CN105145553A - Indissolvable pesticide solid dispersion composition - Google Patents
Indissolvable pesticide solid dispersion composition Download PDFInfo
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Abstract
The invention relates to indissolvable pesticide solid dispersion. The solid dispersion comprises an indissolvable pesticide, a solubilizer and a macromolecular carrier, wherein the weight ratio of the indissolvable pesticide to the solubilizer to the macromolecular carrier is (1-10):(1-10):(80-98); the indissolvable pesticide mainly comprises one of cypermethrin, deltamethrin, bifenthrin, efficient cyhalothrin, indoxacarb, abamectin, abamectin-aminomethyl, chlorfenapyr, chlorpyrifos, lufenuron, fipronil, Dufulin, azoxystrobin and epoxiconazole. Through the adoption of the indissolvable pesticide solid dispersion, the solubility of an unprocessed indissolvable pesticide in water can be improved, the product has good uniformity, and the bioavailability of a final pesticide preparation is improved.
Description
Technical field
The present invention relates to technical field of pesticide, be specifically related to a kind of solid dispersion composition of indissoluble agricultural chemicals.
Background technology
Because indissoluble agricultural chemicals hydrophily is poor, when making preparation, usually make the form of missible oil, certain infringement is caused to environment.In order to improve the solvability of indissoluble agricultural chemicals in water, can adopt solid dispersion technology, drug micronization method, cyclodextrin forms inclusion compound, liposome.Due to drug micronization method solubilizing effect poor repeatability; Cyclodextrin and liposome cost too high, and inventor test find solid dispersion technology good, simple to operate to insoluble medicine solubilizing effect, cost is low.When preparing solid dispersions, conventional macromolecule carrier mainly contains polyethylene glycol (PEG), poly-(NVP) (PVP).Solid dispersion preparation method mainly contains fusion method, solvent method, solvent-fusion method.
In the solid pharmaceutical preparation field of indissoluble agricultural chemicals, discloseder technical schemes have at present:
Chinese patent: title: a kind of pesticide nano solid dispersions and preparation method thereof; Application Number (patent): CN201510109887.2; The applying date: 2015.03.13; Open (bulletin) number: CN104798772A; Open (bulletin) day: 2015.07.29; Application (patent right) people: Institute of Environment and Sustainable Development in Agriculture, CAAS.This invention relates to a kind of pesticide nano solid dispersions and preparation method thereof, described pesticide nano solid dispersions is made up of 0.001-90 weight portion agricultural chemicals, 0.001-50 part surfactant and 5-99.9 part water-solubility carrier, and described agricultural chemicals is selected from the insecticide of one or more slightly solubilities, bactericide, weed killer herbicide or plant growth regulator; Described solid dispersions particle diameter is less than 1 μm.Compared with prior art, pesticide dispersion particle diameter of the present invention less evenly, the better effects if that surfactant is coated to it, surface-active contents can lower than 1%, even lower than 0.1%, and maintain good dispersiveness and stability, organic solvent can be stopped completely, significantly save production cost.Not only can save Pesticide use amount by improving effective rate of utilization, and the agricultural product that significantly can reduce remains of pesticide, hazardous solvent and auxiliary agent are residual and environmental pollution, guarantee grain, food and ecological safety.Simultaneously this application also disclose " described pesticide nano solid dispersions, described insecticide is selected from pyrethroid, carbamate, organic phosphor, organic sulfur, organic choline, nereistoxin, anabasine, phenyl ureide, Avermectin, pyridaben, acequinocyl, Phenylpyrazole, indoxacarb or diafenthiuron insecticides;
Described bactericide is selected from anilino-pyridine, antibiotic, aromatic hydrocarbon, dinitroaniline, allylamine, benzsulfamide, benzimidazole, benzisothiazole, benzophenone, benzo yl pyrimidines, phentriazine, benzyq carbamate, carbamate, carboxylic acid amides, carboxylic acid diamides, chlorine nitrile, cyanoimidazole, cyclopropane carboxamide, ethylamino thiazole carboxylic acid amides, imidazoles, hydroxyl anilid, imidazolone, isobenzofuranone, methoxy acrylate, methoxycarbamate, morpholine, N-carbanilate, oxazolidinedione, phenyl-acetamides, phenyl amide, phenylpyrrole, phenylurea, thiophosphate, phthalamic acid, phthalimide, piperazine, piperidines, propionamide, pyridine, pyridylmethyl acid amides, toluamide, triazine or triazole bactericidal agent,
Described weed killer herbicide is selected from acid amides, aryloxyphenoxypropionate, benzene oxycarboxylic acid, organic phosphor, benzamide, benzofuran, benzoic acid, benzothiadiazine ketone, carbamate, chloroacetamide, picolinic acid, chlorine carboxylic acid, cyclohexanedione, dinitroaniline, diphenyl ether, isoxazole, isoxazole alkane ketone, N-phenylphthalimide, oxadiazole, oxazolidinedione, oxygen yl acetamide, carbanilate, phenyl pyridazine, sulfonylamino carboxyl Triazolinones, sulphonyl triazol carboxylic acid amides, triazolo pyrimidine, triketone, uracil or carbamide herbicides,
Described plant growth regulator is selected from maleic hydrazide, naphthalene methyl acetate, 6-benzylaminopurine, brassinosteroid, ammonia oxygen ethyl vinyl glycine or multiple-effect azole plant growth regulator.”
