CN104542624B - A kind of complex composition containing methylsulfonyl bacterium azoles and preparation - Google Patents
A kind of complex composition containing methylsulfonyl bacterium azoles and preparation Download PDFInfo
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Abstract
The open a kind of complex composition of the present invention and preparation thereof; this complex composition contains two kinds of active component; the first active component is methylsulfonyl bacterium azoles; second active ingredient is selected from any one in fosthiazate, avilamycin, the methaldehyde; wherein the chemical name of methylsulfonyl bacterium azoles is 2 (to fluorophenyl) 5 mesyl 1; 3,4 diazole.Complex composition and preparation thereof that the present invention provides have obvious synergistic function relative to single dose, and controlling crop diseases and insect pests not only increases prevention effect, also reduces the usage amount of pesticide; reduce cost; lasting period is long, decreases times for spraying, beneficially the protection of environment.
Description
Technical field
The present invention relates to technical field of pesticide, particularly relate to a kind of complex composition containing methylsulfonyl bacterium azoles and preparation thereof.
Background technology
Known to fosthiazate, chemical name is O-ethyl-S-sec-butyl-2-oxo-1,3-thiazoles alkane-3-base phosphonothiolic acid
Ester, chemical molecular formula: C9H18NO3PS2, molecular weight: 283.3.
Avilamycin (abamectin) is known, and No. CA is 71751-41-2, is a kind of agricultural or beast being widely used
Use Insecticidal and acaricidal agent.
The methaldehyde (metaldehyde), CA registration number: 108-62-3, chemical name is 2,4,6,8-tetramethyl-1,3,
5,7-tetra-epoxide cyclooctane, its chemical formula is C8H16O4.The methaldehyde is the molluscicide that a kind of selectivity is strong, is a kind of stomach toxicity
Agent, has certain attracting action to Pomacea canaliculata, and plant does not absorb this medicine, thus without at plant interior accumulation, in people and animals
Deng poison, it is mainly used in preventing and treating Mollusca, such as Limax, Pomacea canaliculata etc. on crop.
Owing to fosthiazate, avilamycin, the methaldehyde use the time long, insect has produced certain resisting to these three medicament
The property of medicine, preventive effect declines, and the preventing and treating spectrum of above-mentioned three kinds of medicaments is narrow, limits the range of these medicaments.Secondly, crops are sending out
While endophytic bacteria sexually transmitted disease (STD) evil, it is also possible to can be caused harm by some insects.Therefore, in the urgent need to exploitation a kind of wide spectrum, height
The complex composition of effect.
To this end, Guizhou University's independent research have new type bactericide " the one class preventing and control crop antibacterial of independent intellectual property rights
The diazole sulfone compound (Patent No. ZL201110314246.2) of disease ", its structural formula is:
The step of preparation process of this compound and condition:
(1) preparation of different replacing acid methyl ester intermediate: with different organic acid and absolute methanol as raw material, at concentrated sulphuric acid
Lower back flow reaction 6-10 hour of catalysis, reduce pressure separating methanol, and after saturated sodium bicarbonate aqueous solution adjusts ph=7, separatory obtains different first
Acid methyl ester；
(2) preparation of different substituted formylhydrazine intermediate: be dissolved in methanol with different methyl formates, the most slowly add
40%-80% hydrazine hydrate, till back flow reaction is complete, separates out different substituted formylhydrazine after cooling；
(3) 2-sulfydryl-5-replaces the preparation of-1,3,4-diazole intermediate: with the formylhydrazine of above-mentioned preparation and KOH, two
Nitric sulfid is raw material, and ethanol is solvent, and back flow reaction is complete, de-ethanol, adjusts PH=5 to obtain 2-sulfydryl-5-and replaces-1,3,4-
Diazole；
(4) 2-thioether-5-replaces the preparation of-1,3,4-diazole intermediate: replace-1,3,4-with above-mentioned 2-sulfydryl-5-
Diazole is raw material, after hydro-oxidation sodium water dissolution, is reacted by dimethyl sulfate (second) ester or the halogenated hydrocarbons etc. of mole with 1-2
To corresponding sulfide compound；
(5) 2-methyl (ethyl) sulfonyl-5-replaces the preparation of-1,3,4-diazole.
With corresponding thioether as raw material, it is dissolved in glacial acetic acid, 2%-7% potassium permanganate solution or 30% hydrogen peroxide
Oxidation obtains corresponding sulfone compound.
Summary of the invention
For diazole sulfone compound, applicant researches and develops further, as Rn fluorine in halogen atom, R2Select C1-C5
The methyl of alkyl i.e. obtains the structural formula of diazole sulfone compound:
Its chemical name is 2-(to fluorophenyl)-5-mesyl-1,3,4-diazole, is called for short methylsulfonyl bacterium azoles.
The concrete syntheti c route of compound methylsulfonyl bacterium azoles is as follows:
(1) synthesis to fluorobenzoyl hydrazine
(2) the 2-sulfydryl-5-synthesis to fluorophenyl-1,3,4-diazole
(3) the 2-Dimethyl sulfide-5-synthesis to fluorophenyl-1,3,4-diazole
(4) 2-(to fluorophenyl)-5-mesyl-1,3,4-diazole target compound is prepared
Applicant further study show that, methylsulfonyl bacterium azoles is the preventing and treating bacterial disease medicament of novel structure, can pass through
Suppression pathogen energy synthesis, the growth of suppression antibacterial and breeding.Methylsulfonyl bacterium azoles has the feature of interior suction, conduction, penetrates into leaf
After sheet epidermis, energy transporting is to other positions of same blade.Substantial amounts of isolated test shows, methylsulfonyl bacterium azoles is thin to causing plant
The various pathogenetic bacterias of fungus diseases have good inhibiting effect, the most directly suppress bacterial multiplication.Through repeatedly pot experiment and field
Between the test of pesticide effectiveness checking, show that methylsulfonyl bacterium azoles is respectively provided with preferable prevention effect to crop bacterial disease, especially to Oryza sativa L.
Bacterial leaf-blight, slice disease, tobacco bacterial wilt, bacterial wilt of tomato, citrus bacterial canker disease etc. all have good control effect, and energy one
Determine in degree, to stimulate plant growth healthy and strong, improve the resistance of crop.This compound has efficiently, wide spectrum, use safety spy
Point, is an antibacterial having much exploitation potential quality.
Find through test, methylsulfonyl bacterium azoles and fosthiazate, avilamycin or methaldehyde mixture preventing and treating bacterial disease effect
Fruit is the most prominent.Methylsulfonyl bacterium azoles is different with the mechanism of action of fosthiazate, avilamycin or the methaldehyde, the two compounding application
Decrease every mu of dosage used and spraying times, can preferably ensure the safety in production of agricultural and protect ecology
Environment.
In view of this, the deficiency existed for prior art, it is an object of the invention to provide a kind of bacterium azoles Han methylsulfonyl
Complex composition and preparation, this complex composition and preparation thereof relative to single dose, there is obvious synergistic function, use
Not only increase prevention effect in preventing and treating diseases and pests of agronomic crop, also reduce the usage amount of pesticide, reduce cost accounting, simultaneously
Also delay the pest and disease damage Drug resistance to each single dose.
For realizing the purpose of the present invention, the technical scheme is that
Thering is provided a kind of complex composition containing methylsulfonyl bacterium azoles, this complex composition contains two kinds of active component, the first
Active component is methylsulfonyl bacterium azoles, and second active ingredient is selected from any one in fosthiazate, avilamycin, the methaldehyde,
Wherein the chemical name of methylsulfonyl bacterium azoles is 2-(to fluorophenyl)-5-mesyl-1,3,4-diazole.
The above-described complex composition containing methylsulfonyl bacterium azoles, it is preferable that when second active ingredient is selected from fosthiazate
Time, described methylsulfonyl bacterium azoles is 1:1 to 1:100 with the weight ratio of fosthiazate；When second active ingredient is selected from avilamycin,
Described methylsulfonyl bacterium azoles is 500:1 to 1:100 with the weight ratio of avilamycin；When second active ingredient is selected from the methaldehyde
Time, the weight ratio of described methylsulfonyl bacterium azoles and the methaldehyde is 10:1 to 1:100.
The above-described complex composition containing methylsulfonyl bacterium azoles, it is highly preferred that when second active ingredient is selected from thiazole
During phosphine, described methylsulfonyl bacterium azoles is 1:4 to 1:30 with the weight ratio of fosthiazate；When second active ingredient is selected from avilamycin
Time, described methylsulfonyl bacterium azoles is 100:1 to 1:20 with the weight ratio of avilamycin；When second active ingredient is selected from the methaldehyde
Time, the weight ratio of described methylsulfonyl bacterium azoles and the methaldehyde is 2:1 to 1:20.
