CN113355382A - Production process of abamectin - Google Patents
Production process of abamectin Download PDFInfo
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- CN113355382A CN113355382A CN202110820101.3A CN202110820101A CN113355382A CN 113355382 A CN113355382 A CN 113355382A CN 202110820101 A CN202110820101 A CN 202110820101A CN 113355382 A CN113355382 A CN 113355382A
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- mycelium
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- methanol
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 25
- 239000005660 Abamectin Substances 0.000 title claims abstract description 21
- IBSREHMXUMOFBB-JFUDTMANSA-N 5u8924t11h Chemical compound O1[C@@H](C)[C@H](O)[C@@H](OC)C[C@@H]1O[C@@H]1[C@@H](OC)C[C@H](O[C@@H]2C(=C/C[C@@H]3C[C@@H](C[C@@]4(O3)C=C[C@H](C)[C@@H](C(C)C)O4)OC(=O)[C@@H]3C=C(C)[C@@H](O)[C@H]4OC\C([C@@]34O)=C/C=C/[C@@H]2C)/C)O[C@H]1C.C1=C[C@H](C)[C@@H]([C@@H](C)CC)O[C@]11O[C@H](C\C=C(C)\[C@@H](O[C@@H]2O[C@@H](C)[C@H](O[C@@H]3O[C@@H](C)[C@H](O)[C@@H](OC)C3)[C@@H](OC)C2)[C@@H](C)\C=C\C=C/2[C@]3([C@H](C(=O)O4)C=C(C)[C@@H](O)[C@H]3OC\2)O)C[C@H]4C1 IBSREHMXUMOFBB-JFUDTMANSA-N 0.000 title claims abstract description 20
- 229950008167 abamectin Drugs 0.000 title claims abstract description 20
- 238000002425 crystallisation Methods 0.000 claims abstract description 39
- 230000008025 crystallization Effects 0.000 claims abstract description 39
- 238000000034 method Methods 0.000 claims abstract description 19
- 238000000855 fermentation Methods 0.000 claims abstract description 17
- 230000004151 fermentation Effects 0.000 claims abstract description 17
- 239000000725 suspension Substances 0.000 claims abstract description 15
- 238000002386 leaching Methods 0.000 claims abstract description 13
- 238000012258 culturing Methods 0.000 claims abstract description 8
- 230000001580 bacterial effect Effects 0.000 claims abstract description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 66
- 238000001035 drying Methods 0.000 claims description 16
- 230000008020 evaporation Effects 0.000 claims description 15
- 238000001704 evaporation Methods 0.000 claims description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000013078 crystal Substances 0.000 claims description 6
- 238000004806 packaging method and process Methods 0.000 claims description 4
- 238000009833 condensation Methods 0.000 claims description 3
- 230000005494 condensation Effects 0.000 claims description 3
- 238000007602 hot air drying Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 238000002156 mixing Methods 0.000 claims 1
- 238000011084 recovery Methods 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 7
- 239000012535 impurity Substances 0.000 abstract description 6
- 239000003814 drug Substances 0.000 description 4
- 229940079593 drug Drugs 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- KWGRBVOPPLSCSI-WPRPVWTQSA-N (-)-ephedrine Chemical compound CN[C@@H](C)[C@H](O)C1=CC=CC=C1 KWGRBVOPPLSCSI-WPRPVWTQSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 208000005374 Poisoning Diseases 0.000 description 2
- 230000002950 deficient Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 231100000572 poisoning Toxicity 0.000 description 2
- 230000000607 poisoning effect Effects 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 208000024891 symptom Diseases 0.000 description 2
- 230000008673 vomiting Effects 0.000 description 2
- 206010000383 Accidental poisoning Diseases 0.000 description 1
- 208000012661 Dyskinesia Diseases 0.000 description 1
- 239000009471 Ipecac Substances 0.000 description 1
- 208000006550 Mydriasis Diseases 0.000 description 1
- 206010044565 Tremor Diseases 0.000 description 1
- 206010047700 Vomiting Diseases 0.000 description 1
- RRZXIRBKKLTSOM-XPNPUAGNSA-N avermectin B1a Chemical compound C1=C[C@H](C)[C@@H]([C@@H](C)CC)O[C@]11O[C@H](C\C=C(C)\[C@@H](O[C@@H]2O[C@@H](C)[C@H](O[C@@H]3O[C@@H](C)[C@H](O)[C@@H](OC)C3)[C@@H](OC)C2)[C@@H](C)\C=C\C=C/2[C@]3([C@H](C(=O)O4)C=C(C)[C@@H](O)[C@H]3OC\2)O)C[C@H]4C1 RRZXIRBKKLTSOM-XPNPUAGNSA-N 0.000 description 1
