CN106342905B - A kind of agricultural insecticidal composite containing Herba speranskiae tuberculatae extract - Google Patents
A kind of agricultural insecticidal composite containing Herba speranskiae tuberculatae extract Download PDFInfo
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
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- A01N43/36—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom five-membered rings
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/72—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms
- A01N43/88—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms six-membered rings with three ring hetero atoms
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
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Abstract
The invention discloses one kind to contain Herba speranskiae tuberculatae extract agricultural insecticidal composite, including the first active constituent and the second active constituent, the weight ratio of first active constituent and the second active constituent is 15:1~1:5, first active constituent is Herba speranskiae tuberculatae extract, and the second active constituent is one of Tolfenpyrad, emamectin benzoate, imidacloprid, capillary, spiral shell worm ethyl ester, buprofezin pesticide.Agricultural insecticidal composite of the invention can be configured to agriculturally to allow using suspending agent, aqueous emulsion and microemulsion, to brassicaceous vegetable diamondback moth, cabbage caterpillar, apple scale insect, apple aphid, Cucumber blight has preferable preventive effect.Present invention efficiently solves the undesirable problems of Herba speranskiae tuberculatae extract insecticide preventive effect, reduce Tolfenpyrad, emamectin benzoate, imidacloprid, capillary, spiral shell worm ethyl ester, the dosage of buprofezin pesticide, alleviate the pressure to environment, the two compounding has significant synergies and good to crop safety.
Description
Technical field
The invention belongs to technical field of compounded pesticide, are related to a kind of agricultural insecticidal composite, and in particular to one kind is containing saturating
The agricultural insecticidal composite of bone grass extract.The present invention gives the preparation formulation of the Pesticidal combination and agriculturally
Using.
Background technique
With people's environmental protection, the enhancing of social sustainable development consciousness, the side effect of pesticide is minimized, exploitation biology
Reasonable pesticide has become global common recognition.Botanical pesticide has low toxicity, low-residual, substantially harmless to non-target organism, right
The advantages that environmental nonpollution, development and appliable plant source pesticide have been increasingly becoming a kind of trend.And as the public eats green
Product, the demand of pollution-free food are increasing, and market is also growing day by day to the demand of botanical pesticide.Develop plant source agriculture
Medicine becomes the inexorable trend of society and scientific development.
Lopseed (Phryma leptostachya L.) is Phrymaceae lopseed category herbaceos perennial, also known as old
Woman's needlework, malicious fly grass, american lopseed herb or root, a horse light etc..Lopseed is general to be distributed in the Himalaya, North America and east Asia,
It has been used as traditional pesticide plant in East Asia.It is each that lopseed in China is mainly distributed on northeast, North China and the Yangtze river basin
Ground.According to records, lopseed herb and root are toxic, hyoscine, and nature and flavor are puckery;Energy heat-clearing, controls impetigo, scabies and worm sore;Root can
Fly maggot is killed, herb can kill vegetables cabbage caterpillar.In recent years, Inst. of Pesticides, Xibei Univ. of Agricultural &. Forestry Science &. Technolo is to lopseed
System research, has developed lopseed microemulsion formulation, has good preventive effect to cabbage caterpillar, oriental armyworm, diamondback moth etc..
Tolfenpyrad, emamectin benzoate, imidacloprid, capillary, spiral shell worm ethyl ester, Buprofezin are to develop in recent years
Some efficient pesticides, the mechanism of action is more unique, has the function of efficient, wide spectrum to crop various pests, and be poison
Lower, the environmentally safe insecticide variety of property, becomes presently preferred insecticide.
The physicochemical properties of above-mentioned several pesticides, insecticidal mechanism is briefly described below and in application agriculturally.
Tolfenpyrad, other titles: it is bright to catch worm, English common name: Tolfenpyrad, chemical name: N- [4- (4- methyl
Phenoxy group) benzyl] the chloro- 5- pyrazolecarboxamide of -1- methyl -3- ethyl -4-.Tolfenpyrad is the exploitation of Mitsubishi chemical company
Novel pyrazole heterocyclic Insecticidal and acaricidal agent, the mechanism of action are that the electronics in the metabolic system for hinder mitochondria conveys system multiple
Fit I prevents insect from providing and storing energy so that electronics reception and registration be made to be hindered, and referred to as Mitochondrial electron is conveyed multiple
Fit Inhibitors.Insecticidal spectrum is wide, has action of contace poison.There is special efficacy to lepidoptera pest diamondback moth, Thysanoptera thrips.The medicine
There is preferable quick-acting, the lasting period was longer, up to 10 days or so.It is widely used in the crops such as prevention and treatment vegetables, fruit tree, flowers, tealeaves
On pest,
Emamectin benzoate also known as emaricin (because of spit of fland of going out), English common name: Emamectin.Methylamino Avermectin
Element is efficient insecticide, the acaricide of the novel semi-artificial synthesis of one kind synthesized from fermented product AVERMECTIN B1.Methylamino AVM hereinafter
The Action mechanism of rhzomorph is to hinder nerve conduction, leads to insect paralysis, is unable to normal activity and lethal dies.Insect is acted on
Mode is mainly stomach poison function, and contact efficacy is slow, needs 3~4d or so that can just make insect death, is mainly used for preventing and treating cross
Flower section vegetables diamondback moth, cabbage caterpillar, the pests such as beet armyworm and oriental tobacco budworm.
Imidacloprid, English common name: Imidacloprid, chemical name: 1- (6- chloropyridine -3- pyridylmethyl)-N-
Nitroimidazoline -2- base amine.Imidacloprid is nitro-methylene-type systemic insecticide, is the effect of nicotinic acetylcholine receptor
Body, interference pest movements nervous system make its chemical signal transmit failure, have tag, stomach toxicity and the multiple drug effect of interior suction.Imidacloprid
With wide spectrum, efficiently, low toxicity, low-residual, pests are not easy to produce resistance, the features such as to people, animal, plant and natural enemies security, mainly
For preventing and treating sucking pest, such as aphid, leafhopper, thrips, trialeurodes vaporariorum and colorado potato bug and frit fly.
Capillary also known as chlorfenapyr, English common name: Chlorfenapyr, chemical name: bromo- 2- (4- chlorphenyl) -1-
Ethoxyl methyl -5- trifluoromethyl pyrpole -3- nitrile;The bromo- 2- of 4- (4- chlorphenyl) -1- ethoxyl methyl -5- trifluoromethyl pyrpole -
3- nitrile.Capillary is new pyrrole class compound, is acted on the mitochondria of insect bodies inner cell, and the intracorporal more function of insect are passed through
Energy oxidizing ferment works, and mainly inhibits the conversion of adenosine diphosphate (ADP) (ADP) to atriphos (ATP).Capillary has stomach toxicity
And action of contace poison.On blade face, permeability is strong, has certain systemic action, and with insecticidal spectrum is wide, preventive effect is high, holding effect is long, safety
The characteristics of.Capillary is mainly used for preventing and treating brassicaceous vegetable diamondback moth, cabbage caterpillar, the pests such as beet armyworm.
Spiral shell worm ethyl ester, English common name: SpirotetraMat, chemical name: cis- -3- (2,5- 3,5-dimethylphenyl) -8-
Methoxyl group -2- oxo -1- azaspiro [4.5] decyl- 3- alkene -4- base ethyl carbonate, cis- -4- (ethyl oxy carbonyl) -8- methoxyl group -
3- (2,5- xylyl) -1- azaspiro [4.5] decyl- 3- alkene -2- ketone.Spiral shell worm ethyl ester is the season of Bayer Cropscience Co., Ltd's exploitation
The two-way uptake and translocation insecticide of Mek-Tol Unit, can effectively prevent various suckings pest, such as aphid, thrips, wood louse, aleyrodid
With scale insect etc..Lasting period is up to 8 weeks, and applicable chief crop includes cotton, soybean, citrus, tropical fruit tree, nut, Portugal
Grape, hops, potato and vegetables etc., and important beneficial insect such as ladybug, wasp fly and parasitic wasp are had good selectivity.
