CN101822250A - Water based pesticide preparation of osthole and application thereof - Google Patents
Water based pesticide preparation of osthole and application thereof Download PDFInfo
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Abstract
The invention discloses a water based pesticide preparation of osthole and an application thereof. The water based pesticide preparation of osthole comprises osthole suspension preparation, water-soluble liquid preparation and microemulsion preparation. The experimental study shows that the osthole suspension preparation, water-soluble liquid preparation and microemulsion preparation provided by the invention have good water solubility; the stability experimental study shows that the water based preparations of osthole provided by the invention have good stability; simultaneously, crop antibacterial experiments show that the osthole suspension preparation, water-soluble liquid preparation and microemulsion preparation provided by the invention have good control effects on powdery mildew, downy mildew and the like; and further, the toxicity experimental study shows that the osthole suspension preparation, water-soluble liquid preparation and microemulsion preparation provided by the invention have low toxicity. Thus the water based pesticide preparation of osthole can be hopefully developed into a new generation environment-friendly green antibacterial and insecticidal preparation for agricultural use.
Description
Technical field
The present invention relates to a kind of pesticidal preparations, being specifically related to the Osthole is the water base property pesticidal preparations and the application on agricultural thereof of main active.
Background technology
Coumarin kind compound Osthole chemical name is 8-(3-methyl-2-butene base) methyl ether umbelliferone, it is main component in the Carrot family plant frutus cnidii, also be root and the rhizome of Imperatoria ostruthium, circle Radix Angelicae Sinensis, Angelica pubescens, bolt wing celery, and the root skin of rutaceae anise, Calusena lansium, the active component of the acrial part of single leaf rue etc.The killing pests and suppressing bacteria activity of this compound has had multinomial report.Chinese invention patent (ZL 200410069127.5) " Osthole and built composition for preventing and controlling crop powdery mildew thereof " discloses the operation technique and the effect of Osthole and built composition for preventing and controlling crop powdery mildew thereof.Chinese invention patent (ZL200610098286.7) " application in preparation control rice green smut agricultural chemicals of Osthole and compound thereof " discloses the application that prevents and treats rice green smut about Osthole and nitrile bacterium azoles, composite jinggangmycin thing.Osthole belongs to the coumarin kind compound of lactone type, its poorly water-soluble of its structures shape, be difficult for making water-soluble formulation, but the pesticidal preparations that uses on the agricultural carries out dispenser with water as retarder thinner mostly, and Osthole is owing to be the coumarin kind compound of lactone type, its chemical property less stable, especially the easy open loop of lactonic ring structure under alkaline environment, thereby lose the effect of insecticidal and antibacterial, the Osthole Agrotechnical formulation that uses on the market is because stability is bad, desinsection or antibiotic effect reduce even the drug effect disappearance after the long term storage, also do not have steady quality and the effective water base property of Osthole preparation in the market.
Summary of the invention
Goal of the invention: the objective of the invention is in order to solve the deficiencies in the prior art, the water base property of the Osthole preparation of a kind of good water solubility and stable in properties is provided, this water base property preparation comprises Osthole suspension formulation, the water-soluble liquor of Osthole and Osthole microemulsion, and another object of the present invention provides the application of the water base property of Osthole preparation on agricultural.
Technical scheme: in order to realize above purpose, the technical scheme that the present invention takes is:
A kind of Osthole suspension formulation, it is made by following raw materials by weight percent: Osthole 0.1～50%, wetting dispersing agent 1～5%, tackifier 0.2～5%, antifreezing agent 0.1～5%, defoamer 0.2～4%, surplus water are mended to 100%.
As preferred version, Osthole suspension formulation provided by the invention is made by following raw materials by weight percent: Osthole 1～40%, wetting dispersing agent 1～3%, tackifier 0.5～3%, antifreezing agent 0.5～3%, defoamer 0.5～3%, surplus water are mended to 100%.
As preferred version, Osthole suspension formulation provided by the invention is made by following raw materials by weight percent: Osthole 15～30%, wetting dispersing agent 1～3%, tackifier 1～3%, antifreezing agent 0.5～2%, defoamer 1～3%, surplus water are mended to 100%.
As preferred version, above-described wetting dispersing agent is one or more mixtures in alkyl phenol formaldehyde resin polyoxyethylene ether, alkylbenzenesulfonate, long-chain fatty alcohol APEO, phenethyl phenol polyethenoxy ether, alkylphenol polyoxyethylene, the fatty alcohol sulfate salt, the less Osthole of polarity can be well dispersed in the dispersant after adding wetting dispersing agent, then by in the big solvent of the water-soluble isopolarity of high polarity of dispersant, thereby can solve the problem of the poorly water-soluble of Osthole.
As preferred version, wherein said tackifier are polyvinyl alcohol, xanthans, sodium alginate, xanthan gum or hydroxypropyl methylcellulose.
As preferred version, described antifreezing agent is ethylene glycol, propane diols or glycerine, and described defoamer is organosilicon or polyethers.Add antifreezing agent preparation can not solidified at low temperatures, can keep steady quality.
The water-soluble liquor of a kind of Osthole, it is made by following raw materials by weight percent: Osthole 0.1～50%, emulsifier 10～20%, solubilizer 1～15%, retarder thinner 10～20%, the surplus water is mended to 100%.
As preferred version, the water-soluble liquor of Osthole provided by the invention, it is made by following raw materials by weight percent: Osthole 1～50%, emulsifier 10～20%, solubilizer 5～10%, retarder thinner 10～15%, the surplus water is mended to 100%.
As more excellent technical scheme, the water-soluble liquor of Osthole provided by the invention, it is made by following raw materials by weight percent: Osthole 10～35%, emulsifier 10～15%, solubilizer 5～10%, retarder thinner 10～15%, the surplus water is mended to 100%.
