CN101692808A - Emamectin benzoate solid lipid nanoparticle and preparation method and application thereof in pesticide formulation - Google Patents
Emamectin benzoate solid lipid nanoparticle and preparation method and application thereof in pesticide formulation Download PDFInfo
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Abstract
The invention discloses an emamectin benzoate solid lipid nanoparticle and a preparation method for a water dispersible granule, a suspension concentrate and wettable powder of the composition of the emamectin benzoate solid lipid nanoparticle with lufenuron, indoxacarb, pleocidin, chlorfenapyr and chlorantraniliprole. Compared with the composition preparation which is prepared by directly adopting the emamectin benzoate raw pesticide as raw material, the emamectin benzoate solid lipid nanoparticle has the advantages of improving the chemical stability of hot and cold storage, reducing the photolysis rate, prolonging efficacy time, reducing dosage, and significantly improving insecticidal effect.
Description
Technical field
The present invention relates to nanometer formulation and the preparation technology and the application in pesticidal preparations field, particularly biopesticide.
Background technology
Emamectin-benzoate (emamectin benzoate) is to react by Wilkinson as parent compound with soil actinomycetes (Streptomyces avermitilis MA-4680) fermented product Avermectin B1 to carry out a kind of new and effective semisynthetic macrolide antiinsect antibiotic that structural modification obtains, its the most responsive target in insect bodies is the spread effect to neurotransmitter such as glutamine GABA inhibition chloride channel, cause cell function forfeiture and muscular paralysis effect by shifting the high-affinity binding site, upset nerve conduction, insect contacts or gets the food back and stops feed at once, and irreversible paralysis effect and death take place.Though emamectin-benzoate is to the ultraviolet light instability, easily decompose under the slant acidity condition, but it has low toxicity, efficiently, high selectivity reaches and characteristics such as Environmental compatibility is good, to some insects such as diamond-back moth, beet armyworm, prodenia litura, the insecticidal activity of intractable such as cabbage caterpillar and cotton bollworm resistant insect and various harmful mites is than the high 1-3 of a parent compound Avermectin order of magnitude, it has stomach toxicity and action of contace poison, under low-down dosage, has good effect and to natural enemies security, so emamectin-benzoate is widely used in the mixed pesticide preparation, to enlarge insecticidal spectrum, improve drug effect and reduce cost. be for example: Chinese invention patent application " a kind of insecticides with synergistic effect " (publication number CN101380008) discloses with lufenuron and emamectin-benzoate composition pesticide and the preparation method as active component; Publication number is that the patent application " composition pesticide of indoxacarb and first dimension salt " of CN101263823 discloses with indoxacarb and emamectin-benzoate composition pesticide and the preparation method as active component; Publication number is that the patent application " Pesticidal combination that contains multiple killing teichomycin and emamectin-benzoate " of CN101322493 discloses with pleocidin and emamectin-benzoate composition pesticide and the preparation method as active component, and publication number is that the patent application " Pesticidal combination that contains emamectin-benzoate and capillary " of CN101322495 discloses with capillary and emamectin-benzoate composition pesticide and the preparation method as active component.
But, the results showed that the preparation of above composition all exists the active component emamectin-benzoate seriously to decompose easily photodissociation in the use, degradation problem under the drug effect in cold and hot storage experiment.In order to address this problem, publication number is that the patent application of CN1663379A discloses the method that adopts situ aggregation method to prepare emamectin-benzoate microcapsules, though make emamectin-benzoate be difficult for being destroyed by atmosphere, sunlight and rainwater or running off, can prolong the medicament term of validity, but its complicated process of preparation, and can only be used to prepare suspending agent.
Summary of the invention
The objective of the invention is to: emamectin benzoate solid lipid nanoparticle that a kind of technology is simple, stability is high and preparation method thereof is provided, and the application of the said goods in pesticidal preparations is provided.
Nanometer technology is a new technique, nanosecond science and technology belong to the forward position cross discipline, the system that nanometer technology and nano material are applied to field of pharmaceutical preparations comprise nanoparticle (Nanoparticles, NP), nanocapsule (Nanocapstles, NC), nano-micelle (Nanomicelle, NM), lipid nanometer body (Nano-liposemes, NL) and nanometer microemulsion (Nano-emulsion, NE) etc.Wherein, NP generally is meant by natural or macromolecular material is made, and (1.0～500nm) solid colloid particulate, or be called colloid bearer (colloidal.carriers), active component is positioned at particle inside by dissolving, package action to granularity at nanoscale.This novel medicament preparation has slow-release function, can improve medicine stability, dispersiveness, service efficiency and drug effect simultaneously.Solid lipid nano (Solid lipid nanopartides, SLN) be with natural or synthetic lipoid as carrier matrix, active ingredient is wrapped in the lipoid nuclear.
In order to solve the stability problem of emamectin-benzoate, the inventor is through big quantity research and test, discovery is made solid lipid nano granule with emamectin-benzoate and carrier matrix, can improve its chemical stability, improve compound property, help the ultraviolet light photodissociation, prolong the lasting period, and significantly promote drug effect.The preparation method of above-mentioned emamectin benzoate solid lipid nanoparticle is:
1) emamectin-benzoate and fatty acid are dissolved in the organic solvent together, the concentration that makes emamectin-benzoate is 1%-15%, and the concentration of fatty acid is 30%-80%; 2) the polyvinyl alcohol water is made into the aqueous solution that concentration is 0.1%-10%; 3) with 1) in organic solution and 2) in polyvinyl alcohol water solution in 1: 3-1: 10 ratio is mixed, make mixed liquor emulsification by stirring or vibration or high shear, use littleization of ultrasonic then, make it become the 100-500 nano_scale particle, stirred 1-20 hour, final drying can make emamectin benzoate solid lipid nanoparticle again.
