CN1839695A

CN1839695A - Aqueous pesticide and preparation method thereof

Info

Publication number: CN1839695A
Application number: CNA2005100114855A
Authority: CN
Inventors: 米鹤都; 高志钢
Original assignee: Huajing Wufang Practical Nanometer Science & Technology Developing Co Ltd Be
Current assignee: Mi Hedu
Priority date: 2005-03-28
Filing date: 2005-03-28
Publication date: 2006-10-04
Anticipated expiration: 2025-03-28
Also published as: CN100563447C

Abstract

The invention relates to a water-based pesticide, which comprises pesticide active ingredient, pricklyash peel extract, emulsifying agent, auxiliary solvent, stabilizer and water as dispersing agent. The invention also relates to the process for preparing the pesticide.

Description

A kind of aqueous pesticide and preparation method thereof

Technical field

The present invention relates to pesticide field, specifically, the present invention relates to a kind of aqueous pesticide and preparation method thereof.

Background technology

The widely-used meeting of chemical pesticide pollutes environment, and people and animals are also had certain murder by poisoning, therefore, reduces toxicity, improves the inexorable trend that drug effect is the agricultural chemicals development.And there are problems such as scarce capacity, cost height in China's present pesticide original medicine research and development, research and develop by formulation therefore that to reduce toxicity, improve drug effect be a kind of economy mode efficiently.

At present, China is more single in the formulations of pesticide, and 70-80% is missible oil and wetting powder in all preparations.Obviously, this far can not adapt to the variation of current agricultural production development to the agricultural chemicals demand, and has influenced the marketing and the service life of Pesticidal products to a great extent.Therefore, more should pay attention to the transformation of existing formulation and the novel form that research and development meet production and environmental requirement.

The novel form of agricultural chemicals also can increase new feature to agricultural chemicals, more can give full play to the action characteristic of former medicine self, overcome and remedy the deficiency of the original formulation of agricultural chemicals, toxicity and excitant to people and animals are all lower, and can alleviate poisoning to crop, improve physico chemistry and biological property, enlarge range of application, prolong the service life of medicament etc.

Comparatively convenient and what generally use is liquid formulation in the agricultural chemicals, wherein using maximum formulations is missible oil.Missible oil needs to use a large amount of organic solvents in process, as benzene,toluene,xylene or the like, the use of a large amount of organic solvents not only causes the waste of industrial chemicals, and since the combustibility of solvent on transportation, storage and container selection, also be restricted.Simultaneously, brought very big murder by poisoning for environment and human health.Developed country limits or forbids using in a large number the pesticide new variety registration of toxic organic solvent preparations such as benzene,toluene,xylene from sustainable development target.Therefore, reduce or avoid these virulent organic solvents, develop the trend of the times that novel liquid formulation has become the agricultural chemicals development.Wherein, Water-borne modification is exactly one of dominant direction of formulations of pesticide development.A series of water base property novel forms such as aqueous solvent, microemulsion, emulsion, suspending agent, suspended emulsion, microcapsule formulations etc. have appearred in recent years.

Aqueous solvent comprises: active ingredient forms the homogeneous liquid preparation of true solution behind soluble concentrate (soluble concentrate the is called for short SL) dilute with water.The aqueous solution preparation of aqua (aqueous solution is called for short AS) active ingredient and auxiliary agent.But active ingredient forms the glue-like preparation of true solution behind glue (water soluble gel the is called for short GW) dilute with water.China is used for the former medicine content generally not high (as dimehypo) of process water solvent, is difficult to be processed into the aqueous solvent of high concentration, thereby packing charges and storage fee are with higher.

External principal item has 41% farming to reach (aqueous solvent that is the processing of 360g/l glyphosate and 15% auxiliary agent), 48% Dicamba, 20% Gramoxone and 25% prowers aqueous solvent etc.China's principal item has glyphosate and amine salt, 2-first-4-chlorine, jinggangmeisu, ethrel, dimehypo, single carbonamidine aqueous solvent etc.

Microemulsion (Microemulsion) is one of novel form that meets the agricultural chemicals developing direction, and international code name: the ME of formulation is made up of water, water-insoluble and water-soluble substance, and former medicine is with the microparticulate preparation wherein of 0.01-0.1 μ.It is a stable homogeneous phase on the thermodynamics, the solubility system.Outward appearance is transparence, and microcosmic is to be the limiting condition that aqueous emulsion fully disperses for the big micellar dispersion that expands.Its physics, chemical stability are good, and is strong to plant and insect tissue cell permeability, the absorption ratio height, and preventive effect is good, simultaneously, has production, storing and safe in utilization, and environmental pollution is little, helps the improvement of ecotope.

External existing kind is commodity such as 10% efficient phenothrin, 5% permethrin, 30% binapacryl microemulsion.China has microemulsions such as 5% beta-cypermethrin, 3% Acetamiprid, 0.5% first dimension salt and 10% Feng Wei.

Aqueous emulsion (claim emulsion again, emulsion in water is called for short EW) aqueous emulsion is that active ingredient is dissolved in the organic solvent, and is dispersed in the continuous phase water with small liquid pearl, becomes heterogeneous emulsion preparation.It is oil-in-water type (O/W) emulsion dispersion.The active ingredient particle diameter that aqueous emulsion is dispersed in the water is 0.1～50 μ m, thereby outward appearance is a milky, it is hydrophobic liquid or LMP (＜60 ℃) solid pesticide, an amount of water-immiscible solvent or solvent-free leaving,, former medicine is scattered in the water by suitable emulsifier through high degree of agitation, add auxiliary agents such as stabilizing agent, antifreezing agent then, make through high speed shear, wherein active ingredient must be medium-term and long-term stable at water, and solvability is less in the water.The processing maximum concentration is generally below 30%.As if it should be noted that required solvent ratios is several times of active substance when the solid active agents (as fenoxapropPethyl) of indissoluble is compared in dissolving, the ratio that has even surpass water has lost oil-in-water meaning.The processing cost of aqueous emulsion generally is lower than the missible oil of equal specification.

Abroad the aqueous emulsion in China's registration has: 6.9% prestige frost (fenoxapropPethyl), 45% Shi Baoke (prochloraz), 10.4% row happiness towns (bioallethrin), 60% rich ground (butachlor), 5% difficult to understand fly gram (cypermethrin), 10% extremely and spray gram, 13% alkynes mite-azoles mite (speed despot mite).Domestic principal item has: 2.5% gamma cyhalothrin aqueous emulsion, 16% high chlorbenside list aqueous emulsion, 4.5% high performance aqueous emulsion of cypermethrin, 30% chlorpyrifos aqueous emulsion, 60% butachlor aqueous emulsion etc.

Suspending agent (aqueous suspension concentrate is called for short SC) is non-water-soluble solid active ingredient and relevant auxiliary agent, forms the thickness suspension preparation of high degree of dispersion in water, uses behind the dilute with water.The advantage of this formulation is: (1) no dust harzard, and to operator and Environmental security.(2) with water be matrix, not inflammable the and drug injury problem that produces by organic solvent.(3) compare with wetting powder, allow to select for use the former medicine of different-grain diameter, so that make the biological effect physical stability of preparation reach best.(4) liquid suspension spreads in water well, can directly make spray liquid and use.(5) than great, packaging volume is little.

External principal item has: 43% tebuconazole suspension concentrates, the sweet suspending agent of 30.15% pyrrole ether grass, 24% thifluzamide suspending agent, 2.25% formamido group Sulfometuron Methyl oil-suspending agent, 12.5% epoxiconazole suspension concentrate, 1% remove barnyard grass peace suspending agent etc.Domestic a few days ago registered suspending agent kind has: sulphur deflocculant more than 50%, 40% tpn suspending agent, 10% rattle away mite piperazine suspending agent, 24% methoxyfenozide suspending agent, 18,%00 white urea suspending agent, 30% mancozeb suspending agent etc.

Suspended emulsion (aqueous suspo-emul-sion is called for short SE) is to contain two kinds of water-fast active ingredients at least, and stably being dispersed in water with solia particle and fine liquid pearl form is continuous-flow heterogeneous liquid preparation mutually.Suspended emulsion is the stabilising system of a three-phase, has the advantage of suspending agent and emulsion, has broken the single formulation that only disposes with solid or the former medicine of liquid, has realized the simultaneous mixing formulation of the former medicine of solid-liquid body.This formulation advantage is: (1) higher suspension rate and high dispersive homogeneity.(2) stability for storage.(3) of reduced contamination to environment is lower to operator's murder by poisoning.(4) with water be medium, storing safety.(5) has good biologically active.In the time of the former medicine of a kind of water insoluble solid and a kind of water-insoluble liquid crude need being made mix preparation, it is particularly suitable to be processed into suspended emulsion.

Domestic have 40% cyanogen Tianjin second suspended emulsion, 40% different third careless green bristlegrass suspended emulsion, 40% green second green bristlegrass suspended emulsion at present.

Microcapsule formulations also is called micro-capsule suspension (aqueous capsule sus-pension is called for short CS).It is as cyst wall or cyst membrane with macromolecular material, by chemistry, physics or physicochemical method, to wrap up as the pesticidal active substance of the capsule heart, form a kind of translucent microencapsulation, and they are stably disperseed, are suspended in the water as continuous phase with finite concentration.This formulation characteristic and performance: it separates oil phase and water (1), so some hydrolabil pesticide activity component (as organophosphorus insecticide) is difficult to make aqueous emulsion and microemulsion, can make microcapsule formulations.(2) suppress decomposition and the loss that environmental factor such as light, heat, air, rainwater, soil, microorganism and other chemical substance cause, improved the stability of medicament itself, helped ecology and environment.(3) cyst membrane can suppress the volatility of agricultural chemicals, shelters its original peculiar smell, reduces its contact toxicity, toxicity on inhalation and poisoning, alleviates it to people and animals' excitant with to toxicity of fish etc.(4) introduce control release technic, improve the availability of agricultural chemicals, prolong its drug effect phase, thereby can reduce the quantity and the frequency of dispenser, alleviate the pressure of agricultural chemicals environment.(5) provide convenience for the composite of pesticidal active substance of multiple different performance.(6) the cyst membrane existence has also improved preparation colloid physical stability.

The primary commercial kind has 15% Imidacloprid microcapsule suspending agent, 36% clomazone microcapsule suspending agent, 20% to occupy U.S. desinsection microcapsule suspending agent etc.

Improve aqueous pesticide to the control of insect with increase biologically active such as lasting period, the wettability, adhesivity and the permeability that increase active ingredient in the aqueous pesticide are very important.Generally adopt the method for adding suitable auxiliary agent in aqueous pesticide to increase wettability, adhesivity and the permeability of active ingredient in the aqueous pesticide both at home and abroad, selected auxiliary agent mainly contains dispersant, wetting agent, emulsifier, synergist, bleeding agent, spreader-sticker, sticker, stabilizing agent, thickener, film forming agent, anticoalescent, anti-caking agent, disintegrant, defoamer, the antipoison of preventing drift agent, antistatic agent, poisoning palliative, weed killer herbicide and propellant etc.At present, insecticides adjuvant is being just big, high-effect towards molecular weight, low consumption, multi-functional, high-quality, inexpensive direction develop, but finds as yet relevant Chinese prickly ash or pepper extract (zanthoxylum husk cream p.e) etc.s to be applied to the report of aqueous pesticide with the effect of raising agricultural chemicals both at home and abroad.

Summary of the invention

The purpose of this invention is to provide a kind of aqueous pesticide that contains pepper extract; Further purpose provides the preparation method of described aqueous pesticide.Pepper extract among the present invention can make up widely with aqueous pesticide, except direct minimizing pesticide dosage, also can reduce spraying times, in addition, because the joint toxicity of pepper extract and agricultural chemicals is antagonism, not only reduced the toxicity of agricultural chemicals, also reduced the residual of agricultural chemicals, so it uses the safety in utilization that has also just increased agricultural chemicals.

The invention provides a kind of aqueous pesticide, it comprises pesticide activity component and pepper extract, and described pesticide activity component and pepper extract amount ratio by weight are 1: 0.005-100.Preferably, pesticide activity component and pepper extract by weight amount ratio be 1: 0.01-50.

Aqueous pesticide of the present invention, wherein pesticide activity component is selected from one or more in insecticide, bactericide and the weed killer herbicide.

Aqueous pesticide of the present invention, one or more in the insecticide of the preferred organochlorine class of wherein said insecticide, pyrethroid, carbamates, organic phosphates, nereistoxin, biological species insecticide and other types (, azoles mite ester grand, Imidacloprid etc.) as Avermectin, Affirm (Merck Co.) and salt thereof, fluorine bell urea, flufenoxuron, Acarus tritici urea, desinsection; Described bactericide is selected from organic sulfur class, organo-arsenic class, organic phosphates, substituted benzene, azole, antibiotics, 1,2, one or more in the 4-triazole bactericidal agent; Described weed killer herbicide is selected from one or more in the phenoxy carboxylic acid, amide-type, substituted urea class, phenyl amines, carbamates, triazine, organic phosphates weed killer herbicide (as glyphosate, increase sweet phosphine, careless ammonium phosphine, bilanafos);

In the further preferred 5a,6,9,9a-hexahydro-6,9-methano-2,4 of described pesticide activity component, gamma cyhalothrin, decis, cypermethrin and various isomer, Hostathion, carbosulfan, Methomyl, Avermectin, Affirm (Merck Co.) and salt thereof, fluorine bell urea, azoles mite ester, Imidacloprid, tolelofos-methyl, triazolone, the matrine one or more.

In aqueous pesticide of the present invention, except containing pesticide activity component and pepper extract, also can contain cosolvent, emulsifier, wherein the percentage by weight of various components is:

Pesticide activity component 0.1-30%

Pepper extract 0.1-30%

Cosolvent 1-10%

Emulsifier 5-20%

Water surplus.

Also contain stabilizing agent in the aqueous pesticide of the present invention, the percentage by weight of its each component is:

Pesticide activity component 0.1-30%

Pepper extract 0.1-30%

Cosolvent 1-10%

Emulsifier 5-20%

Stabilizing agent 5-10%

Water surplus.

Among the present invention, cosolvent is meant alcohols (as ethanol, isopropyl alcohol, n-butanol, n-amyl alcohol, hexanol etc.), ketone (as acetone, cyclohexanone etc.), amide-type (as dimethyl formamide etc.), naphthenic (as cyclohexane etc.), aromatic hydrocarbons (as benzene,toluene,xylene, Fluhyzon etc.), also can be to well known to a person skilled in the art other cosolvent.Cosolvent can be wherein any one, or multiple combination.

