CN103300015A - Sterilizing composition comprising boscalid and pyrisoxazole - Google Patents
Sterilizing composition comprising boscalid and pyrisoxazole Download PDFInfo
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- CN103300015A CN103300015A CN2013102013637A CN201310201363A CN103300015A CN 103300015 A CN103300015 A CN 103300015A CN 2013102013637 A CN2013102013637 A CN 2013102013637A CN 201310201363 A CN201310201363 A CN 201310201363A CN 103300015 A CN103300015 A CN 103300015A
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Abstract
The invention relates to a sterilizing composition comprising boscalid and pyrisoxazole. The effective components of the composition are boscalid and pyrisoxazole which form a binary complex. The weight ratio of boscalid to pyrisoxazole is (1:40)-(40:1). The effective components of boscalid and pyrisoxazole in the preparation account for 1-80% in percentage by weight, and the balance is auxiliary components permitted to be used and accepted in pesticide. The dosage form of the sterilizing composition provided by the invention is missible oil, suspending agent, wettable powder, water dispersible granules, emulsion in water, microemulsion, granules and microcapsule. The composition is mainly used for preventing and treating powdery mildew, gray mold, various rots, brown rot, root rot and the like.
Description
Technical field
The present invention relates to the agriculture chemical compounding technical field, particularly relate to a kind of bactericidal composition that contains Boscalid and SYP-Z048.
Background technology
Boscalid is the Novel tobacco acid amide fungicides by BASF Aktiengesellschaft's exploitation, be mainly used in preventing and treating powdery mildew, gray mold, various rot, brown rot and root rot etc., Boscalid belongs to succinic acid ubiquinone reductase inhibitor in mitochondrial respiratory chain, sprouting to spore has very strong inhibition ability, and with other bactericide without cross resistance.The chemistry of Boscalid is called the chloro-N-of 2-(4-chlorodiphenyl-2-yl) vitamin PP, and its chemical structural formula is
.
SYP-Z048 is the bactericide of Shenyang Chemical Engineering Inst's initiative, belongs to the synthetic inhibition bactericide of sterol, by the root dispenser, can effectively control not generation and the harm of disease of leaf on the ground.Bactericidal activity with wide spectrum; there is protection and therapeutic action and good interior absorption simultaneously; be mainly used in the control of plant botrytis, the chemistry of SYP-Z048 is called N-methyl-3-(4-chlorine) phenyl-5-methyl-5-pyridine-3-methyl-oxazoline, and its chemical structural formula is
.
Using chemical agent is the most effectively means of controlling plant diseases.But long-term use single chemical bactericide continuously high dose, easily cause the problems such as residual, the environmental pollution of medicament and anti-pesticide resistance fungi development.Reasonably chemical bactericide is composite or be mixed and have the expansion fungicidal spectrum, improve control efficiency, extend the optimum period for applying fertilizer, reduce dosage, reduce poisoning, reduce residual, delay Antifungal resistance and the positive characteristics such as drug-fast generation and development, bactericide compounded is one of the effective method the most addressed the above problem.Exploitation new product bactericide price is constantly soaring, and by contrast, exploitation is efficient with research, low toxicity, low-residual composite be mixed there is small investment, the lead time is short and be subject to domestic and international attention, the numerous and confused dynamics that develops that strengthens.We filter out Boscalid and SYP-Z048 and carry out compositely on the basis of lab screening and field trial, have obvious synergistic effect.And there is no at present the people about the composite bactericidal composition of Boscalid and SYP-Z048 and application reported.
Summary of the invention
Based on above situation, the object of the invention is to provide a kind of new and effective pesticide sterilizing composite.Be mainly used in preventing and treating powdery mildew, gray mold, various rot, brown rot and root rot etc.
Technical scheme of the present invention realizes by following measures:
A kind of bactericidal composition that contains Boscalid and SYP-Z048, two yuan of the active ingredient Boscalid of this bactericidal composition and SYP-Z048s are composite, and all the other are auxiliary element.In wherein said bactericidal composition, the mass ratio of active ingredient Boscalid and SYP-Z048 is 1～40: 40～1, described bactericidal composition of the present invention is through the toxicity test experimental verification, the mass ratio of Boscalid and SYP-Z048 is 1～40: 40～1 o'clock, and synergistic effect is better.
