CN103141488B - 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 PDF

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CN103141488B
CN103141488B CN201310032748.5A CN201310032748A CN103141488B CN 103141488 B CN103141488 B CN 103141488B CN 201310032748 A CN201310032748 A CN 201310032748A CN 103141488 B CN103141488 B CN 103141488B
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nimbin
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polyoxyethylene
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徐凯
郑伟尉
陈梅生
张岚岚
阚志强
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Zhejiang A&F University ZAFU
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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

Insecticide of nimbin and fructus cnidii complex and preparation method thereof
Technical field
The present invention relates to a kind of insecticide with plant resource nimbin and fructus cnidii complex that is mainly used in the pest such as control pears cecidomyiia 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, within 2009, Chinese pear tree harvest area is 125.8 ten thousand hm2, accounts for 72.3% of world's pears gross area; Gross annual output amount is 1438.8 ten thousand t, accounts for 65.7% of Gross World Product.Pears cecidomyiia was pear tree minor pests in the past, caused harm lighter, but in recent years all occurred seriously, to have become the primary pest of pears in the main pears of China producing region, easily caused pear tree early leaf fall and obviously affected yield and quality.At present control pears cecidomyiia is mainly to spray chemical insecticides such as killing chrysanthemum ester, Imidacloprid as main, but chemical control easily develops immunity to drugs, and cannot apply in Organic pear orchard.
Nimbin is the vegetable insecticide extracting from print chinaberry (Azadirachta indica A.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, for one of Typical Representative of botanical pesticide, to insect have food refusal, disturb lay eggs, interference insect variation, it cannot be changed in quality and reach desinsection object 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 establishing in large scale print chinaberry, and nimbin raw material can be self-supporting, cost, and what print chinaberry preparation answers 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 white, needle-shaped crystals powder, be soluble in methyl alcohol, ethanol, chloroform, acetone and ethyl acetate etc., water insoluble and benzinum.
The botanical pesticide of preparing with Osthole, set it as insecticide the various pests such as beet armyworm, tea geometrid, Colcaphellusbowringi, various aphids are all had to the effect of tagging significantly, 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 insect nervous system, cause insect muscle non-functional to shrink, finally die of exhaustion.Osthole, to people and animals and other mammalian safe, is difficult for producing anti-medicine, 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, cost reduces relatively, its preparation is extensive as biological insecticides application prospect.
Nimbin and Osthole are used for preventing and treating pears cecidomyiia and have not been reported.The present invention uses separately and composite rear Toxicity Determination and field efficiency test to pears cecidomyiia by research botanical pesticide nimbin and Osthole, evaluate 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 object.
Summary of the invention
It is a kind of for preventing and treating the nimbin of pears cecidomyiia and insecticide of fructus cnidii complex and preparation method thereof that the technical problem to be solved in the present invention is to provide.
Solve the problems of the technologies described above by the following technical programs and be achieved:
This nimbin is coordinated and is formed by following raw materials according and weight portion thereof with the insecticide of fructus cnidii complex: 0.1~5 part of nimbin, 0.1~5 part of Osthole, 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, add bamboo vinegar or pyroligneous liquor to 100 part.
Wherein:
The weight portion preferred proportion of described nimbin and Osthole is (5~1): (1~2);
Described solvent is at least one in the quality ethanol that is 95% than concentration, 95% acetone, 95% isopropyl alcohol;
Described emulsifier is at least one in the quality polyoxyethylene sorbitan fatty acid ester that is 99% than concentration, 99% sorbitan fatty acid ester, 99% castor oil polyoxyethylene ether, 99% polyoxyethylene fatty acid ester, sodium lignin sulfonate, desugar condensation sodium lignin sulfonate;
At least one in the propane diols polyoxyethylene poly-oxygen propylene aether that described dispersant is Sodium Polyacrylate, quality is 99% than concentration, 99% block polyoxyethylene polyoxypropylene ether, glycerine polyoxyethylene polyoxypropylene blocked copolymer, alkylphenol polyoxyethylene formaldehyde condensation products sodium sulphate;
Described antioxidant is any in quality be 90% than concentration vitamin e, sodium sulphite or ascorbic acid;
Described stabilizing agent is at least one in methylcellulose, sodium carboxymethylcellulose, hydroxypropyl cellulose, xanthans, tertiary sodium phosphate, sorb sodium alkoxide, the quality epoxidised soybean oil that is 98% than concentration;
Described bleeding agent is at least one in the quality azone that is 99% than concentration, 99% fatty alcohol-polyoxyethylene ether, 99% isomerous tridecanol polyoxyethylene ether, disecoctylmaleate sodium sulfonate;
Described antifreezing agent is any in the quality propane diols that is 99% than concentration, 98% glycerine, 95% ethylene glycol, 98% polyethylene glycol or sorbierite.