Described fatty acid is to contain carbon number more than 10, fusing point at the plant resource fatty acid more than 30 ℃, at least a in preferred capric acid, lauric acid, arachidic acid, stearic acid, the palmitic acid.
Described organic solvent can be isopropyl alcohol or ethyl acetate; Described drying means is a boulton process, or freeze-drying, or spray drying process.
The emamectin benzoate solid lipid nanoparticle that makes with said method, comprise following components in weight percentage: emamectin-benzoate 1%-15%, fatty acid 30%-80%, polyvinyl alcohol 5%-25%, described fatty acid are at least a in capric acid, lauric acid, arachidic acid, stearic acid, the palmitic acid.
Fatty acid is biocompatible lipoid carrier matrix, it has many advantages: the blade face compatibility is good, help the absorption and the transportation of medicine, good target is arranged, can improve the chemical stability of medicine, improve compound property, help the ultraviolet light photodissociation, the prolong drug lasting period, significantly promote drug effect.Make the emamectin benzoate solid lipid nanoparticle that carrier matrix prepares with fatty acid, it is high to have stability, and toxicity is low, and technology is simple, and cost is relatively low, the advantage of energy large-scale production.
In following explanation and describing, emamectin benzoate solid lipid nanoparticle is also referred to as the female powder of solid lipid nano emamectin-benzoate or abbreviates the solid lipid nano emamectin-benzoate as or lipid nanometer first dimension salt.
Emamectin benzoate solid lipid nanoparticle of the present invention can be used for preparing preparations such as water dispersible granules, suspending agent, wetting powder; Can also increase the active ingredient (X) of other non-solid lipid nanometerization in the described preparation as required, can comprise Acarus tritici urea, indenes worm prestige, pleocidin, capillary, Rynaxypyr etc. with other active ingredient (X) that the solid lipid nano emamectin-benzoate prepares compound formulation, the weight ratio of solid lipid nano emamectin-benzoate and active ingredient (X) is 1: 1-800.
When solid lipid nano emamectin-benzoate of the present invention was used to prepare water dispersible granules, it was formed and also comprise the surfactant that accounts for weight of formulation 1%-10%, the auxiliary agent of 1%-5%, the disintegrant of 0%-15%, the adhesive of 1%-5% and the carrier of 1%-80% except that active ingredient; Described surfactant comprises lignosulfonates, lauryl sodium sulfate, fatty acid sulphate, aliphatic alcohol polyethenoxy, nekal, in the dodecyl polyoxyethylene ether phosphate one or more, described auxiliary agent comprises the benzylphenol APEO, Tea Saponin, in the alkylphenol polyoxyethylene one or more, described disintegrant comprises bentonite, ammonium sulfate, urea, in the magnesium sulfate one or more, described adhesive comprises polyethylene glycol, cyclodextrin, starch, a kind of in the sodium silicate, described carrier comprises diatomite, kaolin, white carbon, a kind of in the nacrite.
When solid lipid nano emamectin-benzoate of the present invention was used to prepare suspending agent, its constituent also comprised the surfactant that accounts for weight of formulation 1%-10%, the auxiliary agent of 1%-5% and the carrier of 1%-80% except that active ingredient; Described surfactant is one or more in phenethyl phenol APEO (602#, 603#, 600#), alkylphenol polyoxyethylene or its phosphate, fatty alcohol-polyoxyethylene ether (JFC), lignosulfonates, the naphthalenesulfonate formaldehyde condensation compound; Described auxiliary agent is antifreeze ethylene glycol, thickener xanthans, defoamer silicone; Described carrier is a water.
When solid lipid nano emamectin-benzoate of the present invention was used to prepare wetting powder, it was formed and also include the surfactant that accounts for weight of formulation 1%-10% and the carrier of 1%-80% except that active ingredient; Described surfactant is lignosulfonates, lauryl sodium sulfate, fatty acid sulphate, aliphatic alcohol polyethenoxy, nekal, benzylphenol APEO, alkylphenol polyoxyethylene, draw back in the powder one or more, and described carrier is a kind of in kaolin, precipitated calcium carbonate, clay, the white carbon.
Compare with the complex composition preparation of the former powder production of direct employing emamectin-benzoate, the complex composition preparation of using solid lipid nano emamectin-benzoate of the present invention production has following advantage: (1) cold and hot storage stability significantly promotes, through the time stabilization time, storage life, shelf-life prolong; (2) stability to ultraviolet light significantly promotes, and can reduce the ultraviolet light photodissociation in the medication process, keeps drug effect better; (3) the solid lipid nano emamectin-benzoate has better compatibility to plant leaf blade, is more conducive to the target transportation, improves absorption ratio; During (4) as foliage-spray, the biochemical degradation metabolism under the blade top layer of solid lipid nano emamectin-benzoate slows down, and bin stability significantly promotes, and has prolonged the drug effect phase; During (5) as Ji Shi or seed dressing, solid lipid nano emamectin-benzoate stability promotes, and the drug effect phase prolongs, and control efficiency significantly promotes; (6) dosage reduces, and helps delaying drug resistance and environmental protection.
Embodiment
In order to make purpose of the present invention, technical scheme and advantage clearer, the present invention describes with following specific embodiment, but the present invention is limited to these examples absolutely not.The following stated only is the present invention embodiment preferably, only is used to explain the present invention, can not therefore be interpreted as the restriction to claim of the present invention.Should be pointed out that all any modifications of being made within the spirit and principles in the present invention, be equal to replacement and improvement etc., all should be included within protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with appended claims.
