CN1891709A - Natamycin extracting and purifying method - Google Patents
Natamycin extracting and purifying method Download PDFInfo
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- CN1891709A CN1891709A CN 200510035585 CN200510035585A CN1891709A CN 1891709 A CN1891709 A CN 1891709A CN 200510035585 CN200510035585 CN 200510035585 CN 200510035585 A CN200510035585 A CN 200510035585A CN 1891709 A CN1891709 A CN 1891709A
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Abstract
The invention relates to a method for the extraction and purification of natamycin, in which, it adopts the microbes' fermentation method to extract and purify the natamycin from the natamycin's broth which has been cultivated and fermented through five steps under the technology conditions. The product has the advantage of high yield, high purity (>= 80%) and low cost.
Description
Technical field
The present invention relates to the extracting and purifying method of a kind of extracting and purifying method of antifongin, particularly a kind of tennecetin.
Background technology
The molecular formula of tennecetin is C
33H
47NO
13Molecular weight is 665.75, and its structural formula is:
It is a kind of polyene macrolide antifungal element, and it can suppress the growth of harmful fungoid and not act on human body beneficial's flora, can be used as food preservatives and uses.At present commercially available tennecetin price is higher, and its application is subjected to certain influence.
The natamycin fermentation liquor of bacterial classification behind cultivation, fermentating metabolism that the present invention adopts microbe fermentation method promptly to be added when fermentation, the target product tennecetin that obtains after certain step and processing condition, it has productive rate height, purity height, low cost and other advantages.
Summary of the invention
The object of the present invention is to provide a kind of processing method of extracting tennecetin in the purifying biological fermented liquid efficiently.
Purpose of the present invention can reach by following measure, and this method may further comprise the steps and processing condition:
Step 1. concentrating under reduced pressure method or centrifuging concentrated broth
The natamycin fermentation liquor that the fermentation back is obtained concentrates with concentrating under reduced pressure method or centrifuging, and its temperature of concentrating under reduced pressure method is controlled at 50～60 ℃;
Step 2. is washed concentrated solution or solid with clean water
When fermented liquid is concentrated into can not concentrate the time or after centrifugal, add concentrate primary fermentation liquid long-pending 10% clean water flushing concentrated solution or solid after, reconcentration anhydrates to can not concentrate the time or centrifugal solid;
Step 3. solubilizing agent and adding extracts after the pH value of extracting solution is regulated in acid, alkali.
(1: solvent 1V/V) (methyl alcohol, acetone, ethanol) extracts the tennecetin in the concentrated broth for adding and concentrated broth or solid equal-volume; Add acid or add and extract after alkali is regulated the pH value of extracting solution, regulate pH value 1.0～4.5 when adding acid,, extract 2～25 ℃ of temperature, extraction time 0.5～4.5h if regulate pH value 10.0～11.0 when adding alkali;
The solid-liquid separation of step 4. extracting solution obtains supernatant liquor
After reaching extraction time, extracting solution carries out solid-liquid separation with centrifugal method, obtains the pH value that supernatant liquor step 5. is regulated supernatant liquor, carries out solid-liquid separation, collects solid.
Supernatant liquor is regulated pH value 5.5～7.0 through adding acid or alkali, carries out solid-liquid separation after leaving standstill 1～2h, collects solid, uses the washing solid 2 times of 2 times of volumes of solid afterwards, promptly gets tennecetin behind the solid drying.
The present invention has following advantage: productive rate height, purity height (〉=80%), cost are low.
Embodiment
The present invention will now be further detailed embodiment.
Example 1
Step 1. decompression method concentrated broth.
Get 400 liters of the natamycin fermentation liquors (tennecetin content is 6.0g/L) that the fermentation back is obtained, be positioned in 500 liters of vacuum concentration pots, under 50～60 ℃ of temperature, concentrate, till can not concentrating.
Step 2. is washed concentrated solution with clean water.
With 40 liters of clean waters flushing concentrated solutions, reconcentration anhydrates to can not concentrate the time.
Step 3. solubilizing agent and adding extracts after the pH value of extracting solution is regulated in acid
Add with concentrate after the isopyknic acetone of fermented liquid, allow fermented liquid and acetone stir.PH value to 1.0 is regulated in acid with 20～30% (available hydrochloric acid, acetic acid, phosphoric acid, nitric acid, sulfuric acid, carbonic acid), extracts 3h down at 5 ℃.
The solid-liquid separation of step 4. extracting solution obtains supernatant liquor
After reaching extraction time, extracting solution carries out solid-liquid separation with centrifugal method, obtains supernatant liquor.Step 5. is regulated the supernatant liquor pH value, carries out solid-liquid separation, collects solid.
Alkali with 20～30% (can use sodium hydroxide, potassium hydroxide) is regulated pH value to 6.0, leaves standstill 1.5h, and is centrifugal, collects solid, with clean washing solid twice, promptly gets tennecetin 1450g after the drying, and purity is 88%.
Example 2
Step 1. centrifuging concentrated broth.
It is centrifugal with whizzer to get the natamycin fermentation liquor 4000 liters (tennecetin content is 5.5g/L) that is obtained after the fermentation, collects solid.
Step 2. is washed solid with clean water.
With 400 liters of clean water flushing solid 20min, centrifugal again after having washed, collect solid.
Step 3. solubilizing agent and adding extracts after alkali is regulated the pH value of extracting solution.。
Add with centrifugal after the isopyknic methyl alcohol of solid, allow solid and methyl alcohol stir.Alkali with 20～30% (can use sodium hydroxide, potassium hydroxide) is regulated pH value to 10.9, extracts 0.5h down at 25 ℃.