As preferred version, water-soluble liquor provided by the invention, described emulsifier are one or more mixtures in alkylphenol polyoxyethylene first condensation product, alkyl polyoxyethylene ether, polyoxyethylene carboxylate, benzylbiphenyl phenol polyethenoxy ether, polyoxyethylene nonylphenol ether, phenethyl phenol polyethenoxy ether, the hungry salt of styrene APEO sulfuric acid, alkylbenzenesulfonate, the alkane naphthalene sulfonate.The present invention selects the emulsifier of nonionic and ionic for use, when emulsifier is dispersed in dispersate surperficial, can form film or electric double layer, can make disperse phase have electric charge, so just can stop the droplet of disperse phase to condense mutually, makes the emulsion of formation more stable.After the Osthole lower polarity joined in the emulsifier, Osthole was dissolved in emulsifier and obtains transparent liquid.
As preferred version, water-soluble liquor provided by the invention, described solubilizer can be one or more in polyvinyl alcohol, neopelex, the Tween-80, can improve the water-soluble of Osthole after adding solubilizer, the present invention preferably can increase the water-soluble of Osthole, but can not destroy polyvinyl alcohol, neopelex or the Tween-80 of Osthole structure.As preferred version, described retarder thinner is a kind of in ketone, alcohols or the aromatic hydrocarbon or their mixture, as acetone, butanone, cyclohexanone, and methyl alcohol, ethanol, propyl alcohol etc.The dissolubility of alcohol compound is good, can make the Osthole dissolving, and alcohol compound again can the big solvent of water-soluble isopolarity, therefore add thinner such as ethanol and cooperate the solubilization of solubilizer again, can make polarity low, the water-soluble enhancing of structural unstable Osthole, and structure can keep stable.
A kind of Osthole microemulsion, it is made by following raw materials by weight percent: Osthole 0.1～50%, emulsifier 5～20%, antifreezing agent and stabilizing agent 0.1～5%, retarder thinner 10～30%, the surplus water is mended to 100%.
As preferred version, Osthole microemulsion provided by the invention, it is made by following raw materials by weight percent: Osthole 1～50%, emulsifier 5～15%, antifreezing agent and stabilizing agent 1～5%, retarder thinner 15～30%, the surplus water is mended to 100%.
As preferred version, Osthole microemulsion provided by the invention, it is made by following raw materials by weight percent: Osthole 10～40%, emulsifier 10～15%, antifreezing agent and stabilizing agent 1～3%, retarder thinner 15～30%, the surplus water is mended to 100%.
As preferred version, wherein said emulsifier is one or more mixtures in styryl phenol APEO, phenethyl phenol polyethenoxy polyethenoxy ether, alkylphenol polyoxyethylene formaldehyde condensation products, phenethyl agglomeration oxygen vinethene formaldehyde condensation products, the calcium dodecyl benzene sulfonate.The present invention selects the emulsifier of nonionic and ionic for use, when emulsifier is dispersed in dispersate surperficial, can form film or electric double layer, can make disperse phase have electric charge, so just can stop the droplet of disperse phase to condense mutually, makes the emulsion of formation more stable.After the Osthole lower polarity joined in the emulsifier, Osthole can fully be dissolved in emulsifier and obtain transparent liquid.
As preferred version, described antifreezing agent and stabilizing agent are ethylene glycol, propane diols or glycerine, add antifreezing agent and stabilizing agent after Osthole water-based microemulsion have good antifreezing effect, good stability especially can long term storage.
As preferred version, described retarder thinner is a kind of in ketone, alcohols or the aromatic hydrocarbon or their mixture, as acetone, butanone, cyclohexanone, and methyl alcohol, ethanol, propyl alcohol etc.The dissolubility of alcohol compound is good, can make Osthole dissolving, and alcohol compound again can the big solvent of water-soluble isopolarity, and therefore add thinner such as ethanol and can make polarity low, the water-soluble enhancing of structural unstable Osthole, and structure can keep stable.
Osthole suspension formulation provided by the invention, water-soluble liquor or microemulsion are in the application of the powdery mildew that is used for preventing and treating melon and fruit, vegetables, cereal crop, downy mildew, anthracnose, gray mold.
As preferred version, Osthole suspension formulation provided by the invention, water-soluble liquor or microemulsion are especially in use in the application in control cucumber, pumpkin, custard squash, watermelon, balsam pear, muskmelon, strawberry, apple, grape, banana, mango, capsicum, tomato powdery mildew, the downy mildew.
The preparation method of Osthole suspension formulation: the former medicine of Osthole and wetting dispersing agent, tackifier, antifreezing agent, defoamer and a spot of water are mixed stirring, after stirring material is joined sand mill and carry out sand milling, water is mended to 100% then, and sand milling makes material reach the requirement granula and promptly obtains suspending agent again.
The preparation method of the water-soluble liquor of Osthole with the former medicine of Osthole and emulsifier, solubilizer and retarder thinner, mixes and stirs, and after stirring, water is mended to 100% then, and is fully miscible again, promptly gets the water-soluble liquor of Osthole.
The preparation method of Osthole microemulsion, with the former medicinal solvent dissolving of Osthole, treat to stir after it fully dissolves, add emulsifier, antifreezing agent and stabilizing agent during stirring, after treating above-mentioned system mixing, again water is slowly added in the above-mentioned mixed liquor, stir again and promptly get the microemulsion product.
Beneficial effect: Osthole suspension formulation provided by the invention, water-soluble liquor and microemulsion, with the Osthole is main active, through lot of experiments, having added can increase the water miscible cosolvent of Osthole and can make the stability-enhanced stabilizing agent of Osthole, and each component is carried out scientific matching, the water base property of the Osthole that obtains preparation, comprise Osthole suspension formulation, water-soluble liquor and microemulsion, the good water solubility of these three kinds of preparations, solved the Osthole poorly water-soluble, problem that can not extensive use.
And studies show that through stability experiment Osthole suspension formulation provided by the invention, water-soluble liquor and microemulsion have good stability, show active component Osthole good stability in these three kinds water base property preparations, be difficult for losing efficacy; Simultaneously through the crop antibacterial experiment is shown, Osthole suspension formulation provided by the invention, water-soluble liquor and microemulsion have good control efficiency to powdery mildew and downy mildew etc., and the toxicity that further shows the water base property of Osthole provided by the invention preparation through toxicity test research is low, safe in utilization.
