CN108184833A - Pyrethrins microcapsule formulations with beta-cyclodextrin or derivatives thereof for wall material and its preparation method and application - Google Patents
Pyrethrins microcapsule formulations with beta-cyclodextrin or derivatives thereof for wall material and its preparation method and application Download PDFInfo
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- CN108184833A CN108184833A CN201711428891.0A CN201711428891A CN108184833A CN 108184833 A CN108184833 A CN 108184833A CN 201711428891 A CN201711428891 A CN 201711428891A CN 108184833 A CN108184833 A CN 108184833A
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- cyclodextrin
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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
- A01N25/26—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 in coated particulate form
- A01N25/28—Microcapsules or nanocapsules
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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
- A01N53/00—Biocides, pest repellants or attractants, or plant growth regulators containing cyclopropane carboxylic acids or derivatives thereof
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Abstract
The present invention provides pyrethrins microcapsule formulations with beta cyclodextrin or derivatives thereof for wall material and its preparation method and application, belong to technical field of insecticide.The microcapsule formulations are made of wall material and the core material being wrapped in wall material；The raw material of core material includes natural pyrethrin and solvent, and the quality of the natural pyrethrin and the volume ratio of solvent are（1~5）g：（5~25）mL；The solvent is aqueous dispersant or ethyl alcohol；The raw material of wall material is beta cyclodextrin or the derivative and water of beta cyclodextrin；The volume ratio of the quality and water of the beta cyclodextrin or beta cyclodextrin derivative is（9~15）g：（50~100）mL.The derivative of beta cyclodextrin or beta cyclodextrin is coated natural pyrethrin core material by the preparation method of desinsection microcapsule formulations using envelope combined techniques, liquid pesticide microencapsulation can be achieved, active ingredient sustained releaseization, have the characteristics that it is anti-decompose, efficiently, low toxicity, it is safe, available for driving away and killing mosquito etc..
Description
Technical field
The invention belongs to technical field of insecticide, and in particular to the pyrethrins with beta-cyclodextrin or derivatives thereof for wall material
Microcapsule formulations and its preparation method and application.
Background technology
China is large agricultural country, while is also pesticide producing and uses big country.The a large amount of of pesticide are used to ensure agricultural product
Supply is made that significant contribution.However, pesticide is a handle " double-edged sword ".Pesticide exposure during Pesticide use makes the producer long
Phase exposed to pesticides may result in acute poisoning, and the part pesticide active chemical that can cause to be difficult to decompose is in agricultural product
In aggregation, form serious Pesticide Residue.Pesticide Residue not only jeopardizes the health of the domestic common people, can also produce
The raw worry to agricultural product security problem and fear.It is reported that due to the food of edible pollution by pesticides pesticide occurs for China every year
Average annual nearly 200,000 people of the number of poisoning, accounts for about the 1/3 of food poisoning total number of persons.In carcinogenic factor, pesticide factor accounts for about 60%
Proportion.More than 90% pesticide is to enter human body by food chain, and only 10% is by air and drinking water.Pesticide product
Kind, access times and usage amount are to influence the principal element of pesticide residue.
Pyrethrins is a kind of to knock down that fast, insecticidal power is strong, wide spectrum, low toxicity, low-residual insecticide.There is broad spectrum activity simultaneously
It is pesticidal, the favourable agents of the sanitary insect pests such as prevention mosquito, fly, lice, flea are not only, to more than 40 evils belonged to of 200 various plants
Worm also has good control effect, such as leafhopper, beetle, lepidopterous larvae.Existing pyrethrins dosage form is mainly that missible oil is gentle
Mist agent although contact efficacy is preferable, can reach 99%, have the following disadvantages：Containing a large amount of organic solvent, such as just oneself
Alkane, discharge not only cause the wasting of resources, but also serious pollution of ecological environment；Easily by daylight, air, higher temperature and metal
Ion dissociation, wherein the decomposition with ultraviolet light is most strong, the lasting period is short.Therefore, to reach high during practical application desinsection
Imitating insecticidal effect needs dispenser repeatedly, cause to take a lot of work, be time-consuming, expense medicine the problems such as.