One, the preparation of the female powder of solid lipid nano emamectin-benzoate
The female powder of embodiment 1:4% solid lipid nano emamectin-benzoate
The content of emamectin-benzoate is 40 gram/kilograms
The content of capric acid is 785 gram/kilograms
Polyvinyl alcohol content is 165 gram/kilograms
Former medicine 41.5 grams of 97% emamectin-benzoate and 785 gram capric acid are dissolved in the 100 gram isopropyl alcohols together, mix with 2200 grams, 7.5% polyvinyl alcohol water solution then, by stirring mixed liquor is mixed and be the emulsification shape, use littleization of ultrasonic then, stir 2 hours female powder of last obtained by freeze drying 4% solid lipid nano emamectin-benzoate again.
The female powder of embodiment 2:8% solid lipid nano emamectin-benzoate
The content of emamectin-benzoate is 80 gram/kilograms
Lauric content is 760 gram/kilograms
Polyvinyl alcohol content is 160 gram/kilograms
Former medicine 82.5 grams of 97% emamectin-benzoate and 760 gram lauric acid are dissolved in the 200 gram isopropyl alcohols together, mix with 2000 grams, 8% polyvinyl alcohol water solution then, by high shear mixed liquor is mixed to the emulsification shape, use littleization of ultrasonic then, stir after 3.5 hours and make the female powder of 8% solid lipid nano emamectin-benzoate through vacuum drying again.
The female powder of embodiment 3:12% solid lipid nano emamectin-benzoate
The content of emamectin-benzoate is 120 gram/kilograms
The content of palmitic acid is 700 gram/kilograms
Polyvinyl alcohol content is 180 gram/kilograms
Former medicine 124 grams of 97% emamectin-benzoate and 700 gram palmitic acid are dissolved in the 300 gram isopropyl alcohols together, mix with 2000 grams, 9% polyvinyl alcohol water solution then, by vibration mixed liquor is mixed to the emulsification shape, use littleization of ultrasonic then, stir the spray-dried more female powder of 12% solid lipid nano emamectin-benzoate that makes after 5 hours.
The female powder of embodiment 4:12% solid lipid nano emamectin-benzoate
The content of emamectin-benzoate is 120 gram/kilograms
The content of arachidic acid is 700 gram/kilograms
Polyvinyl alcohol content is 180 gram/kilograms
Former medicine 124 grams of 97% emamectin-benzoate and 700 gram arachidic acids are dissolved in the 300 gram isopropyl alcohols together, mix with 2000 grams, 9% polyvinyl alcohol water solution then, by vibration mixed liquor is mixed to the emulsification shape, use littleization of ultrasonic then, stir after 5 hours the more female powder of obtained by freeze drying 12% solid lipid nano emamectin-benzoate.
The female powder of embodiment 5:12% solid lipid nano emamectin-benzoate
The content of emamectin-benzoate is 120 gram/kilograms
Stearic content is 700 gram/kilograms
Polyvinyl alcohol content is 180 gram/kilograms
Former medicine 124 grams of 97% emamectin-benzoate and 700 gram stearic acid are dissolved in the 300 gram isopropyl alcohols together, mix with 2000 grams, 9% polyvinyl alcohol water solution then, by vibration mixed liquor is mixed to the emulsification shape, use littleization of ultrasonic then, stir after 5 hours and make the female powder of 12% solid lipid nano emamectin-benzoate through vacuum drying again.
Two, complex composition preparation method and cold and hot storage decomposition, ultraviolet light photodissociation, the living survey are tested
The used pesticide active ingredient of following examples except that have indicate all by 100% purity meter, in practical operation, convert according to the actual purity of used former medicine, difference is adjusted with filler or water.
Embodiment 6:30.5% Acarus tritici urea lipid nanometer emamectin benzoate water dispersible granule preparation method
Acarus tritici urea 30% (weight)
12% lipid nanometer first dimension salt 4.2% (weight) (first dimension salt rolls over hundred 0.5%)
Lignosulfonates 5% (weight)
Lauryl sodium sulfate 8% (weight)
Cyclodextrin 5% (weight)
Urea 3% (weight)
Polyethylene glycol 3% (weight)
Diatomite is supplied 100% (weight)
Said mixture is evenly mixed, and comminution by gas stream adds suitable quantity of water and mediates, and the mixture pelleting of gained, is drying to obtain product.
The stability and the biological test of pesticide effectiveness of embodiment 6 obtained products:
Cold and hot storage stability test:
30.5% Acarus tritici urea lipid nanometer emamectin benzoate water dispersible granule and 30.5% common Acarus tritici urea emamectin benzoate water dispersible granule are carried out cold and hot storage experiment simultaneously with more stable property.
Laboratory sample is cutd open the bottle encapsulation with 6 peaces, get 2 encapsulation samples and in 54 ℃ of constant temperature ovens, do the heat storage, get 2 and in 0 ℃ of refrigerator, do cold storage, get 2 and at room temperature place.Took out the contrast resolution ratio of handling cold storage sample of sample determination and heat storage sample in 14 days later on.Experimental result such as following table:
Table 6-1 Acarus tritici urea lipid nanometer first dimension salt and the cold and hot storage stability of common Acarus tritici urea first dimension salt are relatively
Annotate: component content * 100% to be detected in cold and hot storage contrast resolution ratio=(composition to be detected in component content to be detected in the cold storage sample-Re storage sample)/cold storage sample; Cold storage sample was stored 14 days under 0 ℃ of condition, and heat storage sample detects after storing 14 days under 54 ℃ of conditions.
The ultraviolet light photolysis experiments:
Uviol lamp while treatment with irradiation sample with 2 parallel 30W, ultraviolet lamp tube center position liquid level of solution distance is 40cm, measure the absorbance of each material and calculate remaining emamectin-benzoate amount under its different irradiations at corresponding ultraviolet absorption peak place respectively with high performance liquid chromatography with ultraviolet specrophotometer, conclusion sees the following form.
