CN104920450A - Doramectin and organophosphate compound microemulsion and preparation method thereof - Google Patents
Doramectin and organophosphate compound microemulsion and preparation method thereof Download PDFInfo
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- CN104920450A CN104920450A CN201510306262.5A CN201510306262A CN104920450A CN 104920450 A CN104920450 A CN 104920450A CN 201510306262 A CN201510306262 A CN 201510306262A CN 104920450 A CN104920450 A CN 104920450A
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- doractin
- microemulsion
- profenofos
- hostathion
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Abstract
The invention relates to a doramectin and organophosphate (triazophos, chlorpyrifos, profenofos, phoxim and the like) microemulsion and a preparation method thereof. The microemulsion is characterized by comprising the following raw materials by weight: 0.3 to 8 percent of doramectin fine powder, 8 to 30 percent of organophosphates (triazophos, chlorpyrifos, profenofos, phoxim and the like), 1 to 20 percent of a solvent, 1 to 20 percent of a cosolvent, 5 to 30 percent of a surfactant, 1 to 3 percent of an anti-freezing agents, and the balance of water. The preparation method comprises the following steps: taking the cosolvent, the raw pesticides and the surfactant according to the proportion; mixing the materials in a reaction still to obtain a uniform mixture; adding water; stirring till a homogeneous transparent liquid, namely the microemulsion, is obtained. The microemulsion is high in stability, safer and more convenient to use, higher in pesticide effect, and specially in controlling effect of pests and mites.
Description
[technical field] the present invention relates to a kind of agricultural double-crossed Insecticidal and acaricidal agent, specifically a kind of doractin and organic phosphates (Hostathion, chlopyrifos, Profenofos, phoxim etc.) complex microemulsion and preparation method thereof.
[technical background] is in the use of traditional agricultural chemicals, mainly missible oil and pulvis, when the level of the productive forces is not very high in the past, play a significantly greater role for preventing damage by disease and insect, but because missible oil is all that former medicine and emulsifiers dissolve are formed in organic solvent, in the process used, very large burden is caused to environment.Pulvis, due in use, is easy to drift, brings adverse influence, develop a kind of novel form to user and surrounding environment, outstanding aobvious important.
Microemulsion is compared with missible oil and is saved a large amount of organic solvent, to human and environment safety (solvent-free toxicity own); Flash-point is high, nonflammable, storage, transportation safety, volatility be little, the stink that alleviates agricultural chemicals, cost slightly lower than cream preparation, the preparation that content is lower, advantage is more obvious.
Doractin is a kind of novel macrolides compound, all has kill effect efficiently to nematode, insect and mite, with Avermectin action effect and insecticidal effect similar.Also be a kind of efficient, broad spectrum insecticide, have stomach toxicity and action of contace poison to mite, and have faint fumigation action, without interior absorption, but have very strong osmosis to blade, the longevity of residure is long, can not ovicidal.Mechanism of action is the release of Transfer Medium r-aminobutyric acid of exciting nerve, and disturbs normal neurophysiology movable.Owing to there being osmosis, affect little by rainwater, to crop safety.Citrus red mite, rust mite, short hairs mite etc. can be prevented and treated.Organophosphorus insecticide is strong to insect (evil mite) virulence, higher than organochlorine insecticides, higher than or be equivalent to carbamate insecticide, lower than pyrethroid insecticides, insecticidal spectrum is wide, great majority are with tagging and stomach poison function, temperature is higher, show higher insecticidal power, pest resistance development is slower, easy degraded, environmental pollution is little, can metabolic degradation and detoxifying in plant corpus, can or drench with rain through Exposure to Sunlight and degrade on plant corpus surface, therefore in agricultural product, residual quantity is lower, easily be hydrolyzed in water or in soil, environmental pollution is little, easy metabolic degradation and excreting in animal body, to people without cumulative toxicity.Both match and have strong desinsection, kill mite, ovicidal effect.