The formulations of pesticide that described bactericidal composition of the present invention can be prepared are missible oil, suspending agent, wetting powder, water dispersible granules, aqueous emulsion, microemulsion, granule, microcapsule formulations.Wherein active ingredient Boscalid and the SYP-Z048 gross mass in preparation accounts for 1%～80% of the whole quality of the pharmaceutical preparations, while wherein accounting for 5%～50%, and toxicity and the residual balance preferably that reaches, cost is also lower.
The specific embodiments of the formulations of pesticide that bactericidal composition of the present invention is mixed with is as follows:
Described bactericidal composition is cream preparation, and the mass fraction of component is: 1～40 part of Boscalid; 1～40 part of SYP-Z048; 10～30 parts of conventional emulsifiers; 20～50 parts of conventional solvents; 1～5 part of conventional synergist.The concrete production stage of this cream preparation adds emulsifier, the synergist rear oily liquids that becomes transparent and homogeneous that stirs again for first active ingredient Boscalid and SYP-Z048 being added in solvent after dissolving fully, filling, can be made into the cream preparation of the present composition.
Described bactericidal composition is suspending agent, and the mass fraction of component is: 1～40 part of Boscalid; 1～40 part of SYP-Z048; 5～20 parts of dispersants; 1～5 part of antifreezing agent; 0.1～2 part of thickener; 0.1～0.8 part of defoamer; 0～10 part of penetrating agent; 0.1～5 part of pH value conditioning agent; Water, surplus.The concrete production stage of this suspending agent is for first mixing other auxiliary agents, mix through high speed shear, add active ingredient Boscalid and SYP-Z048, in ball crusher, abrading-ball is 2～3 hours, make a diameter all below 5mm, can be made into the suspending agent preparation of the present composition.
Described bactericidal composition is wetting powder, and the mass fraction of component is: 1～40 part of Boscalid; 1～40 part of SYP-Z048; 3～10 parts of dispersants; 1～5 part of wetting agent; Filler, surplus.The concrete production stage of this wetting powder is: by above-mentioned formula, the active ingredient Boscalid is mixed with SYP-Z048 and dispersant, wetting agent and filler, uniform stirring in stirred tank, mixing after airslide disintegrating mill, can be made into the wetting powder of the present composition.
Described bactericidal composition is water dispersible granules, and the mass fraction of component is: 1～40 part of Boscalid; 1～40 part of SYP-Z048; 3～10 parts of dispersants; 1～10 part of wetting agent; 1～5 part of disintegrant; Filler, surplus.The concrete production stage of this water dispersible granules is: by above-mentioned formula, the active ingredient Boscalid is mixed with SYP-Z048 and dispersant, wetting agent, disintegrant and filler, with micro jet, pulverize, through mediating, then add in the fluidized bed prilling dryer and carry out granulation, drying, screening by sample analysis, can be made into the water dispersible granules of the present composition.
Described bactericidal composition is aqueous emulsion, and the mass fraction of component is: 1～40 part of Boscalid; 1～40 part of SYP-Z048; 3～30 parts of emulsifier; 5～15 parts of solvents; 2～15 parts of stabilizing agents; 1～5 part of antifreezing agent; 0.1～8 part of defoamer; 0.2～2 part of thickener; Water, surplus.The concrete production stage of this aqueous emulsion is: at first Boscalid and SYP-Z048, solvent and emulsifier, cosolvent are added together, make to be dissolved into uniform oil phase; By part water, antifreeze, other the insecticides adjuvant such as antimicrobial mixes into uniform water; When the reactor high speed stirs, oil phase is added to water, slowly add water until reach the phase inversion point, open clipper and carry out high speed shear, and add remaining water, shear about half an hour, form the aqueous emulsion of oil-in-water type, can be made into the aqueous emulsion of the present composition.