The present invention also provides for a kind of pesticidal preparations containing methylsulfonyl bacterium azoles, and this pesticidal preparations includes above-mentioned complex composition
The acceptable adjuvant with on pesticide, is then prepared as pesticidal preparations.
The above-described pesticidal preparations containing methylsulfonyl bacterium azoles, it is preferable that by weight, above-mentioned complex composition accounts for above-mentioned
The weight percentage of pesticidal preparations is 0.1%-90%.
The above-described pesticidal preparations containing methylsulfonyl bacterium azoles, by weight, above-mentioned complex composition accounts for above-mentioned pesticide system
The weight percentage of agent more preferably 1%-80%.
The above-described pesticidal preparations containing methylsulfonyl bacterium azoles, on described pesticide, acceptable adjuvant is filler and auxiliary agent
Mixture.
The above-described pesticidal preparations containing methylsulfonyl bacterium azoles, described auxiliary agent includes emulsifying agent, wetting agent, dispersant.
Add other conventional functionality auxiliary agents such as antifreeze, thickening agent, stabilizer, defoamer, disintegrating agent if desired.
Emulsifying agent includes T-20, T-40, T-60, T-80, T-85 selected from polyoxyethylene sorbitan fatty acid ester series,
Fatty alcohol-polyoxyethylene ether series includes that AEO-9, OS-15, JFC, condensation compound of alkyl phenol and epoxy ethane OP series include OP-
10, OP-15, OP-18, OP-20, NPE series includes NP-10, NP-15, NP-18, NP-20, styryl
Phenol formaldehyde resin polyether series include 33#, 34#, 36#, 37#, triphen ethyl phenol polyoxyethylene ether series include 601#,
602#, 603#, double phenethyl phenol polyethenoxy ether series include that 604#, 605#, 606#, calcium dodecyl benzene sulfonate (are called for short
One or more in 500#).
Wetting agent includes lauryl alcohol polyethylene glycol oxide base ether, sodium lauryl sulphate, dodecylbenzene sodium sulfonate, fatty acid amide
N-metilsulfate, base sodium naphthalene sulfonate, sodium laurylsulfate, sodium butylnaphthalenesulfonate.
Dispersant includes diisobutyl LOMAR PWA EINECS 246-676-2 (abbreviation pulls open powder), di-2-ethylhexylphosphine oxide bitter edible plant sodium sulfonate (being called for short NNO), acrylic acid
With propionic acid amide. copolymer (being called for short DA), dispersing agent MF (being called for short MF), sodium polyacrylate (being called for short DC), desaccharide also
The sodium lignin sulfonate (being called for short M-9) of classification, the sodium lignin sulfonate (being called for short M-10) of condensation and modification, lignosulfonates (letter
Claim M-11), poly carboxylic acid derivative's (be called for short CF), sodium lignin sulfonate (being called for short M-14)
Thickening agent includes arabic gum, gelatin, polyvinylpyrrolidone, xanthan gum, aluminium-magnesium silicate, polyvinyl alcohol and poly-vinegar
Vinyl acetate.
Antifreezing agent includes glycerol, propylene glycol, ethylene glycol, isopropanol, carbamide.
Film former includes hydroxypropyl cellulose, methylcellulose, sodium polyacrylate, polyacrylamide, pectin.
Disintegrating agent includes sodium chloride, ammonium chloride, sodium sulfate, ammonium sulfate.
Filler include white carbon, Kaolin, potter's clay, bentonite, kieselguhr, attapulgite, earth powder, clay, river sand or
Carbamide.
Solvent includes Ketohexamethylene, Eucalyptus oil, toluene, dimethylbenzene, trimethylbenzene, dimethylformamide, dimethyl sulfoxide, N methyl
Ketopyrrolidine, glycol dimethyl ether, ethanol, methanol, solvent naphtha, Oleum Terebinthinae, Oleum Ricini or methyl naphthalene.
The above-described pesticidal preparations containing methylsulfonyl bacterium azoles, the pesticidal preparations that the present invention provides can be configured to wettable powder
Agent, water dispersible granules, microemulsion, aqueous emulsion, ultra low volume liquids, suspending agent, suspension emulsion, soluble liquid, soluble powder,
Seed dressing, seed coat agent, dry suspending agent, granule, cream and other dosage form being agriculturally suitable for.
In some embodiments that the present invention provides, the dosage form of pesticidal preparations of the present invention is preferably wettable powder, water-dispersible
Granule, suspending agent, microemulsion, aqueous emulsion, cream, seed coat agent or granule.
The present invention is mixed by methylsulfonyl bacterium azoles and any one in fosthiazate, avilamycin, the methaldehyde
Manufacture into preparation, mainly with bacterial disease and nematicide or demodicid mite class, Limax etc. as controlling object, for Oryza sativa L., melon, solanberry
Class, beans and Caulis et Folium Lactucae sativae, Chinese cabbage etc. crops.
More specifically, the compound pesticide composition that the present invention provides, when active component is methylsulfonyl bacterium azoles and fosthiazate,
It is mainly used in preventing and treating following bacterial disease and nematodiasis: Cucumber wilt and root knot nematode disease, bacterial wilt of tomato and root knot
Nematicide, pepper ralstonia solanacearum and root knot nematode disease, bacterial wilt of peanut and root knot nematode disease, tobacco bacterial wilt and root knot nematode disease,
Soft rot of cabbage and root knot nematode disease, Caulis et Folium Lactucae sativae bacterial leaf spot and root knot nematode disease, bacterial blight of rice and bacterial stripe
Disease and Oryza sativa L. nematicide.
When active component is methylsulfonyl bacterium azoles and avilamycin, it is mainly used in preventing and treating following bacterial disease, nematicide
Evil and demodicid mite class: Cucumber wilt and root knot nematode disease, bacterial wilt of tomato and root knot nematode disease, pepper ralstonia solanacearum and root-knot nematode
Disease, bacterial wilt of peanut and root knot nematode disease, tobacco bacterial wilt and root knot nematode disease, soft rot of cabbage and root knot nematode disease, Caulis et Folium Lactucae sativae
Bacterial leaf spot and root knot nematode disease, bacterial blight of rice and bacterial stripe and Oryza sativa L. nematicide, citrus bacterial canker disease
And citrus red mite, Fructus Mangifera Indicae bacterial leaf spot and red spider, cucumber bacterial angular leaf spot and tetranychid.
When active component is methylsulfonyl bacterium azoles and the methaldehyde, it is mainly used in preventing and treating following bacterial disease and Limax:
Soft rot of crucifers and Limax, paddy bacterial root rot and Pomacea canaliculata, peach bacterial shot hole and Limax, Fructus Cucumidis sativi are thin
Bacterium property angular leaf spot and Limax.
In the middle of some embodiments of the present invention, methylsulfonyl bacterium azoles and fosthiazate compound, and preventing and treating bacterial wilt of peanut, Chinese cabbage are soft
Maize ear rot, tomato root-knot eelworm, Fructus Cucumidis sativi root-knot nematode；Methylsulfonyl bacterium azoles and abamectin compounded, preventing and treating citrus bacterial canker disease, Semen arachidis hypogaeae are blue or green
Rot, citrus red mite, peanut root-knot nematode；Methylsulfonyl bacterium azoles and the methaldehyde compound, and control of plant bacterial wilt, Chinese cabbage are soft
Maize ear rot, brassicaceous vegetable Limax.
Complex composition and preparation thereof that the present invention provides have the advantages that relative to prior art
Complex composition and preparation thereof that the present invention provides have obvious synergistic function relative to single dose, in preventing and treating
During pest and disease damage, not only increase prevention effect, also reduce the usage amount of pesticide, reduce cost.The most also delay pest and disease damage
Drug resistance to each single dose.
Detailed description of the invention
Below by embodiment, the invention will be further described.It should be understood that and prepare described in the embodiment of the present invention
Method is only used for the present invention rather than limitation of the present invention being described, to system of the present invention under the concept thereof of the present invention
The simple modifications of Preparation Method broadly falls into the scope of protection of present invention.The methylsulfonyl former medicine of bacterium azoles used in the present invention is by Guizhou
University provides, and other former medicine used and preparation are commercial.
Embodiment prepared by preparation
One, the preparation of water dispersible granules
Preparation technology: by active component, wetting agent, dispersant, white carbon, filler mix homogeneously, through jet mill powder
After broken, stirring 30min, through mediating, rear addition carries out pelletize, is dried, obtains agriculture of the present invention in fluidized-bed granulation dryer
The water dispersible granules of medicine preparation.
