CN107853299A - A kind of blade face affinity type pesticide nano drug-loading system preparation method - Google Patents
A kind of blade face affinity type pesticide nano drug-loading system preparation method Download PDFInfo
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- CN107853299A CN107853299A CN201711258337.2A CN201711258337A CN107853299A CN 107853299 A CN107853299 A CN 107853299A CN 201711258337 A CN201711258337 A CN 201711258337A CN 107853299 A CN107853299 A CN 107853299A
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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
- 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
- A01N25/22—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 ingredients stabilising the active ingredients
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/48—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with two nitrogen atoms as the only ring hetero atoms
- A01N43/56—1,2-Diazoles; Hydrogenated 1,2-diazoles
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/90—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
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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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- Agronomy & Crop Science (AREA)
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- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention discloses a kind of blade face affinity type pesticide nano drug-loading system preparation method.This method includes preparing the steps such as PLA carrier, colostric fluid, nano medicament carrying system and the affine sex modification to nano medicament carrying system.300~800nm of average particle size range of affinity type pesticide nano drug-loading system in blade face of the present invention；Drugloading rate can reach more than 15%, and envelop rate reaches more than 75%；Compared with the former medicine of AVM, the photostability of effective component significantly improves in nano medicament carrying system, and has obvious slow release effect.Blade face affinity type pesticide nano drug-loading system preparation technology of the present invention is simple, and preparation cost is low with equipment investment cost, does not produce pollutant, stable and reliable product quality, and behavior is detained on the blade face that can be obviously improved agricultural chemicals drop.Therefore, blade face affinity type pesticide nano drug-loading system production method of the present invention has boundless application prospect.
Description
【Technical field】
The present invention relates to a kind of pesticide nano drug-loading system for having and orienting affine function, and in particular to a kind of blade face is affine
Type pesticide nano drug-loading system and preparation method thereof, belongs to agricultural chemical insecticide field.
【Background technology】
Agricultural chemicals is efficient, quick, economical, easy due to having the characteristics that, it is developed into a kind of extremely important agricultural
The means of production, it is the main means for preventing and treating crop diseases and pest crop smothering, to ensureing that agricultural production tool is of great significance.I
State is always an agricultural pest hotspot, and based on this, since the nineties in last century, the Pesticide use amount in China is always
In year after year incremental trend, to usage amount in 2012 more than 1,800,000 tons.Because most crop leaf surfaces have wax
The hydrophobic micro-nano structure such as layer, fine hair, mastoid process so that agricultural chemicals drop is difficult to be attached on crop blade face and tumble and miss the target, and leads
Cause the effective rate of utilization of traditional formulations of pesticide extremely low；During field rotating medicine ratio is lost in caused by drift, spring, drippage
Up to 70%~90%；The decoction that blade face crop blade face can be reached is typically less than 30%；Final harmful organism is by dose deficiency
0.1%, most decoctions miss the target into surrounding environment, cause environmental pollution.By the food security of pollution by pesticides initiation, it is good for
The problems such as health risk and ecological disruption, cause the highest attention of the whole society and national governments.
Forefathers, which study, to be found, marine mussel class biology by its byssus can secrete it is a kind of have high intensity, high tenacity with
And the adhesion protein of extremely strong Adhesion property, it can almost be attached on all base materials, cause the very big pass of scientist
Note.Wherein, DOPA (3,4- dihydroxy-L- phenylalanines) is the main component that adhesion is played in the adhesion protein, but its
Complicated extraction process and ultralow yield and expensive price allow its application to be restricted.Shown by research, extensively
The vegatable tannin being present in bark, tree root, leaf and fruit, possess with design feature as DOPA, have substantial amounts of adjacent
Resorcinol groups, also there is very strong adhesion to crop surface, therefore can be as a kind of compatibility carrier, for changing
Kind formulations of pesticide function.
【The content of the invention】
The purpose of the present invention is missed the target the defects of serious for traditional formulations of pesticide, and nanometer technology is mutually tied with pesticide manufacturing
Close, utilize the surface modificability of nano-carrier, there is provided a kind of blade face affinity type pesticide nano drug-loading system and its preparation side
Method.The pesticide nano drug-loading system of the present invention matches with blade face biosurface structure feature, can improve attachment, the infiltration of agricultural chemicals
With the behavior such as deposition, be advantageous to agricultural chemicals drop and be equably covered in crop surface or run to play drug effect in harmful organism body.
The purpose of the present invention is accomplished by the following way：
A kind of preparation method of blade face affinity type pesticide nano drug-loading system provided by the invention, comprises the following steps：
A, the synthesis of PLA carrier material
According to dichloromethane and HO-PLA-COOCH2CH3Weight than 10: 1, by H0-PLA-COOCH2CH3It is fused to dichloro
Solution 1 is obtained in methane solvent；Then triethylamine is dissolved in dichloro than 1: 0.003 according to the weight of dichloromethane and triethylamine
Solution 2 is obtained in methane, solution 2 is mixed into above-mentioned solution 1；Under condition of ice bath, weight ratio is slowly added dropwise as 0.001: 106
Chloroacetic chloride：Dichloromethane solution is to above-mentioned mixed liquor；After stirring 4h at room temperature, with 1.0% NaHCO3Extraction, then with distill
Water cleans twice；The organic phase anhydrous Na that will be collected into2SO4It is dried overnight；PLA carrier is obtained after rotary evaporation organic phase
Material；
B, colostric fluid is prepared
By the polyvinyl alcohol polyvinyl alcohol water solution soluble in water for obtaining concentration and being 0.5~2.0% by weight；
According to the weight of slightly solubility agricultural chemicals, PLA carrier material and organic solvent than 1: 1~5: 20~30, by slightly solubility
Agricultural chemicals is dissolved in organic solvent with the obtained PLA carrier materials of step A, obtains organic solution；
According to organic solution and the weight of polyvinyl alcohol water solution than 1: 1~5, above-mentioned organic solution is added drop-wise to above-mentioned poly-
In vinyl alcohol aqueous solution, 0.5~1.0h is stirred, obtains colostric fluid；
C, pesticide nano drug-loading system is prepared
The colostric fluid that step B is obtained is carried out under conditions of 300~500W of power with ultrasonic device supersound process 3~
5min；Then it is stirred overnight under the conditions of normal temperature with 1000~1500rpm of rotating speed, obtains pesticide nano drug-loading system；
D, blade face affinity type pesticide nano drug-loading system is prepared
The Aqueous Solutions of Polyethylene Glycol that concentration is 40mg/mL, molecular weight is 6000~10000 is added into step C to obtain
Pesticide nano drug-loading system, then the tannin aqueous acid that concentration is 40mg/mL is added in above-mentioned mixed solution, described poly- second
Two alcohol solutions, pesticide nano drug-loading system and tannin aqueous acid three volume ratio be 1: 5: 1~2, at room temperature stir 0.5~
1.0h, that is, obtain described blade face affinity type pesticide nano drug-loading system；
The average particle size range of the blade face affinity type pesticide nano drug-loading system of above-mentioned gained is 300~800nm, drugloading rate
Up to 15~45%, envelop rate is 75~90%.
