CN104872136B - A kind of microbicide compositions and preparation and its application - Google Patents
A kind of microbicide compositions and preparation and its application Download PDFInfo
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- 0 *c(cccc1)c1[N+]([O-])=O Chemical compound *c(cccc1)c1[N+]([O-])=O 0.000 description 7
- WPYUHDLKCHKILL-UHFFFAOYSA-N C[n]1nc(C(F)F)c(C(NC2C=CC=CC2Oc2ccc(C(F)(F)F)cc2Cl)=O)c1 Chemical compound C[n]1nc(C(F)F)c(C(NC2C=CC=CC2Oc2ccc(C(F)(F)F)cc2Cl)=O)c1 WPYUHDLKCHKILL-UHFFFAOYSA-N 0.000 description 1
- GANGZLOSMUFZAG-UHFFFAOYSA-N Cc(cc1)cc(Cl)c1Oc1ccccc1[N+]([O-])=O Chemical compound Cc(cc1)cc(Cl)c1Oc1ccccc1[N+]([O-])=O GANGZLOSMUFZAG-UHFFFAOYSA-N 0.000 description 1
- HFZWRUODUSTPEG-UHFFFAOYSA-N Oc(ccc(Cl)c1)c1Cl Chemical compound Oc(ccc(Cl)c1)c1Cl HFZWRUODUSTPEG-UHFFFAOYSA-N 0.000 description 1
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Abstract
The present invention relates to disinfectant use in agriculture field, a kind of microbicide compositions and preparation and its application, more particularly to a kind of bactericidal composition and preparation and its application for preventing and treating rice sheath blight disease are disclosed.Said composition is a kind of bactericidal composition containing pyrazol acid amide compounds and jinggangmeisu.The pesticidal preparations that said composition is processed can be used to prevent and treat rice sheath blight disease, have treatment and protective effect concurrently, with good synergistic effect, and have the advantages that to crop safety.
Description
Technical field
The present invention relates to disinfectant use in agriculture field, specifically, it is related to a kind of microbicide compositions and preparation and its application,
More particularly to a kind of bactericidal composition and preparation and its application for preventing and treating rice sheath blight disease.
Background technology
Rice sheath blight disease is the important disease in paddy rice producing region, is one of major disease of China paddy rice three, is produced in national each paddy rice
Qu Douyou occurs, and the Yangtze river basin and South Rice Region of China generation are heavier, especially occurs with the high-yield field of dense planting hybrid paddy rice of short stem the most general
All over and it is serious.Mainly caused by Deuteromycotina Rhizoctonia solani Kuhn (Rhizoctonia solani), disease extends from bottom to top,
Sword-like leave, or even fringe portion morbidity, sheet lodging can be arrived when serious.The heavier field of morbidity, the general underproduction 5~10% is serious reachable
50~70%.With the popularization of Multi spike cultivar of short stem, the raising of Planting Densities and Fertilization Level, it has also become rice high yield stable yields
An outstanding problem.
Jinggangmeisu (jinggangmycin) is the antibiotic that a kind of actinomyces produce, with stronger absorbability, easily quilt
Somatic cells absorb and rapid conduction in it, disturb and suppress somatic cells growth and development.It is mainly used in rice sheath blight disease
Preventing and treating.But it is administered alone that dose is increasing in recent years, in order to extend the service life of medicament, there is provided preventive effect, Jiang Jinggang is mould
Element and the bactericide compounded of other mechanisms of action will be science, the development need of the rational use of medicines.
The content of the invention
It is an object of the invention to provide a kind of microbicide compositions, bactericide to control of plant disease effect is significant
Preparation and its application prepared by composition, are especially to provide a kind of antimicrobial combination to rice sheath blight disease controlling effect is significant
Preparation and its application prepared by thing, the microbicide compositions.
The present inventor has found by in-depth study, by the pyrazol acid amide compounds and well of following ad hoc structures
Ridge mycin compounding use, pyrazol acid amide compounds and the respective drug effect of jinggangmeisu are not offset not only, conversely, also having non-
Often obvious synergistic effect, the prevention effect to fungus-caused plant disease is significantly improved, particularly to rice sheath blight disease
Prevention effect is significantly improved, and this completes the present invention.
That is, to achieve these goals, according to the first aspect of the invention, the invention provides a kind of antimicrobial combination
Thing, wherein, the active component of the microbicide compositions includes jinggangmeisu and pyrazol acid amide compounds, the pyrazol acid amide
Compound be compound shown in following formula (1) and/or compound shown in formula (2),
According to the second aspect of the invention, the invention provides above-mentioned microbicide compositions in rice sheath blight disease is prevented and treated
Using.
According to the third aspect of the invention we, the invention provides a kind of preparation as prepared by above-mentioned microbicide compositions,
Wherein, the formulation of the preparation is missible oil, aqueous emulsion, microemulsion, soluble liquid, aqueous suspension agent, suspension emulsion, ultra-low volume spray
It is mist agent, oil-suspending agent, microcapsule suspending agent, water surface film-spreading oil solution, wettable powder, water-dispersible granules, dry suspending agent, solvable
Property pulvis or soluble granula, emulsifiable pulvis, emulsifiable granule, granule, solid microcapsule formulation, effervescent tablet, bubble
Rise granule, water floating dispersible granule or seed coat agent.
According to the fourth aspect of the invention, the application the invention provides above-mentioned preparation in rice sheath blight disease is prevented and treated.