Invention content
In view of this, the purpose of the present invention is to provide the micro- glue of pyrethrins with beta-cyclodextrin or derivatives thereof for wall material
Wafer and its preparation method and application, the microcapsule formulations avoid using organic solvent, environmentally friendly, and with efficiently and long
Imitate the effect of desinsection.
In order to achieve the above-mentioned object of the invention, the present invention provides following technical scheme：
The present invention provides the pyrethrins microcapsule formulations with beta-cyclodextrin or derivatives thereof for wall material, by wall material and are wrapped in wall
The volume ratio of core material composition in material, the core material and wall material is 1：2.5~20；The raw material of core material include natural pyrethrin and
Solvent, the quality of the natural pyrethrin and the volume ratio of solvent are（1~5）g：（5~25）mL；The solvent is dispersant water
Solution or ethyl alcohol；
The raw material of wall material is one kind and water at least in the derivative of beta-cyclodextrin or beta-cyclodextrin；The beta-cyclodextrin or β-
The quality of the derivative of cyclodextrin and the volume ratio of water are（9~15）g：（50~100）mL.
Preferably, when the solvent of core material is ethyl alcohol, the raw material of wall material is beta-cyclodextrin derivative and water；It is molten when core material
When agent is aqueous dispersant, the raw material of wall material is beta-cyclodextrin and water；The beta-cyclodextrin derivative include methyl flamprop,
Ethyl cyclodextrin, hydroxypropyl cyclodextrin or one kind in sulphur butyl cyclodextrin and several.
Preferably, the quality of the beta-cyclodextrin derivative and the volume ratio of water are（1~2）g：（10~20）mL；β-ring paste
The quality of essence and the volume ratio of water are（1~5）g：（10~20）mL.
Preferably, the quality of the natural pyrethrin and the volume ratio of dispersant are（2~4）g：（8~15）mL.
Preferably, the dispersant in the aqueous dispersant include sodium lignin sulfonate or one kind in Arabic gum or
Two kinds.
The present invention provides the preparation methods of the pyrethrins microcapsule formulations, include the following steps：
（1）Natural pyrethrin and aqueous dispersant or ethyl alcohol are mixed into 5 ~ 30 min, obtain natural pyrethrin dispersant
Aqueous solution or natural pyrethrin ethanol solution；
（2）The derivative and water of beta-cyclodextrin or beta-cyclodextrin are mixed, the water-bath under the conditions of 50 ~ 80 DEG C, obtain β-ring paste
The derivative solution of smart solution or beta-cyclodextrin；
（3）By the step（1）In obtained natural pyrethrin aqueous dispersant be added to the step（2）In obtain
In beta-cyclodextrin solution or by the step（1）In obtained natural pyrethrin ethanol solution be added to the step 2）
In in the obtained derivative solution of beta-cyclodextrin, form mixture, by being ultrasonically treated, separation of solid and liquid obtains pyrethrins
Microcapsule formulations.
Wherein described step（1）And step（2）Between there is no the limitation of time sequencing.
Preferably, step（3）Described in the supersonic frequency that is ultrasonically treated be 20KHz ~ 40KHz；The time of supersound process is
30~60min；The temperature of supersound process is 20 DEG C ~ 30 DEG C.
Preferably, step（3）Described in further include drying after separation of solid and liquid；The temperature of the drying is 50 ~ 60 DEG C.
The present invention also provides pyrethrins microcapsules prepared by the pyrethrins microcapsule formulations or the method
Application of the agent in pest control.
Preferably, it is one or more of to include sanitary insect pest, parazoon or agricultural pests for the pest；The health evil
It is one or more of that worm includes mosquito, fly, cockroach or ant；The parazoon includes louse or flea；The agricultural evil
It is one or more of that worm includes Asiatic migrotory locust, Chinese rice grasshopper or Oriental burmeister.