- KWGRBVOPPLSCSI-UHFFFAOYSA-N d-ephedrine Natural products CNC(C)C(O)C1=CC=CC=C1 KWGRBVOPPLSCSI-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229960002179 ephedrine Drugs 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 210000003205 muscle Anatomy 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 210000004916 vomit Anatomy 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/44—Preparation of O-glycosides, e.g. glucosides
- C12P19/60—Preparation of O-glycosides, e.g. glucosides having an oxygen of the saccharide radical directly bound to a non-saccharide heterocyclic ring or a condensed ring system containing a non-saccharide heterocyclic ring, e.g. coumermycin, novobiocin
- C12P19/62—Preparation of O-glycosides, e.g. glucosides having an oxygen of the saccharide radical directly bound to a non-saccharide heterocyclic ring or a condensed ring system containing a non-saccharide heterocyclic ring, e.g. coumermycin, novobiocin the hetero ring having eight or more ring members and only oxygen as ring hetero atoms, e.g. erythromycin, spiramycin, nystatin
- C12P19/623—Avermectin; Milbemycin; Ivermectin; C-076
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H17/00—Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
- C07H17/04—Heterocyclic radicals containing only oxygen as ring hetero atoms
- C07H17/08—Hetero rings containing eight or more ring members, e.g. erythromycins
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Biotechnology (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
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- Bioinformatics & Cheminformatics (AREA)
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- Fodder In General (AREA)
Abstract
The invention discloses a production process of abamectin, which comprises the following production steps: s1, strain culture: firstly, culturing a strain, placing the strain on a culture shelf for culture, and then producing an inclined plane on the surface of the strain after the culture is finished so as to drip a strain suspension downwards and collect the strain suspension; s2, fermentation: culturing the collected bacterial suspension, and adding corresponding culture solution. The invention adopts a mode of improving crystallization processing in the production process and a mode of three-time crystallization, which is different from the traditional abamectin processing technology, so that the purity of the mycelium can be greatly improved, and two processes of leaching and desugaring are additionally added in the two processes of fermentation and crystallization, so that impurities in the mycelium can be removed before the mycelium is crystallized, and granular impurities and other components in the mycelium are removed, so that the mycelium after crystallization processing can be purer, and the production technology is more reasonable.
Description
Technical Field
The invention relates to the technical field of chemical substances, in particular to a production process of abamectin.
Background
The avermectin is a chemical substance and has a molecular formula of C49H75NO 13; C48H73NO13, wherein the original drug is white or light yellow crystalline powder, the melting point is 141-146 ℃, the original drug is soluble in acetone and methanol, slightly soluble in water and insoluble in hexane, the original drug is stable under the common storage condition when being stored, and the toxicity and the poisoning symptoms are as follows: the original medicine has high toxicity, the preparation has low toxicity and is nearly nontoxic; the early symptoms after poisoning are mydriasis, dyskinesia and trembling muscle, vomit is caused when serious, and vomiting is induced immediately when accidental poisoning is cured and ipecac syrup or ephedrine is taken for patients.
When the existing abamectin is produced, the whole processing and production process is simple, so that the condition that the purity and the quality of the mycelium cannot reach the standard easily during subsequent production is caused, a large number of defective products are easy to appear after the finished product is produced, and the high-quality requirement of the product cannot be met during production.