According to the microbicide compositions that the present invention is provided, it has obvious synergistic function, and bactericidal effect is good, medication
Low cost, is not likely to produce resistance, good to crop safety.The microbicide compositions that particularly present invention is provided are to rice sheath blight disease
Prevention effect is notable.
Other features and advantages of the present invention will be described in detail in subsequent specific embodiment part.
Specific embodiment
Specific embodiment of the invention is described in detail below.It should be appreciated that described herein specific
Implementation method is merely to illustrate and explain the present invention, and is not intended to limit the invention.
The active component of the microbicide compositions that the present invention is provided includes jinggangmeisu and pyrazol acid amide compounds, described
Pyrazol acid amide compounds are compound shown in following formula (1) and/or compound shown in formula (2)
Pyrazol acid amide compounds shown in Chinese style (1) of the present invention can be using the synthesis shown in following synthetic route (1)
Route synthesizes：
Pyrazol acid amide compounds shown in Chinese style (2) of the present invention can be using the synthesis shown in following synthetic route (2)
Route synthesizes：
In addition, jinggangmeisu can synthesize obtaining, it is also possible to by commercially available, such as can be purchased from the remittance of Zhejiang Province Tonglu
Rich bio tech ltd.
In the present invention, the active component include jinggangmeisu and the pyrazol acid amide compounds, jinggangmeisu and
The weight ratio of the pyrazol acid amide compounds can change in very large range, specifically, for example, jinggangmeisu and the pyrrole
The weight ratio of azoles amides compound is 1：1000~1000：1.Although in the present invention, as long as the active component includes institute
Significant synergistic function is shown by stating jinggangmeisu and the pyrazol acid amide compounds, but should from further improving
Consider in terms of synergistic function, preferably the weight ratio of jinggangmeisu and the pyrazol acid amide compounds is 1：50~50：
1；More preferably the weight ratio of jinggangmeisu and the pyrazol acid amide compounds is 1：25~25：1；Further preferred jinggangmeisu
It is 1 with the weight ratio of the pyrazol acid amide compounds：15~15：1.
In microbicide compositions of the invention, content of the active component in microbicide compositions can be in very big model
Enclose interior change, specifically, active component content in the composition be 1~95 weight %, preferably 5-90 weight %, it is more excellent
Elect 5-80 weight % as.
In microbicide compositions of the invention, in addition to the active ingredient (s, microbicide compositions are generally also containing conventional on agricultural chemicals
Various surfactants and carrier.
Above-mentioned surfactant can be the various surfactants well known to formulations of pesticide field, and the present invention is preferably breast
One or more in agent, dispersant and wetting agent.
Other carriers in addition to above-mentioned surfactant can be the various carriers well known to formulations of pesticide field, including each
Silicates are planted, carbonate, Sulfates is oxide-based, phosphoric acid salt, plant vector class, synthetic vectors class.Specifically,
For example：It is white carbon, kaolin, diatomite, clay, talcum, organobentonite, float stone, titanium dioxide, dextrin, cellulose powder, light
Matter calcium carbonate, soluble starch, cornstarch, sawdust powder, mixture, glucose, the malt of urea, amine fertilizer, urea and amine fertilizer
Sugar, sucrose, Anhydrous potassium carbonate, natrium carbonicum calcinatum, Carbon Dioxide hydrogen potassium, anhydrous sodium bicarbonate, attapulgite, Anhydrous potassium carbonate with
One or more in the mixture and natrium carbonicum calcinatum of Carbon Dioxide hydrogen potassium and the mixture of anhydrous sodium bicarbonate.
Mentioned emulsifier can be the various emulsifying agents well known to formulations of pesticide field, and specifically, the emulsifying agent can be
Calcium dodecyl benzene sulfonate, three phenethyl phenol polyoxyethylene ether phosphates, AEO, alkylphenol-polyethenoxy
Ether, alkylphenol-polyethenoxy polyethenoxy ether, fatty amine, the ethylene oxide adduct of fatty acid amide, polyoxyethylene carboxylate,
Rosin acid ethylene oxide adduct, polyol fatty acid ester and its ethylene oxide adduct, styryl phenyl APEO,
Alkyl phenol formaldehyde resin polyoxyethylene ether, terminal hydroxy group polyoxyethylene poly-oxygen propylene aether, styrylphenol formaldehyde resin polyoxy second
Alkene polyethenoxy ether, one or more combinations in castor oil polyoxyethylene ether.
Above-mentioned dispersant can be the various dispersants well known to formulations of pesticide field, and specifically, the dispersant is propylene
Sour homopolymers sodium salt, Malaysia acid disodium salt, naphthalene sulfonic acid-formaldehyde condensation product sodium salt, rosin segmented APEO polyethenoxy ether sulphur
Hydrochlorate, terminal hydroxy group polyoxyethylene poly-oxygen propylene aether block copolymer, three phenethyl phenol polyoxyethylene ether phosphates, fatty alcohol polyoxy
Ethene ether phosphate, one or more combinations in p-hydroxyphenyl lignin sulfonic acid sodium salt.
Above-mentioned wetting agent can be the various wetting agents well known to formulations of pesticide field, and specifically, the wetting agent can be
Lauryl sodium sulfate, Teepol, neopelex, AEO, alkylnaphthalene sulfonate, alkane
One or more in base phenol resin polyoxyethylene ether sulfate.