Buprofezin also known as Buprofezin, buprofezin.English common name: Buprofezin, chemical name: 2- tertiary butyl imido
Base -3- isopropyl -5- phenyl -3,4,5,6- tetrahydro -2H-1,3,5- thiadiazine -4- ketone.Buprofezin is opened by Japanese pesticide company
The diazthines insect growth regulator, IGR of hair.By inhibiting chitin synthesis and interference metabolism, prevent pest from normally sloughing off
Skin and abnormal and gradually dead.Active feature high, selectivity is good, the residual period is long.There is special efficacy to plant hopper, leafhopper, aleyrodid,
Also there is preferable control efficiency to some scale insects such as arrowhead scales, long white a red-spotted lizards.
The new type disinsections such as Tolfenpyrad, emamectin benzoate, imidacloprid, capillary, spiral shell worm ethyl ester, Buprofezin in recent years
Quickly, market sales volume increases the development speed of agent year by year.Since its preventive effect is preferable, peasant is largely used for multiple times, and leads to many evils
Worm gradually generates resistance to it, and dosage is caused to continue to increase, and persticide residue increases, and also produces to non-target organism and environment
Adverse effect is given birth to.
Summary of the invention
The technical problem to be solved in the present invention: as the Herba speranskiae tuberculatae extract of botanical pesticide, have to certain crop pests
There is certain cytotoxicity.But since active component content of the Herba speranskiae tuberculatae extract to crop pest is lower, quick-acting is poor, right
The effect of controlling of crop pest is generally not so good as chemical pesticide.Above-mentioned chemical pesticide Tolfenpyrad, emamectin benzoate, imidacloprid,
Capillary, spiral shell worm ethyl ester, Buprofezin have the relatively new mechanism of action and excellent control efficiency, but various agricultural pest is right
Plurality of kind produces drug resistance.Chemical pesticide dosage is reduced by rational mixture, to crops No-harmful apple orchard
It is of great significance;The application for also having expanded botanical pesticide simultaneously, explores botanical pesticide-chemical pesticide and is used in combination
New model.
Solve the scheme of technical problem: bright people is by long-term a large amount of test discovery, by Herba speranskiae tuberculatae extract and effect machine
Manage different novel pesticide Tolfenpyrads, emamectin benzoate, imidacloprid, capillary, spiral shell worm ethyl ester, one in Buprofezin
Kind is used in combination, and is had significant synergies, can be significantly improved and prevent cabbage caterpillar, diamondback moth, scale insect, aphid, aleyrodid
Effect is controlled, dosage is reduced, expands prevention spectrum, control cost is reduced, can solve resistance problem, prolong the service life, is improved
Safety to crop.
The present invention using Herba speranskiae tuberculatae extract as the first active constituent, chemical pesticide Tolfenpyrad, emamectin benzoate,
One of imidacloprid, capillary, spiral shell worm ethyl ester, Buprofezin are used as the second active constituent, the first active constituent and the second activity
Ingredient binary built forms the agricultural insecticidal composite with compound synergic.
Specifically, the technical scheme is that a kind of agricultural insecticidal composite containing Herba speranskiae tuberculatae extract, packet
Include the first active constituent Herba speranskiae tuberculatae extract and the second active constituent Tolfenpyrad, emamectin benzoate, imidacloprid, worm
The mass ratio of one of mite nitrile, spiral shell worm ethyl ester, Buprofezin, the first active constituent and the second active constituent is 15:1~1:5.
Herba speranskiae tuberculatae extract of the present invention can be prepared by following methods:
With the smashed lopseed of organic solvent soaking at room temperature, ultrasonic extraction, filtering is sloughed after organic solvent up to deep
Careless extract.
Preferably, organic solvent here, for example methanol, ethyl alcohol, acetone, ethyl acetate, methylene chloride, chlorine can be used
Imitative or its mixed solvent.For using mixed solvent to extract the situation of lopseed, as the component and each component of mixed solvent
Between ratio, the present invention do not limit particularly.
Further preferred preparation method as Herba speranskiae tuberculatae extract of the present invention:
After dry lopseed crushes, for 24 hours with methanol soaking at room temperature;It uses ultrasonic extraction 3 times again, each ultrasonic extraction
30min, filtering;It repeats to extract 3 times, Herba speranskiae tuberculatae extract is concentrated under reduced pressure to obtain in merging filtrate.
Agricultural insecticidal composite of the present invention containing Herba speranskiae tuberculatae extract, the dosage forms of pesticidal preparations be suspending agent,
Aqueous emulsion or microemulsion.
The present invention also further provides the agricultural insecticidal composite containing Herba speranskiae tuberculatae extract in prevention and treatment crops worm
Purposes in evil.
This agricultural insecticidal composite can be used for preventing and treating a variety of insect pests of multiple kinds of crops, for example, brassicaceous vegetable is small
Diamond-back moth, cabbage caterpillar, apple scale insect, apple aphid, Cucumber blight.
Compared with prior art, what the present invention generated has the beneficial effect that following aspect:
(1) Herba speranskiae tuberculatae extract is as a kind of new plant insecticide, to the prevention and treatment of crop pest with stomach function regulating of tagging
Based on toxic action, but due in extract active component content it is lower, cause its to prevention and treatment target preventive effect it is poor.Azoles worm acyl
Amine, emamectin benzoate, imidacloprid, capillary, spiral shell worm ethyl ester, Buprofezin these types insecticide action are more special,
To prevention and treatment target significant effect, but chronic administration is easy to generate resistance.
The present invention is by the different Herba speranskiae tuberculatae extract of the mechanism of action and Tolfenpyrad, emamectin benzoate, imidacloprid, worm
One of mite nitrile, spiral shell worm ethyl ester, Buprofezin carry out binary built, form novel botanical pesticide-chemical pesticide composite class
The agricultural insecticidal composite of type.The activity and insecticidal effect of the Pesticidal combination are not the active simple superposition of each component, and
It is to have significant synergistic effect, has not only overcome the poor disadvantage of botanical pesticide preventive effect, but also reduces the use agent of chemical pesticide
Amount.In addition, the advantages of agricultural insecticidal composite is also manifested by, component is reasonable, and good disinsection effect improves crop safety,
The generation of delaying drug resistance, and the requirement of current pesticide reduction synergy has been adapted to, improve the quality of agricultural product.
(2) present invention expands prevention spectrum, to primary pest such as the brassicaceous vegetable diamondback moth, dark greyish green of multiple kinds of crops
Worm, apple yellow aphid, Cucumber blight, apple scale insect have good control efficiency.
(3) present invention is prepared for the preparation of different dosage forms, learns through safety evaluatio, and each preparation is good to crop safety,
Meet the security requirement of pesticidal preparations.
Specific embodiment
In order to which the purpose of the present invention, technical solution and beneficial effect is more clearly understood, with reference to embodiments, to this
Invention is further elaborated.
(1) preparation of Herba speranskiae tuberculatae extract
Herba speranskiae tuberculatae extract described in the present embodiment can be prepared conventionally, such as Soakage extraction method, ultrasonic vibration
Extraction method etc..In order to sufficiently prepare the Herba speranskiae tuberculatae extract, the yield of Herba speranskiae tuberculatae extract is improved, while shortening described in preparation
The time of Herba speranskiae tuberculatae extract.The present embodiment preferably uses Soakage extraction to extract the method combined with ultrasonic vibration, and preparation is saturating
Bone grass extract.
Lopseed preferably selects the lopseed after drying, and organic solvent Soakage extraction is used after crushing.The present embodiment is for choosing
There are many organic solvents, such as methanol, ethyl alcohol, acetone, ethyl acetate, methylene chloride, chloroform or its mixed solvent.