Water dispersible granules containing methylsulfonyl bacterium azoles Yu lythidathion
Water dispersible granules containing methylsulfonyl bacterium azoles Yu avilamycin
Water dispersible granules containing methylsulfonyl bacterium azoles Yu the methaldehyde
Two, the preparation of microemulsion
Preparation technology: added by active component in solvent, obtains transparent mixed liquor after stirring；To above-mentioned mixed liquor
Middle addition emulsifying agent, stirring is completely dissolved to it；Under the mixing speed of 50r/min, the water of surplus is joined above-mentioned dissolving
Have in the mixed liquor of emulsifying agent, at ambient temperature, stir 30min, obtain the microemulsion of homogeneous transparent；In above-mentioned microemulsion
Add antifreezing agent, stir, obtain the microemulsion of pesticidal preparations of the present invention.Formula forms:
Microemulsion containing methylsulfonyl bacterium azoles Yu avilamycin
Microemulsion containing methylsulfonyl bacterium azoles Yu lythidathion
Microemulsion containing methylsulfonyl bacterium azoles Yu the methaldehyde
Three, the preparation of wettable powder
Preparation technology: by active component, wetting agent, dispersant, filler mix homogeneously, after jet mill is pulverized, stir
Mix 30min, obtain the wettable powder of pesticidal preparations of the present invention.
Wettable powder containing methylsulfonyl bacterium azoles Yu avilamycin
Wettable powder containing methylsulfonyl bacterium azoles Yu lythidathion
Wettable powder containing methylsulfonyl bacterium azoles Yu the methaldehyde
Four, the preparation of suspending agent
Preparation technology: by emulsifying agent, antifreezing agent, thickening agent, moisture content mixing, through high speed shear mix homogeneously, be sequentially added into
Active component, abrading-ball 2～3 hours in ball crusher, prepare the suspending agent of pesticidal preparations of the present invention.
Suspending agent containing methylsulfonyl bacterium azoles Yu lythidathion
Suspending agent containing methylsulfonyl bacterium azoles Yu avilamycin
Suspending agent containing methylsulfonyl bacterium azoles Yu the methaldehyde
Five, the preparation of aqueous emulsion
Preparation technology: by active component, emulsifying agent, solvent mixing, be dissolved into uniform oil phase；By part water, antifreezing agent
Mix uniformly aqueous phase；While high-speed stirred, oil phase is added aqueous phase in a kettle., opens cutter and carry out
High speed shear, and add remaining water and supply, shear about half an hour, form aqueous emulsion.I.e. prepare the water and milk of described pesticidal preparations
Agent.
Aqueous emulsion containing methylsulfonyl bacterium azoles Yu lythidathion
Aqueous emulsion containing methylsulfonyl bacterium azoles Yu the methaldehyde
Aqueous emulsion containing methylsulfonyl bacterium azoles Yu avilamycin
Six, the preparation of cream
Preparation technology: active component is added and obtains transparent mixing after stirring in the mixed liquor of solvent and emulsifying agent
Liquid, i.e. prepares the cream of described pesticidal preparations
Cream containing methylsulfonyl bacterium azoles Yu avilamycin
Cream containing methylsulfonyl bacterium azoles Yu the methaldehyde
Seven, suspension seed-coating agent
By active component through comminution by gas stream, adding assistant (including wetting dispersing agent, emulsifying agent), film former, thickening agent, anti-
After freezing after agent is thoroughly mixed with water, put into sand mill in proportion and grind 2 times, until it is 2-3 that the fineness of the particles of suspension reaches D50
μm, D90 ＜ 8 μm, obtain the suspension seed-coating agent of pesticidal preparations of the present invention.
Suspension seed-coating agent containing methylsulfonyl bacterium azoles Yu avilamycin
Suspension seed-coating agent containing methylsulfonyl bacterium azoles Yu the methaldehyde
Suspension seed-coating agent containing methylsulfonyl bacterium azoles Yu lythidathion
Eight granules
Preparation technology: by active component, auxiliary agent (including wetting dispersing agent, emulsifying agent), disintegrating agent, filler mix homogeneously,
Pulverize, stir after adding water-wet, then use screw extruder pelletizer pelletize, sieve after drying, obtain of the present invention
The granule of pesticidal preparations.
Granule containing methylsulfonyl bacterium azoles Yu avilamycin
| Embodiment | Methylsulfonyl bacterium azoles | Avilamycin | Auxiliary agent | Disintegrating agent | Filler |
| 86 | 0.09g | 0.01g | Pull open powder 1g | Ammonium sulfate 10g | 100g supplied by carbamide |
| 87 | 0.25 | 0.75g | NNO is 2g | Ammonium chloride 10g | 100g supplied by carbamide |
| 88 | 2.5g | 2.5g | DC is 1g | Sodium sulfate 10g | River sand supplies 100g |
| 89 | 0.5g | 10g | M-14 is 3g | Sodium chloride 10g | Bentonite supplies 100g |
| 90 | 0.1g | 10g | CF5g | Ammonium sulfate 10g | Clay supplies 100g |
Granule containing methylsulfonyl bacterium azoles Yu lythidathion
| Embodiment | Methylsulfonyl bacterium azoles | Lythidathion | Auxiliary agent | Disintegrating agent | Filler |
| 91 | 0.1g | 0.9g | MF is 3g | Ammonium sulfate 15g | 100g supplied by carbamide |
| 92 | 1g | 10g | NNO is 3g | Ammonium chloride 12g | Potter's clay supplies 100g |
| 93 | 1g | 4g | DA is 3g | Ammonium sulfate 10g | Kaolin supplies 100g |
Granule containing methylsulfonyl bacterium azoles Yu the methaldehyde
| Embodiment | Methylsulfonyl bacterium azoles | The methaldehyde | Auxiliary agent | Disintegrating agent | Filler |
| 94 | 0.1g | 10g | NP-10 is 4g | Ammonium sulfate 15g | Kieselguhr supplies 100g |
| 95 | 0.2g | 0.4g | OP-10 is 4g | Sodium sulfate 10g | 100g supplied by carbamide |
| 96 | 1g | 9g | T-80 is 4g | Sodium chloride 15g | Kaolin supplies 100g |
| 97 | 1g | 3g | T-60 is 4g | Ammonium chloride 10g | River sand supplies 100g |
Pesticidal preparations of the present invention is in addition to can being made into above dosage form, it is also possible to make micro-capsule suspension, injection drying agent, ultralow
The multiple dosage form such as volume liquids.
BIOLOGICAL ACTIVITY EXAMPLES
For the design of the present invention, methylsulfonyl bacterium azoles is combined by inventor herein with the indoor of fosthiazate complex composition
Virulence and field efficacy have carried out detailed test and checking.
Toxicity Determination:
Whether there are potentiation and potentiation the most notable in order to clear and definite methylsulfonyl bacterium azoles and fosthiazate compound, invention
People has carried out substantial amounts of indoor joint toxicity measuring and screening, and result draws, in certain ratio range, methylsulfonyl bacterium azoles and
Fosthiazate is compounding all has potentiation to bacterial disease and nematicide, in preferred ratio range, and potentiation highly significant, under
Face illustrates this conclusion with several concrete Toxicity Determination embodiments.
The test of following indoor biometrics uses the abundant method of Sun Yun to calculate co-toxicity coefficient (CTC) and evaluates mixed effect.
A. toxicity index (ATI)=(standard agent EC is surveyed50/ reagent agent EC50)×100
B. toxicity index (ATI)=(standard agent LC is surveyed50/ reagent agent LC50)×100
Note: when carrying out indoor bioassay as antibacterial, actual measurement toxicity index a formula calculates；Enter as insecticide
Row room
During interior bioassay, actual measurement toxicity index b formula calculates.
Theoretical toxicity index (TTI)=A medicament ATI × A medicament percentage composition+B medicament ATI × B medicament in mixture
Percentage composition in mixture
Co-toxicity coefficient (CTC)=[mixture actual measurement toxicity index (ATI)/mixture theory toxicity index (TTI)] × 100
The co-toxicity coefficient (CTC) >=120 of built agent shows as potentiation；CTC≤80 show as antagonism；80 ＜
CTC ＜ 120 shows as summation action.
Toxicity Determination embodiment one: the Toxicity Determination test of preventing and treating bacterial wilt of peanut
Test method: after being activated in NA culture medium by bacterial wilt of peanut pathogen, be made into bacterium stock solution with sterilized water, by bacterium
The clump count that stock solution grows after being diluted to coated plate 100ul is the bacteria suspension of about 100, standby.
