CN108739803A - A kind of short-chain amylose nanometer Prochloraz pesticide and preparation method thereof - Google Patents
A kind of short-chain amylose nanometer Prochloraz pesticide and preparation method thereof Download PDFInfo
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- CN108739803A CN108739803A CN201810681518.4A CN201810681518A CN108739803A CN 108739803 A CN108739803 A CN 108739803A CN 201810681518 A CN201810681518 A CN 201810681518A CN 108739803 A CN108739803 A CN 108739803A
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- Prior art keywords
- short
- prochloraz
- pesticide
- chain amylose
- nanometer
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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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
- A01N25/10—Macromolecular compounds
-
- 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
- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
- A01N47/28—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N<
- A01N47/38—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N< containing the group >N—CO—N< where at least one nitrogen atom is part of a heterocyclic ring; Thio analogues thereof
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/04—Polysaccharides, i.e. compounds containing more than five saccharide radicals attached to each other by glycosidic bonds
Abstract
The invention discloses a kind of short-chain amylose nanometer Prochloraz pesticide and preparation method thereof, the method includes：Short-chain amylose nanometer Prochloraz pesticide is made by enzyme solution shearing, sonic oscillation and magnetic agitation in starch.Preparation method of the present invention is simple, and raw material are easy to get, and pollution is small, at low cost.The short chain nanometer Prochloraz pesticide is biodegradable, and residual risk is small, and its grain size is smaller, it is distributed uniform, strong adhesive force is not easy to tumble and be fallen by rain drop erosion, and permeability is preferable, there is certain slow releasing function, the lasting period for extending pesticide, the utilization rate of pesticide is improved, being compatible with the environment property is good, meet environment friendly agricultural theory, achieves significant using effect.
Description
Technical field
The present invention relates to a kind of pesticides more particularly to a kind of short-chain amylose nanometer Prochloraz pesticide and preparation method thereof, belong to
In technical field of pesticide.
Background technology
Prochloraz is broad-spectrum germicide.It is to inhibit ergosterol biosynthesis, has protection and eradicant action, to more
Kind crop sac fungus and Fungi Imperfecti disease have notable preventive effect.It can be used for preventing cereal crop stem, leaf, many diseases on fringe,
Such as powdery mildew, leaf spot；This product can be used for many pathogens of fruit tree, vegetables, mushroom, turf and ornamental plant.And this
Invention is mainly used for the prevention of the leaf blight of corn.
The dosage form of the Prochloraz of country's registration is mostly aqueous emulsion and missible oil, and minority is suspending agent and wettable powder.These
Some organic solvents and surfactant harmful to environment can be all more or less added in process in dosage form.With society
The development of meeting, people increasingly pay attention to the protection to environment, and the formulations of pesticide develop towards environmentally protective direction, this is to need at present
Technical problems to be solved.
Invention content
The technical problem to be solved by the present invention is to：A kind of short-chain amylose nanometer Prochloraz pesticide and preparation method thereof is provided,
The nano pesticide dosage form of high dispersive is prepared using biodegradable material, it is at low cost, it is environmentally protective, it can prepare the lasting period
Long, bioavilability is high, remains low Pesticidal products, and to promoting pesticide reduction to use, agriculture sustainable development has important
Meaning, the above-mentioned problem of effective solution.
The technical scheme is that：A kind of short-chain amylose nanometer Prochloraz pesticide, the short-chain amylose nanometer Prochloraz
Pesticide includes：Short-chain amylose and Prochloraz, mass percent are：Short-chain amylose 50%-80%, Prochloraz 20%-50%.
A kind of preparation method of short-chain amylose nanometer Prochloraz pesticide, the method step are：
One, short-chain amylose is produced；
Two, it weighs short-chain amylose and is add to deionized water and short-chain amylose liquid, autoclave sterilization is made；
Three, gained short-chain amylose liquid is subjected to water-bath balance, places into ultrasonic machine and carry out ultrasound, completes dissolving, obtain short
Chain starch solution；
Four, hot acetate dissolution is added in Prochloraz pesticide, then the short-chain amylose solution obtained by step 3 is added drop-wise to dissolving
In the Prochloraz pesticide of completion, and pesticide and short-chain amylose solution are uniformly mixed and carry out magnetic agitation, centrifugation is washed with hot acetic acid
It washs three times, freeze-drying obtains short-chain amylose nanometer Prochloraz pesticide.