Described bactericidal composition is microemulsion, and the mass fraction of component is: 1～40 part of Boscalid; 1～40 part of SYP-Z048; 10～30 parts of emulsifier, 1～8 part of antifreezing agent, 0.5～10 part of stabilizing agent, 20～50 parts of conventional solvent cosolvents.Boscalid and SYP-Z048 are dissolved fully with cosolvent, then add other compositions such as emulsifier, antifreezing agent stabilizing agent, evenly mix, finally add water, after fully stirring, can be made into microemulsion.
Described bactericidal composition is granule, and the mass fraction of component is: 1～40 part of Boscalid; 1～40 part of SYP-Z048; 1～10 part of wetting dispersing agent; 0.1～5 part of thickener; 0.1～5 part of defoamer; Castor oil, surplus is supplied.The active ingredient Boscalid is mixed in the ratio of formula with each components such as SYP-Z048, dispersant, stabilizing agent, defoamer and solvents, after putting into the grinding of sand milling still, send in mixer for well-distribution and mix and get product.
Described bactericidal composition is microcapsule formulations, and the mass fraction of component is: 1～40 part of Boscalid; 1～40 part of SYP-Z048; 5～20 parts, urea; 5～20 parts, formaldehyde; 5～20 parts of emulsifying dispersants; 1～5 part of antifreezing agent; 0.1～2 part of thickener; 0.1～0.8 part of defoamer; Water, surplus.In being housed, the there-necked flask of agitating device adds urea and formaldehyde (the amount of substance ratio is about l:1.5～2.0), with the pH value to 8 of sodium hydroxide solution regulator solution～9 left and right, then be warming up to 70～80 ℃, reaction obtains stable urea resin prepolymer.The former medicine of getting a certain amount of Boscalid and SYP-Z048 is dissolved in cyclohexane, and adds emulsifying dispersant in solution, follows vigorous stirring, the O/W type stable emulsion that to be made into the aqueous solution of take containing emulsifying dispersant be water.Above-mentioned urea resin prepolymer is added in emulsion, regulate the pH value, polymerization reaction take place under the acid catalysis condition, be wrapped oil phase substance, forms microcapsule granule.Slowly heat up, solidify, temperature is controlled at 40～50 ℃, hardening time 1h.Selection adds appropriate auxiliary agent, the microcapsule suspending agent that gets final product stablely.
Wherein above-described emulsifier is selected from calcium dodecyl benzene sulfonate and aliphatic acid polyethenoxy ether, the alkylphenol polyoxyethylene sulfosuccinate, styrylphenol polyoxyethylene ether, polyoxyethylene nonylphenol ether, castor oil polyoxyethylene ether, aliphatic acid polyethenoxy base ester, any or more than one any mixtures than forming in polyoxyethylene aliphatic alcohol ether.
Described solvent is dimethylbenzene or biodiesel, toluene, and diesel oil, methyl alcohol, ethanol, n-butanol, isopropyl alcohol, turpentine oil, solvent naphtha, dimethyl formamide, dimethyl sulfoxide (DMSO), one or more in the water equal solvent are arbitrarily than the mixture formed.
Described dispersant is selected from polycarboxylate, lignosulfonates, alkylphenol polyoxyethylene methyl ether condensate sulfate, the alkylsulfonate calcium salt, the naphthalene sulfonic acid-formaldehyde condensation product sodium salt, alkylphenol polyoxyethylene, polyoxyethylene carboxylate, aliphatic amine polyoxyethylene ether, one or more in the fatty acid glyceride APEO.
Described wetting agent is selected from lauryl sodium sulfate, calcium dodecyl benzene sulfonate, and Nekal BX, moistening bleeding agent F, alkylbenzenesulfonate polyoxyethylene triphen is phosphenylic acid salt dimly, spaonin powder, silkworm excrement, one or more in the soapberry powder.
Described disintegrant is selected from bentonite, urea, ammonium sulfate, aluminium chloride, citric acid, succinic acid, one or more in sodium bicarbonate.
Described thickener is selected from xanthans, carboxymethyl cellulose, carboxyethyl cellulose, methylcellulose, Magnesiumaluminumsilicate, in polyvinyl alcohol one or more.
Described stabilizing agent is selected from sodium citrate, a kind of in resorcinol.
Described antifreezing agent is selected from ethylene glycol, propane diols, one or more in glycerine.
