CN110037058A - Cause the compound of insect muscle cramp - Google Patents
Cause the compound of insect muscle cramp Download PDFInfo
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- CN110037058A CN110037058A CN201910268955.8A CN201910268955A CN110037058A CN 110037058 A CN110037058 A CN 110037058A CN 201910268955 A CN201910268955 A CN 201910268955A CN 110037058 A CN110037058 A CN 110037058A
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
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- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/02—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms
- A01N43/04—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom
- A01N43/14—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom six-membered rings
- A01N43/16—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom six-membered rings with oxygen as the ring hetero atom
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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- A01N51/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds having the sequences of atoms O—N—S, X—O—S, N—N—S, O—N—N or O-halogen, regardless of the number of bonds each atom has and with no atom of these sequences forming part of a heterocyclic ring
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- A01N53/00—Biocides, pest repellants or attractants, or plant growth regulators containing cyclopropane carboxylic acids or derivatives thereof
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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- A01N57/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds
- A01N57/10—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-oxygen bonds or phosphorus-to-sulfur bonds
- A01N57/16—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-oxygen bonds or phosphorus-to-sulfur bonds containing heterocyclic radicals
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- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
- A01N59/20—Copper
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- C08B30/00—Preparation of starch, degraded or non-chemically modified starch, amylose, or amylopectin
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Abstract
The present invention provides the compound for causing insect muscle cramp, belongs to field of biotechnology, comprising that can cause insect muscle cramp and lead to dead active insecticidal compounds；Copper-based sterilization component with stomach poison function；Attractant containing plant protein hydrolysate or animal hydrolyzed protein or higher fatty acids or sugar；And starch base covering material.Above-mentioned compound the preparation method comprises the following steps: disperse copper-based sterilization component in protective starch base covering material, dispersed phase compound is made in and the dispersion formed after being dried, then mix with active insecticidal compounds and attractant.Compound provided by the invention is to existing insecticide without cross tolerance, and not easy to reunite, mobility and suspension are good, and lasting medicine is excellent, carries out improper interference to insect nerve system, causes insect muscle cramp and then benumbs lethal；Preparation method can reduce molecular crystalline performance, improve coating film mechanical performance, tensile strength and barrier property, extend pharmaceutical activity and shelf storage life.
Description
Technical field
The invention belongs to field of biotechnology, and in particular to cause the compound of insect muscle cramp.
Background technique
Insect infection is chief threat for important economical crops (such as soybean and cotton), the yield of plant by
The negative effect of insect infestations.Chemical Control is to prevent and control the important way of pest in agricultural.But, available reagent is to certain
The effect of the pest of a little types is unsatisfactory, has selectivity to invertebrate such as insect, spider and its larva, and to ridge
Vertebrate such as mammal, fish, poultry and other types have very little toxicity or nontoxic, and exist residual and it is environmentally hazardous
Disadvantage；There is harmful influence with toxicity or on mammal, fish, poultry or other types for not being product target, such as
Organic phosphorus compound and carbamates inhibit the activity of the acetylcholinesterase of insect and all animal species, it is known that kill
Worm amidine and relevant formamidine act on the intracorporal octopamine receptor of insect, but due to the potential cardiac toxic to vertebrate
With the carcinogenicity on animal and the various influences of different insects have been exited from the market；Several have although being used alternatingly
The arrestant of different role mode is applicable to good Pest management, but the control insect that this method cannot be satisfied with；
The use of drug is only to take band-like application, spot application and soil application directly to connect to avoid with natural enemy high-incidencely in insect
Touching, selective and impermanency reagent use increase environmental safety and reduce the generation of insect-resistant, but in reality
Majority can only individually control insect pest in the use of border, to prevent insect from generating cross tolerance.Further, since making for a long time
With conventional pesticide, many pests generate drug resistance and drug resistance to common pesticide, and at present to the use of pesticidal agents
Environment and economic requirement (such as in action spectrum, toxicity, selectivity, rate of application, the formation of residue and good preparative capacibility
Aspect) it is increasing.
Although insecticide and composition are developed to control such as crop pests, the pest for polluting environment or food
The pests such as the wooden pest, but still need to continually develop and explore new method and drug to control these pests, this desinsection is multiple
It needs to have high synergistic effect with composition, there is no cross tolerance, low environmental impact to existing insecticide, by relevant workload
The advantages of obviously reducing with cost.