Wherein preferred cosolvent is ethanol, isopropyl alcohol, n-butanol, n-amyl alcohol, acetone, cyclohexanone, dimethyl formamide, cyclohexane, benzene, toluene and/or dimethylbenzene.

Among the present invention, emulsifier is meant non-ionic surface active agent and/or anion surfactant.The non-ionic surface active agent that can adopt is selected from: castor oil ethylene oxide adduct, phenethyl phenol polyethenoxy ether, phenethyl phenol polyethenoxy polyethenoxy ether, phenethyl phenol polyethenoxy ether phosphate, alkylphenol polyoxyethylene formaldehyde condensation products, benzylbiphenyl phenol polyethenoxy ether, alkylphenol polyoxyethylene or xenol APEO etc.The anion surfactant that can adopt is selected from: alkylbenzenesulfonate is (as C ₁₀-C ₁₄The calcium of-alkyl benzene sulphonate, magnesium, sodium salt), C ₈-C ₂₀-alkylsurfuric acid sodium salt (as lauryl sodium sulfate salt) or styrene polyoxyethylene ether ammonium sulfate salt etc.

The compound of wherein preferred nonionic and anion surfactant.When the present invention specifically implements, preferably adopt commercially available various emulsifier types, for example: emulsifier can be selected from No. 500, farming breast, agricultural emulsifier NO series (as the newborn 601-606 of farming number), Nongru-700 series is (as peaceful newborn No. 36, No. 37, peaceful breast, Nongru-700-1,700-2, the newborn SPF of farming), NP-10, No. 1600 series of farming breast are (as farming breast 1601,1602, peaceful breast 33, No. 34), No. 2000, farming breast, No. 11, farming breast, No. 12, farming breast, PF-690, BY series is (as peaceful newborn 110,120,130,140, the EL emulsifier), tween series is (as Tween-40, Tween-60, Tween-80), Sorpol series (Sorpol KS, Sorpol KD, Sorpol-2676, Sorpol-2678S etc.) or have any one or a multiple combination in the emulsifier of similar features.

Can also contain stabilizing agent in the aqueous pesticide of the present invention, be used to increase the physics and the chemical stability of microemulsion.Accord with stabilizing agent of the present invention and be 2-expoxy propane, butyl glycidyl ether, polyethylene glycol diglycidyl ether or sorbierite, isopropyl alcohol, n-butanol, ethylene glycol, polyethylene glycol, urea, propane diols, glycerine and well known to a person skilled in the art stabilizing agent as any one.

Wherein preferred ethylene glycol, polyethylene glycol, urea and glycerine, its consumption is 5-10%.This class stabilizing agent has the dual function of stabilizing agent and antifreezing agent.

The water that adopts among the present invention can be running water, deionized water etc., deionized waters such as wherein preferred distilled water.

In addition, aqueous pesticide of the present invention can also add other auxiliary element such as antifreezing agent (as ethylene glycol, propane diols, glycerine, polyethylene glycol, sorbierite etc.), preservative (as formaldehyde) etc.These processing aids generally add the amount of 0.1-10%.

Aqueous pesticide of the present invention can be made the form of aqueous solvent, microemulsion, emulsion, suspending agent, suspended emulsion or microcapsule formulations.

The present invention also provides a kind of method for preparing described aqueous pesticide, and it comprises the steps:

1. pepper extract is dissolved in the dispersion medium water, forms solution A;

2. with pesticide activity component and cosolvent and/or emulsifier and/or auxiliary element, stir, form solution B;

3. merge solution A and B, homogenize.

The present invention also provides the method for the described aqueous pesticide of another kind of preparation, and it comprises the steps:

1. incite somebody to action the not water miscible pepper extract of tool and pesticide activity component, cosolvent and/or emulsifier and/or stabilizing agent, stir, make solution A;

2. merge solution A and dispersion medium water, homogenize.

This method can adopt conventional method and apparatus to finish, referring to: formulations of pesticide process technology (second edition) 406-408 page or leaf, Liu Bulin chief editor, Chemical Industry Press.

The preparation method of preferred aqueous pesticide of the present invention is: pesticide activity component is dissolved in the cosolvent, drop into emulsifier, drop into remaining auxiliary element again (for example when containing stabilizing agent, drop into stabilizing agent again), stir, mix homogenize with the dispersion medium water that contains pepper extract then.

The present invention also can adopt the method for emulsifying technology and nanometer technology (for example liquid flow depth degree ultra micro disperses) combination to prepare.

Chinese prickly ash (Pericarpium Zanthoxyli) is the pericarp of rutaceae Chinese prickly ash Zanthoxylumbungeanum Maxim..The ripening fruits of gathering autumn is dried, and removes seed and impurity

Differentiate:

Thin-layer method (TLC): 0.5 gram Chinese prickly ash powder is put into 5ml ethanol, soaked 30 minutes, make sample with leachate.Prepare 0.1% magnoline ethanolic solution, get two drips of solution on (containing 1%H-CMC) thin-layer silicon offset plate, the TLC plate is placed in butanols-acetate-water (7: 1: 2) solution to stretch rises to about 10 centimeters, take out and dry, and with Dragendorff's reagent spraying, leachate can demonstrate yellow spotting with the tomographic map of contrast liquid phase correspondence position.

Contain volatile oil in the Chinese prickly ash pericarp, contain different anisole (isobutyl anisole) and (the right dragon of left ox) geraniol in the oil, have special strong aroma.Japan pepper essential oil content is generally 4%～7%.The main component of Japan pepper essential oil is xanthoxylin (xanthoxylin/pharmaco), citrene (Limonene), cumic alcohol (Cumicalcohol), dragon geraniol (Geraniol), cumal (Cuminaldehyde), piperitone (Piperitone), phellandrene (phellandrena), sabinene (Sabinene), xanthoxylin (xanthoxyletin, Xanthoxylin), citronellol (Citronellol) and phytosterol (Phytosterol) and unsaturated fatty acid (Chemical Con stituents from the Leaves of Zanthoxylumschinifolium Journal of the Chinese Chemical Society such as (Unsaturated aliphaticacid), 2002,49,125-128.)

One skilled in the art will appreciate that the difference according to the pesticide activity size, the content of pesticide activity component can change in certain scope.For example, for emamectin-benzoate, in aqueous pesticide of the present invention, its content can be low to moderate 0.1%.According to the general needs of using, for general farm chemical ingredients, active component content is generally in the scope of 1-20%.

Correspondingly, because the agricultural chemicals active component content changes within the specific limits in the aqueous pesticide of being prepared of the present invention, the amount of the pepper extract of Cai Yonging also can be different in the present invention.As mentioned above, in the aqueous pesticide of the present invention, change in the weight ratio scope that does not coexist certain of pepper extract according to active component, as long as can realize purpose of the present invention and effect.

Research and experiment through the present inventor shows that pepper extract and pesticide activity component combination can be played the effect that strengthens drug effect and reduce toxicity.Be embodied in:

(1) synergistic effect: pepper extract can promote the absorption of plant to agricultural chemicals, can improve the biologically active of agricultural chemicals and plant growth regulator, can obviously improve the effect of agricultural chemicals;

(2) slow releasing function: pepper extract has the obvious suppression effect to the decomposition rate of agricultural chemicals, and big more its decomposition rate of the consumption of pepper extract is slow more;

(3) toxic action falls: but those activity to the enzyme of toxicity of pesticide sensitivity in the pepper extract passivation biology excite the activity that agricultural chemicals is had the antagonism enzyme, alleviate and reduce the toxicity of agricultural chemicals.

The technology of the present invention advance is with water to be matrix, with the thermodynamic stable system that two phases (particularly O/W type) exist, active ingredient is distributed between the 10-70nm.Show following characteristics: synergistic effect is remarkable, Environmental compatibility good, activity is high, safety is good, production cost is low, market capacity is big.

Adopt aqueous pesticide of the present invention can farthest reduce the use of organic solvent, and synergistic effect is remarkable, thereby reduces the pollution of agricultural chemicals, improve safety in utilization environment; Simultaneously, because the processing characteristics of preparation of the present invention has also improved the medicament storage-stable, and to adhesiveness and the permeability of plant, to insect preventive effect height, the lasting period is long.

Embodiment

Pepper extract is known commercially available prod, can buy from Nanyang Zhang Zhongjing modern Chinese herbal medicine Development Co., Ltd.(trade name: Japan pepper essential oil.Products material: it is raw material that superfine clovershrub Chinese prickly ash is produced in Hancheng, selected Shaanxi.Production technology: zanthoxylum powder essence to the 40--60 order, is produced the molecular clock dehydration with the supercritical CO 2 extraction process.Main component: citrene, citronellol, eugenol, sanshool.Product performance: adopt new and high technology productions such as supercritical CO 2 extraction, whole process is carried out under cryogenic conditions, does not have any organic solvent residual.Properties of product are stable, and anti-seasoning is slightly soluble in ethanol, propane diols, and 25 ℃ are thick shape lotion with interior depositing, and occur with crystallization, are heated to be the yellow green transparency liquid more than 45 ℃.Storage condition: keep in Dark Place 18 months shelf-lifves below 25 ℃.

Trade name: Chinese prickly ash oil.Products material: high-quality clovershrub Chinese prickly ash is produced in the Hancheng, Shanxi.Production technology: this product is to be equipped with senior refining vegetable oil and other natural essence oil with the Japan pepper essential oil that the supercritical CO 2 extraction is produced, and filters to form after fully mixing polishing profit flavor.Main component: Japan pepper essential oil (supercritical extract), refining vegetable oil.Storage condition: keep in Dark Place 12 months shelf-lifves below 25 ℃.)

Among the present invention, described pepper extract can also be pepper water extract, Chinese prickly ash organic solvent (benzinum, n-hexane, absolute ether, ethyl acetate, absolute ethyl alcohol, the methyl alcohol etc.) extract that oneself prepares.

Preparation embodiment 1: the absolute ethyl alcohol extraction method prepares pepper extract

The dried flower green pepper is pulverized, in the Soxhlet extractor of packing into after the metering, extracted 18～30 hours with absolute ethyl alcohol, solvent is colourless in Soxhlet extractor, and extract removes solvent with rotary evaporator, gets pepper extract.

Preparation embodiment 2: the ethyl acetate extraction legal system is equipped with pepper extract

The dried flower green pepper is pulverized, in the Soxhlet extractor of packing into after the metering, use ethyl acetate extraction 18～30 hours, solvent is colourless in Soxhlet extractor, and extract removes solvent with rotary evaporator, gets pepper extract.

Preparation embodiment 3: the aqueous solvent extraction method prepares pepper extract

The dried flower green pepper is pulverized, in the flask of packing into after the metering, be heated to 95 ℃ with a small amount of absolute ethyl alcohol (consumption 5～10%) and water equal solvent and extracted 18～30 hours, solvent is a brown in flask, and centrifugation removes the Chinese prickly ash slag, gets pepper extract.

Example of formulations 1:2.5% gamma cyhalothrin aqueous emulsion

Be dissolved in the water 5 kilograms of pepper extracts (preparation embodiment 1) standby earlier.(folding hundred when former medicine content is not 100%, is 100% by the conversion of its percentage composition with 25 kilograms.) the former medicine of gamma cyhalothrin places 60 kilograms of composite emulsifiers (agricultural newborn 500#, EL-40,700#), and drop into and to be heated to former medicine in reactor or the reaction pot and to melt fully, again the fusion mixture input is contained in the dispersion medium water (supplying surplus) of pepper extract and stir, be mixed to white strongly at homogenizer.Promptly get 1000 kilogram of 2.5% gamma cyhalothrin aqueous emulsion.

The quality of the above-mentioned microemulsion product of preparing meets following technical indicator after tested:

Index name	Index
Index name	Index	Gamma cyhalothrin content (%m/m) (20 ℃)	≥2.5
The pH value	6.0-7.0	Gamma cyhalothrin content (%m/m) (20 ℃)	≥2.5
The pH value	6.0-7.0	Stability of emulsion (diluting 200 times)	Qualified
Low-temperature stability (0 ± 2 ℃)	Qualified	Stability of emulsion (diluting 200 times)	Qualified
Low-temperature stability (0 ± 2 ℃)	Qualified	Heat storage stability (54 ± 2 ℃)	Qualified
Annotate: during ordinary production, low-temperature stability and heat storage stability test were carried out once in per 3 months at least		Heat storage stability (54 ± 2 ℃)	Qualified

Example of formulations 2:20% tolelofos-methyl microemulsion

Be dissolved in the water 20 kilograms of pepper extracts (preparation embodiment 3) standby earlier.200 kilograms of (folding hundred) former medicines of tolelofos-methyl are dissolved in 200 kilograms of toluene and the 5 kilograms of carrene, drop into 200 kilograms of composite emulsifiers (farming breast 500, agricultural newborn 600-2, Nongru-700-2) again, stir.Input contains in the dispersion medium water (supplying surplus) of pepper extract then, is mixed to strongly evenly at homogenizer.Promptly get 1000 kilogram of 20% tolelofos-methyl microemulsion.

Index name	Index
Index name	Index	Tolelofos-methyl content (%m/m) (20 ℃)	≥20
The pH value	4.0-6.0	Tolelofos-methyl content (%m/m) (20 ℃)	≥20
The pH value	4.0-6.0	Stability of emulsion (diluting 200 times)	Qualified
Low-temperature stability (0 ± 2 ℃)	Qualified	Stability of emulsion (diluting 200 times)	Qualified
Low-temperature stability (0 ± 2 ℃)	Qualified	Heat storage stability (54 ± 2 ℃)	Qualified

Transparency temperature scope (0-50 ℃)	Qualified
Transparency temperature scope (0-50 ℃)	Qualified	Annotate: during ordinary production, low-temperature stability and heat storage stability test were carried out once in per 3 months at least

Example of formulations 3:5% fluorine bell urea suspending agent

Earlier 20 kilograms of pepper extracts (Chinese prickly ash oil), 50 kilograms of (folding hundred) former medicines of fluorine bell urea and 15 kilograms of composite emulsifiers (agricultural newborn 500#, Tween-80) are mixed, place dispersion medium water (supplying surplus), milling in ball mill is mixed to evenly.Promptly get 1000 kilogram of 5% fluorine bell urea suspending agent.

