Summary of the invention
The technical problem that the present invention will solve is: to bactericide resistance and pedo relict problem in practical application; The bactericide that filters out two kinds of different sterilizing mechanismses carries out composite, and to improve the bactericidal agent for preventing and treating effect, delaying drug resistance produces; Reduce amount of application, reduce the control cost.
For solving the problems of the technologies described above, the invention provides a kind of bactericidal composition, said composition comprises A and two kinds of active ingredients of B, and active component A is SSF 126 (Metominostrobin), and active component B is for being selected from Prochloraz (Prochloraz).The inventor finds that through test above-mentioned bactericidal composition synergy is obvious, the more important thing is that amount of application reduces, and reduces use cost.It is different with the compound structure type of B component to contain component A, and mechanism of action is different, and both are composite can to enlarge fungicidal spectrum, and can delay the generation and the development speed of pathogen resistance to a certain extent, and does not have cross resistance between component A and the B component.
Another object of the present invention provides the preparation method who comprises two kinds of effective constituents A and B bactericidal composition and prevents and treats the application of crop pest at agriculture field.
In the above-mentioned bactericidal composition, the weight ratio between weight two components of component A and B component is 0.02~50.According to physicochemical property between the component and practical application, the preferred weight ratio of active component SSF 126 (A) and active component Prochloraz (B) is 0.05~30, and A and two kinds of active components of B account for the 5-90% of bactericide gross weight.
The invention provides the purposes of bactericidal composition in controlling plant diseases of forming by component A (SSF 126) and B component (Prochloraz), like SSF 126 and Prochloraz is composite that rice blast is had very high preventive effect.
Above-mentioned composition also comprises carrier, auxiliary agent and/or surfactant.In the process of using, can mix auxiliary agent commonly used.
Proper auxiliary agent can be solid or liquid, and they are material commonly used in the formulation process normally, mineral matter for example natural or regeneration, solvent, dispersant, wetting agent, adhesive, thickener, adhesive or fertilizer.
The application process of the present composition comprises the acrial part that composition of the present invention is used for plant growing, particularly leaf portion or blade face.Frequency of using and amount of application depend on the biology and the weather life condition of pathogene.Can be with the growth place of plant, like the rice field, soak with the liquid preparation of composition, perhaps composition is applied in the soil with solid form, as with particle form (soil application), composition can be by soil in plant root gets into plant corpus (systemic action).
These compositions can only comprise active component and use; Also can be mixed together use with additive; Therefore composition of the present invention can be prepared into various formulations, for example wetting powder, suspending agent, oil-suspending agent, water dispersible granules, aqueous emulsion, microemulsion.According to the character of these compositions and use composition the purpose and the ambient conditions that will reach, can select with composition with spraying, atomizing, dust, broadcast sowing or sprinkle the method for watering etc. and so on and use.
Available known method can become various formulations with preparation of compositions of the present invention, can active ingredient and auxiliary agent like solvent, solid carrier, can evenly be mixed, grind when needing with surfactant, is prepared into needed formulation.
Above-mentioned solvent can be selected from aromatic hydrocarbon, preferably contains 8-12 carbon atom, like xylene mixture or substituted benzene, phthalate; Sad like Dibutyl phthalate or phthalandione two, fat hydrocarbon, like cyclohexane or paraffin, pure and mild ethylene glycol and their ether and ester; Like ethanol, ethylene glycol, glycol monomethyl methyl; Ketone, like cyclohexanone, the solvent of strong polarity, like the N-N-methyl-2-2-pyrrolidone N-, dimethyl sulfoxide (DMSO) or dimethyl formamide and vegetable oil or vegetable oil are like soybean oil.
Above-mentioned solid carrier, but as be used for the normally natural minerals filler of pulvis and dispersant, for example talcum, kaolin, montmorillonite or atlapulgite.For the physical property of management group compound, also can add polymolecularity silicic acid or polymolecularity adsorpting polymerization thing carrier, for example granular absorption carrier or non-absorption carrier, suitable granular absorption carrier is a porous type, like float stone, bentonite or bentonite; Suitable non-absorption carrier such as calcite or sand.In addition, can use the granular material of being prefabricated into of a large amount of inorganic in nature or organic character as carrier, particularly dolomite.