Disclosure of Invention
The invention provides a production process of abamectin, aiming at the defects in the background technology.
The invention adopts the following technical scheme to solve the phenomenon, and the production process of the abamectin comprises the following steps:
s1, firstly, culturing the strain, putting the strain on a culture shelf for culture, and then after the culture is finished, producing an inclined plane on the surface of the strain so as to drip the strain suspension downwards and collecting the suspension;
s2, culturing the collected bacterial suspension, adding corresponding culture solution, and then placing in a fermentation tank for fermentation after the culture is completed, wherein the fermentation temperature is 28 +/-0.5 ℃ and the fermentation time is 210-320 h;
s3, when the fermentation is finished, mycelium can be extracted from the bacterial suspension, then the mycelium is filtered and is subjected to hot air drying treatment by a hot air blower, and then the leaching work can be started;
s4, when the leaching process is finished, desugaring treatment can be started, the desugaring treatment is firstly carried out, the desugaring treatment is placed in an evaporation kettle and is recovered by methanol condensation, and then water with the mass of 5-6 times that of the desugaring treatment is added;
s5, adding desugarized bodies into an evaporation kettle with the mass of about 2 times of methanol and the evaporation temperature of 60-85 ℃ for concentration and evaporation during primary crystallization, recovering methanol, adding 3 times of methanol to complete primary crystallization, and performing secondary crystallization and tertiary crystallization;
s6, drying the mycelium after the three-time crystallization, and placing the mycelium in a drying box for drying;
s7, adding the dried mycelium into a pulverizer, and starting the pulverizer to pulverize, mix and process the mycelium;
and S8, finally, taking out the produced finished abamectin product, weighing according to a certain weight, and packaging by adopting a sealed container to finish the production and processing work.
In a further preferred embodiment of the present invention, in step S1, the culture temperature should be maintained at about 28 ℃. + -. 0.5 ℃ and the culture time should be 10 to 12 days.
As a further preferred embodiment of the present invention, in step S2, it is necessary to maintain the culture temperature at 28 ℃. + -. 0.5 ℃ for a culture time of 50h to 60 h.
As a further preferred mode of the present invention, in step S3, the temperature of drying is controlled to be 120 ℃ to 150 ℃ while the mycelium is leached with methanol of a mass of 100-200 times that of the mycelium, and the number of leaching is set to three.
In a further preferred embodiment of the present invention, the evaporation temperature is 80 ℃ or lower in step S4, and hot water at 80 ℃ is used for desugaring.
As a further preferable mode of the present invention, in step S5, when the secondary crystallization is started, methanol of 7 to 8 times of the crystals is added and decolorized with 3 to 4% of activated carbon, thereby completing the secondary crystallization, and finally, when the tertiary crystallization is started, methanol of 9 to 10 times of the crystals is added and decolorized with 3 to 4% of activated carbon, thereby completing the tertiary crystallization.
As a further preferable mode of the present invention, in step S6, the drying time is 30min while the temperature is set between 60 ℃ and 80 ℃.
In a more preferred embodiment of the present invention, in step S7, the pulverization time is 8min to 13min, and the rotation speed of the pulverizer is 120 r/min.
The invention adopts a mode of improving crystallization processing in the production process and a mode of three-time crystallization, which is different from the traditional abamectin processing technology, so that the purity of the mycelium can be greatly improved, and two processes of leaching and desugaring are additionally added in the two processes of fermentation and crystallization, so that the impurities of the mycelium can be reduced before the mycelium is crystallized, and the particle impurities and other components contained in the mycelium are removed, so that the mycelium after crystallization processing can be purer, the quality of the finished abamectin is improved, and the excellent effect during production is greatly improved.