Take 400ul bacteria suspension to mix with equivalent pesticide single dose, take 100ul with liquid-transfering gun, be placed in the NA flat board being ready for
On, with sterilized " L " shape Glass rod by bacteria suspension coating uniformly, cultivate 48h for 28 DEG C, count clump count, and press formula calculating
Bacteriostasis rate, bacterium colony suppression ratio (%)=(comparison clump count-process clump count)/comparison clump count × 100, often process repetition 4
Secondary, replace pesticide-treated for comparison with sterilized water, the result of gained uses Excel software analysis, calculates the EC of each medicament50, and
Co-toxicity coefficient is calculated according to the abundant method of Sun Yun.Measurement result is shown in Table 1, table 2:
Table 1 methylsulfonyl bacterium azoles and fosthiazate compound the joint toxicity measuring result of preventing and treating bacterial wilt of peanut
| Composition | EC50(μg/ml) | ATI | TTI | CTC |
| Methylsulfonyl bacterium azoles (A) | 15.46 | 100.00 | / | / |
| Fosthiazate (B) | 78.43 | 19.71 | / | / |
| A:B=2:1 | 19.37 | 79.81 | 73.24 | 108.98 |
| A:B=1:1 | 20.17 | 76.65 | 59.86 | 128.05 |
| A:B=1:2 | 23.38 | 66.12 | 46.47 | 142.28 |
| A:B=1:4 | 26.17 | 59.08 | 35.77 | 165.16 |
| A:B=1:6 | 27.39 | 56.44 | 31.18 | 181.02 |
| A:B=1:9 | 27.26 | 56.71 | 27.74 | 204.44 |
| A:B=1:13 | 30.22 | 51.16 | 25.45 | 201.04 |
| A:B=1:18 | 33.91 | 45.59 | 23.94 | 190.46 |
| A:B=1:24 | 37.63 | 41.08 | 22.92 | 179.22 |
| A:B=1:30 | 41.97 | 36.84 | 22.30 | 165.17 |
| A:B=1:38 | 45.25 | 34.17 | 21.77 | 156.94 |
| A:B=1:48 | 49.21 | 31.42 | 21.35 | 147.15 |
| A:B=1:60 | 52.89 | 29.23 | 21.03 | 139.01 |
| A:B=1:74 | 55.57 | 27.82 | 20.78 | 133.87 |
| A:B=1:88 | 58.18 | 26.57 | 20.61 | 128.91 |
| A:B=1:100 | 61.93 | 24.96 | 20.51 | 121.73 |
| A:B=1:105 | 65.25 | 23.69 | 20.47 | 115.75 |
From toxicity test result table 1, methylsulfonyl bacterium azoles and fosthiazate be compounding preventing and treating in the range of 1:1 to 1:100
The co-toxicity coefficient of bacterial wilt of peanut all reaches more than 120, shows obvious synergistic function.Particularly, at 1:4 to 1～30
In the range of co-toxicity coefficient more than 160, potentiation is especially pronounced.
Table 2 methylsulfonyl bacterium azoles and the joint toxicity measuring result of abamectin compounded preventing and treating bacterial wilt of peanut
| Composition | EC50(μg/ml) | ATI | TTI | CTC |
| Methylsulfonyl bacterium azoles (A) | 15.97 | 100.00 | / | / |
| Avilamycin (C) | 66.40 | 24.05 | / | / |
| A:C=500:1 | 13.28 | 120.26 | 99.85 | 120.44 |
| A:C=350:1 | 12.58 | 126.95 | 99.78 | 127.22 |
| A:C=250:1 | 11.83 | 135.00 | 99.70 | 135.41 |
| A:C=150:1 | 11.25 | 141.96 | 99.50 | 142.67 |
| A:C=100:1 | 10.63 | 150.24 | 99.25 | 151.37 |
| A:C=85:1 | 10.04 | 159.06 | 99.12 | 160.48 |
| A:C=65:1 | 9.36 | 170.62 | 98.85 | 172.61 |
| A:C=45:1 | 8.90 | 179.44 | 98.35 | 182.45 |
| A:C=25:1 | 8.45 | 188.99 | 97.08 | 194.68 |
| A:C=1:1 | 13.73 | 116.31 | 62.03 | 187.53 |
| A:C=1:4 | 23.11 | 69.10 | 39.24 | 176.10 |
| A:C=1:9 | 30.26 | 52.78 | 31.65 | 166.77 |
| A:C=1:13 | 34.45 | 46.36 | 29.48 | 157.27 |
| A:C=1:20 | 38.39 | 41.60 | 27.67 | 150.35 |
| A:C=1:45 | 43.15 | 37.01 | 25.70 | 144.00 |
| A:C=1:65 | 46.70 | 34.20 | 25.20 | 135.69 |
| A:C=1:85 | 49.87 | 32.02 | 24.93 | 128.43 |
| A:C=1:100 | 53.58 | 29.81 | 24.80 | 120.17 |
From toxicity test result table 2, methylsulfonyl bacterium azoles and avilamycin are compounding in the range of 500:1 to 1:100
The co-toxicity coefficient of preventing and treating bacterial wilt of peanut all reaches more than 120, shows obvious synergistic function.Particularly, at 100:1 extremely
In the range of 1:20, co-toxicity coefficient is more than 150, and potentiation is especially pronounced.
Toxicity Determination embodiment two: prevent and treat the Toxicity Determination test of soft rot of cabbage
Test method: strain cultured in test tube is extracted test tube tampon at alcohol burner, pours 10ml sterilized water into,
With disinfection inoculation pin, pathogenic bacteria on inclined-plane is scraped gently, make spore suspension, then this spore suspension is poured in advance equipped with several
In the sterilizing triangular flask of glass bead, filter bacterium solution with sterile gauze after shake 5min, put in another sterilizing triangular flask, i.e. make institute
Need bacterium solution.
By beef extract-peptone agar culture medium melt, when being cooled to 45 DEG C～50 DEG C, aseptically together with
0.2ml bacterial suspension is poured into the most rapidly in sterilizing culture dish, every ware 15ml culture medium, shakes up rear cooled and solidified.Use sterilizing
After card punch (aperture 4mm) punching, 1ml medicinal liquid is dripped in circular hole, be placed in 28 DEG C of calorstats cultivation 2d after, use vernier calliper
Chi is pressed decussation method and is measured 2 diameters of inhibition zone, averages, and calculates suppression ratio, obtains virulence curve and EC50, and press
The abundant method of Sun Yun calculates co-toxicity coefficient.The results are shown in Table 3, table 4:
Table 3 methylsulfonyl bacterium azoles and fosthiazate compound the joint toxicity measuring result preventing and treating soft rot of cabbage
| Composition | EC50(μg/ml) | ATI | TTI | CTC |
| Methylsulfonyl bacterium azoles (A) | 13.78 | 100.00 | / | / |
| Fosthiazate (B) | 85.82 | 16.06 | / | / |
| A:B=2:1 | 17.83 | 77.29 | 72.02 | 107.31 |
| A:B=1:1 | 19.12 | 72.07 | 58.03 | 124.20 |
| A:B=1:3 | 24.83 | 55.50 | 37.04 | 149.82 |
| A:B=1:4 | 25.96 | 53.08 | 32.85 | 161.61 |
| A:B=1:7 | 28.47 | 48.40 | 26.55 | 182.31 |
| A:B=1:10 | 27.83 | 49.51 | 23.69 | 209.03 |
| A:B=1:14 | 32.18 | 42.82 | 21.65 | 197.76 |
| A:B=1:19 | 36.61 | 37.64 | 20.25 | 185.84 |
| A:B=1:24 | 41.01 | 33.60 | 19.41 | 173.07 |
| A:B=1:30 | 45.24 | 30.46 | 18.76 | 162.32 |
| A:B=1:37 | 48.38 | 28.48 | 18.27 | 155.93 |
| A:B=1:47 | 52.52 | 26.24 | 17.81 | 147.36 |
| A:B=1:58 | 54.99 | 25.06 | 17.48 | 143.36 |
| A:B=1:72 | 58.26 | 23.65 | 17.21 | 137.46 |
| A:B=1:86 | 62.01 | 22.22 | 17.02 | 130.55 |
| A:B=1:100 | 65.48 | 21.04 | 16.89 | 124.61 |
| A:B=1:105 | 69.28 | 19.89 | 16.85 | 118.05 |
From toxicity test result table 3, methylsulfonyl bacterium azoles and lythidathion be compounding preventing and treating in the range of 1:1 to 1:100
The co-toxicity coefficient of soft rot of cabbage all reaches more than 120, shows obvious synergistic function.Particularly, 1:4's to 1:30
In the range of co-toxicity coefficient more than 160, potentiation is especially pronounced.
