CN101693732B - Method for extracting and purifying natamycin - Google Patents
Method for extracting and purifying natamycin Download PDFInfo
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- CN101693732B CN101693732B CN2009101631630A CN200910163163A CN101693732B CN 101693732 B CN101693732 B CN 101693732B CN 2009101631630 A CN2009101631630 A CN 2009101631630A CN 200910163163 A CN200910163163 A CN 200910163163A CN 101693732 B CN101693732 B CN 101693732B
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- tennecetin
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- ion exchange
- exchange resin
- methyl alcohol
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Abstract
The invention relates to a method for extracting and purifying natamycin. The natamycin is extracted from fermenting liquor, and the target product natamycin is extracted and purified by five steps and process conditions. The invention has the advantages of simple and convenient process, high yield, high purity (dry basis content larger than and equal to 95 percent) and low cost.
Description
The present invention relates to a kind of tennecetin extracting and purifying method.Belong to chemical technology field.
Tennecetin is a kind of polyene macrolide antifungal element, and it can suppress harmful fungoid, and the growth of mould and do not act on human body beneficial's flora can be used as food preservatives and uses.Tennecetin all has production at home and abroad, mainly is to adopt microbe fermentation method promptly to add the fermented liquid that obtains containing tennecetin behind bacterial classification, the fermentating metabolism in nutrient solution, obtains the target product tennecetin after certain step and processing condition.The also more for example Virahol extraction of extracting method, aqueous two-phase extraction, the ultrafiltration nanofiltration is extracted or the like,
English Patent GB846933 has reported from fermented liquid with Combination utmost point solvent such as methyl alcohol, butanols and glycerine, adopts extraction process to extract tennecetin.Patent GB2106498 has reported the volume method of enrichment and used the Butanol Recycling tennecetin from filtered liquid, thereby obtained a kind of antimycotic mixture stoste, therefrom separable tennecetin.World patent wo92/10580 has reported under low pH and has used the dissolve with methanol tennecetin, removes solid substance then, improves pH with the precipitation tennecetin.The multistage purifying of these leaching process general requirements, process cost are relatively more expensive, and tennecetin is very responsive to acid degradation, has the low shortcoming of extracted amount.United States Patent (USP) 5942611 has been reported a kind of method of effective extraction high quality tennecetin, this procedure mainly comprised for four steps: 1) use the cross flow filter fermented liquid, be concentrated into fermented liquid concentration and reach 10-50% (W/V), in the concentration process, can under 50-70 ℃ of condition, heat fermented liquid to improve steam output and filtering rate.2) pH that regulates fermented liquid is at 10-11, and the water-miscible organic solvent of interpolation q.s such as ethanol, propyl alcohol, Virahol, glycerine etc. dissolve the tennecetin in the fermented liquid.Can by add antioxidant such as xitix, BHA, BHT wait the stability that further improves tennecetin.3) remove by cross flow filter and do not have active fermentation insolubles.4) pH that regulates filtered liquid makes the tennecetin precipitation in the 5.5-7.5 scope.The crystal that filtration obtains separating out can be used for being further purified drying.This method, drying products purity can reach 94-99% (no crystal water calculates), and the tennecetin rate of recovery can reach more than 40%.
But all there is the equipment requirements height in above method, complex process, and product purity is low, and extraction efficiency is poor, and extraction cost height, solvent are difficult to problems such as recovery.
The present invention is directed to the shortcoming that prior art exists, proposed a kind of extraction and purification process of tennecetin, it is easy that it has technology, yield height, purity height, low cost and other advantages.
The present invention is a kind of method of extraction purifying of tennecetin, is to extract tennecetin from fermented liquid, it is characterized in that said method is made up of the following step:
(1) the ph value of adjusting fermented liquid, filtration is collected solid respectively and filtered liquid is standby;
(2) wash the solid of collecting, filter, collect solid and filtered liquid respectively, add certain amount of organic solvent in the solid again, stir, soak.
(3) pH value of the above-mentioned solution of adjusting filters, and collects supernatant liquor;
(4) supernatant liquor is adsorbed by ion exchange resin column, the supernatant liquor after the absorption is collected standby; Wash ion exchange resin column with organic solvent, collect elutriant, regulate the ph value, concentrate, collect solid;
(5) solid of collecting with the pure water washing, the water that has washed is collected standby, promptly gets tennecetin behind the solid drying.