Described defoamer is selected from silicone oil, silicone compound, C
10-20the saturated fat acid compounds, C
8-10one or more of fatty alcohol.
Described filler is selected from kaolin, diatomite, bentonite, attapulgite, white carbon, starch, one or more in precipitated calcium carbonate.
The present invention be take the composite bactericide that Boscalid and SYP-Z048 be active ingredient and is had obvious synergistic effect, delays the drug-fast generation in key, and has reduced to become to produce cost and use cost, can be used for the improvement of resistance disease.Be mainly used in preventing and treating powdery mildew, gray mold, various rot, brown rot and root rot etc.
Embodiment
For making technical scheme of the present invention, purpose and advantage are clearer, and the present invention describes with following specific embodiment, but the present invention is not limited to these examples.The mode that effect experiment of the present invention adopts indoor biometrics and field trial to combine, if no special instructions, the ratio of below mentioning is all ratio of quality and the number of copies.
Embodiment: Boscalid proportioning co-toxicity experiments different from SYP-Z048.
1.1 reagent agent
The former medicine of 95% Boscalid, the former medicine of 95% SYP-Z048, above-mentioned former medicine provides by research and development department of extra large rel medicine company limited company.
1.2 test target
Never executed Boscalid and SYP-Z048 from Shouguang, Shandong and cucumber of the same type gathers and separates potted plantly, for the examination cucumber variety: Chang Chun Mi Ci.
1.3 test method
1.3.1 medicament preparation
First use the former medicine of acetone solution, according to the result of preliminary experiment, two appropriate former medicines are made into to several different proportionings, then it is stand-by with acetone, each processing to be diluted to respectively to several concentration gradients.
Susceptible cucumber variety Chang Chun Mi Ci cultivation, in pot for growing seedlings, is placed in to greenhouse and cultivates, and plant grows to three to four leaf after dates, gathers the blade of identical leaf age, for cultivation and the mensuration of powdery mildew of cucumber bacterium.
1.3.2 the cultivation of powdery mildew of cucumber bacterium and the preparation of spore suspension
The powdery mildew of cucumber bacterium adopts the plants method to cultivate under 20 ℃, the condition of 12h alternation of light and darkness, and every 30 d turn culture 1 time.During inoculation, with the conidium on sterile water wash-out incidence of leaf, being mixed with spore concentration is l * 10
6the suspension of individual/mL.
1.3.3 strains tested sensitivity testing
Adopt leaf dish moisturizing method to carry out toxicity test.First the blade of collection is prepared into to the leaf dish that diameter is 1.5cm, mix at random, be placed in respectively the series concentration liquid configured and soak lh, 50 leaf dishes of each concentration, test is with the blank that is treated to of adding medicine not, after soaking end, leaf faces up and puts on the blotting paper wetting in identical liquor strength, liquid on the leaf dish is blotted, the spore suspension l0L prepared is inoculated in to leaf dish central authorities, after room temperature is placed 5 min, is placed under 20 ℃, the condition of 1 2h alternation of light and darkness and cultivates, measure the onset area on the leaf dish after 10d, calculate EC
50.
On the basis of preliminary experiment, respectively single dose Boscalid and SYP-Z048 are carried out to toxicity test in order to upper method, the two EC
50value is respectively 5.05 ㎎/l and 6.35 ㎎/l.
The percentage that accounts for the leaf disc area according to lesion area is divided sick level
0 grade: anosis;
1 grade: the sorus area accounts for below 5% of whole leaf area;
3 grades: the sorus area accounts for below the 6%-10% of whole leaf area;
5 grades: the sorus area accounts for below the 11%-20% of whole leaf area;
7 grades: the sorus area accounts for below the 21%-50% of whole leaf area;
9 grades: the sorus area accounts for more than 50% of whole leaf area;
1.3.4 mixture toxicity test and interpretation of result
Carry out the toxicity test of mixture according to mixed ratio by single dose toxicity test method.
If contrast lethality<5%, do not proofread and correct, the contrast lethality, between 5%-20%, is proofreaied and correct by formula 2, the contrast lethality > 20%, test need be reformed.