Table 4 methylsulfonyl bacterium azoles and the methaldehyde compound the joint toxicity measuring result of preventing and treating soft rot of Chinese cabbage
| Composition | EC50(μg/ml) | ATI | TTI | CTC |
| Methylsulfonyl bacterium azoles (A) | 13.13 | 100.00 | / | / |
| The methaldehyde (D) | 195.62 | 6.71 | / | / |
| A:D=15:1 | 12.53 | 104.79 | 94.17 | 111.28 |
| A:D=10:1 | 11.94 | 109.97 | 91.52 | 120.16 |
| A:D=5:1 | 11.12 | 118.08 | 84.45 | 139.81 |
| A:D=2:1 | 12.65 | 103.79 | 68.90 | 150.64 |
| A:D=1:1 | 14.73 | 89.14 | 53.36 | 167.06 |
| A:D=1:3 | 23.55 | 55.75 | 30.03 | 185.64 |
| A:D=1:9 | 45.70 | 28.73 | 16.04 | 179.11 |
| A:D=1:14 | 60.20 | 21.81 | 12.93 | 168.67 |
| A:D=1:18 | 71.51 | 18.36 | 11.62 | 157.99 |
| A:D=1:20 | 77.23 | 17.00 | 11.15 | 152.42 |
| A:D=1:30 | 93.42 | 14.05 | 9.72 | 144.58 |
| A:D=1:60 | 122.10 | 10.75 | 8.24 | 130.48 |
| A:D=1:100 | 143.23 | 9.17 | 7.64 | 120.06 |
From toxicity test result table 4, methylsulfonyl bacterium azoles and the methaldehyde are compounding anti-in the range of 10:1 to 1:100
The co-toxicity coefficient controlling soft rot of cabbage all reaches more than 120, shows obvious synergistic function.Particularly, at 2:1 to 1:20
In the range of co-toxicity coefficient more than 150, potentiation is especially pronounced.
Toxicity Determination embodiment three: the Toxicity Determination test of preventing and treating tomato root-knot eelworm
Test method: the pieces of an egg use water of picking root-knot nematode cleans from live body host plant, is placed in the wet filter of culture dish
On paper, hatch at 20 DEG C～25 DEG C, it is thus achieved that the second instar larvae that age is consistent, with water by resuspended for nematicide floating to every milliliter >=100
Nematicide, standby.With the former medicine of acetone solution, then it is diluted to required concentration with the aqueous solution containing 0.1% Tween 80.
Process of the test: draw medicinal liquid 3ml with liquid-transfering gun and be separately added in test tube, then draws the equivalent nematicide prepared and hangs
Supernatant liquid 3ml adds in test tube, makes medicinal liquid and nematicide suspension mixed in equal amounts uniform.The above-mentioned mixed liquor of 3ml is pipetted with liquid-transfering gun
In the aperture of porous biochemical test plate, add a cover, in 25 DEG C of constant temperature culture 24h.Often process 4 times and repeat, and set without medicament
Process as blank.From each process, take 1ml mixed liquor observe nematicide death condition, every repeated measures line under solving plane mirror
Borer population is no less than 100, the bus borer population of record investigation and verge of death borer population, calculates mortality rate, makees regression analysis, calculate each medicine
The LC of agent50, and press Sun Yun abundant method calculating co-toxicity coefficient.The results are shown in Table 5:
Table 5 methylsulfonyl bacterium azoles and fosthiazate compound the joint toxicity measuring result of preventing and treating tomato root-knot eelworm
From toxicity test result table 5, methylsulfonyl bacterium azoles and lythidathion be compounding preventing and treating in the range of 1:1 to 1:100
The co-toxicity coefficient of tomato root-knot eelworm all reaches more than 120, shows obvious synergistic function.Particularly, at 1:4 to 1:30
In the range of co-toxicity coefficient more than 160, potentiation is especially pronounced.
Toxicity Determination embodiment four: the Toxicity Determination test of preventing and treating Fructus Cucumidis sativi root-knot nematode
Test prepares: from live body host plant, the pieces of an egg use water of picking root-knot nematode cleans, and is placed in the wet filter of culture dish
On paper, hatch at 20 DEG C～25 DEG C, it is thus achieved that the second instar larvae that age is consistent, with water by resuspended for nematicide floating to every milliliter >=100
Nematicide, standby.With the former medicine of acetone solution, then it is diluted to required concentration with the aqueous solution containing 0.1% Tween 80.
Process of the test: draw medicinal liquid 3ml with liquid-transfering gun and be separately added in test tube, then draws the equivalent nematicide prepared and hangs
Supernatant liquid 3ml adds in test tube, makes medicinal liquid and nematicide suspension mixed in equal amounts uniform.The above-mentioned mixed liquor of 3ml is pipetted with liquid-transfering gun
In the aperture of porous biochemical test plate, add a cover, in 25 DEG C of constant temperature culture 24h.Often process 4 times and repeat, and set without medicament
Process as blank.From each process, take 1ml mixed liquor observe nematicide death condition, every repeated measures line under solving plane mirror
Borer population is no less than 100, the bus borer population of record investigation and verge of death borer population, calculates mortality rate, makees regression analysis, calculate each medicine
The LC50 of agent, and press Sun Yun abundant method calculating co-toxicity coefficient.The results are shown in Table 6:
Table 6 methylsulfonyl bacterium azoles and fosthiazate compound the joint toxicity measuring result of preventing and treating Fructus Cucumidis sativi root-knot nematode
From toxicity test result table 6, methylsulfonyl bacterium azoles and lythidathion be compounding preventing and treating in the range of 1:1 to 1:100
The co-toxicity coefficient of Fructus Cucumidis sativi root-knot nematode all reaches more than 120, shows obvious synergistic function.Particularly, at 1:4 to 1:30
In the range of co-toxicity coefficient more than 160, potentiation is especially pronounced.
Toxicity Determination embodiment five: the Toxicity Determination test of preventing and treating citrus bacterial canker disease
Test is with reference to " pesticide bioassay technology " (the old spring edits, and publishing house of Beijing Agricultural University publishes) and " agriculture
Bioassay test criterion NY/T1156.2-2006 in coyote hole ".This test uses inhibition zone method.On aseptic operating platform, by NA
Culture medium is poured on NA flat board, and after drying, the citrus processing bacteria suspension spreading rod taking 0.1ml is applied to NA flat board equably
On.After drying, punch in flat board central authorities with the card punch of diameter 7mm, then take 100 μ l medicinal liquids in aperture.Each concentration 5
Repeat.The process of sterilized water is added as blank in aperture.The calorstat aseptic culture of 28 ± 0.5 DEG C it is placed on after process,
Take out after 2d.Use decussation method to measure the antibacterial circle diameter (in units of millimeter) of each process respectively, and calculate inhibition zone
The meansigma methods of diameter, suppression ratio.Utilize DPS data processing software to carry out statistical analysis, calculate the EC of each medicament50, then by grandson
Yun Peifa (CTC) calculates and evaluates mixed effect, uses EC50Value calculates co-toxicity coefficient.
Table 7 methylsulfonyl bacterium azoles and the joint toxicity measuring result of abamectin compounded preventing and treating citrus bacterial canker disease
| Composition | EC50(μg/ml) | ATI | TTI | CTC |
| Methylsulfonyl bacterium azoles (A) | 7.58 | 100.00 | / | / |
| Avilamycin (C) | 76.88 | 9.86 | / | / |
| A:C=500:1 | 6.21 | 122.06 | 99.82 | 122.28 |
| A:C=400:1 | 5.91 | 128.26 | 99.78 | 128.55 |
| A:C=300:1 | 5.63 | 134.64 | 99.70 | 135.04 |
| A:C=200:1 | 5.28 | 143.56 | 99.55 | 144.21 |
| A:C=100:1 | 5.06 | 149.80 | 99.11 | 151.15 |
| A:C=80:1 | 4.77 | 158.91 | 98.89 | 160.70 |
| A:C=60:1 | 4.49 | 168.82 | 98.52 | 171.35 |
| A:C=40:1 | 4.23 | 179.20 | 97.80 | 183.22 |
| A:C=20:1 | 4.08 | 185.78 | 95.71 | 194.12 |
| A:C=1:1 | 7.37 | 102.85 | 54.93 | 187.24 |
| A:C=1:5 | 17.09 | 44.35 | 24.88 | 178.25 |
| A:C=1:10 | 24.77 | 30.60 | 18.05 | 169.50 |
| A:C=1:15 | 30.49 | 24.86 | 15.49 | 160.46 |
| A:C=1:20 | 35.55 | 21.32 | 14.15 | 150.67 |
| A:C=1:40 | 44.25 | 17.13 | 12.06 | 142.06 |
| A:C=1:60 | 48.81 | 15.53 | 11.34 | 136.98 |
| A:C=1:80 | 54.01 | 14.03 | 10.97 | 127.91 |
| A:C=1:100 | 58.54 | 12.95 | 10.75 | 120.43 |
From toxicity test result table 7, methylsulfonyl bacterium azoles and avilamycin are compounding in the range of 500:1 to 1:100
The co-toxicity coefficient of citrus bacterial canker disease all reaches more than 120, shows obvious synergistic function.Particularly, at 100:1 to 1:20
In the range of co-toxicity coefficient more than 150, potentiation is especially pronounced.