Preferably, in step B and D, described slightly solubility agricultural chemicals is emamectin-benzoate, Avermectin
Element, gamma cyhalothrin and/or Rynaxypyr.
Certainly, it is every pesticide nano drug-loading system to be prepared using the inventive method, it may have nanometer of the present invention
Other slightly solubility agricultural chemicals of drug-loading system basic performance can also apply production method of the present invention, and these slightly solubility agricultural chemicals are also at this
Within the protection domain of invention.
In the present invention, if the weight of slightly solubility agricultural chemicals and PLA ratio is more than 1: 1, drugloading rate is too high, easily leads
Cause the sedimentation of slightly solubility agricultural chemicals；If the weight of slightly solubility agricultural chemicals and PLA ratio is less than 1: 5, drugloading rate is too low；Therefore, indissoluble
Property agricultural chemicals and PLA weight ratio 1: 1~5 to be rational；
Preferably, in stepb, the weight ratio of described slightly solubility agricultural chemicals and described PLA carrier material is 1: 1
~3.
Preferably, in stepb, described organic solvent is dichloromethane or chloroform.
Preferably, in stepb, described organic solution and the weight of polyvinyl alcohol water solution are than 1: 3~4.
Invention further provides a kind of blade face affinity type pesticide nano drug-loading system obtained by above-mentioned preparation method.
In the present invention, step A main purpose is to prepare polylactic acid polymer, and it is mainly used in forming agricultural chemicals of the present invention
The carrier material of nano medicament carrying system；
In the present invention, the basic role of the polyvinyl alcohol in step B is to reduce solution surface tension, is advantageous to poly- breast
Acid parcel slightly solubility agricultural chemicals.If polyvinyl alcohol water solution concentration is less than described concentration range, stabilization can not be formed
Emulsion, influence PLA parcel slightly solubility agricultural chemicals；If concentration is higher than described scope, PLA can be made in globulation
Easily tangled with polyvinyl alcohol molecule chain, it is difficult to be removed it in washing process, so as to influence the water of nano medicament carrying system
Dispersiveness and release dynamics；
In the present invention, organic solution is added drop-wise in polyvinyl alcohol water solution, forms oil-in-water emulsion.It is if organic
When the weight of solution and polyvinyl alcohol water solution is than more than described scope, then stable colostric fluid can not be formed；
The organic solvent that the present invention uses all is current market sales of product.
The ultrasonic device that the present invention uses is current market sales of equipment, such as by the new sesame biotechnology share in Ningbo
The equipment that Co., Ltd is sold with trade name JY 92-II.
In the present invention, described ultrasonic effect is further equably to emulsify just milk solution, reduces nano medicament carrying system
Average grain diameter, increase its stability.
In the present invention, the main function of described ice bath is due to local temperature when ultrasound can be reduced under cryogenic conditions
Raise too fast, cause the quick volatilization of organic solvent in emulsion, be unfavorable for the formation of nano medicament carrying system.
In the present invention, the adhesive for functioning as tannic acid polymerization of described polyethylene glycol.
In the present invention, the effect of described tannic acid is to carry out affine modification to described nano medicament carrying system surface,
Improve nano medicament carrying system and the affinity on crop blade face.In the present invention, if the concentration of tannin aqueous acid exceedes such as
Upper described scope, then easily cause nano medicament carrying system that aggregation sedimentation occurs；If concentration is less than scope as described above,
Surface is affine, and sex modification is incomplete.
The particle size analyzer sold by Malvern companies with trade name Zetasizer Nano ZS90 is used according to its specification
The particle diameter distribution of the method measure PLA parcel emamectin-benzoate nano medicament carrying system of description, the nanometer
The average grain diameter of drug-loading system about 300nm；The SEM that the nano medicament carrying system is obtained using conventional electron microscope is schemed, referring to attached
Fig. 1.
The particle size analyzer sold by Malvern companies with trade name Zetasizer Nano ZS90 is used according to its specification
The method measure PLA of description wraps up the particle diameter distribution of avermectin nanometer medicine-carried system, and the nano medicament carrying system is averaged
Particle diameter about 300nm；The SEM that the nano medicament carrying system is obtained using conventional electron microscope is schemed, referring to accompanying drawing 2.
The performance test of pesticide nano drug-loading system of the present invention is described below：
I, the avermectin nanometer medicine-carried system sustained release performance test of blade face affinity type
Take 95mL, 60% methanol release solution to brown reaction bulb；10mg blade faces affinity type avermectin nanometer is weighed to carry
Medicine system, it is placed in treated bag filter, and adds 5mL release solutions, is suspended in after the sealing of both ends in reaction bulb；In 25 DEG C
In water bath with thermostatic control shaking table concussion dialysis 165h, respectively at 1h, 3h, 6h, 10h, 21h, 35h, 45h, 58h, 69h, 78h, 98h,
118h, 142h and 165h take out 5mL dialyzates from reaction, while supplement equivalent release solution.Utilize high performance liquid chromatograph
Measure takes the content of AVM in liquid, calculates the accumulative release rate of Each point in time AVM, the result is listed in attached
Fig. 3.It was found from accompanying drawing 3, in 165h the release of AVM tend to balance, reach 99%.