As Herba speranskiae tuberculatae extract preparation preferred method, specifically: weigh lopseed crush after, methanol soaking at room temperature
After for 24 hours, three times (30min/ times) using ultrasonic extraction, repeat to extract three times.Lopseed is concentrated under reduced pressure to obtain in filtering, merging filtrate
Extract, yield 4.2-5.6%.
(2) preparation prepares part
Agricultural insecticidal composite of the present invention, first group is divided into the Herba speranskiae tuberculatae extract that can be prepared by the above method,
Second component selects one of Tolfenpyrad, emamectin benzoate, imidacloprid, capillary, spiral shell worm ethyl ester, Buprofezin.
The agricultural insecticidal composite can be configured to a variety of dosage forms such as suspending agent, aqueous emulsion or microemulsion.To this field
For those of ordinary skill, when preparing dosage form, in addition to containing active insecticidal components for the election, it is also necessary to creatively select a variety of
Auxiliary agent.When preparing above-mentioned dosage form, it can according to need selection and use different auxiliary ingredients for pesticide preparations (auxiliary agent).It is described auxiliary
Co-ingredients can be one of decentralized medium, dispersing agent, emulsifier, wetting agent, thickener, defoaming agent, antifreezing agent, filler etc.
Or it is several.
The preparation method of the corresponding preparations of the agricultural insecticidal composite containing Herba speranskiae tuberculatae extract is illustrated first.
When preparing corresponding suspending agent, workable auxiliary agent has: dispersing agent selects polycarboxylic acid salt (TERSPERSE
2700, T36 etc.), lignin sulfonate (Ufoxane 3A, Borresperse NA, Borresperse CA-SA etc.), naphthalene
With alkyl naphthalene formaldehyde condensate sulfonate class (NNO, MF, Morwet D-425, Tamol NN, TERSPERSE2020 etc.), pull open
Powder BX (nekal), EO-PO block polyether class (polyoxyethylene polyoxypropylene block copolymer), alkyl phenol polyoxy second
It is one or more in alkenyl ether phosphate, alkylphenol polyoxyethylene ether formaldehyde condensate sulfate (SOPA);Wetting agent is selected
It is Sulfates (K-12), Sulfonates (ABS-Na, BX, Terwet 1004 etc.), a kind of in compound wetting agent (Morwet EFW)
Or it is a variety of;Thickener select starch, polyvinyl alcohol, sodium carboxymethylcellulose, one of or it is a variety of;Filler selection diatomite,
One of kaolin, white carbon black, attapulgite, clay, urea, cornstarch, sodium sulphate are a variety of.
When preparing corresponding aqueous emulsion, workable auxiliary agent has: emulsifier selects BY (castor oil polyoxyethylene ether) system
Column emulsifier (BY-110, BY-125, BY-140), agriculture breast 400, peaceful cream 33,32,4203,4103, calcium dodecyl benzene sulfonate,
Fatty alcohol polyoxyethylene ether, Nongru-700 # (common name: alkyl phenol formaldehyde resin polyoxyethylene ether), agriculture breast 2201, this disk -60#
(common name: sorbitan monostearate), Tween-60 # (common name: sorbitan monostearate polyoxyethylene ether),
One of agriculture breast 1601# (common name: phenethyl phenol polyoxyethylene poly-oxygen propylene aether) or a variety of;Assistant for emulsifying agent such as methanol,
One of isopropanol, n-butanol, ethyl alcohol are a variety of;Solvent selects cyclohexanone, N-Methyl pyrrolidone, dimethylbenzene, toluene, molten
It is one or more in agent oil.It is one or more in stabilizer selection triphenyl phosphite, epoxychloropropane;Water is deionized water.
When preparing corresponding microemulsion, workable auxiliary agent has: emulsifier selects calcium dodecyl benzene sulfonate (agriculture breast
500#), Nongru-700 # (common name: alkyl phenol formaldehyde resin polyoxyethylene ether), agriculture breast 2201#, this disk -60# (common name: lose
Water sorbitan stearate), Tween-60 # (common name: polyoxyethylene sorbitan stearate), TX-10 (common name: pungent
Base phenol polyethenoxy (10) ether), agriculture breast 1601 (common name: triphenoethyl benzene phenol polyoxyethylene polyoxypropylene block polymer),
It is one or more in agriculture breast 600#, agriculture breast 400#;One of assistant for emulsifying agent such as methanol, isopropanol, n-butanol, ethyl alcohol is more
Kind;Solvent select cyclohexanone, N-Methyl pyrrolidone, dimethylbenzene, toluene, in solvent naphtha (trade mark: S-150, S-180, S-200)
It is one or more;It is one or more in stabilizer selection triphenyl phosphite, epoxychloropropane;Water is deionized water.
Pesticidal combination of the invention includes the first active constituent and the second active constituent, and the first active constituent is lopseed
Extract, the second active constituent be Tolfenpyrad, emamectin benzoate, imidacloprid, capillary, spiral shell worm ethyl ester, in Buprofezin
One kind.It should be noted that the effective component (or active constituent) in each example of formulations of subordinate is weight after folding hundred.Mirror
In length, the present invention has chosen Tolfenpyrad, emamectin benzoate, imidacloprid, capillary, spiral shell worm ethyl ester, Buprofezin activity
Ingredient is illustrated.
Example of formulations 1
Weigh 250 grams of Herba speranskiae tuberculatae extracts, 50 grams of Tolfenpyrads, 50 grams of sodium lignin sulfonates, 20 grams of Nekal BX (two fourths
Base sodium naphthalene sulfonate), 30 grams of K-12 (lauryl sodium sulfate), 20 grams of PVA (polyvinyl alcohol, molecular weight 2000), 20 grams of polyethylene
100 grams of pyrrolidones, kaolin, water supplies 1000 grams.The method that the frequent regulation of above-mentioned raw materials takes suspending agent mixes, sand mill
Be sanded to partial size less than 5 μm, produce active constituent content be 30% Herba speranskiae tuberculatae extract Tolfenpyrad suspending agent.
Example of formulations 2
Weigh 150 grams of Herba speranskiae tuberculatae extracts, 10 grams of emamectin benzoates, 25 grams of T36 (polycarboxylate), 30 grams of pull open powders
BX (nekal), 20 grams of K-12 (lauryl sodium sulfate), 100 grams of soil of roc profit, water supplies 1000 grams.Above-mentioned raw materials
The method that frequent regulation takes suspending agent mix, sand mill be sanded to partial size less than 5 μm, to produce active constituent content saturating for 16%
Bone grass extract emamectin benzoate suspending agent.
Example of formulations 3
Weigh 200 grams of Herba speranskiae tuberculatae extracts, 40 grams of imidacloprids, 30 grams of alkyl phenol polyoxyethylene ether phosphates, 50 grams of polyoxies
Ethylene polyoxypropylene block copolymers, 40 grams of calcium dodecyl benzene sulfonates, 30 grams of Nongru-700 #, 20 grams of castor oil polyoxyethylenes
Ether, 1 gram of polyvinyl alcohol, 100 grams of bentonites, 20 grams of BHT, water supply 1000 grams.Above-mentioned raw materials through mixing, with sand mill be sanded to
For partial size less than 5 μm, obtaining active constituent content is 24% Herba speranskiae tuberculatae extract imidacloprid suspending agent.
Example of formulations 4
Weigh 250 grams of Herba speranskiae tuberculatae extracts, 50 grams of capillaries, 30 grams of alkyl phenol polyoxyethylene ether phosphates, 50 grams of polyoxies
Ethylene polyoxypropylene block copolymers, 40 grams of calcium dodecyl benzene sulfonates, 30 grams of Nongru-700 #, 20 grams of castor oil polyoxyethylenes
Ether, 1 gram of polyvinyl alcohol, 100 grams of bentonites, 20 grams of BHT, water supply 1000 grams.Above-mentioned raw materials through mixing, with sand mill be sanded to
For partial size less than 5 μm, obtaining active constituent content is 30% Herba speranskiae tuberculatae extract capillary suspending agent.