The logarithm value of drug concentration (mg/L) of take is independent variable x, and the probability value of corrected mortality of take is dependent variable y, sets up respectively the virulence regression equation formula, adopts DPS software to calculate the LC of single dose and each proportioning mixture
50calculate co-toxicity coefficient (CTC) according to the abundant method of Sun Yun.Co-toxicity coefficient CTC, computing formula is as follows: (take Boscalid as the standard medicament, its toxicity index is 100):
The LC of the toxicity index of SYP-Z048 (TI)=Boscalid
50the LC of/SYP-Z048
50* 100
The LC of the true toxicity index (ATI) of M=Boscalid
50the LC of/M
50* 100
The TI of the TI of the theoretical toxicity index (TTI) of M=Boscalid * P Boscalid+SYP-Z048s * P SYP-Z048
The TTI of the ATI/M of the co-toxicity coefficient of M (CTC)=M * 100
In formula:
M is Boscalid and the mixture of the different proportionings of SYP-Z048
The P Boscalid is Boscalid shared ratio in mixture
The P SYP-Z048 is SYP-Z048 shared ratio in mixture.
2.1 toxicity test result
Table 1 Boscalid and the SYP-Z048 toxicity test to powdery mildew of cucumber
As can be seen from the table, the result of the test of different proportion proportioning shows, dilute respectively and all show stronger synergistic effect in the active ingredient ratio, wherein take Boscalid: SYP-Z048 as 1:10～10:1 the time the good suggestion of synergistic effect suitable proportion 1:10～10:1 left and right mixture preparation is carried out to further field control effectiveness test, to estimate its field practical application effect.
3 field trials are prevented and treated powdery mildew of cucumber, the experimental result of grape grey mould
3.1 field trial is prevented and treated powdery mildew of cucumber
3.1.1 test method
Test is at 4 points of Pingdu City cucumber Di，Mei community, Shandong investigation, and every some investigation 2 strains, put down in writing occurring degree by staging, and grade scale is as follows:
0 grade: anosis;
1 grade: the sorus area accounts for below 5% of whole leaf area;
3 grades: the sorus area accounts for below the 6%-10% of whole leaf area;
5 grades: the sorus area accounts for below the 11%-20% of whole leaf area;
7 grades: the sorus area accounts for below the 21%-50% of whole leaf area;
9 grades: the sorus area accounts for more than 50% of whole leaf area.
3.1.2 control time and number of times
Test is investigated 4 times altogether, radix investigation before medicine, for the first time after medicine 10 days, after 10 days and medicine, within 21 days, investigated after medicine for the second time.
3.1.3 drug effect computational methods
Sick leaf rate (%)=sick number of sheets/investigate total number of sheets * 100
Disease index=∑ (the sick numbers of sheets at different levels * relative level numerical value)/(investigating total number of sheets * 9) * 100
Control efficiency (%)=(disease index after disease index before 1-(blank district medicine * treatment region medicine)/(disease index before disease index after blank district medicine * treatment region medicine)) * 100.
3.1.4 poisoning investigation method
After dispenser, whether continuous 15d range estimation medicament has poisoning to crop.
3.1.5 result of the test and analysis
Each processes the effect of preventing and treating powdery mildew of cucumber.Table 2
As shown in Table 2 Boscalid and SYP-Z048 with 1:6 ratio composite bactericide for powdery mildew of cucumber control successful higher than Boscalid and SYP-Z048 single dose, bactericidal effect increases progressively with the increase of dosage.According to the field range estimation, in the test dose scope, plant growth is normal, and the poisoning phenomenon to cucumber does not all appear in each treatment agent, illustrates that it is safe to cucumber.Advise that the bactericide different from the mechanism of action mixes use to delay the drug-fast generation of germ.
3.2 field trial control grape grey mould
3.2.1 test method
Test is located in Jinhua Academy of Agricultural Sciences proving ground beam-connected greenhouse.Experimental cultivar is that rattan is harvested grape, the age of tree 4 years, seeding row spacing 1m * 4m, pergola system.The sterilization of this garden booth anniversary epiphragma ，Qing garden is not thorough, and in soil, invalid body is more, and grape grey mould occurs more serious over the years.Be experimental field the faintly acid sandy loam, the content of organic matter is lower, and Fertilization Level is medium, the moisture abundance, and it is moistening that soil keeps for a long time.