In the step 2, a concentration of 1%-10% of short-chain amylose liquid.
In the step 3, water-bath equilibration time is 1-6h, and the supersonic frequency of -90 DEG C of temperature 70 C, ultrasonic machine is
40KHz, ultrasonic time 0.5-1h.
In the step 4, the mass fraction content of Prochloraz is 98% in the nano pesticide, and 10-1000mg miaows is fresh
Amine pesticide, which is added in the hot acetic acid of 2-5ml, to be dissolved, then the Prochloraz pesticide that dissolving is completed is added dropwise in 20-50ml short-chain amylose liquid
It is uniformly mixed, the rotating speed of magnetic agitation is 50-1700r/min, mixing time 2-10h, centrifugal rotational speed 3000-6000r/
Min, freeze-drying temperature are -80 DEG C, pressure 20-40Pa, freeze-drying time 12-24h, and short-chain amylose nanometer Prochloraz is made
The embedding rate of pesticide is 60%-90%.
The method and step for producing short-chain amylose is：
One, starch is weighed, phosphate buffer is added into starch, is stirred evenly, is fully gelatinized, is cooled to room temperature；
Two, it toward addition Propiram enzyme solution in the starch emulsion being gelatinized, is sufficiently stirred, is put into water-bath and is digested；
Three, the starch fluid after enzymolysis boiled again, centrifuged, absolute ethyl alcohol is added and washs and precipitates, is put into 4 DEG C of refrigerators
A static evening；
Four, static good starch fluid is removed supernatant, leaves precipitation, precipitation, which is packed into bag filter, dialyses, thoroughly
The starch fluid that analysis is completed is packed into after culture dish carries out pre-freeze processing and is freeze-dried, and obtains short-chain amylose；
In the step 1, starch is waxy corn starch, and the mass percent concentration of starch emulsion is 1%-10%, phosphorus
The molar ratio of acid buffer is 3molNacl：94molKcl：200molNa2HPO4：40molNaH2PO4, pH value 4-5.
In the step 2, Propiram enzyme solution is formulated as accurately measuring in 1ml addition 55-100ml deionized waters, enzymolysis
Time is 6-10h, and temperature is 60 DEG C.
In the step 3, boiling time is 5-15min, and centrifugal rotational speed 3000-5000r/min is washed with absolute ethyl alcohol
The volume ratio for washing sedimentation starch liquid is 1：5.
In the step 4, dialysis bag retention molecular weight MW:500-MW:1000, freeze-drying temperature is -80 DEG C, pressure
Power is 20-40Pa, freeze-drying time 12-24h.
The beneficial effects of the invention are as follows：Compared with traditional farm chemical carrier, nano-carrier of the invention is with grain size is small, compares table
The characteristics such as area is big, can improve medicament to target deposition, transfer efficiency and bioavilability, reduce and be lost in, it is residual to reduce pesticide
It stays and environmental pollution.Meanwhile drug-loaded nanoparticles have the function of pesticide action-controlling, can control medicine with environmental protection sensibility pesticide
Object rate of release extends the lasting period, reduces the loss of the drug effects such as leaching, decomposition.Nano pesticide be at present for relatively new type agriculture
One of pharmaceutically dosage form, nano pesticide can directly by water-insoluble agricultural chemical nanosizing or using nano material by coupling, absorption,
It the modes such as wraps up, inlay and loading pesticide structure nano medicament carrying system, being conducive to improve the dissolubility of pesticide activity component, dispersion
Property, wetability, uniformity, stability, reduce pesticide residue and environmental pollution.
Description of the drawings
Fig. 1：For the grain size distribution of nanometer Prochloraz；
Fig. 2：For the transmission electron microscope picture of nanometer Prochloraz；
Fig. 3：For the scanning electron microscope (SEM) photograph of nanometer Prochloraz.
Specific implementation mode
To make the object, technical solutions and advantages of the present invention clearer, the present invention is made below in conjunction with the accompanying drawings further
Detailed description.
