CN104920450B - A kind of doractin and organic phosphates complex microemulsion and preparation method thereof - Google Patents
A kind of doractin and organic phosphates complex microemulsion and preparation method thereof Download PDFInfo
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- CN104920450B CN104920450B CN201510306262.5A CN201510306262A CN104920450B CN 104920450 B CN104920450 B CN 104920450B CN 201510306262 A CN201510306262 A CN 201510306262A CN 104920450 B CN104920450 B CN 104920450B
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Abstract
The present invention relates to a kind of doractin and organic phosphates (triazophos, chlopyrifos, Profenofos, phoxim etc.) microemulsion and preparation method thereof, the invention is characterised by realizing by following step：Doractin and organic phosphates (triazophos, chlopyrifos, Profenofos, phoxim etc.) microemulsion, percentage by weight is：Doractin fine powder 0.3 8%；Organic phosphates (triazophos, chlopyrifos, Profenofos, phoxim etc.) 8 30%；Solvent 1% 20%；Cosolvent 1% 20%；Surfactant 5% 30%；Antifreezing agent 1% 3%；Remaining is water.Its preparation method is：Weigh by proportioning and mix, cosolvent, active compound, surfactant mix homogeneously in a kettle. finally adds water, and the liquid for being stirred for into homogeneous phase transparent obtains final product this product.This product has good stability, using safer, more convenient, drug effect is higher the features such as, have specially good effect to insect pest, mite class.
Description
【Technical field】The present invention relates to a kind of agricultural double-crossed Insecticidal and acaricidal agent, specifically a kind of doractin with
Organic phosphates (triazophos, chlopyrifos, Profenofos, phoxim etc.) complex microemulsion and preparation method thereof.
【Technical background】In the use of traditional pesticide, mainly cream and powder are not very in the past level of the productive forces
In the case of height, for preventing pest and disease damage from playing a significantly greater role, but due to cream be all active compound and emulsifying agent be dissolved in organic
Formed in solvent, very big burden is caused during use to environment.Powder is due in use, it is easy to float
Move, detrimental effect is brought to user and surrounding, develop a kind of novel form, show especially important.
Microemulsion save compared with cream a large amount of organic solvents, to human and environment safety (the solvent-free toxicity of itself)；
Flash-point is high, nonflammable, and storage, transportation safety, volatility is little, the stink that alleviates pesticide, cost are slightly less than cream preparation, content
Lower preparation, advantage are more obvious.
Doractin is a kind of new macrolides compound, nematicide, insecticide and demodicid mite is respectively provided with and is efficiently killed
Effect, similar with avilamycin action effect and insecticidal effect.And a kind of efficient, broad spectrum insecticide, there is stomach toxicity to demodicid mite
And action of contace poison, and have faint fumigation action, and without absorbability, but there are very strong osmosiss to blade, the longevity of residure is long, it is impossible to
Ovicidal.Mechanism of action is the release for stimulating neurotransmitter r- aminobutyric acids, disturbs normal nervous physiology activity.Due to having
Osmosiss, affected by rainwater little, to crop safety.Citrus red mite, rust mite, short hairs demodicid mite etc. can be prevented and treated.Organophosphorus insecticide
Strong to insect (evil mite) virulence, higher than organochlorine insecticides, higher than or equivalent to carbamate insecticidess, less than intending removing
Worm chrysanthemum ester insecticide, insecticidal spectrum are wide, and, with tagging and stomach poison function, temperature is higher, shows higher parasite killing for great majority
Effect, pest resistance development are relatively slow, and degradable, environmental pollution is little, in the plant body can metabolic degradation and detoxify, in plant
Body surface face through Exposure to Sunlight or can drench with rain and degrade, and therefore in agricultural product, residual quantity is relatively low, is easily hydrolyzed in water or in soil, right
Environmental pollution is little, in animal body easily metabolic degradation and excrete, to people without cumulative toxicity.Both match and there is strong killing
Worm, mite killing, ovicidal effect.
【Content of the invention】It is an object of the invention to provide a kind of doractin and organic phosphates (triazophos, chlopyrifos,
Profenofos, phoxim etc.) complex microemulsion and preparation method thereof.