Embodiment
Below in conjunction with specific embodiment, further illustrate the present invention, should understand these embodiment only is used to the present invention is described and is not used in and limit the scope of the invention, after having read the present invention, those skilled in the art all fall within the application's claims institute restricted portion to the modification of the various equivalent form of values of the present invention.
Embodiment 1
The Osthole suspension formulation is made up of following materials: Osthole 15%, wetting dispersing agent: alkyl phenol formaldehyde resin polyoxyethylene ether 1.5%, tackifier: xanthans 0.5%, antifreezing agent: ethylene glycol 1%, defoamer: organosilicon 1.5%, surplus are that water is mended to 100%.(lot number 01)
Embodiment 2
The Osthole suspension formulation is made up of following materials: Osthole 1%, wetting dispersing agent: alkylbenzenesulfonate 1%, tackifier: polyvinyl alcohol 1%, antifreezing agent: propane diols 0.3%, defoamer: polytrimethylene ether 2%, surplus are that water is mended to 100%.(lot number 02)
Embodiment 3
The Osthole suspension formulation is made up of following materials: Osthole 40%, wetting dispersing agent: phenethyl phenol polyethenoxy ether 5%, tackifier: sodium alginate 4%, antifreezing agent: glycerine 3%, defoamer: poly-propyl ether 4%, surplus are that water is mended to 100%.(lot number 03)
Embodiment 4
The water-soluble liquor of Osthole is made up of following materials: Osthole: retarder thinner 30%: ethanol 15%, solubilizer: polyvinyl alcohol 8%, emulsifier: phenethyl phenol polyethenoxy ether 18%, surplus are that water is mended to 100%.(lot number 04)
Embodiment 5
The water-soluble liquor of Osthole is made up of following materials: Osthole: solvent 1%: ethanol 10%, solubilizer: neopelex 10%, emulsifier: the hungry salt 15% of styrene APEO sulfuric acid, surplus are that water is mended to 100%.(lot number 05)
Embodiment 6
The water-soluble liquor of Osthole is made up of following materials: Osthole: retarder thinner 15%: acetone 15%, solubilizer: 6% Tween-80, emulsifier: polyoxyethylene nonylphenol ether 12%, surplus are that water is mended to 100%.(lot number 06)
Embodiment 7
The Osthole microemulsion is made up of following materials: Osthole 50%, retarder thinner: ethanol 20%, emulsifier: alkylphenol polyoxyethylene formaldehyde condensation products 15%, antifreezing agent: glycerine 0.2%, surplus are that water is mended to 100%.(lot number 07)
Embodiment 8
The Osthole microemulsion is made up of following materials: Osthole 1%, retarder thinner: acetone 30%, emulsifier: styryl phenol APEO 10%, antifreezing agent and stabilizing agent: propane diols 2%, surplus are that water is mended to 100%.(lot number 08)
Embodiment 9
The Osthole microemulsion is made up of following materials: Osthole 15%, retarder thinner: toluene 30%, emulsifier: alkylphenol polyoxyethylene formaldehyde condensation products 20%, antifreezing agent and stabilizing agent: ethylene glycol 3%, surplus are that water is mended to 100%.(lot number 09)
Embodiment 10: concentration is the toxicity test experience of 50% Osthole suspension formulation, water-soluble liquor and microemulsion
The desired SOP system of this test basis State Standard of the People's Republic of China GB 15670-1995 " agriculture chemical registration toxicology test method " designs and implements.Testing result is as follows:
The toxicity testing result of 50% Osthole suspension formulation:
Rat acute per os LD
50 
Belong to the micro-virus kind agricultural chemicals
♀＞5000mg/Kg belongs to the micro-virus kind agricultural chemicals
Rat acute is through skin LD
50 Belong to the micro-virus kind agricultural chemicals
♀＞5000mg/Kg belongs to the micro-virus kind agricultural chemicals
It is 4 (1h) that lagophthalmos stimulates integration, is 0 (1: 100) dilution behind the 48h
To the eye nonirritant.
It is 0 (4h) that the rabbit skin stimulates integration, to the skin nonirritant.
Skin allergic reaction sensitization rate is 0, belongs to weak sensitizer.
The toxicity testing result of the water-soluble liquor of 50% Osthole:
Rat acute per os LD
50 Belong to the micro-virus kind agricultural chemicals
♀＞5000mg/Kg belongs to the micro-virus kind agricultural chemicals
Rat acute is through skin LD
50 
Belong to the micro-virus kind agricultural chemicals
♀＞5000mg/Kg belongs to the micro-virus kind agricultural chemicals
It is 4 (1h) that lagophthalmos stimulates integration, is 0 (1: 100) dilution behind the 48h
To the eye nonirritant.
It is 0 (4h) that the rabbit skin stimulates integration, to the skin nonirritant.
Skin allergic reaction sensitization rate is 0, belongs to weak sensitizer.
The toxicity testing result of 50% Osthole microemulsion:
Rat acute per os LD
50 
Belong to the micro-virus kind agricultural chemicals
♀＞5000mg/Kg belongs to the micro-virus kind agricultural chemicals
Rat acute is through skin LD
50 
Belong to the micro-virus kind agricultural chemicals
♀＞5000mg/Kg belongs to the micro-virus kind agricultural chemicals
It is 4 (1h) that lagophthalmos stimulates integration, is 0 (1: 100) dilution behind the 48h
To the eye nonirritant.
It is 0 (4h) that the rabbit skin stimulates integration, to the skin nonirritant.
Skin allergic reaction sensitization rate is 0, belongs to weak sensitizer.
Drawn by above toxicity test result, concentration provided by the invention is that the toxicity of 50% Osthole suspension formulation, water-soluble liquor and microemulsion is lower, at the rat acute per os with in sturdy testing, and LD
50All, belong to the micro-virus kind agricultural chemicals, meet national standard less than 5000mg/kg.