[summary of the invention] the object of the present invention is to provide a kind of doractin and organic phosphates (Hostathion, chlopyrifos, Profenofos, phoxim etc.) complex microemulsion and preparation method thereof.
Another object of the present invention is to provide a kind of doractin and organic phosphates (Hostathion, chlopyrifos, Profenofos, phoxim etc.) is compositely prepared efficiently for former medicine, low toxicity, environment amenable environment-friendly pesticide, miticide, prevents and treats one-tenth mite mite on the crop such as cotton, oranges and tangerines and ovum and vegetables diamond-back moth, cabbage caterpillar if can be used for; Insect on rice-stem borer, rice leaf roller, plant hopper.
Object of the present invention is achieved through the following technical solutions:
A kind of doractin and organic phosphates (Hostathion, chlopyrifos, Profenofos, phoxim etc.) complex microemulsion, its preparation method comprises following steps:
(1) by doractin, organic phosphates (Hostathion, chlopyrifos, Profenofos, phoxim etc.) composite former medicine is dissolved in cosolvent, stirs and forms the solution of transparence.
(2) surfactant is put in the solvent of the first step, fully dissolve, form homogeneous solution.
(3) aqueous solution to be added slowly in the solution of second step and to stir, forming homogeneous solution.
(4) finally in the solution of the 3rd step, add antifreezing agent, stir into transparent homogeneous liquid.
1, described doractin and organic phosphates (Hostathion, chlopyrifos, Profenofos, phoxim etc.) complex microemulsion, is characterized in that described cosolvent is selected from: the one in cyclohexanone, DMF, methyl alcohol, 1-METHYLPYRROLIDONE, dimethylbenzene.
2, described doractin and organic phosphates (Hostathion, chlopyrifos, Profenofos, phoxim etc.) complex microemulsion, is characterized in that described surfactant is selected from: one or more in calcium dodecyl benzene sulfonate, 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, alkylphenol polyoxyethylene formaldehyde condensation products.
3, described doractin and organic phosphates (Hostathion, chlopyrifos, Profenofos, phoxim etc.) complex microemulsion, is characterized in that described antifreezing agent is selected from: one or more in ethylene glycol, propane diols, glycerine, polyethylene glycol.
Preferably, the doractin in complex microemulsion of the present invention is the composition containing doractin that Chinese patent application 2015101288326 (it includes reference herein in full, just looks like all repeat record in this article to go over) is recorded.Use the doractin of said composition cost not only than pure low, and the doractin that effect substantially identical (even can exceed) is pure.The described composition containing doractin can be prepared by the following method:
(1) streptomycete (preferably streptomycete D126 strain) is inoculated in the seed culture medium (formula of preferred described seed culture medium: glucose 15g, sucrose 5g, soybean meal 15g, dusty yeast 5g, pH 7.0,1L is settled to distilled water) middle cultivation (preferably with 30 DEG C of cultivations), obtain actication of culture thing;
(2) actication of culture thing is inoculated in the expansion medium (formula of preferred described expansion medium; Glucose 10g, sucrose 10g, soybean meal 15g, dusty yeast 5g, pH 7.0, is settled to 1L with distilled water) middle cultivation (preferably with 30 DEG C of cultivations), obtain expansion culture;
(3) expansion culture is inoculated in fermentation medium (formula of preferred described fermentation medium: corn flour 50g, soybean meal 50g, CaCO
35g, NaCl 3g, K
2hPO
42g, MgSO
41g, vitamin h 0.05g, pH 7.0, is settled to 1L with distilled water) middle cultivation (preferably with 28 DEG C of cultivations), obtain fermentation culture medium; With,
(4) fermentation culture medium is filtered, retain thalline, add organic solvent (preferably alcohol, as methyl alcohol or ethanol), filter after lixiviate, collect filtrate and add the NaCl aqueous solution (the preferred saturated NaCl aqueous solution) and dilute organic solvent (preferably dilution organic solvent concentration to 15 ~ 35% (V/V)), filter after separating out precipitation, collecting precipitation is also dry.