Table 6-2 Acarus tritici urea lipid nanometer first dimension salt and common Acarus tritici urea first dimension salt ultraviolet light are relatively stable down
Biological effect experiment:
For clear and definite Acarus tritici urea lipid nanometer emamectin benzoate water dispersible granule and common Acarus tritici urea first dimension salt pair cotton bollworm control difference on effect, carried out drug effect test of field zone.
Handle 6000 times of 1:30.5% Acarus tritici urea lipid nanometer emamectin benzoate water dispersible granules
Handle 2: 6000 times of common 30.5% Acarus tritici urea emamectin benzoate water dispersible granules
Handle 3: blank
The effect of table 6-3 different disposal control cotton bollworm
Below the experimental technique that adopted of cold and hot storage stability test and the ultraviolet light photolysis experiments of each embodiment and condition etc. identical with present embodiment, experimental result is only listed in therefore explanation no longer one by one.
Embodiment 7:10.1% Acarus tritici urea lipid nanometer first dimension salt suspension agent preparation method
Acarus tritici urea 10% (weight)
4% lipid nanometer first dimension salt 2.5% (weight) (first dimension salt rolls over hundred 0.1%)
JFC 6% (weight)
600# 2% (weight)
Ethylene glycol 5% (weight)
Water is supplied 100% (weight)
Various compositions are mixed, in sand mill, be ground to the active ingredient particle diameter less than 4 μ m.
The above embodiment stability and the biological test of pesticide effectiveness:
Cold and hot storage stability test:
Dimension salt suspension agent of 10.1% Acarus tritici urea lipid nanometer first and common 10.1% Acarus tritici urea first dimension salt suspension agent are carried out cold and hot storage experiment simultaneously with more stable property, experimental result such as following table:
Table 7-1 Acarus tritici urea lipid nanometer first dimension salt and the cold and hot storage stability of common Acarus tritici urea first dimension salt are relatively
The ultraviolet light photolysis experiments:
Table 7-2 Acarus tritici urea lipid nanometer first dimension salt and common Acarus tritici urea first dimension salt ultraviolet light are relatively stable down
Biological effect experiment:
For the control efficiency difference of clear and definite Acarus tritici urea lipid nanometer first dimension salt suspension agent and common Acarus tritici urea first dimension salt pair cotton bollworm, carried out drug effect test of field zone.
Handle 2000 times of 1:10.1% Acarus tritici urea lipid nanometer first dimension salt suspension agent
Handle 2: 2000 times of common 10.1% Acarus tritici urea first dimension salt suspension agent
Handle 3: blank
The effect of table 7-3 different disposal control cotton bollworm
Embodiment 830% Acarus tritici urea lipid nanometer first dimension salt wetting powder preparation method
Acarus tritici urea 29.5% (weight)
4% lipid nanometer first dimension salt 12.5% (weight) (first dimension salt rolls over hundred 0.5%)
Calcium lignosulfonate 13% (weight)
Lauryl sodium sulfate 3% (weight)
Draw back powder 5% (weight)
Kaolin is supplied 100% (weight)
Mentioned component is mixed, behind comminution by gas stream, cross 325 mesh sieves and promptly get product.
The above embodiment stability and the biological test of pesticide effectiveness:
Cold and hot storage stability test:
30% Acarus tritici urea lipid nanometer first dimension salt wetting powder and common 30% Acarus tritici urea first dimension salt wetting powder are carried out cold and hot storage experiment simultaneously with more stable property, experimental result such as following table:
Table 8-1 Acarus tritici urea lipid nanometer first dimension salt and the cold and hot storage stability of common Acarus tritici urea first dimension salt are relatively
The ultraviolet light photolysis experiments:
Table 8-2 Acarus tritici urea lipid nanometer first dimension salt and common Acarus tritici urea first dimension salt ultraviolet light are relatively stable down
Biological effect experiment:
For the control efficiency difference of clear and definite Acarus tritici urea lipid nanometer first dimension salt wetting powder and common Acarus tritici urea first dimension salt pair cotton bollworm, carried out drug effect test of field zone.
Handle 6000 times of 1:30% Acarus tritici urea lipid nanometer first dimension salt wetting powders
Handle 2: 6000 times of common 30% Acarus tritici urea first dimension salt wetting powders
Handle 3: blank
The effect of table 8-3 different disposal control cotton bollworm
Embodiment 9:25% indenes worm prestige lipid nanometer emamectin benzoate water dispersible granule preparation method
Indenes worm prestige 24.5% (weight)
4% lipid nanometer first dimension salt 12.5% (weight) (first dimension salt rolls over hundred 0.5%)
Lignosulfonates 20% (weight)
Lauryl sodium sulfate 10% (weight)
Ammonium sulfate 5% (weight)
Diatomite is supplied 100% (weight)
Said mixture is evenly mixed, and comminution by gas stream adds suitable quantity of water and mediates, and the mixture pelleting of gained, is drying to obtain product.
The above embodiment stability and the biological test of pesticide effectiveness:
Cold and hot storage stability test:
25% indenes worm prestige lipid nanometer emamectin benzoate water dispersible granule and 25% common indenes worm prestige emamectin benzoate water dispersible granule are carried out cold and hot storage experiment simultaneously with more stable property, experimental result such as following table:
Table 9-1 indenes worm prestige lipid nanometer first dimension salt and the cold and hot storage stability of common indenes worm prestige first dimension salt are relatively
The ultraviolet light photolysis experiments:
Table 9-2 indenes worm prestige lipid nanometer first dimension salt and common indenes worm prestige first dimension salt ultraviolet light are relatively stable down
Biological effect experiment:
For the control efficiency difference of clear and definite indenes worm prestige lipid nanometer emamectin benzoate water dispersible granule and common indenes worm prestige first dimension salt pair diamond-back moth, carried out drug effect test of field zone.