Microbicide compositions of the invention, it is various that the microbicide compositions can also be commonly used containing formulations of pesticide field
Preparation used additives, specifically, said preparation used additives can for solvent, cosolvent, thickener, antifreezing agent, capsule material, protective agent, disappear
One or more in infusion, disintegrant, stabilizer, preservative and binding agent.
Above-mentioned solvent can be the various solvents well known to formulations of pesticide field, and specifically, the solvent can be organic molten
One or more in agent, vegetable oil, mineral oil, solvent naphtha and water.
Wherein, the organic solvent includes 1-METHYLPYRROLIDONE, tetrahydrofuran, dimethyl sulfoxide (DMSO), N, the N- dimethyl last of the ten Heavenly stems
Acid amides, DMF, trimethylbenzene, durene, dimethylbenzene, toluene, octane, heptane, methyl alcohol, isopropanol, n-butanol,
One or more in tetrahydrofurfuryl alcohol, tributyl phosphate, 1,4- dioxane and cyclohexanone.
The vegetable oil includes methylated vegetable oils, turpentine-based vegetable oil, turpentine oil, epoxidized soybean oil, soybean oil, peanut
One or more in oil, rapeseed oil, castor oil, corn oil and pine-seed oil.
The mineral oil includes one or more in liquid wax, machine oil, kerosene and lubricating oil.
Meanwhile, above-mentioned solvent can also be used as cosolvent.
Above-mentioned antifreezing agent can be the various antifreezing agents well known to formulations of pesticide field, and the present invention is preferably ethylene glycol, third
One or more in glycol, glycerine and urea.
Above-mentioned thickener can be the various thickeners well known to formulations of pesticide field, and specifically, the thickener can be
Xanthans, polyvinyl alcohol, POLYPROPYLENE GLYCOL, polyethylene glycol, white carbon, diatomite, kaolin, clay, sodium alginate, alumina silicate
One or more in magnesium, lagoriolite, carboxymethylcellulose calcium, HPMC and organobentonite.
Above-mentioned capsule material can be formulations of pesticide field well known to various capsule materials, the present invention be preferably polyurethane, polyureas or
Lauxite.
Above-mentioned protective agent can be the various protective agents well known to formulations of pesticide field, and the present invention is preferably polyvinyl alcohol
And/or polyethylene glycol.
Above-mentioned defoamer can be the various defoamers well known to formulations of pesticide field, and the present invention is preferably organic silica
One or more in alkane, tributyl phosphate and silicone.
Aforementioned stable agent is selected from triphenyl phosphite, epoxychloropropane, aceticanhydride.Foregoing preservatives are selected from benzoic acid, benzene first
Sour sodium, BIT (abbreviation BIT), one or more in Kathon CG and potassium sorbate.
The present invention also provides application of the above-mentioned microbicide compositions in rice sheath blight disease is prevented and treated.
The present invention also provides a kind of preparation as prepared by above-mentioned microbicide compositions, the formulation of the preparation is missible oil,
Aqueous emulsion, microemulsion, soluble liquid, aqueous suspension agent, suspension emulsion, ultra-low volume spray agent, oil-suspending agent, microcapsule suspending agent,
It is water surface film-spreading oil solution, wettable powder, water-dispersible granules, dry suspending agent, soluble powder or soluble granula, emulsifiable
Pulvis, emulsifiable granule, granule, solid microcapsule formulation, effervescent tablet, effervescent, water floating dispersible granule
Or seed coat agent.
As described above, the formulation of microbicide compositions of the invention can be various doses well known to formulations of pesticide field
Type, specifically, can for missible oil, aqueous emulsion, microemulsion, soluble liquid, aqueous suspension agent, suspension emulsion, ultra-low volume spray agent,
Oil-suspending agent, microcapsule suspending agent, water surface film-spreading oil solution, wettable powder, water-dispersible granules, dry suspending agent, soluble powder
Agent or soluble granula, emulsifiable pulvis, emulsifiable granule, granule, solid microcapsule formulation, effervescent tablet, effervesce
Granula, water floating dispersible granule or seed coat agent, above-mentioned formulation can be prepared by the conventional method of this area.
Under preferable case, the composition of the cream preparation weight percent is active component 1~95%, cosolvent 0-
20%th, emulsifying agent 1~30%, solvent complements to 100%.
The preparation method of above-mentioned cream preparation can for example include mixing each active component, solvent, cosolvent and emulsifying agent
Close stirring and form it into homogeneous transparent oil phase, you can obtain cream preparation.
Under preferable case, the composition of the aqueous emulsion or microemulsion weight percent is active component 1~95%, emulsifies
Agent 1~30%, cosolvent 0~30%, solvent 1~30%, antifreezing agent 0~10%, thickener 0~10%, water are complemented to
100%.
Under preferable case, the method for producing aqueous emulsion can for example be included active component, emulsifying agent, cosolvent and molten
Agent mixes, and becomes homogeneous oil phase；Water, thickener, antifreezing agent etc. are mixed, makes it into homogeneous water phase.Under high speed shear,
Water is added to oil phase or oil phase is added to water phase, form the aqueous emulsion of favorable dispersibility.
Under preferable case, the preparation method of the microemulsion is that emulsifying agent, solvent is mixed into homogeneous by active component
Transparent oil phase.Under conditions of stirring.It is gradual to add water, form it into the microemulsion of transparent and homogeneous.
Under preferable case, the composition of the aqueous suspension agent weight percent is active component 1~95%, surfactant
1~30%, antifreezing agent 1~10%, thickener 0.1~5%, water complement to 100%.