The beneficial effects of the present invention are：
The present invention provides the pyrethrins microcapsule formulations with beta-cyclodextrin or derivatives thereof for wall material, by wall material and are wrapped in wall
The volume ratio of core material composition in material, the core material and wall material is 1：2.5~20；The raw material of core material include natural pyrethrin and
Solvent, the quality of the natural pyrethrin and the volume ratio of solvent are（1~5）g：（5~25）mL；The solvent is dispersant water
Solution or ethyl alcohol；The raw material of wall material is beta-cyclodextrin or the derivative and water of beta-cyclodextrin；The beta-cyclodextrin or β-ring
The quality of the derivative of dextrin and the volume ratio of water are（9~15）g：（50~100）mL.With beta-cyclodextrin and its derivative in the present invention
Object is aggregated into as wall material, beta-cyclodextrin by 7 glucosylation units with α -1,4 glycosidic bonds, and intramolecule is in " V " word for one
The hydrophobic cavities of type.Hydrophobic centers add object to form inclusion network and object, and object hydrophobicity is stronger, forms the ability of inclusion complex
It is stronger.By the use of beta-cyclodextrin and its derivative as wall material natural pyrethrin microencapsulation, can avoid using organic solvent,
Cost is reduced, is reduced environmental pollution；Liquid pesticide microencapsulation can effectively prevent decomposing, and reduce pesticide and be lost in and decompose, improve
The stability of pesticide, and make it have sustained release, ultra high efficiency, it is nontoxic, economical, safe the characteristics of, be a kind of environmentally friendly preparation.
Meanwhile solid, liquid pesticidal isoreactivity substance are coated on shape in cyst material by the present invention using microcapsules technology
Into small cryptomere preparation, the defects of liquid pesticide solidification can be made, be readily transported and stored, overcome present in conventional formulation.
Description of the drawings
Fig. 1 is the natural pyrethrin microcapsules scanning electron microscope (SEM) photograph being prepared in embodiment 1；
Fig. 2 is the sustained release situation for measuring microcapsule formulations in embodiment 7 using the method for constant temperature thermal weight loss.
Specific embodiment
The present invention provides the pyrethrins microcapsule formulations with beta-cyclodextrin or derivatives thereof for wall material, by wall material and package
The volume ratio of core material composition in wall material, the core material and wall material is 1：2.5~20；The raw material of core material includes pyrethrum
Ester and solvent, the quality of the natural pyrethrin and the volume ratio of solvent are（1~5）g：（5~25）mL；The solvent is dispersion
Agent aqueous solution or ethyl alcohol；
The raw material of wall material is one kind and water at least in the derivative of beta-cyclodextrin or beta-cyclodextrin；The beta-cyclodextrin or
The quality of the derivative of beta-cyclodextrin and the volume ratio of water are（9~15）g：（50~100）mL.
Preferably, the raw material of wall material is beta-cyclodextrin derivative and water when the solvent of core material is ethyl alcohol；The solvent of core material is
The raw material of wall material is beta-cyclodextrin and water during aqueous dispersant；The beta-cyclodextrin derivative includes methyl flamprop, ethyl
Cyclodextrin, hydroxypropyl cyclodextrin and one kind in sulphur butyl cyclodextrin and several.
In the present invention, the mass ratio of the wall material and core material is 1：2.5 ~ 20, preferably 1：4 ~ 15, more preferably 1:5 ~ 8,
Most preferably 1:6.
In the present invention, the raw material of core material includes natural pyrethrin and solvent.The quality of the natural pyrethrin and molten
The volume ratio of agent is（1~5）g：（5~25）mL；The solvent is aqueous dispersant or ethyl alcohol.