It is (triazophos, chlopyrifos, Profenofos, pungent that another object of the present invention is to provide a kind of doractin and organic phosphates
Sulfur phosphorus etc.) compounding for active compound prepare efficiently, low toxicity, environment amenable environment-friendly pesticide, acaricide, can be used to preventing and treating Cotton Gossypii,
On the crops such as Citrus into demodicid mite, deutonymph and ovum and vegetable diamondback moth, Pieris rapae；On rice-stem borer, rice leaf roller, plant hopper
Insect.
The purpose of the present invention is achieved through the following technical solutions：
A kind of doractin and organic phosphates (triazophos, chlopyrifos, Profenofos, phoxim etc.) complex microemulsion, which is made
Preparation Method is comprised the steps of：
(1) by doractin, organic phosphates (triazophos, chlopyrifos, Profenofos, phoxim etc.) compounding active compound is dissolved in and helps
In solvent, stir to form the solution of transparence.
(2) surfactant is put in the solvent of the first step, fully dissolves, form homogeneous solution.
(3) aqueous solution is slowly added in the solution of second step and is stirred, form homogeneous solution.
(4) last addition antifreezing agent in the solution of the 3rd step, stirs into transparent homogeneous liquid.
1st, described doractin and organic phosphates (triazophos, chlopyrifos, Profenofos, phoxim etc.) complex microemulsion,
It is characterized in that described cosolvent is selected from：One kind in Ketohexamethylene, DMF, methanol, N-Methyl pyrrolidone, dimethylbenzene.
2nd, described doractin and organic phosphates (triazophos, chlopyrifos, Profenofos, phoxim etc.) complex microemulsion,
It is characterized in that described surfactant is selected from：Calcium dodecyl benzene sulfonate, alkyl phenol polyoxyethyl ether, benzylphenol polyoxy second
Base ether, benzyl dimethyl phenol polyoxyethyl ether, phenyl phenol polyoxyethyl ether, phenylpropyl phenethyl phenol polyoxyethyl ether, alkyl phenol
One kind or many in formaldehyde resin polyoxyethyl ether, phenethyl phenol polyoxyethyl propyl ether, APES formaldehyde condensation product
Kind.
3rd, described doractin and organic phosphates (triazophos, chlopyrifos, Profenofos, phoxim etc.) complex microemulsion,
It is characterized in that described antifreezing agent is selected from：One or more in ethylene glycol, Propylene Glycol, glycerol, Polyethylene Glycol.
Preferably, the doractin in complex microemulsion of the invention is that (which is complete for Chinese patent application 2015101288326
Text is included herein with reference to just looking like herein all to repeat record to go over) compositionss containing doractin recorded.Use
Said composition cost is not only low than pure doractin, and the pure doractin of effect essentially identical (or even can exceed that).Described
Compositionss containing doractin can be prepared via a method which：
(1) by streptomycete (preferably streptomycete D126 strains) be inoculated in seed culture medium (preferably described seed culture medium
Formula：Glucose 15g, sucrose 5g, Semen sojae atricolor powder 15g, yeast powder 5g, pH 7.0, are settled to 1L with distilled water) middle culture is (preferably
Cultivated with 30 DEG C), obtain actication of culture thing；
(2) actication of culture thing is inoculated in the amplification culture base (formula of preferably described amplification culture base；Glucose 10g, sugarcane
Sugared 10g, Semen sojae atricolor powder 15g, yeast powder 5g, pH 7.0, are settled to 1L with distilled water) middle culture (preferably being cultivated with 30 DEG C), must expand
Big culture；
(3) will be enlarged by culture and be inoculated in the fermentation medium (formula of preferably described fermentation medium：Semen Maydis powder 50g, greatly
Semen Glycines powder 50g, CaCO35g, NaCl 3g, K2HPO42g, MgSO41g, biotin 0.05g, pH 7.0, are settled to distilled water
In 1L), culture (preferably being cultivated with 28 DEG C), obtains fermentation culture medium；With,
(4) fermentation culture medium is filtered, retains thalline, add organic solvent (preferably alcohol, such as methanol or ethanol), after extraction
Filter, collect filtrate and add NaCl aqueous solutions (preferably saturation NaCl aqueous solution) dilution organic solvent (preferably to dilute organic molten
Agent concentration is to 15～35% (V/V)), filter after separating out precipitation, collect and precipitate and dry.
