CN110105415A - A kind of method that avermectin B2a fine powder and ointment can be prepared simultaneously - Google Patents
A kind of method that avermectin B2a fine powder and ointment can be prepared simultaneously Download PDFInfo
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- CN110105415A CN110105415A CN201910301062.9A CN201910301062A CN110105415A CN 110105415 A CN110105415 A CN 110105415A CN 201910301062 A CN201910301062 A CN 201910301062A CN 110105415 A CN110105415 A CN 110105415A
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- avermectin
- ointment
- fine powder
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/02—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
- A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/12—Powders or granules
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/90—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
-
- 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
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- 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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- General Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
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- Environmental Sciences (AREA)
- Dentistry (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Plant Pathology (AREA)
- Agronomy & Crop Science (AREA)
- Pest Control & Pesticides (AREA)
- Biochemistry (AREA)
- Biotechnology (AREA)
- Genetics & Genomics (AREA)
- Molecular Biology (AREA)
- Toxicology (AREA)
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- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Saccharide Compounds (AREA)
Abstract
The invention discloses the method that avermectin B2a fine powder and ointment can be prepared simultaneously in one kind, including Avermectin B1a crystalline mother solution concentration desolventizing, washing, decrease temperature crystalline, be centrifuged, obtain avermectin B2a fine powder, desolventizing is evaporated under reduced pressure in recrystallization mother liquor and methanol is added adjusts to obtain B2a ointment；The present invention screens solvent and optimized production process extracts B2a component fine powder and obtains B2a ointment by the research to B2a component；Since B2a component is to be extracted in by-product to extract again by B1a, method of the invention can expand avermectin industrial chain.
Description
Technical field
The present invention relates to preparation technique of pesticide field, in particular to avermectin B2a essence can be prepared in one kind simultaneously
The method of powder and ointment.
Background technique
Avermectin, English name Avermectins are by big village's intelligence of Japanese North university etc. and U.S. Merck company
The one kind developed first has ten hexa-atomic Macrocyclic lactone compounds of desinsection, mite killing, eelworm-killing activity, by grey chain in streptomycete
Mould Streptomyces avermitilis fermentation generates.It is made of 8 kinds of homologues, B1 and B2 are ratios in reorganization homologue
Higher two kinds.The B1 fine powder and B1 ointment desinsection wide spectrum of traditional mode of production, but B2 component has special the killing property to nematode, has
The drug effect that B1a does not have.
Summary of the invention
The technical problem to be solved in the present invention is to provide one kind, and avermectin B2a fine powder and ointment can be prepared simultaneously
Method.
In order to solve the above-mentioned technical problem, the technical solution of the present invention is as follows:
A kind of method that avermectin B2a fine powder and ointment can be prepared simultaneously, includes the following steps:
(a) desolventizing is concentrated in Avermectin B1a crystalline mother solution: desolventizing is evaporated under reduced pressure in Avermectin B1a crystalline mother solution
Concentrate is obtained, the first solvent of addition is warming up to 80-85 DEG C of stirring 30-45min and sufficiently dissolves in Xiang Suoshu concentrate, is extracted
Take liquid；
(b) it washes: the 80-85 DEG C of hot water stirs 30-35min of the extract liquor volume 25-30% is added, stand 1-2h,
Remove water phase and newborn phase, the extract liquor after being washed；
(c) extract liquor after the washing crystal precipitation has been cooled to decrease temperature crystalline, centrifugation: using recirculated water water-bath；
Using the closed centrifugation of centrifuge, coarse-grain of avermectin B2a is obtained；
(d) it obtains avermectin B2a fine powder: coarse-grain of the avermectin B2a being recrystallized: Xiang Suoshu avermectin
The second solvent is added in coarse-grain of B2a and 2-3% active carbon is warming up to 80-85 DEG C of stirring 30-45min, undercurrent filtering, to filter
Liquid carries out decrease temperature crystalline, obtains avermectin B2a fine powder after centrifugation, drying；
(e) desolventizing is evaporated under reduced pressure in recrystallization mother liquor: the mother of generation will be centrifuged in the avermectin B2a recrystallization process
Desolventizing is evaporated under reduced pressure to solvent-free abjection in liquid；
(f) methanol is added to adjust to obtain B2a ointment: adjusts B2a content with methanol, obtain avermectin B2a ointment, guarantees
B2a content is greater than 10% in ointment.
Preferably, the first solvent in the step (a) is toluene.
Preferably, the additional amount of the first solvent in the step (a) and the volume ratio of the concentrate are 2.5-3.0:
1。
Preferably, the extract liquor in the step (c) after washing is cooled to 0-5 DEG C using recirculated water water-bath, maintains 2-4h.
Preferably, the weight ratio of coarse-grain of the second solvent in the step (d) and avermectin B2a is 5-6:1.
