CN103141488A - Pesticide compounded by azadirachtin and cnidium lactone and preparation method thereof - Google Patents
Pesticide compounded by azadirachtin and cnidium lactone and preparation method thereof Download PDFInfo
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Abstract
A pesticide compounded by azadirachtin and cnidium lactone comprises the raw material medicines in parts by weight as follows: 0.1-5 parts of azadirachtin, 0.1-5 parts of cnidium lactone, 5-15 parts of an emulsifying agent; 1-6 parts of a dispersing agent, 0.5-2 parts of an antioxidant agent, 0.5-1 part of a stabilizing agent, 0.5-10 parts of a penetrating agent, 1-10 parts of an antifreeze agent, 1-3 parts of a defoaming agent, and a bamboo vinegar or a wood vinegar is added to obtain 100 parts. The pesticide is prepared by six steps including the filtration of bamboo (wood) vinegar, the preparation of an oil phase, an aqueous phase and a mixed solution, and the preparation of an insecticide suspension emulsion; the pesticide is mainly applied to the prevention of contarinia pyrivora, the synergism effect is remarkable, and the prevention and treatment efficiency in the fields is excellent; and the pesticide does not enable insects to generate resistance to drugs for long-term use, can be decomposed automatically, and is safe, efficient, free from pollution, low in cost and good in persistence.
Description
Technical field
The present invention relates to a kind of be mainly used in the pest such as control pears cecidomyiia with insecticide of plant resource nimbin and fructus cnidii complex and preparation method thereof.
Background technology
China's pear tree area under cultivation and output all occupy first place in the world, and according to FAO (Food and Agriculture Organization of the United Nation) (FAO) statistics, Chinese pear tree harvest area in 2009 is 125.8 ten thousand hm
2, account for 72.3% of world's pears gross area; The gross annual output amount is 1438.8 ten thousand t, accounts for 65.7% of Gross World Product.The pears cecidomyiia was the pear tree minor pests in the past, caused harm lighter, but in recent years all occured seriously to have become the primary pest of pears in the main pears of China producing regions, easily caused the pear tree early leaf fall and obviously affected yield and quality.At present control pears cecidomyiia is mainly spraying chemical insecticides such as killing chrysanthemum ester, Imidacloprid as main, but chemical control easily develops immunity to drugs, and can't use in Organic pear orchard.
Nimbin is the vegetable insecticide that extracts from seal chinaberry (Azadirachta indicaA.Juss) tree, and its sterling is white amorphous substance, is soluble in methyl alcohol, ethanol, acetone, methyl-sulfoxide isopolarity organic solvent.Nimbin is outstanding biopesticide recognized in the world, be one of Typical Representative of botanical pesticide, to insect food refusal is arranged, disturb lay eggs, the interference insect variation, it can't be changed in quality reach the desinsection purpose for adult, repellent larva and the effect that suppresses its growth, being widely used in preventing and treating the various pests on the crops such as vegetables, fruit tree, is a kind of efficient, low-residual and high selectivity and the harmless boilogical agricultural chemicals that is difficult for developing immunity to drugs.To people, animal, birds and honeybee safety, to predatism and parasite disturb less, without obviously poisoning, easily degraded in environment.China's South Guangdong, Hainan, Yunnan and some areas, Sichuan are establishing in large scale seal chinaberry, and the nimbin raw material can be self-supporting, cost, seal chinaberry preparation answer the apparatus realistic meaning.
Osthole is present in the extract of Umbelliferae annual herb plant cnidium monnieri (Cnidium monnieri (L) Cuss.) fruit in a large number, its sterling is the white, needle-shaped crystals powder, be soluble in methyl alcohol, ethanol, chloroform, acetone and ethyl acetate etc., water insoluble and benzinum.