Embodiment 11:1%, 15% Osthole suspending agent are to the control efficiency of cucumber downy mildew
1 experimental scheme and arrangement
1.1 medicament
1.1.1 test medicine
1% Osthole suspending agent: lot number 002 and 15% Osthole suspending agent: lot number 001.
1.1.2 contrast medicament
Jules Rimet (69% dimethomorph wetting powder, give birth to farmingization Co., Ltd and produce, LS20040833) by the Qingdao profit
1.1.3 dosing and processing numbering
Table 1 reagent agent experimental scheme
| Handle numbering | Medicament | Formulation rate (active ingredient amount) |
| ??A 1 | 1%, 15% Osthole suspending agent | ??30g/hm 2 |
| ??A 2 | 1%, 15% Osthole suspending agent | ??22.5g/hm 2 |
| ??A 3 | 1%, 15% Osthole suspending agent | ??18g/hm 2 |
| ??A 4 | Jules Rimet | ??714.15g/hm 2 |
| ??A 5 | Blank | ??/ |
1.1.4 sub-district area and repetition
Sub-district area: 18.90m
2
Number of repetition: repeat 4 times
1.2 application method
1.2.1 using method
Weigh up by the sub-district area and respectively to handle medicament and convert water cucumber blade face even spraying.
1.2.3 spraying equipment
Sharp agricultural HD400 type knapsack hand sprayer.
1.2.4 spraying time and number of times
Whole test dispenser twice altogether is respectively at executing medicine for the first time on June 30th, 2009; Executed medicine for the second time on July 10th, 2009.
2 investigation methods, time and number of times
2.1 control time and number of times
Investigate altogether twice.Spray for the first time each sub-district morbidity radix of the medicine same day (June 30) investigation earlier; 7 days drug effect after the dispenser of investigation on July 17 secondary.
2.2 investigation method
Every sub-district is 5 samplings at random, every fixed two strains, every strain from the bottom the 3rd leaf up investigate 10 leaves.The investigation standard is as the criterion according to GB/T17980.26-2000 in " field control effectiveness test criterion (-) ".Sick level is divided into nine grades in the ratio that lesion area accounts for blade area:
0 grade: no scab;
1 grade: lesion area accounts for below 5% of whole leaf area;
3 grades: lesion area accounts for 6%～10% of whole leaf area;
5 grades: lesion area accounts for 11%～25% of whole leaf area;
7 grades: lesion area accounts for 26%～50% of whole leaf area;
9 grades: lesion area accounts for more than 50% of whole leaf area.
2.3 drug effect computational methods
Disease index and control efficiency are calculated respectively as follows.
In the formula: CK
0Disease index before the dispenser of-blank district; CK
1Disease index after the dispenser of-blank district;
PT
0Disease index before the dispenser of-chemicals treatment district; PT
1Disease index after the dispenser of-chemicals treatment district.
Table 1 1% and 15% Osthole suspending agent control cucumber downy mildew test result of the test
As can be seen from Table 1, reagent agent 1%, 15% Osthole suspending agent all has good control efficiency to cucumber downy mildew, and preventive effect improves with the increase of handling dosage.Wherein 15% Osthole suspending agent 30,22.5,18g/hm
2With contrast medicament Jules Rimet 714.15g/hm
2, the preventive effect to cucumber downy mildew behind twice medicine is respectively 76.94%, 72.53%, 66.81% and 79.29%.The result who preventive effect is carried out variance analysis shows: 15% Osthole suspending agent 30g/hm
2Preventive effect and contrast medicament Jules Rimet 714.15g/hm to cucumber downy mildew
2Preventive effect suitable, difference is not remarkable; 15% Osthole suspending agent 30g/hm
2To the preventive effect of cucumber downy mildew be higher than 22.5,18g/hm
2Preventive effect, significant difference; 15% Osthole suspending agent 22.5,18g/hm
2Preventive effect significant difference between processing.
Embodiment 12 1%, the water-soluble liquor of 30% Osthole are to the control efficiency of powdery mildew of strawberry
1 experimental scheme and arrangement:
1.1 medicament
1.1.1 test medicine and treatment dosage
The water-soluble liquor of 1% Osthole (lot number 05), the water-soluble liquor of 30% Osthole (lot number 04), chemicals treatment is: the water-soluble liquor 22.5g/hm of 1% and 30% Osthole
2, 18.0g/hm
2, 15.0g/hm
2
1.1.2 contrast medicament
The contrast chemicals treatment is 10% generation high-moisture shot agent 45.0g/hm
2, just reach earlier (China) Investment Co., Ltd and produce.
1.2 arrange the sub-district
13.2.1 arrange the sub-district: randomized arrangement is adopted in the experimental plot.
1.2.2 sub-district area and repetition
If 3 processing of test medicine, contrast medicament 1 processing, 1 processing of blank repeats for 4 times, totally 20 sub-districts, sub-district area 18m
2, establish guard row.
1.3 insecticide-applying way
1.3.1 spraying time and number of times
At the strawberry initial bloom stage, the blade powdery mildew begins medication when sporadicly taking place, and the fruit morbidity is zero, and administration time is respectively on November 11st, 2009, November 18, November 23, shared medicine 3 times.Fine during dispenser, do not have in the canopy and reveal.
2 investigation
2.1 investigation method and grade scale
Only sporadicly take place on the powdery mildew of strawberry blade in early stage in the experimental field, powdery mildew mainly occurs on the fruit.Because morbidity is lighter, each handles the whole fruits of investigation.The killed stage division of strawberry fruit:
0 grade: no scab
1 grade: scab accounts for below 5% of whole fruit area; 3 grades: scab accounts for 6%～15% of whole fruit area;
5 grades: scab accounts for 16%～25% of whole fruit area; 7 grades: scab accounts for 26%～50% of whole fruit area;
9 grades: scab accounts for more than 51% of whole fruit area.
2.2 control time and number of times
The fruit morbidity is zero before the dispenser, last investigation on back 6 days (November 29) strawberry fruit incidence, and duration of test is investigated once altogether.