Summary of the invention
The purpose of the present invention is to provide one kind to existing insecticide without cross tolerance, not easy to reunite, mobility and suspension
Property is good, and lasting medicine is excellent, and the compound for causing insect muscle cramp of improper interference is carried out to insect nerve system.
Molecular crystalline performance can be reduced the purpose of the present invention is to provide a kind of, it is strong to improve coating film mechanical performance, tension
Degree and barrier property extend the preparation method of the compound for causing insect muscle cramp of pharmaceutical activity and shelf storage life.
The technical solution that the present invention is taken to achieve the above object are as follows:
The compound for causing insect muscle cramp includes,
A, at least one active insecticidal compounds, above-mentioned active insecticidal compounds can cause insect muscle cramp and cause dead
It dies；
B, at least one copper-based sterilization component, above-mentioned copper-based sterilization component have stomach poison function；
C, at least one attractant, above-mentioned attractant are containing plant protein hydrolysate or animal hydrolyzed protein or higher fatty acids
Or sugar lure auxiliary material；
D, at least one starch base covering material.The compound obtains collaboration effect by rational mixture between effective component
Fruit, can by tagging, stomach toxicity, interior suction and fumigation effect the normal conduction of insect nerve system is interfered, make insect flesh
Meat spasm, paralysis and it is dead, complete the purpose killed, and insect not only can be effectively prevented without cross tolerance to existing insecticide
Infringement, can also promote lesion caused by plant growth and pre- bacteriological protection, have the characteristics that efficient, low toxicity, safety, be suitble to agriculture
The insect control in the places such as field, fruit-bearing forest, green lawn, warehouse, household.
Preferably, the weight accounting for each component that compound includes is as follows: active insecticidal compounds 20~60%, it is copper-based
Sterilization component 20~40%, attractant 10~20%, starch base covering material 10~20%, total amount is in terms of 100%.
Further preferably, active insecticidal compounds are one or more neurotransmitter excitants or antagonist, above-mentioned nerve
It include: 1) pyrethroid compound in mediator excitant or antagonist, such as cypermethrin, Permethrin, ethofenprox；2) organic phosphorus
Compound, such as first Toyodan, parathion-methyl, diazinon, Hostathion；3) Macrocyclic lactone compounds, such as pleocidin remove entomogenous fungi
Element；4) acetylcholine-receptor ligands compound, such as imidacloprid, Acetamiprid, Diacloden；5) with the natural extraction of insecticidal activity
Object, such as Scopoletin, wilforine.Effective component such as Scopoletin in active insecticidal compounds can inhibit acetylcholine ester
Enzymatic activity causes acetyl choline content to increase, and block nerves conduction inhibits Na+-K+Atpase activity makes intracellular K+Ionic product
It is tired, lead to cell water suction rupture；If wilforine can cause insect musculature lesion, to muscle cell membrane and organelle intracellular
(sarcoplasmic reticulum, mitochondria etc.) all has destruction, may act on RyR and inositol triphosphate receptor (IP on sarcoplasmic reticulum3R),
Cause the calcium ion in sarcoplasmic reticulum calcium library to discharge, lead to cellular calcium homeostasis, and then causes myocyte's structural damage or even bad
Dead or apoptosis further results in insect and the symptoms such as the weak and limp, paralysis of muscle occurs, gradually dead.
Preferably, compound is applied to insect and its habitat in a manner of continuous or interval, amount of application is 200~
500g/ hectare/time.Preferably, agriculturally suitable auxiliary agent, solvent, carrier or surfactant can be added when compound is applied
Deng, such as kaolin, clay, water, butanol, vegetable oil, phosphatide, organic solvent, lignosulfonates.
Preferably, insect includes Diptera, Hymenoptera, Orthoptera, Blattaria and coleoptera.
The invention also discloses a kind of preparation methods of above-mentioned compound for causing insect muscle cramp, by killing copper-based
Bacterium ingredient is scattered in protective starch base covering material, and the dispersion formed after being dried, then with active parasite killing
Object and attractant mixing are closed, dispersed phase compound is made.Copper-based sterilization component can make insect protein qualitative change by systemic action
Property, to generate toxicity, while copper ion can participate in and promote the redox reaction of plant, respiration and photosynthetic work
With to promote the metabolism and synthesis of carbohydrate and protein, raising chlorophyll stability enables plant cold resistance, drought resisting
Power greatly enhances, simultaneously because copper ion makes the ability of protein denaturation, so using starch base covering material by copper-based sterilization
Ingredient and attractant are separated.
