CN1035333C - Method for prodn. of salino mycin and its sodium salt - Google Patents
Method for prodn. of salino mycin and its sodium salt Download PDFInfo
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- CN1035333C CN1035333C CN92103152A CN92103152A CN1035333C CN 1035333 C CN1035333 C CN 1035333C CN 92103152 A CN92103152 A CN 92103152A CN 92103152 A CN92103152 A CN 92103152A CN 1035333 C CN1035333 C CN 1035333C
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- salinomycin
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Abstract
The present invention relates to a technological method for extracting salinomycin and sodium salt thereof in fermentation liquor. The fermentation liquor is filtered by adding a filtering aid after being acidified, filter residues are extracted and filtered with alcohol, filter liquor is decolorized and filtered by activated carbon and concentrated, and a product can be obtained by adding water. The present invention has the advantages of convenient technology, low cost, low toxicity of a used solvent, etc.
Description
The present invention relates to a kind of method of from the microbiotic biosynthetic products, extracting microbiotic crystallization product.
According to reported in literature, the processing method of extracting Salinomycin. crystallization product from fermented liquid has:
(1) United States Patent (USP) 3857948 (1974)
With filtering fermentation liquor, mycelium in the filter residue is used N-BUTYL ACETATE after self-dissolving, organic solvent extraction such as acetone and chloroform, extraction liquid is purified with alumina column chromatography behind vacuum concentration, with vinyl acetic monomer, normal butane or the mixture wash-out of the two, collect activated part, behind the vacuum concentration again through Sephadex LH-20 chromatography, the collection active princlple is concentrated into dried, promptly gets the Salinomycin. powder.
(2) the clear 53-148595 of Japanese Patent number:
It is 4.5～5 that nutrient solution is transferred pH with dilute hydrochloric acid, stirred 10 minutes down at 60 ℃, add 4% (W/V) flocculating aids, filter, twice of N-BUTYL ACETATE extracting of filter residue, extracting solution is with 50 liters of washings of 5% aqueous sodium carbonate, evaporated under reduced pressure gets meal, adds 100 liters of n-hexane dissolution meal, is evaporated to 40 liters, put 5 ℃ of refrigerations down, get the Salinomycin Sodium crude product.Through chromatographic separation or with normal hexane recrystallization repeatedly, obtain pure Salinomycin Sodium.
(3) microbiotic the 5th phase of nineteen eighty-two report: the diatomite of adding 4% in fermented liquid, filter, filter residue extracts twice with the N-BUTYL ACETATE of 1/2 volume, and extracting solution is removed water with 5% sodium hydrogen carbonate solution thorough washing, and organic layer is evaporated to oily matter.With the oily matter alumina column chromatography, with acetic acid second vinegar: methyl alcohol (100: 0 → 100: 2 → 100: 20) wash-out, collect and merge Bacillus subtilus is had the active part elutriant of inhibition, concentrating under reduced pressure, the enriched material silica gel column chromatography is used chloroform: methyl alcohol (100: 0 → 100: 2 → 100: 20) wash-out, collect the Rf value component close with Salinomycin., be concentrated into dried, recrystallization in aqueous acetone, white salt mycin sodium salt crystal product.
The above several method of Jie Shaoing, used organic solvent great majority are all toxic.Owing to also contain quite a large amount of oil in the fermented liquid, other organic solvents except that acetone also are extracted into oil in the organic phase in the extraction Salinomycin., and further oil removing is pretty troublesome on technology.Though adopt acetone can avoid this shortcoming, the acetone boiling point is low, volatilization loss is bigger in process of production.In addition, use a layer post layer and separate and carry out recrystallization repeatedly and all make production process route long, be difficult to realize suitability for industrialized production.
The object of the present invention is to provide a kind of like this processing method of extracting Salinomycin. and sodium salt thereof from the Salinomycin. fermented liquid, its production technique is simple and direct, and used solvent toxicity is low, and product purity and recovery rate height.
The present invention is achieved in that the fermented liquid acidifying, regulate pH1～6, add various flocculating aidss 1～5% such as diatomite, oxalic acid, yellowish-white salt, zinc sulfate, in vacuum or add and depress filtration, discard filtrate, filter residue low toxicity organic solvent extraction, used low toxicity organic solvent is advisable with alcohols or acetone, preferably use alcohol,, get filtrate then in vacuum or add and depress filtration, add discoloring agent such as gac decolours, in vacuum or add and depress filtration, get filtrate concentrating, promptly get the Salinomycin. crystallization after adding suitable quantity of water.If filtrate adds adjusting PH with base earlier greater than 7 after concentrating, add water again, can get the Salinomycin Sodium crystallization.
Provide several embodiment below:
One, fermented liquid is 100 liters, and fermentation unit is 20000U/ml, adds oxalic acid and transfers pH=1, filter, the alcohol that filter residue adds 2 times of amounts stirred 2 hours, filtered, filtrate adds 1 kilogram of gac, stirs after-filtration, and filter is concentrated into about 10 liters, add 20 liters in water, leave standstill after the stirring, have crystallization to separate out, filter and obtain the crystallization of white salt mycin, oven-dried weight 1400 grams, yield 70%.