Embodiment 1：Precise 2g active ingredients be 98% Prochloraz active compound be added in the hot acetic acid of 50ml complete it is molten
Solution；Again precise 8g short chains nano-starch be dissolved into be prepared into 100ml deionized waters 8% starch fluid, high temperature and pressure goes out
The starch fluid that sterilizing is completed is put into ultrasound 10min in 40KHz ultrasonic machines and further dissolved by bacterium 30min, the shallow lake that ultrasound is completed
Powder liquid, which is put into 70 DEG C of water-bath, balances 1h, completes dissolving.50ml Prochloraz liquids are added drop-wise to 8% short chain nano-starch
In liquid 100ml, mixed liquor the magnetic agitation 2h, 3000r/min of starch fluid and liquid are centrifuged 5min, take out pellet frozen drying
12h obtains 20% short-chain amylose nanometer Prochloraz pesticide.Short-chain amylose nanometer Prochloraz pesticide grain size prepared by this law exists
Between 100-500nm, embedding rate is 65% or more.
Take 98% Prochloraz active compound of active ingredient and the above-mentioned short-chain amylose nanometer Prochloraz pesticide powder difference prepared
Be added 2ml hot acetic acid and sterile water be configured to 5 concentration be respectively 6ug/ml, 12ug/ml, 24ug/ml, 48ug/ml,
Leaf blight of corn pathogen, is inoculated into containing above 5 concentration by the liquid of 96ug/ml, three repetitions of a concentration respectively
On short-chain amylose nanometer Prochloraz pesticide and the culture medium of Prochloraz active compound, leaf blight of corn pathogen is inoculated into not drug containing
It is used as blank control on culture medium, is cultivated 8 days for 27 DEG C in incubator, measures the result as shown in following table one.
The short-chain amylose nanometer Prochloraz pesticide of table one 20% and 98% Prochloraz active compound are to vigor in leaf blight of corn room
It measures
Note：Same row different size lowercase alphabet shows notable in 0.05,0.01 level difference.Using DPS7.05 versions into
Row difference analysis, similarly hereinafter.
The data from table one it can be seen that, with 20% short chain nanometer Prochloraz pesticide and 98% Prochloraz active compound concentration by
Cumulative big, inhibiting rate is also in increase tendency.Wherein, under 5 various concentrations, 20% short-chain amylose nanometer Prochloraz pesticide is to jade
Pole significant difference is presented in the growth inhibition ratio of rice leaf blight mycelia.In a concentration of 12ug/ml, 24ug/ml, 48ug/ml and 96ug/
When ml, two kinds of pesticides are extremely notable to the mycelial growth inhibition rate difference of the leaf blight of corn；And in maximum concentration 96ug/ml, it receives
Rice Prochloraz pesticide has reached 92.45% to the inhibiting rate of the mycelia growth of the leaf blight of corn, and the inhibiting rate of Prochloraz active compound is only
It is 81.77%.This shows the suppression that nanometer Prochloraz pesticide grows leaf blight of corn mycelia made of short chain nano-starch
Effect processed is got well than active compound Prochloraz.Compared with traditional pesticide, starch itself belongs to natural macromolecular substances, nontoxic, passes through
The mode of pesticide is included with starch can prepare environmental protection, low toxicity and the green that can reduce persticide residue to a certain extent
Pesticide.
Embodiment 2：Precise 1g active ingredients be 98% Prochloraz active compound be added in the hot acetic acid of 25ml complete it is molten
Solution；Again precise 1g short chains nano-starch be dissolved into be prepared into 100ml deionized waters 1% starch fluid, high temperature and pressure goes out
The starch fluid that sterilizing is completed is put into ultrasound 10min in 40KHz ultrasonic machines and further dissolved by bacterium 30min, the shallow lake that ultrasound is completed
Powder liquid, which is put into 90 DEG C of water-bath, balances 6h, completes dissolving.25ml Prochloraz liquids are added drop-wise to 1% short chain nano-starch
In liquid 100ml, mixed liquor the magnetic agitation 10h, 6000r/min of starch fluid and liquid are centrifuged 5min, it is dry to take out pellet frozen
It is dry for 24 hours, obtain 50% short-chain amylose nanometer Prochloraz pesticide.Short-chain amylose nanometer Prochloraz pesticide grain size prepared by this law exists
Between 100-500nm, embedding rate is 80% or more.