Preferably, the decrease temperature crystalline temperature in the step (d) are as follows: 0-5 DEG C, maintain 2-4h.
Preferably, the drying temperature in the step (d) are as follows: room temperature dries 60-90min, 90-100 DEG C of drying 90-
120min。
Preferably, the second solvent in the step (d) is benzene.
Preferably, the evaporating temperature in the step (e) is 90-100 DEG C.
By adopting the above technical scheme, the present invention screens solvent and optimized production process extracts by the research to B2a component
B2a component fine powder simultaneously obtains B2a ointment；Since B2a component is to be extracted in by-product to extract again by B1a, method of the invention can
Expand avermectin industrial chain.
Detailed description of the invention
Fig. 1 is flow chart of the invention.
Specific embodiment
Specific embodiments of the present invention will be further explained with reference to the accompanying drawing.It should be noted that for
The explanation of these embodiments is used to help understand the present invention, but and does not constitute a limitation of the invention.In addition, disclosed below
The each embodiment of the present invention involved in technical characteristic can be combined with each other as long as they do not conflict with each other.
Embodiment 1
As shown in Figure 1, a kind of method that avermectin B2a fine powder and ointment can be prepared simultaneously, including walk as follows
It is rapid:
(a) desolventizing is concentrated in Avermectin B1a crystalline mother solution: desolventizing is evaporated under reduced pressure in Avermectin B1a crystalline mother solution
Concentrate is obtained, addition toluene is warming up to 83 DEG C of stirring 35min and sufficiently dissolves in Xiang Suoshu concentrate, obtains extract liquor, wherein
The toluene additional amount and the volume ratio of the concentrate are 2.8:1；
(b) wash: being added 83 DEG C of hot water stirs 33min of the extract liquor volume 28%, stand 1.5h, remove water phase and
Newborn phase, the extract liquor after being washed；
(c) decrease temperature crystalline, centrifugation: the extract liquor after the washing is cooled to 3 DEG C using recirculated water water-bath, maintains 3h；
Using the closed centrifugation of centrifuge, coarse-grain of avermectin B2a is obtained；
(d) it obtains avermectin B2a fine powder: coarse-grain of the avermectin B2a being recrystallized: Xiang Suoshu avermectin
Benzene is added in coarse-grain of B2a and 2.5% active carbon is warming up to 83 DEG C of stirring 38min, wherein the benzene and avermectin B2a
The weight ratio of coarse-grain is 5.5:1, and undercurrent filtering carries out decrease temperature crystalline to filtrate, wherein the decrease temperature crystalline temperature are as follows: 3
DEG C, 3h is maintained, obtains avermectin B2a fine powder, the drying temperature after centrifugation, drying are as follows: room temperature dries 75min, 95 DEG C of bakings
Dry 105min；
(e) desolventizing is evaporated under reduced pressure in recrystallization mother liquor: the mother of generation will be centrifuged in the avermectin B2a recrystallization process
Desolventizing is evaporated under reduced pressure to solvent-free abjection in liquid, wherein the evaporating temperature is 95 DEG C；
(f) methanol is added to adjust to obtain B2a ointment: adjusts B2a content with methanol, obtain avermectin B2a ointment, guarantees
B2a content is greater than 10% in ointment.
Embodiment 2
As shown in Figure 1, a kind of method that avermectin B2a fine powder and ointment can be prepared simultaneously, including walk as follows
It is rapid:
(a) desolventizing is concentrated in Avermectin B1a crystalline mother solution: desolventizing is evaporated under reduced pressure in Avermectin B1a crystalline mother solution
Concentrate is obtained, addition toluene is warming up to 80 DEG C of stirring 30min and sufficiently dissolves in Xiang Suoshu concentrate, obtains extract liquor, wherein
The toluene additional amount and the volume ratio of the concentrate are 2.5:1；
(b) it washes: 80 DEG C of hot water stirs 30min of the extract liquor volume 25% is added, stand 1h, remove water phase and cream
Phase, the extract liquor after being washed；
(c) decrease temperature crystalline, centrifugation: the extract liquor after the washing is cooled to 0 DEG C using recirculated water water-bath, maintains 2h；
Using the closed centrifugation of centrifuge, coarse-grain of avermectin B2a is obtained；
(d) it obtains avermectin B2a fine powder: coarse-grain of the avermectin B2a being recrystallized: Xiang Suoshu avermectin
Benzene is added in coarse-grain of B2a and 2% active carbon is warming up to 80 DEG C of stirring 30min, wherein the benzene and avermectin B2a one
The weight ratio of secondary coarse-grain is 5:1, and undercurrent filtering carries out decrease temperature crystalline to filtrate, wherein the decrease temperature crystalline temperature are as follows: 0 DEG C,
2h is maintained, obtains avermectin B2a fine powder, the drying temperature after centrifugation, drying are as follows: room temperature dries 60min, 90 DEG C of drying
90min；
(e) desolventizing is evaporated under reduced pressure in recrystallization mother liquor: the mother of generation will be centrifuged in the avermectin B2a recrystallization process
Desolventizing is evaporated under reduced pressure to solvent-free abjection in liquid, wherein the evaporating temperature is 90 DEG C；
(f) methanol is added to adjust to obtain B2a ointment: adjusts B2a content with methanol, obtain avermectin B2a ointment, guarantees
B2a content is greater than 10% in ointment.