Toxicity Determination embodiment six: the Toxicity Determination test of preventing and treating citrus red mite
Test method: with reference to " farm-chemical indoor determination test rule NY/T1154.12-2008 " test method.This reality
Test employing tetranychid slide infusion process.Double faced adhesive tape is cut into 2cm length, is affixed on one end of microscope slide, then choose healthy female one-tenth demodicid mite, will
Its back sticks at and (is careful not to adhere demodicid mite foot, antenna and mouthpart) on double faced adhesive tape, every 30, puts into and is lined with wet sponge container
In, close the lid, under the conditions of being placed in (25 ± 1) DEG C.Microscopy after 2h, rejects dead and injured individual, supplies every 30.Former medicine
It is configured to mother solution with organic solvent methanol, then is configured to 5～7 with the tween 80 aqueous solution of 0.1% according to the method for equal difference
Series mass concentration.Take out after microscope slide is dipped in medicinal liquid the 5s that vibrates gently, suck unnecessary medicinal liquid with absorbent paper, be placed in and be lined with
In the white disk of wet sponge, use the covered rearing with plastic film that light transmission is good.Often process 4 times and repeat, and set the process without medicament
Make blank.Process be placed on temperature be (25 ± 1) DEG C, the photoperiod be to raise and observe under L:D=(16:8) h.Place
After reason, 48h checks examination worm death condition, records total borer population and dead borer population respectively.DPS data processing software is utilized to carry out statistical
Analysis, calculates the EC of each medicament50, then calculate by the abundant method of Sun Yun (CTC) and evaluate mixed effect, use EC50Value calculates poison system altogether
Number.
Table 8 methylsulfonyl bacterium azoles and the abamectin compounded joint toxicity measuring result preventing and treating citrus red mite
From toxicity test result table 8, methylsulfonyl bacterium azoles and avilamycin are compounding in the range of 500:1 to 1:100
The co-toxicity coefficient of citrus red mite all reaches more than 120, shows obvious synergistic function.Particularly, at 100:1 to 1:20
In the range of co-toxicity coefficient more than 150, potentiation is especially pronounced.
Toxicity Determination embodiment seven: the Toxicity Determination test of preventing and treating peanut root-knot nematode
Test prepares: from live body host plant, the pieces of an egg use water of picking root-knot nematode cleans, and is placed in the wet filter of culture dish
On paper, hatch at 20 DEG C～25 DEG C, it is thus achieved that the second instar larvae that age is consistent, with water by resuspended for nematicide floating to every milliliter >=100
Nematicide, standby.With the former medicine of acetone solution, then it is diluted to required concentration with the aqueous solution containing 0.1% Tween 80.
Process of the test: draw medicinal liquid 3ml with liquid-transfering gun and be separately added in test tube, then draws the equivalent nematicide prepared and hangs
Supernatant liquid 3ml adds in test tube, makes medicinal liquid and nematicide suspension mixed in equal amounts uniform.The above-mentioned mixed liquor of 3ml is pipetted with liquid-transfering gun
In the aperture of porous biochemical test plate, add a cover, in 25 DEG C of constant temperature culture 24h.Often process 4 times and repeat, and set without medicament
Process as blank.From each process, take 1ml mixed liquor observe nematicide death condition, every repeated measures line under solving plane mirror
Borer population is no less than 100, the bus borer population of record investigation and verge of death borer population, calculates mortality rate, makees regression analysis, calculate each medicine
The LC of agent50, and press Sun Yun abundant method calculating co-toxicity coefficient.The results are shown in Table 9:
Table 9 methylsulfonyl bacterium azoles and the abamectin compounded joint toxicity measuring result preventing and treating Fructus Cucumidis sativi root-knot nematode
From toxicity test result table 9, methylsulfonyl bacterium azoles and avilamycin are compounding in the range of 500:1 to 1:100
The co-toxicity coefficient of Fructus Cucumidis sativi root-knot nematode all reaches more than 120, shows obvious synergistic function.Particularly, at 100:1 to 1:
In the range of 20, co-toxicity coefficient is more than 150, and potentiation is especially pronounced.
Toxicity Determination embodiment eight: the Toxicity Determination test of control of plant bacterial wilt
After being activated in NA culture medium by bacterial wilt of tomato pathogen, it is made into bacterium stock solution with sterilized water, bacterium stock solution is diluted
The bacteria suspension that clump count is about 100 grown after becoming coated plate 100ul, standby.
Take 400ul bacteria suspension to mix with equivalent pesticide single dose, take 100ul with liquid-transfering gun, be placed in the NA flat board being ready for
On, with sterilized " L " shape Glass rod by bacteria suspension coating uniformly, cultivate 48h for 28 DEG C, count clump count, and press formula calculating
Bacteriostasis rate, bacterium colony suppression ratio (%)=(comparison clump count-process clump count)/comparison clump count × 100, often process repetition 4
Secondary, replace pesticide-treated for comparison with sterilized water, the result of gained uses Excel software analysis, calculates the EC of each medicament50, and
Co-toxicity coefficient is calculated according to the abundant method of Sun Yun.Test result refers to table 10.
Table 10 methylsulfonyl bacterium azoles and the methaldehyde compound the joint toxicity measuring result of control of plant bacterial wilt
| Composition | EC50(μg/ml) | ATI | TTI | CTC |
| Methylsulfonyl bacterium azoles (A) | 15.37 | 100.00 | / | / |
| The methaldehyde (D) | 175.30 | 8.77 | / | / |
| A:D=20:1 | 14.27 | 107.71 | 95.66 | 112.60 |
| A:D=10:1 | 13.69 | 112.27 | 91.71 | 122.43 |
| A:D=6:1 | 12.77 | 120.36 | 86.97 | 138.40 |
| A:D=2:1 | 14.70 | 104.56 | 69.59 | 150.25 |
| A:D=1:1 | 16.34 | 94.06 | 54.38 | 172.96 |
| A:D=1:5 | 34.21 | 44.93 | 23.97 | 187.41 |
| A:D=1:10 | 49.66 | 30.95 | 17.06 | 181.40 |
| A:D=1:13 | 58.81 | 26.14 | 15.28 | 170.99 |
| A:D=1:17 | 70.43 | 21.82 | 13.84 | 157.72 |
| A:D=1:20 | 77.44 | 19.85 | 13.11 | 151.37 |
| A:D=1:40 | 107.50 | 14.30 | 10.99 | 130.06 |
| A:D=1:70 | 125.35 | 12.26 | 10.05 | 121.97 |
| A:D=1:100 | 144.33 | 10.65 | 9.67 | 110.11 |
From toxicity test result table 10, methylsulfonyl bacterium azoles and the methaldehyde are compounding in the range of 10:1 to 1:100
The co-toxicity coefficient of control of plant bacterial wilt all reaches more than 120, shows obvious synergistic function.Particularly, at 2:1 to 1:
In the range of 20, co-toxicity coefficient is more than 150, and potentiation is especially pronounced.
Toxicity Determination embodiment nine: the Toxicity Determination test of preventing and treating brassicaceous vegetable Limax
Test method: with reference to " NY/T 1154.2-2006 farm-chemical indoor determination test rule insecticide the 2nd
Point: stomach poison activity test clamp poison blade is sent out " and " NY/T 1154.7-2006 farm-chemical indoor determination test rule insecticide
7th part: the synergy of mixture measures " test result refers to table 11.
Table 11 methylsulfonyl bacterium azoles and the methaldehyde compound the joint toxicity measuring result of preventing and treating brassicaceous vegetable Limax
| Composition | LC50(μg/ml) | ATI | TTI | CTC |
| Methylsulfonyl bacterium azoles (A) | 115.43 | 100.00 | / | / |
| The methaldehyde (D) | 3.11 | 3711.58 | / | / |
| A:D=13:1 | 28.23 | 408.89 | 357.97 | 114.23 |
| A:D=10:1 | 22.43 | 514.62 | 428.33 | 120.15 |
| A:D=7:1 | 16.12 | 716.07 | 551.45 | 129.85 |
| A:D=2:1 | 5.84 | 1976.54 | 1303.86 | 151.59 |
| A:D=1:1 | 3.63 | 3179.89 | 1905.79 | 166.85 |
| A:D=1:2 | 2.50 | 4617.20 | 2507.72 | 184.12 |
| A:D=1:7 | 2.06 | 5603.40 | 3260.13 | 171.88 |
| A:D=1:16 | 2.03 | 5686.21 | 3499.13 | 162.50 |
| A:D=1:19 | 2.11 | 5470.62 | 3531.00 | 154.93 |
| A:D=1:20 | 2.16 | 5343.98 | 3539.60 | 150.98 |
| A:D=1:50 | 2.25 | 5130.22 | 3640.76 | 140.91 |
| A:D=1:80 | 2.43 | 4750.21 | 3666.99 | 129.54 |
| A:D=1:100 | 2.60 | 4439.62 | 3675.82 | 120.78 |
From toxicity test result table 11, methylsulfonyl bacterium azoles and the methaldehyde are compounding in the range of 10:1 to 1:100
The co-toxicity coefficient of control of plant bacterial wilt all reaches more than 120, shows obvious synergistic function.Particularly, at 2:1 to 1:
In the range of 20, co-toxicity coefficient is more than 150, and potentiation is especially pronounced.