Take 98% Prochloraz active compound of active ingredient and the above-mentioned short-chain amylose nanometer Prochloraz pesticide powder difference prepared
Be added 2ml hot acetic acid and sterile water be configured to 5 concentration be respectively 6ug/ml, 12ug/ml, 24ug/ml, 48ug/ml,
Leaf blight of corn pathogen, is inoculated into containing above 5 concentration by the liquid of 96ug/ml, three repetitions of a concentration respectively
On short-chain amylose nanometer Prochloraz pesticide and the culture medium of Prochloraz active compound, leaf blight of corn pathogen is inoculated into not drug containing
It is used as blank control on culture medium, is cultivated 8 days for 27 DEG C in incubator, measures the result as shown in following table two.
The short-chain amylose nanometer Prochloraz pesticide of table 2 50% and 98% Prochloraz active compound are to vigor in leaf blight of corn room
It measures
From two data of table it is found that with pesticide concentration increase, to the inhibiting rate of the mycelia of leaf blight of corn growth also with
Increase, and 50% short-chain amylose nanometer Prochloraz pesticide is under 5 various concentrations, poor to the inhibiting rate of leaf blight of corn mycelia
The opposite sex shows the pole level of signifiance；And Prochloraz active compound is under 5 various concentrations, to the difference of the inhibiting rate of leaf blight of corn mycelia
The opposite sex is in the level of signifiance.Meanwhile 50% inhibiting rate of the short-chain amylose nanometer Prochloraz pesticide under 5 concentration be above 98%
Prochloraz active compound is to the inhibiting rate of the mycelia growth of the leaf blight of corn, and 50% short-chain amylose nanometer Prochloraz pesticide is in 5 differences
Under concentration, to the mycelial growth inhibition rate of the leaf blight of corn between 24.05%-94.11%, and Prochloraz active compound exists
Between 18.92%-81.77%, this shows the inhibition of 50% short-chain amylose nanometer Prochloraz pesticide to leaf blight of corn mycelia
Growth is better than Prochloraz active compound.
It can be seen that again in identical concentration by the data comparison of table one and table two, 50% short-chain amylose nanometer
The inhibiting rate of Prochloraz pesticide is all slightly above the inhibiting rate of 20% short-chain amylose nanometer Prochloraz pesticide.In conclusion 3 agricultures
Medicine is to leaf blight of corn mycelia growth inhibitory effect：The short-chain amylose of 50% short-chain amylose nanometer Prochloraz pesticide > 20%
The Prochloraz active compound of nanometer Prochloraz pesticide > 98%.
Place is not described in detail by the present invention, is the known technology of those skilled in the art of the present technique.Finally illustrate, the above reality
Apply that example is merely illustrative of the technical solution of the present invention and unrestricted, although having been carried out specifically to the present invention with reference to preferred embodiment
It is bright, it will be understood by those of ordinary skill in the art that, technical scheme of the present invention can be modified or replaced equivalently, and
The objective and range for not departing from technical solution of the present invention, are intended to be within the scope of the claims of the invention.
Claims (10)
1. a kind of short-chain amylose nanometer Prochloraz pesticide, which is characterized in that the short-chain amylose nanometer Prochloraz pesticide includes：
Short-chain amylose and Prochloraz, mass percent are：Short-chain amylose 50%-80%, Prochloraz 20%-50%.
2. a kind of preparation method of short-chain amylose nanometer Prochloraz pesticide according to claim 1, it is characterised in that：It is described
Method and step is：
One, short-chain amylose is produced；
Two, it weighs short-chain amylose and is add to deionized water and short-chain amylose liquid, autoclave sterilization is made；
Three, gained short-chain amylose liquid is subjected to water-bath balance, places into ultrasonic machine and carry out ultrasound, completes dissolving, obtain short chain shallow lake
Powder solution；
Four, hot acetate dissolution is added in Prochloraz pesticide, then the short-chain amylose solution obtained by step 3 is added drop-wise to dissolving and is completed
Prochloraz pesticide in, and pesticide and short-chain amylose solution are uniformly mixed and carry out magnetic agitation, centrifugation washs three with hot acetic acid
Secondary, freeze-drying obtains short-chain amylose nanometer Prochloraz pesticide.
3. a kind of preparation method of short-chain amylose nanometer Prochloraz pesticide according to claim 2, it is characterised in that：It is described
In step 2, a concentration of 1%-10% of short-chain amylose liquid.