Two, fermented liquid is 100 liters, and fermentation unit 2000U/ml adds hydrochloric acid and transfers pH=1, add 4% diatomite, stirred 10 minutes, filter, filter residue adds triplication alcohol and stirred 2 hours, filters, and filtrate adds 1 kilogram of gac, stir after-filtration, filtrate is concentrated into about 10 liters, adds 20 liters in water, leave standstill crystallization after the stirring, filter the crystallization of white salt mycin, oven-dried weight 1450 gram, yield 72.5%.
Three, fermented liquid is 100 liters, and fermentation unit 25000U/ml adds phosphoric acid and transfers pH=1, add each 0.1 kilogram in yellow prussiate of potash and zinc sulfate, be heated to 60 ℃, stirred 30 minutes, filter, filter residue adds triplication alcohol and stirred 2 hours, filters, filtrate adds 1 kilogram of gac, stirs after-filtration, and filtrate is concentrated into about 10 liters, concentrated solution adjusting PH with base 10, add 20 liters in water again, leave standstill crystallization after the stirring, filter white Salinomycin Sodium crystallization.Oven-dried weight 1480 grams, recovery rate 74.1%.
The invention has the advantages that technology is simpler, do not need chromatography and repeatedly the recrystallization, just Can obtain qualified crystallization product. Used industrial alcohol is than used the having of the method for Introduction of Literatures The machine solvent toxicity is low, price is also low more than one times, and whole process ground cost is more than 50%.
Claims (6)
1. processing method of from the Salinomycin. fermented liquid, extracting Salinomycin. and sodium salt thereof, it is characterized in that the fermented liquid acidifying, transfer pH 1～6, add flocculating aids, filter, get filter residue with alcoholic solvent or acetone extract, filter, get filtrate and add bleaching agent bleaching, filter, add after filtrate concentrates that water obtains the Salinomycin. crystallization or filtrate concentrated after add adjusting PH with base earlier and add water again greater than 7 and get the Salinomycin Sodium crystallization.
2. processing method according to claim 1, used acid are various organic acids or mineral acid; Regulating acidity is advisable with pH1～6.
3. processing method according to claim 1 is characterized in that used flocculating aids is diatomite, yellow prussiate of potash or zinc sulfate.
4. processing method according to claim 1 is characterized in that used alcoholic solvent is an alcohol.
5. processing method according to claim 1 is characterized in that used discoloring agent is a gac.
6. processing method according to claim 1, when it is characterized in that filtering with vacuum filtration or pressure filtration.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN92103152A CN1035333C (en) | 1992-04-28 | 1992-04-28 | Method for prodn. of salino mycin and its sodium salt |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN92103152A CN1035333C (en) | 1992-04-28 | 1992-04-28 | Method for prodn. of salino mycin and its sodium salt |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1078263A CN1078263A (en) | 1993-11-10 |
| CN1035333C true CN1035333C (en) | 1997-07-02 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN92103152A Expired - Fee Related CN1035333C (en) | 1992-04-28 | 1992-04-28 | Method for prodn. of salino mycin and its sodium salt |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1035333C (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102702376A (en) * | 2012-05-24 | 2012-10-03 | 河北科技师范学院 | Process for extracting chestnut polysaccharide by pressurized solvent extraction method |
| CN104447789B (en) * | 2014-12-15 | 2018-09-14 | 山东齐发药业有限公司 | A kind of preparation method of Salinomycin Sodium fine work |
| CN104546739A (en) * | 2015-01-20 | 2015-04-29 | 山西新源华康化工股份有限公司 | Extraction process of salinomycin |
| CN105800828B (en) * | 2016-04-27 | 2019-07-23 | 滨海明鸿精细化工有限公司 | The recovery method of sodium pyrithione in a kind of waste water |
| CN108342426B (en) * | 2018-03-30 | 2019-01-01 | 内蒙古拜克生物有限公司 | A kind of method of fermenting and producing salinomycin |
| CN108440558B (en) * | 2018-03-30 | 2019-04-09 | 内蒙古拜克生物有限公司 | A kind of method of purification of Salinomycin Sodium |
| CN108484630B (en) * | 2018-03-30 | 2019-03-05 | 内蒙古拜克生物有限公司 | A kind of salinomycin method of purification |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3857948A (en) * | 1972-03-03 | 1974-12-31 | Kaken Chemical Co | Salinomycin |
| JPS53148595A (en) * | 1977-06-01 | 1978-12-25 | Kaken Pharmaceut Co Ltd | Preparation of salinomycines |
-
1992
- 1992-04-28 CN CN92103152A patent/CN1035333C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3857948A (en) * | 1972-03-03 | 1974-12-31 | Kaken Chemical Co | Salinomycin |
| JPS53148595A (en) * | 1977-06-01 | 1978-12-25 | Kaken Pharmaceut Co Ltd | Preparation of salinomycines |
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| Publication number | Publication date |
|---|---|
| CN1078263A (en) | 1993-11-10 |
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