The quality of the above-mentioned suspending agent product of preparing meets following technical indicator after tested:

Index name		Index
Index name		Index	Fluorine bell urea content (%m/m) (20 ℃)		≥5
The pH value		6.0-8.0	Fluorine bell urea content (%m/m) (20 ℃)		≥5
The pH value		6.0-8.0	Pourability	Residue % after toppling over≤	3
Residue % after cleaning≤	0.2			Residue % after toppling over≤	3
Residue % after cleaning≤	0.2	Suspensibility % 〉=		95
Screen analysis (by 75 μ m testing sieves) 〉=		Suspensibility % 〉=		95	99.9
Screen analysis (by 75 μ m testing sieves) 〉=		Low-temperature stability (0 ± 2 ℃)		Qualified	99.9
Heat storage stability (54 ± 2 ℃)		Low-temperature stability (0 ± 2 ℃)		Qualified	Qualified
Heat storage stability (54 ± 2 ℃)		Viscosity (0-50 ℃)		Qualified	Qualified
Annotate: during ordinary production, low-temperature stability and heat storage stability test were carried out once in per 3 months at least				Qualified

Example of formulations 4:15% triazophos micro-emulsion

Be dissolved in the water 20 kilograms of pepper extracts (preparation embodiment 2) standby earlier.150 kilograms of (folding hundred) Hostathions are dissolved in 150 kilograms of toluene and the 5 kilograms of carrene, drop into 180 kilograms of composite emulsifiers (farming breast 500, farming breast 1601, Nongru-700-2) again, stir.Drop into then and contain in the dispersion medium water (supplying surplus) of pepper extract, be mixed to strongly evenly at homogenizer.Promptly get 1000 kilogram of 15% triazophos micro-emulsion.

Index name	Index
Index name	Index	Hostathion content (%m/m) (20 ℃)	≥15
The pH value	3.0-6.0	Hostathion content (%m/m) (20 ℃)	≥15
The pH value	3.0-6.0	Stability of emulsion (diluting 200 times)	Qualified
Low-temperature stability (0 ± 2 ℃)	Qualified	Stability of emulsion (diluting 200 times)	Qualified
Low-temperature stability (0 ± 2 ℃)	Qualified	Heat storage stability (54 ± 2 ℃)	Qualified
Transparency temperature scope (0-50 ℃)	Qualified	Heat storage stability (54 ± 2 ℃)	Qualified
Transparency temperature scope (0-50 ℃)	Qualified	Annotate: during ordinary production, low-temperature stability and heat storage stability test were carried out once in per 3 months at least

Example of formulations 5:20% carbosulfan suspending agent

20 kilograms of pepper extracts (Japan pepper essential oil), the former medicine of carbosulfan 200 kilograms of (folding hundred) and 15 kilograms of composite emulsifiers (farming breast 500, agricultural newborn 600-1) mixing, place dispersion medium water (supplying surplus), milling in the colloid mill is mixed to evenly.Promptly get 1000 kilogram of 20% carbosulfan suspending agent.

Index name		Index
Index name		Index	Carbosulfan content (%m/m) (20 ℃)		≥20
The pH value		6.0-8.0	Carbosulfan content (%m/m) (20 ℃)		≥20
The pH value		6.0-8.0	Pourability	Residue % after toppling over≤	3
Residue % after cleaning≤	0.2			Residue % after toppling over≤	3
Residue % after cleaning≤	0.2	Suspensibility % 〉=		95
Screen analysis (by 75 μ m testing sieves) 〉=		Suspensibility % 〉=		95	99.9
Screen analysis (by 75 μ m testing sieves) 〉=		Low-temperature stability (0 ± 2 ℃)		Qualified	99.9
Heat storage stability (54 ± 2 ℃)		Low-temperature stability (0 ± 2 ℃)		Qualified	Qualified
Heat storage stability (54 ± 2 ℃)		Viscosity (0-50 ℃)		Qualified	Qualified
Annotate: during ordinary production, low-temperature stability and heat storage stability test were carried out once in per 3 months at least				Qualified

Example of formulations 6:20% 5a,6,9,9a-hexahydro-6,9-methano-2,4 microemulsion

Be dissolved in the water 20 kilograms of pepper extracts (preparation embodiment 3) standby earlier.200 kilograms of (folding hundred) former medicines of 5a,6,9,9a-hexahydro-6,9-methano-2,4 are dissolved in 300 kilograms of dimethylbenzene and the 10 kilograms of carrene, drop into 260 kilograms of composite emulsifiers (farming breast 500, agricultural newborn 600-1, farming breast 1602) again, stir.Drop into then and contain in the dispersion medium water (supplying surplus) of pepper extract, be mixed to strongly evenly at homogenizer.Promptly get 1000 kilogram of 20% 5a,6,9,9a-hexahydro-6,9-methano-2,4 microemulsion.

Index name	Index
Index name	Index	5a,6,9,9a-hexahydro-6,9-methano-2,4 content (%m/m) (20 ℃)	≥20
The pH value	5.0-7.0	5a,6,9,9a-hexahydro-6,9-methano-2,4 content (%m/m) (20 ℃)	≥20
The pH value	5.0-7.0	Stability of emulsion (diluting 200 times)	Qualified
Low-temperature stability (0 ± 2 ℃)	Qualified	Stability of emulsion (diluting 200 times)	Qualified
Low-temperature stability (0 ± 2 ℃)	Qualified	Heat storage stability (54 ± 2 ℃)	Qualified
Transparency temperature scope (0-50 ℃)	Qualified	Heat storage stability (54 ± 2 ℃)	Qualified
Transparency temperature scope (0-50 ℃)	Qualified	Annotate: during ordinary production, low-temperature stability and heat storage stability test were carried out once in per 3 months at least

Example of formulations 7:5% azoles mite ester microemulsion

Be dissolved in the water 20 kilograms of pepper extracts (preparation embodiment 3) standby earlier.50 kilograms of (folding hundred) former medicines of azoles mite ester are dissolved in 150 kilograms of toluene, drop into 180 kilograms of composite emulsifiers (farming breast 500, Nongru-700-1, farming breast 1602) again, stir.Drop into then and contain in the dispersion medium water (supplying surplus) of pepper extract, be mixed to strongly evenly at homogenizer.Promptly get 1000 kilogram of 5% azoles mite ester microemulsion.

Index name	Index
Index name	Index	Azoles mite ester content (%m/m) (20 ℃)	≥5
The pH value	5.0-7.0	Azoles mite ester content (%m/m) (20 ℃)	≥5
The pH value	5.0-7.0	Stability of emulsion (diluting 200 times)	Qualified
Low-temperature stability (0 ± 2 ℃)	Qualified	Stability of emulsion (diluting 200 times)	Qualified
Low-temperature stability (0 ± 2 ℃)	Qualified	Heat storage stability (54 ± 2 ℃)	Qualified

Example of formulations 8:0.5% emamectin benzoate microemulsion

Be dissolved in the water 30 kilograms of pepper extracts (preparation embodiment 3) standby earlier.5 kilograms of (folding hundred) former medicines of emamectin-benzoate are dissolved in 40 kilograms of n-amyl alcohols, drop into 140 kilograms of composite emulsifiers (farming breast 500, farming breast 11, farming breast 1602) again, stir.Drop into then and contain in the dispersion medium water (supplying surplus) of pepper extract, be mixed to strongly evenly at homogenizer.Promptly get 1000 kilogram of 0.5% emamectin benzoate microemulsion.

Index name	Index
Index name	Index	Emamectin-benzoate content (%m/m) (20 ℃)	≥0.5
The pH value	5.0-7.0	Emamectin-benzoate content (%m/m) (20 ℃)	≥0.5
The pH value	5.0-7.0	Stability of emulsion (diluting 200 times)	Qualified
Low-temperature stability (0 ± 2 ℃)	Qualified	Stability of emulsion (diluting 200 times)	Qualified
Low-temperature stability (0 ± 2 ℃)	Qualified	Heat storage stability (54 ± 2 ℃)	Qualified
Transparency temperature scope (0-50 ℃)	Qualified	Heat storage stability (54 ± 2 ℃)	Qualified
Transparency temperature scope (0-50 ℃)	Qualified	Annotate: during ordinary production, low-temperature stability and heat storage stability test were carried out once in per 3 months at least

Example of formulations 9:20% triazolone suspending agent

Be dissolved in the water 20 kilograms of pepper extracts (preparation embodiment 1) standby earlier.200 kilograms of (folding hundred) former medicines of triazolone and 15 kilograms of composite emulsifiers (farming breast 500, farming breast 12) are mixed, place the dispersion medium water (supplying surplus) that contains pepper extract, milling in the ball mill is mixed to evenly.Promptly get 1000 kilogram of 20% triazolone suspending agent.

Index name

Index

Triazolone (%m/m) (20 ℃)		≥20
Triazolone (%m/m) (20 ℃)		≥20	The pH value		6.0-8.0
Pourability	Residue % after toppling over≤	3	The pH value		6.0-8.0
	Residue % after toppling over≤	3	Residue % after cleaning≤	0.2
	Suspensibility % 〉=		Residue % after cleaning≤	0.2	95
Screen analysis (by 75 μ m testing sieves) 〉=			99.9		95
Screen analysis (by 75 μ m testing sieves) 〉=		Low-temperature stability (0 ± 2 ℃)		Qualified
Heat storage stability (54 ± 2 ℃)		Low-temperature stability (0 ± 2 ℃)		Qualified	Qualified
Heat storage stability (54 ± 2 ℃)		Viscosity (0-50 ℃)		Qualified	Qualified
Annotate: during ordinary production, low-temperature stability and heat storage stability test were carried out once in per 3 months at least				Qualified

Example of formulations 10:2.5% decis microemulsion

Be dissolved in the water 20 kilograms of pepper extracts (preparation embodiment 3) standby earlier.25 kilograms of (folding hundred) deltamethrin original medicines are dissolved in 100 kilograms of toluene, drop into 160 kilograms of composite emulsifiers (farming breast 500, farming breast 12, peaceful breast 110) again, stir.Input contains in the dispersion medium water (supplying surplus) of pepper extract then, is mixed to strongly evenly at homogenizer.Promptly get 1000 kilogram of 2.5% decis microemulsion.

Index name	Index
Index name	Index	Decis content (%m/m) (20 ℃)	≥2.5
The pH value	5.0-7.0	Decis content (%m/m) (20 ℃)	≥2.5
The pH value	5.0-7.0	Stability of emulsion (diluting 200 times)	Qualified
Low-temperature stability (0 ± 2 ℃)	Qualified	Stability of emulsion (diluting 200 times)	Qualified
Low-temperature stability (0 ± 2 ℃)	Qualified	Heat storage stability (54 ± 2 ℃)	Qualified
Transparency temperature scope (0-50 ℃)	Qualified	Heat storage stability (54 ± 2 ℃)	Qualified
Transparency temperature scope (0-50 ℃)	Qualified	Annotate: during ordinary production, low-temperature stability and heat storage stability test were carried out once in per 3 months at least

Example of formulations 11:5% Imidacloprid micro-capsule suspension

Be dissolved in the water 20 kilograms of pepper extracts (preparation embodiment 2) standby earlier.50 kilograms of (folding hundred) Imidacloprids and 30 kilograms of composite emulsifiers (farming breast 500, NP-10) and 50 kilograms of cosolvents (ethylene glycol) are placed the dispersion medium water (supplying surplus) that contains pepper extract, in colloid mill, mill and be mixed to evenly, the macromolecular material that adds at last 50 kilograms again stirs as cyst wall or cyst membrane.Promptly get 1000 kilogram of 5% Imidacloprid microcapsule suspending agent.

The quality of the above-mentioned microcapsule suspending agent product of preparing meets following technical indicator after tested:

Index name		Index
Index name		Index	Imidacloprid (%m/m) (20 ℃)		≥5
The pH value		6.0-8.0	Imidacloprid (%m/m) (20 ℃)		≥5
The pH value		6.0-8.0	Pourability	Residue % after toppling over≤	3
Residue % after cleaning≤	0.2			Residue % after toppling over≤	3
Residue % after cleaning≤	0.2	Suspensibility % 〉=		95
Screen analysis (by 75 μ m testing sieves) 〉=		Suspensibility % 〉=		95	99.9
Screen analysis (by 75 μ m testing sieves) 〉=		Low-temperature stability (0 ± 2 ℃)		Qualified	99.9
Heat storage stability (54 ± 2 ℃)		Low-temperature stability (0 ± 2 ℃)		Qualified	Qualified
Heat storage stability (54 ± 2 ℃)		Viscosity (0-50 ℃)		Qualified	Qualified
Annotate: during ordinary production, low-temperature stability and heat storage stability test were carried out once in per 3 months at least				Qualified

Example of formulations 12:0.3% aqueous matrine solution

Be dissolved in the water 20 kilograms of pepper extracts (preparation embodiment 1) standby earlier.3 kilograms of (folding hundred) matrine total alkalis and 60 kilograms of composite emulsifiers (farming breast 500, NP-10, Tween-60) and 10 kilograms of cosolvent ethylene glycol are mixed, input contains in the dispersion medium water (supplying surplus) of pepper extract then, is mixed to strongly evenly at homogenizer.Promptly get 1000 kilogram of 0.3% aqueous matrine solution.

The quality of the above-mentioned aqua product of preparing meets following technical indicator after tested:

Index name	Index
Index name	Index	Matrine content (%m/m) (20 ℃)	≥0.3

The pH value	5.0-7.0
The pH value	5.0-7.0	Dilution stability	Qualified
Low-temperature stability (0 ± 2 ℃)	Qualified	Dilution stability	Qualified
Low-temperature stability (0 ± 2 ℃)	Qualified	Heat storage stability (54 ± 2 ℃)	Qualified
Water insoluble matter content (%m/m) (20 ℃)	≤0.05	Heat storage stability (54 ± 2 ℃)	Qualified
Water insoluble matter content (%m/m) (20 ℃)	≤0.05	Annotate: during ordinary production, low-temperature stability and heat storage stability test were carried out once in per 3 months at least

The high chlorine suspension emulsion of the rich propylene of example of formulations 13:0.25%

Be dissolved in the water 100 kilograms pepper extracts (Chinese prickly ash oil) and 50 kilograms of stabilizing agents (butyl glycidyl ether) standby.1.5 kilograms of former medicines of beta-cypermethrin (folding hundred) and 1 kilogram of former medicine of rich d-trans Allethrin 93 (folding hundred) are placed reactor or reaction pot, xylene soluble with 4 kilograms, and then add 20 kilograms of composite emulsifiers (farming breast 500, NP-10, Tween-60) and stir, add under the high shear condition of stirring then and contain in the dispersion medium water (supplying surplus) of pepper extract and stabilizing agent, pH to 5～7 are transferred with watery hydrochloric acid in the back that is uniformly dispersed.Promptly get 1000 kilograms the high chlorine suspension emulsion of 0.25% rich propylene.