2.3 survey data and calculating
Respectively handle the state of an illness according to above stage division record, calculate disease leaf (really) rate, disease index, suitable preventive effect, The data Deng Kenshi duncan's new multiple range method (DMRT) carries out statistical analysis.
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Table 2 1% and the water-soluble liquor of 30% Osthole are to the control efficiency of powdery mildew of strawberry
From table 2 experimental result as can be seen, the water-soluble liquor 22.5,18 of reagent agent 1% and 30% Osthole, 15g/hm
2Three treatment dosage all have the better prevention effect, the water-soluble liquor 22.5,18 of 30% Osthole, 15g/hm to the fruit face of powdery mildew of strawberry
2The control efficiency of three treatment dosage is respectively 90.71%, 80.35% and 69.44%, and drug effect improves with concentration and increases significant difference between the three: contrast medicament 10% generation high-moisture shot agent 45.0g/hm
2Fruit face control efficiency to powdery mildew of strawberry is 81.80%, with the water-soluble liquor 18g/hm of 30% Osthole
2Control efficiency between difference not remarkable, and significantly be lower than the water-soluble liquor 22.5g/hm of 30% Osthole
2Control efficiency, be significantly higher than the water-soluble liquor 15g/hm of 30% Osthole
2Control efficiency.Test medicine 1% and the water-soluble liquor of 30% Osthole have the better prevention effect to powdery mildew of strawberry.In the working concentration scope, there is not poisoning to produce, safe in utilization, can on producing, use, the suggestion working concentration is 22.5-18g/hm
2, 5～6 days at interval, use continuously 3～4 times.
Embodiment 13 1% and 30% Osthole suspension formulation are to the control efficiency of powdery mildew of cucumber
1 experimental scheme and arrangement:
1.1 medicament
1.1.1 test medicine and treatment dosage
1% Osthole suspending agent: lot number 002,15% Osthole suspending agent: lot number 001.Chemicals treatment is: 1%, the Osthole suspending agent of 15% 2 kind of concentration designs 22.5g/hm respectively
2, 18.0g/hm
2, 15.0g/hm
2
1.1.2 contrast medicament
The contrast chemicals treatment is 10% generation high-moisture shot agent 45.0g/hm
2, Syngenta Co.,Ltd produces.
1.2 arrange the sub-district
13.2.1 arrange the sub-district: randomized arrangement is adopted in the experimental plot.
1.2.2 sub-district area and repetition
The Osthole suspending agent of two kinds of concentration is respectively established 3 processing, and the contrast medicament is established 1 processing, and blank is established 1 processing, repeats respectively 4 times, and each concentration Osthole suspending agent is established 20 sub-districts altogether, each sub-district area 18m
2
1.3 insecticide-applying way
1.3.1 spraying time and number of times
During the fragmentary scab of first meeting with medicine (March 15) for the first time, according to PD respectively at March 22, March 29 with second and medicine for the third time, shared medicine three times.
2 investigation
2.1 investigation method and grade scale
Every sub-district is got 4 investigation at random, every some investigation 2 strains, and whole blades are investigated in every strain, account for the percentage classification of whole leaf area by scab on the blade.
Grade scale: 0 grade: no scab; 1 grade: scab accounts for below 5% of whole leaf area; 3 grades: scab accounts for 6%～10% of whole leaf area; 5 grades: scab accounts for 11%～20% of whole leaf area; 7 grades: scab accounts for 21%～40% of whole leaf area; 9 grades: scab accounts for more than 40% of whole leaf area.
2.2 control time and number of times
Be fragmentary morbidity (March 15) before the dispenser, radix is considered as zero; Respectively at 6 days investigation incidences behind 1,3 medicine, duration of test is investigated three times altogether.
2.3 survey data and calculating
Field investigation is respectively handled the disease number of sheets and is write down the state of an illness, calculates disease index, relative control effect according to above stage division, and The data Deng Kenshi duncan's new multiple range method (DMRT) carries out statistical analysis.
3 experimental results
3.1 concentration is 1% Osthole suspending agent the control efficiency of powdery mildew of cucumber is shown in Table 3:
Table 3 1% Osthole suspending agent is to the control efficiency of powdery mildew of cucumber
As can be seen from Table 3,1% Osthole suspending agent 15.0g/hm
2, 18.0g/hm
2, 22.5g/hm
2Three kinds of administering modes increase with concentration the control efficiency of powdery mildew of cucumber and improve, and along with the increase of medication number of times, 1% Osthole suspending agent is also increasing the control efficiency of powdery mildew of cucumber.6 days 1% Osthole suspending agent 22.5g/hm after the medication for the first time
2And 18.0g/hm
2Control efficiency between difference not remarkable, and be significantly higher than 15.0g/hm
2There is significant difference between control efficiency of each processing of Osthole suspending agent in 6 days 1% after the medication for the third time.Contrast medicament 10% generation high-moisture shot agent 45.0g/hm
2Control efficiency in twice investigation, all remain on about 90%, each is handled to be higher than test medicine, but after the medication for the third time with 1% Osthole suspending agent 22.5g/hm
2Control efficiency between difference not remarkable.6 days 1% Osthole suspending agent 22.5g/hm after the medication for the third time
2, 18.0g/hm
2, 15.0g/hm
2Control efficiency to powdery mildew of cucumber is respectively 90.14%, 84.84%, 76.36%, 10% generation high-moisture shot agent 45.0g/hm
2Control efficiency be 93.40%.
To be 15% Osthole suspending agent be shown in Table 4 the control efficiency of powdery mildew of cucumber concentration:
Table 4 15% Osthole suspending agent is to the control efficiency of powdery mildew of cucumber
As can be seen from Table 4,15% Osthole suspending agent 15.0g/hm
2, 18.0g/hm
2, 22.5g/hm
2Three kinds of administering modes increase with concentration the control efficiency of powdery mildew of cucumber and improve, and along with the increase of medication number of times, 15% Osthole suspending agent also increases the control efficiency of powdery mildew of cucumber.6 days 15% Osthole suspending agent 22.5g/hm after the medication for the third time
2, 18.0g/hm
2, 15.0g/hm
2Control efficiency to powdery mildew of cucumber is respectively 91.60%, 86.03%, 78.71%, 10% generation high-moisture shot agent administering mode 45.0g/hm
2Control efficiency be 93.21%.15% Osthole suspending agent 22.5g/hm wherein
2Control efficiency and 10% generation high-moisture shot agent 45.0g/hm
2Control efficiency approaching.