Land for growing field crops test examples
In order to the most of the present invention based on methylsulfonyl bacterium azoles complex composition to the bacterial disease on Fructus Lycopersici esculenti and Fructus Cucumidis sativi
Evil and the prevention effect of respective propagation medium, and verify whether the synergistic results of compounding Toxicity Determination is suitable in field.This
Patent application people different regions at home have carried out substantial amounts of field test.It is exemplified below several embodiment to illustrate.With Carapax et Plastrum Testudinis
Sulphonyl bacterium azoles is referred to as first sulphur.Comparison medicament:
| Group | Medicament title | Registration card number | Organization | Medicament is originated |
| CK1 | 30% methylsulfonyl bacterium azoles wettable powder | / | / | Self-control |
| CK2 | 5% fosthiazate granule | PD20140836 | Hebei Sannong Agricultural Chemical Co., Ltd. | Commercial |
| CK3 | 20% Fosthiazate aqueous emulsion | PD20141205 | Guangdong Zhongxun Agricultural Technology Co., Ltd. | Commercial |
| CK4 | 5% avermectin micro-emulsion | PD20083100 | Chambroad Agrochemical Technology Co., Ltd. | Commercial |
| CK5 | 0.5% Abamectin | PD20110133 | Shenzhen Nuopuxin Agricultural Chemical Co., Ltd | Commercial |
| CK6 | 80% methaldehyde wettable powder | PD20121096 | Feng Wei chemical plant, Xuzhou, Jiangsu Province | Commercial |
| CK7 | 6% methaldehyde granule | PD20140376 | Anji County, Zhejiang Province Bang Hua Chemical Co., Ltd. | Commercial |
CK1:30% methylsulfonyl bacterium azoles wettable powder
Compound method: by methylsulfonyl bacterium azoles 30g, sodium lauryl sulphate 2g, pull open powder 7g, Kaolin supply 100g mixing
Uniformly, after jet mill is pulverized, stir 30min, obtain 30% methylsulfonyl bacterium azoles wettable powder.
Field test embodiment one: the field control effectiveness test of preventing and treating bacterial wilt of peanut
Test method: specify application method with reference to " pesticide field efficacy medicine test criterion (NY/T1464.32-2010) ",
Spray dispenser for the first time when beginning to see diseased plant, second time spray dispenser after 10d.Dispenser twice altogether, each process plot area is
40m2, number of repetition 4 times.
Investigation method: specify investigation method with reference to " pesticide field efficacy medicine test criterion (NY/T1464.32-2010) ", the
After secondary dispenser, whole plant are investigated in each community by 10d, 20d, record total strain number and diseased plant number, calculate diseased plant rate and preventing and treating is anti-
Effect.
Measurement result refers to table 12, table 13.
The field control effectiveness test result of table 12 methylsulfonyl bacterium azoles fosthiazate preventing and treating bacterial wilt of peanut
From result of the test table 12, preventing bacterial wilt of peanut at Semen arachidis hypogaeae their early stage, the pesticidal preparations of the present invention is having
In the case of effect composition dosage is less relative to single dose, prevention effect (the effective ingredient dosage of 10 days after medicine for the second time
40g/667m2) obviously higher than the prevention effect of single dose, all exceed single dose at least 20.0%, show obvious potentiation.
After medicine, the preventive effect of 20 days remains to reach more than 78% for the second time, and the lasting period is long.
The field control effectiveness test result of table 13 methylsulfonyl bacterium azoles avilamycin preventing and treating bacterial wilt of peanut
From result of the test table 13, preventing bacterial wilt of peanut at Semen arachidis hypogaeae their early stage, the pesticidal preparations of the present invention is having
In the case of effect composition dosage is less relative to single dose, prevention effect (effective ingredient dosage 7g/ of 10 days after medicine for the second time
667m2) obviously higher than the prevention effect of single dose, respectively higher than single dose 14.72%～63.82%, show obvious potentiation
Effect.After medicine, the preventive effect of 20 days remains to reach more than 72.68% for the second time, and the lasting period is long.
Field test embodiment two: prevent and treat the field control effectiveness test of soft rot of cabbage
Test method and computational methods are with reference to " GB/T17980.114-2004 pesticide field efficacy medicine test criterion (two) the
114 parts: bactericidal agent for preventing and treating soft rot of Chinese cabbage ", every plot area 30m2, often process 4 times and repeat, if clear water is processed as blank
Comparison, carries out spraying dispenser in their early stage, is spaced the dispenser of 7 days second time.Before first time medicine, for the second time after medicine 7 days,
14 days survey results after medicine for the second time, investigate incidence in units of strain, calculate diseased plant rate, preventive effect.The results are shown in Table 14, table
15:
Table 14 methylsulfonyl bacterium azoles fosthiazate prevents and treats the field control effectiveness test result of soft rot of cabbage
From result of the test table 14, preventing soft rot of cabbage at the initial stage of a disease, the pesticidal preparations of the present invention is effectively becoming
In the case of demultiplexing dose is less relative to single dose, prevention effect (effective ingredient dosage 40g/ of 7 days after medicine for the second time
667m2) obviously higher than the prevention effect of single dose, all exceed single dose at least 15.93%, show obvious potentiation.The
After secondary medicine, the preventive effect of 14 days remains to reach more than 77%, and the lasting period is long.
The field control effectiveness test result of table 15 methylsulfonyl bacterium azoles methaldehyde preventing and treating soft rot of Chinese cabbage
From result of the test table 15, preventing soft rot of cabbage at the initial stage of a disease, the pesticidal preparations of the present invention is effectively becoming
In the case of demultiplexing dose is less relative to single dose, prevention effect (effective ingredient dosage 9g/ of 7 days after medicine for the second time
667m2) obviously higher than the prevention effect of single dose, exceed single dose 4.77%～70.54% respectively, show obvious potentiation and make
With.After medicine, the preventive effect of 14 days remains to reach more than 79.44% for the second time, and the lasting period is long.
Field test embodiment three: the field control effectiveness test of preventing and treating tomato root-knot eelworm
Test method and computational methods are with reference to " GB/T17980.38-2000 pesticide field efficacy medicine test criterion () the 38th
Part: nematicide preventing and treating root nematicide ", every plot area 30m2, often process 4 times and repeat, if clear water be processed as blank right
According to, carry out spraying dispenser when first meeting morbidity strain, be spaced the dispenser of 7 days second time.Before first time medicine, for the second time after medicine 10
My god, 20 days survey results after medicine for the second time, investigate incidence with strain for unit classification, calculate disease index, preventive effect.Result is shown in
Table 16:
The field control effectiveness test result that table 16 methylsulfonyl bacterium azoles fosthiazate preventing and treating tomato root-knot eelworm is sick
From result of the test table 16, prevention tomato root-knot eelworm is sick at the initial stage of a disease, and the pesticidal preparations of the present invention is having
In the case of effect composition dosage is less relative to single dose, prevention effect (effective ingredient dosage 40g/ of 7 days after medicine for the second time
667m2) obviously higher than the prevention effect of single dose, all exceed single dose at least 14.18%, show obvious potentiation.The
After secondary medicine, the preventive effect of 14 days remains to reach more than 77%, and the lasting period is long.
Field test embodiment four: the field control effectiveness test of preventing and treating Fructus Cucumidis sativi root-knot nematode
Test method and computational methods are with reference to " GB/T17980.38-2000 pesticide field efficacy medicine test criterion () the 38th
Part: nematicide preventing and treating root nematicide ", every plot area 30m2, often process 4 times and repeat, carry out when first meeting morbidity strain
Root granule spreads fertilizer over the fields dispenser, or wettable powder is mixed soil and spread fertilizer over the fields dispenser, if spreading soil to be processed as blank.Before medicine, after medicine
10 days, 20 days survey results after medicine, investigate incidence with strain for unit classification, calculate disease index, preventive effect.The results are shown in Table
17:
The field control effectiveness test result of table 17 methylsulfonyl bacterium azoles fosthiazate preventing and treating Cucumber root-knot nematode disease
From result of the test table 17, preventing Cucumber root-knot nematode disease at the initial stage of a disease, the pesticidal preparations of the present invention is having
In the case of effect composition dosage is less relative to single dose, prevention effect (effective ingredient dosage 120g/ of 10 days after medicine
667m2) obviously higher than the prevention effect of single dose, all exceed single dose at least 17.95%, show obvious potentiation.Medicine
The preventive effect of latter 20 days remains to reach more than 80%, and the lasting period is long.