Example of formulations 5
Weigh 300 grams of Herba speranskiae tuberculatae extracts, 50 grams of spiral shell worm ethyl esters, 30 grams of fatty alcohol polyoxyethylene ether, 30 grams of diffusants
NNO, 60 grams of agriculture breast 500#, 30 grams of agriculture breast 2201#, 30 grams of polyvinyl alcohol, 100 grams of bentonites, 10 grams of sanloses,
Water supplies 1000 grams.Above-mentioned raw materials are sanded to partial size with sand mill less than 5 μm, obtaining active constituent content is through mixing
35% Herba speranskiae tuberculatae extract spiral shell worm ethyl ester suspending agent.
Example of formulations 6
Weigh 100 grams of Herba speranskiae tuberculatae extracts, 100 grams of Buprofezins, 40 grams of TX-10,50 grams of Nongru-700 #, 30 grams of agriculture breasts
500#, 40 grams of agriculture breast 1601#, 150 grams of cyclohexanone, 50 grams of N-Methyl pyrrolidones, 50 grams of n-butanols are dissolved completely and are mixed
Uniformly, deionized water adds to 1000 grams, and it is 20% Herba speranskiae tuberculatae extract Buprofezin micro emulsion that active constituent content is made after stirring
Agent.
Example of formulations 7
Weigh 100 grams of Herba speranskiae tuberculatae extracts, 50 grams of Buprofezins, 40 grams of Nongru-700 #, 30 grams of agriculture breast 500#, 60 grams of agriculture breasts
600#, 100 grams of cyclohexanones, 50 grams of isopropanols, 10 grams of epoxychloropropane are dissolved completely and are uniformly mixed, and deionized water adds to
1000 grams, it is 15% Herba speranskiae tuberculatae extract thiazine ketone aqueous emulsion that active constituent content is made after stirring.
(3) Biometric portion
1, indoor virulence experimental section
Indoor toxicity test embodiment 1: wild cabbage plutella xylostella indoor toxicity test
In order to prevent and treat the diamondback moth on the brassicaceous vegetable vegetables in agricultural production, inventor with Herba speranskiae tuberculatae extract with
Tolfenpyrad, emamectin benzoate, capillary have carried out the synergy research of mutual compounding.Method particularly includes:
Subjects are diamondback moth, Plutella xylostella.Raw medicine is configured to the test medicine needed, test
Method is with reference to " People's Republic of China's farm-chemical indoor determination test rule of agricultural industry criteria NY/T1154.6-2006 is killed
The 6th part of worm agent: biocidal activity tests dip method ", " People's Republic of China's agricultural industry criteria NY/T1154.7-2006
The 7th part of farm-chemical indoor determination test rule insecticide: mixed synergy measurement ".
5 various concentration gradients are arranged in single dose and each Mixed Pharmacy first, and (death rate is pressed in the range of 5%~90%
Geometric progression setting).With the pure water added with a small amount of surfactant (Tween 80), it is almost the same, healthy to choose Individual Size
Diamondback moth, it is spare.By equipped with diamondback moth leaching worm cage leaching it is into the liquid gently shake, sucked through taking-up in 5 seconds with blotting paper
The medical fluid of adhesive surface and surrounding, 4 repetitions of every processing, every repetition 10, and set the corresponding organic solvent processing without medicament
As control.48h checks test worm death condition after processing, records total borer population and dead borer population.Dead judgment criteria are as follows: with small writing brush
It flips the completely motionless person of polypide and is denoted as dead worm.
Then thermostatic chamber is moved to, is cultivated under conditions of 20 DEG C~24 DEG C of temperature, the work of investigation in 48 hours borer population, meter after processing
Calculate Revision insect recluced rate.
Calculation method:
Revision insect recluced rate=(living after insect population number-processing before handling to go out to count)/insect population number × 100 before handling
Control efficiency (%)=[(processing Revision insect recluced rate-control Revision insect recluced rate)/(100- compares Revision insect recluced rate)]
×100
By the linear regression analysis between the probit value of preventive effect and the logarithm of series of concentrations, the LC of each medicament is found out50
Value calculates the co-toxicity coefficient (CTC) of mixture with Sun Yunpei's Method, evaluates reagent agent to the activity of germ with this.
The co-toxicity coefficient (CTC) >=120 of compound preparation shows as synergistic effect;CTC≤80 show as antagonism;80 <
CTC < 120 shows as summation action.
The experimental result of the present embodiment is shown in Table 1-1 to table 1-3.
Table 1-1 Herba speranskiae tuberculatae extract compounds the indoor toxicity test to wild cabbage plutella xylostella with Tolfenpyrad
Chemicals treatment | Virulence regression equation | Related coefficient (r) | LC50(mg/L) | Co-toxicity coefficient (CTC) |
Herba speranskiae tuberculatae extract (A) | Y=0.7019+1.7291X | 0.9764 | 305.93 | - |
Tolfenpyrad (B) | Y=2.8994+1.8122X | 0.9884 | 14.43 | - |
A:B=1:5 | Y=2.5372+2.3425X | 0.9904 | 11.26 | 152.35 |
A:B=1:2.5 | Y=2.9400+1.7778X | 0.9944 | 14.41 | 137.60 |
A:B=1:1 | Y=3.1320+1.4657X | 0.9881 | 18.82 | 146.44 |
A:B=2.5:1 | Y=1.8666+2.0285X | 0.9668 | 35.05 | 128.89 |
A:B=5:1 | Y=1.0211+2.2927X | 0.9894 | 54.39 | 128.81 |
A:B=10:1 | Y=1.4754+1.8513X | 0.9886 | 80.15 | 134.57 |
A:B=15:1 | Y=1.2909+1.8513X | 0.9896 | 100.82 | 134.11 |
Table 1-2 Herba speranskiae tuberculatae extract compounds the indoor toxicity test to wild cabbage plutella xylostella with emamectin benzoate
Table 1-3 Herba speranskiae tuberculatae extract compounds the indoor toxicity test to wild cabbage plutella xylostella with capillary
Chemicals treatment | Virulence regression equation | Related coefficient (r) | LC50(mg/L) | Co-toxicity coefficient (CTC) |
Herba speranskiae tuberculatae extract (A) | Y=0.7019+1.7291X | 0.9764 | 305.93 | - |
Capillary (B) | Y=4.650+1.7991X | 0.9850 | 1.55 | - |
A:B=1:5 | Y=4.6362+2.0231X | 0.9978 | 1.51 | 123.05 |
A:B=1:2.5 | Y=4.4644+2.2963X | 0.9930 | 1.71 | 126.64 |
A:B=1:1 | Y=4.2321+2.0995X | 0.9916 | 2.32 | 132.95 |
A:B=2.5:1 | Y=4.0419+1.5893X | 0.9814 | 4.01 | 133.59 |
A:B=5:1 | Y=3.4834+1.915X | 0.9753 | 6.19 | 146.53 |
A:B=10:1 | Y=3.0227+2.0051X | 0.9917 | 9.69 | 167.47 |
A:B=15:1 | Y=2.1778+2.2465X | 0.9842 | 18.04 | 127.76 |
The The Toxicity Determination result of table 1-1 to table 1-3 show: Herba speranskiae tuberculatae extract and Tolfenpyrad, methylamino AVM hereinafter
One of rhzomorph, capillary have higher poison to brassicaceous vegetable wild cabbage plutella xylostella for 15:1~1:5 is mixed with weight ratio
Power has significant synergistic effect.