Preferably, protective starch base covering material adds copper-based sterilization component after carrying out Fruit storage again；
The vacuum degree of above-mentioned vacuum outgas is 0.05~0.1MPa, and the time is 10~15min.Starch base covering material is coated on copper-based kill
Bacterium ingredient surface can not only prevent copper-based ingredient from causing drug effect in storage life to lose to external migration, but also surface can have been prevented to draw
Lure internally penetrates into and causes to go bad, to lose the attracting action to insect, and covering material is polysaccharide, by plant or
It after insect adsorption, can be absorbed by fast decoupled, so that sterilization component generation acts on, while covering material has during storage
Stable physical compatibility activity, can safely pack and use in instant preparation, increase the safety of environment, reduce pest
Drug resistance extends the duration of efficacy of compound.
Preferably, copper-based sterilization component is after being crystallized in water-soluble chitosan solution by copper sulphate and milk of lime,
Colloid mill scale is ground under conditions of being 22~27 and drying is made.Copper-based sterilization component grain diameter after colloidal film is ground
Small, particle surface free energy becomes larger, and particle sinking speed is slower, can have in covering material when being coated preferably outstanding
Buoyancy energy and mobile performance, are more advantageous to and are equably wrapped in material.
Further preferably, the weight ratio of copper sulphate and milk of lime is 5~7:10；The mass concentration of water-soluble chitosan solution
It is 0.5~2%；Crystallizing required temperature is 60~80 DEG C, and the time is 20~30min.What copper sulphate and milk of lime were formed copper-based kills
Bacterium ingredient is mainly basic copper sulfate, in water be in slightly soluble state, chitin there are in the environment of, crystallize the alkali formula sulfuric acid of formation
Copper is in developmental process, and chitin influences crystal by hydrogen bond, using the hydroxyl in chitin molecule as site, with crystal
In calcium ion between formed connection, the metastable basic copper sulfate crystal of induced synthesis, this metastable state crystal is due to heating power
Learn it is unstable, be difficult to generate cenotype, therefore be less likely to occur agglomeration between crystal fine particle, mobility and suspendability obtain
To be promoted, simultaneously because the specific surface area of metastable state crystal and surface Gibbs function are all very big, therefore when subsequent cladding, it can be fast
Rapid hardening gathers and coats starch-based material, thereby reduces surface Gibbs function to increase surface area, the thermodynamics for reaching new is steady
Stationary state is conducive to improve drug in the intracorporal lasting medicine of insect.
Preferably, starch base covering material is made by following steps: by the shallow lake containing 50~70wt% amylose
Powder raw material is configured to the solution that concentration is 3~5% (w/v), after glycerol, succinic acid and ethylene oxide is added, in ultrasonic environment
After lower pre-gelatinized, then be placed in 110~130 DEG C, 40~60min of processing under 0.09~0.12MPa to obtain the final product.
Further preferably, the additive amount of glycerol, succinic acid and ethylene oxide be respectively starch raw material weight 15~20%,
0.06~0.15% and 0.2~0.4%；Above-mentioned ultrasonic power is 800~1200W, and pre-gelatinized uses temperature for 80~95 DEG C
Water-bath, gelatinization time be 20~30min.It is gelatinized in ultrasonic environment, can use the mechanism and cavitation of ultrasonic wave
Effect, makes starch molecular chain be fully extended and interrupt, the hydroxyl in strand is exposed, hydroxyl and hydrophilic carboxyl ester
Change, substituted starch intramolecular and intermolecular hydrogen bond, reduce crystal property of the starch molecule in gelatinization, at the same carboxyl with surpassed
The ethylene oxide that sound wave is opened is connected with hydrogen bond, is formed starch matrix gel, is then obtained under high pressure-temperature with network knot
The starch film of structure, this starch molecule-carboxy-epoxy base network structure have space during starch drying and forming-film
Inhibition, while wherein each group institute is electrically charged mutually exclusive, and starch molecular chain is made to participate in rearranging in film forming procedure,
It forms starch micro-domains to increase, micro-domains bulk density increases, and then makes the mechanical performance, tensile strength and barrier property of coating film
It can be improved, be conducive to the cladding to copper-based ingredient and the infiltration barrier to attractant, extend compound pharmaceutical activity and goods
Frame storage life, and the starch film after rearrangement is easier to degrade in plant and insect bodies, is beneficial to drug release and absorption.