Example of formulations 14:10% first cyanogen four mite suspension emulsions

Be dissolved in the water 5 kilograms pepper extracts (Japan pepper essential oil) and 100 kilograms of stabilizing agents (sorbierite) standby.60 kilograms of former medicines of fenpropathrin (folding hundred) and 40 kilogram of four former medicine of mite piperazine (folding hundred) are placed reactor or reaction pot, xylene soluble with 100 kilograms, and then add 40 kilograms of composite emulsifiers (farming breast 500, NP-10) and stir, add under the high shear condition of stirring then and contain in the dispersion medium water (supplying surplus) of pepper extract and stabilizing agent, pH to 5～7 are transferred with watery hydrochloric acid in the back that is uniformly dispersed.Promptly get 1000 kilograms 10% first cyanogen, four mite suspension emulsions.

Toxicity test example 1: gamma cyhalothrin aqueous emulsion animal toxicity test

1), acute oral toxicity test

With the Wistar rat is experimental animal, presses HornShi method (State Standard of the People's Republic of China GB 15193.3), has designed 1000,464,215 and 4 dosage of 100mg/kg, and female tom carries out respectively.The contamination back continues to observe 14 days, record animal poisoning symptom and death time.

Try to achieve this medicine to male and female rat oral LD according to dead result ₅₀As follows respectively:

Male rat: 387mg/kg (320-451mg/kg)

Female rats: 405mg/kg

This medicament toxicity is for poisoning, and its former medicine toxicity is high poison.

2), acute dermal toxicity test

With the Wistar rat is experimental animal, presses the HornShi method, has designed 2150,1000,464 and 215mg/Kg4 dosage, and female tom carries out respectively.The contamination back continues to observe 14 days, record animal poisoning symptom and death time.

According to dead result try to achieve this medicine to the male and female rat through skin LD ₅₀As follows respectively:

Male rat:＞2150mg/kg

Female rats:＞2150mg/kg

This medicament toxicity is low toxicity, and its former medicine toxicity is for poisoning.

3), acute percutaneous stimulation test

With the large ear rabbit is experimental animal, and according to the method for State Standard of the People's Republic of China GB15670 " agriculture chemical registration toxicology test method " regulation, animal self skin was observed 14 days behind the coating in contrast continuously.

According to acute toxicity evaluation criterion among the State Standard of the People's Republic of China GB15670 " agriculture chemical registration toxicology test method " and result of the test, this medicine is " nonirritant " to skin irritatin intensity.

4), the floating agent eye irritant test of 2.5% gamma cyhalothrin water

With the large ear rabbit is experimental animal, and according to the method for State Standard of the People's Republic of China GB15670 " agriculture chemical registration toxicology test method " regulation, animal self was observed 14 days behind the coating to branch hole in contrast continuously.

Stimulate evaluation criterion and result of the test according to eye among the State Standard of the People's Republic of China GB15670 " agriculture chemical registration toxicology test method ", it is " slight excitant " that this medicine stimulates stimulus intensity to eye.

Toxicity test example 2: decis microemulsion animal toxicity test

In this test example the 2.5% decis microemulsions that are used for preparation enforcement 10 preparations are tested, the result is as follows:

1), acute oral toxicity test

With the Wistar rat is experimental animal, presses the HornShi method, has designed 1000,464,215 and 100mg/kg4 dosage, and female tom carries out respectively.The contamination back continues to observe 14 days, record animal poisoning symptom and death time.

Male rat: 475mg/kg

Female rats: 492mg/kg

2), acute dermal toxicity test

Male rat:＞2150mg/kg

Female rats:＞2150mg/kg

3), acute percutaneous stimulation test

4), eye irritant test

Toxicity test example 3:5% Imidacloprid microcapsule suspending agent animal toxicity test

In this test example the 5% Imidacloprid microcapsule suspending agents that are used for preparation enforcement 11 preparations are tested, the result is as follows:

1), acute oral toxicity test

Male rat: 871mg/kg

Female rats: 892mg/kg

2), acute dermal toxicity test

With the Wistar rat is experimental animal, presses the HornShi method, has designed 4640,2150,1000 and 464mg/Kg4 dosage, and female tom carries out respectively.The contamination back continues to observe 14 days, record animal poisoning symptom and death time.

Male rat:＞4640mg/kg

Female rats:＞4640mg/kg

This medicament toxicity is low toxicity, and its former medicine toxicity is low toxicity.

3), acute percutaneous stimulation test

4), eye irritant test

Stimulate evaluation criterion and result of the test according to eye among the State Standard of the People's Republic of China GB15670 " agriculture chemical registration toxicology test method ", it is " nonirritant " that this medicine stimulates stimulus intensity to eye.

Biological Examples 1:2.5% gamma cyhalothrin aqueous emulsion is to the Toxicity Determination test of cotton bollworm

Present embodiment is the Toxicity Determination test of carrying out at cotton bollworm.

Reagent agent:

The medicament 1:2.5% time ^Aqueous emulsion (gamma cyhalothrin commercially available prod, Syngenta Co.,Ltd produces);

Medicament 2:2.5% gamma cyhalothrin aqueous emulsion (example of formulations 1 of the present invention);

Medicament 3: Pericarpium Zanthoxyli extract (the present invention prepares embodiment 1)

Test is a cotton bollworm with worm, 3 instar larvaes, and sensitive strain (compares with sensitive population, to the time ^The about 5-10 of resistant multiple doubly), test by plant protection research institute of the Chinese Academy of Agricultural Sciences.

Adopt dip method, measure the virulence of tagging of above-mentioned medicament.Drug concentration gradient employing 50,25,12.5,6.25,3.125,1.56ppm handle, and every processing repeats for 6 times, 48 of every duplication examination worms.Soak 5 seconds of worm, take out and be poured on the blotting paper, inhale and remove unnecessary soup, will try worm and put into 24 hole test boxs respectively, put into the constant incubator cultivation and investigated the insect population lethality in 24,48 hours and see the following form 1.

Table 1 gamma cyhalothrin preparation is to the Toxicity Determination result of cotton bollworm

Reagent agent	Review time	Toxicity regression formula (Y=)	LD ₅₀(95% confidence limit) (μ g/ml)	LC ₉₀Value (μ g/ml)	The synergy multiple
Reagent agent	Review time	Toxicity regression formula (Y=)	LD ₅₀(95% confidence limit) (μ g/ml)	LC ₉₀Value (μ g/ml)	The synergy multiple	Medicament 3	24 hours	——	0	0	0
Medicament 2	4.1040+2.0153x	2.78(1.87-4.36)	12.06	2.79		Medicament 3		——	0	0	0
Medicament 2	4.1040+2.0153x	2.78(1.87-4.36)	12.06	2.79	Medicament 1	2.9708+2.2803x		7.76(5.99-10.06)	28.35	1.0
Medicament 3	48 hours	——	0	0	Medicament 1	2.9708+2.2803x		7.76(5.99-10.06)	28.35	1.0	0
Medicament 3		——	0	0	Medicament 2	4.1273+2.0689x	2.64(1.68-4.15)	22.02	2.82		0
Medicament 1		3.9439+2.3593x	7.44(5.77-9.59)	26.03	Medicament 2	4.1273+2.0689x	2.64(1.68-4.15)	22.02	2.82	1.0

Annotate: the LC of synergy multiple=contrast medicament ₅₀The LC of value/synergy medicament ₅₀Value

The floating agent of biological Examples 2:2.5% gamma cyhalothrin water is to the cotton bollworm control field control effectiveness test

Present embodiment is the field control effectiveness test that carries out at cotton bollworm.

Experimental condition: experimental field be test cotton field, Hebei, the test kind is conventional cotton 492, sowing by the end of April, and rich water quality management unanimity in the experimental plot, the growing way unanimity, the worm amount takes place medium.Worm age is mostly in 3-4 age, whole test phase medication secondary.

Reagent agent:

Medicament 1,2.5% time ^Aqueous emulsion (gamma cyhalothrin commercially available prod, Syngenta Co.,Ltd produces);

Medicament 2,2.5% gamma cyhalothrin aqueous emulsion (example of formulations 1 of the present invention);

Spray method: above-mentioned five processing, each repeats twice, 15 square metres of each sub-district areas, the experimental plot is district's group arrangement at random in the field.With the conventional spraying of KIM-9MATABI knapsack hand sprayer.

Investigation method: take five point samplings in each sub-district before the spray medicine, all borer populations of living on the fixed point investigation 5-10 strain cotton, as the insect population radix, 1,7 day remaining borer population alive of investigation behind the medicine.

Result of the test shows that the control efficiency of 2 pairs of cotton bollworms of medicament obviously improves than medicament 1, significance test, and control efficiency increases significantly.The result sees following table 2 for details.

The field control effectiveness test result of table 2 gamma cyhalothrin preparation control cotton bollworm

Reagent agent and concentration	Repeat	Worm lives before the medicine	Behind the medicine 1 day			Behind the medicine 7 days
			Behind the medicine 1 day			Behind the medicine 7 days			Borer population alive	Rate goes down	Correcting controling effect	Borer population alive	Rate goes down	Correcting controling effect
			Medicament 2 1000X	1	50	1	98	98a	Borer population alive	Rate goes down	Correcting controling effect	Borer population alive	Rate goes down	Correcting controling effect	0	100	99a
2	50	1		1	50	1	98		98	1	98				0	100
2	50	1		Medicament 1 1000X	1	50	3		98	1	98	94	95a	3	94	94.9b
2	51	2	96		1	50	3	2	96.1			94		3	94
2	51	2	96		Medicament 2 1500X	1	50	2	96.1	3	94	96a		2	96		97b
2	51	1	98	1		1	50	98		3	94			2	96
2	51	1	98	1		Medicament 1 1500X	1	98	50	7	86.3		88.2c	6	88.2	88.9c
2	51	5	90	5	90		1		50	7	86.3			6	88.2
2	51	5	90	5	90		Medicament 2 2000X	1	51	3	94.1	94.1a		3	94.1		94.1b
2	54	3	94.1	3	94.1			1	51	3	94.1			3	94.1
2	54	3	94.1	3	94.1	Medicament 1 2000X		1	50	10	80		81a	9	82	81.7d
2	50	9	82	9	82			1	50	10	80			9	82
2	50	9	82	9	82		The CK blank	1	30	30	0			30	0
2	31	31	0	30	3.2			1	30	30	0			30	0

Test period :-11 days on the 4th July in 2003, numeral back, table back English alphabet difference, the expression significant difference (p=0.05, HSD), significant difference between a, b, c, the d, alphabetical identical no significant difference.

Poisoning does not take place in for examination concentration.Field trial shows, microemulsion of the present invention is compared with similar medicament the cotton bollworm control effect in the field has significant difference.

Biological Examples 3:20% tolelofos-methyl microemulsion is to the Toxicity Determination test of sclerotinia rot of colza

Present embodiment is the Toxicity Determination test at Sclerotinia sclerotiorum (Sclerotiniascleroiorum).

Test medicine:

Medicament 1:20% highly skilled man missible oil (tolelofos-methyl commercially available prod, the highly dense Kang Fengnongization in Shandong Co., Ltd)

Medicament 2:20% tolelofos-methyl microemulsion

Medicament 3:20% tolelofos-methyl microemulsion (example of formulations 2 of the present invention)

Medicament 4: Pericarpium Zanthoxyli extract (the present invention prepares embodiment 3)

Annotate: the composition of medicament 2 and medicament 3 and prepare similarly, the difference of the two is that the former does not contain pepper extract.

Subjects:

Sclerotinia sclerotiorum (Sclerotiniascleroiorum).

Test method:

Contain the activity that toxic medium method is measured above-mentioned medicament 1, medicament 2 and medicament 3 and 4 pairs of Sclerotinia sclerotiorums of medicament in indoor employing.The 45mlPSA medium of in the 100ml triangular flask, packing into, being cooled to (45～50) after the sterilization ℃ presses predetermined close and adds different reagent agent 5ml, on average pouring 3 diameters after shaking up into is in the culture dish of 9cm, makes the flat board that contains the variable concentrations medicament, is contrast with the sterile water.From cultivating 7 days germ colony edge, cut-off is the lawn of 5mm directly, and bacterium faces down, and inserts in the plate, and each medicament is established 5 concentration, 3 repetitions.24 ℃ of following constant temperature culture 4 days are measured colony diameter with the cross method of scoring.Calculate the EC of medicament ₅₀Value is obtained virulence regression equation, and estimates the bacteriostatic activity Toxicity Determination result of medicament, sees Table 3.Result of the test shows that under indoor isolated condition, pepper extract does not have bacteriostasis to Sclerotinia sclerotiorum, and medicament 3 effects are better.

Table 3 tolelofos-methyl preparation is to the toxicity test result of Sclerotinia sclerotiorum

Reagent agent

Toxicity regression formula (Y=)

Correlation coefficient r

EC ₅₀Value (mg/L)

EC ₉₀Value (mg/L)

Medicament 1	Y＝3.7439+2.1126X	0.9646	3.647	25.92
Medicament 1	Y＝3.7439+2.1126X	0.9646	3.647	25.92	Medicament 2	Y＝4.0749+1.6112X	0.9934	3.281	20.46
Medicament 3	Y＝5.4198+1.6107X	0.9967	0.3988	5.644	Medicament 2	Y＝4.0749+1.6112X	0.9934	3.281	20.46
Medicament 3	Y＝5.4198+1.6107X	0.9967	0.3988	5.644	Medicament 4	——	——	——	——

Can draw Pericarpium Zanthoxyli extract from above result and not have bactericidal action.

Biological Examples 4:20% tolelofos-methyl microemulsion is to the field control effectiveness test of sclerotinia rot of colza

Present embodiment is the field control effectiveness test that carries out at sclerotinia rot of colza.

Test medicine:

Medicament 2:20% tolelofos-methyl microemulsion

Controlling object:

Cotton in seedling stage damping off (RhizoctoniasolaniK.)

Anthracnose (ColletotrichumgossypiiS.).

Test method:

Test is experimental field carried out in the Chinese Academy of Agricultural Sciences Institute of Plant Protection, and kind is a middle cotton institute 35, sowing on April 21, and seeding quantity is lint photon 28kg/hm ^-2, evenly (medium laying particular stress on), field management unanimity take place in the field seedling diseases.Blank, totally 4 processing repeat 4 times, and district's group is arranged at random, sub-district area 25m ²

The field trial investigation:

After planting manually ditch between every cell row immediately, 100 seeds of uniform broadcasting were investigated the number of once emerging, and were calculated emergence rate in per 3 days.The 50% beginning sub-district fixed point of emerging is investigated, and once total strain number of investigation in 3 days and dead seedling number calculate seedling protecting effect; After the last time investigation, each sub-district choose at random cotton seedling investigation disease index of 100 strains and various seedling diseases proportion calculate protection effect.In the indoor germination test of doing.With diameter 180mm culture dish, the sterilization treatment river sand that interior dress 0.5cm is thick (water content 20%), every ware is broadcast 100 seeds, places constant incubator (25 ± 1) ℃ cultivation down, and the investigation germinative number calculates germination rate.Indoor bacteria inhibition assay: from the mycelium tip picking diameter of new cultivation is 0.5cm bacterium piece, be connected on the PDA medium of different soups (above-mentioned medicament 1-3 respectively dilutes 10000 times), place the grown cultures case under (18 ± 1) ℃ (inhibition rhizoctonia solani) or (25 ± 1) ℃ (inhibition anthrax) condition, to cultivate, every processing repeats 4 times, measure colony diameter, calculate bacteriostasis rate.And to above-mentioned data carry out the DuncanShi multiple range test and handle between multiple ratio, to estimate the difference of each chemicals treatment in this test, the results are shown in Table 4.