Indoor toxicity test embodiment 2: cabbage pieris indoor toxicity test
In order to prevent and treat the cabbage caterpillar on the brassicaceous vegetable vegetables in agricultural production, inventor with Herba speranskiae tuberculatae extract with
Tolfenpyrad, emamectin benzoate, capillary have carried out the synergy research of mutual compounding.Method particularly includes:
Subjects are cabbage caterpillar.Raw medicine is configured to the test medicine needed, test method refers to " Chinese people's republicanism
The 6th part of the state's farm-chemical indoor determination test rule of agricultural industry criteria NY/T1154.6-2006 insecticide: insecticide is living
Property test dip method ", " People's Republic of China's farm-chemical indoor determination of agricultural industry criteria NY/T1154.7-2006 test
The 7th part of criterion insecticide: mixed synergy measurement ".
5 various concentration gradients are arranged in single dose and each Mixed Pharmacy first, and (death rate is pressed in the range of 5%~90%
Geometric progression setting).With the pure water added with a small amount of surfactant (Tween 80), it is almost the same, healthy to choose Individual Size
Cabbage caterpillar, it is spare.By equipped with cabbage caterpillar leaching worm cage leaching it is into the liquid gently shake, sucked through taking-up in 5 seconds with blotting paper
The medical fluid of adhesive surface and surrounding, 4 repetitions of every processing, every repetition 10, and set the corresponding organic solvent processing without medicament
As control.48h checks test worm death condition after processing, records total borer population and dead borer population.Dead judgment criteria are as follows: with small writing brush
It flips the completely motionless person of polypide and is denoted as dead worm.
Then thermostatic chamber is moved to, is cultivated under conditions of 20 DEG C~24 DEG C of temperature, the work of investigation in 48 hours borer population, meter after processing
Calculate Revision insect recluced rate.
Calculation method:
Revision insect recluced rate=(living after insect population number-processing before handling to go out to count)/insect population number × 100 before handling
Control efficiency (%)=[(processing Revision insect recluced rate-control Revision insect recluced rate)/(100- compares Revision insect recluced rate)]
×100
By the linear regression analysis between the probit value of preventive effect and the logarithm of series of concentrations, the LC of each medicament is found out50
Value calculates the co-toxicity coefficient (CTC) of mixture with Sun Yunpei's Method, evaluates reagent agent to the activity of germ with this.
The co-toxicity coefficient (CTC) >=120 of compound preparation shows as synergistic effect;CTC≤80 show as antagonism;80 <
CTC < 120 shows as summation action.
The experimental result of the present embodiment is shown in Table 2-1 to table 2-3.
Table 2-1 Herba speranskiae tuberculatae extract compounds the indoor toxicity test to cabbage pieris with Tolfenpyrad
Chemicals treatment | Virulence regression equation | Related coefficient (r) | LC50(mg/L) | Co-toxicity coefficient (CTC) |
Herba speranskiae tuberculatae extract (A) | Y=0.0087+2.2093X | 0.9764 | 181.65 | - |
Tolfenpyrad (B) | Y=3.2355+1.8147X | 0.9835 | 9.38 | - |
A:B=1:5 | Y=3.1564+1.9253X | 0.9933 | 9.03 | 123.38 |
A:B=1:2.5 | Y=3.0848+1.9135X | 0.9848 | 10.02 | 128.41 |
A:B=1:1 | Y=2.5003+2.1584X | 0.9888 | 14.39 | 123.97 |
A:B=2.5:1 | Y=2.1039+2.2544X | 0.9978 | 19.26 | 150.97 |
A:B=5:1 | Y=1.7882+2.2084X | 0.9970 | 28.47 | 157.12 |
A:B=10:1 | Y=1.2067+2.2545X | 0.9978 | 48.15 | 141.32 |
A:B=15:1 | Y=1.2936+2.0437X | 0.9907 | 65.10 | 129.91 |
Table 2-2 Herba speranskiae tuberculatae extract compounds the indoor toxicity test to cabbage pieris with emamectin benzoate
Table 2-3 Herba speranskiae tuberculatae extract compounds the indoor toxicity test to cabbage pieris with capillary
Chemicals treatment | Virulence regression equation | Related coefficient (r) | LC50(mg/L) | Co-toxicity coefficient (CTC) |
Herba speranskiae tuberculatae extract (A) | Y=0.0087+2.2093X | 0.9764 | 181.65 | - |
Capillary (B) | Y=4.8278+1.8051X | 0.9844 | 1.24 | - |
A:B=1:5 | Y=4.8352+2.2886X | 0.9950 | 1.18 | 125.93 |
A:B=1:2.5 | Y=4.7495+2.0158X | 0.9905 | 1.33 | 130.17 |
A:B=1:1 | Y=4.5202+1.776X | 0.9778 | 1.86 | 132.43 |
A:B=2.5:1 | Y=3.6725+2.9836X | 0.9935 | 2.79 | 152.95 |
A:B=5:1 | Y=3.3101+2.4684X | 0.9855 | 4.84 | 148.65 |
A:B=10:1 | Y=2.8012+2.4684X | 0.9854 | 7.78 | 164.12 |
A:B=15:1 | Y=2.4213+2.398X | 0.9887 | 11.89 | 151.36 |
The The Toxicity Determination result of table 2-1 to table 2-3 show: Herba speranskiae tuberculatae extract and Tolfenpyrad, methylamino AVM hereinafter
One of rhzomorph, capillary have higher virulence to cabbage pieris for 1:15~5:1 is mixed with weight ratio, have significant
Synergistic effect.
Indoor toxicity test embodiment 3: apple scale insect indoor toxicity test
In order to prevent and treat the apple scale insect in agricultural production, inventor is with Herba speranskiae tuberculatae extract and spiral shell worm ethyl ester, Buprofezin
The synergy research of mutual compounding is carried out.Test method refers to " People's Republic of China (PRC) agricultural industry criteria NY/T1154.12-
The 12nd part of 2008 farm-chemical indoor determination test rule insecticide: biocidal activity tests tetranychid slide infusion process ", " in
Magnificent the 7th, people's republic's agricultural industry criteria farm-chemical indoor determination test rule of NY/T1154.7-2006 insecticide
Point: mixed synergy measurement ".
Method particularly includes: subjects are apple scale insect, predominantly apple ball a red-spotted lizard (Rhodococcus sariuoni),
Incubates nymph acquires field, does not apply any pesticide before adopting, and polypide growth is consistent.Raw medicine is configured to the investigational agent needed first
Agent, the leaching slide method then recommended using FAO (Food and Agriculture Organization of the United Nation), is attached to glass slide one for the segment that double faced adhesive tape is cut into 3cm long
Then end tears the scraps of paper on viscose glue off with tweezers, choose almost the same, the healthy scale insect of Individual Size, provoked with small writing brush,
Its back is attached on viscose glue and is made its feeler and foot are not stuck, every slide is 30 viscous.4h first is transferred in moisturizing condition, with double
Cylinder dissection spectroscopy, dead worm is chosen and is discarded, then is mended viscous.Then by the slide for being stained with scale insect leaching it is into the liquid gently shake,
The medical fluid of adhesive surface and surrounding, 4 repetitions of every processing, every repetition 30 are sucked with blotting paper through taking-up in 5 seconds, and sets and is free of
The corresponding organic solvent processing of medicament is as control.48h checks test worm death condition after processing, records total borer population and dead borer population,
Calculate Revision insect recluced rate.Dead judgment criteria are as follows: flip the completely motionless person of polypide with small writing brush or the slight springing person of foot is denoted as extremely
Worm.
Calculation method:
Revision insect recluced rate=(living after insect population number-processing before handling to go out to count)/insect population number × 100 before handling
Control efficiency (%)=[(processing Revision insect recluced rate-control Revision insect recluced rate)/(100- compares Revision insect recluced rate)]
×100
By the linear regression analysis between the probit value of preventive effect and the logarithm of series of concentrations, the LC of each medicament is found out50
Value calculates the co-toxicity coefficient (CTC) of mixture with Sun Yunpei's Method, evaluates reagent agent to the activity of germ with this.
The co-toxicity coefficient (CTC) >=120 of compound preparation shows as synergistic effect;CTC≤80 show as antagonism;80 <
CTC < 120 shows as summation action.