The invention has the benefit that
1) compound of insect muscle cramp is caused to obtain collaboration effect by rational mixture between effective component in the present invention
Fruit, can by tagging, stomach toxicity, interior suction and fumigation effect the normal conduction of insect nerve system is interfered, make insect muscle
Spasm, paralysis and it is dead, complete the purpose killed, and to existing insecticide without cross tolerance, insect not only can be effectively prevented and invade
Evil, can also promote lesion caused by plant growth and pre- bacteriological protection, have the characteristics that efficiently, low toxicity, safety, suitable farmland,
The insect control in the places such as fruit-bearing forest, green lawn, warehouse, household；
2) copper-based sterilization component contained by compound can make insect protein be denaturalized by systemic action in the present invention, thus
Toxicity is generated, while copper ion can participate in and promote the redox reaction, respiration and photosynthesis of plant, to promote
Into the metabolism and synthesis of carbohydrate and protein, chlorophyll stability is improved, increases plant cold resistance, drought-resistant ability greatly
By force；
3) starch base covering material is polysaccharide in the present invention, both copper-based ingredient can be prevented to cause storage life to external migration
Interior drug effect is lost, and surface attractant can be prevented internally to penetrate into and cause to go bad, and the attracting action to insect is lost, in quilt
It after plant or insect adsorption, can be absorbed by fast decoupled, so that sterilization component generation acts on, while covering material is in storage process
In with stable physical compatibility activity, can safely pack and be used in instant preparation, increase the safety of environment, drop
Low pest resistance to insecticide extends the duration of efficacy of compound；
4) preparation method of compound is simple in the present invention, and strong operability is not allowed between crystal fine particle during the preparation process
Agglomeration easily occurs, improves mobility and suspendability, reduces crystal property of the molecule in gelatinization, improves coating film
Mechanical performance, tensile strength and barrier property are conducive to improve drug in the intracorporal lasting medicine of insect, extend compound medicine
Object activity and shelf storage life, are beneficial to drug release and absorption.
The compound for causing insect muscle cramp is provided present invention employs above-mentioned technical proposal, compensates for the prior art
Deficiency, reasonable design, easy operation.
Detailed description of the invention
Fig. 1 is the surface scan Electronic Speculum schematic diagram of the made starch base coating film of embodiment 7 in test example 1；
Fig. 2 is the surface scan Electronic Speculum schematic diagram of the made starch base coating film of embodiment 3 in test example 1.
Specific embodiment
Technical solution of the present invention is described in further detail below in conjunction with specific embodiment and attached drawing:
Embodiment 1:
The compound for causing insect muscle cramp includes,
A, at least one active insecticidal compounds, above-mentioned active insecticidal compounds can cause insect muscle cramp and cause dead
It dies；
B, at least one copper-based sterilization component, above-mentioned copper-based sterilization component have stomach poison function；
C, at least one attractant, above-mentioned attractant are containing plant protein hydrolysate or animal hydrolyzed protein or higher fatty acids
Or sugar lure auxiliary material；
D, at least one starch base covering material.The compound obtains collaboration effect by rational mixture between effective component
Fruit, can by tagging, stomach toxicity, interior suction and fumigation effect the normal conduction of insect nerve system is interfered, make insect flesh
Meat spasm, paralysis and it is dead, complete the purpose killed, and insect not only can be effectively prevented without cross tolerance to existing insecticide
Infringement, can also promote lesion caused by plant growth and pre- bacteriological protection, have the characteristics that efficient, low toxicity, safety, be suitble to agriculture
The insect control in the places such as field, fruit-bearing forest, green lawn, warehouse, household.
The weight accounting for each component that compound includes is as follows: active insecticidal compounds 40%, copper-based sterilization component 30%,
Attractant 15%, starch base covering material 15%, total amount is in terms of 100%.