According to the chemical property of the active ingredient in the composition of the present invention, suitable surfactant is lignin sulfonic acid, naphthalene sulfonic acids, phenolsulfonic acid, alkali salt or amine salt, alkylaryl sulfonates, alkyl sulfate; Alkylsulfonate, aliphatic alcohol sulfate, fatty acid and sulphated fatty alcohol glycol ether, the condensation product of sulfonated naphthalene and naphthalene derivatives and formaldehyde in addition; The condensation product of naphthalene or naphthalene sulfonic acids and phenol and formaldehyde, NONIN HS 240, ethoxylation isooctylphenol; Octyl phenol, nonyl phenol, alkylaryl polyglycol ether; Tributyl benzene polyglycol ether, three stearyl phenyl polyglycol ethers, alkyl aryl polyether alcohol; Ethoxylated castor oil, polyoxyethylene alkyl ether, ethylene oxide condensation product, ethoxylation polyoxypropylene; Lauric acid polyglycol ether acetal, sorbitol ester, lignin sulfite waste liquor and methylcellulose.
Two kinds of active ingredients show as synergistic effect in the composition of the present invention, and the specific activity of said composition is used the activity expection summation of single compound, and the independent activity of single compound is more remarkable.Synergistic effect shows as and allows that amount of application reduces, wideer antifungal control spectrum, instant effect, more lasting control efficiency, through only once or minority use better controlling plant harmful fungoid several times and widened the possible administration interval time.These characteristics are special needs in the plant epiphyte control practice process.
Other characteristics that show of bactericidal composition of the present invention mainly show as: 1, because two single thinner architectural differences of this composition are very big; The mechanism of action is different fully; There is not cross resistance, can delays two single agent and use the resistance problem that is produced separately; 2, composition of the present invention is good to crop safety, preventive effect.Through evidence, microbicide compositions chemical property of the present invention is stable, and synergy is remarkable, and controlling object is shown tangible synergy and complementation.
Embodiment
In order to make the object of the invention, technical scheme and advantage clearer,, the present invention is further elaborated below in conjunction with embodiment.Should be appreciated that specific embodiment described herein only in order to explaining the present invention, and be not used in qualification the present invention, all any modifications of within spirit of the present invention and principle, being made, be equal to and replace and improvement etc., all should be included within protection scope of the present invention.
Percentage all is weight percentage in all prescriptions of following examples.The processing technology of the various preparations of the present composition is prior art, can change to some extent according to different situations.
One, formulation prepares embodiment
(1) processing of water dispersible granules and embodiment
Active component SSF 126 and Prochloraz, auxiliary agent and filler is even by the mixed of prescription, become wetting powder through comminution by gas stream, add the granulation of a certain amount of water extrusion again, after dry screened, make the water dispersible granules product.
Embodiment 1:86% SSF 126 Prochloraz water dispersible granules
SSF 126 82%, Prochloraz 4%, dodecyl sodium sulfate 3%, Negel 2%, ammonium sulfate 2%, precipitated calcium carbonate complements to 100%.
Embodiment 2:65% SSF 126 Prochloraz water dispersible granules
SSF 126 3%, Prochloraz 62%, methyl naphthalene sulfonate formaldehyde condensate 5%, sodium lignin sulfonate 3%, lauryl sodium sulfate 4%, diatomite complements to 100%.
(2) processing of suspending agent and embodiment
Each component such as active component SSF 126 and Prochloraz, dispersant, wetting agent, thickener and water is even by the mixed of prescription, after sand milling and/or high speed shear, obtain semi-finished product, add water after the analysis and mix to filter and get product.
Embodiment 3:35% SSF 126 Prochloraz suspending agent
SSF 126 30%, Prochloraz 5%, sodium lignin sulfonate 7%, xanthans 0.8%, bentonite 3%, Magnesiumaluminumsilicate 1%, ethylene glycol 4%, water complements to 100%.
Embodiment 4:18% SSF 126 Prochloraz suspending agent
SSF 126 6%, Prochloraz 12%, methyl naphthalene sulfonate formaldehyde condensate 6%, bentonite 4%, glycerine 5%, water complements to 100%.
(3) processing of wetting powder and embodiment
The active component SSF 126 is fully mixed with Prochloraz, various auxiliary agent and filler etc. in proportion, after ultrafine crusher is pulverized, make wetting powder.