Below the present invention carried out detail describe:
The present invention is applicable to biological fermentation process production tennecetin.After fermentation was finished, the ph value of regulating fermented liquid by the method that adds acid or alkali was to 5.0-8.5, and optimum value is PH6.5.With filtering method collect solid (thalline and crystallization) respectively and filter after liquid filtering liquid, wash solid one time with filtered liquid again, consumption is the 5%-80% of fermentating liquid volume.Add organic solvent then in solid, volume of organic solvent is 5 to 50 times of solid volume.Organic solvent can be that methyl alcohol, ethanol, glycerine or methanol content are not less than 5% methanol mixture.Add acid or alkali and regulate pH value, fully stir, make it even to 5.0-8.5.After stirring, carry out the solid-liquid body with filter method and separate, obtain to contain the supernatant liquor of tennecetin; Supernatant liquor is fed ion exchange resin column, and tennecetin is wherein adsorbed by ion exchange resin, uses methyl alcohol (content is 75-99%) that tennecetin is eluted again.Elutriant is regulated the ph value to 7.0-8.0 through adding acid or alkali, concentrates, and collects solid, and the pure water washing with 3-20 times of volume of solid promptly gets tennecetin behind the solid drying.Ion exchange resin can be used the macropore weakly acidic cation-exchange resin, acrylic acid series D113 for example, D152 or the like.Regulate the acid or the alkali of Ph value usefulness and can use hydrochloric acid, acetic acid, phosphoric acid, fumaric acid or sodium hydroxide, potassium hydroxide, yellow soda ash, sodium bicarbonate.The present invention needs with the pure water washing except that last product, and other each step washing is to remove crystalline concentrated solution or above liquid mixture behind the filtered liquid, supernatant liquor, condensing crystal after the ion exchange resin treatment after the waste liquid of pure water or each collection step comprises filtration with liquid.Make the water and the organic solvent that use among the present invention can realize whole recovery and reuse.
The present invention has following advantage: technology is easy, yield is high, purity high (contents on dry basis 〉=95%), cost are low, and solvent easily reclaims, and is beneficial to environmental protection.
Embodiment 1
Step 1, get 1.5 liters of the fermented liquids (tennecetin content is 6.0g/L) that fermentation back is obtained, the hydrochloric acid with 5% is regulated pH value to 6.5, adds 15g diatomite and does flocculating aids, filters with the B of 2L, till the surperficial absence of liquid of bacterium cake.
Step 2, wash the bacterium cake, drain the bacterium cake with the above-mentioned filtered liquid of 300ml top.
The methyl alcohol that step 3, adding are equivalent to 10 times of volumes of filter cake volume stirs.Hydrochloric acid with 5% is regulated ph value to 6, stirs.
Step 4, carry out solid-liquid separation, obtain supernatant liquor with B.
Step 5, the ion exchange resin column of supernatant liquor by handling well, pillar is collected elutriant with the methanol-eluted fractions of content 95% afterwards.
Step 6, regulate elutriant pH value to 8 with 5% sodium hydroxide, vacuum concentration is collected solid, washs solid with pure water, promptly gets tennecetin 8.2g after the drying, and purity is 89%.Moisture 7.5%, contents on dry basis 96.21%, yield 81%.
Embodiment 2
Step 1, get 20 tons of the fermented liquids (tennecetin content is 6.0g/L) that fermentation back is obtained, regulate pH value to 6.5 with 5% hydrochloric acid, add then on the 200kg diatom and do flocculating aids, Plate Filtration is to there not being the filtrate outflow.
Step 2, wash the bacterium cake with 10 tons of above-mentioned filtered liquids tops, Plate Filtration is to there not being filtrate outflow.
The methyl alcohol that step 3, adding are equivalent to 10 times of volumes of filter cake volume stirs.Hydrochloric acid with 5% is regulated ph value to 6, stirs.
Step 4, carry out solid-liquid separation, obtain supernatant liquor with the undercurrent sheet frame.