Active insecticidal compounds be one or more neurotransmitter excitants or antagonist, above-mentioned neurotransmitter excitant or
It include: 1) pyrethroid compound in antagonist, such as cypermethrin, Permethrin, ethofenprox；2) organic phosphorus compound, such as first
Toyodan, parathion-methyl, diazinon, Hostathion；3) Macrocyclic lactone compounds, such as pleocidin, avermectin；4) acetyl gallbladder
Alkali receptor ligand compound, such as imidacloprid, Acetamiprid, Diacloden；5) with the natural extract of insecticidal activity, such as Anisodus luridus
Element, wilforine.Preferred active insecticidal compounds in the present embodiment are as follows: cypermethrin, Hostathion, imidacloprid, Anisodus luridus
Element, each component are mixed with identical weight point ratio.Effective component such as Scopoletin in active insecticidal compounds can inhibit acetyl
Cholinesterase activity causes acetyl choline content to increase, and block nerves conduction inhibits Na+-K+Atpase activity makes intracellular K+
Ion accumulation leads to cell water suction rupture；If wilforine can cause insect musculature lesion, to muscle cell membrane and intracellular
Organelle (sarcoplasmic reticulum, mitochondria etc.) all has destruction, may act on RyR and inositol triphosphate receptor on sarcoplasmic reticulum
(IP3R), cause the calcium ion in sarcoplasmic reticulum calcium library to discharge, lead to cellular calcium homeostasis, so cause myocyte's structure by
Damage, or even necrosis or apoptosis further result in insect and the symptoms such as the weak and limp, paralysis of muscle occur, gradually dead.
Compound is applied to insect and its habitat in a manner of continuous or interval, and amount of application is 500g/ hectare/time.It is excellent
Agriculturally suitable auxiliary agent, solvent, carrier or surfactant etc. can be added when applying in selection of land, compound, and such as kaolin glues
Soil, water, butanol, vegetable oil, phosphatide, organic solvent, lignosulfonates etc..
Insect includes Diptera, Hymenoptera, Orthoptera, Blattaria and coleoptera.
A kind of preparation method of the above-mentioned compound for causing insect muscle cramp, by dispersing guarantor for copper-based sterilization component
In the starch base covering material of shield property, and the dispersion formed after being dried, then it is mixed with active insecticidal compounds and attractant
It closes, dispersed phase compound is made.Copper-based sterilization component can make insect protein be denaturalized by systemic action, to generate poison
Property, while copper ion can participate in and promote the redox reaction, respiration and photosynthesis of plant, to promote carbon water
The metabolism and synthesis of compound and protein improve chlorophyll stability, greatly enhance plant cold resistance, drought-resistant ability, simultaneously
Since copper ion makes the ability of protein denaturation, so separated copper-based sterilization component and attractant using starch base covering material
It comes.
Protective starch base covering material adds copper-based sterilization component after carrying out Fruit storage again；Above-mentioned vacuum is de-
The vacuum degree of gas is 0.05MPa, time 15min.Starch base covering material is coated on copper-based sterilization component surface, can both hinder
Only copper-based ingredient causes drug effect in storage life to lose to external migration, and surface attractant can be prevented internally to penetrate into and cause
It is rotten, to lose the attracting action to insect, and covering material is that polysaccharide can be quick after by plant or insect adsorption
It decomposes and absorbs, so that sterilization component generation acts on, while covering material has stable physical compatibility activity during storage,
It can safely pack and be used in instant preparation, increase the safety of environment, reduce pest resistance to insecticide, extend compound
Duration of efficacy.
Copper-based sterilization component is after being crystallized in water-soluble chitosan solution by copper sulphate and milk of lime, in colloid mill scale
It is ground under conditions of being 22 and dry obtained.Copper-based sterilization component grain diameter after colloidal film is ground is small, and particle surface is certainly
By that can become larger, particle sinking speed is slower, can have better suspendability and flowing in covering material when being coated
Performance is more advantageous to and is equably wrapped in material.
The weight ratio of copper sulphate and milk of lime is 5:10；The mass concentration of water-soluble chitosan solution is 2%；Needed for crystallization
Temperature is 60 DEG C, time 30min.The copper-based sterilization component that copper sulphate and milk of lime are formed is mainly basic copper sulfate, in water
In be in slightly soluble state, in the environment of chitin exists, crystallize the basic copper sulfate of formation in developmental process, chitin is by hydrogen
Key influences crystal, forms connection between the calcium ion in site, with crystal using the hydroxyl in chitin molecule, induction
Form metastable basic copper sulfate crystal, this metastable state crystal due to thermodynamic instability, be difficult to generate cenotype,
It is less likely to occur agglomeration between crystal fine particle, mobility and suspension can be promoted, simultaneously because metastable state crystal
Specific surface area and surface Gibbs function are all very big, therefore when subsequent cladding, can quickly agglomerate and coat starch-based material, to increase
Add surface area to thereby reduce surface Gibbs function, reach new thermodynamics stable state, is conducive to improve drug in insect bodies
Interior lasting medicine.