Embodiment 5:45% SSF 126 Prochloraz wetting powder
SSF 126 25%, Prochloraz 20%, calcium lignosulfonate 7%, neopelex 12%, bentonite 16%, attapulgite complements to 100%.
Embodiment 6:76% SSF 126 Prochloraz wetting powder
SSF 126 73%, Prochloraz 3%, alkyl polyoxy ethyl ether sulfonate 1% draws back powder 4%, bentonite 1.5%, white carbon 5%, diatomite complements to 100%.
Embodiment 7:58% SSF 126 Prochloraz wetting powder
SSF 126 4%, Prochloraz 54%, alkylsulfonate 6%, sodium lignin sulfonate 6%, white carbon 11%, kaolin complements to 100%.
(4) processing of microemulsion and embodiment
SSF 126 and Prochloraz fully after the dissolving, are stirred in solvent, add emulsifier, builder and antifreeze simultaneously, treat above-mentioned system mixing after, again water is slowly added in the above-mentioned mixed liquor, can be made into the microemulsion of different content after fully stirring.
Embodiment 8:12% SSF 126 Prochloraz microemulsion
SSF 126 4%, Prochloraz 8%, acetone 15%, compound sodium nitrophenolate 0.5%, alkyl polyoxyethylene ether and NPE 5%, propane diols 1%, urea 2%, water complements to 100%.
Embodiment 9:16% SSF 126 Prochloraz microemulsion
SSF 126 12%, Prochloraz 4%, polyoxyethylene carboxylate and phenethyl phenol polyethenoxy ether 4%, glycerine 2%, methyl alcohol 11%, azone 1%, water complements to 100%.
(5) processing of aqueous emulsion and embodiment
In the emulsification still; SSF 126 and Prochloraz, solvent, auxiliary agent are mixed under mechanical agitation, drop into emulsifier then and stabilizing agent stirs, add entry at last; Under 100-12000 rev/min rotating speed, stirred 10-30 minute, make it to become the product of even emulsus.
Embodiment 10:30% SSF 126 prochloraz aqueous emulsion
SSF 126 18%, Prochloraz 12%, N-repefral 4%, nonyl phenol benzene oxygen vinethene 3%; 2,6 di tert butyl 4 methyl phenol 2%, ethylene glycol 3%, polyvinyl alcohol 1%; Sodium Benzoate 1%, silicone defoaming agent 0.8%, water complements to 100%.
Embodiment 11:45% SSF 126 prochloraz aqueous emulsion
SSF 126 8%, Prochloraz 37%, butylated hydroxy anisole 4% gathers isosuccinic acid acid anhydride-ethylene glycol copolymer 3%, propane diols 2%, xanthans 3%, polyvinyl alcohol 1%, silicone defoaming agent 1.2%, water complements to 100%.
(6) processing of oil-suspending agent and embodiment
With the mixed of each component such as active component SSF 126 and Prochloraz, dispersant, stabilizing agent, antifoaming agent and solvent, after putting into the sand milling still and grinding, send into the interior mixing of homogeneous blender and get product by prescription.
Embodiment 12:15% SSF 126 Prochloraz oil-suspending agent
SSF 126 5%, Prochloraz 10%, sodium lignin sulfonate 8%, bentonite 4%, xanthans 1%, silicone defoaming agent 2%, soybean oil complements to 100%.
Embodiment 13:28% SSF 126 Prochloraz oil-suspending agent
SSF 126 24%, Prochloraz 4% draws back powder 8%, bentonite 5%, organic silicone 2%, machine oil complements to 100%.
Two, drug effect demonstration test
(1) biologicall test embodiment 1
1, SSF 126 and Prochloraz are composite tests the rice blast toxicity test
Subjects: rice blast fungus (pick up from the field and through separation and purification)
Test method: pot-culture method.Choose the consistent paddy rice seedling in tri-leaf period of growth potential, every basin 2 young plants, 5 basins are selected in each processing for use.Pyricularia oryzae is cultivated on tomato juice oat agar medium; Wash spore with sterile water after producing spore; Be made into the spore suspension of 1 * 105 spore/ml after double gauze filters, spray inoculation is in supplying on the examination rice seedling equably, puts black plastic sack after the inoculation and preserves moisture and cultivate 24h.Behind the inoculation 24h; Carry out chemicals treatment, each medicament is provided with about 25 ℃, cultivate under the condition of relative moisture >=90%, behind the 7d according to the incidence of the whole strain blade of morbidity grade scale investigation of rice blast; As the standard medicament, calculate disease index and control efficiency with SSF 126.