II, blade face affinity type emamectin-benzoate nano medicament carrying system sustained release performance test
Blade face affinity type emamectin-benzoate nano drug-carrying system has been carried out according to the same manner described with I
The sustained release performance test of system, nano medicament carrying system sustained release result are listed in accompanying drawing 4.It was found from accompanying drawing 4, in 118h methylamino Ah
The release of dimension rhzomorph benzoate tends to balance, and reaches 90%.
Fig. 3 shows that the nano medicament carrying system prepared by this patent has the function being sustained with Fig. 4 results.
III, the avermectin nanometer medicine-carried system of blade face affinity type drugloading rate and envelop rate
Take the avermectin nanometer medicine-carried system of 10mg blade faces affinity type, ultrasound makes to being dissolved completely in 5mL dichloromethane
Nano medicament carrying system is opened completely, discharges whole AVMs；It is placed in fume hood after making dichloromethane volatilization completely, then it is complete
Fully dissolved is made into testing sample, after testing sample is filtered, then using high performance liquid chromatograph measure Avermectin in 5mL methanol
Plain concentration.
Drugloading rate and envelop rate are calculated according to following formula：
Drugloading rate (drug-loading capacity, DLC)=(in solution AVM concentration × liquor capacity)/receive
Rice drug-loading system gross mass × 100%；
Medication amount × 100% of medication amount/input of envelop rate (drug loading, DL)=reality.
Result of the test is listed in Table 1 below.
Table 1：The drugloading rate and envelop rate of the avermectin nanometer medicine-carried system of blade face affinity type
| AVM raw material dosage * | 20% | 30% | 50% |
| Drugloading rate | 18% | 23% | 40.2% |
| Envelop rate | 90% | 76.7% | 80.4% |
*：AVM raw material dosage refers to the AVM gross weight put into during production nano medicament carrying system, similarly hereinafter
IV, blade face affinity type gamma cyhalothrin nano medicament carrying system drugloading rate and envelop rate
The same manner according to being described with III determines the load of blade face affinity type gamma cyhalothrin nano medicament carrying system
Dose and envelop rate
Table 2：The drugloading rate and envelop rate of blade face affinity type gamma cyhalothrin nano medicament carrying system
| Gamma cyhalothrin raw material dosage* | 20% | 30% | 50% |
| Drugloading rate | 17.8% | 25% | 37% |
| Envelop rate | 89% | 83.3% | 74% |
V, the light degradation experiment of nano medicament carrying system
Take the former medicine of AVM and its each 100mg solids of nano medicament carrying system, be placed in xenon arc lamp illumination box 25 DEG C,
Continuous illumination under the conditions of 250W, 5mg solid samples are taken respectively at 12h, 24h, 48h, 72h and 96h, are dissolved completely in dichloromethane
Nano medicament carrying system is opened completely in alkane and discharge active compound, be placed in fume hood after making dichloromethane volatilization completely, then by original
Medicine is dissolved completely in methanol dissolving, is ultrasonically treated, filtering, and obtained filtrate determines wherein active compound using high performance liquid chromatograph
Content, result above is listed in accompanying drawing 5.From accompanying drawing 5 as can be seen that illumination 96h after, nano medicament carrying system only degrade less than
50%, the result shows PLA and tannic acid is good pharmaceutical carrier, can substantially reduce the light degradation speed of AVM
Rate, improve its photostability.
VI, nano medicament carrying system temperature stability test
Weigh the nano medicament carrying system after 10g is freezed to be put in the brown vial of cleaning, 0 DEG C of ice is individually positioned in after sealing
Temperature stability experiment is carried out in case, 25 DEG C of drying at room temperature devices and 54 DEG C of insulating boxs, in the 2nd, 4,6,8,10,12 and 14d of storage
Testing sample is taken out, the solution to be measured that concentration is 0.1% is configured at room temperature, its particle diameter distribution is determined with dynamic light scattering
And PdI, result above are listed in accompanying drawing 6；And optics and Electronic Speculum sign are carried out to its pattern, result above is listed in accompanying drawing 7.
Dynamic light scattering result (Fig. 6) can be seen that under 0 DEG C and 25 DEG C of two kinds of storage temperature, two kinds of nano drug-carrying systems
The average grain diameter and PdI of system have almost no change；But after two weeks are stored under the conditions of 54 DEG C, PdI is dramatically increased, this is with 54
The glass transition temperature (about 60 DEG C) of DEG C very close PLA is relevant, and the nothing for causing high molecular polymer PLA is determined
Shape part is converted to thawed state from frozen state, becomes a kind of phenomenon of relaxation (Fig. 7).Based on the experimental result, can demonstrate,prove
Nano medicament carrying system prepared by the bright this patent stable performance in low temperature (0 DEG C) and normal temperature (25 DEG C) environment, can be with long-term storage.