Field test embodiment five: the field control effectiveness test of preventing and treating citrus bacterial canker disease
Test method and computational methods are with reference to " pesticide field efficacy medicine test criterion two (GB/T 17980.103-2004) "
Start dispenser for the first time in c itrus canker stadium, altogether dispenser 2 times, set up 7 communities, each community 3 strain, repeat 4
Secondary, Gong28Ge community.Control time investigates disease index before medicine, and after medicine, 7d, 14d investigate disease index for the second time, calculate it
Preventive effect, as shown in table 18.Two strains are investigated in every community, and the sampling of 5, all directions, every 10 fruits of investigation and two are pressed in every strain
Whole blades on the tip.
The field control effectiveness test result of table 18 methylsulfonyl bacterium azoles avilamycin preventing and treating citrus bacterial canker disease
From result of the test table 18, preventing citrus bacterial canker disease at the initial stage of a disease, the pesticidal preparations of the present invention is effectively becoming
In the case of demultiplexing dose is less relative to single dose, 20d blade and the preventing and treating effect of fruit after preventing and treating citrus bacterial canker disease second time medicine
Really (effective ingredient dosage 40g/667m2) it is respectively higher than single dose 11.19%～60.13% and 15.26%～62.80%, table
Reveal obvious potentiation, after the second medicine the prevention effect of 30d blade and fruit remain to reach more than 73.04% and
More than 70.88%, the lasting period is long.
Field test embodiment six: the field control effectiveness test of preventing and treating citrus red mite
Test method and computational methods are with reference to " pesticide field efficacy medicine test criterion one (GB/T 17980.11-2000) ".
The dispenser when averagely every leaf has demodicid mite alive more than 2, dispenser is once altogether.If 7 communities, every plot area 3 tree,
Being repeated 4 times, Gong28Ge community, protected row between community, each community uses the group arrangement of random district.After medicine 1d, 3d, 10d,
15d, 20d, 30d investigate.25 blades, at the East, West, South, North of tree, the middle tender tip of five positions labelling, are investigated altogether in every community
On movable mite population.Blade face, the quantity of statistics acarid is directly observed with hand magnifier.
The field control effectiveness test result of table 19 methylsulfonyl bacterium azoles avilamycin preventing and treating citrus red mite
From measurement result table 19: prevent citrus red mite at the initial stage of a disease, the pesticidal preparations of the present invention is effectively becoming
In the case of demultiplexing dose is less relative to single dose, 1d, 3d, 10d, 15d, 20d preventing and treating effect after preventing and treating medicine of citrus red mite
Really (effective ingredient dosage 4g/667m2) obviously higher than the prevention effect of single dose, the prevention effect of 15d all exceeds single dose extremely
Few 27.03%, show obvious potentiation, after medicine, the preventive effect of 30d remains to reach more than 83.54%, and the lasting period is long.
Field test embodiment seven: the field control effectiveness test of preventing and treating peanut root-knot nematode
Test method and computational methods are with reference to " pesticide field efficacy medicine test criterion one (GB/T17980.38-2000) ".
When first meeting morbidity strain, carry out root granule spread fertilizer over the fields dispenser, or wettable powder is mixed soil and spread fertilizer over the fields dispenser, if spreading soil
Being processed as blank, dispenser 1 time, sets up 7 communities, every plot area 30m altogether2, often process 4 times and repeat, Gong28Ge community.
Before medicine, after medicine 10 days, within 20 days, investigate after medicine.Searching is injured suspicious diseased plant, uses diagonal 5 sampling or randomization
Method, every some investigation two strains, calculate disease index and prevention effect.
Table 20 methylsulfonyl bacterium azoles avilamycin prevents and treats the field control effectiveness test result of groundnut root knot nematode disease
From result of the test table 20, preventing groundnut root knot nematode disease at the initial stage of a disease, the pesticidal preparations of the present invention is having
In the case of effect composition dosage is less relative to single dose, prevention effect (effective ingredient dosage 16g/667m of 10d after medicine2)
Higher than single dose 24.00%～50.70%, showing obvious potentiation, after medicine, the prevention effect of 20d remains to reach
More than 73.04%, the lasting period is long.
Field test embodiment eight: the field control effectiveness test of control of plant bacterial wilt
Test method: specify application method with reference to " pesticide field efficacy medicine test criterion (NY/T1464.32-2010) ",
First time spray pesticide when beginning to see diseased plant, second time spray pesticide after 5d.Dispenser twice altogether, each process plot area is
20m2, number of repetition 4 times.
Investigation method: specify investigation method with reference to " pesticide field efficacy medicine test criterion (NY/T1464.32-2010) ", the
After secondary dispenser, whole plant are investigated in each community by 7d, 14d, record total strain number and diseased plant number, calculate diseased plant rate and preventing and treating is anti-
Effect.
Result of the test is shown in Table 21.
The field control effectiveness test result of table 21 methylsulfonyl bacterium azoles methaldehyde control of plant bacterial wilt
From result of the test table 21, preventing bacterial wilt of tomato at the initial stage of a disease, the pesticidal preparations of the present invention is effectively becoming
In the case of demultiplexing dose is less relative to single dose, prevention effect (effective ingredient dosage 10g/ of 7d after medicine for the second time
667m2) higher than single dose at least 10.44%, showing obvious potentiation, after the second medicine, the prevention effect of 14d remains to reach
More than 78.61%, the lasting period is long.
Field test embodiment nine: the field control effectiveness test of preventing and treating brassicaceous vegetable Limax
Test method: with reference to " pesticide field efficacy medicine test criterion GB/T17980.69-2004 ", uniform for afternoon selected from fine day
The application method spread pesticides, if 7 communities, every plot area 30m2, each process sets 4 repetitions, altogether She28Ge community.
Investigation method: investigate each community abiogenous Limax quantity before dispenser, every community can random inspection 2m2, as often
During square metre less than 20, gather same age size the most in the wild and congener Limax adds to 20 every square metre.After medicine
When 3 times investigating, soil table level plant base portion and the individuality of top death can only be observed, table soil should not be stirred, in case powder embedment
Under soil, Limax (symptom is body, abdomen, liquefies enough, ungauged regions ability, and head, abdomen expose) dead in investigation is individual at record number
Amount.When investigating for the last time, stir under table soil at 1cm～3cm simultaneously, note the dead individuals below relatively large clod.Result is shown in
Table 21.
The field control effectiveness test result of table 22 methylsulfonyl bacterium azoles methaldehyde preventing and treating brassicaceous vegetable Limax
From result of the test table 22, when preventing and treating brassicaceous vegetable Limax, the pesticidal preparations of the present invention is effectively becoming
In the case of demultiplexing dose is less relative to single dose, prevention effect (effective ingredient dosage 20g/667m of 7d after medicine2) the highest
Go out single dose at least 9.61%, show obvious potentiation, and after medicine, the prevention effect of 21d remains to reach more than 82%, holds
The effect phase is long.
Claims (8)
1. the complex composition containing methylsulfonyl bacterium azoles, it is characterised in that: described complex composition contains two kinds of active component,
The first active component is methylsulfonyl bacterium azoles, and second active ingredient is avilamycin, the wherein chemical name of methylsulfonyl bacterium azoles
For 2-(to fluorophenyl)-5-mesyl-1,3,4-diazole；Described methylsulfonyl bacterium azoles is 500 with the weight ratio of avilamycin:
1 to 1:100.
Complex composition containing methylsulfonyl bacterium azoles the most according to claim 1, it is characterised in that: described methylsulfonyl bacterium azoles with
The weight ratio of avilamycin is 100:1 to 1:20.
3. the pesticidal preparations containing methylsulfonyl bacterium azoles, it is characterised in that include compounding group described in any one of claim 1-2
Acceptable adjuvant on compound and pesticide, is then prepared as pesticidal preparations.
Pesticidal preparations containing methylsulfonyl bacterium azoles the most according to claim 3, it is characterised in that by weight, described compounding
It is 0.1%-90% that compositions accounts for the weight percentage of described pesticidal preparations.
Pesticidal preparations containing methylsulfonyl bacterium azoles the most according to claim 4, it is characterised in that by weight, described compounding
It is 1%-80% that compositions accounts for the weight percentage of described pesticidal preparations.
Pesticidal preparations containing methylsulfonyl bacterium azoles the most according to claim 3, it is characterised in that acceptable adjuvant on pesticide
For filler and the mixture of auxiliary agent.
Pesticidal preparations containing methylsulfonyl bacterium azoles the most according to claim 3, it is characterised in that the dosage form of described pesticidal preparations
For wettable powder, water dispersible granules, suspending agent, microemulsion, aqueous emulsion, cream, suspension seed-coating agent or granule.
8. claim 1-2 arbitrary described complex composition application in terms of preventing and treating crop bacterial disease and/or insect pest.
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