Botanical pesticide with the Osthole preparation, it is all had to various pests such as beet armyworm, tea geometrid, Colcaphellusbowringi, various aphids the effect of tagging significantly as insecticide, its mode of action is take action of contace poison as main, stomach poison function is auxiliary, liquid enters in insect bodies by External absorbability, act on the insect nervous system, cause insect muscle non-functional to shrink, finally die of exhaustion.Osthole is difficult for producing anti-medicine to people and animals and other mammalian safe, easily degraded in environment.Osthole and multiple biopesticide and/or chemical pesticide be composite obvious synergistic effect.
Cnidium monnieri all has distribution as traditional Chinese medicine in China's most area, main product in Zhejiang, the ground such as Jiangsu, Hebei, Shandong, raw material sources are extensive, the cost relative reduce, its preparation is extensive as the biological insecticides application prospect.
Nimbin and Osthole are used for control pears cecidomyiia and yet there are no report.The present invention uses separately and composite rear Toxicity Determination and field efficiency test to the pears cecidomyiia by research botanical pesticide nimbin and Osthole, estimate the composite effect of this two Plants source pesticide, and then verify reasonable compound proportion, inquire into the control efficiency of nimbin and fructus cnidii complex, with reach reduce Pesticide environment pollute, reduce pest resistance to insecticide and purpose.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of nimbin for control pears cecidomyiia and insecticide of fructus cnidii complex and preparation method thereof.
Solve the problems of the technologies described above by the following technical programs and be achieved:
This nimbin is coordinated by following raw materials according and weight portion thereof with the insecticide of fructus cnidii complex and forms: 0.1～5 part of nimbin, Osthole 0.1-5 part, 5～15 parts of solvents, 5～15 parts of emulsifier, 1～6 part of dispersant, 0.5～2 part of antioxidant, 0.5～1 part of stabilizing agent, 0.5～10 part of bleeding agent, antifreeze 1-10 part, as 1～3 part of the organosilicon of defoamer, add bamboo vinegar or pyroligneous liquor to 100 part.
The weight portion preferred proportion of described nimbin and Osthole is (5～1): (1-2), optimal proportion is 2: 1.
Described solvent is quality is at least a in 98% ethanol, 95% acetone, 95% isopropyl alcohol than concentration.
Described emulsifier is quality is at least a in 99% polyoxyethylene sorbitan fatty acid ester, 99% sorbitan fatty acid ester, 99% castor oil polyoxyethylene ether, 99% polyoxyethylene fatty acid ester, sodium lignin sulfonate, desugar condensation sodium lignin sulfonate than concentration.
Described dispersant is Sodium Polyacrylate, quality is at least a in 99% propane diols polyoxyethylene poly-oxygen propylene aether, 99% block polyoxyethylene polyoxypropylene ether, glycerine polyoxyethylene polyoxypropylene blocked copolymer, alkylphenol polyoxyethylene formaldehyde condensation products sodium sulphate than concentration.
Described antioxidant is that quality is any in 90% vitamin e, sodium sulphite or ascorbic acid than concentration.
Described stabilizing agent is that methylcellulose, sodium carboxymethylcellulose, hydroxypropyl cellulose, xanthans, tertiary sodium phosphate, sorb sodium alkoxide, quality are at least a in 98% epoxidised soybean oil than concentration.
Described bleeding agent is quality is at least a in 99% azone, 99% fatty alcohol-polyoxyethylene ether, 99% isomerous tridecanol polyoxyethylene ether, disecoctylmaleate sodium sulfonate than concentration.
Described antifreezing agent is quality is 99% propane diols, 98% glycerine, 95% ethylene glycol, 98% polyethylene glycol or any in sorbierite than concentration.