VII, nano medicament carrying system cucumber blade face hold-up
The cucumber leaves of vigorous period in illumination box are gathered, blade are gently rinsed with deionized water, except defoliation table
The various floating dust in face, it is careful not to destroy the structural form of blade, after naturally dry, with scissors along blade main lobe arteries and veins by leaf
Piece is divided into two, and is separately immersed in control nano medicament carrying system (Abam-PLA-NS) and blade face affinity type nano medicament carrying system
(Abam-PLA-Tannin-NS) in decoction, carefully taken out after soaking 30s, after naturally dry, half is placed on clean filter paper
On, second half is rinsed with 100mL deionized waters, after naturally dry, is positioned in vacuum drying oven and is dried 6h.After drying
In SEM under the conditions of 3kV, 10 μ A, deposition of the two kinds of nano medicament carrying systems of observation on cucumber leaf shows blade
As, and record hold-up of two kinds of nano medicament carrying systems on cucumber blade face using high performance liquid chromatograph.Result above is listed in
Accompanying drawing 8 and Fig. 9.It can be seen that from HPLC and Electronic Speculum result and spray two kinds of nano medicament carrying systems of same concentrations in Huang respectively
On melon blade face, after isometric Fluid Dynamics wash away, there is more Abam-PLA-Tannin-NS to be trapped in cucumber leaves table
Face, the phenomenon illustrate that Abam-PLA-Tannin-NS has more preferable blade face affinity, demonstrates again compared with the control
The addition of tannic acid, the affinity with target blade face can be increased, improve the target blade face hold-up of nano medicament carrying system indirectly.
The beneficial effects of the invention are as follows：Obtained using blade face affinity type pesticide nano drug-loading system preparation method of the present invention
The average particle size range of nano medicament carrying system is 300~800nm；Their drugloading rate can reach more than 15%, and envelop rate reaches
To more than 75%；Compared with the former medicine of AVM, the photostability of active ingredient significantly improves in nano medicament carrying system, and has
There is slow release effect.Simple production process of the present invention, production cost is low with equipment investment cost, does not produce pollutant, product quality
It is reliable and stable, there is good deposition effect on blade face crop blade face.Therefore, affinity type pesticide nano in blade face of the present invention carries medicine system
Controlling Preparation Method has boundless application prospect.
【Brief description of the drawings】
The hydration particle diameter distribution of Fig. 1 emamectin benzoates nano medicament carrying system (Ema-PLA-NS) and SEM images.
The hydration particle diameter distribution of the avermectin nanometer medicine-carried systems of Fig. 2 (Abam-PLA-NS) and SEM images.
The sustained release behavior of Fig. 3 the former medicine of AVM and its nano medicament carrying system.
The sustained release behavior of Fig. 4 emamectin benzoates active compound and its nano medicament carrying system.
The light solution curve of Fig. 5 the former medicine of AVM and its nano medicament carrying system.
The particle diameter of nano medicament carrying system and PdI changes under Fig. 6 different temperatures.
The optical signature of nano medicament carrying system and SEM images under Fig. 7 different temperatures.
Image (SEM) is detained on the blade face of Fig. 8 difference nano medicament carrying systems.
The blade residual quantity (HPLC) of Fig. 9 difference nano medicament carrying systems.
【Embodiment】
The principle and feature of the present invention are described with the following Examples, illustrated embodiment is served only for explaining this hair
It is bright, it is not intended to limit the scope of the present invention.
Embodiment 1：Blade face affinity type gamma cyhalothrin nano medicament carrying system production
The implementation steps of the embodiment are as follows：
A, the synthesis of PLA carrier material
According to dichloromethane and HO-PLA-COOCH2CH3Weight than 10: 1, by HO-PLA-COOCH2CH3It is fused to dichloro
Solution 1 is obtained in methane solvent；Then triethylamine is dissolved in dichloro than 1: 0.003 according to the weight of dichloromethane and triethylamine
Solution 2 is obtained in methane, solution 2 is mixed into above-mentioned solution 1；Under condition of ice bath, it is 0.001: 106 that weight ratio, which is slowly added dropwise,
Chloroacetic chloride：Dichloromethane solution is to above-mentioned mixed liquor；After stirring 4h at room temperature, with 1.0% NaHCO3Extraction, then use distilled water
Cleaning is twice；The organic phase anhydrous Na that will be collected into2SO4It is dried overnight；PLA carrier material is obtained after rotary evaporation organic phase
Material；
B, colostric fluid is prepared
By the polyvinyl alcohol polyvinyl alcohol water solution soluble in water for obtaining concentration and being 2.0% by weight；According to slightly solubility
The weight of agricultural chemicals gamma cyhalothrin, PLA carrier material and dichloromethane is than 1: 4: 30 by slightly solubility agricultural chemicals and step A
Obtained PLA carrier material is dissolved in dichloromethane, obtains the organic solution of dichloromethane；
Above-mentioned organic solution is added drop-wise to than 1: 5 according to the organic solution of dichloromethane and the weight of polyvinyl alcohol water solution
In above-mentioned polyvinyl alcohol water solution, 1.0h is stirred, obtains described colostric fluid；
C, gamma cyhalothrin nano medicament carrying system is prepared
To the colostric fluid that step B is obtained with carrying out supersound process 3min under the conditions of ultrasonic device 300W；Then normal temperature with
It is stirred overnight under 1000rpm speed conditions, obtains gamma cyhalothrin nano medicament carrying system；
D, blade face affinity type gamma cyhalothrin nano medicament carrying system is prepared
The pesticide nano that the Aqueous Solutions of Polyethylene Glycol addition step C that concentration is 40mg/mL, molecular weight is 10000 is obtained
Drug-loading system, then the tannin aqueous acid that concentration is 40mg/mL is added in above-mentioned mixed solution, described polyethylene glycol is water-soluble
Liquid, pesticide nano drug-loading system and tannin aqueous acid three volume ratio are 1: 5: 2, stir 1.0h at room temperature, you can obtain institute
The blade face affinity type gamma cyhalothrin nano medicament carrying system stated.
Analyzed and determined using the method for this specification description, the blade face affinity type gamma cyhalothrin nano drug-carrying system
The average grain diameter 800nm of system, drugloading rate 15%, envelop rate 75%.