The experimental result of the present embodiment is shown in Table 3-1 to table 3-2.
The indoor toxicity test of table 3-1 Herba speranskiae tuberculatae extract and buprofezin compound to apple scale insect
Chemicals treatment | Virulence regression equation | Related coefficient (r) | LC50(mg/L) | Co-toxicity coefficient (CTC) |
Herba speranskiae tuberculatae extract (A) | Y=0.9570+1.6756X | 0.9841 | 258.73 | - |
Buprofezin (B) | Y=3.0518+1.9679X | 0.9850 | 9.77 | - |
A:B=1:5 | Y=2.5735+2.4744X | 0.9973 | 9.56 | 121.72 |
A:B=1:2.5 | Y=2.5075+2.4317X | 0.9967 | 10.59 | 127.24 |
A:B=1:1 | Y=2.6894+2.0896X | 0.9872 | 12.76 | 147.56 |
A:B=2.5:1 | Y=1.3835+2.5895X | 0.9899 | 24.92 | 125.38 |
A:B=5:1 | Y=1.0972+2.5202X | 0.9907 | 35.37 | 139.41 |
A:B=10:1 | Y=1.5744+1.9659X | 0.9851 | 55.27 | 141.15 |
A:B=15:1 | Y=1.0123+2.1474X | 0.9905 | 71.94 | 138.72 |
Table 3-2 Herba speranskiae tuberculatae extract compounds the indoor toxicity test to apple scale insect with spiral shell worm ethyl ester
The Toxicity Determination result (table 3-1, table 3-2) shows: one in Herba speranskiae tuberculatae extract and spiral shell worm ethyl ester, Buprofezin
Kind, there is preferable virulence to apple scale insect for 15:1~1:5 is mixed with weight ratio, there is significant synergistic effect.
Indoor toxicity test embodiment 4: apple yellow aphid indoor toxicity test
Indoor toxicity test embodiment 5: Cucumber blight indoor toxicity test
In order to prevent and treat the aphid for endangering apple, cucumber in agricultural production, inventor is with Herba speranskiae tuberculatae extract and imidacloprid
The synergy research of mutual compounding is carried out.Test method refers to " People's Republic of China (PRC) agricultural industry criteria NY/T1154.12-
The 12nd part of 2008 farm-chemical indoor determination test rule insecticide: biocidal activity tests tetranychid slide infusion process ", " in
Magnificent the 7th, people's republic's agricultural industry criteria farm-chemical indoor determination test rule of NY/T1154.7-2006 insecticide
Point: mixed synergy measurement ".Method particularly includes:
Subjects are apple yellow aphid (Aphis ciricola), Cucumber blight (Aphis gossypii), pick up from field,
Any pesticide is not applied before adopting, polypide growth is consistent.Raw medicine is configured to the test medicine needed first, then uses the United Nations's grain
The segment that double faced adhesive tape is cut into 3cm long is attached to glass slide one end by the leaching slide method of agriculture Organisation recommendations, is then torn off with tweezers viscous
The scraps of paper on glue are chosen almost the same, the healthy aphid of Individual Size, are provoked with small writing brush, its back is attached on viscose glue and
It is stuck its feeler and foot not, every slide is 30 viscous.4h first is transferred in moisturizing condition, spectroscopy is dissected with the bitubular, by dead worm
Choose and discard, then mends viscous.Then by the slide for being stained with aphid leaching it is into the liquid gently shake, inhaled through taking-up in 5 seconds with blotting paper
The medical fluid of adhesive surface and surrounding, 4 repetitions of every processing, every repetition 30 are gone, and is set at the corresponding organic solvent without medicament
Reason is as control.48h checks test worm death condition after processing, records total borer population and dead borer population, calculates Revision insect recluced rate.Death is sentenced
Disconnected standard are as follows: flip the completely motionless person of polypide with small writing brush or the slight springing person of foot is denoted as dead worm.
Calculation method:
Revision insect recluced rate=(living after insect population number-processing before handling to go out to count)/insect population number × 100 before handling
Control efficiency (%)=[(processing Revision insect recluced rate-control Revision insect recluced rate)/(100- compares Revision insect recluced rate)]
×100
By the linear regression analysis between the probit value of preventive effect and the logarithm of series of concentrations, the LC of each medicament is found out50
Value calculates the co-toxicity coefficient (CTC) of mixture with Sun Yunpei's Method, evaluates reagent agent to the activity of germ with this.
The co-toxicity coefficient (CTC) >=120 of compound preparation shows as synergistic effect;CTC≤80 show as antagonism;80 <
CTC < 120 shows as summation action.
The experimental result of the present embodiment is shown in Table 4-1 to table 4-2.
Table 4-1 Herba speranskiae tuberculatae extract compounds the indoor toxicity test to apple yellow aphid with imidacloprid
Chemicals treatment | Virulence regression equation | Related coefficient (r) | LC50(mg/L) | Co-toxicity coefficient (CTC) |
Herba speranskiae tuberculatae extract (A) | Y=0.5819+1.8088X | 0.9886 | 277.10 | - |
Imidacloprid (B) | Y=4.0589+1.8051X | 0.9844 | 3.32 | - |
A:B=1:5 | Y=3.8221+2.4342X | 0.9941 | 3.05 | 130.31 |
A:B=1:2.5 | Y=3.8831+2.0876X | 0.9821 | 3.43 | 134.86 |
A:B=1:1 | Y=3.8098+1.8599X | 0.9721 | 4.36 | 150.49 |
A:B=2.5:1 | Y=3.5382+1.7149X | 0.9942 | 7.12 | 158.46 |
A:B=5:1 | Y=2.3860+2.417X | 0.9701 | 12.06 | 155.84 |
A:B=10:1 | Y=2.2397+2.0879X | 0.9806 | 20.99 | 155.37 |
A:B=15:1 | Y=2.6202+1.5947X | 0.9781 | 31.07 | 144.92 |
Table 4-2 Herba speranskiae tuberculatae extract compounds the indoor toxicity test to Cucumber blight with imidacloprid
Chemicals treatment | Virulence regression equation | Related coefficient (r) | LC50(mg/L) | Co-toxicity coefficient (CTC) |
Herba speranskiae tuberculatae extract (A) | Y=0.1380+2.0051X | 0.9789 | 265.96 | - |
Imidacloprid (B) | Y=5.7994+1.5128X | 0.9898 | 0.30 | - |
A:B=1:5 | Y=6.3688+2.4949X | 0.9892 | 0.28 | 128.54 |
A:B=1:2.5 | Y=6.1532+2.3566X | 0.9888 | 0.32 | 131.19 |
A:B=1:1 | Y=5.7687+1.9951X | 0.9894 | 0.41 | 146.18 |
A:B=2.5:1 | Y=5.2869+1.7438X | 0.9873 | 0.69 | 151.75 |
A:B=5:1 | Y=4.8663+2.2394X | 0.9924 | 1.15 | 155.64 |
A:B=10:1 | Y=4.4462+1.6307X | 0.9742 | 2.19 | 149.00 |
A:B=15:1 | Y=3.9805+2.0079X | 0.9891 | 3.22 | 146.59 |
(table 4-1 to table 4-2) shows: Herba speranskiae tuberculatae extract and imidacloprid are with weight ratio for 15:1 for The Toxicity Determination result
~1:5 is mixed to have higher virulence to apple yellow aphid, Cucumber blight, there is significant synergistic effect.
2, field trial part
Field trial embodiment 1: prevention and treatment brassicaceous vegetable diamondback moth field trial
(the 30% Herba speranskiae tuberculatae extract Tolfenpyrad of example of formulations 1 has been carried out in Shaanxi Province's Yangling Area within 2015
Suspending agent), example of formulations 2 (16% Herba speranskiae tuberculatae extract emamectin benzoate suspending agent) and example of formulations 4 (30%
Herba speranskiae tuberculatae extract capillary suspending agent) prevention and treatment brassicaceous vegetable diamondback moth field trial.
