CN102633862A - Preparation method of farm-oriented nikkomycin - Google Patents
Preparation method of farm-oriented nikkomycin Download PDFInfo
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- CN102633862A CN102633862A CN2012101230995A CN201210123099A CN102633862A CN 102633862 A CN102633862 A CN 102633862A CN 2012101230995 A CN2012101230995 A CN 2012101230995A CN 201210123099 A CN201210123099 A CN 201210123099A CN 102633862 A CN102633862 A CN 102633862A
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Abstract
The invention provides a preparation method of farm-oriented nikkomycin. The preparation method comprises the steps of: regulating pH value of streptomyces tendae fermentation liquor to 2-7; controlling the weight percent content of the nikkomycin in the fermentation liquor with the pH to be 0.1-12 percent; and spraying and drying the fermentation liquor with the content in a spraying and drying tower at a temperature of 50-150 DEG C. The invention also provides a series of preparation methods of the nikkomycin with the purity from low to high (yield from high to low), and an optimal process condition. The invention can be selectively used in processing of various kinds of nikkomycin pesticides; and the integral yield is higher than that of reports in the prior art.
Description
Technical field
The invention belongs to microbial source biological bactericide field, be specifically related to the former medicament preparation of nikemycin.
Background technology
Nikemycin class (Nikkomycins) microbiotic is that German Research person in 1976 finds, adheres to researching and developing this brand-new type antifungal drug for many years both at home and abroad always.Nikemycin is new Polyoxin again, is a kind of nucleosides peptide antibiotics, with chitin synthetase substrate UDN-N-acetylglucosamine similar structure is arranged, and is the strong competitive inhibitor of chitin synthetase, and it is synthetic effectively to suppress in the cell walls Regitex FA.
Contain 20 various ingredients in the nikemycin fermented liquid, wherein studying more biologically active components is Nikemycin Z and X.Agricultural nikemycin is an effective constituent with the X component generally, and it has antimycotic, insect and acarid effect extremely extremely, and control effect is good; Anti-fungus spectra is wide; Select strong toxicity, because extremely low, and decompose easily at nature to Mammals and honeybee and the equal toxicological harmless effect of plant or toxicity; Thereby be a kind of comparatively ideal agricultural antibiotic, have good popularizing application prospect.
The streptomyces ansochromogenes 7100 that Institute of Microorganism, Academia Sinica is separated to from the soil of northeast is good generation bacterium of nikemycin; The nikemycin that it produced all has very strong restraining effect to a lot of phytopathogenic fungis; Field test results proves that also this microbiotic has good control effect to many fungoid Plant diseasess, also has certain preventive and therapeutic effect to harmful insect, mite class simultaneously.
About the existing report of the extraction process of nikemycin, mainly be ion-exchange-resin process or concentrating under reduced pressure method.Like " Hua Zhong Agriculture University " 2007, " nikemycin extraction process, the HPLC quantitative analysis method and the formulation preliminary study " of Wang Zhixin master's Diplomarbeit report.But the preparation method as the former medicine of nikemycin of processing the types of formulation raw material does not appear in the newspapers as yet.
Summary of the invention
In view of this, in order to overcome the defective of prior art, the invention provides a kind of former medicament preparation of nikemycin that can be used for all kinds of preparation processing.
The former medicament preparation of a kind of agricultural nikemycin provided by the invention, said method comprises step: (1)
The pH value of adjustment streptomyces tendae fermented liquid is to 2-7, and the nikemycin weight percent content is at 0.1%-12% in the fermented liquid of the said pH of (2) control, and spraying drying is carried out with 50 ℃-150 ℃ of the temperature fermented liquid to said content in the dried tower of spray in (3).
Further, the said fermented liquid pH value of said step (1) adjustment is 3.0, and (2) obtain the fermented liquid that weight percent content is the said pH of 0.1%-2%, and spraying drying is carried out to said content fermented liquid for 85 ℃ with temperature in (3) in the dried tower of spray.
Adjust the pH value of fermented liquid with 33% technical hydrochloric acid or 90% above oxalic acid, the nikemycin weight percent content generally is not higher than 2% in the fermented liquid, and content is lower than that 0.1% fermented liquid is directly abandoned or with using it for anything else.