Under preferable case, the composition of the oil-suspending agent weight percent is active component 1~95%, emulsifying agent 1~
30%th, dispersant 0.1%~10%, thickener 0.1~5%, oil complement to 100%.
The preparation method of water/oil-suspending agent：With water or oil as medium, by active component, surfactant, etc. auxiliary agent add
In sand milling kettle, it is ground to certain particle diameter, filters.The thickener that will be measured again is added in ground mother liquor, is cut
Cut and be uniformly dispersed.It is made oil-suspending agent or aqueous suspension agent.
Under preferable case, the soluble granula, soluble powder, water dispersible granules or wettable powder percentage by weight
Several compositions is active component 1~95%, surfactant 1~30%, other carriers complement to 100%.
Wherein, the preparation method of water-dispersible granules and soluble granula is：By each active component, dispersant, wetting agent.
Carrier etc. is well mixed, and then by air-flow crushing to certain particle diameter, adds water and is mediated, and is eventually adding in comminutor
Row granulation, water-dispersible granules or soluble granula are can obtain after drying..
The preparation method of soluble powder and wettable powder is：By each active component, various auxiliary agents and other carriers etc.
Filler is sufficiently mixed, and uses ultra-fine pulverizer disintegrating.
Under preferable case, the composition of above-mentioned microcapsule suspending agent weight percent is active component 1~95%, solvent 1~
30%th, protective agent 0.1~5.0%, defoamer 0.05~1.0%, capsule material 1~30%, dispersant 1~30%, wetting agent 0~
30%th, antifreezing agent 0~10%, thickener 0.1~5%, water complement to 100%.
Preparation method：Solvent, capsule material are mixed, active component is subsequently adding；Be added into again by protective agent, antifreezing agent,
Emulsified in the mixture of defoamer and water composition, stirring is until polymerisation is completed；Add thickener, dispersant and wetting
Agent, the microcapsule suspending agent stablized.
Present invention also offers application of the above-mentioned preparation in rice sheath blight disease is prevented and treated.
Microbicide compositions of the invention can be provided in finished product preparation form, i.e., each material is blended in composition；
Can also be provided with independent dosage form, voluntarily be mixed in bucket or tank using preceding, and selected according to the concentration of required active material
Mix with water to selecting property and be diluted.
Composition of the invention can also have sterilized, desinsection or the compound of herbicidal performance to be used in mixed way with other, also may be used
It is used in mixed way with nematicide, protective agent, growth regulator, nutrient for plants or soil conditioner.
The application method of microbicide compositions of the invention is simple, before plant disease sprouting or after sprouting, to work
The place of thing and plant growth is applied according to a conventional method, such as mixes soil, spraying, injection, cast, and its amount of application is according to weather conditions
Or depending on crop condition, generally apply 1-100g for every mu, it is diluted to 1-2000mg/L administrations.Diluent is preferably water.
Microbicide compositions of the invention, its bactericidal effect is generally relevant with extraneous factor such as weather, but by using suitable
When formulation can slow down the influence of weather.
The present invention is further detailed below by way of specific embodiment, but the present invention is not limited in following realities
Apply example.
Jinggangmeisu is purchased from Zhejiang Tonglu Huifeng Bioscience Co., Ltd. (purity is in following test case and preparation example
60%).
In following preparation example, percentage composition is weight percentage in all formulations proportioning.
In following test case and preparation example, the compound shown in formula (1) and formula (2) is (below also by formula (1) and formula (2) institute
The compound for showing is referred to as Y12196 and Y13149) carried out according to foregoing synthetic route (1) and synthetic route (2)
Synthesis, its specific synthetic method is as follows.
1st, the synthesis of the chloro- 1- of 2,4- bis- (2- nitro-phenoxies) benzene
By 2.82g (20mmol) 2- fluoronitrobenzenes and 4.89g (30mmol) 2,4 dichloro phenol, 4.15g (30mmol)
K2CO3In adding to 100ml mono- necks bottle with 50ml DMF, after being heated to reflux 5h, DMF is removed under reduced pressure, three are washed with the 10%NaOH aqueous solution
It is secondary, it is extracted with ethyl acetate, anhydrous Na2SO4Precipitation after drying, obtains 2,4- bis- chloro- 1- (2- nitro-phenoxies) benzene 5.50g, yield
97%.
2nd, the synthesis of 2- (2,4 dichloro benzene epoxide) aniline
Chloro- 1- (2- nitro-phenoxies) benzene of 5.50g (19.36mmol) 2,4- bis- 100ml ethanol is dissolved, is added
1.04g (19.36mmol) ammonium chlorides and 10ml water, add 3.24g (58.08mmol) iron powder in three batches after being heated to reflux, reaction
By reaction system silica gel suction filtration after 6h, ethanol is removed in rotation, adds 100ml ethyl acetate, is washed with 60ml × 3 time saturated common salt,
Precipitation after drying, obtains 2- (2,4- dichlorophenoxy) aniline 4.50g, yield 91%.
3rd, the synthesis of 2- (2- chloro-trifluoromethyl phenoxies) aniline
By 5.00g (45.82mmol) Ortho-Aminophenols and the chloro- 4- fluoride trifluoro toluenes of 9.10g (45.82mmol) 3-, 9.50g
(68.73mmol)K2CO3In adding to 250ml mono- necks bottle with 100ml DMF, after being heated to reflux 5h, DMF is removed under reduced pressure, with 10%
The NaOH aqueous solution is washed three times, is extracted with ethyl acetate, anhydrous Na2SO4Precipitation after drying, obtains 2- (the chloro- 4- trifluoromethylbenzenes oxygen of 2-
Base) aniline 9.53g, yield 72%.