Embodiment 2：Blade face affinity type Rynaxypyr nano medicament carrying system production
The implementation steps of the embodiment are as follows：
A, the synthesis of PLA carrier material
According to dichloromethane and HO-PLA-COOCH2CH3Weight than 10: 1, by HO-PLA-COOCH2CH3It is fused to dichloro
Solution 1 is obtained in methane solvent；Then triethylamine is dissolved in dichloro than 1: 0.003 according to the weight of dichloromethane and triethylamine
Solution 2 is obtained in methane, solution 2 is mixed into above-mentioned solution 1；Under condition of ice bath, it is 0.001: 106 that weight ratio, which is slowly added dropwise,
Chloroacetic chloride：Dichloromethane solution is to above-mentioned mixed liquor；After stirring 4h at room temperature, with 1.0% NaHCO3Extraction, then use distilled water
Cleaning is twice；The organic phase anhydrous Na that will be collected into2SO4It is dried overnight；PLA carrier material is obtained after rotary evaporation organic phase
Material；
B, colostric fluid is prepared
By the polyvinyl alcohol polyvinyl alcohol water solution soluble in water for obtaining concentration and being 1.0% by weight；According to slightly solubility
The weight of agricultural chemicals Rynaxypyr, PLA and dichloromethane is than 1: 2: 25, poly- breast that slightly solubility agricultural chemicals and step A are obtained
Acid support material is dissolved in dichloromethane, obtains the organic solution of dichloromethane；
According to organic solution and the weight of the aqueous solution than 1: 5, it is water-soluble that above-mentioned organic solution is added drop-wise to above-mentioned polyvinyl alcohol
In liquid, 1.0h is stirred, obtains described colostric fluid；
C, Rynaxypyr nano medicament carrying system is prepared
To the colostric fluid that step B is obtained with carrying out supersound process 5min under the conditions of ultrasonic device 300W；Then normal temperature with
It is stirred overnight under 1000rpm speed conditions, obtains Rynaxypyr nano medicament carrying system；
D, blade face affinity type Rynaxypyr nano medicament carrying system is prepared
The pesticide nano that the Aqueous Solutions of Polyethylene Glycol addition step C that concentration is 40mg/mL, molecular weight is 10000 is obtained
Drug-loading system, then the tannin aqueous acid that concentration is 40mg/mL is added in above-mentioned mixed solution, described polyethylene glycol is water-soluble
Liquid, pesticide nano drug-loading system and tannin aqueous acid three volume ratio are 1: 5: 1, stir 1.0h at room temperature, you can obtain institute
The blade face affinity type Rynaxypyr nano medicament carrying system stated.
Analyzed and determined using the method for this specification description, the blade face affinity type Rynaxypyr nano medicament carrying system
Average grain diameter 500nm, drugloading rate 30%, envelop rate 90%.
Embodiment 3：Blade face affinity type gamma cyhalothrin nano medicament carrying system production
The implementation steps of the embodiment are as follows：
A, the synthesis of PLA carrier material
According to dichloromethane and HO-PLA-COOCH2CH3Weight than 10: 1, by HO-PLA-COOCH2CH3It is fused to dichloro
Solution 1 is obtained in methane solvent；Then triethylamine is dissolved in dichloro than 1: 0.003 according to the weight of dichloromethane and triethylamine
Solution 2 is obtained in methane, solution 2 is mixed into above-mentioned solution 1；Under condition of ice bath, it is 0.001: 106 that weight ratio, which is slowly added dropwise,
Chloroacetic chloride：Dichloromethane solution is to above-mentioned mixed liquor；After stirring 4h at room temperature, with 1.0% NaHCO3Extraction, then use distilled water
Cleaning is twice；The organic phase anhydrous Na that will be collected into2SO4It is dried overnight；PLA carrier material is obtained after rotary evaporation organic phase
Material；
B, colostric fluid is prepared
By the polyvinyl alcohol polyvinyl alcohol water solution soluble in water for obtaining concentration and being 1.0% by weight；According to slightly solubility
The weight of agricultural chemicals gamma cyhalothrin, PLA and dichloromethane obtains slightly solubility agricultural chemicals and step A poly- than 1: 2: 25
Lactic acid carrier material is dissolved in dichloromethane, obtains the organic solution of dichloromethane；
According to organic solution and the weight of the aqueous solution than 1: 5, it is water-soluble that above-mentioned organic solution is added drop-wise to above-mentioned polyvinyl alcohol
In liquid, 1.0h is stirred, obtains described colostric fluid；
C, gamma cyhalothrin nano medicament carrying system is prepared
To the colostric fluid that step B is obtained with carrying out supersound process 4min under the conditions of ultrasonic device 500W；Then normal temperature with
It is stirred overnight under 1000rpm speed conditions, obtains gamma cyhalothrin nano medicament carrying system；
D, blade face affinity type gamma cyhalothrin nano medicament carrying system is prepared
The obtained pesticide nanos of the Aqueous Solutions of Polyethylene Glycol addition step C that concentration is 40mg/mL, molecular weight is 6000 are carried
Medicine system, then the tannin aqueous acid that concentration is 40mg/mL is added in above-mentioned mixed solution, described polyethylene glycol is water-soluble
Liquid, pesticide nano drug-loading system and tannin aqueous acid three volume ratio are 1: 5: 1, stir 1.0h at room temperature, you can obtain institute
The blade face affinity type gamma cyhalothrin nano medicament carrying system stated.
Analyzed and determined using the method for this specification description, the blade face affinity type gamma cyhalothrin nano drug-carrying system
The average grain diameter 650nm of system, drugloading rate 30%, envelop rate 90%.