In the present invention, when the solvent of core material is aqueous dispersant, the raw material of wall material is beta-cyclodextrin and water.Beta-cyclodextrin
Quality and the volume ratio of water be preferably（1~5）g：（10~20）ML, more preferably 3g：（10~20）ML, most preferably 1g：
10mL.The quality of the natural pyrethrin and the volume ratio of aqueous dispersant are preferably（2~4）g：（8~15）ML, more preferably
It is 1：5.The mass concentration of the aqueous dispersant is preferably 10% ~ 50%；More preferably 15%.In the present invention, the dispersant
Preferably one or both of sodium lignin sulfonate and Arabic gum.When the dispersant is two kinds, the lignin sulfonic acid
The mass ratio of sodium and Arabic gum is preferably 1 ~ 6:1, more preferably 2 ~ 4:1.The dispersant uniformly dispersing can naturally remove
Worm chrysanthemum ester liquid, is embedded convenient for subsequent step.In the present invention, the source of the dispersant is not particularly limited, using this
Dispersant known to field technology personnel.In the embodiment of the present invention, the source of the dispersant is purchased from Chinese medicines group
Learn reagent Co., Ltd.The source of the dispersant is not particularly limited, and is using dispersion well-known to those skilled in the art
It can.In the embodiment of the present invention, dispersant is purchased from as Sinopharm Chemical Reagent Co., Ltd..
In the present invention, when the solvent of core material is ethyl alcohol, the raw material of wall material is preferably beta-cyclodextrin derivative and water；The β-
Cyclodextrine derivatives include methyl flamprop, ethyl cyclodextrin, hydroxypropyl cyclodextrin and one kind in sulphur butyl cyclodextrin and several
Kind.The quality of the beta-cyclodextrin derivative and the volume ratio of water are preferably（1~2）g：（10~20）ML, more preferably 1g：
10mL.The quality of the natural pyrethrin and the volume ratio of ethyl alcohol are preferably（0.6~1）g：（6~15）ML, more preferably 1g：
10mL。
In the present invention, the natural pyrethrin is by pyrethrins I, pyrethrins II, cineraria ester I, cineraria ester II
With 6 kinds of insecticidal active ingredient compositions of jasmolin I and II grade of jasmolin.It is counted using natural pyrethrin as 100%, pyrethrins 1
It is 36.99%, pyrethrins II is 22.56.The source of the natural pyrethrin is not particularly limited, using art technology
Natural pyrethrin known to personnel.In the embodiment of the present invention, the source of the natural pyrethrin is Honghe, Yunnan
Sen Ju Co., Ltds.
The present invention also provides the preparation methods of the desinsection microcapsule formulations, include the following steps：
1）Natural pyrethrin and aqueous dispersant or ethyl alcohol are mixed into 5 ~ 30 min, obtain natural pyrethrin dispersant water
Solution or natural pyrethrin ethanol solution；
2）The derivative and water of beta-cyclodextrin or beta-cyclodextrin are mixed, the water-bath under the conditions of 50 ~ 80 DEG C obtains beta-cyclodextrin
The derivative solution of solution or beta-cyclodextrin；
3）By the step 1）In obtained natural pyrethrin aqueous dispersant add in the step 2）In obtained β-ring
In dextrin solution or by the step 1）In obtained natural pyrethrin ethanol solution add in the step 2）In obtain
In the derivative solution of beta-cyclodextrin, mixture is formed, by being ultrasonically treated, separation of solid and liquid obtains desinsection microcapsule formulations.
Wherein described step 1）With step 2）Between there is no the limitation of time sequencing.
Natural pyrethrin and aqueous dispersant or ethyl alcohol are mixed 5 ~ 30 min by the present invention, obtain natural pyrethrin
Dispersant solution or natural pyrethrin ethanol solution.
In the present invention, the method for the mixing is not particularly limited, using mixing side well-known to those skilled in the art
Method.
In the present invention, the time of the mixing is preferably 10 ~ 20 min, more preferably 15min.
The present invention mixes the derivative and water of beta-cyclodextrin or beta-cyclodextrin, and the water-bath under the conditions of 50 ~ 80 DEG C obtains
The derivative solution of beta-cyclodextrin solution or beta-cyclodextrin.
In the present invention, the method for the mixing is not particularly limited, using mixing side well-known to those skilled in the art
Method.The temperature of the water-bath is preferably 55 ~ 70 DEG C, more preferably 60 DEG C.