Control efficiency is converted into probability value (y), and soup is done height (μ g/ml) and is converted logarithm value (x) to, calculates concentration EC50 in virulence equation and the inhibition with method of least squares, calculates the toxicity index level co-toxicity coefficient (CTC) of medicament according to the abundant method of Sun Yun.Toxicity test result sees table 1.
Actual measurement toxicity index (ATI)=(standard medicament EC50/ supplies reagent agent EC50) * 100
The percentage composition of B in percentage composition+B medicament toxicity index * mixture of A in theoretical toxicity index (TTI)=A medicament toxicity index * mixture
Co-toxicity coefficient (CTC)=[mixture actual measurement toxicity index (the ATI)/theoretical toxicity index (TTI) of mixture] * 100
CTC≤80, the composition performance is antagonism, 80<CTC<120, the composition performance is summation action, CTC>=120, the composition performance is synergistic effect.
The composite toxicity test interpretation of result of the different proportionings of table 1 SSF 126 to rice blast with Prochloraz
The medicament title |
EC
50(μg/ml)
|
ATI |
TTI |
Co-toxicity coefficient (CTC) |
SSF 126 |
6.25 |
100.00 |
/ |
/ |
Prochloraz |
7.41 |
84.34 |
/ |
/ |
Proportioning SSF 126: Prochloraz=50: 1 |
2.7633 |
226.18 |
98.69 |
229.18 |
Proportioning SSF 126: Prochloraz=30: 1 |
2.4731 |
252.72 |
99.53 |
253.91 |
Proportioning SSF 126: Prochloraz=10: 1 |
2.2819 |
273.89 |
98.49 |
278.09 |
Proportioning SSF 126: Prochloraz=1: 1 |
2.1856 |
285.96 |
92.17 |
310.25 |
Proportioning SSF 126: Prochloraz=1: 10 |
2.7526 |
227.06 |
94.82 |
239.46 |
Proportioning SSF 126: Prochloraz=1: 30 |
3.2025 |
195.16 |
84.81 |
230.11 |
Proportioning SSF 126: Prochloraz=1: 50 |
3.4132 |
183.11 |
84.65 |
216.32 |
Result's (table 1) shows, SSF 126 and Prochloraz are between proportioning 50: 1~1: 50 (being ratio 50~0.02), and co-toxicity coefficient explains that all more than 200 the composite control to rice blast of SSF 126 and Prochloraz has significant synergies.
(2) field control effectiveness test
1, adopt the method for parallel test to verify SSF 126 and the composite field control effect of Prochloraz to rice blast.
(1) test place: test arrangement is paddy field on abutment farm, east, Dafeng City, and the plot is smooth, and rice blast morbidity throughout the year is heavier, and rice seedling is in tillering stage;
(2) test method: at the initial stage of a disease, carry out the spraying first time immediately, carry out the dispenser second time after 7 days, each handles 4 sub-districts, each sub-district 20 square meter.Before medicine with medicine for the second time after 10 days investigation statistics incidences, 5 random sampling in each sub-district, every some investigation 5 strain paddy rice, disease index and control efficiency are calculated in the lesion area of every blade accounts for blade area on the whole strain paddy rice of investigation percentage and classification.
Expection preventive effect (%)=X+Y-XY/100 (wherein, X, Y are single agent preventive effect)
Grade scale:
0 grade: no scab;
1 grade: leaf spot lesion is less than 5, and length is less than 1cm;
3 grades: leaf spot lesion 6-10, part scab length is greater than 1cm;
5 grades: leaf spot lesion 11-25, the part scab is linked to be sheet, and lesion area accounts for the 10-25% of leaf area;
7 grades: leaf spot lesion is more than 26, and scab is linked to be sheet, and lesion area accounts for the 26-50% of leaf area;
9 grades: scab is linked to be sheet, lesion area account for leaf area more than 50% or full leaf withered.
The composite field efficiency test result of table 3 SSF 126 and Prochloraz to rice blast
Measure result's (table 3) and show, SSF 126 and Prochloraz are composite obviously to be improved the preventive effect of preventing and treating rice blast, explains that the two compositely has significant synergistic effect to rice blast.