This nimbin comprises the steps: with the method for producing insecticide of fructus cnidii complex
(1) bamboo vinegar or pyroligneous liquor are filtered after standing 5~8 months, collect as mother liquor;
(2) in proportion nimbin, Osthole and antioxidant are joined in solvent and dissolved, mix by colloid mill, make oil phase;
(3) in emulsifier, add a small amount of step (1) gained bamboo vinegar or pyroligneous liquor stirring and dissolving, make water;
(4) water is added to oil phase, mix by colloid mill;
(5) in other auxiliary agent, add respectively a small amount of step (1) gained bamboo vinegar or pyroligneous liquor stirring and dissolving, add step (4) gained mixture, be ground;
(6) in the mixed liquor making to step (5), add step (1) gained bamboo vinegar or pyroligneous liquor to 100 part, after stirring evenly, make desinsection suspension emulsion of the present invention.
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, easily 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 pears cecidomyiia, also greatly reduced the consumption of nimbin and Osthole, thereby reduced cost accounting.Nimbin to insect have food refusal, disturb lay eggs, interference insect variation effect; Osthole is to insect take action of contace poison as main, and stomach poison function is auxiliary.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 to 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, harmless to human body and crop.
Embodiment
The present invention is below 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 enough bamboo vinegars or pyroligneous liquor are filtered and make mother liquor after standing 5~8 months, again by 0.1 part of nimbin, 0.1 part of Osthole and 0.5 part of antioxidant join in 5 parts of organic solvents and dissolve, after being mixed, colloid mill makes oil phase, in 5 parts of emulsifier, add a small amount of bamboo (wood) vinegar liquid again, after stirring evenly, make water, water and oil phase are mixed by colloid mill, again other auxiliary agent of remainder is added respectively to a small amount of bamboo vinegar or pyroligneous liquor by weight portion separately, this mixture and water oil mixture are mixed again, in colloid mill, be ground, finally remaining bamboo (wood) vinegar liquid is added entirely, make total addition of bamboo (wood) vinegar liquid reach 85.3 parts, after stirring evenly, make this desinsection suspension emulsion.
All the other embodiment 2~9, all, by the raw material of corresponding embodiment in table 1 and weight portion ratio thereof, 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
Figure GDA0000491789010000061
Figure GDA0000491789010000071
Below the Toxicity Determination relevant with the application tested 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 try worm
Pears cecidomyiia is picked up from field, and 2 in the same size, healthy instar larvaes of laboratory picking are done examination worm.
1.1.2 reagent agent
25% nimbin, Yunnan Nan Bao plant Co., Ltd; 20% Osthole, Xi'an Tian Ben biotechnology Co., Ltd.Reagent agent nimbin (A) and Osthole (B) are with acetone solution and be diluted to 1000mg/L mother liquor.Between nimbin and Osthole respectively (A: B) 5: 1 in mass ratio, 3: 1,2: 1,1: 1,1: 2,1: 3, within 1: 5, compound proportion was diluted to 5 concentration gradient liquids.
1.2 assay method
Press the method that NY/T1154.7-2006 recommends, with micro syringe drop for reagent liquid in 2 instar larvae chest backboards, every processing repeats for 4 times, 30 of every repetitions contrast inspection record death condition after 4d by acetone treatment.It is synergistic effect that co-toxicity coefficient (CTC value) is greater than at 120 o'clock, and 80≤CTC≤120 are summation action, and being less than at 80 o'clock is antagonism.
1.3 toxicity test results
Adopt drop method to nimbin and Osthole different proportion the virulence after composite measure.Result shows, nimbin and Osthole optimum ratio are 5: 1,3: 1,1: 1,1: 2, and their co-toxicity coefficient is all greater than 120, shows notable synergistic effect, and wherein best proportioning is 2: 1, and co-toxicity coefficient is 233.46 (tables 2).
Table 2 nimbin and fructus cnidii complex toxicity test
Figure GDA0000491789010000081
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 in the ethanol of solvent and acetone and dissolve, mix by colloid mill, make oil phase; Colloid mill does not do specific (special) requirements, can reach the uniform effect of mixed house.