Above step reaches wherein nikemycin content through the pH of adjustment fermented liquid, and the spraying drying temperature, makes the former medicine yield of nikemycin of preparation be up to 80%.The former medicine purity of nikemycin is 30-40%, because the former medicine of nikemycin of preparation contains mycelia, when process preparation, need pass through coarse reduction and fine powder is broken, and operation is complicacy, and energy consumption is higher, and the preparation wetting time that is processed into is longer.
Further; Behind the filtering fermentation liquor of the said pH of said step (2); Adopt the film under vacuum thickner at relative vacuum degree-0.09Mpa; Concentrate the fermentation filtered liq between 50 ℃-100 ℃ of the temperature to weight percent content 0.5%-5%, by weight concentrated ferment filtrate: carrier=1:0.01-1 adds carrier, paddle rotating speed 10 ~ 120r/min slurrying.
Be preferably, said carrier is one or more the combination in WHITE CARBON BLACK, kaolin, wilkinite, zeyssatite, attapulgite, light calcium carbonate, talcum powder, potter's clay, pyrophyllite, smectite, clay, illite, mica powder, perlite, the calcite.
More preferably do, said step (2) adopts the film under vacuum thickner to concentrate said fermentation filtered liq and is weight percentage 4% to nikemycin content, and thickening temperature is 60 ℃.
More preferably, said step (2) is by weight concentrating the fermentation filtered liq: kaolin=1:0.05 adds the slurrying of carrier kaolin, and the paddle rotating speed is 50r/min during slurrying.
The former medicine of nikemycin of above step preparation, its purity is increased to 50-60%, and when process preparation, it is broken directly to carry out fine powder, and operation is simple, and energy consumption is lower.And the preparation that processes, wetting time is short.Because contain carrier in the former medicine, good fluidity is beneficial to follow-up preparation processing; The product moisture absorption reduces, and the raising of stable effective ingredients property prolongs the shelf lives of former medicine.Meanwhile, its yield directly spraying drying slightly reduces, and reduces to 75% by 80%.
Further; Said step (2) is carried out according to following step by step: A. filters the fermented liquid of said pH, and the said ferment filtrate of B. adsorbs through 001 * 1,001 * 2,001 * 3,001 * 4 or 001 * 5 h type resin, flow velocity be 1/10-1/100 resin volume/minute; C. adopt concentration 0.01mol/L-1mol/L ammoniacal liquor to carry out wash-out; Flow velocity be 1/10-1/100 resin volume/minute, D. adopts 001 * 12,001 * 13 or 001 * 14 resin to remove ammonium radical ion in the elutriant, flow velocity be 1/10-1/100 resin volume/minute; E. adopt the film under vacuum thickner to concentrate the said ammonium radical ion elutriant that goes; Make nikemycin content between weight percent 1% ~ 12%, the relative vacuum degree is controlled at-0.09Mpa when concentrating, and temperature is controlled between 50 ℃ ~ 100 ℃.
Be preferably; Said step (2) is carried out according to following step by step: A. filters the fermented liquid of said pH, and the said ferment filtrate of B. adsorbs through 001 * 3 h type resin, flow velocity be 1/50 resin volume/minute; C. adopting concentration is that the ammoniacal liquor of 0.5mol/l carries out wash-out; Flow velocity be 1/50 resin volume/minute, D. adopts 001 * 14 h type resin to remove ammonium radical ion in the elutriant, flow velocity be 1/50 resin volume/minute; E. concentrate the said ammonium radical ion elutriant that goes, making nikemycin content is 8% at weight percent.
More preferably, said step (2) adopts the film under vacuum thickner at 60 ℃ the said ammonium radical ion elutriant that goes to be concentrated.
The former medicine purity of nikemycin of above-mentioned steps preparation is brought up to 70-80%, owing to removed impurity, is full water-soluble, both can be processed into solid preparation and also can be processed into liquid preparation.Meanwhile, the former medicine yield of nikemycin is reduced to 60-63%.Because resin takes off assorted and takes off complicated procedures of forming such as ammonium, makes former medicine production cost that certain increase arranged.
Beneficial effect of the present invention is:
1. the invention provides the former medicine purity of nikemycin a series of preparing methods of (yield is from high to low) from low to high, and optimum process condition, can select to be used for the processing of all kinds of nikemycin pesticide preparation.And whole yield all is higher than the report of prior art.