Embodiment 14: the water-soluble liquor of Osthole is to the control efficiency of cucumber downy mildew
1 experimental scheme and arrangement
1.1 medicament
1.1.1 test medicine
The water-soluble liquor of 1% Osthole (lot number 05), the water-soluble liquor of 30% Osthole (lot number 04), chemicals treatment is: the water-soluble liquor 30g/hm of 1% and 30% Osthole
2, 22.5g/hm
2, 18.0g/hm
2
1.1.2 contrast medicament
Jules Rimet (69% dimethomorph wetting powder, give birth to farmingization Co., Ltd and produce, LS20040833) by the Qingdao profit
1.1.3 dosing and processing numbering
| Handle numbering | Medicament | Formulation rate (active ingredient amount) |
| ??1 | The water-soluble liquor of 1% Osthole | ??30g/hm 2 |
| ??2 | The water-soluble liquor of 1% Osthole | ??22.5g/hm 2 |
| ??3 | The water-soluble liquor of 1% Osthole | ??18g/hm 2 |
| ??4 | The water-soluble liquor of 30% Osthole | ??30g/hm 2 |
| ??5 | The water-soluble liquor of 30% Osthole | ??22.5g/hm 2 |
| ??6 | The water-soluble liquor of 30% Osthole | ??18g/hm 2 |
| ??7 | Jules Rimet | ??714.15g/hm 2 |
| ??8 | Blank | ??/ |
1.1.4 sub-district area and repetition
Sub-district area: 18.90m
2, number of repetition: repeat 4 times
1.2 application method
1.2.1 using method
Weigh up by the sub-district area and respectively to handle medicament and convert water cucumber blade face even spraying.
1.2.3 spraying equipment
Sharp agricultural HD400 type knapsack hand sprayer.
1.2.4 spraying time and number of times
Whole test dispenser twice altogether is respectively at executing medicine for the first time on June 30th, 2009; Executed medicine for the second time on July 10th, 2009.
2 investigation methods, time and number of times
2.1 control time and number of times
Investigate altogether twice.Spray for the first time each sub-district morbidity radix of the medicine same day (June 30) investigation earlier; 7 days drug effect after the dispenser of investigation on July 17 secondary.
2.2 investigation method
Every sub-district is 5 samplings at random, every fixed two strains, every strain from the bottom the 3rd leaf up investigate 10 leaves.The investigation standard is as the criterion according to GB/T17980.26-2000 in " field control effectiveness test criterion (-) ".Sick level is divided into nine grades in the ratio that lesion area accounts for blade area:
0 grade: no scab; 1 grade: lesion area accounts for below 5% of whole leaf area; 3 grades: lesion area accounts for 6%～10% of whole leaf area; 5 grades: lesion area accounts for 11%～25% of whole leaf area; 7 grades: lesion area accounts for 26%～50% of whole leaf area; 9 grades: lesion area accounts for more than 50% of whole leaf area.
2.3 drug effect computational methods
Disease index and control efficiency are calculated respectively as follows.
In the formula: CK
0Disease index before the dispenser of-blank district; CK
1Disease index after the dispenser of-blank district;
PT
0Disease index before the dispenser of-chemicals treatment district; PT
1Disease index after the dispenser of-chemicals treatment district.
3 experimental results
3.1 the concrete experimental result of the water-soluble liquor control cucumber downy mildew of 1% Osthole is shown in Table 5:
The water-soluble liquor control of table 5 1% Osthole cucumber downy mildew result of the test
As can be seen from Table 5, the water-soluble liquor of reagent agent 1% Osthole improves with the increase of handling dosage the preventive effect of cucumber downy mildew.The water-soluble liquor administering mode 30,22.5 of 1% Osthole, 18g/hm
2With contrast medicament Jules Rimet administering mode 714.15g/hm
2, the control efficiency to cucumber downy mildew after twice administration is respectively 76.94%, 72.53%, 66.81% and 79.29%.The result who control efficiency is carried out variance analysis shows: the water-soluble liquor of 1% Osthole is at 30g/hm
2Preventive effect and contrast medicament Jules Rimet 714.15g/hm to cucumber downy mildew
2Preventive effect suitable, difference is not remarkable; The water-soluble liquor of 1% Osthole is at 30g/hm
2The time preventive effect of cucumber downy mildew is higher than administering mode 22.5,18g/hm
2, significant difference has statistical significance.
3.2 the concrete experimental result of the water-soluble liquor control cucumber downy mildew of 30% Osthole is shown in Table 6:
The water-soluble liquor control of table 6 30% Osthole cucumber downy mildew result of the test
As can be seen from Table 6, the water-soluble liquor of reagent agent 30% Osthole improves with the increase of handling dosage the control efficiency of cucumber downy mildew.The water-soluble liquor administering mode 30,22.5 of 30% Osthole, 18g/hm
2With contrast medicament Jules Rimet administering mode 714.15g/hm
2, the control efficiency to cucumber downy mildew after twice administration is respectively 82.27%, 76.28%, 74.46 and 82.89%.The result who control efficiency is carried out variance analysis shows: the water-soluble liquor of 30% Osthole is at 30g/hm
2Preventive effect and contrast medicament Jules Rimet 714.15g/hm to cucumber downy mildew
2Control efficiency suitable, difference is not remarkable; The water-soluble liquor of 30% Osthole is at 30g/hm
2The time preventive effect of cucumber downy mildew is higher than administering mode 22.5,18g/hm
2, significant difference has statistical significance.