(3) in the polyoxyethylene sorbitan fatty acid ester as emulsifier, castor oil polyoxyethylene ether, add appropriate step (1) gained bamboo (wood) vinegar liquid stirring and dissolving, make water.
(4) water is added to oil phase, mix by colloid mill.
(5) in other auxiliary agent, add respectively appropriate step (1) gained bamboo (wood) vinegar liquid stirring and dissolving, then add step (4) gained mixture, be ground;
(6) in the mixed liquor making to step (5), add step (1) gained bamboo (wood) vinegar liquid to full dose, stir evenly and obtain 3% nimbin Osthole suspension emulsion.
The raw material type of five examples of table 3 and weight portion proportioning value thereof
Figure GDA0000491789010000091
Figure GDA0000491789010000101
Example two, three, four, five, all, by raw material and weight portion ratio thereof separately in table 3, makes with the preparation method identical with example one.
3, field efficacy evaluation test
Field efficacy evaluation test is carried out in Cui Guan theatre, Yuhang District, Zhejiang Province.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 15,45,90mg/L drug concentration sprays; With 0.5% nimbin emulsion (Yunnan bright Neem industry exploitation limited company produces) and 0.4% Osthole EC (Wuhan City, Hubei Province Tian Hui 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 contrast medicament, and establish clear water contrast (CK).
Randomised block design, 3 strain pear trees are processed in every community, and every processing repeats 3 times.Spraying time is the larva harm initial stage on April 19th, 2012.Before spray medicine every tree press East, West, South, North, in 1 of 5 prosperous extending shoot of the random listing mark in orientation, investigate 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 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-spray medicine of 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 (Osthole ratio is the highest), and this may be main with Osthole action of contace poison; After spray medicine, 5d preventive effect is 69.33%~91.16%, is up to example three compounded pesticides (nimbin and Osthole ratio are 2: 1); After spray medicine, 10d preventive effect is 78.41%~94.16%, and the highest is still example three compounded pesticides.Anti-all preventive effects higher than 0.5% nimbin and 0.4% Osthole of putting of 10d after 5 nimbins and fructus cnidii complex insecticide spray medicine, 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 spray medicine, but 5 nimbins are contrary with 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 and produces.
Table 4 nimbin and the field control effect of fructus cnidii complex insecticide to pears cecidomyiia
Figure GDA0000491789010000121

Claims (2)

1. the insecticide of a nimbin and fructus cnidii complex, it is characterized in that coordinating and forming by following raw materials according and weight portion thereof: 0.1~5 part of nimbin, 0.1~5 part of Osthole, 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;
Wherein:
Described nimbin and the weight ratio of Osthole are (5~1): (1~2);
Described solvent is at least one in the quality ethanol that is 95% than concentration, 95% acetone, 95% isopropyl alcohol;
Described emulsifier is at least one in the quality polyoxyethylene sorbitan fatty acid ester that is 99% than concentration, 99% sorbitan fatty acid ester, 99% castor oil polyoxyethylene ether, 99% polyoxyethylene fatty acid ester, sodium lignin sulfonate, desugar condensation sodium lignin sulfonate;
At least one in the propane diols polyoxyethylene poly-oxygen propylene aether that described dispersant is Sodium Polyacrylate, quality is 99% than concentration, block polyoxyethylene-polyethenoxy ether of 99%, glycerine polyoxyethylene polyoxypropylene blocked copolymer, alkylphenol polyoxyethylene formaldehyde condensation products sodium sulphate;
Described antioxidant is any in quality be 90% than concentration vitamin e, sodium sulphite or ascorbic acid;
Described stabilizing agent is at least one in methylcellulose, sodium carboxymethylcellulose, hydroxypropyl cellulose, xanthans, tertiary sodium phosphate, sorb sodium alkoxide, the quality epoxidised soybean oil that is 98% than concentration;
Described bleeding agent is at least one in the quality azone that is 99% than concentration, 99% fatty alcohol-polyoxyethylene ether, 99% isomerous tridecanol polyoxyethylene ether, disecoctylmaleate sodium sulfonate;
Described antifreezing agent is any in the quality propane diols that is 99% than concentration, 98% glycerine, 95% ethylene glycol, 98% polyethylene glycol or sorbierite.
2. the insecticide preparation method of a nimbin as claimed in claim 1 and fructus cnidii complex is characterized in that comprising 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: in proportion nimbin, Osthole and antioxidant are joined in solvent and dissolved, 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 to 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 making to step (5), make desinsection suspension emulsion of the present invention after stirring evenly.
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