Handle 4000 times of 1:25% indenes worm prestige lipid nanometer emamectin benzoate water dispersible granules
Handle 2: 4000 times of common 25% indenes worm prestige emamectin benzoate water dispersible granules
Handle 3: blank
The effect of table 9-3 different disposal control diamond-back moth
Embodiment 10:8% indenes worm prestige lipid nanometer first dimension salt suspension agent preparation method
Indenes worm prestige 7.9% (weight)
4% lipid nanometer first dimension salt 2.5% (weight) (first dimension salt rolls over hundred 0.1%)
Sodium lignin sulfonate 5% (weight)
Fatty alcohol-polyoxyethylene ether 15% (weight)
Xanthans 2% (weight)
Water is supplied 100% (weight)
Various compositions are mixed, in sand mill, be ground to the active ingredient particle diameter less than 4 μ m.
The above embodiment stability and the biological test of pesticide effectiveness:
Cold and hot storage stability test:
Dimension salt suspension agent of 8% indenes worm prestige lipid nanometer first and common 8% indenes worm prestige first dimension salt suspension agent are carried out cold and hot storage experiment simultaneously with more stable property, experimental result such as following table:
Table 10-1 indenes worm prestige lipid nanometer first dimension salt and the cold and hot storage stability of common indenes worm prestige first dimension salt are relatively
The ultraviolet light photolysis experiments:
Table 10-2 indenes worm prestige lipid nanometer first dimension salt and common indenes worm prestige first dimension salt ultraviolet light are relatively stable down
Biological effect experiment:
For the control efficiency difference of clear and definite indenes worm prestige lipid nanometer first dimension salt suspension agent and common indenes worm prestige first dimension salt pair diamond-back moth, carried out drug effect test of field zone.
Handle 1000 times of 1:8% indenes worm prestige lipid nanometer first dimension salt suspension agent
Handle 2: 1000 times of common 8% indenes worm prestige first dimension salt suspension agent
Handle 3: blank
The effect of table 10-3 different disposal control diamond-back moth
Embodiment 11:15% indenes worm prestige lipid nanometer first dimension salt wetting powder preparation method
Indenes worm prestige 14.5% (weight)
4% lipid nanometer first dimension salt 12.5% (weight) (first dimension salt rolls over hundred 0.5%)
Lauryl sodium sulfate 5% (weight)
Lignosulfonates 5% (weight)
Kaolin is supplied 100% (weight)
Mentioned component is mixed, behind comminution by gas stream, cross 325 mesh sieves and promptly get product.
The above embodiment stability and the biological test of pesticide effectiveness:
Cold and hot storage stability test:
15% indenes worm prestige lipid nanometer first dimension salt wetting powder and common 15% indenes worm prestige first dimension salt wetting powder are carried out cold and hot storage experiment simultaneously with more stable property.
Table 11-1 indenes worm prestige lipid nanometer first dimension salt and the cold and hot storage stability of common indenes worm prestige first dimension salt are relatively
The ultraviolet light photolysis experiments:
Table 11-2 indenes worm prestige lipid nanometer first dimension salt and common indenes worm prestige first dimension salt ultraviolet light are relatively stable down
Biological effect experiment:
For the control efficiency difference of clear and definite indenes worm prestige lipid nanometer first dimension salt wetting powder and common indenes worm prestige first dimension salt pair diamond-back moth, carried out drug effect test of field zone.
Handle 3000 times of 1:15% indenes worm prestige lipid nanometer first dimension salt suspension agent
Handle 2: 3000 times of common 15% indenes worm prestige first dimension salt suspension agent
Handle 3: blank
The effect of table 11-3 different disposal control diamond-back moth
Embodiment 12:10% pleocidin lipid nanometer emamectin benzoate water dispersible granule preparation method
Pleocidin 8% (weight)
4% lipid nanometer first dimension salt 50% (weight) (first dimension salt rolls over hundred 2%)
Lauryl sodium sulfate 8% (weight)
Lignosulfonates 8% (weight)
Cyclodextrin 5% (weight)
Diatomite is supplied 100% (weight)
Said mixture is evenly mixed, and comminution by gas stream adds suitable quantity of water and mediates, and the mixture pelleting of gained, is drying to obtain product.
The above embodiment stability and the biological test of pesticide effectiveness:
Cold and hot storage stability test:
10% pleocidin lipid nanometer emamectin benzoate water dispersible granule and 10% common pleocidin emamectin benzoate water dispersible granule are carried out cold and hot storage experiment simultaneously with more stable property.
Table 12-1 pleocidin lipid nanometer first dimension salt and the cold and hot storage stability of common pleocidin first dimension salt are relatively
The ultraviolet light photolysis experiments:
Table 12-2 pleocidin lipid nanometer first dimension salt and common pleocidin first dimension salt ultraviolet light stability are relatively
Biological effect experiment:
For the control efficiency difference of clear and definite pleocidin lipid nanometer emamectin benzoate water dispersible granule and common pleocidin first dimension salt pair diamond-back moth, carried out drug effect test of field zone.
Handle 8000 times of 1:10% pleocidin lipid nanometer emamectin benzoate water dispersible granules
Handle 2: 8000 times of common 10% pleocidin emamectin benzoate water dispersible granules
Handle 3: blank
The effect of table 12-3 different disposal control diamond-back moth
The agent of embodiment 13:15% pleocidin lipid nanometer first dimension salt suspension
12% lipid nanometer first dimension salt 42% (weight) (first dimension salt rolls over hundred 5%)
Pleocidin 10% (weight)
Farming newborn 600# 5% (weight)
JFC 4% (weight)
Water is supplied 100% (weight)
Various compositions are mixed, in sand mill, be ground to the active ingredient particle diameter less than 4 μ m.