Tolelofos-methyl suppresses the pathogen effect assessment: medicament 3 suppresses upright withered remarkable with the anthrax bacteria effect, bacteriostasis rate to rhizoctonia solani was 100% on the 5th day, fungistatic effect is better than medicament 1 (missible oil) and medicament 2 significantly, the effect that medicament 2 suppresses rhizoctonia solani is also more obvious, and the 5th day bacteriostasis rate reaches more than 82%.To the inhibitory action of anthrax bacteria, medicament 3 fungistatic effects are best, and the 5th day bacteriostasis rate is 100%, are medicament 2 secondly, and the fungistatic effect of medicament 1 is relatively poor, and bacteriostasis rate all is lower than 70%.

The diseases prevention of table 4 tolelofos-methyl preparation seed treatment is protected and is produced effect

Reagent agent	Extension rate	Suppress rhizoctonia solani				Suppress anthrax bacteria
		Suppress rhizoctonia solani				Suppress anthrax bacteria				The 3rd day		The 5th day		The 3rd day		The 5th day
		Bacteriostasis rate (%)	p＝0.05 ^a	Bacteriostasis rate (%)	p＝0.05	Bacteriostasis rate (%)	p＝0.05	Bacteriostasis rate (%)	p＝0.05	The 3rd day		The 5th day		The 3rd day		The 5th day
		Bacteriostasis rate (%)	p＝0.05 ^a	Bacteriostasis rate (%)	p＝0.05	Bacteriostasis rate (%)	p＝0.05	Bacteriostasis rate (%)	p＝0.05	Medicament 1	10000	67.1	B	54.5	C	76.4	B	69.4	B
Medicament 2	10000	87.2	B	82.6	B	90.7	B	84.6	B	Medicament 1	10000	67.1	B	54.5	C	76.4	B	69.4	B

Medicament 3

10000

100

A

100

A

100

A

100

A

A:p=0.05 represents 5% significant difference.

Biological Examples 5:5% fluorine bell urea suspending agent is to the Toxicity Determination of cotton bollworm

Present embodiment is the Toxicity Determination test at cotton bollworm.

Test medicine:

Medicament 1:5% volt worm missible oil (fluorine bell urea commercially available prod, Rui Ze insecticide factory in Dalian produces)

Medicament 2:5% fluorine bell urea suspending agent

Medicament 3:5% fluorine bell urea suspending agent (example of formulations 3 of the present invention)

Controlling object:

Cotton bollworm (HelicoverpaarmigeraH ü bner) 4 instar larvaes.

Test method:

Adopt dip method, measure the virulence of tagging of above-mentioned medicament.The drug concentration gradient is handled, and every processing repeats for 6 times, 48 of every duplication examination worms.Soak 5 seconds of worm, take out and be poured on the blotting paper, inhale and remove unnecessary soup, will try worm and put into 24 hole test boxs respectively, put into the constant incubator cultivation and investigated the insect population lethality in 24 hours, see the following form 5.

Table 5 fluorine bell urea preparation is to the Toxicity Determination result of cotton bollworm

Formulation	Toxicity regression formula (Y=)	LD ₅₀(95% confidence limit) (μ g/ml)	LC ₉₀Value (μ g/ml)	The synergy multiple
Formulation	Toxicity regression formula (Y=)	LD ₅₀(95% confidence limit) (μ g/ml)	LC ₉₀Value (μ g/ml)	The synergy multiple	Medicament 1	4.9439+1.6593x	1.0086(1.99-0.16)	10.35	1.0
Medicament 2	2.9708+2.2803x	0.9844(1.77-0.19)	9.03	1.0	Medicament 1	4.9439+1.6593x	1.0086(1.99-0.16)	10.35	1.0
Medicament 2	2.9708+2.2803x	0.9844(1.77-0.19)	9.03	1.0	Medicament 3	4.1273+2.0689x	0.2564(0.68-0.15)	6.027	3.93

The field control effectiveness test of biological Examples 6:5% fluorine bell urea control resistant bollworm

Present embodiment is the Toxicity Determination test at resistant bollworm.

Test medicine:

Medicament 1:5% volt worm missible oil (commercially available prod, Rui Ze insecticide factory in Dalian produces)

Medicament 2:5% fluorine bell urea suspending agent

Controlling object:

Cotton bollworm (HelicoverpaarmigeraH ü bner).

Test method:

Sub-district area 55m ², randomized arrangement repeats 4 times.For the examination cotton variety is conventional cotton 492, planting density 4.4 ten thousand strain/mus, and on the occasion of the second-generation cotton bollworm ovum hatching Sheng phase, water consumption is mu 50L during the dispenser.

Lasting effect to cotton bollworm the results are shown in Table 6.

The field control effectiveness test result of table 6 fluorine bell urea preparation control cotton bollworm

Medicament	Extension rate	Before the dispenser		After the dispenser the 1st day		After the dispenser the 3rd day		After the dispenser the 7th day
		Before the dispenser		After the dispenser the 1st day		After the dispenser the 3rd day		After the dispenser the 7th day		The ovum number	Borer population	Residual worm	Preventive effect	Residual worm	Preventive effect	Residual worm	Preventive effect
		Medicament 1	1000	159	77	38	29	53	63	The ovum number	Borer population	Residual worm	Preventive effect	Residual worm	Preventive effect	Residual worm	Preventive effect	43	60
Medicament 2	1000	Medicament 1	1000	159	77	38	29	53	63	149	44	37	8	35	69	19	78	43	60
Medicament 2	1000	Medicament 3	1000	195	53	34	28	32	79	149	44	37	8	35	69	19	78	9	91
Blank		Medicament 3	1000	195	53	34	28	32	79	144	89	81	-	150	-	91	-	9	91

By table 6 as seen, after the dispenser the 1st day, the preventive effect of 3 processing of fluorine bell urea was all not obvious.After the dispenser the 3rd day, the preventive effect of 3 processing of fluorine bell urea rose to 63%-79%, but the residual worm amount of hundred strains of 3 processing of fluorine bell urea still is higher than index for control.The 7th day control efficiency after the dispenser (removing medicament 1) rises gradually.The preventive effect of 1000 times of processing of medicament 3 is 91%, is significantly higher than 1000 times of processing (60% and 78%) of medicament 1 and medicament 2.Result of the test shows that the control efficiency of 3 pairs of cotton bollworms of medicament obviously improves than medicament 1 (missible oil) and medicament 2, significance test, and control efficiency increases significantly.

Biological Examples 7:15% Hostathion is to the Toxicity Determination of rice-stem borer

Present embodiment is the Toxicity Determination test at rice-stem borer.

Test medicine:

Medicament 1:20% opens order missible oil (Hostathion commercially available prod, Hubei Province's sand swell reach limited company and produce)

Medicament 2:15% triazophos micro-emulsion

Medicament 3:15% triazophos micro-emulsion (example of formulations 4 of the present invention)

Controlling object:

The examination of rice-stem borer (Chilosuppressalis) 2 instar larvaes is raised for the indoors artificial feed by worm.

Test method:

Adopt infusion process.Rice-stem borer 2 instar larvaes of indoor feeding are immersed in the soup of the variable concentrations for preparing with above-mentioned reagent agent, to try worm after about 3 seconds takes out, be placed on the blotting paper polypide is dried, put into culture dish then and raise, through 24 hours checkout facility results with artificial feed.Environmental temperature is controlled at 26 ± 1 ℃ during mensuration, and each reagent agent is established 5 of various concentrations over control treatment on the preliminary experiment basis, and every processing repeats 4 times, 25 of every repetition worm examinations.According to 24 hours result of the tests, utilize sun, the co-toxicity coefficient of y-p and JohnsonER (1996) method calculation combination agent, the synergy situation of the size examination combination agent of usefulness co-toxicity coefficient.

Result of the test:, try to achieve the virulence regression equation formula of each reagent agent according to 24 hours result of the tests of each concentration of treatment of each reagent agent.

Table 7 Hostathion preparation is to the Toxicity Determination result of rice-stem borer

Reagent agent

Toxicity regression formula (Y=)

Correlation coefficient r

LC ₅₀Value (mg/L)

LC ₉₀Value (mg/L)

Medicament 1	Y＝3.7439+2.1126X	0.9646	3.647	25.92
Medicament 1	Y＝3.7439+2.1126X	0.9646	3.647	25.92	Medicament 2	Y＝4.0749+1.6112X	0.9934	3.611	25.46
Medicament 3	Y＝5.4198+1.6107X	0.9967	1.078	19.64	Medicament 2	Y＝4.0749+1.6112X	0.9934	3.611	25.46

Biological Examples 8:15% triazophos micro-emulsion is to the field control effectiveness test of rice-stem borer

Present embodiment is the field control effectiveness test at the resistant rice striped rice borer.

Reagent agent:

Medicament 2:15% triazophos micro-emulsion

Controlling object:

In the 1st generation of rice-stem borer (Chilosuppressalis), be gold early 47 for studying thing.

Test method:

Test is established 2 and is handled, promptly medicament 3 every mu use 100ml, 125ml and handle; Compare chemicals treatment with medicament 1 and 2 each 100ml; Other establishes spray clear water blank.Experimental plot area 30m ², repeating 4 times, district's group is arranged at random.Each is handled all in dispenser in the morning on May 19, and application method adopts the spraying of workers and peasants' 16 type manual sprayers, and every mu of water yield is all calculated by 50kg.Field 1 generation striped rice borer is 2 instar larvae peak periods during dispenser, and dispenser same day is overcast to cloudy, and mean temperature of air is 20.7 ℃, the 5th it rains behind the medicine.

Investigation method:

Behind the medicine the 4th day, withered sheath strain 10 strains of all choosing at random of each sub-district, borer population is anyway looked in stripping, calculates lethality; 200 clumps of parallel samplings are adopted in (June 9) the every sub-district, typing back of causing harm, and investigate withered heart strain number, calculate withered heart rate and seedling protecting effect at last, and behind medicine visual observations rice drug misadventuring situation repeatedly.

Control efficiency:

Show that in paddy rice the 1st generation striped rice borer typing " Invest, Then Investigate " result that causes harm 2 processing of medicament 3 have extremely significant seedling protecting effect, effect is 96.6%-98.3%, and there were significant differences with medicament 1 and medicament 2.2 processing of medicament 3 have extremely significant insecticidal effect to paddy rice the 1st generation striped rice borer.The insect population lethality reaches 94.6%-98.3% behind the 3d, and medicament--medicament 1 and medicament 2 have significant difference with contrast.

Table 8 Hostathion preparation is to the field control effectiveness test result of rice-stem borer

Reagent agent and consumption	Seedling protecting effect		Insecticidal effect
	Seedling protecting effect		Insecticidal effect			Average withered heart rate	Average seedling protecting effect	Average desinsection number	Average total borer population	Control efficiency
	Medicament 3 (125ml)	0.04aA	96.6％	28.0	28.8	Average withered heart rate	Average seedling protecting effect	Average desinsection number	Average total borer population	Control efficiency	97.4％
Medicament 3 (100ml)	Medicament 3 (125ml)	0.04aA	96.6％	28.0	28.8	0.03aA	98.3％	29.3	29.8	98.3％	97.4％
Medicament 3 (100ml)	Medicament 2 (100ml)	0.12bC	89.3％	26.0	29.0	0.03aA	98.3％	29.3	29.8	98.3％	89.6％
Medicament 1 (100ml)	Medicament 2 (100ml)	0.12bC	89.3％	26.0	29.0	0.08bB	92.8％	30.3	33.2	91.3％	89.6％
Medicament 1 (100ml)	Blank	3.58cC	-	0	27.0	0.08bB	92.8％	30.3	33.2	91.3％	-

Repeatedly the visual observations result shows behind medicine, and each handles paddy rice does not all have the poisoning generation.Illustrate under this experimental condition that the medicament of participating in the experiment is safe to paddy rice.

Biological Examples 9:20% carbosulfan suspending agent is to the Toxicity Determination test of cotten aphid

Present embodiment is the Toxicity Determination test at cotten aphid.

Test medicine:

Good year winter missible oil (carbosulfan commercially available prod, Fu Meishi company produces) of medicament 1:20%

Medicament 2:20% carbosulfan suspending agent

Medicament 3:20% carbosulfan suspending agent (example of formulations 5 of the present invention)

Controlling object:

Cotten aphid (AphisgossypiiGlover).

The blade medicine embrane method is adopted in this test, the fresh cabbage blade of not used agricultural chemicals (oneself cultivation) was dipped in respectively in above-mentioned each reagent agent solution of series concentration 10 seconds, taking-up is dried in the shade and is placed in the 9cm plastic culture dish, and every ware inserts 25 of aphids, and each concentration is established three repetitions.Handle 24 hours result of the test respectively according to each reagent agent, try to achieve the virulence regression equation formula of each reagent agent.

Table 9 carbosulfan preparation is to the Toxicity Determination result of cotten aphid

Reagent agent	Toxicity regression formula (Y=)	Correlation coefficient r	LC ₅₀Value (mg/L)	LC ₉₀Value (mg/L)
Reagent agent	Toxicity regression formula (Y=)	Correlation coefficient r	LC ₅₀Value (mg/L)	LC ₉₀Value (mg/L)	Medicament 1	Y＝3.8914+2.0164X	0.9764	2.476	15.26
Medicament 2	Y＝4.7193+1.5915X	0.9942	2.514	16.63	Medicament 1	Y＝3.8914+2.0164X	0.9764	2.476	15.26
Medicament 2	Y＝4.7193+1.5915X	0.9942	2.514	16.63	Medicament 3	Y＝5.5181+1.5174X	0.9971	1.028	8.82

Biological Examples 10:20% carbosulfan suspending agent is to the citrus aphid field control effectiveness test

Present embodiment is at the citrus aphid field control effectiveness test.