2. the present invention adopts simple drying process with atomizing, and finds out best spraying drying temperature, and temperature during spraying drying is if be lower than 50 ℃, and material can stick in the tower, can not discharge smoothly, causes long-time high temperature, and the nikemycin yield is lower; Temperature is in the time of 75 ℃ ~ 85 ℃, and product moisture content can not satisfy the requirement of Pesticidal products; And temperature can cause the product high bake to decompose when surpassing 85 ℃, and the nikemycin yield reduces once more.When temperature was 85 ℃, the nikemycin yield was the highest, and dry loss of weight is 3.0%-3.5%, met the product standard requirement.Make that the former medicine production of high yield nikemycin becomes possibility in the industrial production.
Embodiment
Further illustrate the present invention among the embodiment below, this does not limit the scope of the invention.
Embodiment 1
The nikemycin fermented liquid, using 33% technical hydrochloric acid adjustment pH is 3.0, nikemycin content is 1% in the fermented liquid.Weigh nikemycin fermented liquid 1000kg, get into the spray-drying tower spraying drying through preheating, regulate EAT, temperature maintenance is at 85 ℃ in the tower when making spraying drying, and the powder of collecting promptly gets the former medicine of nikemycin of the present invention.
Embodiment 2
The nikemycin fermented liquid, using 33% technical hydrochloric acid adjustment pH is 3.0, nikemycin content is 0.8% in the fermented liquid.Weigh nikemycin fermented liquid 1000kg, get into the spray-drying tower spraying drying through preheating, regulate EAT, temperature maintenance is at 85 ℃ in the tower when making spraying drying, and the powder of collecting promptly gets the former medicine of nikemycin of the present invention.
Embodiment 3
The nikemycin fermented liquid; Using 33% technical hydrochloric acid adjustment pH is 3.0; Nikemycin content is 1% in the fermented liquid, weighs nikemycin fermented liquid 1000kg, filtering fermentating liquid; Adopt the film under vacuum thickner at relative vacuum degree-0.09Mpa, it is 4% that 60 ℃ of concentrated down fermentation filtered liqs of temperature make nikemycin content.In uncovered stirring tank, add above-mentioned nikemycin concentrated filtrate earlier, open then and stir, the control rotating speed is 50r/min.By weight concentrating the fermentation filtered liq: kaolin=1:0.05 adds the carrier kaolin, under rotating speed 30r/min condition, evenly adds kaolin with the speed of PM 1kg, processes slurries.Slurries get into the spray-drying tower spraying drying through preheating, regulate EAT, and temperature maintenance is at 85 ℃ in the tower when making spraying drying, and the powder of collecting promptly gets the former medicine of nikemycin of the present invention.
Embodiment 4
The nikemycin fermented liquid; Using 33% technical hydrochloric acid adjustment pH is 3.0; Nikemycin content is 1% in the fermented liquid, weighs nikemycin fermented liquid 1200kg, filtering fermentating liquid; Adopt the film under vacuum thickner at relative vacuum degree-0.09Mpa, it is 4% that 60 ℃ of concentrated down fermentation filtered liqs of temperature make nikemycin content.In uncovered stirring tank, add above-mentioned nikemycin concentrated filtrate earlier, open then and stir, the control rotating speed is 50r/min.By weight concentrating the fermentation filtered liq: kaolin=1:0.05 adds the carrier kaolin, under rotating speed 30r/min condition, evenly adds kaolin with the speed of PM 1kg, processes slurries.Slurries get into the spray-drying tower spraying drying through preheating, regulate EAT, and temperature maintenance is at 85 ℃ in the tower when making spraying drying, and the powder of collecting promptly gets the former medicine of nikemycin of the present invention.
Embodiment 5
The nikemycin fermented liquid, using 33% technical hydrochloric acid adjustment pH is 3.0, nikemycin content is 1.2% in the fermented liquid, weighs nikemycin fermented liquid 1000kg, filtering fermentating liquid, filtrating is through the absorption of 001 * 3 h type resin, flow velocity be 1/50 resin volume/minute.The resin that absorption is accomplished, the washing back adopts ammoniacal liquor to carry out wash-out, washes effective constituent, ammonia concn is 0.5mol/L, flow velocity be 1/50 resin volume/minute.Adopt 001 * 14 resin to go out the ammonium radical ion, flow velocity be 1/50 resin volume/minute.Adopt the film under vacuum thickner at relative vacuum degree-0.09Mpa, 60 ℃ of temperature concentrate the elutriant that removes the ammonium radical ion down, and to make nikemycin content be 8%.Go the concentrate eluant of ammonium radical ion to get into the spray-drying tower spraying drying through preheating, regulate EAT, temperature maintenance is at 85 ℃ in the tower when making spraying drying, and the powder of collecting promptly gets the former medicine of nikemycin of the present invention.