Embodiment 3
As shown in Figure 1, a kind of method that avermectin B2a fine powder and ointment can be prepared simultaneously, including walk as follows
It is rapid:
(a) desolventizing is concentrated in Avermectin B1a crystalline mother solution: desolventizing is evaporated under reduced pressure in Avermectin B1a crystalline mother solution
Concentrate is obtained, addition toluene is warming up to 85 DEG C of stirring 45min and sufficiently dissolves in Xiang Suoshu concentrate, obtains extract liquor, wherein
The toluene additional amount and the volume ratio of the concentrate are 3.0:1；
(b) it washes: 85 DEG C of hot water stirs 35min of the extract liquor volume 30% is added, stand 2h, remove water phase and cream
Phase, the extract liquor after being washed；
(c) decrease temperature crystalline, centrifugation: the extract liquor after the washing is cooled to 5 DEG C using recirculated water water-bath, maintains 4h；
Using the closed centrifugation of centrifuge, coarse-grain of avermectin B2a is obtained；
(d) it obtains avermectin B2a fine powder: coarse-grain of the avermectin B2a being recrystallized: Xiang Suoshu avermectin
Benzene is added in coarse-grain of B2a and 3% active carbon is warming up to 85 DEG C of stirring 45min, wherein the benzene and avermectin B2a one
The weight ratio of secondary coarse-grain is 6:1, and undercurrent filtering carries out decrease temperature crystalline to filtrate, wherein the decrease temperature crystalline temperature are as follows: 5 DEG C,
4h is maintained, obtains avermectin B2a fine powder, the drying temperature after centrifugation, drying are as follows: room temperature dries 90min, 100 DEG C of drying
120min；
(e) desolventizing is evaporated under reduced pressure in recrystallization mother liquor: the mother of generation will be centrifuged in the avermectin B2a recrystallization process
Desolventizing is evaporated under reduced pressure to solvent-free abjection in liquid, wherein the evaporating temperature is 100 DEG C；
(f) methanol is added to adjust to obtain B2a ointment: adjusts B2a content with methanol, obtain avermectin B2a ointment, guarantees
B2a content is greater than 10% in ointment.
The present invention screens solvent and optimized production process extracts B2a component fine powder and obtains by the research to B2a component
B2a ointment；Since B2a component is to be extracted in by-product to extract again by B1a, method of the invention can expand avermectin industry
Chain.
In conjunction with attached drawing, the embodiments of the present invention are described in detail above, but the present invention is not limited to described implementations
Mode.For a person skilled in the art, in the case where not departing from the principle of the invention and spirit, to these embodiments
A variety of change, modification, replacement and modification are carried out, are still fallen in protection scope of the present invention.
Claims (9)
1. the method that avermectin B2a fine powder and ointment can be prepared simultaneously in one kind, it is characterised in that: including walking as follows
It is rapid:
(a) desolventizing is concentrated in Avermectin B1a crystalline mother solution: Avermectin B1a crystalline mother solution reduction vaporization desolventizing is obtained
Concentrate, Xiang Suoshu concentrate the first solvent of interior addition are warming up to 80-85 DEG C of stirring 30-45min and sufficiently dissolve, extracted
Liquid；
(b) it washes: the 80-85 DEG C of hot water stirs 30-35min of the extract liquor volume 25-30% is added, stand 1-2h, removal
Water phase and newborn phase, the extract liquor after being washed；
(c) extract liquor after the washing crystal precipitation has been cooled to decrease temperature crystalline, centrifugation: using recirculated water water-bath；It uses
The closed centrifugation of centrifuge obtains coarse-grain of avermectin B2a；
(d) it obtains avermectin B2a fine powder: coarse-grain of the avermectin B2a being recrystallized: Xiang Suoshu avermectin B2a
The second solvent is added in coarse-grain and 2-3% active carbon is warming up to 80-85 DEG C of stirring 30-45min, undercurrent filtering, to filtrate
Decrease temperature crystalline is carried out, obtains avermectin B2a fine powder after centrifugation, drying；
(e) desolventizing is evaporated under reduced pressure in recrystallization mother liquor: the mother liquor that generation is centrifuged in the avermectin B2a recrystallization process is subtracted
Pressure evaporates desolventizing to solvent-free abjection；
(f) methanol is added to adjust to obtain B2a ointment: adjusts B2a content with methanol, obtain avermectin B2a ointment, guarantees ointment
Middle B2a content is greater than 10%.