Starch base covering material is made by following steps: the starch raw material containing 50wt% amylose being configured to dense
Degree is that the solution of 5% (w/v) after pre-gelatinized under ultrasonic environment, then is placed in after glycerol, succinic acid and ethylene oxide is added
110 DEG C, to obtain the final product, above-mentioned ultrasonic power is 800W to processing 60min under 0.12MPa, pre-gelatinized uses temperature for 95 DEG C of water-bath,
Gelatinization time is 20min, and the additive amount of glycerol, succinic acid and ethylene oxide is respectively the 15% of starch raw material weight, 0.06%
With 0.4%.It is gelatinized in ultrasonic environment, can use the mechanism and cavitation of ultrasonic wave, fill starch molecular chain
Point stretch and interrupt, the hydroxyl in strand is exposed, hydroxyl and hydrophilic carboxyl esterification, substituted starch intramolecular and
Intermolecular hydrogen bond reduces crystal property of the starch molecule in gelatinization, while carboxyl and the ethylene oxide opened by ultrasonic wave
It is connected with hydrogen bond, forms starch matrix gel, the starch film with network structure, this starch are then obtained under high pressure-temperature
Molecule-carboxy-epoxy base network structure has steric restriction effect during starch drying and forming-film, while wherein each
Group institute is electrically charged mutually exclusive, and starch molecular chain is made to participate in rearranging in film forming procedure, forms starch micro-domains and increases,
Micro-domains bulk density increases, and then is improved the mechanical performance, tensile strength and barrier property of coating film, is conducive to pair
The cladding of copper-based ingredient and the infiltration of attractant is obstructed, extend compound pharmaceutical activity and shelf storage life, and after resetting
Starch film is easier to degrade in plant and insect bodies, is beneficial to drug release and absorption.
Embodiment 2:
The weight accounting of the compound for causing insect muscle cramp, each component for including is as follows: active insecticidal compounds
60%, copper-based sterilization component 20%, attractant 10%, starch base covering material 10%, total amount is in terms of 100%.Above-mentioned compound
Insect and its habitat are applied in a manner of continuous or interval, amount of application is 250g/ hectare/time.
A kind of preparation method of the above-mentioned compound for causing insect muscle cramp, the specific steps are as follows:
1) copper sulphate and milk of lime are taken by weight the ratio of 7:10, is separately heated to 70 DEG C, then prepare mass concentration and be
1.3% water-soluble chitosan solution, copper sulphate and milk of lime are successively added in water-soluble chitosan solution, at 70 DEG C
After being sufficiently stirred and crystallizing 20min, crystalline solid is ground under conditions of scale is 25 with colloid mill, then will ground by filtering
The spray drying at 100 DEG C of mill gained is spare to get copper-based sterilization component；
2) starch raw material containing 55wt% amylose is configured to the solution that concentration is 3.5% (w/v), be added sweet
After oil, succinic acid and ethylene oxide, it is gelatinized 20min in the water-bath that ultrasonic power is 1200W, temperature is 95 DEG C, then be placed in
130 DEG C, processing 50min to get starch base coats film liquid under 0.09MPa, spare, above-mentioned glycerol, succinic acid and ethylene oxide
Additive amount is respectively 20%, 0.08% and the 0.3% of starch raw material weight；
3) starch base is coated into film liquid vacuum outgas 10min under conditions of vacuum degree is 0.1Mpa, be then added copper-based
Sterilization component after being sufficiently stirred, is spray-dried to get copper-based sterilization component covering body；
4) copper-based sterilization component covering body is mixed with active insecticidal compounds and attractant, dispersed phase compound is made,
Butanol, vegetable oil, phosphatide, organic solvent or lignosulfonates can also further be added, suspension-type compound is made.
Embodiment 3:
The weight accounting of the compound for causing insect muscle cramp, each component for including is as follows: active insecticidal compounds
45%, copper-based sterilization component 25%, attractant 15%, starch base covering material 15%, total amount is in terms of 100%.Above-mentioned compound
Insect and its habitat are applied in a manner of continuous or interval, amount of application is 450g/ hectare/time.