Embodiment 15 1% and 50% Osthole microemulsion are to the control efficiency of powdery mildew of cucumber
1 experimental scheme and arrangement:
1.1 medicament
1.1.1 test medicine and treatment dosage
1% Osthole microemulsion (lot number 08) and 50% Osthole microemulsion (lot number 07).
Chemicals treatment is: 1% and 50% Osthole microemulsion 22.5g/hm
2, 18.0g/hm
2, 15.0g/hm
2
1.1.2 contrast medicament
The contrast chemicals treatment is 10% generation high-moisture shot agent 45.0g/hm
2, Syngenta Co.,Ltd produces.
1.2 arrange the sub-district
13.2.1 arrange the sub-district: randomized arrangement is adopted in the experimental plot.
1.2.2 sub-district area and repetition
3 processing of test medicine, contrast medicament 1 processing, 1 processing of blank repeats for 4 times, totally 20 sub-districts, sub-district area 18m
2
1.3 insecticide-applying way
1.3.1 spraying time and number of times
During the fragmentary scab of first meeting with medicine (March 15) for the first time, according to PD respectively at March 22, March 29 with second and medicine for the third time, shared medicine three times.
2 investigation
2.1 investigation method and grade scale
Every sub-district is got 4 investigation at random, every some investigation 2 strains, and whole blades are investigated in every strain, account for the percentage classification of whole leaf area by scab on the blade.
Grade scale:
0 grade: no scab
1 grade: scab accounts for below 5% of whole leaf area;
3 grades: scab accounts for 6%～10% of whole leaf area;
5 grades: scab accounts for 11%～20% of whole leaf area;
7 grades: scab accounts for 21%～40% of whole leaf area;
9 grades: scab accounts for more than 40% of whole leaf area.
2.2 control time and number of times
Be fragmentary morbidity (March 15) before the dispenser, radix is considered as zero; 6 days investigation incidences after each medication, duration of test is investigated four times altogether.
2.3 survey data and calculating
Field investigation is respectively handled the disease number of sheets and is write down the state of an illness, calculates disease index, relative control effect according to above stage division, and The data Deng Kenshi duncan's new multiple range method (DMRT) carries out statistical analysis.
??????????????????????????????????????????????????????????????????????
?????????????????????????????????????????????????????????????????????????
3, experimental result: concrete experimental result is shown in table 7 and table 8:
Table 7 1% Osthole microemulsion is prevented and treated the powdery mildew of cucumber result of the test
As can be seen from Table 7, reagent agent 1% Osthole microemulsion improves with the increase of handling dosage the control efficiency of powdery mildew of cucumber.1% Osthole microemulsion insecticide-applying way 30,22.5,18g/hm
2With the high water insecticide-applying way of contrast medicament generation 45.0g/hm
2, the control efficiency to powdery mildew of cucumber after twice dispenser is respectively 85.82%, 82.81%, 73.15% and 83.53%.The result who control efficiency is carried out variance analysis shows: 1% Osthole microemulsion is 30 at administering mode, 22.5g/hm
2The high water 45.0g/hm of medicament generation is shone in control efficiency comparison to powdery mildew of cucumber
2Control efficiency better; 1% Osthole microemulsion 30,22.5g/hm
2The time control efficiency of powdery mildew of cucumber is higher than administering mode 18g/hm
2, significant difference has statistical significance.
Table 8 50% Osthole microemulsion is to the control efficiency of powdery mildew of cucumber
As can be seen from Table 8,50% Osthole microemulsion 15.0g/hm
2, 18.0g/hm
2, 22.5g/hm
2The control efficiency of powdery mildew of cucumber increased with concentration improve, and along with the increase of medication number of times, 50% Osthole microemulsion is also increasing the control efficiency of powdery mildew of cucumber.6 days 50% Osthole microemulsion 22.5g/hm after first and second time medication
2And 18.0g/hm
2Control efficiency between difference not remarkable, and be significantly higher than 15.0g/hm
2There is significant difference between control efficiency of each processing of Osthole microemulsion in 6 days 50% after the medication for the third time.Contrast medicament 10% generation high-moisture shot agent 45.0g/hm
2Control efficiency in three investigation, all remain on about 90%, each is handled to be higher than test medicine, but after the medication for the third time with 50% Osthole microemulsion 22.5g/hm
2Control efficiency between difference not remarkable.6 days 50% Osthole microemulsion 22.5g/hm after the medication for the third time
2, 18.0g/hm
2, 15.0g/hm
2Control efficiency to powdery mildew of cucumber is respectively 90.25%, 85.12%, 76.42%.
The stability experiment research of the water base property of embodiment 16 Ostholes preparation (suspending agent, water-soluble liquor and microemulsion)
Osthole suspending agent provided by the invention, water-soluble liquor and microemulsion the key technical indexes are as shown in table 9
Table 9 Osthole suspending agent, water-soluble liquor and microemulsion the key technical indexes
| Index name | Index |
| Osthole content (%) | ??≥0.1 |
| Index name | Index |
| The pH value | ??6.5～7.2 |
| Stability | Qualified |
| The pourability index | Qualified |
According to the requirement of Chinese Pharmacopoeia stability test guideline, the Osthole suspending agent is carried out quality stability investigate, through 40 ℃ of 6 months (being equivalent to normal temperature 2 years) of acceleration and 12 months study on the stability of long-term stable experiment, the result is shown in table 10 and table 11:
6 months stability experiment results of table 10 accelerated test
Table 11 long-time stability experiment (12 months) result
Conclusion: draw Osthole suspending agent provided by the invention, water-soluble liquor and microemulsion good stability in the long-term stable experiment of 6 months accelerated test and 12 months by table 10 and table 11 experimental result, steady quality, the effective component of osthole Stability Analysis of Structures, can guarantee still to keep good drug effect after the long term storage, and the proterties such as water-soluble of three kinds of preparations meets the requirements.