Test medicine:

Medicament 2:20% carbosulfan suspending agent

Subjects: crop is a citrus, and controlling object is aphid (ToxopteracitricidusKirkaldy).

Test method: handling medicament 3 for establishing 3000 times of liquid, two concentration of 1500 times of liquid, is contrast agents with medicament 1 and medicament 2 each 1500 times of liquid, is blank totally 6 processing with the spray clear water; Every processing sub-district area 45m ², systematic arrangement repeats 4 times, and each establishes certain guard row between handling; At cotten aphid initial stage of origination (July 24) with workers and peasants 16 type sprayer even spraying, behind preceding 1 day of medicine and medicine, reason district sampling throughout in 1 day, 3 days, 7 days, every sampling point 5 strains, the statistics aphid number of living calculates insect population go down rate and preventive effect.

Result of the test shows, 1500,3000 times of liquid of medicament 3 to the cotten aphid medicine after 1 day preventive effect be respectively 90.6%, 92.5%, be respectively 99.2%, 97.79% in 3 days behind the medicine, be respectively 98.1%, 93.8% in 7 days behind the medicine, each phase preventive effect is all than 1500 times of liquid preventive effect height of medicament 1 and medicament 2, the analysis of 7 days preventive effect significances of difference is that 2 concentration differences of medicament 3 are not remarkable behind the medicine, but all and medicament 1 and 2 of medicaments utmost point significant difference is arranged.

The field control effectiveness test result of table 10 carbosulfan preparation EC against Citrus Aphides

Reagent agent	Extension rate	The insect radix	After the dispenser first day		After the dispenser the 3rd day		After the dispenser the 7th day
			After the dispenser first day		After the dispenser the 3rd day		After the dispenser the 7th day		Borer population	Preventive effect	Borer population	Preventive effect	Borer population	Preventive effect
			Medicament 1	1500	458.3	46.8	89.4	40.5	Borer population	Preventive effect	Borer population	Preventive effect	Borer population	Preventive effect	92.2	41.3	88.6
Medicament 2	1500	288.2	Medicament 1	1500	458.3	46.8	89.4	40.5	30.4	89.3	22.1	93.1	23.4	87.9	92.2	41.3	88.6
Medicament 2	1500	288.2	Medicament 3	1500	650.0	54.3	90.6	8.8	30.4	89.3	22.1	93.1	23.4	87.9	99.2	7.5	98.1
Medicament 3	3000	237.3	Medicament 3	1500	650.0	54.3	90.6	8.8	15.8	92.5	9.3	97.7	9.0	93.8	99.2	7.5	98.1
Medicament 3	3000	237.3	Blank	-	320.8	286.3	0	538.3	15.8	92.5	9.3	97.7	9.0	93.8	0	196.5	0

Poisoning does not take place in for examination concentration.Field trial shows, medicament 3 is compared with similar medicament (medicament 1 and 2) the citrus aphid control efficiency in the field has significant difference.

Biological Examples 11:20% 5a,6,9,9a-hexahydro-6,9-methano-2,4 microemulsion is to the Toxicity Determination test of apple aphid

Present embodiment is the Toxicity Determination test at apple aphid.

Test medicine:

Medicament 1:35% matches red missible oil (5a,6,9,9a-hexahydro-6,9-methano-2,4 commercially available prod, Ai Gefu company produces)

Medicament 2:20% 5a,6,9,9a-hexahydro-6,9-methano-2,4 microemulsion

Medicament 3:20% 5a,6,9,9a-hexahydro-6,9-methano-2,4 microemulsion (example of formulations 6 of the present invention)

Controlling object:

Apple aphid (AphispomiVanDeGeer).

Test method:

The blade medicine embrane method is adopted in this test, the fresh cabbage blade of not used agricultural chemicals (oneself cultivation) was dipped in respectively in above-mentioned each reagent agent solution of series concentration 10 seconds, taking-up is dried in the shade and is placed in the 9cm plastic culture dish, and every ware inserts 50 of aphids, and each concentration is established three repetitions.Check statistics after 24 hours, calculate LC ₅₀Result of the test.

Table 11 endosulfan formulation is to the Toxicity Determination result of apple aphid

Reagent agent	Toxicity regression formula (Y=)	Correlation coefficient r	LC ₅₀Value (mg/L)	LC ₉₀Value (mg/L)
Reagent agent	Toxicity regression formula (Y=)	Correlation coefficient r	LC ₅₀Value (mg/L)	LC ₉₀Value (mg/L)	Medicament 1	Y＝4.8739+3.2154X	0.9867	10.17	25.92
Medicament 2	Y＝4.9721+2.5121X	0.9928	9.41	24.64	Medicament 1	Y＝4.8739+3.2154X	0.9867	10.17	25.92
Medicament 2	Y＝4.9721+2.5121X	0.9928	9.41	24.64	Medicament 3	Y＝6.1298+2.4172X	0.9971	3.91	20.44

The result shows: from LD ₅₀Medicament 3 is than the good drug efficacy of the drug effect of medicament 1.

Biological Examples 12:20% 5a,6,9,9a-hexahydro-6,9-methano-2,4 microemulsion is to the field control effectiveness test of cotten aphid

Present embodiment is the field control effectiveness test at cotten aphid.

Test medicine:

Medicament 2:20% 5a,6,9,9a-hexahydro-6,9-methano-2,4 microemulsion

Controlling object:

Cotten aphid (Aphisgossypii Glover).

Test method: with 2000 times of processing of above-mentioned medicament, be blank, establish 6 processing altogether with the spray clear water; Every processing sub-district area 30m ², systematic arrangement repeats 4 times, and each establishes certain guard row between handling; At cotten aphid initial stage of origination (July 24) with workers and peasants 16 type sprayer even spraying, behind preceding 1 day of medicine and medicine, reason district sampling throughout in 1 day, 3 days, 7 days, every sampling point 5 strains, the statistics aphid number of living calculates insect population go down rate and preventive effect.

Result of the test shows, 2000 times of liquid of medicament 3 to the cotten aphid medicine after 1 day preventive effect be 99.7%, 3 days is 99.9% behind the medicine, be respectively 97.8% in 7 days behind the medicine, each phase preventive effect is all than 2000 times of liquid preventive effect height of medicament 1 and medicament 2, and the analysis of 7 days preventive effect significances of difference is that there were significant differences for medicament 3 and medicament 1 and 2 behind the medicine.

Table 12 endosulfan formulation is to the field control effectiveness test result of cotten aphid

The medicament title	Extension rate (doubly)	Aphid number (head) alive before the medicine	Handle back each day correction preventive effect (%)
			Handle back each day correction preventive effect (%)			1	3	7
			Medicament 1	2000	1250	1	3	7	79.8	93.0	85.9
Medicament 2	2000	1594	Medicament 1	2000	1250	88.7	92.8	83.4	79.8	93.0	85.9
Medicament 2	2000	1594	Medicament 3	2000	1450	88.7	92.8	83.4	99.7	99.9	97.8

Poisoning does not take place in for examination concentration.

Biological Examples 13:5% azoles mite ester microemulsion is to the Toxicity Determination test of two-spotted spider mite

Present embodiment is the Toxicity Determination test at two-spotted spider mite.

Test medicine:

Medicament 1:5% despot mite spirit suspending agent (azoles mite ester commercially available prod, Nihon Nihyaku Co., Ltd produces)

Medicament 2:5% azoles mite ester microemulsion

Medicament 3:5% azoles mite ester microemulsion (example of formulations 7 of the present invention)

For trying insect:

Two-spotted spider mite (Tetranychusurticae) indoor feeding.

Test method:

To grow to the cotton seedling of 2 cotyledons, after contaminating 24 hours with the two-spotted spider mite of indoor feeding, the seedling that will have two-spotted spider mite carries out chemicals treatment with leaf dipping method, and the cotton seedling of every strain has into mite 60-70 head approximately, every kind of medicament is established 5 concentration, every concentration repeats 3 times, makes blank with the cotton seedling that soaks, and the plant of handling is put into (23 ± 1 ℃) in the thermostatic chamber, check anyway after 24 hours to become the mite number, calculate miticidal effect with biological statistical method.

Table 13 azoles mite ester formulation is to becoming the Toxicity Determination result of mite

Reagent agent	Virulence regression equation (y=)	LC ₅₀Value (ppm)	LC ₉₀Value (ppm)	Correlation coefficient r	Relative virus force
					Relative virus force		LC ₅₀	LC ₉₀
					Medicament 1	0.5611+4.0422x	LC ₅₀	LC ₉₀	11.86	39.28	0.9771	1	1
Medicament 2	2.0633+3.5627x	6.67	19.31	0.9969	Medicament 1	0.5611+4.0422x	1.78	1.57	11.86	39.28	0.9771	1	1
Medicament 2	2.0633+3.5627x	6.67	19.31	0.9969	Medicament 3	2.4512+4.1025x	1.78	1.57	3.14	10.96	0.9987	3.78	3.58

The result shows: from LD ₅₀Medicament 3 drug effects significantly are better than medicament 1 and medicament 2.

Biological Examples 14:5% azoles mite ester microemulsion is to the field control effectiveness test of cotton red spider

Present embodiment is the field control effectiveness test at two-spotted spider mite.

Test medicine:

Medicament 2:5% azoles mite ester microemulsion

For trying insect:

Two-spotted spider mite (Tetranychusurticae) indoor feeding.

Test method:

Become mite to originate in the epicotyledonary ovum of cotton seedling in 24 hours, handle with the above-mentioned reagent agent soup dipping of variable concentrations, be put into afterwards in the thermostatic chamber, check the hatching number of ovum after the week, every concentration repeats 3 times, and statistics is killed the ovum effect.

Result of the test:

One-tenth mite on the cotton seedling, soup shows poisoning symptom after handling very soon, and creep speed is slow, and disequilibrium is knocked down, twitches, is rolled, and causes death at last.

The ovum effect extremely of table 14 azoles mite ester formulation

Reagent agent	Concentration (ppm)	For examination ovum grain number	Ovum hatching number	Incubation rate (%)
Reagent agent	Concentration (ppm)	For examination ovum grain number	Ovum hatching number	Incubation rate (%)	Medicament 1	80	247	0	0
40	204	68	33.3			80	247	0	0
40	204	68	33.3	20		235	108	45.9
Medicament 2	40	215	0	20		235	108	45.9	0
	40	215	0	20	228	35	15.4		0
	10	203	86	20	228	35	15.4	42.4
	10	203	86	Medicament 3	8	199	0	42.4	0
4	233	5	2.1		8	199	0		0
4	233	5	2.1		2	219	9	4.1
Blank		198	-		2	219	9	4.1	100

From the table the result as can be seen, medicament 3 is lethality＞90% under 2ppm, 8ppm can kill 100% ovum, drug effect significantly is better than medicament 1 and medicament 2.

Biological Examples 15:0.5% emamectin benzoate microemulsion is to the Toxicity Determination test of cotton bollworm

Present embodiment is the Toxicity Determination test at cotton bollworm.

Test medicine:

This microemulsion of the anti-moth of medicament 1:0.5% (emamectin-benzoate commercially available prod, Hebei Weiyuan Biochemical Co., Ltd. produces)

Medicament 2:0.5% emamectin benzoate microemulsion

Medicament 3:0.5% emamectin benzoate microemulsion (example of formulations 8 of the present invention)

Test method:

Test is cotton bollworm (HelicoverpaarmigeraH ü bner) with worm, 4 instar larvaes.

Adopt dip method, measure medicament its virulence of tagging.The drug concentration gradient is handled, and every processing repeats for 6 times, 48 of every duplication examination worms.Soak 5 seconds of worm, take out and be poured on the blotting paper, inhale and remove unnecessary soup, will try worm and put into 24 hole test boxs respectively, put into the constant incubator cultivation and investigated the insect population lethality in 48 hours.

The Toxicity Determination result of table 15 Affirm (Merck Co.) preparation

For the reagent type	Toxicity regression formula (Y=)	LD ₅₀(95% confidence limit) (μ g/ml)	LC ₉₀Value (μ g/ml)	The synergy multiple
For the reagent type	Toxicity regression formula (Y=)	LD ₅₀(95% confidence limit) (μ g/ml)	LC ₉₀Value (μ g/ml)	The synergy multiple	Medicament 1	4.9439+1.6593x	1.0086(1.99-0.16)	10.35	1.0
Medicament 2	2.9708+2.2803x	0.9844(1.77-0.19)	9.03	1.0	Medicament 1	4.9439+1.6593x	1.0086(1.99-0.16)	10.35	1.0
Medicament 2	2.9708+2.2803x	0.9844(1.77-0.19)	9.03	1.0	Medicament 3	4.1273+2.0689x	0.2564(0.68-0.15)	6.027	3.82

The field control effectiveness test of biological Examples 16:0.5% emamectin benzoate microemulsion control cotton bollworm

Present embodiment is the field control effectiveness test at cotton bollworm.

Test medicine:

Medicament 2:0.5% emamectin benzoate microemulsion

Experimental condition: experimental field be test cotton field, Hebei, the test kind is conventional cotton 492, sowing by the end of April, and rich water quality management unanimity in the experimental plot, the growing way unanimity, the worm amount takes place medium.Worm age is mostly in 3-4 age, whole test phase medication three times.

Spray method: every small size is 50m ², each reprocessing three times, 25 square metres of each sub-district areas, the experimental plot is district's group arrangement at random in the field.With the conventional spraying of KIM-9MATABI knapsack hand sprayer.

Result of the test shows that the control efficiency of 3 pairs of cotton bollworms of medicament obviously improves than medicament 1 and medicament 2, significance test, and control efficiency increases significantly.

The field efficacy result of table 16 emamectin-benzoate preparation control cotton bollworm

For agent medicament and concentration	Radix before the medicine		Medicine one day after		Behind the medicine seven days
	Radix before the medicine		Medicine one day after		Behind the medicine seven days		The ovum number	The larva number	Rate goes down	Proofread and correct preventive effect	Rate goes down	Proofread and correct preventive effect
	Medicament 1 1000X	66	54	75	73.4	80.8	The ovum number	The larva number	Rate goes down	Proofread and correct preventive effect	Rate goes down	Proofread and correct preventive effect	72.6c
Medicament 2 1000X	Medicament 1 1000X	66	54	75	73.4	80.8	76	63	78.6	77.2	84.6	79.5b	72.6c
Medicament 2 1000X	Medicament 3 1000X	59	68	88.3	87.6	98.2	76	63	78.6	77.2	84.6	79.5b	97.4a
Blank CK	Medicament 3 1000X	59	68	88.3	87.6	98.2	71	65	7.0	-	30.1	-	97.4a

Poisoning does not take place in for examination concentration.Field trial shows, medicament 3 is compared with similar medicament (medicament 1 and medicament 2) the cotton bollworm control effect in the field has significant difference.