Preferably in the method, the volume < of seed culture medium expands the volume of the volume < fermentation medium of medium, and the volume ratio of preferred seed medium, expansion medium and fermentation medium is 1: 15 ~ 25: 100 ~ 200; In step (4), the ratio (g/mL) of the weight of thalline and the volume of organic solvent is 1: 2 ~ 8, is preferably 1: 3 ~ 6; Be 75 ~ 85% containing the content of doractin in the composition of doractin, be preferably 77 ~ 83%; And/or the composition containing doractin also contains impurity A and impurity B, and the content of preferred impurity A is 6 ~ 9%, and also preferably the content of impurity B is 2 ~ 4%.Wherein, impurity A is the composition corresponding to peak at the 17 ~ 18min place on the HPLC collection of illustrative plates of the composition containing doractin prepared by the method; Impurity B is the composition corresponding to peak at the 12.9 ~ 13.9min place on the HPLC collection of illustrative plates of the composition containing doractin prepared by the method.As indicated without contrary, HPLC condition is: HPLC chromatographic column filler: Hypersil ODS2 5 μm; Chromatography column size: 4.6*250mm; Sample size; 20 μ l; Mobile phase (volume ratio): methyl alcohol: acetonitrile: water=67: 15: 18; Flow velocity: 1.0ml/min; Determined wavelength: 245nm.
Also preferably, the doractin in complex microemulsion of the present invention is the composition containing doractin, and the described composition containing doractin comprises doractin and comprises impurity A and/or impurity B.
The doractin of formula processing of the present invention is compared with organic phosphates (Hostathion, chlopyrifos, Profenofos, phoxim etc.) complex microemulsion prior art, in conventional missible oil formulation, aromatic organic solvent content is at 60-90%, and microemulsion is only containing 1-20%, reduce environmental pollution.Conventional cream preparation is mixed with and obtains liquid thin pearl fineness when spraying emulsion is 0.1-1.0 micron, and to obtain liquid thin pearl fineness when microemulsion is mixed with sprinkling emulsion be 0.001-0.01 micron, improves the availability of control efficiency and medicament.Have heat storage more stable, refrigeration without precipitate; Preparation of the present invention, to environment, people and animals and other beneficial organism safety, not easily produces poisoning; Formulation technique is simpler, easy to use, cost is lower is suitable for large scale application.
[embodiment] essence for a better understanding of the present invention, demonstrates technology contents of the present invention below.
Embodiment 1: take 95% doractin former medicine 0.32kg, 97% chlopyrifos former medicine 20.6kg is dissolved in 10kg cyclohexanone and stirs to transparent; Get calcium dodecyl benzene sulfonate 4.0kg, alkyl phenol polyoxyethyl ether 4.0kg, benzylphenol polyoxyethyl ether 4.0kg, benzyl dimethyl phenol polyoxyethyl ether 4.0kg add in oil and stir to transparent; Slowly add water 50.08kg again, fully stir, finally add 3kg ethylene glycol and stir to clarify transparent, 20.3% doractin chlorpyrifos micro emulsion can be obtained.
Embodiment 2: take 95% doractin former medicine 0.53kg, 92% Phoxim original medicine 21.7kg is dissolved in 15kg cyclohexanone and stirs to transparent; Get phenyl phenol polyoxyethyl ether 4.0kg, phenylpropyl phenethyl phenol polyoxyethyl ether 5.0kg, alkylphenol-formaldehyde resin polyoxyethyl ether 5.0kg, phenethyl phenol polyoxyethyl propyl ether 4.0kg add oil phase and stir to transparent; Slowly add water 41.77kg again, fully stir, finally add 3kg ethylene glycol and stir to clarify transparent, 20.5% doractin phoxim microemulsion can be obtained.