4. a kind of preparation method of short-chain amylose nanometer Prochloraz pesticide according to claim 2, it is characterised in that：It is described
In step 3, water-bath equilibration time is 1-6h, and the supersonic frequency of -90 DEG C of temperature 70 C, ultrasonic machine is 40KHz, and ultrasonic time is
0.5-1h。
5. a kind of preparation method of short-chain amylose nanometer Prochloraz pesticide according to claim 2, it is characterised in that：It is described
In step 4, the mass fraction content of Prochloraz is 95% in the nano pesticide, and 2- is added in 10-1000mg Prochloraz pesticides
It is dissolved in the hot acetic acid of 5ml, then the Prochloraz pesticide that dissolving is completed is added dropwise in 20-50ml short-chain amylose liquid and is uniformly mixed, magnetic
The rotating speed of power stirring is 50-1700r/min, mixing time 2-10h, centrifugal rotational speed 3000-6000r/min, freeze-drying
Temperature is -80 DEG C, pressure 20-40Pa, freeze-drying time 12-24h, and the embedding rate of short-chain amylose nanometer Prochloraz pesticide is made
For 70%-95%.
6. a kind of preparation method of short-chain amylose nanometer Prochloraz pesticide according to claim 2, it is characterised in that：It is described
The method and step for producing short-chain amylose is：
One, starch is weighed, phosphate buffer is added into starch, is stirred evenly, is fully gelatinized, is cooled to room temperature；
Two, it toward addition Propiram enzyme solution in the starch emulsion being gelatinized, is sufficiently stirred, is put into water-bath and is digested；
Three, the starch fluid after enzymolysis boiled again, centrifuged, absolute ethyl alcohol is added and washs and precipitates, it is static to be put into 4 DEG C of refrigerators
One evening；
Four, static good starch fluid is removed supernatant, leaves precipitation, precipitation loading bag filter is dialysed, having dialysed
At starch fluid be packed into culture dish carry out pre-freeze processing after be freeze-dried, obtain short-chain amylose.
7. a kind of preparation method of short-chain amylose nanometer Prochloraz pesticide according to claim 6, it is characterised in that：It is described
In step 1, starch is waxy corn starch, and the mass percent concentration of starch emulsion is 1%-10%, mole of phosphate buffer
Than for 3molNacl：94molKcl：200molNa2HPO4：40molNaH2PO4, pH value 4-5.
8. a kind of preparation method of short-chain amylose nanometer Prochloraz pesticide according to claim 6, it is characterised in that：It is described
In step 2, Propiram enzyme solution is formulated as accurately measuring in 1ml addition 55-100ml deionized waters, enzymolysis time 6-10h,
Temperature is 60 DEG C.
9. a kind of preparation method of short-chain amylose nanometer Prochloraz pesticide according to claim 6, it is characterised in that：It is described
In step 3, boiling time is 5-15min, centrifugal rotational speed 3000-5000r/min, and sedimentation starch liquid is washed with absolute ethyl alcohol
Volume ratio be 1：5.
10. a kind of preparation method of short-chain amylose nanometer Prochloraz pesticide according to claim 6, it is characterised in that：Institute
It states in step 4, dialysis bag retention molecular weight MW:500-MW:1000, freeze-drying temperature is -80 DEG C, pressure 20-
40Pa, freeze-drying time 12-24h.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810681518.4A CN108739803A (en) | 2018-06-27 | 2018-06-27 | A kind of short-chain amylose nanometer Prochloraz pesticide and preparation method thereof |
| CN201910270795.0A CN109792986A (en) | 2018-06-27 | 2019-04-04 | A kind of short-chain amylose nano pesticide and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810681518.4A CN108739803A (en) | 2018-06-27 | 2018-06-27 | A kind of short-chain amylose nanometer Prochloraz pesticide and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN108739803A true CN108739803A (en) | 2018-11-06 |
Family
ID=63974238
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| CN201810681518.4A Withdrawn CN108739803A (en) | 2018-06-27 | 2018-06-27 | A kind of short-chain amylose nanometer Prochloraz pesticide and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109221200A (en) * | 2018-11-19 | 2019-01-18 | 贵州大学 | A kind of short-chain amylose nanometer tricyclazole pesticide and preparation method thereof |
-
2018
- 2018-06-27 CN CN201810681518.4A patent/CN108739803A/en not_active Withdrawn
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109221200A (en) * | 2018-11-19 | 2019-01-18 | 贵州大学 | A kind of short-chain amylose nanometer tricyclazole pesticide and preparation method thereof |
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