In the present invention, the water-bath process is preferably stirred.In the present invention, the method for the stirring does not have special limit
System, using stirring means well-known to those skilled in the art.The rotating speed of the stirring is preferably 500 ~ 1500rpm, more
Preferably 600 ~ 900rpm.It preferably includes to stand cooling after the water-bath.The time for standing cooling is 1 ~ 4h, more excellent
It is selected as 1 ~ 2h.
Obtain natural pyrethrin dispersant solution or natural pyrethrin ethanol solution and beta-cyclodextrin solution or β-
After the derivative solution of cyclodextrin, the natural pyrethrin dispersant solution is added in the beta-cyclodextrin solution by the present invention
In or the natural pyrethrin ethanol solution added in the derivative solution of the beta-cyclodextrin, form mixture, warp
Supersound process is crossed, separation of solid and liquid obtains desinsection microcapsule formulations.
In the present invention, the supersonic frequency of the supersound process is preferably 20KHz ~ 40KHz, more preferably 30KHz；At ultrasound
The time of reason is preferably 30 ~ 60min, more preferably 40min；The temperature of supersound process is preferably 20 ~ 30 DEG C, more preferably 25
℃。
In the present invention, the preferred vacuum filter of separation of solid and liquid.The method of the vacuum filter is not particularly limited, and is used
The method of vacuum filter well-known to those skilled in the art.
In the present invention, drying is further included after the separation of solid and liquid；The temperature of the drying is preferably 50 ~ 60 DEG C, more preferably
It is 55 DEG C.
The present invention provides the desinsection microcapsule formulations or the desinsection microcapsule formulations of the method preparation in pest control
In application.
In the present invention, the pest preferably includes sanitary insect pest, parazoon and agricultural pests；The sanitary insect pest is excellent
Choosing includes mosquito, fly, cockroach or ant；The parazoon preferably includes louse or flea；Agricultural pests preferably include
Asiatic migrotory locust, Chinese rice grasshopper or Oriental burmeister.
Water is added to be modulated into the lotion of a concentration of 50ppm microcapsules prepared by said program, using spray-on process（Pressure atomization
Method, vapodusting）Directly sprayed.The amount of application of the microcapsule formulations is 50 kgs/acre.Preferably occur using opportunity in adult
Preceding medication.The frequency of application is 12 ~ 17d.Requirement is uniformly thoughtful during spray, accomplishes that blade back, blade face and polypide are all stained with liquid.
With reference to embodiment to pyrethrins micro- glue provided by the invention with beta-cyclodextrin or derivatives thereof for wall material
Wafer and its preparation method and application is described in detail, but they cannot be interpreted as the limit to the scope of the present invention
It is fixed.
Embodiment 1
Prepare microcapsules：
1st, it is accurate to weigh 1 g natural pyrethrin samples, the dissolving of 5 ml ethyl alcohol is added in, obtains solution A；
2nd, 9 g of beta-cyclodextrin is weighed, adds in 100 g of distilled water, 80 DEG C of stirring in water bath, then dissolving stands, is cooled to room
Temperature is for use to get B；
3rd, above-mentioned solution A is added in B, embedding is completed after 20 min of ultrasound, filtered, be freeze-dried under low-temperature condition to obtain the final product
Natural pyrethrin microcapsules.
The microcapsule formulations of preparation under electron microscopic are observed, are taken pictures, shown in the result is shown in Figure 1.It can be seen by Fig. 1
Go out, the smooth near-rhombic structure in surface.
Embodiment 2
Prepare microcapsules：
1st, it is accurate to weigh 1 .2 g natural pyrethrin samples, it adds in 12 ml Qulas and leads to op-10 dissolvings, obtain solution E；
2nd, 8.8 g of beta-cyclodextrin derivative is weighed, adds in 88 g of distilled water, 80 DEG C of water-baths, stirring, then dissolving stands, is cold
But to room temperature for use to get F；
3rd, above-mentioned E solution is added in F, 55 DEG C of 4 h of stirring in water bath, then 43 DEG C of 16 h of heat preservation, vacuum filter are dried at room temperature
24 h, 50 DEG C of 24 h of oven drying are to get natural pyrethrin microcapsules.