This nimbin comprises the steps: with the method for producing insecticide of fructus cnidii complex
(1) bamboo vinegar or this vinegar liquid are filtered after standing 5～8 months, collect as mother liquor;
(2) nimbin, Osthole and antioxidant are joined in solvent dissolve in proportion, mix by colloid mill, make oil phase;
(3) add a small amount of step (1) gained bamboo vinegar or pyroligneous liquor stirring and dissolving in emulsifier, make water;
(4) water is added oil phase, mix by colloid mill;
(5) add respectively a small amount of step (1) gained bamboo vinegar or pyroligneous liquor stirring and dissolving in other auxiliary agent, add step (4) gained mixture, be ground;
(6) add step (1) gained bamboo vinegar or pyroligneous liquor to 1100 part in the mixed liquor that makes to step (5), make desinsection suspension emulsion of the present invention after stirring evenly.
The invention has the beneficial effects as follows:
Two kinds of main active ingredients of this insecticide are nimbin and Osthole, all derive from plant, Environmental compatibility is good, toxicity is low, easy degraded, has higher safety than chemical insecticide, is the desirable agricultural chemicals of the organic fruit industry of development, the sustainable development of promotion fruit tree industry.
After two kinds of main active ingredient nimbins of this insecticide and fructus cnidii complex synergistic effect is remarkable, not only improved the preventive effect to the pears cecidomyiia, also greatly reduced the consumption of nimbin and Osthole, thereby reduced cost accounting.Nimbin to insect food refusal is arranged, disturb lay eggs, interference insect variation effect; Take action of contace poison as main, stomach poison function is auxiliary to Osthole to insect.Two kinds of modes of action complement each other, and insect is difficult for developing immunity to drugs.
Main auxiliary agent bamboo vinegar or the pyroligneous liquor of this insecticide have several functions, and the tissue of plant is had good permeability and absorbability, can improve the effect of the applications of pesticide, and can reduce formulation rate.The present invention's raw material used is easy to get, and is non-harmful material, and is harmless to human body and crop.
Embodiment
Following the present invention is described in further detail in conjunction with nine embodiment, and the raw material type of every embodiment and weight portion proportioning value thereof are as shown in table 1.
embodiment 1: raw material and the weight portion ratio thereof of pressing embodiment 1 correspondence in table 1, first the bamboo vinegar of capacity or pyroligneous liquor are filtered after standing 5～8 months and make mother liquor, again with 0.1 part of nimbin, 0.1 part Osthole and 0.5 part of antioxidant join in 5 parts of organic solvents and dissolve, after being mixed, colloid mill makes oil phase, add a small amount of bamboo (wood) vinegar liquid again in 5 parts of emulsifier, make water after stirring evenly, water and oil phase are passed through the colloid mill mixing, again other auxiliary agent of remainder is added respectively a small amount of bamboo vinegar or pyroligneous liquor by separately weight portion, this mixture and water oil mixture are mixed again, be ground in colloid mill, at last remaining bamboo (wood) vinegar liquid is added entirely, make total addition of bamboo (wood) vinegar liquid reach 85.3 parts, make this desinsection suspension emulsion after stirring evenly.
All the other embodiment 2～9 all by raw material and the weight portion ratio thereof of corresponding embodiment in table 1, make with the method identical with embodiment 1, and wherein embodiment 4 is preferred.Nine embodiment raw material types of table 1 and weight portion proportioning value thereof
The below is with the Toxicity Determination experiment relevant with the application and comprise that the situation of the field control effect test of five experimental examples makes a presentation:
1, Toxicity Determination experiment
1.1 materials and methods
1.1.1 examination worm
The pears cecidomyiia is picked up from the field, and laboratory picking in the same size, 2 healthy instar larvaes are done the examination worm.
1.1.2 reagent agent
25% nimbin, south, Yunnan precious plant Co., Ltd; 20% Osthole, sky, Xi'an this biotechnology Co., Ltd.Reagent agent nimbin (A) and Osthole (B) are with acetone solution and be diluted to the 1000mg/L mother liquor.Between nimbin and Osthole, (A: B) 5: 1,3: 1,2: 1,1: 1,1: 2,1: 3, compound proportion was diluted to 5 concentration gradient liquids in 1: 5 in mass ratio respectively.