Osthole suspending agent by above variable concentrations, water-soluble liquor and microemulsion are to the detection of preventive and therapeutic effects such as the powdery mildews of crops and downy mildew, experimental result shows Osthole suspending agent provided by the invention, water-soluble liquor and microemulsion have the effect of good mildew-resistance and downy mildew, the present invention simultaneously is to the Osthole suspending agent of variable concentrations, water-soluble liquor and microemulsion have carried out toxicity test research, experimental result shows that three kinds of preparations of Osthole are little toxicity pesticidal preparations, meet national regulation, in order to investigate the Osthole suspending agent, the stability of water-soluble liquor and microemulsion, pertinent regulations according to Chinese Pharmacopoeia have been carried out the study on the stability experiment, draw three kinds of preparations of Osthole provided by the invention by experimental result and have good stability, can long term storage can not lose efficacy, therefore Osthole suspending agent provided by the invention, water-soluble liquor and microemulsion are expected to exploitation becomes the new generation of green environmental protection, the pesticidal preparations of high-efficiency low-toxicity.
Claims (10)
1. Osthole suspension formulation, it is characterized in that it is made by following raw materials by weight percent: Osthole 0.1～50%, wetting dispersing agent 1～5%, tackifier 0.2～5%, antifreezing agent 0.1～5%, defoamer 0.2～4%, surplus water are mended to 100%.
2. Osthole suspension formulation according to claim 1, it is characterized in that described wetting dispersing agent is one or more mixtures in alkyl phenol formaldehyde resin polyoxyethylene ether, alkylbenzenesulfonate, long-chain fatty alcohol APEO, phenethyl phenol polyethenoxy ether, alkylphenol polyoxyethylene, the fatty alcohol sulfate salt.
3. Osthole suspension formulation according to claim 1 is characterized in that, described tackifier are polyvinyl alcohol, xanthans, sodium alginate, xanthan gum or hydroxypropyl methylcellulose.
4. Osthole suspension formulation according to claim 1 is characterized in that, described antifreezing agent is ethylene glycol, propane diols or glycerine, and described defoamer is organosilicon or polyethers.
5. water-soluble liquor of Osthole, it is characterized in that it is made by following raw materials by weight percent: Osthole 0.1～50%, emulsifier 10～20%, solubilizer 1～15%, retarder thinner 10～20%, the surplus water is mended to 100%.
6. water-soluble liquor according to claim 5, it is characterized in that, described emulsifier is the alkylphenol polyoxyethylene formaldehyde condensation products, alkyl polyoxyethylene ether, polyoxyethylene carboxylate, the benzylbiphenyl phenol polyethenoxy ether, polyoxyethylene nonylphenol ether, the phenethyl phenol polyethenoxy ether, the hungry salt of styrene APEO sulfuric acid, alkylbenzenesulfonate, one or more mixtures in the alkane naphthalene sulfonate, described solubilizer is polyvinyl alcohol, neopelex, in the Tween-80 one or more, described retarder thinner are ketone, a kind of in alcohols or the aromatic hydrocarbon or their mixture.
7. Osthole microemulsion, it is characterized in that it is made by following raw materials by weight percent: Osthole 0.1～50%, emulsifier 5～20%, antifreezing agent and stabilizing agent 0.1～5%, retarder thinner 10～30%, the surplus water is mended to 100%.
8. claim 1 or 2 described Osthole suspension formulations are in the application of the powdery mildew that is used for preventing and treating melon and fruit, vegetables, cereal crop, downy mildew, anthracnose, gray mold.
9. the water-soluble liquor of the described Osthole of claim 5 is in the application of the powdery mildew that is used for preventing and treating melon and fruit, vegetables, cereal crop, downy mildew, anthracnose, gray mold.
10. the described Osthole microemulsion of claim 7 is in the application of the powdery mildew that is used for preventing and treating melon and fruit, vegetables, cereal crop, downy mildew, anthracnose, gray mold.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102007908A (en) * | 2010-12-14 | 2011-04-13 | 江苏农林职业技术学院 | Botanical fungicide for preventing and curing powdery mildew of crops |
| CN103601714A (en) * | 2013-08-21 | 2014-02-26 | 陕西康禾立丰生物科技药业有限公司 | Preparation method of cnidium lactone aqueous preparation and composition of the cnidium lactone aqueous preparation |
| CN104488869A (en) * | 2014-11-28 | 2015-04-08 | 江苏省农药研究所股份有限公司 | Bactericidal composition of 2-cyano-3-amino-3-ethyl phenylacrylate and cnidium lactone |
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| CN102007908A (en) * | 2010-12-14 | 2011-04-13 | 江苏农林职业技术学院 | Botanical fungicide for preventing and curing powdery mildew of crops |
| CN102007908B (en) * | 2010-12-14 | 2013-04-24 | 江苏农林职业技术学院 | Botanical fungicide for preventing and curing powdery mildew of crops |
| CN103601714A (en) * | 2013-08-21 | 2014-02-26 | 陕西康禾立丰生物科技药业有限公司 | Preparation method of cnidium lactone aqueous preparation and composition of the cnidium lactone aqueous preparation |
| CN103601714B (en) * | 2013-08-21 | 2016-12-21 | 陕西康禾立丰生物科技药业有限公司 | Osthole water preparation preparation method and combinations thereof thing |
| CN104488869A (en) * | 2014-11-28 | 2015-04-08 | 江苏省农药研究所股份有限公司 | Bactericidal composition of 2-cyano-3-amino-3-ethyl phenylacrylate and cnidium lactone |
| CN106342833A (en) * | 2016-08-29 | 2017-01-25 | 田文华 | Sterilized composition containing fluoxastrobin and cnidium lactone |
| CN106342833B (en) * | 2016-08-29 | 2018-11-30 | 东阳市天齐知识产权运营有限公司 | A kind of bactericidal composition containing fluoxastrobin and Osthole |
| CN110278970A (en) * | 2019-07-31 | 2019-09-27 | 黑龙江省农业科学院植物保护研究所 | A kind of Chinese herbal medicine type seed coat agent and preparation method thereof |
| CN115053905A (en) * | 2022-07-08 | 2022-09-16 | 河北上瑞生物科技有限公司 | Pesticide composition, method and application |
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