The above embodiment stability and the biological test of pesticide effectiveness:
Cold and hot storage stability test:
Dimension salt suspension agent of 15% pleocidin lipid nanometer first and common 15% pleocidin first dimension salt suspension agent are carried out cold and hot storage experiment simultaneously with more stable property.
Table 13-1 pleocidin lipid nanometer first dimension salt and the cold and hot storage stability of common pleocidin first dimension salt are relatively
The ultraviolet light photolysis experiments:
Table 13-2 pleocidin lipid nanometer first dimension salt and common pleocidin first dimension salt ultraviolet light stability are relatively
Biological effect experiment:
For the control efficiency difference of clear and definite pleocidin lipid nanometer first dimension salt suspension agent and common pleocidin first dimension salt pair diamond-back moth, carried out drug effect test of field zone.
Handle 10000 times of 1:15% pleocidin lipid nanometer first dimension salt suspension agent
Handle 2: 10000 times of common 15% pleocidin first dimension salt suspension agent
Handle 3: blank
The effect of table 13-3 different disposal control diamond-back moth
Embodiment 14:20% pleocidin lipid nanometer first dimension salt wetting powder
Pleocidin 19% (weight)
12% lipid first dimension salt 8.5% (weight) (first dimension salt rolls over hundred 1%)
Lauryl sodium sulfate 6% (weight)
Calcium lignosulfonate 6% (weight)
Nekal BX 3% (weight)
Diatomite is supplied 100% (weight)
Various compositions are mixed, promptly obtain product by 325 mesh sieves through comminution by gas stream.
The above embodiment stability and the biological test of pesticide effectiveness:
Cold and hot storage stability test:
20% pleocidin lipid nanometer first dimension salt wetting powder and common 20% pleocidin first dimension salt wetting powder are carried out cold and hot storage experiment simultaneously with more stable property.
Table 14-1 pleocidin lipid nanometer first dimension salt and the cold and hot storage stability of common pleocidin first dimension salt are relatively
The ultraviolet light photolysis experiments:
Table 14-2 pleocidin lipid nanometer first dimension salt and common pleocidin first dimension salt ultraviolet light stability are relatively
Biological effect experiment:
For the control efficiency difference of clear and definite pleocidin lipid nanometer first dimension salt wetting powder and common pleocidin first dimension salt pair diamond-back moth, carried out drug effect test of field zone.
Handle 9000 times of 1:20% pleocidin lipid nanometer first dimension salt wetting powders
Handle 2: 9000 times of common 20% pleocidin first dimension salt wetting powders
Handle 3: blank
The effect of table 14-3 different disposal control diamond-back moth
Embodiment 15:10% capillary lipid nanometer first dimension salt suspension agent preparation method
12% lipid nanometer first dimension salt 42% (weight) (first dimension salt rolls over hundred 5%)
Capillary 5% (weight)
Sodium lignin sulfonate 4% (weight)
Xanthans 0.2% (weight)
JFC 5% (weight)
Water is supplied 100% (weight)
Mix back ball milling 2～3 hours in ball mill, particle diameter is all got final product below 4 μ m.
The above embodiment stability and the biological test of pesticide effectiveness:
Cold and hot storage stability test:
10% lipid nanometer first dimension salt capillary suspending agent and common 10% first dimension salt capillary suspending agent are carried out cold and hot storage experiment simultaneously with more stable property.
Table 15-1 capillary lipid nanometer first dimension salt and the cold and hot storage stability of common capillary first dimension salt are relatively
The ultraviolet light photolysis experiments:
Table 15-2 capillary lipid nanometer first dimension salt and common capillary first dimension salt ultraviolet light are relatively stable down
Biological effect experiment:
For the control efficiency difference of clear and definite capillary lipid nanometer emamectin benzoate water dispersible granule and common capillary first dimension salt pair beet armyworm, carried out drug effect test of field zone.
Handle 5000 times of 1:10% lipid nanometer first dimension salt capillary suspending agents
Handle 2: 5000 times of common 10% first dimension salt capillary suspending agents
Handle 3: blank
The effect of table 15-3 different disposal control beet armyworm
Embodiment 16:30% capillary lipid nanometer emamectin benzoate water dispersible granule preparation method
Capillary 26% (weight)
12% lipid nanometer first dimension salt 34% (weight) (first dimension salt rolls over hundred 4%)
Lignosulfonates 10% (weight)
Lauryl sodium sulfate 5% (weight)
Ammonium sulfate 5% (weight)
Diatomite is supplied 100% (weight)
Said mixture is evenly mixed, and comminution by gas stream adds suitable quantity of water and mediates, and the mixture pelleting of gained, is drying to obtain product.
The above embodiment stability and the biological test of pesticide effectiveness:
Cold and hot storage stability test:
30% capillary lipid nanometer emamectin benzoate water dispersible granule and 30% common capillary emamectin benzoate water dispersible granule are carried out cold and hot storage experiment simultaneously with more stable property.
Table 16-1 capillary lipid nanometer first dimension salt and the cold and hot storage stability of common capillary first dimension salt are relatively
The ultraviolet light photolysis experiments:
Table 16-2 capillary lipid nanometer first dimension salt and common capillary first dimension salt ultraviolet light are relatively stable down
Biological effect experiment:
For the control efficiency difference of clear and definite capillary lipid nanometer emamectin benzoate water dispersible granule and common capillary first dimension salt pair beet armyworm, carried out drug effect test of field zone.
Handle 6000 times of 1:30% capillary lipid nanometer emamectin benzoate water dispersible granules
Handle 2: 6000 times of common 30% capillary emamectin benzoate water dispersible granules
Handle 3: blank
The effect of table 16-3 different disposal control beet armyworm
Embodiment 17:30% capillary lipid nanometer first dimension salt wetting powder preparation method
Capillary 28% (weight)
8% lipid nanometer first dimension salt 25% (weight) (first dimension salt rolls over hundred 2%)
Calcium lignosulfonate 13% (weight)
Lauryl sodium sulfate 3% (weight)
Draw back powder 5% (weight)
Kaolin is supplied 100% (weight)
Various compositions are mixed, promptly obtain product by 325 mesh sieves through comminution by gas stream.