Embodiment 3: take 95% doractin former medicine 1.06kg, 90% Hostathion former medicine 22.2kg is dissolved in 20kg cyclohexanone and stirs to transparent; Get that alkyl divides APEO 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 add in oil phase and stir to transparent; Slowly add water 33.74kg again, fully stir, finally add 3kg ethylene glycol and stir to clarify transparent, 21% doractin triazophos micro-emulsion can be obtained.
Claims (6)
1. a doractin and organic phosphates (Hostathion, chlopyrifos, Profenofos, phoxim etc.) complex microemulsion and preparation method thereof, its preparation method comprises following steps:
(1) by doractin, organic phosphates (Hostathion, chlopyrifos, Profenofos, phoxim etc.) former medicine is dissolved in cosolvent, stirs and forms the solution of transparence.
(2) surfactant is put in the solvent of the first step, fully dissolve, form homogeneous solution.
(3) aqueous solution to be added slowly in the solution of second step and to stir, forming homogeneous solution.
(4) finally in the solution of the 3rd step, add antifreezing agent, stir into transparent homogeneous liquid.
2. the doractin according to claim 1 step (1) and organic phosphates (Hostathion, chlopyrifos, Profenofos, phoxim etc.) microemulsion, is characterized in that described cosolvent is selected from: the one in cyclohexanone, DMF, methyl alcohol, 1-METHYLPYRROLIDONE, dimethylbenzene.
3. the doractin according to claim 1 step (2) and organic phosphates (Hostathion, chlopyrifos, Profenofos, phoxim etc.) microemulsion, is characterized in that described surfactant is selected from: one or more in calcium dodecyl benzene sulfonate, 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, alkylphenol polyoxyethylene formaldehyde condensation products.
4. the doractin according to claim 1 step (4) and organic phosphates (Hostathion, chlopyrifos, Profenofos, phoxim etc.) microemulsion, is characterized in that described antifreezing agent is free: one or more in ethylene glycol, propane diols, glycerine, polyethylene glycol.
5. complex microemulsion according to claim 1, wherein, doractin is the composition containing doractin, and the described composition containing doractin comprises doractin and comprises impurity A and/or impurity B, wherein, impurity A is the composition corresponding to peak at the 17 ~ 18min place on HPLC collection of illustrative plates; Impurity B is the composition corresponding to peak at the 12.9 ~ 13.9min place on HPLC collection of illustrative plates.
6. complex microemulsion according to claim 5, wherein, the described composition containing doractin is prepared by the following method:
(1) streptomycete is inoculated in seed culture medium (formula of preferred described seed culture medium: glucose 15g, sucrose 5g, soybean meal 15g, dusty yeast 5g, pH 7.0, is settled to 1L with distilled water) middle cultivation (preferably with 30 DEG C of cultivations), obtain actication of culture thing; (2) actication of culture thing is inoculated in the expansion medium (formula of preferred described expansion medium: glucose 10g, sucrose 10g, soybean meal 15g, dusty yeast 5g, pH 7.0,1L is settled to distilled water) middle cultivation (preferably with 30 DEG C of cultivations), obtain expansion culture;
(3) expansion culture is inoculated in fermentation medium (formula of preferred described fermentation medium: corn flour 50g, soybean meal 50g, CaCO
35g, NaCl 3g, K
2hPO
42g, MgSO
41g, vitamin h 0.05g, pH 7.0, is settled to 1L with distilled water) middle cultivation (preferably with 28 DEG C of cultivations), obtain fermentation culture medium; With,
(4) fermentation culture medium is filtered, retain thalline, add organic solvent (preferably alcohol, as methyl alcohol or ethanol), filter after lixiviate, collect filtrate and add the NaCl aqueous solution (the preferred saturated NaCl aqueous solution) and dilute organic solvent (preferably dilution organic solvent concentration to 15 ~ 35% (V/V)), filter after separating out precipitation, collecting precipitation is also dry.
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Citations (7)
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| 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 |
| CN1504095A (en) * | 2002-11-30 | 2004-06-16 | 吴学民 | Chlorpyrifos, methylamino abamectin microemulsion |
| 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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- 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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