The solid-liquid separation of step 4. extracting solution obtains supernatant liquor
After reaching extraction time, extracting solution carries out solid-liquid separation with centrifugal method, obtains supernatant liquor step 5. and regulates the supernatant liquor pH value, carries out solid-liquid separation, collects solid.
PH value to 6.0 is regulated in acid with 20～30% (available hydrochloric acid, acetic acid, phosphoric acid, nitric acid, sulfuric acid, carbonic acid), leaves standstill 1.5h, and is centrifugal, collects solid, with clean washing solid twice, promptly gets tennecetin 13.5kg after the drying, and purity is 90%.
Claims (1)
1, a kind of extracting and purifying method of tennecetin is characterized in that: this method may further comprise the steps and processing condition:
Step 1. concentrating under reduced pressure method or centrifuging concentrated broth
The natamycin fermentation liquor that the fermentation back is obtained concentrates with concentrating under reduced pressure method or centrifuging, and its temperature of concentrating under reduced pressure method is controlled at 50～60 ℃;
Step 2. is washed concentrated solution or solid with clean water
When fermented liquid is concentrated into can not concentrate the time or after centrifugal, add concentrate primary fermentation liquid long-pending 10% clean water flushing concentrated solution or solid after, reconcentration anhydrates to can not concentrate the time or centrifugal solid; Step 3. solubilizing agent and adding extracts after the pH value of extracting solution is regulated in acid, alkali;
(1: solvent 1V/V) (methyl alcohol, acetone, ethanol) extracts the tennecetin in the concentrated broth for adding and concentrated broth or solid equal-volume; Add acid or add and extract after alkali is regulated the pH value of extracting solution, regulate pH value 1.0～4.5 when adding acid,, extract 2～25 ℃ of temperature, extraction time 0.5～4.5h if regulate pH value 10.0～11.0 when adding alkali;
The solid-liquid separation of step 4. extracting solution obtains supernatant liquor
After reaching extraction time, extracting solution carries out solid-liquid separation with centrifugal method, obtains the pH value that supernatant liquor step 5. is regulated supernatant liquor, carries out solid-liquid separation, collects solid
Supernatant liquor carries out solid-liquid separation after adding acid or alkali adjusting pH value 5.5～7.0, leaving standstill 1～2h, collect solid, and the water with 2 times of volumes of solid cleans solid 2 times afterwards, promptly gets tennecetin behind the solid drying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100355851A CN100393738C (en) | 2005-07-05 | 2005-07-05 | Natamycin extracting and purifying method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100355851A CN100393738C (en) | 2005-07-05 | 2005-07-05 | Natamycin extracting and purifying method |
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| Publication Number | Publication Date |
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| CN1891709A true CN1891709A (en) | 2007-01-10 |
| CN100393738C CN100393738C (en) | 2008-06-11 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB2005100355851A Expired - Fee Related CN100393738C (en) | 2005-07-05 | 2005-07-05 | Natamycin extracting and purifying method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101062934B (en) * | 2007-05-31 | 2010-05-19 | 山东鲁抗医药股份有限公司 | Method for extracting natamycin from fermentation technique culture |
| CN101418027B (en) * | 2008-12-22 | 2011-07-20 | 山东省生物药物研究院 | Method for recovering natamycin |
| CN103665074A (en) * | 2014-01-07 | 2014-03-26 | 厦门大学 | Extraction and purification method for natamycin in fermentation broth |
| CN112543761A (en) * | 2018-08-16 | 2021-03-23 | 帝斯曼知识产权资产管理有限公司 | Novel all-trans polyene amphoteric macrolides and process for purifying natamycin thereof |
| CN112585150A (en) * | 2018-08-16 | 2021-03-30 | 帝斯曼知识产权资产管理有限公司 | Novel epolyonic amphomacrolides and process for purifying natamycin |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AU2408092A (en) * | 1991-08-05 | 1993-03-02 | Bio-Technical Resources | Continuous natamycin production |
| DK0754239T3 (en) * | 1994-03-31 | 1998-05-18 | Cultor Oy | Process for recovery of natamycin |
| US5985845A (en) * | 1999-01-21 | 1999-11-16 | Carter; A. Franklin | Methods for reducing mortality rates in poultry |
| US6239113B1 (en) * | 1999-03-31 | 2001-05-29 | Insite Vision, Incorporated | Topical treatment or prevention of ocular infections |
| CN1515678A (en) * | 2003-08-25 | 2004-07-28 | 天津科技大学 | Preparation method of natamycin |
-
2005
- 2005-07-05 CN CNB2005100355851A patent/CN100393738C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101062934B (en) * | 2007-05-31 | 2010-05-19 | 山东鲁抗医药股份有限公司 | Method for extracting natamycin from fermentation technique culture |
| CN101418027B (en) * | 2008-12-22 | 2011-07-20 | 山东省生物药物研究院 | Method for recovering natamycin |
| CN103665074A (en) * | 2014-01-07 | 2014-03-26 | 厦门大学 | Extraction and purification method for natamycin in fermentation broth |
| 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 |
| CN112543761A (en) * | 2018-08-16 | 2021-03-23 | 帝斯曼知识产权资产管理有限公司 | Novel all-trans polyene amphoteric macrolides and process for purifying natamycin thereof |
| CN112585150A (en) * | 2018-08-16 | 2021-03-30 | 帝斯曼知识产权资产管理有限公司 | Novel epolyonic amphomacrolides and process for purifying natamycin |
| CN112585150B (en) * | 2018-08-16 | 2024-03-29 | 帝斯曼知识产权资产管理有限公司 | New epoxypolyene ampholytic macrolides and process for purifying natamycin |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100393738C (en) | 2008-06-11 |
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