It is preferred that in the method, the volume of the volume ＜ fermentation medium of the volume ＜ amplification culture base of seed culture medium,
The volume ratio of preferred seed culture medium, amplification culture base and fermentation medium is 1: 15～25: 100～200；In step (4),
The ratio (g/mL) of the volume of the weight of thalline and organic solvent is 1: 2～8, preferably 1: 3～6；Compositionss containing doractin
The content of middle doractin is 75～85%, preferably 77～83%；And/or, the compositionss containing doractin also contain impurity A
And impurity B, the preferably content of impurity A is 6～9%, it is also preferred that the content of impurity B is 2～4%.Wherein, impurity A is the method
The composition corresponding to the peak at 17～18min on the HPLC collection of illustrative plates of the compositionss containing doractin for preparing；Impurity B is the party
The composition corresponding to the peak at 12.9～13.9min on the HPLC collection of illustrative plates of the compositionss containing doractin prepared by method.Such as nothing
Indicate on the contrary, HPLC conditions are：HPLC chromatographs column packing：Hypersil ODS2 5μm；Chromatography column size：4.6*250mm；Enter
Sample amount；20μl；Mobile phase (volume ratio)：Methanol: acetonitrile: water=67: 15: 18；Flow velocity：1.0ml/min；Detection wavelength：
245nm.
It is also preferred that the doractin in the complex microemulsion of the present invention is the compositionss containing doractin, described containing many
The compositionss of rhzomorph are drawn comprising doractin and comprising impurity A and/or impurity B.
The doractin of the formula processing of the present invention is multiple with organic phosphates (triazophos, chlopyrifos, Profenofos, phoxim etc.)
Compare with microemulsion prior art, in conventional cream dosage form, in 60-90%, and microemulsion is comprised only aromatic organic solvent content
1-20%, reduces environmental pollution.It is that 0.1-1.0 is micro- that conventional cream preparation is configured to obtain medicinal liquid thin pearl fineness when spraying Emulsion
Rice, and obtain the thin pearl fineness of medicinal liquid for 0.001-0.01 microns during the be configured to sprinkling Emulsion of microemulsion, improve prevention effect with
The utilization rate of medicament.There is heat to store up more stable, cold preservation without precipitate；The preparation of the present invention is to environment, people and animals and other beneficial lifes
Thing safety, is not likely to produce poisoning；Preparation preparing process is simpler, easy to use, the relatively low spread that is suitable for of cost should
With.
【Embodiment】In order to be better understood from the essence of the present invention, the technology contents of the present invention are demonstrated below.
Embodiment 1：Weigh 95% doractin active compound 0.32kg, 97% chlopyrifos active compound 20.6kg and be dissolved in 10kg hexamethylenes
It is evenly stirred until in ketone transparent；Take calcium dodecyl benzene sulfonate 4.0kg, alkyl phenol polyoxyethyl ether 4.0kg, benzylphenol polyoxy second
It is evenly stirred until in base ether 4.0kg, benzyl dimethyl phenol polyoxyethyl ether 4.0kg addition oil transparent；It is slow added into water
50.08kg, is sufficiently stirred for, and is eventually adding 3kg ethylene glycol and stirs to clarify transparent, 20.3% doractin chlopyrifos can be obtained micro-
Emulsion.
Embodiment 2：Weigh 95% doractin active compound 0.53kg, 92% Phoxim original medicine 21.7kg and be dissolved in 15kg hexamethylenes
It is evenly stirred until in ketone transparent；Take phenyl phenol polyoxyethyl ether 4.0kg, phenylpropyl phenethyl phenol polyoxyethyl ether 5.0kg, alkyl
It is transparent that fluosite polyoxyethyl ether 5.0kg, phenethyl phenol polyoxyethyl propyl ether 4.0kg add oil phase to be evenly stirred until；Delay again
Slow add water 41.77kg, be sufficiently stirred for, be eventually adding 3kg ethylene glycol and stir to clarify transparent, 20.5% doractin can be obtained
Phoxim microemulsion.