4th, the synthesis of the compound shown in formula (1)
0.50g (1.97mmol) 2- (2,4- dichlorophenoxy) aniline is dissolved in 20ml dichloromethane, 0.30g is added
(2.95mmol) triethylamine, then 3- difluoromethyl -1- methyl isophthalic acid H- pyrazoles -4- formyl chlorides are slowly added dropwise under condition of ice bath
0.46g(2.36mmol).30ml dichloromethane, 50ml × 3 time saturated aqueous common salt will be added in system after TLC monitoring reactions completely
Wash, anhydrous sodium sulfate drying, column chromatography purifies to obtain compound I 0.70g, yield 86%.
5th, the synthesis of the compound shown in formula (2)
0.57g (1.97mmol) 2- (2- chloro-trifluoromethyl phenoxies) aniline is dissolved in 20ml dichloromethane, is added
0.30g (2.95mmol) triethylamine, then 3- difluoromethyl -1- methyl isophthalic acid H- pyrazoles -4- formyls are slowly added dropwise under condition of ice bath
Chlorine 0.46g (2.36mmol).30ml dichloromethane, 50ml × 3 time saturated common salt will be added in system after TLC monitoring reactions completely
Washing, anhydrous sodium sulfate drying, column chromatography purifies to obtain compound I 0.75g, yield 85%.
Obtained formula (1) is as follows to the related nuclear magnetic data of the compound shown in formula (2)：
Compound shown in formula (1):1H NMR(600MHz,CDCl3) δ 8.67 (s, 1H), 8.55 (d, J=8.4Hz, 1H),
7.99 (s, 1H), 7.48 (t, J=8.4Hz, 1H), 7.21 (m, 2H), 7.04 (s, 1H), 6.92 (t, J=48.6Hz, 1H),
6.74 (d, J=13.8Hz, 1H), 3.95 (s, 3H) .MS:M/z=411.29 (M+) .m.p.:102.5-103.6℃.
Compound shown in formula (2):1H NMR(600MHz,CDCl3) δ 8.62 (s, 1H), 8.58 (d, J=8.4Hz, 1H),
7.99 (s, 1H), 7.75 (s, 1H), 7.46 (d, J=9Hz, 1H), 7.24 (d, J=7.8Hz, 1H), 7.11 (t, J=7.8Hz,
1H), (s, the 3H) .MS of 6.99 (d, J=9Hz, 1H), 6.87 (t, J=53.4Hz, 1H), 6.86 (s, 1H), 3.92:M/z=
445.15(M+).m.p.:114.3-115.4℃.
Test case 1
This test case is used to illustrate the indoor virulence that jinggangmeisu is compounded to rice sheath blight disease with pyrazol acid amide compounds
Determine
Subjects：Rice sheath blight disease (Rhizoctonia solani)
Test method：With reference to《People's Republic of China (PRC) agricultural industry criteria NY/T 1156.2-2006》Mycelial growth speed
Rate method.Each medicament is set 5 dosage treatment by active constituent content respectively, and above-mentioned each pathogen PDA culture medium culture is treated
When bacterium colony just covers with culture dish, bacterium block is broken into colony edge with the card punch of diameter 5mm, moved to bacterium block in advance with transfer needle
The toxic PDA culture medium center being configured to, is subsequently placed in culture in 25 DEG C of incubators, and often treatment is repeated 4 times.Depending on CK colony growths
Situation, each treatment colony diameter cm is measured using crossing method slide calliper rule, is obtained correction and is suppressed percentage.By inhibiting rate
Linear regression analysis between probit value and the logarithm value of series concentration, obtains the EC of each medicament50Value, further according to the abundant method meters of Sun Yun
Calculate co-toxicity coefficient (CTC).
Drug effect is calculated：Two diameters are surveyed in each bacterium colony right-angled intersection, and bacterium colony size is represented with its average.Obtain as the following formula
Colony growth inhibiting rate：Colony growth inhibiting rate %=(blank bacterium colony increases diameter-chemicals treatment bacterium colony and increases diameter)
× 100/ blank bacterium colony increases diameter.
Result carries out data analysis statistical with 3.11 professional versions of DPS, obtains regression straight line, EC50, coefficient correlation.According to grandson
The EC of each treatment that Yun Pei (Y-P Sun) methods will be determined50It is converted into actual poison exponent (ATI)；According to the proportioning of mixture, obtain
Theoretical toxicity index (TTI), the co-toxicity coefficient (CTC) of mixture is calculated by following equation.
Co-toxicity coefficient (CTC)=[the actual toxicity index of mixture (ATI)/mixture theoretical toxicity index (TTI)] × 100
The actual toxicity index of mixture (ATI)=(EC of standard agent50The EC of/mixture50)×100
There is the TI × mixture of the content+B agent of A in the TI of mixture theoretical toxicity index (TTI)=A agent × mixture active ingredient
The content of B in effect composition
Toxicity index (TI)=(EC of standard agent50The EC of/reagent agent50(one kind in A agent, B agent is made) × 100
It is standard agent)
A agent, B agent are respectively two kinds of mutually mixed active components, and mixture is the mixture after A agent is mutually mixed with B agent.
Evaluation criterion：When CTC >=120, synergistic effect is shown as；When CTC≤80, antagonism is shown as；80 ＜ CTC ＜
120, show as summation action.