Drawings
FIG. 1 is a flow chart of the production process of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a technical scheme that: the production process of abamectin includes the following steps:
s1, firstly, culturing the strain, putting the strain on a culture shelf for culture, and then after the culture is finished, producing an inclined plane on the surface of the strain so as to drip the strain suspension downwards and collecting the suspension;
s2, culturing the collected bacterial suspension, adding corresponding culture solution, and then placing in a fermentation tank for fermentation after the culture is completed, wherein the fermentation temperature is 28 +/-0.5 ℃ and the fermentation time is 210-320 h;
s3, when the fermentation is finished, mycelium can be extracted from the bacterial suspension, then the mycelium is filtered and is subjected to hot air drying treatment by a hot air blower, and then the leaching work can be started;
s4, when the leaching process is finished, desugaring treatment can be started, the desugaring treatment is firstly carried out by placing the desugaring treatment in an evaporation kettle, concentrating and recovering by adopting methanol condensation, and then water with the mass of 5-6 times of that of the desugaring treatment is added;
s5, adding desugarized bodies into an evaporation kettle with the mass of about 2 times of methanol and the evaporation temperature of 60-85 ℃ for concentration and evaporation during primary crystallization, recovering methanol, adding 3 times of methanol to complete primary crystallization, and performing secondary crystallization and tertiary crystallization;
s6, drying the mycelium after the three-time crystallization, and placing the mycelium in a drying box for drying;
s7, adding the dried mycelium into a pulverizer, and starting the pulverizer to pulverize, mix and process the mycelium;
and S8, finally, taking out the produced finished abamectin product, weighing according to a certain weight, and packaging by adopting a sealed container to finish the production and processing work.
In step S1, the culture temperature is maintained at 28 ℃. + -. 0.5 ℃ for 10-12 days.
In step S2, the culture temperature is maintained at 28 ℃. + -. 0.5 ℃ and the culture time is maintained at 50-60 h.
In step S3, the temperature of drying was controlled to be 120-150 ℃ while the mycelium was leached with methanol of 100-200 times the mass, and the number of leachings was set to three.
In step S4, the evaporation temperature is less than or equal to 80 ℃, and hot water with the temperature of 80 ℃ is needed for desugaring.
In step S5, adding methanol 7-8 times of the crystal when the secondary crystallization is started, decoloring by using 3-4% of activated carbon to finish the secondary crystallization, and finally adding methanol 9-10 of the crystal when the tertiary crystallization is started, decoloring by using 3-4% of activated carbon to finish the tertiary crystallization.
In step S6, the drying time is 30min, and the temperature is set between 60 ℃ and 80 ℃.
In step S7, the pulverizing time is 8min-13min, and the rotation speed of the pulverizer is 120 r/min.
In conclusion, the method is different from the traditional abamectin processing technology, the crystallization processing mode is improved in the production process, the mode of three-time crystallization is adopted, the purity of the mycelium can be greatly improved, two processes of leaching and desugaring are additionally added in the two processes of fermentation and crystallization, the impurities of the mycelium can be reduced before the mycelium is crystallized, and the particle impurities and other components contained in the mycelium are removed, so that the mycelium after the crystallization processing can be purer, the quality of the finished abamectin is improved, the excellent effect during production is greatly improved, the whole processing and production technology is more refined, the condition that more defective goods are easy to appear is avoided, and the production technology is more reasonable.