1.2 assay method
Press the method that NY/T1154.7-2006 recommends, supply reagent liquid in 2 instar larvae chest backboards with the micro syringe drop, every processing repeats for 4 times, and 30 of every repetitions are done contrast with acetone treatment, inspection record death condition after 4d.Co-toxicity coefficient (CTC value) was synergistic effect greater than 120 o'clock, and 80≤CTC≤120 are summation action, was antagonism less than 80 o'clock.
1.3 toxicity test result
Adopt drop method to nimbin and Osthole different proportion the virulence after composite measure.Result shows, nimbin and Osthole optimum ratio be 5: 1,3: 1,, 1: 1,1: 2, their co-toxicity coefficient shows the notable synergistic effect all greater than 120, wherein best proportioning is 2: 1, co-toxicity coefficient is 233.46 (tables 2).
Table 2 nimbin and fructus cnidii complex toxicity test
2, example
Preparation 3%, 2%, 1.5%, 0.5% and 1.8% 5 kind of nimbin Osthole suspension emulsion, these five compounded pesticides examples are all prepared each component according to the weight portion in table 3, and all components is commercial conventional pesticide raw material and auxiliary agent.
The preparation method of example one compounded pesticides is:
(1) bamboo (wood) vinegar liquid is filtered after standing 5～8 months, collect as mother liquor.
(2) proportionally nimbin, Osthole and vitamin e are joined as dissolving in the ethanol of solvent and acetone, mix by colloid mill, make oil phase; Colloid mill is not done specific (special) requirements, can reach the uniform effect of mixed house and get final product.
(3) toward as adding appropriate step (1) gained bamboo (wood) vinegar liquid stirring and dissolving in the polyoxyethylene sorbitan fatty acid ester of emulsifier, castor oil polyoxyethylene ether, make water.
(4) water is added oil phase, mix by colloid mill.
(5) add respectively appropriate step (1) gained bamboo (wood) vinegar liquid stirring and dissolving in other auxiliary agent, then add step (4) gained mixture, be ground;
(6) add step (1) gained bamboo (wood) vinegar liquid to full dose in the mixed liquor that makes to step (5), stir evenly and namely get 3% nimbin Osthole suspension emulsion.
The raw material type of five examples of table 3 and weight portion proportioning value thereof
Example two, three, four, five all by separately raw material and weight portion ratio thereof in table 3, is made with the preparation method identical with example one.
3, field efficacy evaluation test
The field efficacy evaluation test is preced with the theatre Zhejiang Province's Yuhang District kingfisher and is carried out.Reagent agent is nimbin and fructus cnidii complex example one, example two, example three, example four and five dose out powders of example, all by 15,45, the 90mg/L drug concentration sprays; With 0.5% nimbin emulsion (Yunnan bright Neem industry exploitation limited company produces) and 0.4% Osthole EC (sky, Wuhan City, Hubei Province favour biotechnology Co., Ltd) (two pharmacy application concentration be 15,45,90mg/L), and 10% imidacloprid wettable powder (Shanghai east wind insecticide factory) (application concentration 67mg/L) be the contrast medicament, and establish clear water contrast (CK).
Randomised block design, 3 strain pear trees are processed in every residential quarter, and every processing repeats 3 times.Spraying time is the larva harm initial stage on April 19th, 2012.Before the spray medicine every tree press East, West, South, North, in 1 of 5 prosperous extending shoot of the random listing mark in orientation, investigate the insect population radix; First with being watered spraying after a small amount of water-soluble solution reagent agent, spraying equipment adopts MATABI Super Green16 type knapsack sprayer again, operating pressure 2.0 bar, reverse side even medicine, till dripping.Respectively at after the spray medicine 1,5, the 10d investigation borer population of living calculates insect population decline rate and preventive effect, and computing formula is as follows:
Borer population * 100 before insect population decline rate (%)=(borer population after the front borer population of spray medicine-spray medicine)/spray medicine;
Preventive effect (%)=(processing insect population decline rate-contrast insect population decline rate)/(100-contrast insect population decline rate) * 100.
