step total recovery is 98.0%;
(2) concentrated
The vat liquor that step (1) is collected is at 70 ℃ of vacuum concentration evaporates to dryness;
(3) dissolve
, with step (2) gained solid 750mL dissolve with methanol, filter;
(4) concentrated
With the filtrate in step (3) at 60 ℃ of vacuum concentration evaporates to dryness;
(5) water extraction
Dry-matter in step (4) is dissolved in 750mL water, filters, filter cake is dried to obtain enramycin, the total recovery of leaching process is 80%, and enramycin content is 86%.
Embodiment 4
(1) lixiviate
1. the enramycin bacterium slag of 250g drying is soaked 35min with the extraction agent that volume is 1500mL, extraction agent used is the ethanol of 400mL, the methyl alcohol of 500mL and the acidic aqueous solution of hydrochloric acid and formic acid composition, its pH is 5.5,, at 65 ℃ of lower stirring and refluxing 2.5hr, then filters;
2. with step the filter cake in 1. use with step 1. the same extraction agent of same amount soak 30min,, at 65 ℃ of lower stirring and refluxing 2.5hr, refilter;
3. with step 1. and the filtrate 2. merge to obtain vat liquor, lixiviate step total recovery is 98.6%;
(2) concentrated
The vat liquor that step (1) is collected is extremely done at 75 ℃ of lower vacuum concentration;
(3) dissolve
Gained solid in step (2) is dissolved in the 500mL dissolve with ethanol, filters;
(4) concentrated
Filtrate in step (3) is extremely done at 65 ℃ of vacuum concentration;
(5) water extraction
Dry-matter in step (4) is dissolved in 500mL water, filter, filter cake is dried to obtain enramycin, the total recovery of leaching process is 83%, and enramycin content is 82%.
Claims (8)
1. the extracting method of an enramycin, concrete steps are as follows:
(1) lixiviate
1. the enramycin bacterium slag of drying is soaked 20 ~ 40min with extraction agent, then stirring and refluxing 1 ~ 4hr at 50 ℃ ~ 80 ℃ temperature, refilter;
2. with step 1. in the filter cake of gained soak 20 ~ 40min with extraction agent again, the backflow of repeating step in 1., then filter;
3. with step 1. and 2. the filtrate of gained merge to obtain vat liquor;
(2) concentrated
Vat liquor vacuum concentration at 60 ~ 80 ℃ of temperature that step (1) is collected is extremely done;
(3) dissolve
Step (2) gained dissolution of solid in ethanol or methyl alcohol, is filtered;
(4) concentrated
The filtrate of step (3) vacuum concentration at 50 ~ 70 ℃ of temperature is extremely done;
(5) water extraction
Dry-matter in step (4) is dissolved in the water, filters, filter cake is dried to obtain enramycin;
Wherein, the extraction agent in described step (1) is the acidic aqueous solution of organic solvent;
Described organic solvent is one or more in acetone, methyl alcohol, ethanol;
Acid in described acidic aqueous solution is one or more in hydrochloric acid, sulfuric acid, acetic acid, formic acid.
2. the extracting method of a kind of enramycin according to claim 1, it is characterized in that: the volume fraction that the organic solvent in described extraction agent accounts for extraction agent is 40 ~ 60%.
3. the extracting method of a kind of enramycin according to claim 1 is characterized in that: described step (1) 1. in the Solvent quantity of every Kern's mycin bacterium slag be 2 ~ 10mL.
4. the extracting method of a kind of enramycin according to claim 1, it is characterized in that: the pH value of described extraction agent is 4 ~ 6.
5. the extracting method of a kind of enramycin according to claim 4 is characterized in that: in described step (1), 1. temperature is 60 ~ 70 ℃.
6. the extracting method of a kind of enramycin according to claim 1, it is characterized in that: the temperature in described step (2) is 70 ~ 80 ℃.
7. the extracting method of a kind of enramycin according to claim 1, it is characterized in that: the temperature in described step (4) is 60 ~ 70 ℃.
8. the extracting method of a kind of enramycin according to claim 1, it is characterized in that: the ethanol in described step (3) or the consumption of methyl alcohol are every Kern's mycin bacterium slag 1 ~ 5mL; Water in described step (5) is pure water, and its consumption is every Kern's mycin bacterium slag 1 ~ 3mL.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011102880996A CN102391363B (en) | 2011-09-26 | 2011-09-26 | Method for extracting enramycin |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011102880996A CN102391363B (en) | 2011-09-26 | 2011-09-26 | Method for extracting enramycin |
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| CN102391363A CN102391363A (en) | 2012-03-28 |
| CN102391363B true CN102391363B (en) | 2013-11-13 |
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|---|---|---|---|
| CN2011102880996A Active CN102391363B (en) | 2011-09-26 | 2011-09-26 | Method for extracting enramycin |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103232530B (en) * | 2013-04-17 | 2014-10-29 | 南京工业大学 | Method for separating enramycin A and B |
| CN104447958B (en) * | 2014-12-11 | 2019-05-10 | 新疆天富阳光生物科技有限公司 | The method of enramycin is extracted from fermentation liquid |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE1617881C2 (en) * | 1965-10-13 | 1984-07-05 | Takeda Chemical Industries, Ltd., Osaka | Antibiotic enduracidin and its manufacture |
| JPS6038120B2 (en) * | 1980-10-31 | 1985-08-30 | 武田薬品工業株式会社 | Production method of the antibiotic enzyuracydin |
| CN101245362B (en) * | 2008-03-24 | 2011-05-11 | 南京工业大学 | Method for producing polypeptide antibiotic enramycin by fermentation method |
| CN101597578B (en) * | 2009-07-01 | 2011-08-31 | 南京工业大学 | Enramycin producing strain and method for extracting same by using macroporous resin |
| CN101899490B (en) * | 2010-07-14 | 2012-09-05 | 山东胜利股份有限公司 | Method for producing enramycin by using microbial fermentation |
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Effective date of registration: 20171204 Address after: 313000 Zhejiang city of Huzhou province Deqing County Zhongguan town Hengtang Bridge No. 81 Patentee after: Zhejiang biok Biology Technology Co. Ltd. Address before: 313220 Huzhou City, Zhejiang Province, Deqing County Zhong Guan Town Industrial Zone Patentee before: Zhejiang Shenghua Biok Biology Co., Ltd. |
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