Table 1
| Medicament | EC50(μg/mL) | ATI | TTI | Co-toxicity coefficient CTC |
| Jinggangmeisu (A) | 352.59 | 100 | ||
| Y12196(B1) | 0.0127 | 2776299.21 | ||
| Y13149(B2) | 0.0041 | 8599756.10 | 168720.71 | 122.93 |
| A+B1(50：1)(1) | 0.4800 | 73456.25 | 54535.28 | 134.69 |
| A+B1(25：1) | 0.2400 | 146912.50 | 106876.89 | 137.46 |
| A+B1(12：1) | 0.1200 | 293825.00 | 213653.79 | 137.52 |
| A+B1(6：1) | 0.0440 | 801340.91 | 396699.89 | 202.00 |
| A+B1(4：1) | 0.0323 | 1091609.91 | 555339.84 | 196.57 |
| A+B1(2：1) | 0.0097 | 3634948.45 | 925499.74 | 392.76 |
| A+B1(1：1) | 0.0065 | 5424461.54 | 1388199.61 | 390.76 |
| A+B1(1：2) | 0.0063 | 5596666.67 | 1850899.47 | 302.38 |
| A+B1(1：4) | 0.0072 | 4897083.33 | 2221059.37 | 220.48 |
| A+B1(1：6) | 0.0077 | 4579090.91 | 2379699.32 | 192.42 |
| A+B1(1：12) | 0.0082 | 4299878.05 | 2562745.42 | 167.78 |
| A+B1(1：25) | 0.0092 | 3832500.00 | 2669522.32 | 143.57 |
| A+B1(1：50) | 0.0102 | 3456764.71 | 2721863.93 | 127.00 |
| A+B2(50：1) | 0.1700 | 207405.88 | 330856.00 | 133.21 |
| A+B2(25：1) | 0.0800 | 440737.50 | 661612.01 | 133.23 |
| A+B2(12：1) | 0.0400 | 881475.00 | 1228622.30 | 143.49 |
| A+B2(6：1) | 0.0200 | 1762950.00 | 1720031.22 | 262.81 |
| A+B2(4：1) | 0.0078 | 4520384.62 | 2866652.03 | 315.38 |
| A+B2(2：1) | 0.0039 | 9040769.23 | 4299928.05 | 328.00 |
| A+B2(1：1) | 0.0025 | 14103600.00 | 5733204.07 | 292.86 |
| A+B2(1：2) | 0.0021 | 16790000.00 | 6879824.88 | 269.74 |
| A+B2(1：4) | 0.0019 | 18557368.42 | 7371233.80 | 136.67 |
| A+B2(1：6) | 0.0035 | 10074000.00 | 7938244.09 | 143.28 |
| A+B2(1：12) | 0.0031 | 11373870.97 | 8269000.10 | 129.21 |
| A+B2(1：25) | 0.0033 | 10684545.45 | 8431135.39 | 123.00 |
| A+B2(1：50) | 0.0034 | 10370294.12 | 168720.71 | 122.93 |
Remarks：(1)Numeric ratio in the bracket of expression is two kinds of weight proportions of medicament.
Preparation example 1
This preparation example is used to illustrate the preparation of soluble powder
Weigh 70% jinggangmeisu, 10%Y13149,4% white carbon, 2% alkylnaphthalene sulfonate condensation polymer and (be purchased from Acker
It is Nobel Chemical Co., Ltd. of Soviet Union, same as below), 1.5% lauryl sodium sulfate, ammonium sulfate add to 100%.
Preparation method：Produced by above-mentioned raw materials are blended, after the trapping of ultra micro air-flow crushing, cloth bag 80% jinggangmeisu-
Y13149 soluble powders Y1.
Preparation example 2
This preparation example is used to illustrate the preparation of soluble powder
Weigh 40% jinggangmeisu, 20%Y12196,3% white carbon, 2% alkylnaphthalene sulfonate condensation polymer, 2% 2 isobutyl
Base sodium naphthalene sulfonate, ammonium sulfate add to 100%.
It is soluble 60% jinggangmeisu-Y12196 to be produced by above-mentioned raw materials are blended, after the trapping of ultra micro air-flow crushing, cloth bag
Pulvis Y2.
Preparation example 3
This preparation example is used to illustrate the preparation of suspending agent
Weigh 10% jinggangmeisu, 20%Y13149,2%TERSPERSE 2500 and (be purchased from Hensel Man, following phase
Together), 3%TERSPERSE 4896 (being purchased from Hensel Man, same as below), 0.2% xanthans, 3% white carbon, 5% second two
Alcohol, 0.3% benzoic acid, 0.5% organic silicon defoamer (trade name：S-29 Nanjing "four news" (new ideas applied chemistry product company produces, following phase
Together), deionized water adds to 100%.
Preparation method：By active ingredient, wetting agent, dispersant, antifreezing agent etc. is well mixed, adds and be ground in sand mill
After certain particle diameter, filtering.Add and 30% jinggangmeisu-Y13149 suspending agents are obtained by the xanthans for preparing is stirred until homogeneous
Y3。
Preparation example 4
This preparation example is used to illustrate the preparation of suspending agent
(alkylnaphthalene sulfonate formaldehyde condensation products are purchased from Shanghai day to weigh 25% jinggangmeisu, 25%Y12196,2%NNO
It is altar auxiliary agent Co., Ltd, same as below), 2%TERSPERSE 2500,0.1% xanthans, 3% white carbon, 5% propane diols,
0.5% Sodium Benzoate, 0.5% organic silicon defoamer, deionized water add to 100%.