The above embodiment stability and the biological test of pesticide effectiveness:
Cold and hot storage stability test:
30% capillary lipid nanometer first dimension salt wetting powder and common 30% capillary first dimension salt wetting powder are carried out cold and hot storage experiment simultaneously with more stable property.
Table 17-1 capillary lipid nanometer first dimension salt and the cold and hot storage stability of common capillary first dimension salt are relatively
The ultraviolet light photolysis experiments:
Table 17-2 capillary lipid nanometer first dimension salt and common capillary first dimension salt ultraviolet light are relatively stable down
Biological effect experiment:
For the control efficiency difference of clear and definite capillary lipid nanometer first dimension salt wetting powder and common capillary first dimension salt pair beet armyworm, carried out drug effect test of field zone.
Handle 5000 times of 1:30% capillary lipid nanometer first dimension salt wetting powders
Handle 2: 5000 times of common 30% capillary first dimension salt wetting powders
Handle 3: blank
The effect of table 17-3 different disposal control beet armyworm
Embodiment 18:5% Rynaxypyr lipid nanometer emamectin benzoate water dispersible granule
Rynaxypyr 4% (weight)
4% lipid nanometer first dimension salt 25% (weight) (first dimension salt rolls over hundred 1%)
Lauryl sodium sulfate 6% (weight)
Lignosulfonates 6% (weight)
Urea 5% (weight)
Polyethylene glycol 3% (weight)
Diatomite is supplied 100% (weight)
Said mixture is evenly mixed, and comminution by gas stream adds suitable quantity of water and mediates, and the mixture pelleting of gained, is drying to obtain product.
The above embodiment stability and the biological test of pesticide effectiveness:
Cold and hot storage stability test:
5% Rynaxypyr lipid nanometer emamectin benzoate water dispersible granule and 5% common Rynaxypyr emamectin benzoate water dispersible granule are carried out cold and hot storage experiment simultaneously with more stable property.
Table 18-1 Rynaxypyr lipid nanometer first dimension salt
Compare with the cold and hot storage stability of common Rynaxypyr first dimension salt
The ultraviolet light photolysis experiments:
Table 18-2 Rynaxypyr lipid nanometer first dimension salt and common Rynaxypyr first dimension salt
Ultraviolet light stability down compares
Biological effect experiment:
For clear and definite Rynaxypyr lipid nanometer emamectin benzoate water dispersible granule and common Rynaxypyr emamectin benzoate water dispersible granule to the control efficiency difference of rice leaf roller, carried out drug effect test of field zone.
Handle 2500 times of 1:5% Rynaxypyr lipid nanometer emamectin benzoate water dispersible granules
Handle 2: 2500 times of common 5% Rynaxypyr emamectin benzoate water dispersible granules
Handle 3: blank
The effect of table 18-3 different disposal control rice leaf roller
The agent of embodiment 19:5% Rynaxypyr lipid nanometer first dimension salt suspension
Rynaxypyr 4% (weight)
4% lipid nanometer first dimension salt 25% (weight) (first dimension salt rolls over hundred 1%)
Ethylene glycol 5% (weight)
JFC 11% (weight)
600# 7% (weight)
Water is supplied 100% (weight)
Various compositions are mixed, in sand mill, be ground to the active ingredient particle diameter less than 4 μ m.
The above embodiment stability and the biological test of pesticide effectiveness:
Cold and hot storage stability test:
Dimension salt suspension agent of 5% Rynaxypyr lipid nanometer first and common 5% Rynaxypyr first dimension salt suspension agent are carried out cold and hot storage experiment simultaneously with more stable property.
Table 19-1 Rynaxypyr lipid nanometer first dimension salt and the cold and hot storage stability of common Rynaxypyr first dimension salt are relatively
The ultraviolet light photolysis experiments:
Table 19-2 Rynaxypyr lipid nanometer first dimension salt and common Rynaxypyr first dimension salt ultraviolet light are relatively stable down
Biological effect experiment:
Tie up the control efficiency difference of salt suspension agent for salt suspension agent of clear and definite Rynaxypyr lipid nanometer first dimension and common Rynaxypyr first, carried out drug effect test of field zone rice leaf roller.
Handle 2500 times of 1:5% Rynaxypyr lipid nanometer first dimension salt suspension agent
Handle 2: 2500 times of common 5% Rynaxypyr first dimension salt suspension agent
Handle 3: blank
The effect of table 19-3 different disposal control rice leaf roller
Embodiment 20:5% Rynaxypyr lipid nanometer first dimension salt wetting powder
Rynaxypyr 4% (weight)
4% lipid nanometer first dimension salt 25% (weight) (folding first dimension salt 1%)
Lauryl sodium sulfate 5% (weight)
Lignosulfonates 7% (weight)
Nekal BX 2.5% (weight)
Kaolin is supplied 100% (weight)
Various compositions are mixed, promptly obtain product by 325 mesh sieves through comminution by gas stream.
The above embodiment stability and the biological test of pesticide effectiveness:
Cold and hot storage stability test:
5% Rynaxypyr lipid nanometer first dimension salt wetting powder and common 5% Rynaxypyr first dimension salt wetting powder are carried out cold and hot storage experiment simultaneously with more stable property.