Embodiment 4：Blade face affinity type Rynaxypyr nano medicament carrying system production
The implementation steps of the embodiment are as follows：
A, the synthesis of PLA carrier material
According to dichloromethane and HO-PLA-COOCH2CH3Weight than 10: 1, by HO-PLA-COOCH2CH3It is fused to dichloro
Solution 1 is obtained in methane solvent；Then triethylamine is dissolved in dichloro than 1: 0.003 according to the weight of dichloromethane and triethylamine
Solution 2 is obtained in methane, solution 2 is mixed into above-mentioned solution 1；Under condition of ice bath, it is 0.001: 106 that weight ratio, which is slowly added dropwise,
Chloroacetic chloride：Dichloromethane solution is to above-mentioned mixed liquor；After stirring 4h at room temperature, with 1.0% NaHCO3Extraction, then use distilled water
Cleaning is twice；The organic phase anhydrous Na that will be collected into2SO4It is dried overnight；PLA carrier material is obtained after rotary evaporation organic phase
Material；
B, colostric fluid is prepared
By the polyvinyl alcohol polyvinyl alcohol water solution soluble in water for obtaining concentration and being 0.5% by weight；According to slightly solubility
The weight of agricultural chemicals Rynaxypyr, PLA and dichloromethane is than 1: 2: 25, poly- breast that slightly solubility agricultural chemicals and step A are obtained
Acid support material is dissolved in dichloromethane, obtains the organic solution of dichloromethane；
According to organic solution and the weight of the aqueous solution than 1: 1, it is water-soluble that above-mentioned organic solution is added drop-wise to above-mentioned polyvinyl alcohol
In liquid, 1.0h is stirred, obtains described colostric fluid；
C, Rynaxypyr nano medicament carrying system is prepared
To the colostric fluid that step B is obtained with carrying out supersound process 4min under the conditions of ultrasonic device 500W；Then normal temperature with
It is stirred overnight under 1000rpm speed conditions, obtains Rynaxypyr nano medicament carrying system；
D, blade face affinity type Rynaxypyr nano medicament carrying system is prepared
The pesticide nano that the Aqueous Solutions of Polyethylene Glycol addition step C that concentration is 40mg/mL, molecular weight is 10000 is obtained
Drug-loading system, then the tannin aqueous acid that concentration is 40mg/mL is added in above-mentioned mixed solution, described polyethylene glycol is water-soluble
Liquid, pesticide nano drug-loading system and tannin aqueous acid three volume ratio are 1: 5: 1, stir 1.0h at room temperature, you can obtain institute
The blade face affinity type Rynaxypyr nano medicament carrying system stated.
Analyzed and determined using the method for this specification description, the blade face affinity type Rynaxypyr nano medicament carrying system
Average grain diameter 800nm, drugloading rate 26%, envelop rate 78%.
Embodiment 5：The avermectin nanometer medicine-carried system production of blade face affinity type
The implementation steps of the embodiment are as follows：
A, the synthesis of PLA carrier material
According to dichloromethane and HO-PLA-COOCH2CH3Weight than 10: 1, by HO-PLA-COOCH2CH3It is fused to dichloro
Solution 1 is obtained in methane solvent；Then triethylamine is dissolved in dichloro than 1: 0.003 according to the weight of dichloromethane and triethylamine
Solution 2 is obtained in methane, solution 2 is mixed into above-mentioned solution 1；Under condition of ice bath, it is 0.001: 106 that weight ratio, which is slowly added dropwise,
Chloroacetic chloride：Dichloromethane solution is to above-mentioned mixed liquor；After stirring 4h at room temperature, with 1.0% NaHCO3Extraction, then use distilled water
Cleaning is twice；The organic phase anhydrous Na that will be collected into2SO4It is dried overnight；PLA carrier material is obtained after rotary evaporation organic phase
Material；
B, colostric fluid is prepared
By the polyvinyl alcohol polyvinyl alcohol water solution soluble in water for obtaining concentration and being 1.0% by weight；According to slightly solubility
The PLA that the weight of pesticide avermectin, PLA and dichloromethane obtains slightly solubility agricultural chemicals and step A than 1: 5: 20 carries
Body material is dissolved in dichloromethane, obtains the organic solution of dichloromethane；
According to organic solution and the weight of the aqueous solution than 1: 4, it is water-soluble that above-mentioned organic solution is added drop-wise to above-mentioned polyvinyl alcohol
In liquid, 1.0h is stirred, obtains described colostric fluid；
C, avermectin nanometer medicine-carried system is prepared
To the colostric fluid that step B is obtained with carrying out supersound process 5min under the conditions of ultrasonic device 500W；Then normal temperature with
It is stirred overnight under 1000rpm speed conditions, obtains avermectin nanometer medicine-carried system；
D, the avermectin nanometer medicine-carried system of blade face affinity type is prepared
The pesticide nano that the Aqueous Solutions of Polyethylene Glycol addition step C that concentration is 40mg/mL, molecular weight is 10000 is obtained
Drug-loading system, then the tannin aqueous acid that concentration is 40mg/mL is added in above-mentioned mixed solution, described polyethylene glycol is water-soluble
Liquid, pesticide nano drug-loading system and tannin aqueous acid three volume ratio are 1: 5: 1, stir 1.0h at room temperature, you can obtain institute
The avermectin nanometer medicine-carried system of blade face affinity type stated.
Analyzed and determined using the method for this specification description, the avermectin nanometer medicine-carried system of blade face affinity type is put down
Equal particle diameter 300nm, drugloading rate 30%, envelop rate 90%.