Preparation method：By active ingredient, wetting agent, dispersant, antifreezing agent etc. is well mixed, adds and be ground in sand mill
After certain particle diameter, filtering.Add and 50% jinggangmeisu-Y12196 suspending agents are obtained by the xanthans for preparing is stirred until homogeneous
Y4。
Preparation example 5
This preparation example is used to illustrate the preparation of wettable powder
Weigh 30% jinggangmeisu, 30%Y12196,5% calcium lignosulfonate, 2% Nekal BX and (be purchased from the Shanghai the Temple of Heaven
It is auxiliary agent Co., Ltd, same as below), 1% lauryl sodium sulfate, 5% white carbon, kaolin add to 100%.
Preparation method：60% jinggangmeisu-Y12196 wettable powders are obtained by above-mentioned raw materials are blended, after air-flow crushing
Y5。
Preparation example 6
This preparation example is used to illustrate the preparation of wettable powder
Weigh 60% jinggangmeisu, 15%Y13149,4% calcium lignosulfonate, 3%TERSPERSE2700 and (be purchased from Hensel
It is Man, same as below), 2% Nekal BX, 2% lauryl sodium sulfate, 5% white carbon, fine particle calcium carbonate add to 100%.
Preparation method：75% jinggangmeisu-Y13149 wettable powders are obtained by above-mentioned raw materials are blended, after air-flow crushing
Y6。
Preparation example 7
This preparation example is used to illustrate the preparation of microemulsion
Weigh 5% jinggangmeisu, 10%Y12196,4%TX-10 (being purchased from Xingtai blue star auxiliary agent company, same as below),
(being purchased from Nanjing too chemical industry has for 5% Nongru-700 # (being purchased from Nanjing Teva-Chem. Co., Ltd., same as below), 6% agriculture breast 500#
It is limit company, same as below), 4% agriculture breast 1601# (being purchased from Nanjing Teva-Chem. Co., Ltd., same as below), 15% cyclohexanone,
5%N- methyl pyrrolidones, 5% n-butanol, 1% epoxychloropropane, through dissolving completely and be well mixed, deionized water is added to
100%, 15% jinggangmeisu-Y12196 microemulsions Y7 is obtained after stirring.
Preparation example 8
This preparation example is used to illustrate the preparation of microemulsion
Weigh 10% jinggangmeisu, 10%Y13149,5% agriculture breast 400# and (be purchased from Nanjing Teva-Chem. Co., Ltd., below
It is identical), 4% agriculture breast 500#, 6% agriculture breast 1601#, 25% cyclohexanone, 5% dimethylbenzene, 5% isopropanol, 3% phosphorous triphenyl phosphate
Ester, through dissolving completely and be well mixed, deionized water adds to 100%, after stirring be obtained 20% jinggangmeisu-Y13149 microemulsions
Y8。
Preparation example 9
This preparation example is used to illustrate the preparation of aqueous emulsion
Weigh 5% jinggangmeisu, 10%Y12196,3% agriculture breast 2201# and (be purchased from Nanjing Teva-Chem. Co., Ltd., below
It is identical), 1.5% Nonyl pheno (EO=10) ether phosphate (being purchased from Nanjing Teva-Chem. Co., Ltd., same as below),
2.5% triphenoethyl benzene phenol polyethenoxy ether phosphate (agriculture breast 600# acid phosphatide, be purchased from Nanjing Teva-Chem. Co., Ltd.),
2%Span-60# (being purchased from Xingtai blue star auxiliary agent company, same as below), 1% epoxychloropropane, 20% dimethylbenzene, 10% hexamethylene
Ketone, 0.1% xanthans, 0.5% benzoic acid, deionized water add to 100%.
Preparation method：By above-mentioned active ingredient, emulsifying agent, after dispersant is dissolved with solvent, under conditions of high shear, plus
Enter in water phase, add xanthans and stir prepared 15% jinggangmeisu-Y12196 aqueous emulsions Y9.
Preparation example 10
This preparation example is used to illustrate the preparation of aqueous emulsion
Weigh 6% jinggangmeisu, 6%Y13149,2% agriculture breast 2201#, 3% Nonyl pheno (EO=10) ether phosphorus
Acid esters, 2%Span-60#, 2% emulsifying agent T-60 (being purchased from Xingtai blue star auxiliary agent company), 1% triphenyl phosphite, 15% diformazan
Benzene, 10% cyclohexanone, 0.3% xanthans, 0.5% benzoic acid, deionized water add to 100%.
Preparation method：By above-mentioned active ingredient, emulsifying agent, after dispersant is dissolved with solvent, under conditions of high shear, plus
Enter in water phase, add xanthans and stir prepared 12% jinggangmeisu-Y13149 aqueous emulsions Y10.
Control preparation example 1
Weigh 24%Y12196,2%TERSPERSE 2500,3%TERSPERSE 2425 (be purchased from Hensel Man, with
Under it is identical), 0.2% xanthans, 3% white carbon, 5% ethylene glycol, 0.3% benzoic acid, 0.5% organic silicon defoamer, deionization
Water adds to 100%.
Preparation method：By active ingredient, wetting agent, dispersant, antifreezing agent etc. is well mixed, adds and be ground in sand mill
After certain particle diameter, filtering.Add the xanthans for preparing and be stirred until homogeneous and can be prepared by 24%Y12196 suspending agents.