Embodiment 3
Microcapsules are to 4 instar larvae toxicity test of Culex pipiens pallens and aedes albopictus
With gained microcapsule formulations to Culex pipiens pallens (Culexpipienspallens) and aedes albopictus (Aedesalbopictus)
4 instar larvaes carry out toxotest, and used test method is larva infusion process.The liquid of the configured good various concentrations of 1mL is taken to add
In the beaker for entering to fill 149mL dechlorination tap water, stirred with glass bar.30 larvas chosen in advance in another cup together with
50mL water is all injected in above-mentioned beaker, altogether 200mL.With 1mL coordinative solvents（Acetone）It handles as control group.Postscript for 24 hours
The death toll of test worm is recorded, experiment is repeated 3 times.Experimental result is listed in the table below.
Table 1 is to the toxicity test of culex pipiens pallens larvae
Table 2 is to the toxicity test of Aedes Albopictus Larva
The above results show that gained microcapsule formulations of the invention are respectively provided with the larva of 2 kinds of mosquitoes high bioactivity.To light color library
Mosquito and the LC of aedes albopictus50Respectively 0.77 ppm and 1.81 ppm；LC90Respectively 2.63 ppm and 3.73 ppm values.Ginseng
Examine Cheng, et al. (2003) http://www.sciencedirect.com/science/article/pii/
The evaluation criterion of S0960852403000087：LC50>100 μ g/mL are inactive；50 μg/mL <LC50< 100 μg/mL
It is active；LC50<50 μ g/mL are high activity.
Embodiment 4
Microcapsules test striped rice borer insecticidal activity
Microcapsules water dissolution prepared by the embodiment 2 of 10mg is weighed, is configured to the mother liquor of 500ppm.Mother liquor is diluted with water to obtain the final product
To required concentration liquid.Each 3 repetitions of processing, if blank control；Ready-made rice seedling and 10 Chilo spp larvaes are existed
It is impregnated 5 seconds in liquid, is put into culture dish after taking out naturally dry, is enclosed in container.Investigation for 24 hours after as a result, check anyway
Borer population, and it is for statistical analysis.Experimental result is listed in the table below：
Using Biological Statistic Analysis Software, the statistical data such as LC50 are calculated, concrete outcome is as follows：
The Toxicity baseline statistics of 24 hours after 4 medicine of table
The above results show that gained microcapsule formulations insecticidal activity of the invention is high, can be used alone when preventing striped rice borer, due to
Its act on it is quick, when in use between aspect have to, in egg hatching peak medication, drug effect just be played when larvas endanger.
Embodiment 5
Microcapsules provided by the invention test aphid insecticidal activity
1. microcapsules insecticidal activity is tested：Using leaching worm leaf dipping method：Microcapsules prepared by the embodiment 1 of 10mg are weighed with water-soluble
Solution, is configured to the mother liquor of 500ppm, and mother liquor, which is diluted with water, obtains required concentration liquid, 3 repetitions is each handled, if water purification is empty
White control；Ready-made Vicia faba seedling and 30 or so black bean aphid larvae aphids being attached on seedling in liquid are impregnated 5 seconds together, taken out
Bean seedlings are inserted on the sponge of immersion after naturally dry, glass tube on cover, it is normal to cultivate.Investigation 24 hours as a result, checking dead
Borer population living, and it is for statistical analysis.Experimental result is listed in the table below：
5 medicine of the table death rate % of 24 hours
Using Biological Statistic Analysis Software, the statistical data such as LC50 are calculated, concrete outcome is as follows：
The Toxicity baseline statistics of 24 hours after 6 medicine of table
Embodiment 6
Microcapsules provided by the invention test mythimna separata insecticidal activity
1. microcapsules insecticidal activity is tested：
It weighs microcapsules water dissolution prepared by the embodiment 2 of 10mg, is configured to the mother liquor of 500ppm, mother liquor is diluted with water to obtain the final product
To required concentration liquid, 3 repetitions are each handled, if blank control.Ready-made fresh corn leaf section is impregnated 10 in liquid
Second, take out naturally dry；Several pieces blades are put in each culture dish, while access 10 3 instar larvaes, are enclosed in container.Investigation
For 24 hours as a result, check life or death borer population, it is and for statistical analysis.Experimental result is listed in the table below 3：
The 7 medicine death rate of 24 hours of table
Using Biological Statistic Analysis Software, the statistical data such as LC50 are calculated, concrete outcome is as follows：
The Toxicity baseline statistics of 24 hours after 8 medicine of table
The above results show that gained microcapsule formulations insecticidal activity of the invention is high, can be used alone when preventing mythimna separata, due to it
Effect is quick, when in use between aspect have to, in egg hatching peak medication, drug effect just be played when larvas endanger.