A kind of preparation method of the above-mentioned compound for causing insect muscle cramp, the specific steps are as follows:
1) copper sulphate and milk of lime are taken by weight the ratio of 6.5:10, is separately heated to 70 DEG C, then prepare mass concentration
For 1% water-soluble chitosan solution, copper sulphate and milk of lime are successively added in water-soluble chitosan solution, at 70 DEG C
After being sufficiently stirred and crystallizing 25min, crystalline solid is ground under conditions of scale is 26 with colloid mill, then will ground by filtering
The spray drying at 120 DEG C of mill gained is spare to get copper-based sterilization component；
2) by the starch raw material containing 70wt% amylose be configured to concentration be 5% (w/v) solution, be added glycerol,
After succinic acid and ethylene oxide, it is 1000W, is gelatinized 30min in water-bath at a temperature of 90 °C in ultrasonic power, then be placed in 120
DEG C, processing 60min to get starch base coats film liquid, spare, the addition of above-mentioned glycerol, succinic acid and ethylene oxide under 0.1MPa
Amount is respectively 17%, 0.13% and the 0.25% of starch raw material weight；
3) starch base is coated into film liquid vacuum outgas 10min under conditions of vacuum degree is 0.09Mpa, be then added copper-based
Sterilization component after being sufficiently stirred, is spray-dried to get copper-based sterilization component covering body；
4) copper-based sterilization component covering body is mixed with active insecticidal compounds and attractant, dispersed phase compound is made.
Embodiment 4:
The present embodiment and embodiment 3 the difference is that: in the preparation method for causing the compound of insect muscle cramp,
Copper sulphate and milk of lime are crystallized without containing chitin, only in the environment containing water in step 1), be made copper-based sterilization at
Point.In other steps and embodiment 3 always, compound dispersed phase is made.
Embodiment 5:
The present embodiment and embodiment 3 the difference is that: in the preparation method for causing the compound of insect muscle cramp,
The water-bath of raw material is gelatinized in the not environment existing for ultrasonic wave and carries out in step 2), and only water-bath is gelatinized under normal conditions, is made
Starch base coats film liquid.In other steps and embodiment 3 always, compound dispersed phase is made.
Embodiment 6:
The present embodiment and embodiment 3 the difference is that: in the preparation method for causing the compound of insect muscle cramp,
Succinic acid and ethylene oxide are not added in step 2) in raw material, only adds glycerol, starch base is made and coats film liquid.Other steps with
In embodiment 3 always, compound dispersed phase is made.
Embodiment 7:
The present embodiment and embodiment 3 the difference is that: in the preparation method for causing the compound of insect muscle cramp,
Succinic acid and ethylene oxide are not added in step 2) in raw material, only adds glycerol；And the water-bath gelatinization of raw material is not deposited in ultrasonic wave
Environment in carry out, only under normal conditions water-bath be gelatinized, be made starch base coat film liquid.In other steps and embodiment 3
Always, compound dispersed phase is made.
Test example 1:
Starch base coating film structural research
Made starch base coats film liquid in Example 3 and 7 respectively, coating film forming and after drying, and carries out electricity to starch film
Scarnning mirror is specifically detailed in Figure of description 1 and 2.
By Fig. 1 and Fig. 2 as it can be seen that made starch film surface irregularity and structure is uneven in embodiment 7, and embodiment 3
In made starch environmental microbes be improved, reveal more compact state, illustrate to prepare starch film mistake in embodiment 3
Starch molecular chain participation rearranges in journey, forms the more smooth uniform starch film in surface, also changes the anti-of starch film
Tensile strength and barrier property.
Test example 2:
Cause the compound performance test of insect muscle cramp
Example 3,4,5,6 and 7 made compound finished products, respectively correspond and are set as test group 1,2,3,4 and 5, with commercially available
Certain brand insecticide is control group, growth of Chinese cabbage area is applied in respectively by identical dosage (200g/ hectare/time), with leaf mustard
Beetle is subjects, after application 45 days, is assessed the crop by insect infestations, while being carried out to remaining drug
Activity determination, as a result such as the following table 1.