2. the method according to claim 1 that avermectin B2a fine powder and ointment can be prepared simultaneously, feature exist
In: the first solvent in the step (a) is toluene.
3. the method according to claim 1 that avermectin B2a fine powder and ointment can be prepared simultaneously, feature exist
In the additional amount of: the first solvent in the step (a) and the volume ratio of the concentrate be 2.5-3.0:1.
4. the method according to claim 1 that avermectin B2a fine powder and ointment can be prepared simultaneously, feature exist
In: the extract liquor in the step (c) after washing is cooled to 0-5 DEG C using recirculated water water-bath, maintains 2-4h.
5. the method according to claim 1 that avermectin B2a fine powder and ointment can be prepared simultaneously, feature exist
In: the weight ratio of the coarse-grain of the second solvent and avermectin B2a in the step (d) is 5-6:1.
6. the method according to claim 1 that avermectin B2a fine powder and ointment can be prepared simultaneously, feature exist
In: the decrease temperature crystalline temperature in the step (d) are as follows: 0-5 DEG C, maintain 2-4h.
7. the method according to claim 1 that avermectin B2a fine powder and ointment can be prepared simultaneously, feature exist
In: the drying temperature in the step (d) are as follows: room temperature dries 60-90min, 90-100 DEG C of drying 90-120min.
8. the method according to claim 1 that avermectin B2a fine powder and ointment can be prepared simultaneously, feature exist
In: the second solvent in the step (d) is benzene.
9. the method according to claim 1 that avermectin B2a fine powder and ointment can be prepared simultaneously, feature exist
In: the evaporating temperature in the step (e) is 90-100 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910301062.9A CN110105415A (en) | 2019-04-15 | 2019-04-15 | A kind of method that avermectin B2a fine powder and ointment can be prepared simultaneously |
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| CN201910301062.9A CN110105415A (en) | 2019-04-15 | 2019-04-15 | A kind of method that avermectin B2a fine powder and ointment can be prepared simultaneously |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111606960A (en) * | 2020-05-15 | 2020-09-01 | 河北威远生物化工有限公司 | Avermectin B2a solvated crystal |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102977168A (en) * | 2012-12-17 | 2013-03-20 | 石家庄市兴柏生物工程有限公司 | Extraction and preparation method of abamectin B2a |
| CN103333214A (en) * | 2013-07-03 | 2013-10-02 | 大庆志飞生物化工有限公司 | Preparation method of Avermectin B2a fine powder |
| CN104650167A (en) * | 2015-03-10 | 2015-05-27 | 齐鲁制药（内蒙古）有限公司 | Preparation method of high-purity abamectin B2a |
| CN105418707A (en) * | 2015-11-13 | 2016-03-23 | 石家庄市兴柏生物工程有限公司 | Method for extracting abamectin B2 from abamectin ointment |
| CN106977566A (en) * | 2017-04-20 | 2017-07-25 | 河北科技大学 | A kind of method that Avermectin B2 is extracted from abamectin ointment |
| CN107787963A (en) * | 2017-07-03 | 2018-03-13 | 齐鲁制药（内蒙古）有限公司 | A kind of preparation method of anti-caking AVM toluene ointment |
-
2019
- 2019-04-15 CN CN201910301062.9A patent/CN110105415A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102977168A (en) * | 2012-12-17 | 2013-03-20 | 石家庄市兴柏生物工程有限公司 | Extraction and preparation method of abamectin B2a |
| CN103333214A (en) * | 2013-07-03 | 2013-10-02 | 大庆志飞生物化工有限公司 | Preparation method of Avermectin B2a fine powder |
| CN104650167A (en) * | 2015-03-10 | 2015-05-27 | 齐鲁制药（内蒙古）有限公司 | Preparation method of high-purity abamectin B2a |
| CN105418707A (en) * | 2015-11-13 | 2016-03-23 | 石家庄市兴柏生物工程有限公司 | Method for extracting abamectin B2 from abamectin ointment |
| CN106977566A (en) * | 2017-04-20 | 2017-07-25 | 河北科技大学 | A kind of method that Avermectin B2 is extracted from abamectin ointment |
| CN107787963A (en) * | 2017-07-03 | 2018-03-13 | 齐鲁制药（内蒙古）有限公司 | A kind of preparation method of anti-caking AVM toluene ointment |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111606960A (en) * | 2020-05-15 | 2020-09-01 | 河北威远生物化工有限公司 | Avermectin B2a solvated crystal |
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