Table 20-1 Rynaxypyr lipid nanometer first dimension salt and the cold and hot storage stability of common Rynaxypyr first dimension salt are relatively
The ultraviolet light photolysis experiments:
Table 20-2 Rynaxypyr lipid nanometer first dimension salt and common Rynaxypyr first dimension salt ultraviolet light are relatively stable down
Biological effect experiment:
For the control efficiency difference of clear and definite Rynaxypyr lipid nanometer first dimension salt wetting powder and common Rynaxypyr first dimension salt pair rice leaf roller, carried out drug effect test of field zone.
Handle 2000 times of 1:5% Rynaxypyr lipid nanometer first dimension salt wetting powders
Handle 2: 2000 times of common 5% Rynaxypyr first dimension salt wetting powders
Handle 3: blank
The effect of table 20-3 different disposal control rice leaf roller
Cold and hot storage stability test by above embodiment, ultraviolet light stability test and the test of pesticide effectiveness be as can be seen: the agriculture chemical compounding composition chemical stability for preparing as stated above with solid lipid nano emamectin-benzoate of the present invention is good, resolution ratio is low under UV-irradiation, and drug effect has significant lifting.
Remarks: go down rate and preventive effect computing formula of the insect population in this specification is respectively:
Claims (10)
1. emamectin benzoate solid lipid nanoparticle, it is characterized in that: it comprises following components in weight percentage: emamectin-benzoate 1%-15%, fatty acid 30%-80% and polyvinyl alcohol 5%-25%; Described fatty acid is to contain carbon number more than 10, fusing point at the plant resource fatty acid more than 30 ℃.
2. emamectin benzoate solid lipid nanoparticle according to claim 1 is characterized in that: described fatty acid is at least a in capric acid, lauric acid, arachidic acid, stearic acid, the palmitic acid.
3. method for preparing claim 1 or 2 described emamectin benzoate solid lipid nanoparticles, it is characterized in that: be dissolved in emamectin-benzoate and fatty acid in the organic solvent together, the concentration that makes emamectin-benzoate is 1%-15%, and the concentration of fatty acid is 30%-80%; The polyvinyl alcohol water is made into the aqueous solution that concentration is 0.1%-10%; With above-mentioned organic solution and polyvinyl alcohol water solution in proportion 1: 3-1: 10 mix, and with mixed liquor emulsification, use littleization of ultrasonic again, and stirring after 1-20 hour again, drying makes.
4. the preparation method of emamectin benzoate solid lipid nanoparticle according to claim 3, it is characterized in that: described organic solvent is isopropyl alcohol or ethyl acetate, with mixed liquor emulsification is that mode by stirring or vibration or high shear realizes, described drying means is a boulton process, or freeze-drying, or spray drying process.
5. pesticidal preparations that uses the preparation of the described emamectin benzoate solid lipid nanoparticle of claim 1, it is characterized in that: described pesticidal preparations is water dispersible granules, suspending agent or wetting powder.
6. emamectin benzoate solid lipid nanoparticle pesticidal preparations according to claim 5, it is characterized in that: also contain the active ingredient X of another non-lipid nanometerization in the described preparation, the weight ratio of solid lipid nano emamectin-benzoate and active ingredient X is 1: 1-800.
7. emamectin benzoate solid lipid nanoparticle pesticidal preparations according to claim 6 is characterized in that: described active ingredient X is any in Acarus tritici urea, indenes worm prestige, pleocidin, capillary, the Rynaxypyr.
8. according to claim 5,6 or 7 described emamectin benzoate solid lipid nanoparticle pesticidal preparations, it is characterized in that: the water dispersible granules of described solid lipid nano emamectin-benzoate preparation, it is formed and also comprise the surfactant that accounts for weight of formulation 1%-10%, the auxiliary agent of 1%-5%, the disintegrant of 0%-15%, the adhesive of 1%-5% and the carrier of 1%-80% except that active ingredient; Described surfactant comprises lignosulfonates, lauryl sodium sulfate, fatty acid sulphate, aliphatic alcohol polyethenoxy, nekal, in the dodecyl polyoxyethylene ether phosphate one or more, described auxiliary agent comprises the benzylphenol APEO, Tea Saponin, in the alkylphenol polyoxyethylene one or more, described disintegrant comprises bentonite, ammonium sulfate, urea, in the magnesium sulfate one or more, described carrier comprises diatomite, kaolin, white carbon, a kind of in the nacrite, described adhesive comprises polyethylene glycol, cyclodextrin, starch, a kind of in the sodium silicate.
9. according to claim 5,6 or 7 described emamectin benzoate solid lipid nanoparticle pesticidal preparations, it is characterized in that: the suspending agent of described solid lipid nano emamectin-benzoate preparation, it is formed and also comprise the surfactant that accounts for weight of formulation 1%-10%, the auxiliary agent of 1%-5% and the carrier of 1%-80% except that active ingredient; Described surfactant is one or more in fatty alcohol-polyoxyethylene ether (JFC), phenethyl phenol APEO (602#, 603#, 600#), alkylphenol polyoxyethylene or its phosphate, fatty alcohol-polyoxyethylene ether, lignosulfonates, the naphthalenesulfonate formaldehyde condensation compound; Described auxiliary agent comprises antifreeze ethylene glycol, thickener xanthans, defoamer silicone; Described carrier is a water.
10. according to claim 5,6 or 7 described emamectin benzoate solid lipid nanoparticle pesticidal preparations, it is characterized in that: the wetting powder of described solid lipid nano emamectin-benzoate preparation, it is formed and also include the surfactant that accounts for weight of formulation 1%-10%, the carrier of 1%-80% except that active ingredient; Described surfactant comprises lignosulfonates, lauryl sodium sulfate, fatty acid sulphate, aliphatic alcohol polyethenoxy, nekal, benzylphenol APEO, alkylphenol polyoxyethylene, draw back in the powder one or more, and described carrier comprises one or more in kaolin, precipitated calcium carbonate, clay, the white carbon.
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