Embodiment 6
The nikemycin fermented liquid, using 33% technical hydrochloric acid adjustment pH is 3.0, nikemycin content is 1% in the fermented liquid, weighs nikemycin fermented liquid 1300kg, filtering fermentating liquid, filtrating is through the absorption of 001 * 3 h type resin, flow velocity be 1/50 resin volume/minute.The resin that absorption is accomplished, the washing back adopts ammoniacal liquor to carry out wash-out, washes effective constituent, and ammonia concn is 0.5mol/L, the preferred 1/50 resin volume of flow velocity/minute.Adopt 001 * 14 resin to go out the ammonium radical ion, flow velocity be 1/50 resin volume/minute.Adopting the film under vacuum thickner to concentrate and making nikemycin content is 8%, and the relative vacuum degree is controlled at-0.09Mpa when concentrating, and temperature is controlled between 60 ℃.Concentrated filtrate gets into the spray-drying tower spraying drying through preheating, regulates EAT, and temperature maintenance is at 85 ℃ in the tower when making spraying drying, and the powder of collecting promptly gets the former medicine of nikemycin of the present invention.
Test Example 1:
Purity test: to the former medicine purity testing of the foregoing description 1-6 gained nikemycin result
Test Example 2:
Yield test: nikemycin yield among the foregoing description 1-6 is measured the result
Test Example 3:
The inventive method is produced other index contrasts of former medicine
Although pass through with reference to the preferred embodiments of the present invention; Invention has been described; But those of ordinary skill in the art should be appreciated that and can make various changes to it in form with on the details, and the spirit and scope of the present invention that do not depart from appended claims and limited.
Claims (9)
1. former medicament preparation of agricultural nikemycin; It is characterized in that; Said method comprises step: the pH value of (1) adjustment streptomyces tendae fermented liquid is to 2-7; (2) the nikemycin weight percent content is at 0.1%-12% in the fermented liquid of the said pH of control, and spraying drying is carried out with 50 ℃-150 ℃ of the temperature fermented liquid to said content in the dried tower of spray in (3).
2. according to the former medicament preparation of the described agricultural nikemycin of claim 1; It is characterized in that; The said fermented liquid pH value of said step (1) adjustment is 3.0; (2) obtain the fermented liquid that weight percent content is the said pH value of 0.1%-2%, spraying drying is carried out to said content fermented liquid for 85 ℃ with temperature in (3) in the dried tower of spray.
3. according to the former medicament preparation of the described agricultural nikemycin of claim 1; It is characterized in that; Behind the filtering fermentation liquor of the said pH of said step (2), adopt the film under vacuum thickner, concentrate the fermentation filtered liq to weight percent content 0.5%-5% between 50 ℃-100 ℃ of the temperature at relative vacuum degree-0.09Mpa; By weight concentrated ferment filtrate: carrier=1:0.01-1 adds carrier, paddle rotating speed 10 ~ 120r/min slurrying.
4. according to the former medicament preparation of the described agricultural nikemycin of claim 3; It is characterized in that said carrier is one or more the combination in WHITE CARBON BLACK, kaolin, wilkinite, zeyssatite, attapulgite, light calcium carbonate, talcum powder, potter's clay, pyrophyllite, smectite, clay, illite, mica powder, perlite, the calcite.
5. according to the former medicament preparation of the described agricultural nikemycin of claim 3, it is characterized in that said step (2) adopts the film under vacuum thickner to concentrate said fermentation filtered liq and is weight percentage 4% to nikemycin content, thickening temperature is 60 ℃.
6. according to the former medicament preparation of the described agricultural nikemycin of claim 3, it is characterized in that said step (2) is by weight concentrating the fermentation filtered liq: kaolin=1:0.05 adds the slurrying of carrier kaolin, and the paddle rotating speed is 50r/min during slurrying.