Control preparation example 2
Weigh 24%Y13149,2%TERSPERSE 2500,3%TERSPERSE 2425,0.2% xanthans, 3% white
Carbon black, 5% ethylene glycol, 0.3% benzoic acid, 0.5% organic silicon defoamer, deionized water add to 100%.
Preparation method：By active ingredient, wetting agent, dispersant, antifreezing agent etc. is well mixed, adds and be ground in sand mill
After certain particle diameter, filtering.Add the xanthans for preparing and be stirred until homogeneous and can be prepared by 24%Y13149 suspending agents.
Test case 2
This test case prevents and treats rice sheath blight disease field control effectiveness test for explanation
Test site is Shaoxing five and base, according to medicine inspecting institute of the Ministry of Agriculture " GB/T 17980.20-2000 agricultural chemicals field medicine
The regulation of effect test rule (one) bactericidal agent for preventing and treating rice sheath blight disease ", at the cell of test medicine, comparison medicament and blank
Reason is using the arrangement of random district's groups, plot area 15m2, 4 repetitions, this experiment amount to dispenser twice.In hair during first time dispenser
At the sick initial stage, second medicine is applied after two weeks.This experiment amounts to be investigated 2 times, per experimental plot using 5 points of samplings of diagonal, every tune
Connected 5 clumps are looked into, totally 25 clumps, disease grade is recorded.
Disease scale standard is as follows：
0 grade：Complete stool is disease-free；
1 grade：Quaterfoil and its following leaf sheath, blade morbidity (being first piece leaf with sword-like leave)；
3 grades：3rd leaf and its following leaf sheath, blade morbidity；
5 grades：Second leaf and its following leaf sheath, blade morbidity；
7 grades：Sword-like leave blade and its following leaf sheath, blade morbidity；
9 grades：Complete stool falls ill, withered ahead of time.
Drug effect computational methods：
According to investigation result, disease index and preventive effect are calculated according to following (1), (2) formula.
In formula：CK0、CK1The respectively forward and backward disease index of blank district dispenser；PT0、PT1Respectively chemicals treatment
The forward and backward disease index of area's medicine.
In addition, dispenser medicine, active ingredient amount and test result are as shown in table 2
Table 2
Remarks：10% jinggangmeisu aqua is purchased from Zhejiang Tonglu Huifeng Bioscience Co., Ltd.
The bactericidal composition that can be seen that present invention offer from above effect data has spy for preventing and treating rice sheath blight disease
Effect, rationally, with treatment plus protective effect, and bactericidal effect is good for component, thus, it is possible to reduce times for spraying, reduce medication into
This.More importantly its activity and bactericidal effect are not the simple superposition of each component activity, but have significant synergies,
The generation of resistance can be slowed down, to crop safety, meet the security requirement of pesticidal preparations.
The preferred embodiment of the present invention described in detail above, but, the present invention is not limited in above-mentioned implementation method
Detail, in range of the technology design of the invention, various simple variants can be carried out to technical scheme, this
A little simple variants belong to protection scope of the present invention.
It is further to note that each particular technique feature described in above-mentioned specific embodiment, in not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention to it is various can
The combination of energy is no longer separately illustrated.
Additionally, can also be combined between a variety of implementation methods of the invention, as long as it is without prejudice to originally
The thought of invention, it should equally be considered as content disclosed in this invention.
Claims (6)
1. a kind of microbicide compositions, it is characterised in that the active component of the microbicide compositions includes jinggangmeisu and pyrazoles
Amides compound, the pyrazol acid amide compounds are compound shown in following formula (1),
Wherein, the weight ratio of the jinggangmeisu and the pyrazol acid amide compounds is 1：0.5-1.
2. microbicide compositions according to claim 1, wherein, content of the active component in microbicide compositions
It is 1-95 weight %.
3. microbicide compositions according to claim 2, wherein, content of the active component in microbicide compositions
It is 5-90 weight %.
4. application of the microbicide compositions described in claim 1-3 any one in rice sheath blight disease is prevented and treated.
5. the preparation prepared by the microbicide compositions as described in claim 1-3 any one, wherein, the formulation of the preparation
It is missible oil, aqueous emulsion, microemulsion, soluble liquid, aqueous suspension agent, suspension emulsion, ultra-low volume spray agent, oil-suspending agent, micro-capsule
Suspending agent, water surface film-spreading oil solution, wettable powder, water-dispersible granules, dry suspending agent, soluble powder or soluble grain
Agent, emulsifiable pulvis, emulsifiable granule, granule, solid microcapsule formulation, effervescent tablet, effervescent, water floating point
Scattered seed agent or seed coat agent.
6. application of the preparation described in claim 5 in rice sheath blight disease is prevented and treated.
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| CN106993612A (en) * | 2017-05-12 | 2017-08-01 | 江苏克胜作物科技有限公司 | A kind of mechanization prevents and treats spray adjuvantses |
| CN109096209B (en) * | 2017-06-20 | 2022-03-01 | 华中师范大学 | Pyrazinamide compounds, preparation method and application thereof, and bactericide |
| WO2020047716A1 (en) * | 2018-09-03 | 2020-03-12 | 华中师范大学 | Pyrazinamide compound, preparation method therefor and application thereof, and bactericide |
| CN111138300A (en) * | 2018-11-02 | 2020-05-12 | 东莞市东阳光菌阳氢专利农药有限公司 | Preparation method of fluorobenzene ether amide and intermediate thereof |
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