Embodiment 3：Weigh 95% doractin active compound 1.06kg, 90% triazophos active compound 22.2kg and be dissolved in 20kg hexamethylenes
It is evenly stirred until in ketone transparent；Take alkyl point polyoxyethylene ether formaldehyde condensation products 5.0kg, alkylphenol-formaldehyde resin polyoxyethyl ether
6.0kg, phenethyl phenol polyoxyethyl propyl ether 4.0kg, phenylpropyl ethyl phenol polyoxyethyl ether 5.0kg are added and are evenly stirred until in oil phase
Transparent；It is slow added into water 33.74kg, is sufficiently stirred for, is eventually adding 3kg ethylene glycol and stirs to clarify transparent, 21% can be obtained
Doractin triazophos micro-emulsion.
Claims (10)
1. a kind of doractin and organic phosphates active compound complex microemulsion, which is prepared by method preparation：
(1) compositionss containing doractin, organic phosphates active compound are dissolved in cosolvent, stir to form the molten of transparence
Liquid；
(2) surfactant is put in the solvent of the first step, fully dissolves, form homogeneous solution；
(3) water is slowly added in the solution of second step and is stirred, form homogeneous solution；
(4) last addition antifreezing agent in the solution of the 3rd step, stirs into transparent homogeneous liquid,
Characterized in that, the compositionss containing doractin are prepared via a method which：
(1) streptomycete D126 strains are inoculated in seed culture medium and are cultivated with 30 DEG C, obtain actication of culture thing, the seed culture
The formula of base：Glucose 15g, sucrose 5g, Semen sojae atricolor powder 15g, yeast powder 5g, pH 7.0, are settled to 1L with distilled water；
(2) actication of culture thing is inoculated in amplification culture base and is cultivated with 30 DEG C, obtain amplification culture thing, the amplification culture base
Formula：Glucose 10g, sucrose 10g, Semen sojae atricolor powder 15g, yeast powder 5g, pH 7.0, are settled to 1L with distilled water；
(3) will be enlarged by culture to be inoculated in fermentation medium with 28 DEG C of cultures, obtain fermentation culture medium, the fermentation medium
Formula：Semen Maydis powder 50g, Semen sojae atricolor powder 50g, CaCO35g, NaCl 3g, K2HPO42g, MgSO41g, biotin 0.05g, pH
7.0,1L is settled to distilled water；With,
(4) fermentation culture medium is filtered, retains thalline, add methanol or ethanol, filtered after extraction, collected filtrate and add saturation
NaCl aqueous solutions dilution methanol or concentration of alcohol are filtered after separating out precipitation to 15～35%V/V, are collected and are precipitated and dry.
2. microemulsion according to claim 1, it is characterised in that the organic phosphates active compound be triazophos, chlopyrifos, third
Bromine phosphorus or phoxim.
3. microemulsion according to claim 1, it is characterised in that the cosolvent is selected from Ketohexamethylene, DMF, methanol, N- first
One kind in base ketopyrrolidine, dimethylbenzene.
4. microemulsion according to claim 1, it is characterised in that the surfactant is selected from DBSA
Calcium, alkyl phenol polyoxyethyl ether, benzylphenol polyoxyethyl ether, benzyl dimethyl phenol polyoxyethyl ether, phenyl phenol polyoxyethyl ether,
Phenylpropyl phenethyl phenol polyoxyethyl ether, alkylphenol-formaldehyde resin polyoxyethyl ether, phenethyl phenol polyoxyethyl propyl ether, alkyl phenol gather
One or more in oxygen vinyl Ether formaldehyde condensation products.
5. microemulsion according to claim 1, it is characterised in that the antifreezing agent selected from ethylene glycol, Propylene Glycol, the third three
One or more in alcohol, Polyethylene Glycol.