Test method is referring to " pesticide field efficacy medicine test criterion (one) insecticide control brassicaceous vegetable lepidopterous larvae
Sick GB/T 17980.13-2000 ".Field control effectiveness test is in the 5 days-September of September in 2015 13rd in the northwest agriculture of Shaanxi Province Yangling District
Woods University of Science and Technology experimental field carries out, and soil is an animal-drawn seed plough soil, and experimental plot area is 900 square metres.Trial crops are brassicaceous vegetable
(wild cabbage), kind be in sweet No. 8, controlling object be diamondback moth (Plutella xylostella).Experimental field soil pH value 7.1,
Fertility is preferable, experimental field cultivation condition uniformity.Test medicine and extension rate are shown in Table 5.Separately set blank control, every processing 4
Secondary repetition, every 30 ㎡ of plot area, totally 32 cells, random district's groups arrange.Using conventional spray-on process, mu is administered liquid 45kg.The
It is carried out before being once administered to three age of diamondback moth larvae, in wild cabbage positive value growth period, application is primary.
Investigation and statistical method:
Investigate insect population before medicine, 1d, 3d, 7d investigate population number after application after medicine.When investigation, every cell exists
10 plants of wild cabbages are determined in middle position, investigate on determining 10 plants of wild cabbages every time.It is investigated before application and every time after application and records 3 respectively
Larva below age and Larva.
Drug effect calculation method
Formula in field efficacy calculation basis " pesticide field efficacy medicine test criterion " calculates Revision insect recluced rate and prevention and treatment effect
Fruit.
Security survey: every time after spray 10 days after the 1st day and medicine, observation medicament respectively handles the influence to wild cabbage.
Table 5 prevents and treats brassicaceous vegetable (wild cabbage) diamondback moth field test results
Note: in 0.05 horizontal difference between lowercase expression processing.
Field test results (table 5) show: 30% 120,135 grams of Herba speranskiae tuberculatae extract Tolfenpyrad suspending agent effectively at
Point/hectare, 16% 48,54 grams of Herba speranskiae tuberculatae extract emamectin benzoate suspending agent effective component/hectare, 30% lopseed
1 day preventive effect is poor after 67.5,72 grams of effective component/hectares of extract capillary suspending agent are administered wild cabbage plutella xylostella, application
There is preferable preventive effect within 3 days afterwards, 7 days, 1,3 day after application, 30% 135 grams of Herba speranskiae tuberculatae extract Tolfenpyrad suspending agent is effective
Ingredient/hectare, 30% 54 grams of effective component/hectares of Herba speranskiae tuberculatae extract emamectin benzoate suspending agent, 30% lopseed
72 grams of effective component/hectare preventive effects of extract capillary suspending agent are in 0.05 level better than deep to comparison medicament 10%
360 grams of effective component/hectares of herb microemulsion.And from the point of view of dosage, Tolfenpyrad, methylamino Avermectin in three kinds of mixtures
Element and capillary dosage reduce 50% or more, alleviate environmental pressure.
It is observed during test, each chemicals treatment does not generate phytotoxicity phenomenon to crop.
After test result shows Herba speranskiae tuberculatae extract and Tolfenpyrad, emamectin benzoate and capillary mixture, hence it is evident that
The control efficiency to brassicaceous vegetable diamondback moth is improved, dosage is reduced, safety is grown to wild cabbage, is prevention and treatment diamondback moth
Favourable agents.
Field trial embodiment 2: prevention and treatment prevention and treatment brassicaceous vegetable cabbage caterpillar field trial
(the 30% Herba speranskiae tuberculatae extract Tolfenpyrad of example of formulations 1 has been carried out in Shaanxi Province's Yangling Area within 2015
Suspending agent), example of formulations 2 (16% Herba speranskiae tuberculatae extract emamectin benzoate suspending agent) and example of formulations 4 (30%
Herba speranskiae tuberculatae extract capillary suspending agent) prevention and treatment brassicaceous vegetable cabbage caterpillar field trial.
Test method is referring to " pesticide field efficacy medicine test criterion (one) insecticide control brassicaceous vegetable lepidopterous larvae
Sick GB/T 17980.13-2000 ".Testing ground area is 900 square metres.Trial crops are brassicaceous vegetable (wild cabbage), product
Sweet No. 8 in kind being, controlling object is cabbage caterpillar (Pieris rapae).Experimental field soil pH value 7.1, fertility is preferable, experimental field
Cultivation condition uniformity.Test medicine and extension rate are shown in Table 6.Separately set blank control, 4 repetitions of every processing, every cell face
30 ㎡ of product, totally 32 cells, random district's groups arrange.Using conventional spray-on process, mu is administered liquid 45kg.It is administered to cabbage caterpillar for the first time
Larva carried out before three ages, and in wild cabbage positive value growth period, application is primary.
Investigation and statistical method:
Investigate insect population before medicine, 1d, 3d, 7d investigate population number after application after medicine.When investigation, every cell exists
10 plants of wild cabbages are determined in middle position, investigate on determining 10 plants of wild cabbages every time.It is investigated before application and every time after application and records 3 respectively
Larva below age and Larva.
Drug effect calculation method
Formula in field efficacy calculation basis " pesticide field efficacy medicine test criterion " calculates Revision insect recluced rate and prevention and treatment effect
Fruit.
Security survey: every time after spray 10 days after the 1st day and medicine, observation medicament respectively handles the influence to wild cabbage.
Table 6 prevents and treats brassicaceous vegetable (wild cabbage) cabbage caterpillar field test results
Note: in 0.05 horizontal difference between lowercase expression processing.
Field test results (table 6) show: 30% 120,135 grams of Herba speranskiae tuberculatae extract Tolfenpyrad suspending agent effectively at
Point/hectare, 16% 48,54 grams of Herba speranskiae tuberculatae extract emamectin benzoate suspending agent effective component/hectare, 30% lopseed
1 day preventive effect is poor after 67.5,72 grams of effective component/hectares of extract capillary suspending agent are administered cabbage pieris, application
There is preferable preventive effect within 3 days afterwards, 7 days, 1 after application, 3,7 days, in 0.05 horizontal equal no significant difference between each processing.From using
From the point of view of dosage, Tolfenpyrad, emamectin benzoate and capillary dosage reduce 50% or more in three kinds of mixtures, alleviate environment
Pressure.
It is observed during test, each chemicals treatment does not generate phytotoxicity phenomenon to crop.
After test result shows Herba speranskiae tuberculatae extract and Tolfenpyrad, emamectin benzoate and capillary mixture, hence it is evident that
The control efficiency to brassicaceous vegetable cabbage caterpillar is improved, dosage is reduced, safety is grown to wild cabbage, is prevention and treatment cabbage caterpillar
Favourable agents.
Field trial embodiment 3: prevention and treatment apple yellow aphid field trial
(24% Herba speranskiae tuberculatae extract of example of formulations 3 has been carried out in Shaanxi Province, the town Shi De, Liquan County Northern Wei Dynasty village within 2016
Imidacloprid suspending agent) prevention and treatment apple yellow aphid field trial.
Test method is referring to " pesticide field efficacy medicine test criterion (one) insecticide control fruit aphid GB/T 17980.9-
2000".Experimental field soil is an animal-drawn seed plough soil, and experimental plot area is 600 square metres.Trial crops are apple, and kind is Fuji apple.Prevention and treatment
Object is yellow aphids (Aphis citricola).Experimental field soil pH value 7.1, fertility is preferable, experimental field cultivation condition uniform one
It causes.Test medicine and extension rate are shown in Table 7.Separately set blank control, 4 repetitions of every processing, 2 plants of fruit trees of every cell are totally 20 small
Area, random district's groups arrangement.Using conventional spray-on process, mu is administered liquid 200kg.Just peak period carries out spraying time apple aphid, application
Once.