7. according to the former medicament preparation of the described agricultural nikemycin of claim 1; It is characterized in that; Said step (2) is carried out according to following step by step: A. filters the fermented liquid of said pH, and the said ferment filtrate of B. adsorbs through 001 * 1,001 * 2,001 * 3,001 * 4 or 001 * 5 h type resin, flow velocity be 1/10-1/100 resin volume/minute; C. adopt concentration 0.01mol/L-1mol/L ammoniacal liquor to carry out wash-out; Flow velocity be 1/10-1/100 resin volume/minute, D. adopts 001 * 12,001 * 13 or 001 * 14 resin to remove ammonium radical ion in the elutriant, flow velocity be 1/10-1/100 resin volume/minute; E. adopt the film under vacuum thickner to concentrate the said ammonium radical ion elutriant that goes; Make nikemycin content between weight percent 1% ~ 12%, the relative vacuum degree is controlled at-0.09Mpa when concentrating, and temperature is controlled between 50 ℃ ~ 100 ℃.
8. according to the former medicament preparation of the described agricultural nikemycin of claim 7, it is characterized in that said step (2) is carried out according to following step by step: A. filters the fermented liquid of said pH; B. said ferment filtrate adsorbs through 001 * 3 h type resin; Flow velocity be 1/50 resin volume/minute, it is that the ammoniacal liquor of 0.5mol/l carries out wash-out that C. adopts concentration, flow velocity be 1/50 resin volume/minute; D. adopt 001 * 14 h type resin to remove ammonium radical ion in the elutriant; Flow velocity be 1/50 resin volume/minute, E. concentrates the said ammonium radical ion elutriant that goes, making nikemycin content is 8% at weight percent.
9. according to the former medicament preparation of the described agricultural nikemycin of claim 7, it is characterized in that said step (2) adopts the film under vacuum thickner at 60 ℃ the said ammonium radical ion elutriant that goes to be concentrated.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103708960A (en) * | 2013-12-24 | 2014-04-09 | 安徽师范大学 | Liquid-state compound-microorganism bacterial fertilizer as well as production method and application thereof |
| CN106614756A (en) * | 2016-12-20 | 2017-05-10 | 陕西麦可罗生物科技有限公司 | Preparation method of nikkomycin soluble granules |
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| WO1989002744A1 (en) * | 1987-10-02 | 1989-04-06 | The University Of Colorado Foundation, Inc. | Synergistic antifungal protein and compositions containing same |
| WO2000072865A2 (en) * | 1999-05-31 | 2000-12-07 | Fujisawa Pharmaceutical Co., Ltd. | Antifungal combination use |
| CN1548526A (en) * | 2003-05-07 | 2004-11-24 | 中国科学院微生物研究所 | High-yield engineering bacterium of nicomycin x component and its application |
| CN1733921A (en) * | 2004-08-11 | 2006-02-15 | 中国科学院微生物研究所 | Nikemycin biosynthetic controlling gene and proteins encoded thereof and expression engineering bacteria |
| CN101591634A (en) * | 2009-07-02 | 2009-12-02 | 中国科学院微生物研究所 | A kind of method and special culture media and engineering bacteria of producing Nikemycin Z |
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2012
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO1989002744A1 (en) * | 1987-10-02 | 1989-04-06 | The University Of Colorado Foundation, Inc. | Synergistic antifungal protein and compositions containing same |
| WO2000072865A2 (en) * | 1999-05-31 | 2000-12-07 | Fujisawa Pharmaceutical Co., Ltd. | Antifungal combination use |
| WO2000072865A3 (en) * | 1999-05-31 | 2001-05-10 | Fujisawa Pharmaceutical Co | Antifungal combination use |
| CN1548526A (en) * | 2003-05-07 | 2004-11-24 | 中国科学院微生物研究所 | High-yield engineering bacterium of nicomycin x component and its application |
| CN1733921A (en) * | 2004-08-11 | 2006-02-15 | 中国科学院微生物研究所 | Nikemycin biosynthetic controlling gene and proteins encoded thereof and expression engineering bacteria |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103708960A (en) * | 2013-12-24 | 2014-04-09 | 安徽师范大学 | Liquid-state compound-microorganism bacterial fertilizer as well as production method and application thereof |
| CN103708960B (en) * | 2013-12-24 | 2016-06-01 | 安徽师范大学 | A kind of liquid composite microbic bacterial fertilizer and production method and purposes |
| CN106614756A (en) * | 2016-12-20 | 2017-05-10 | 陕西麦可罗生物科技有限公司 | Preparation method of nikkomycin soluble granules |
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