2. conventional pyrethrins missible oil（Comparative example 1）Mythimna separata insecticidal activity is tested
Using leaf dipping method：By diluted water dissolution of the 1% pyrethrins missible oil containing a ten thousandth emulsifier of ethyl alcohol, it is configured to
The mother liquor of 1000ppm.Mother liquor obtains required concentration liquid with the water dilution containing a ten thousandth emulsifier, each to handle 3 times
It repeats, if with the water blank control containing a ten thousandth emulsifier；Ready-made fresh corn leaf section is impregnated 10 seconds in liquid,
Take out naturally dry；Several pieces blades are put in each culture dish, while access 10 3 instar larvaes, are enclosed in container.Investigation is for 24 hours
As a result, check life or death borer population, it is and for statistical analysis.Experimental result is listed in the table below：
9 medicine of the table death rate % of 24 hours
Using Biological Statistic Analysis Software, the statistical data such as LC50 are calculated, concrete outcome is as shown in table 8.
The Toxicity baseline statistics of 24 hours after 10 medicine of table
The above results show that present invention gained microcapsule formulations insecticidal activity is high, can prevent compared to conventional pyrethrins missible oil
It is used alone during black bean aphid.
Embodiment 7
The sustained release performance of beta-cyclodextrin microcapsules prepared by embodiment 1, specific measure side are measured using the method for constant temperature thermal weight loss
Method is：It is dried 1 h by precise and the microcapsules for recording a certain amount of drying at 70 DEG C, and precise simultaneously records knot
Then it is dried 1 h by fruit at 70 DEG C again, precise simultaneously records, so repeatedly until microcapsules constant weight.More than
Method measures constant temperature heating weightless test, and the results are shown in Figure 2.
After heating 16 times, the rate of release of microcapsules has reached stabilization.And initial stage rate of release is very fast, as 3#,
4#, 7# and 8#, after heating 12 times, rate of release reaches a stable level, and burst size is more steady.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (10)
1. the pyrethrins microcapsule formulations with beta-cyclodextrin or derivatives thereof for wall material, it is characterised in that by wall material and be wrapped in wall
The volume ratio of core material composition in material, the core material and wall material is 1：2.5~20；The raw material of core material include natural pyrethrin and
Solvent, the quality of the natural pyrethrin and the volume ratio of solvent are（1~5）g：（5~25）mL；The solvent is dispersant water
Solution or ethyl alcohol；
The raw material of wall material is one kind and water at least in the derivative of beta-cyclodextrin or beta-cyclodextrin；The beta-cyclodextrin or β-
The quality of the derivative of cyclodextrin and the volume ratio of water are（9~15）g：（50~100）mL.
2. pyrethrins microcapsule formulations according to claim 1, which is characterized in that when the solvent of core material is ethyl alcohol, wall
The raw material of material is beta-cyclodextrin derivative and water；When the solvent of core material is aqueous dispersant, the raw material of wall material is β-ring paste
Essence and water；The beta-cyclodextrin derivative includes methyl flamprop, ethyl cyclodextrin, hydroxypropyl cyclodextrin or sulphur butyl cyclodextrin
In one kind and it is several.