3.1.2 control time, method and number of times
Investigate incidence and disease index before dispenser, after medicine 10 days, after medicine, within 10 days and 21 days, investigated for the second time, by tree San Ge position, body upper, middle and lower, each takes out the sick level of 10 inflorescences (fruit ear) investigation at random.Grade scale is as follows:
0 grade: anosis;
1 grade: sick section accounts for below 5% of whole inflorescence (fruit ear);
3 grades: sick section accounts for the 6%-15% of whole inflorescence (fruit ear);
5 grades: sick section accounts for the 16%-25% of whole inflorescence (fruit ear);
7 grades: sick section accounts for the 26%-50% of whole inflorescence (fruit ear);
9 grades: sick section accounts for more than 50% of whole inflorescence (fruit ear).
3.2.3 drug effect computational methods
Diseased fruit rate (the %)=total fruit of disease fruit number/investigation number * 100
Disease index=∑ (sick fruit number * relative level numerical value at different levels)/(the total fruit of investigation number * 9) * 100
Control efficiency (%)=(disease index after disease index before 1-(blank district medicine * treatment region medicine)/(disease index before disease index after blank district medicine * treatment region medicine)) * 100.
3.2.4 poisoning investigation method
After dispenser, whether continuous 10d range estimation medicament has poisoning to crop.
3.2.5 result of the test and analysis
Each processes the effect of control grape grey mould.
The Mixed Pharmacy of different proportion, tested by different consumptions as can be seen from Table 3, Boscalid and SYP-Z048 with 1:6 ratio compound medicine after its right control all be better than contrasting medicament and bactericidal effect and increase progressively with the increase of dosage.According to the field range estimation, in the test dose scope, plant growth is normal, and the poisoning phenomenon to grape does not all appear in each treatment agent, illustrates that it is safe to grape.Advise that the bactericide different from the mechanism of action mixes use to delay the drug-fast generation of germ.
In sum, the Bactericidal composite that the present invention contains Boscalid and SYP-Z048, have good control efficiency to powdery mildew of cucumber, grape grey mould, and it is to the target crop safety.Complex preparation has not only improved preventive effect, and has enlarged fungicidal spectrum, widens the scope of application, reduces costs, and multiple diseases is played to the double effect of controlling of a medicine, alleviates manpower and materials, improves productivity effect.So the invention of this complex preparation is of great significance social tool with popularization.
Claims (4)
1. a bactericidal composition that contains Boscalid and SYP-Z048, it is characterized in that: the active ingredient of this bactericidal composition is Boscalid and SYP-Z048 binary built, all the other are auxiliary element, and wherein the mass ratio of active ingredient Boscalid and SYP-Z048 is 1～40: 40～1.
2. bactericidal composition according to claim 1, it is characterized in that: Boscalid and the SYP-Z048 gross weight in preparation accounts for 1%～80% of the whole quality of the pharmaceutical preparations.
3. bactericidal composition according to claim 2, it is characterized in that: Boscalid and the SYP-Z048 gross weight in preparation accounts for 5%～50% of the whole quality of the pharmaceutical preparations.
4. according to claim 1 or 2 or 3 described bactericidal compositions, it is characterized in that: the formulation of this bactericidal composition is missible oil, suspending agent, wetting powder, water dispersible granules, aqueous emulsion, microemulsion, granule, microcapsule formulations
.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106135232A (en) * | 2015-04-13 | 2016-11-23 | 深圳诺普信农化股份有限公司 | Bactericidal composition |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101087529A (en) * | 2004-12-23 | 2007-12-12 | 巴斯福股份公司 | Fungicidal mixtures |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101087529A (en) * | 2004-12-23 | 2007-12-12 | 巴斯福股份公司 | Fungicidal mixtures |
Non-Patent Citations (1)
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106135232A (en) * | 2015-04-13 | 2016-11-23 | 深圳诺普信农化股份有限公司 | Bactericidal composition |
| CN106135232B (en) * | 2015-04-13 | 2018-06-12 | 深圳诺普信农化股份有限公司 | bactericidal composition |
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Application publication date: 20130918 |