As shown in Table 4, after 5 nimbins and fructus cnidii complex insecticide spray medicine, the preventive effect of 1d is 55.76%～85.56%, is up to example five compounded pesticides (the Osthole ratio is the highest), and this may be main with Osthole action of contace poison; After the spray medicine, the 5d preventive effect is 69.33%～91.16%, is up to example three compounded pesticides (nimbin and Osthole ratio are 2: 1); After the spray medicine, the 10d preventive effect is 78.41%～94.16%, and the highest is still example three compounded pesticides.After 5 nimbins and fructus cnidii complex insecticide spray medicine, 10d anti-put all the preventive effect higher than 0.5% nimbin and 0.4% Osthole, and this illustrates that nimbin and fructus cnidii complex are better than nimbin and Osthole single dose to the field control effect of pears cecidomyiia.After 0.5% nimbin and 0.4% Osthole single dose spray medicine the preventive effect of 10d is all lower than the preventive effect of 5d after the spray medicine, but 5 nimbins are opposite with the fructus cnidii complex insecticide, and after this explanation nimbin and fructus cnidii complex, lasting effect extends.
Above field test results shows, nimbin and fructus cnidii complex insecticide lasting period are long, and field control pears cecidomyiia is respond well, is specially adapted to nuisanceless fruit and Organic Fruit production
Table 4 nimbin and the fructus cnidii complex insecticide field control effect to the pears cecidomyiia
Claims (10)
1. the insecticide of a nimbin and fructus cnidii complex, it is characterized in that being coordinated by following raw materials according and weight portion thereof and form: 0.1～5 part of nimbin, Osthole 0.1-5 part, 5～15 parts of solvents, 5～15 parts of emulsifier, 1～6 part of dispersant, 0.5～2 part of antioxidant, 0.5～1 part of stabilizing agent, 0.5～10 part of bleeding agent, 1～10 part of antifreeze as 1～3 part of the organosilicon of defoamer, adds bamboo vinegar or pyroligneous liquor to 100 part.
2. the insecticide of nimbin as claimed in claim 1 and fructus cnidii complex is characterized in that the weight ratio of described nimbin and Osthole is (5～1): (1～2), or be 2: 1.
3. the insecticide of nimbin as claimed in claim 1 and fructus cnidii complex is characterized in that described solvent be quality is at least a in 95% ethanol, 95% acetone, 95% isopropyl alcohol than concentration.
4. the insecticide of nimbin as claimed in claim 1 and fructus cnidii complex is characterized in that described emulsifier be quality is at least a in 99% polyoxyethylene sorbitan fatty acid ester, 99% sorbitan fatty acid ester, 99% castor oil polyoxyethylene ether, 99% polyoxyethylene fatty acid ester, sodium lignin sulfonate, desugar condensation sodium lignin sulfonate than concentration.
5. the insecticide of nimbin as claimed in claim 1 and fructus cnidii complex is characterized in that described dispersant be Sodium Polyacrylate, quality is at least a in 99% propane diols polyoxyethylene poly-oxygen propylene aether, 99% block polyoxyethylene polyoxypropylene ether, glycerine polyoxyethylene polyoxypropylene blocked copolymer, alkylphenol polyoxyethylene formaldehyde condensation products sodium sulphate than concentration.
6. the insecticide of nimbin as claimed in claim 1 and fructus cnidii complex is characterized in that described antioxidant is that quality is any in 90% vitamin e, sodium sulphite or ascorbic acid than concentration.
7. the insecticide of nimbin as claimed in claim 1 and fructus cnidii complex is characterized in that described stabilizing agent is that methylcellulose, sodium carboxymethylcellulose, hydroxypropyl cellulose, xanthans, tertiary sodium phosphate, sorb sodium alkoxide, quality are at least a in 98% epoxidised soybean oil than concentration.