Biological Examples 17:2.5% decis microemulsion is to the Toxicity Determination test of cabbage caterpillar

Present embodiment is the Toxicity Determination test of carrying out at cabbage caterpillar.

Reagent agent:

Medicament 1:2.5% cream of decamethrin (decis commercially available prod, Beyer Co., Ltd produces)

Medicament 2:2.5% decis microemulsion

Medicament 3:2.5% decis microemulsion (example of formulations 10 of the present invention)

Adopt dip method, medicament to be measured and contrast medicament are diluted with water to 6-9 concentration (0.0975 μ g/ml respectively, 0.195 μ g/ml, 0.39 μ g/ml, 0.78 μ g/ml, 1.56 μ g/ml, 3.125 μ g/ml, 6.25 μ g/ml, 12.5 μ g/ml, 25 μ g/ml) each 500 milliliters, cabbage caterpillar 3 instar larvaes are added gently with tweezers soak in the worm net, behind the sealing network interface, immerse in the above-mentioned soup and rocked for 5 seconds, taking-up is poured on the blotting paper, unnecessary soup is removed in suction, the examination worm is added respectively in the culture dish of diameter 12cm, if 1 fresh cabbage leaves that cleans up in every ware, tighten with rubber band after adding preservative film, put into insulating box and cultivate check result after 24 hours and 48 hours.Each concentration is measured 30 altogether.If clear water contrast.The dead criterion of examination worm: touch polypide with dialling pin, complete motionless person is dead.Go out the LC of microemulsion and missible oil with the calculating computer ₅₀Value, 95% confidence limit, LC ₉₀Value.

Result of the test

Shown in table 17 with dip method to the result of cabbage caterpillar mensuration.Handle after 24 hours the LC of medicament 1 (missible oil contrast) ₅₀Be worth 1.3695 μ g/ml, the LC of medicament 2 and medicament 3 (microemulsion) ₅₀Value is respectively 0.4324 μ g/ml, 0.4161 μ g/ml, and virulence has increased by 3.1,3.3 times respectively.Handle after 48 hours the LC of medicament 2 and medicament 3 ₅₀Value is respectively 0.2812 μ g/ml, 0.2742 μ g/ml, with the LC of medicament 1 ₅₀1.1498 μ g/ml compares, virulence has increased by 4.0,4.2 times respectively.The LC of while medicament 2,3 ₅₀The LC that is worth 95% confidence limit and medicament 1 ₅₀Value confidence limit is not overlapping substantially, illustrates that microemulsion compares with missible oil the virulence of cabbage caterpillar, truly has to significantly improve.

Table 17 decis preparation is to the Toxicity Determination result of cabbage caterpillar

Medicament

Review time

Toxicity regression formula (Y=)

LC ₅₀Value (μ g/ml) ppm

95% confidence limit

LC ₉₀Value (μ g/ml) ppm

The virulence multiple

Medicament 3	24 hours	5.4027+1.0575X	0.4161	0.2266-0.7643	6.8023	3.3
Medicament 3		5.4027+1.0575X	0.4161	0.2266-0.7643	6.8023	3.3	Medicament 2	5.3215+1.0247X	0.4324	0.2352-0.7125	6.9275	3.1
Medicament 1		4.7905+1.5346X	1.3695	0.8063-2.3260	9.3627	1.0	Medicament 2	5.3215+1.0247X	0.4324	0.2352-0.7125	6.9275	3.1
Medicament 1		4.7905+1.5346X	1.3695	0.8063-2.3260	9.3627	1.0	Medicament 3	48 hours	5.6234+1.1093X	0.2742	0.1308-0.5748	3.9333	4.2
Medicament 2	5.5716+1.1083X	0.2812	0.1624-0.6013	3.8954	4.0		Medicament 3		5.6234+1.1093X	0.2742	0.1308-0.5748	3.9333	4.2
Medicament 2	5.5716+1.1083X	0.2812	0.1624-0.6013	3.8954	4.0	Medicament 1	4.9031+1.5978X		1.1498	0.6801-1.9441	7.3077	1.0

Biological Examples 18:2.5% decis microemulsion is to the cotton bollworm control field control effectiveness test

Reagent agent:

Medicament 2:2.5% decis microemulsion

Result of the test shows, medicament 2 and 3 (microemulsion) to the control efficiency of cotton bollworm than the obvious raising of medicament 1 (missible oil), significance test, control efficiency increases significantly.And also there is significant difference between medicament 2 and the medicament 3.The result sees following table 18 for details.

The field control effectiveness test result of table 18 decis preparation control cotton bollworm

Reagent agent and concentration	Repeat	Worm lives before the medicine	Behind the medicine 1 day			Behind the medicine 7 days
			Behind the medicine 1 day			Behind the medicine 7 days			Borer population alive	Rate goes down	Correcting controling effect	Borer population alive	Rate goes down	Correcting controling effect
			Medicament 3 1500 *	1	53	1	98	98a	Borer population alive	Rate goes down	Correcting controling effect	Borer population alive	Rate goes down	Correcting controling effect	0	100	99a
2	52	1		1	53	1	98		98	1	98				0	100
2	52	1		Medicament 2 1500 *	1	50	3		98	1	98	94	96a	2	96	97b
2	51	1	98		1	50	3	1	98			94		2	96
2	51	1	98		Medicament 1 1500 *	1	52	1	98	3	94	95a		3	94		95b
2	51	2	96	2		1	52	96		3	94			3	94
2	51	2	96	2		Medicament 3 3000 *	1	96	51	3	94		94a	3	94	94b
2	54	3	94	3	94		1		51	3	94			3	94
2	54	3	94	3	94		Medicament 2 3000 *	1	50	5	90	91b		6	88.2		89c
2	51	4	92	5	90			1	50	5	90			6	88.2
2	51	4	92	5	90	Medicament 1 3000 *		1	50	10	80		81c	10	80	80d
2	50	9	82	10	80			1	50	10	80			10	80
2	50	9	82	10	80		Blank to clear	1	30	30				30	0
2	31	31		30	0			1	30	30				30	0

Test period :-15 days on the 8th July in 2003, numeral back, table back English alphabet difference, the expression significant difference (p=0.05, HSD)

Biological Examples 19:5% Imidacloprid microcapsule suspending agent is to the Toxicity Determination test of cabbage caterpillar

Present embodiment is the Toxicity Determination test of carrying out at turnip aphid (Lipaphiserysimipseudo-brassicae)

Reagent agent:

Medicament 1:5% receives missible oil (Imidacloprid commercially available prod, Beijing sun in morning plant protection preparation factory produces) according to it

Medicament 2:5% Imidacloprid microcapsule suspending agent

Medicament 3:5% Imidacloprid microcapsule suspending agent (example of formulations 11 of the present invention)

On the basis of preliminary experiment, with above-mentioned 3 kinds of medicaments, be diluted with water to 5 series concentration respectively, concentration range is between causing for examination insect mortality 10%-90%.With reference to the blade infusion process, carry out Toxicity Determination then.Promptly select the higher turnip leaves of insect density, reject other insect and impurity at the binocular stereo microscopically with writing brush, the wingless aphid that keeps individual big or small basically identical, every leaf keeps the 50-70 head, together immerses afterwards in the soup and takes out after 5 seconds, inhales with filter paper and removes unnecessary soup, place culture dish, each concentration repeats 3 times, handles comparing in addition with clear water, moves into then in 28 ± 1 ℃ the incubator.After 48 hours in the dead result of binocular stereo test under microscope aphid, lethality Abbott formula correction, again according to the concentration logarithm---the lethality probit value is analyzed (Bliss) method, obtains the virulence regression equation of each medicament and puts dead middle concentration LC ₅₀Value.

Table 19 Imidacloprid preparation is to the Toxicity Determination result of turnip aphid

Medicament	Toxicity regression formula (Y=)	LC50 value (μ g/ml) ppm	Correlation coefficient r	The virulence multiple
Medicament	Toxicity regression formula (Y=)	LC50 value (μ g/ml) ppm	Correlation coefficient r	The virulence multiple	Medicament 3	2.1350+5.4558x	2.1661	0.9238	3.4
Medicament 2	2.6028+2.7382x	2.4014	0.9574	3.1	Medicament 3	2.1350+5.4558x	2.1661	0.9238	3.4
Medicament 2	2.6028+2.7382x	2.4014	0.9574	3.1	Medicament 1	2.28 35+4.4703x	7.3958	0.9423	1.0

Biological Examples 20:5% Imidacloprid microcapsule suspending agent is a field control effectiveness test at turnip aphid to the field control effectiveness test present embodiment of cotten aphid.

Reagent agent:

Medicament 2:5% Imidacloprid microcapsule suspending agent

Controlling object:

Turnip aphid (Lipaphiserysimipseudo-brassicae).

Test method: 2000 times of soups with above-mentioned each medicament are handled, and are blank totally 6 processing with the spray clear water; Every processing sub-district area 30m ², systematic arrangement repeats 4 times, and each establishes certain guard row between handling; At the turnip aphid initial stage of origination with workers and peasants 16 type sprayer even spraying, behind preceding 1 day of medicine and medicine, reason district sampling throughout in 1 day, 3 days, 7 days, every sampling point 5 strains, the statistics aphid number of living calculates insect population go down rate and preventive effect.

Result of the test shows, 2000 times of liquid of medicament 3 to the turnip aphid medicine after 1 day preventive effect be 92.54%, 3 days is 96.74% behind the medicine, be respectively 97.56% in 7 days behind the medicine, all than 2000 times of liquid preventive effect height of medicament 1 and medicament 2, the analysis of 7 days preventive effect significances of difference is that there were significant differences between medicament 2 and medicament 3 and medicament 1 (missible oil) to each phase preventive effect behind the medicine.

Table 20 Imidacloprid microcapsule suspending agent is to the field control effectiveness test result of turnip aphid

The medicament title	Extension rate (doubly)	Aphid number (head) alive before the medicine	Handle back each day correction preventive effect (%)
			Handle back each day correction preventive effect (%)			1	3	7
			Medicament 1	2000	1250	1	3	7	80.55	85.84	85.9
Medicament 2	2000	1594	Medicament 1	2000	1250	91.32	93.79	95.21	80.55	85.84	85.9
Medicament 2	2000	1594	Medicament 3	2000	1450	91.32	93.79	95.21	92.54	96.74	97.56

Poisoning does not take place in for examination concentration.

Biological Examples 21: pepper extract and triazolone combination are to the control test of root rotof flax (Bipolarissorokininan)

1, Toxicity Determination

Reagent agent:

Medicament 1:2% pepper extract (Chinese prickly ash oil)

Medicament 2:20% triazolone missible oil

Medicament 3:18% triazolone missible oil+2% pepper extract (Chinese prickly ash oil)

Contain the activity that toxic medium method is measured medicament 1, medicament 2 and 3 pairs of root rotof flax bacterium of medicament in indoor employing.The 45ml PSA medium of in the 100ml triangular flask, packing into, being cooled to (45-50) after the sterilization ℃ presses predetermined close and adds different reagent agent 5ml, on average pouring 3 diameters after shaking up into is in the culture dish of 9cm, makes the flat board that contains the variable concentrations medicament, is contrast with the sterile water.From cultivating 7 days germ colony edge, cut-off is the lawn of 5mm directly, and bacterium faces down, and inserts in the plate, and each medicament is established 5 concentration, 3 repetitions.24 ℃ of following constant temperature culture 4 days are measured colony diameter with the cross method of scoring.Calculate the EC of medicament ₅₀Value is obtained virulence regression equation, and estimates the bacteriostatic activity Toxicity Determination result of medicament, sees Table 21.Result of the test shows under indoor isolated condition, the root rotof flax bacterium is not had bacteriostasis, and the triazolone fungistatic effect is better.

The different medicaments of table 21 are to the Toxicity Determination result of root rotof flax

The medicament title	The toxicity regression linear equation	Correlation coefficient and significance thereof	EC50 value (mg/L)
The medicament title	The toxicity regression linear equation	Correlation coefficient and significance thereof	EC50 value (mg/L)	Medicament 1	-	-	-
Medicament 2	P＝2.1749+1.1126X	0.9581**	3.461	Medicament 1	-	-	-
Medicament 2	P＝2.1749+1.1126X	0.9581**	3.461	Medicament 3	P＝3.0619+1.2107X	0.9764**	0.3988

Annotate: * * represents extremely remarkable

The exercising result that is mixed with triazolone shows, can significantly improve the inhibitory action of triazolone to the root rotof flax bacterium, and along with the increase of content, the bacteriostasis degree is stronger

2, seed treatment result

Reagent agent:

Medicament 1:0.2% pepper extract (preparation embodiment 1)

Medicament 2:0.015% triazolone missible oil dilution

Medicament 3:0.2% pepper extract+0.015% triazolone microemulsion dilution

With medicament 1, medicament 2, medicament 3 are handled wheat seed respectively, root rotof flax is had tangible diseases prevention protect the product effect.After carrying out seed treatment, the wheat plant robust growth, growing way is good, and powdery mildew takes place to contrast obviously to alleviate.Medicament 3 has obviously improved its diseases prevention and has protected the product effect.Protect the product effect and bring up to 10.67% by 7.79% of medicament 2.

The diseases prevention of the different medicament seed treatment of table 22 is protected and is produced effect

Medicament and consumption	Seedling stage		Become the strain phase			Output kg/hm2	Protect and produce effect (%)
	Seedling stage		Become the strain phase					The incidence of disease (%)	Preventive effect (%)	The incidence of disease (%)	Disease index	Preventive effect (%)
	Medicament 1	10.8	14.29	81.3	32.9			The incidence of disease (%)	Preventive effect (%)	The incidence of disease (%)	Disease index	Preventive effect (%)	3.80	5915.55	4.66
Medicament 2	Medicament 1	10.8	14.29	81.3	32.9	4.9	61.11	74.5	21.6	36.84	6246.45	7.79	3.80	5915.55	4.66
Medicament 2	Medicament 3	4.3	65.87	69.4	18.2	4.9	61.11	74.5	21.6	36.84	6246.45	7.79	46.78	6412.80	10.67
CK	Medicament 3	4.3	65.87	69.4	18.2	12.6	-	85.9	34.2	-	5795.25	-	46.78	6412.80	10.67

Carry out seed treatment with medicament 2, promoted the growth of wheat root, and the growth of bud is suppressed, improved root/shoot ratio, it is late that wheat is emerged, and emergence rate descends.Its inhibiting mechanism may be owing to directly suppress the synthetic of seed inner gibberellin, suppressed alpha-amylase activity indirectly, and then influence is germinateed and the speed of emerging.