Investigation and statistical method:
Insect population is investigated before medicine, after medicine 1 after application, 3,7,14 days investigation population numbers.It is investigated before spray
It when aphid radix, respectively repeats to fix 2 plants of fruit trees, selectes 5 brachyplasts at random by all directions five positions as listed sampling
Fixed point.Investigation every time, records the aphid amount on continuous 10 leaves of every sampling point.
Drug effect calculation method
Formula in field efficacy calculation basis " pesticide field efficacy medicine test criterion " calculates Revision insect recluced rate and prevention and treatment effect
Fruit.
Security survey: every time after spray 14 days after the 1st day and medicine, observation medicament respectively handles the influence to apple tree.
Table 7 prevents and treats apple aphid field test results
Note: in 0.05 horizontal difference between lowercase expression processing.
Field test results (table 7) show: the dilution of 24% 3000,2000 times of Herba speranskiae tuberculatae extract imidacloprid suspending agent,
70% imidacloprid water dispersible granule of liquid, 14000 times poor to 1 day preventive effect after apple aphid application, 3 after application, has within 7,14 days
Preferable preventive effect, 1 after application, 3,7,14 days, in 0.05 horizontal equal no significant difference between each processing.From the point of view of dosage,
Imidacloprid dosage reduces 60% in 24% Herba speranskiae tuberculatae extract imidacloprid suspending agent, alleviates environmental pressure.
It is observed during test, each chemicals treatment does not generate phytotoxicity phenomenon to crop.
After test result shows Herba speranskiae tuberculatae extract and imidacloprid mixture, hence it is evident that improve the prevention and treatment effect to apple aphid
Fruit reduces dosage, is the anti-favourable agents that eliminate aphis to apple development safety.
Field trial embodiment 4: prevention and treatment apple scale insect field trial
In Xianyang, Shanxi province city, the town Shi De Northern Wei Dynasty village, Liquan County having carried out example of formulations 5 within 2015, (30% lopseed mentions
Take object spiral shell worm ethyl ester suspending agent), example of formulations 6 (20% Herba speranskiae tuberculatae extract Buprofezin microemulsion) prevention and treatment apple shell
Worm field trial.
Test method is referring to " pesticide field efficacy medicine test criterion (one) insecticide control citrus scale insect GB/T
17980.12-2000 ".Trial crops are apple, and kind is Fuji apple, and controlling object is that (principal item is apple ball to scale insect
A red-spotted lizard (Rhodococcus sariuoni).3 mu of testing ground area, Apple Culture management is preferable.Test medicine and dosage are detailed in table
8.Comparison medicament and blank control are separately set, 4 repetitions of every processing, 2 plants of fruit trees of every cell, totally 32 cells, random district's groups arrange.
Using conventional spray-on process, mu is administered liquid 200kg, uniformly sprays apple complete stool.It is administered 1 time, is administered in scale insect nymph altogether.
Investigation and statistical method:
When investigating scale insect radix before spray, respectively repeats to fix 2 plants of fruit trees, be selected at random by all directions five positions
Fixed point of fixed 5 brachyplasts as listed sampling.It 3 after medicine, investigates within 7,14 days, investigates every time, record continuous 10 leaves of every sampling point
On scale insect worm amount.
Preventive effect is calculated according to investigation result.Every time after spray 14 days after the 1st day and medicine, observation medicament is respectively handled to rice
It influences.
Table 8 prevents and treats apple scale insect field test results
Note: in 0.05 horizontal difference between lowercase expression processing.
Field test results (table 8) show: 30% 1500 times of Herba speranskiae tuberculatae extract spiral shell worm ethyl ester suspending agent, 2000 times,
240 grams per liter spiral shell worm ethyl ester suspending agent of 20% 1500 times, 2000 times of Herba speranskiae tuberculatae extract Buprofezin microemulsion and comparison medicament
4000 times, the processing of 25% 2500 times of wettable powder with buprofezin to after apple scale insect medicine 3,7,14 days have it is preferable anti-
Effect is substantially better than 200 times of 10% deep herb microemulsion processing to the preventive effect of apple scale insect in 0.05 level.
Security survey to apple is observed after spray for 14 days after the 1st day and medicine, and each test process is existing without phytotoxicity to apple
As occurring.Test also found that three kinds of Mixed Pharmacies also have good preventive effect to apple aphid.
Test result shows Herba speranskiae tuberculatae extract respectively and after spiral shell worm ethyl ester, Buprofezin mixture, hence it is evident that improves to apple
The control efficiency of scale insect reduces dosage and drug cost, is the ideal for preventing and treating apple scale insect to apple development safety
Medicament.
In conclusion composition of the invention is using Herba speranskiae tuberculatae extract and Tolfenpyrad, emamectin benzoate, pyrrole
The two kinds of active components compound scheme of one of worm quinoline, capillary, spiral shell worm ethyl ester, Buprofezin composition, activity and desinsection effect
Fruit is not the active simple superposition of each component, compared with existing single formulation, in addition to significant insecticidal effect, and Er Qieyou
Significant synergistic effect, it is good to crop safety, meet the security requirement of pesticidal preparations.
Claims (4)
1. a kind of agricultural insecticidal composite containing Herba speranskiae tuberculatae extract, which is characterized in that including the first active constituent lopseed
The mass ratio of extract and the second active constituent Tolfenpyrad, the first active constituent and the second active constituent is 15:1~1:
5;
The Herba speranskiae tuberculatae extract is prepared by the following method: using the smashed lopseed of organic solvent soaking at room temperature, ultrasonic extraction 3
Secondary, each ultrasonic extraction 30min is filtered, and Herba speranskiae tuberculatae extract is concentrated under reduced pressure to obtain in merging filtrate;
The organic solvent selects methanol.
2. according to claim 1 containing the agricultural insecticidal composite of Herba speranskiae tuberculatae extract, which is characterized in that the desinsection group
The dosage form for closing object is suspending agent, aqueous emulsion or microemulsion.
3. use of the agricultural insecticidal composite containing Herba speranskiae tuberculatae extract on prevention and treatment crop pests according to claim 1
On the way.
4. the agricultural insecticidal composite according to claim 3 containing Herba speranskiae tuberculatae extract is on prevention and treatment crop pests
Purposes, which is characterized in that the crop pests include brassicaceous vegetable cabbage caterpillar, apple scale insect, apple aphid, cucumber
Aphid.
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Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1206559A (en) * | 1997-07-30 | 1999-02-03 | 殷剑明 | Pesticide capable of killing beetle and ladybug and its preparation method |
CN104351194A (en) * | 2014-11-11 | 2015-02-18 | 济南新起点医药科技有限公司 | Cotton pesticide |
CN105475292A (en) * | 2015-12-04 | 2016-04-13 | 浙江威尔达化工有限公司 | Insecticidal composition containing tolfenpyrad and tea saponin and application thereof |
-
2016
- 2016-08-28 CN CN201610742930.3A patent/CN106342905B/en not_active Expired - Fee Related
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1206559A (en) * | 1997-07-30 | 1999-02-03 | 殷剑明 | Pesticide capable of killing beetle and ladybug and its preparation method |
CN104351194A (en) * | 2014-11-11 | 2015-02-18 | 济南新起点医药科技有限公司 | Cotton pesticide |
CN105475292A (en) * | 2015-12-04 | 2016-04-13 | 浙江威尔达化工有限公司 | Insecticidal composition containing tolfenpyrad and tea saponin and application thereof |
Non-Patent Citations (3)
Title |
---|
几种复配剂对茶小绿叶蝉田间防效;赵霞 等;《农药》;20160731;第55卷(第7期);第544-546页 * |
新型高效杀虫剂-唑虫酰胺;谭立云;《农药市场信息》;20091231;第38页 * |
长白山野生杀虫植物资源;金大勇 等;《农药》;20031231;第42卷(第6期);第6-11页 * |
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