8. the insecticide of nimbin as claimed in claim 1 and fructus cnidii complex is characterized in that described bleeding agent be quality is at least a in 99% azone, 99% fatty alcohol-polyoxyethylene ether, 99% isomerous tridecanol polyoxyethylene ether, disecoctylmaleate sodium sulfonate than concentration.
9. the insecticide of nimbin as claimed in claim 1 and fructus cnidii complex is characterized in that described antifreezing agent be quality is 99% propane diols, 98% glycerine, 95% ethylene glycol, 98% polyethylene glycol or any in sorbierite than concentration.
10. the insecticide of nimbin as claimed in claim 1 and fructus cnidii complex, is characterized in that this method for producing insecticide comprises the steps:
(1) filtration of bamboo vinegar or pyroligneous liquor: bamboo vinegar or pyroligneous liquor are filtered after standing 5～8 months, collect as mother liquor;
(2) preparation of oil-phase solution: nimbin, Osthole and antioxidant are joined in solvent dissolve in proportion, mix by colloid mill, make oil phase;
(3) preparation of aqueous phase solution: add a small amount of step (1) gained bamboo vinegar or pyroligneous liquor stirring and dissolving in emulsifier, make water;
(4) preparation of oil water phase mixed solution: water is added oil phase, mix by colloid mill;
(5) mixing of other auxiliary agent and oil water phase mixed solution: add respectively a small amount of step (1) gained bamboo vinegar or pyroligneous liquor stirring and dissolving in other auxiliary agent, add step (4) gained mixture, be ground;
(6) making of desinsection suspension emulsion: add step (1) gained bamboo vinegar or pyroligneous liquor to 100 part in the mixed liquor that makes to step (5), make desinsection suspension emulsion of the present invention after stirring evenly.
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| CN103355322A (en) * | 2013-07-11 | 2013-10-23 | 山东省烟台市农业科学研究院 | Compound biological insecticide and application thereof |
| CN103444731A (en) * | 2013-09-15 | 2013-12-18 | 上海悦萌环保科技有限公司 | Cnidium lactone plant source pesticidal missible oil |
| CN104304285A (en) * | 2014-10-28 | 2015-01-28 | 山东中大药业有限公司 | Compound insecticidal water emulsion agent for preventing and treating contariniapyrivora |
| CN107743973A (en) * | 2017-10-17 | 2018-03-02 | 惠州市无龄康态健康科技有限公司 | A kind of composition pesticide containing Osthole |
| CN108041051A (en) * | 2017-12-18 | 2018-05-18 | 成都绿金生物科技有限责任公司 | A kind of medicine fertilizer based on nimbin and preparation method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103355322A (en) * | 2013-07-11 | 2013-10-23 | 山东省烟台市农业科学研究院 | Compound biological insecticide and application thereof |
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| CN104304285A (en) * | 2014-10-28 | 2015-01-28 | 山东中大药业有限公司 | Compound insecticidal water emulsion agent for preventing and treating contariniapyrivora |
| CN107743973A (en) * | 2017-10-17 | 2018-03-02 | 惠州市无龄康态健康科技有限公司 | A kind of composition pesticide containing Osthole |
| CN108041051A (en) * | 2017-12-18 | 2018-05-18 | 成都绿金生物科技有限责任公司 | A kind of medicine fertilizer based on nimbin and preparation method thereof |
| CN108432810A (en) * | 2018-04-11 | 2018-08-24 | 馥稷生物科技发展（上海）有限公司 | A kind of application of vegetable source pesticide composition, preparation and its prevention crop pests |
| CN109588414A (en) * | 2019-01-24 | 2019-04-09 | 中国科学院地理科学与资源研究所 | A kind of green tea tree special plant source composite pesticide and preparation method thereof |
| CN111466385A (en) * | 2020-05-13 | 2020-07-31 | 台州煜农生物科技有限公司 | Celastrus angulatus compound pesticide for preventing and controlling diseases and insect pests of orange trees and preparation method thereof |
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