Table 1 causes the compound performance test of insect muscle cramp
| It is affected crop % | Invasion beetle number/only | Beetle lethal dose % | Pharmaceutical activity residual quantity % | |
| Test group 1 | 7.5 | 90 | 95.6 | 21.7 |
| Test group 2 | 12.5 | 80 | 92.5 | 18.7 |
| Test group 3 | 16.5 | 80 | 91.3 | 16.3 |
| Test group 4 | 15.8 | 80 | 90.0 | 15.7 |
| Test group 5 | 18.3 | 80 | 87.5 | 16.2 |
| Control group | 23.5 | 90 | 88.9 | 11.8 |
As seen from the above table, test group is average to the lethal dose of beetle 90% or more, and control group effect is slightly poor, causes to compare
Group crop be affected quantity compared with test group height, and control group pharmaceutical activity residual quantity also with test group have notable difference, be by
Slow releasing function of the starch film to pharmaceutical activity in the made compound of test group；In test group, test group 1 shows more other tests
Group is excellent, and difference is unobvious between other test groups, is practical operation difference during the preparation process due to other test groups,
The difference of reagent or mode of operation so that product structure, performance change so that the drug effect of compound finished product discharge,
Vital preservation amount is adversely affected.
The prior art of routine techniques dawn known to those skilled in the art in above-described embodiment, therefore herein no longer in detail
It repeats.
The above embodiments are only used to illustrate the present invention, and not limitation of the present invention, the ordinary skill people of this field
Member can also make a variety of changes and modification without departing from the spirit and scope of the present invention.Therefore, all equivalent
Technical solution also belong to scope of the invention, scope of patent protection of the invention should be defined by the claims.
Claims (9)
1. causing the compound of insect muscle cramp, it is characterised in that: include,
A, at least one active insecticidal compounds, the active insecticidal compounds can cause insect muscle cramp and lead to death；
B, at least one copper-based sterilization component, the copper-based sterilization component have stomach poison function；
C, at least one attractant, the attractant are containing plant protein hydrolysate or animal hydrolyzed protein or higher fatty acids or sugar
Lure auxiliary material；
D, at least one starch base covering material.
2. the compound according to claim 1 for causing insect muscle cramp, it is characterised in that: the compound includes
The weight accounting of each component is as follows: active insecticidal compounds 20~60%, copper-based sterilization component 20~40%, and attractant 10~
20%, starch base covering material 10~20%, total amount is in terms of 100%.
3. a kind of preparation method for the compound for causing insect muscle cramp as claimed in claim 1 or 2, it is characterised in that:
Disperse copper-based sterilization component in protective starch base covering material, and the dispersion formed after being dried, then with work
Property Pesticidal compound and attractant mixing, dispersed phase compound is made.
4. a kind of preparation method of compound for causing insect muscle cramp according to claim 3, it is characterised in that: institute
It states after protective starch base covering material carries out Fruit storage and adds copper-based sterilization component again；The vacuum outgas it is true
Reciprocal of duty cycle is 0.05~0.1MPa, and the time is 10~15min.
5. a kind of preparation method of compound for causing insect muscle cramp according to claim 3, it is characterised in that: institute
Stating copper-based sterilization component is after being crystallized in water-soluble chitosan solution by copper sulphate and milk of lime, colloid mill scale be 22~
It is ground under conditions of 27 and dry obtained.
6. a kind of preparation method of compound for causing insect muscle cramp according to claim 5, it is characterised in that: institute
The weight ratio for stating copper sulphate and milk of lime is 5~7:10；The mass concentration of the water-soluble chitosan solution is 0.5~2%；Institute
Stating crystallization required temperature is 60~80 DEG C, and the time is 20~30min.
7. a kind of preparation method of compound for causing insect muscle cramp according to claim 3, it is characterised in that: institute
It states starch base covering material to be made by following steps: the starch raw material containing 50~70wt% amylose is configured to concentration
It after pre-gelatinized under ultrasonic environment, then is placed in after glycerol, succinic acid and ethylene oxide is added for the solution of 3~5% (w/v)
110~130 DEG C, 40~60min of processing under 0.09~0.12MPa to obtain the final product.
8. a kind of preparation method of compound for causing insect muscle cramp according to claim 7, it is characterised in that: institute
The additive amount for stating glycerol, succinic acid and ethylene oxide is respectively 15~20%, 0.06~0.15% and the 0.2 of starch raw material weight
~0.4%.
9. a kind of preparation method of compound for causing insect muscle cramp according to claim 7, it is characterised in that: institute
Stating ultrasonic power is 800~1200W, and the pre-gelatinized use temperature for 80~95 DEG C of water-bath, gelatinization time for 20~
30min。
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