While there have been shown and described what are at present considered the fundamental principles and essential features of the invention and its advantages, it will be apparent to those skilled in the art that the invention is not limited to the details of the foregoing exemplary embodiments, but is capable of other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (8)
1. The production process of abamectin is characterized by comprising the following production steps:
s1, strain culture: firstly, culturing a strain, placing the strain on a culture shelf for culture, and then producing an inclined plane on the surface of the strain after the culture is finished so as to drip a strain suspension downwards and collect the strain suspension;
s2, fermentation: culturing the collected bacterial suspension, adding corresponding culture solution, and fermenting in a fermentation tank at 28 + -0.5 deg.C for 210-320 h;
s3, leaching processing: after fermentation is completed, mycelium can be extracted from the bacterial suspension, then the mycelium is filtered, hot air drying treatment is carried out by a hot air blower, and then leaching work can be carried out on the mycelium;
s4, desugaring: when the leaching processing is finished, the desugaring treatment can be started, firstly the desugaring treatment is carried out by putting the desugaring agent into an evaporation kettle for concentration, methanol condensation is adopted for recovery, and then water with the mass of 5-6 times that of the desugaring treatment is added;
s5, crystallization processing: adding desugarized body into an evaporation kettle with 2 times mass of methanol and the evaporation temperature of 60-85 ℃ for concentration and evaporation, recovering methanol, adding 3 times mass of methanol to complete primary crystallization, and performing secondary crystallization and tertiary crystallization;
s6, drying: drying the mycelium after the third crystallization, and putting the mycelium into a drying oven for drying;
s7, crushing and mixing: adding the dried mycelium into a pulverizer, and starting the pulverizer to pulverize, mix and process the mycelium;
s8, packaging of finished products: and finally, taking out the produced finished abamectin, weighing according to a certain weight, and packaging by adopting a sealed container to finish production and processing.
2. The process according to claim 1, wherein in step S1, the cultivation temperature is maintained at about 28 ℃ ± 0.5 ℃, and the cultivation time is 10-12 days.
3. The process according to claim 1, wherein in step S2, the cultivation temperature is maintained at 28 ℃ ± 0.5 ℃ and the cultivation time is 50-60 h.
4. The process according to claim 1, wherein in step S3, the drying temperature is controlled to 120-150 ℃, and the mycelium is leached with methanol of 100-200 times the mass of the mycelium, and the leaching amount is set to three times.
5. The process for producing abamectin according to claim 1, wherein in step S4, the evaporation temperature is not more than 80 ℃, and hot water with the temperature of 80 ℃ is required for desugaring.
6. The process for producing abamectin according to claim 1, wherein in step S5, methanol is added in an amount of 7-8 times the amount of crystals at the beginning of the second crystallization, and 3% -4% activated carbon is used for decoloring, thereby completing the second crystallization, and finally methanol is added in an amount of 9-10 times the amount of crystals at the beginning of the third crystallization, and 3% -4% activated carbon is used for decoloring, thereby completing the third crystallization.
7. The process according to claim 1, wherein in step S6, the drying time is 30min, and the temperature is set between 60 ℃ and 80 ℃.
8. The process for producing abamectin according to claim 1, wherein in step S7, the crushing time is 8min to 13min, and the rotation speed of the crusher is 120 r/min.
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Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1928075A (en) * | 2006-10-12 | 2007-03-14 | 吴学民 | Strain capable of generating avermectin B component and utilization thereof |
CN102060897A (en) * | 2011-01-07 | 2011-05-18 | 石家庄市兴柏生物工程有限公司 | Method for preparing abamectin |
CN103613624A (en) * | 2013-12-05 | 2014-03-05 | 宁夏启元药业有限公司 | Refining method of avermectin |
CN110964072A (en) * | 2019-11-21 | 2020-04-07 | 宁夏泰益欣生物科技有限公司 | Method for extracting abamectin |
CN112574261A (en) * | 2020-11-29 | 2021-03-30 | 宁夏泰益欣生物科技有限公司 | Crystallization method for improving solubility of abamectin |
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- 2021-07-20 CN CN202110820101.3A patent/CN113355382A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1928075A (en) * | 2006-10-12 | 2007-03-14 | 吴学民 | Strain capable of generating avermectin B component and utilization thereof |
CN102060897A (en) * | 2011-01-07 | 2011-05-18 | 石家庄市兴柏生物工程有限公司 | Method for preparing abamectin |
CN103613624A (en) * | 2013-12-05 | 2014-03-05 | 宁夏启元药业有限公司 | Refining method of avermectin |
CN110964072A (en) * | 2019-11-21 | 2020-04-07 | 宁夏泰益欣生物科技有限公司 | Method for extracting abamectin |
CN112574261A (en) * | 2020-11-29 | 2021-03-30 | 宁夏泰益欣生物科技有限公司 | Crystallization method for improving solubility of abamectin |
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