Medicament 1 on synthetic medium to root rotof flax bacterium unrestraint effect.With fungicide compounding, no matter be indoor or field trial, all played obvious synergistic effect.With medicament 3 has been carried high seed germination rate and emergence rate, has shortened the wheat seedling-growing time, the plant strain growth stalwartness, and the leaf look dark green, reduced the disease index of root rotof flax, has tangible diseases prevention and protect the product effect.Medicament 3 has improved the protection effect of bactericide, has remedied triazolone to the wheat seed germinating and the inhibited deficiency of emerging.When having studied pepper extract and triazolone clear and definite and having used with to the synergistic effect of root rotof flax.

Biological Examples 22:0.3% aqueous matrine solution is to the Toxicity Determination test of vegetable aphid

Present embodiment is the Toxicity Determination test at vegetable aphid.

Test medicine:

The medicament 1:0.3% elder brother of green section sandfly aqua (matrine commercially available prod, Dalian, Liaoning Province biochemistry corporation,Ltd. of green section produces)

2,0.3% aqueous matrine solution (example of formulations 12 of the present invention)

Controlling object:

On the rape plant, gather the aptery blade of band black peach aphid (Myzuspersicae), select the nymph of median size, body colour basically identical as if aphid.

Test method: 0.3% aqueous matrine solution is diluted to 5 series concentration, clean in advance fresh three leaves of choosing of dipping wholeheartedly are with root from native green vegetables seedling 1min respectively, take out and put into Cans respectively after nature dries, every bottle of 1 dish seedling, root is wrapped with wet cotton balls, inserts 20 aphids of getting ready to the dish leaf with the fine, soft fur pen, use black cloth capping bottleneck at last, (L: D=13: 11), every processing repeats 3 times, and is contrast with the clear water to place breeding observing in 25 ℃ of illumination boxs.Under anatomical lens, touch the aphid polypide after 48 hours with banister bruss, aphid six sufficient movable conducts worm alive, on the contrary as dead worm, investigate live aphid number and dead aphid number respectively.Calculate lethality and corrected mortality, ask toxicity regression formula and LD with the probit analysis method ₅₀And LD ₉₅Above-mentioned all calculating are all carried out with Excel software according to the auspicious method of Zhang Zhi.

Adopt infusion process to measure the interior drug abuse power of reagent agent 0.3% aqueous matrine solution to vegetable aphid (black peach aphid), the ratio of killing to black peach aphid under series concentration sees Table 22.

It is as follows to the interior drug abuse power measurement result of black peach aphid to calculate test medicine with the probit value method: toxicity regression formula: Y=4.6260+1.2400x (r=0.9924)

LD ₅₀=2.0027 μ g/ml (95% confidence limit: 1.4246～2.8154 μ g/ml), SE=0.3480

LD ₉₅=42.0916 μ g/ml (95% confidence limit: 19.4232～91.2162 μ g/ml), SE=16.6087

Table 22 0.3% aqueous matrine solution is surveyed the result to the indoor interior drug abuse Lik-Sang of vegetable aphid

Concentration μ g/ml	The concentration logarithm	The dead borer population head of 48h	Lethality %	Corrected mortality %
Concentration μ g/ml	The concentration logarithm	The dead borer population head of 48h	Lethality %	Corrected mortality %	15.2	1.1818	53	88.333	88.135

7.6	0.8808	44	76.333	72.881
7.6	0.8808	44	76.333	72.881	3.8	0.5798	38	63.333	62.711
1.9	0.2788	30	50	49.512	3.8	0.5798	38	63.333	62.711
1.9	0.2788	30	50	49.512	0.95	-0.0223	22	36.667	35.593
CK		1	1.6667		0.95	-0.0223	22	36.667	35.593

Annotate: examination worm sum is 60

Biological Examples 23:0.3% aqueous matrine solution is to the field efficacy determination test of fruit tree yellow aphids

Present embodiment is the field efficacy determination test at the fruit tree yellow aphids.

Test medicine:

Controlling object: fruit tree yellow aphids (AphispomiDeGeer), for the examination tree, 18 years living Gold Delicious apples, seeding row spacing 3m * 4m, growth potential and managerial skills are general.

Test method: this test is carried out in big five another arenaes, orchard, Shahe, adopts 1000 times of the present invention's 0.3% aqueous matrine solutions and terre verte ground, Beijing agricultural chemical of natural plant factory to produce 1000 times of 2 processing of 0.3% aqueous matrine solution, and individual plant district group repeats 4 times.Spray medicine morning May 13, about every strain dosage 25kg, (morning on the same day) fixed branch investigation insect population radix before the spray medicine was investigated the insect population rate that goes down in 4 hours, 24 hours respectively, as control efficiency behind the medicine.

Two kinds of chemical control apple yellow aphids of table 23 effect relatively

Medicament	Insect population radix (head) before the medicine	4 hours preventive effects behind the medicine		24 hours preventive effects behind the medicine
		4 hours preventive effects behind the medicine		24 hours preventive effects behind the medicine		Worm amount (head)	Preventive effect %	Worm amount (head)	Preventive effect %
		Medicament 1	393	35	91.1	Worm amount (head)	Preventive effect %	Worm amount (head)	Preventive effect %	17	95.7
Medicament 2	408	Medicament 1	393	35	91.1	299	26.7	74	81.9	17	95.7

By knowing in the table 23,1000 times of the present invention's 0.3% aqueous matrine solutions are 95.7% to 24 hours preventive effects of yellow aphids, and are effective, and the speed of knocking down is fast, and 4 hours preventive effects reach 91.1% behind medicine; Even and contrast preventive effect after 24 hours also only is 81.9%.

The test of the high chlorine suspension emulsion of the rich propylene of biological Examples 24:0.25% mosquito killing effect

Test medicine:

The rich high chlorine suspension emulsion of propylene (JiangSu Province agricultural chemical Research Institute Co., Ltd production) of medicament 1:0.25%;

The rich high chlorine suspension emulsion of propylene (example of formulations 13 of the present invention) of medicament 2:0.25%.

Test worm kind: the Culex pipiens pallens female adult mosquito of not sucking blood in the back in 2-3 days that sprouts wings, the housefly back 4 days adults that sprout wings, male and female half and half are hand-feeding propagation's sensitive strain.

Test method: by GB GB13917.1-92 agriculture chemical registration hygienic insecticide indoor pharmacodynamic test method; the indoor harmacological effect assay method of propellant; Culex pipiens pallens 20 every group (30 every group of houseflies) is put into bell jar; wait to try worm and recover normal activity; after medicine sprayed into, write down down and out examination worm at regular intervals.After 20 minutes whole insects are shifted in the normal cage, and feed with 5% syrup cotton balls, checked examination worm death toll in 24 hours, test repeats 3 times, the results are shown in Table.

The high chlorine suspension emulsion of table 24 0.25% rich propylene is given birth to and is surveyed the result

Test number (TN)	KT50(min)		24h lethality (%)
	KT50(min)		24h lethality (%)		Mosquito	Fly	Mosquito	Fly
	Medicament 1	3.5	3.6	99.4	Mosquito	Fly	Mosquito	Fly	99.6
Medicament 2	Medicament 1	3.5	3.6	99.4	2.6	2.7	100	99.1	99.6
	2.5	2.6	99.3	99.5	2.6	2.7	100	99.1
	2.5	2.6	99.3	99.5	2.6	2.7	100	100

Measurement result shows, medicament 1 with compare, suitable to the mosquito killing effect, and that medicament 2 is knocked down speed is faster.

Biological Examples 25:10% first cyanogen four mite suspension emulsions are to the control efficiency field control effectiveness test of European red mite

Present embodiment is the control efficiency field control effectiveness test at European red mite.

Test medicine:

Medicament 1:10% first cyanogen four mite suspension emulsions (Xi'an Inst. of Modern Chemistry's production),

Medicament 2:10% first cyanogen four mite suspension emulsions (example of formulations 14 of the present invention)

Subjects: crop is an apple, and controlling object is European red mite (Panonychusulmi).

Test method: test is carried out in Xu Xi Wan Cun apple orchard, Yangling District Li Tai township, and fruit variety is Fuji apple and Qin Guan, age of tree 10a, and seeding row spacing 2.8 * 3.2m grows fine.Test establishes 2000 *, 1500 *, 1000 *, medicament 1 is contrast medicine dilution 1500 * and clear water contrast totally 5 processing, fix the 3rd, 5, No. 7 tree successively and be the investigation tree, every investigation tree respectively selects branch 5 blades of mark of listing by all directions five positions, make, investigate before the spray medicine as if the mite number, investigate the mite number of living respectively in 1 day, 3 days, 7 days behind the spray medicine, add up miticidal effect.While every processing harvesting blade 5 (non-marked blades) after spraying medicine is taken back the indoor culture dish that is lined with wet filter paper of putting into and is preserved moisture, and pursues the hatching number of leaf inspection ovum after 1 week under the binocular anatomical lens, and statistics is killed the ovum effect.Dispenser is sprayed medicine with 3WBS-16 type knapsack hand sprayer, and the spraying liquid amount is advisable by squirting not following of leave dual sides soup, every about hydrojet 1.2kg of tree.

Table 25 10% first cyanogen four mite suspension emulsions control European red mite effect

Reagent agent	Extension rate	The insect radix	After the dispenser first day		After the dispenser the 3rd day		After the dispenser the 7th day
			After the dispenser first day		After the dispenser the 3rd day		After the dispenser the 7th day		The insect population rate that goes down	Preventive effect	Borer population	Preventive effect	Borer population	Preventive effect
			Medicament 1	1500	10503	74.9	73.5	87.0.1	The insect population rate that goes down	Preventive effect	Borer population	Preventive effect	Borer population	Preventive effect	86.8	88.4	88.4
Medicament 2	2000	10191	Medicament 1	1500	10503	74.9	73.5	87.0.1	81.1	96.3	95.1	95.0	98.1	98.0	86.8	88.4	88.4
	2000	10191	1500	9272	90.7	90.2	98.9	98.9	81.1	96.3	95.1	95.0	98.1	98.0	99.7	99.7
	1000	10704	1500	9272	90.7	90.2	98.9	98.9	96.5	80.1	99.6	99.6	100	100	99.7	99.7
	1000	10704	Blank	-	12495	5.2		1.4	96.5	80.1	99.6	99.6	100	100		3.0

Result of the test: the miticidal effect of first cyanogen four mite suspension emulsions is tested and is investigated the insect population radix morning July 29, spray medicine afternoon, 1 day (July 20), 3 days (August 1), 7 days (August 5) are investigated respectively behind the medicine, result's (table 1) shows: 3 concentration of treatment control European red mites of (1) medicament 2 are all obtained positive effect, increase preventive effect with concentration and improve; After the dispenser 1 day, 2000 *, 1500 * and 1000 * preventive effect be followed successively by 80.1%, 90.2% and 96.3%, three kind of concentration dispenser after 3 days and the preventive effect after 7 days reach respectively 95% or more with more than 98%, wherein the preventive effect after 1000 * 7 days reaches 100%.(2) 1 day, 3 days, 7 days preventive effects all are better than contrasting the preventive effect of medicament 1 behind 2 doses of medicines of medicament.(3) dispenser is after 7 days, observe discovery from field investigation, the rate though clear water check plot insect population goes down naturally, but spray medicine district and clear water check plot apple blade color distortion are very big, the blade table of clear water check plot reveals tangible chlorosis spot and shrivelled shape, the sign that untimely defoliation is arranged, and the leaf color in spray medicine district is normal, it is more that tip point grows new leave.

Though the present invention is described in detail with a general description of the specific embodiments above, on basis of the present invention, can to work some will be apparent to those skilled in the art and revise or improve.Therefore, these modifications or improvements all belong to the scope of protection of present invention without departing from theon the basis of the spirit of the present invention.

Claims

1, a kind of aqueous pesticide, it contains pesticide activity component and pepper extract, and described pesticide activity component and pepper extract amount ratio by weight are 1: 0.005-100.

2, aqueous pesticide according to claim 1 is characterized in that, pesticide activity component and pepper extract amount ratio by weight are 1: 0.01-50.

3, aqueous pesticide according to claim 1 is characterized in that, described pesticide activity component is selected from one or more in insecticide, bactericide and the weed killer herbicide.

4, aqueous pesticide according to claim 1, it is characterized in that, described insecticide is selected from the organochlorine class, pyrethroid, carbamates, organic phosphates, nereistoxin, in the biological species insecticide one or more, described bactericide is selected from the organic sulfur class, the organo-arsenic class, organic phosphates, substituted benzene, azole, antibiotics, 1,2, in the 4-triazole bactericidal agent one or more, described weed killer herbicide is selected from phenoxy carboxylic acid, amide-type, substituted urea class, phenyl amines, carbamates, triazine, in the organic phosphates weed killer herbicide one or more.

5, aqueous pesticide according to claim 1, it is characterized in that described pesticide activity component is to be selected from 5a,6,9,9a-hexahydro-6,9-methano-2,4, gamma cyhalothrin, decis, cypermethrin and various isomer, Hostathion, carbosulfan, Methomyl, Avermectin, Affirm (Merck Co.) and salt thereof, fluorine bell urea, azoles mite ester, Imidacloprid, tolelofos-methyl, triazolone, the matrine one or more.

6, aqueous pesticide according to claim 1 is characterized in that, it also contains cosolvent and emulsifier, and the percentage by weight of its each component is:

Pesticide activity component 0.1-30%

Pepper extract 0.1-30%

Cosolvent 1-10%

Emulsifier 5-20%

Water surplus.

7, aqueous pesticide according to claim 6 is characterized in that, it also contains stabilizing agent, and the percentage by weight of its each component is:

Pesticide activity component 0.1-30%

Pepper extract 0.1-30%

Cosolvent 1-10%

Emulsifier 5-20%

Stabilizing agent 5-10%

Water surplus.

According to the arbitrary described aqueous pesticide of claim 1-7, it is characterized in that 8, it is aqueous solvent, microemulsion, aqueous emulsion, suspending agent, suspended emulsion or microcapsule formulations.

9, a kind of method for preparing arbitrary described aqueous pesticide of claim 1-7, it comprises the steps:

2. with pesticide activity component and cosolvent and/or emulsifier and/or stabilizing agent, stir, form solution B;

3. merge solution A and B, homogenize.

10, a kind of method for preparing arbitrary described aqueous pesticide of claim 1-7, it comprises the steps:

1. with pepper extract and pesticide activity component, cosolvent and/or emulsifier and/or stabilizing agent, stir, make solution A;

2. merge solution A and dispersion medium water, homogenize.