Embodiment 6：Blade face affinity type emamectin-benzoate nano medicament carrying system production
The implementation steps of the embodiment are as follows：
A, the synthesis of PLA carrier material
According to dichloromethane and HO-PLA-COOCH2CH3Weight than 10: 1, by HO-PLA-COOCH2CH3It is fused to dichloro
Solution 1 is obtained in methane solvent；Then triethylamine is dissolved in dichloro than 1: 0.003 according to the weight of dichloromethane and triethylamine
Solution 2 is obtained in methane, solution 2 is mixed into above-mentioned solution 1；Under condition of ice bath, it is 0.001: 106 that weight ratio, which is slowly added dropwise,
Chloroacetic chloride：Dichloromethane solution is to above-mentioned mixed liquor；After stirring 4h at room temperature, with 1.0% NaHCO3Extraction, then use distilled water
Cleaning is twice；The organic phase anhydrous Na that will be collected into2SO4It is dried overnight；PLA carrier material is obtained after rotary evaporation organic phase
Material；
B, colostric fluid is prepared
By the polyvinyl alcohol polyvinyl alcohol water solution soluble in water for obtaining concentration and being 1.0% by weight；According to slightly solubility
The weight of agricultural chemicals emamectin-benzoate, PLA and dichloromethane is than 1: 1: 25, by slightly solubility agricultural chemicals and step A
Obtained PLA carrier material is dissolved in dichloromethane, obtains the organic solution of dichloromethane；
According to organic solution and the weight of the aqueous solution than 1: 4, it is water-soluble that above-mentioned organic solution is added drop-wise to above-mentioned polyvinyl alcohol
In liquid, 1.0h is stirred, obtains described colostric fluid；
C, emamectin-benzoate nano medicament carrying system is prepared
To the colostric fluid that step B is obtained with carrying out supersound process 5min under the conditions of ultrasonic device 500W；Then normal temperature with
It is stirred overnight under 1500rpm speed conditions, obtains emamectin-benzoate nano medicament carrying system；
D, blade face affinity type emamectin-benzoate nano medicament carrying system is prepared
The pesticide nano that the Aqueous Solutions of Polyethylene Glycol addition step C that concentration is 40mg/mL, molecular weight is 10000 is obtained
Drug-loading system, then the tannin aqueous acid that concentration is 40mg/mL is added in above-mentioned mixed solution, described polyethylene glycol is water-soluble
Liquid, pesticide nano drug-loading system and tannin aqueous acid three volume ratio are 1: 5: 1, stir 1.0h at room temperature, you can obtain institute
The blade face affinity type emamectin-benzoate nano medicament carrying system stated.
Analyzed and determined using the method for this specification description, the blade face affinity type emamectin-benzoate is received
The average grain diameter 300nm of rice drug-loading system, drugloading rate 45%, envelop rate 90%.
Test example 1：The melon aphid Toxicity Determination of different dosage forms AVM
I, test medicine：
Avermectin nanometer medicine-carried system (Abam-PLA-NS)；
The avermectin nanometer medicine-carried system of blade face affinity type (Abam-PLA-Tannin-NS) prepared by the present invention；
Commercially available water dispersible granules (Kai Wei：Beijing Hua Rongkai prestige plant protection bio tech ltd)；
Commercially available water dispersible granules (kingfisher dimension：Shandong Shen Xing agricultural chemicals Co., Ltd).
II, test method
Using leaf dipping method measure melon aphid indoor virulence on cucumber blade face.Each medicament pure water is configured to 7 by grade ratio
Individual series concentration decoction (ppm)：50th, 25,12.5,6.25,3.12,1.56,0.78, and set the corresponding processing without medicament and do
Blank control；Clean fresh cabbage leaf is broken into diameter 6cm disk with card punch, blade is soaked into 10s in decoction,
Then face of blade is affixed on indoors in culture dish after naturally dry after taking-up；Access what is prepared with writing brush picking black peach aphid
In the culture dish of blade with insecticide, per 20, ware, covered with preservative film, it is 15~20 small with insect needle bundle on film
Hole；Treated aphid is placed in incubator and raised, 25 DEG C of temperature, relative humidity 75%, illumination condition 16: 8 (L: D), often
Processing is repeated 4 times.
Death condition is checked under anatomical lens after 48h, using foot, feeler vibration person as worm living, to the aphid for being difficult to judge life or death
Worm touches polypide with insect needle, is death without any reactor, counts the death toll of aphid.With DPS v12.01 statistical softwares meter
Virulence regression equation, half lethal concentration (LC50) and its 95% confidential interval are calculated, carries out variance analysis and regression analysis, its result
It is listed in Table 3 below.
The result of table 3 shows, compared with two kinds of commercially available medicaments, nano medicament carrying system prepared by the present invention has more preferable desinsection
Activity；In addition, the avermectin nanometer medicine-carried system of blade face affinity type (Abam-PLA-Tannin-NS) performance under same concentrations
Go out more preferable insecticidal effect, the result shows that tannic acid adds the affinity of the nano medicament carrying system and cucumber blade face, makes
More Abam-PLA-Tannin-NS can be trapped in cucumber leaves surface, increase connecing for aphid and effective component indirectly
Have a sudden inspiration meeting, so as to improve insecticidal activity.
Table 3：The melon aphid indoor virulence test result of different dosage forms AVM
Test example 2：The melon aphid Toxicity Determination of different dosage forms emamectin-benzoate (emamectin benzoate)
I, test medicine：
Emamectin benzoate nano medicament carrying system (Ema-PLA-NS)；
Blade face affinity type emamectin benzoate nano medicament carrying system (Ema-PLA-Tannin-NS) prepared by the present invention；
Commercially available water dispersible granules (tortoise beetle bullet：He Huaguanlong agrochemical Co., Ltd)；
(ten thousand rise commercially available missible oil：Shenzhen Nuopuxin Agricultural Chemical Co., Ltd).
II, test method
Using leaf dipping method measure melon aphid indoor virulence on cucumber blade face.Each medicament pure water is configured to 7 by grade ratio
Individual series concentration decoction (ppm)：50th, 25,12.5,6.25,3.12,1.56,0.78, and set the corresponding processing without medicament and do
Blank control；Clean fresh cabbage leaf is broken into diameter 6cm disk with card punch, blade is soaked into 10s in decoction,
Then face of blade is affixed on indoors in culture dish after naturally dry after taking-up；Access what is prepared with writing brush picking black peach aphid
In the culture dish of blade with insecticide, per 20, ware, covered with preservative film, it is 15~20 small with insect needle bundle on film
Hole；Treated aphid is placed in incubator and raised, 25 DEG C of temperature, relative humidity 75%, illumination condition 16：8(L：D), often
Processing is repeated 4 times.
Death condition is checked under anatomical lens after 48h, using foot, feeler vibration person as worm living, to the aphid for being difficult to judge life or death
Worm touches polypide with insect needle, is death without any reactor, counts the death toll of aphid.With DPS v12.01 statistical softwares meter
Virulence regression equation, half lethal concentration (LC50) and its 95% confidential interval are calculated, carries out variance analysis and regression analysis, its result
It is listed in Table 4 below.