3. pyrethrins microcapsule formulations according to claim 2, which is characterized in that the quality of the beta-cyclodextrin derivative
Volume ratio with water is（1~2）g：（10~20）mL；The quality of beta-cyclodextrin and the volume ratio of water are（1~5）g：（10~20）mL.
4. pyrethrins microcapsule formulations according to claim 1, which is characterized in that the quality of the natural pyrethrin and
The volume ratio of aqueous dispersant is（2~4）g：（8~15）mL.
5. the pyrethrins microcapsule formulations according to claim 1 or 4, which is characterized in that in the aqueous dispersant
Dispersant includes one or both of sodium lignin sulfonate or Arabic gum.
6. the preparation method of the pyrethrins microcapsule formulations described in claim 1 ~ 5 any one, which is characterized in that including following
Step：
（1）Natural pyrethrin and aqueous dispersant or ethyl alcohol are mixed into 5 ~ 30 min, obtain natural pyrethrin dispersant
Aqueous solution or natural pyrethrin ethanol solution；
（2）One kind in the derivative of beta-cyclodextrin or beta-cyclodextrin and water are mixed, the water-bath under the conditions of 50 ~ 80 DEG C obtains
To beta-cyclodextrin solution or the derivative solution of beta-cyclodextrin；
（3）By the step（1）In obtained natural pyrethrin aqueous dispersant be added to the step（2）In obtain
In beta-cyclodextrin solution or by the step（1）In obtained natural pyrethrin ethanol solution be added to the step（2）
In in the obtained derivative solution of beta-cyclodextrin, form mixture, by being ultrasonically treated, separation of solid and liquid obtains pyrethrins
Microcapsule formulations；
Wherein described step（1）And step（2）Between there is no the limitation of time sequencing.
7. preparation method according to claim 6, which is characterized in that step（3）Described in be ultrasonically treated when supersonic frequency
For 20KHz ~ 40KHz；The time of supersound process is 30min ~ 60min；The temperature of supersound process is 20 DEG C ~ 30 DEG C.
8. preparation method according to claim 6, which is characterized in that step（3）Described in further include after separation of solid and liquid it is dry
It is dry；The temperature of the drying is 50 ~ 60 DEG C.
9. the side described in pyrethrins microcapsule formulations or claim 6 ~ 8 any one described in claim 1 ~ 5 any one
The application of pyrethrins microcapsule formulations prepared by method in pest control.
10. application according to claim 9, which is characterized in that the pest includes sanitary insect pest, parazoon or agriculture
It is one or more in industry pest；The sanitary insect pest includes one or more in mosquito, fly, cockroach or ant；The animal
Parasite includes louse or flea；The agricultural pests include one or more in Asiatic migrotory locust, Chinese rice grasshopper or Oriental burmeister.
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| CN201711428891.0A CN108184833A (en) | 2017-12-26 | 2017-12-26 | Pyrethrins microcapsule formulations with beta-cyclodextrin or derivatives thereof for wall material and its preparation method and application |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711428891.0A CN108184833A (en) | 2017-12-26 | 2017-12-26 | Pyrethrins microcapsule formulations with beta-cyclodextrin or derivatives thereof for wall material and its preparation method and application |
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| CN110591167A (en) * | 2019-09-16 | 2019-12-20 | 浙江大学 | Degradable mulching film for continuously preventing and treating soybean root rot and preparation method thereof |
| CN111165507A (en) * | 2020-02-08 | 2020-05-19 | 盐城工学院 | Self-heating mosquito repelling and killing tablet |
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| CN110591167A (en) * | 2019-09-16 | 2019-12-20 | 浙江大学 | Degradable mulching film for continuously preventing and treating soybean root rot and preparation method thereof |
| CN111165507A (en) * | 2020-02-08 | 2020-05-19 | 盐城工学院 | Self-heating mosquito repelling and killing tablet |
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Application publication date: 20180622 |