6. the preparation method of a kind of doractin and organic phosphates active compound complex microemulsion, which comprises the steps of：
(1) compositionss containing doractin, organic phosphates active compound are dissolved in cosolvent, stir to form the molten of transparence
Liquid；
(2) surfactant is put in the solvent of the first step, fully dissolves, form homogeneous solution；
(3) water is slowly added in the solution of second step and is stirred, form homogeneous solution；
(4) last addition antifreezing agent in the solution of the 3rd step, stirs into transparent homogeneous liquid,
Characterized in that, the compositionss containing doractin are prepared via a method which：
(1) streptomycete D126 strains are inoculated in seed culture medium and are cultivated with 30 DEG C, obtain actication of culture thing, the seed culture
The formula of base：Glucose 15g, sucrose 5g, Semen sojae atricolor powder 15g, yeast powder 5g, pH 7.0, are settled to 1L with distilled water；
(2) actication of culture thing is inoculated in amplification culture base and is cultivated with 30 DEG C, obtain amplification culture thing, the amplification culture base
Formula：Glucose 10g, sucrose 10g, Semen sojae atricolor powder 15g, yeast powder 5g, pH 7.0, are settled to 1L with distilled water；
(3) will be enlarged by culture to be inoculated in fermentation medium with 28 DEG C of cultures, obtain fermentation culture medium, the fermentation medium
Formula：Semen Maydis powder 50g, Semen sojae atricolor powder 50g, CaCO35g, NaCl 3g, K2HPO42g, MgSO41g, biotin 0.05g, pH
7.0,1L is settled to distilled water；With,
(4) fermentation culture medium is filtered, retains thalline, add methanol or ethanol, filtered after extraction, collected filtrate and add saturation
NaCl aqueous solutions dilution methanol or concentration of alcohol are filtered after separating out precipitation to 15～35%V/V, are collected and are precipitated and dry.
7. preparation method according to claim 6, it is characterised in that the organic phosphates active compound be triazophos, chlopyrifos,
Profenofos or phoxim.
8. preparation method according to claim 6, it is characterised in that the cosolvent is selected from Ketohexamethylene, DMF, methanol, N-
One kind in methyl pyrrolidone, dimethylbenzene.
9. preparation method according to claim 6, it is characterised in that the surfactant is selected from DBSA
Calcium, alkyl phenol polyoxyethyl ether, benzylphenol polyoxyethyl ether, benzyl dimethyl phenol polyoxyethyl ether, phenyl phenol polyoxyethyl ether,
Phenylpropyl phenethyl phenol polyoxyethyl ether, alkylphenol-formaldehyde resin polyoxyethyl ether, phenethyl phenol polyoxyethyl propyl ether, alkyl phenol gather
One or more in oxygen vinyl Ether formaldehyde condensation products.
10. preparation method according to claim 6, it is characterised in that the antifreezing agent selected from ethylene glycol, Propylene Glycol, third
One or more in triol, Polyethylene Glycol.
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| CN102885035A (en) * | 2012-09-28 | 2013-01-23 | 王龙华 | Microemulsion pesticide and production process thereof |
| CN104418927A (en) * | 2013-08-29 | 2015-03-18 | 重庆乾泰生物医药有限公司 | Separation and purification method of doramectin |
| CN104561180A (en) * | 2014-12-26 | 2015-04-29 | 宁夏泰瑞制药股份有限公司 | Culture mediums for producing doramectin through fermentation of mutant streptomyces avermitilis and material supplement method |
-
2015
- 2015-06-08 CN CN201510306262.5A patent/CN104920450B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1504095A (en) * | 2002-11-30 | 2004-06-16 | 吴学民 | Chlorpyrifos, methylamino abamectin microemulsion |
| CN1440655A (en) * | 2003-01-21 | 2003-09-10 | 江苏粮满仓农化有限公司 | Triazophos-avermectin microemulsion and its preparation method |
| CN1947506A (en) * | 2006-05-19 | 2007-04-18 | 东北农业大学 | Method for preparing microemulsion, aqueous emulsion and suspending agent contg. Dola-mycetin and Sala-mycetin |
| CN101705194A (en) * | 2009-08-24 | 2010-05-12 | 东北农业大学 | Streptomyces bacterial strain |
| CN102885035A (en) * | 2012-09-28 | 2013-01-23 | 王龙华 | Microemulsion pesticide and production process thereof |
| CN104418927A (en) * | 2013-08-29 | 2015-03-18 | 重庆乾泰生物医药有限公司 | Separation and purification method of doramectin |
| CN104561180A (en) * | 2014-12-26 | 2015-04-29 | 宁夏泰瑞制药股份有限公司 | Culture mediums for producing doramectin through fermentation of mutant streptomyces avermitilis and material supplement method |
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