The result of table 4 shows that nano medicament carrying system prepared by the present invention has the insecticidal activity suitable with commercially available medicament；Its
In, the blade face affinity type emamectin benzoate nano medicament carrying system (Ema-PLA-Tannin-NS) under same concentrations shows preferably to kill
Worm effect, the result show that tannic acid adds the affinity of the nano medicament carrying system and cucumber blade face so that more
Ema-PLA-Tannin-NS can be trapped in cucumber leaves surface, increase the touch opportunity of aphid and effective component indirectly, from
And improve insecticidal activity.
Table 4：The indoor virulence test result of different dosage forms emamectin benzoate
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art the invention discloses technical scope in, the change or replacement that can readily occur in,
It should all be included within the scope of the present invention.
Claims (7)
1. a kind of preparation method of blade face affinity type pesticide nano drug-loading system, it is characterised in that this method comprises the following steps：
A, the synthesis of PLA carrier material
According to dichloromethane and HO-PLA-COOCH2CH3Weight than 10: 1, by HO-PLA-COOCH2CH3It is molten to be fused to dichloromethane
Solution 1 is obtained in agent；Then triethylamine is dissolved in dichloromethane than 1: 0.003 according to the weight of dichloromethane and triethylamine
Solution 2 is obtained, solution 2 is mixed into above-mentioned solution 1；Under condition of ice bath, the acetyl that weight ratio is 0.001: 106 is slowly added dropwise
Chlorine：Dichloromethane solution is to above-mentioned mixed liquor；After stirring 4h at room temperature, with 1.0% NaHCO3Extraction, then cleaned with distilled water
Twice；The organic phase anhydrous Na that will be collected into2SO4It is dried overnight；PLA carrier material is obtained after rotary evaporation organic phase；
B, colostric fluid is prepared
By the polyvinyl alcohol polyvinyl alcohol water solution soluble in water for obtaining concentration and being 0.5~2.0% by weight；
According to the weight of slightly solubility agricultural chemicals, PLA carrier material and organic solvent than 1: 1~5: 20~30, by slightly solubility agricultural chemicals
The PLA carrier material obtained with step A is dissolved in organic solvent, obtains organic solution；
According to organic solution and the weight of polyvinyl alcohol water solution than 1: 1~5, above-mentioned organic solution is added drop-wise to above-mentioned polyethylene
In alcohol solution, 0.5~1.0h is stirred, obtains colostric fluid；
C, pesticide nano drug-loading system is prepared
3~5min of supersound process is carried out under conditions of 300~500W of power with ultrasonic device to the colostric fluid that step B is obtained；
Then it is stirred overnight under the conditions of normal temperature with 1000~1500rpm of rotating speed, obtains pesticide nano drug-loading system；
D, blade face affinity type pesticide nano drug-loading system is prepared
The Aqueous Solutions of Polyethylene Glycol that concentration is 40mg/mL, molecular weight is 6000~10000 is added to the agricultural chemicals that step C obtains
Nano medicament carrying system, then the tannin aqueous acid that concentration is 40mg/mL is added in above-mentioned mixed solution, described polyethylene glycol
The aqueous solution, pesticide nano drug-loading system and tannin aqueous acid three volume ratio be 1: 5: 1~2, at room temperature stir 0.5~
1.0h, that is, obtain described blade face affinity type pesticide nano drug-loading system；
The average particle size range of the blade face affinity type pesticide nano drug-loading system of above-mentioned gained is 300~800nm, drugloading rate 15
~45%, envelop rate is 75~90%.
2. preparation method according to claim 1, it is characterised in that described slightly solubility agricultural chemicals is emamectin benzoate
Benzoate, AVM, gamma cyhalothrin and/or Rynaxypyr.
3. preparation method according to claim 1, it is characterised in that described organic solvent is dichloromethane or chloroform.
4. preparation method according to claim 1, it is characterised in that described slightly solubility agricultural chemicals carries with described PLA
The weight ratio of body material is 1: 1~3.
5. preparation method according to claim 1, it is characterised in that described organic solution and polyvinyl alcohol water solution
Weight is than 1: 3~4.
6. carried according to the blade face affinity type pesticide nano that preparation method described in any one of Claims 1 to 5 claim obtains
Medicine system.
7. carried according to the blade face affinity type pesticide nano that preparation method described in any one of Claims 1 to 5 claim obtains
Medicine system, applied to preparing agricultural chemical insecticide.
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| CN110050787B (en) * | 2019-04-26 | 2021-07-20 | 中国农业科学院农业环境与可持续发展研究所 | Preparation method of tannic acid modified leaf surface adhesion type pesticide |
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| CN111670899A (en) * | 2020-05-20 | 2020-09-18 | 湖州师范学院 | Camptothecin compound nano drug delivery system and preparation method thereof |
| CN112189675A (en) * | 2020-08-04 | 2021-01-08 | 北京宇悦生物科技有限公司 | Pesticide nano drug-loading system and preparation method thereof |
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| CN115581229B (en) * | 2022-09-29 | 2024-06-25 | 广东省科学院微生物研究所(广东省微生物分析检测中心) | Preparation method and antibacterial application of prochloraz ethyl cellulose nano-particles modified by tannic acid interface |
| CN115836679A (en) * | 2022-10-20 | 2023-03-24 | 江苏艾津作物科技集团有限公司 | Pesticide with adhesion and pH responsiveness to leaves and preparation method thereof |
| CN115836679B (en) * | 2022-10-20 | 2024-05-24 | 江苏艾津作物科技集团有限公司 | Pesticide with adhesiveness and pH responsiveness to leaves and preparation method thereof |
| CN115644175A (en) * | 2022-11-14 | 2023-01-31 | 中国农业科学院农产品加工研究所 | Preparation method of nano embedded pesticide and nano embedded pesticide |
| CN115644175B (en) * | 2022-11-14 | 2023-11-10 | 中国农业科学院农产品加工研究所 | Preparation method of nano-embedded pesticide and nano-embedded pesticide |
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