Step 5, the ion exchange resin column of supernatant liquor by handling well, pillar content is 95% methanol-eluted fractions afterwards, collects elutriant.
Step 6, the sodium hydroxide with 5% are regulated elutriant pH value to 8, and vacuum concentration is collected solid, with pure washing solid, promptly gets tennecetin 113kg after the drying, and purity is 90%.Moisture 7.2%, contents on dry basis 96.98%, yield 85%.
Claims (7)
1. the method for the extraction purifying of a tennecetin is to extract tennecetin from fermented liquid, it is characterized in that described method is made up of the following step:
(1) the pH value of regulating fermented liquid is to 5.0-8.5, and solid collected by filtration and filtered liquid are standby;
(2) wash the solid of collecting, filter, collect solid and filtered liquid respectively, add certain amount of organic solvent methyl alcohol, acetone, ethanol or methyl alcohol and alcoholic acid mixed solution in the solid again, stir, soak;
(3) the pH value of regulating above-mentioned solution is filtered to 5.0-8.5, collects supernatant liquor;
(4) supernatant liquor is adsorbed by ion exchange resin column, resin adopts macropore low-acid cationic resin D113 or D152, and the supernatant liquor after the absorption is collected standby, wash ion exchange resin column with organic solvent, collect elutriant, regulate the pH value to 7.0-8.0, concentrate, collect solid;
(5) solid of collecting with the pure water washing, the water that has washed is collected standby, promptly gets tennecetin behind the solid drying.
2. according to the method for the extraction purifying of the described a kind of tennecetin of claim 1, it is characterized in that: step (1) and (3) pH value should be adjusted to 6.5; Step (4) pH value should be adjusted to 7.0-8.0.
3. according to the method for the extraction purifying of the described a kind of tennecetin of claim 1, it is characterized in that: the described organic solvent of step (2) is methyl alcohol, acetone, ethanol or methyl alcohol and alcoholic acid mixed solution, and methanol content should be not less than 5% in methyl alcohol and the alcoholic acid mixed solution.
4. according to the method for the extraction purifying of the described a kind of tennecetin of claim 1, it is characterized in that: the consumption of step (2) organic solvent be solid volume 5-50 doubly.
5. according to the method for the extraction purifying of the described a kind of tennecetin of claim 1, it is characterized in that: the used ion exchange resin of step (4) ion exchange resin column is macroporous ion exchange resin D113 or D152.
6. according to the method for the extraction purifying of the described a kind of tennecetin of claim 1, it is characterized in that: the used organic solvent of step (4) washing ion exchange resin column is the methyl alcohol of 75-99%.
7. according to the method for the extraction purifying of the described a kind of tennecetin of claim 1, it is characterized in that: the consumption of step (5) pure water be solid volume 3-20 doubly.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2009101631630A CN101693732B (en) | 2009-08-19 | 2009-08-19 | Method for extracting and purifying natamycin |
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| CN2009101631630A CN101693732B (en) | 2009-08-19 | 2009-08-19 | Method for extracting and purifying natamycin |
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| CN101693732A CN101693732A (en) | 2010-04-14 |
| CN101693732B true CN101693732B (en) | 2011-09-21 |
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| CN2009101631630A Expired - Fee Related CN101693732B (en) | 2009-08-19 | 2009-08-19 | Method for extracting and purifying natamycin |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101914123A (en) * | 2010-09-27 | 2010-12-15 | 郑州奇泓生物科技有限公司 | Method for recovering natamycin from waste liquid |
| CN103665074B (en) * | 2014-01-07 | 2016-05-18 | 厦门大学 | The method for extraction and purification of natamycin in a kind of zymotic fluid |
| ES2940488T3 (en) * | 2018-08-16 | 2023-05-08 | Dsm Ip Assets Bv | New epoxidized polyene amphoteric macrolide and procedure to purify natamycin |
| CN115504835B (en) * | 2021-06-22 | 2023-09-22 | 沈阳化工研究院有限公司 | Biological source composite synergist and application thereof |
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2009
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Non-Patent Citations (1)
| Title |
|---|
| 岳昊博等.纳他霉素(Natamycin)的特性、应用及生产和研究状况.《食品科技》.2007,(第3期),162－166页. * |
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