In patent " a kind of pesticide nano solid dispersions and preparation method thereof " (CN201510109887.2), this patent decreases the use of organic solvent, surfactant and auxiliary agent, improve dispersity and the dissolution rate of insoluble drug, but its complicated process of preparation, preparation cost is high; Solid dispersion composition preparation method of the present invention is simple, not only improves the solvability of indissoluble agricultural chemicals in water, also improves the drug effect of insoluble medicine controlling crop diseases and insect pests simultaneously.
Summary of the invention
For present technology Problems existing, the object of the present invention is to provide the solid dispersions of indissoluble agricultural chemicals, the solvability of indissoluble agricultural chemicals in water can be improved.
To achieve these goals, the invention provides following technical scheme:
A solid dispersions for indissoluble agricultural chemicals, this solid dispersions is made up of indissoluble agricultural chemicals, solubilizer and macromolecule carrier, and three's weight ratio is 1 ~ 10:1 ~ 10:80 ~ 98.
The solid dispersions of above-described indissoluble agricultural chemicals, described indissoluble agricultural chemicals is selected from the one in the insecticide of slightly solubility, bactericide.
The solid dispersions of above-described indissoluble agricultural chemicals, described insecticide is cypermethrin, decis, Biphenthrin, gamma cyhalothrin, indoxacarb, Avermectin, Affirm (Merck Co.), capillary, chlopyrifos, lufenuron, ethiprole.
The solid dispersions of above-described indissoluble agricultural chemicals, described bactericide is malicious fluorine phosphorus, Fluoxastrobin, epoxiconazole.
The solid dispersions of arbitrary described indissoluble agricultural chemicals above, described solubilizer comprises: polysorbas20, polysorbate60, Tween 80, PLURONICS F87, Brij35, Emulsifier EL-60.
The solid dispersions of arbitrary described indissoluble agricultural chemicals above, described macromolecule carrier comprises: polyethylene glycol, poly-(NVP).
The solid dispersions of above-described indissoluble agricultural chemicals, described polyethylene glycol is PEG4000, PEG6000, PEG12000, PEG20000; Described poly-(NVP) is PVPK30 and PVPK90.
A preparation method for the solid dispersions of indissoluble agricultural chemicals as above, this solid dispersions is by solvent method, fusion method, solvent-fusion method preparation.
Described solvent method, its preparation method is dissolved in suitable solvent by indissoluble agricultural chemicals, solubilizer and macromolecule carrier, volatilizing except desolventizing fast.Common solvents has: ethanol, acetone, chloroform, and addition is 0.2 ~ 2 times of insoluble medicine.
Described fusion method, its preparation method is that macromolecule carrier is heated to thawing, is then mixed with solubilizer by indissoluble agricultural chemicals, joins in macromolecule carrier, is quickly cooled to cold curing.
Described solvent-fusion method, its preparation method is that macromolecule carrier is heated to thawing, then adopts a small amount of dissolution with solvents indissoluble agricultural chemicals, mixes, join in the macromolecule carrier of thawing, removal of solvent under reduced pressure, be quickly cooled to cold curing with solubilizer.Solvent is low boiling point solvent, and kind has: methyl alcohol, ethanol, acetone, chloroform, carrene.
A kind of pesticidal preparations, described pesticidal preparations comprises the solid dispersions of above-described indissoluble agricultural chemicals, insecticides adjuvant and agricultural chemicals auxiliary element.
Relative to prior art, the present invention has following beneficial effect:
1. the solid dispersions of indissoluble agricultural chemicals of the present invention significantly improves the solvability of former medicine, relative to the solvability of former medicine, the solvability of the solid dispersions that the present invention is corresponding improves 1-1000 doubly, and improve the preventive effect of pesticidal preparations controlling disease worm, preventive effect improves more than 10%.
2 the present invention use the water soluble disperse carrier of solubilizer and the composite composition of macromolecule carrier to prepare solid dispersions, can effectively be highly dispersed in solid carrier material by insoluble drug, the solvability facilitating corresponding solid dispersions greatly improves.
3. owing to using the water soluble disperse carrier of solubilizer and the composite composition of macromolecule carrier to prepare solid dispersions, change the physical state of indissoluble agricultural chemicals, become amorphous, the supersaturation solid solution of part amorphous or medicine, thus the state of medicine high degree of dispersion can be reached; Meanwhile, and water-solubility carrier has good wetability, can promote drug-eluting, improves its solvability, therefore significant in the bioavilability improving medicine.
Embodiment
The technological means realized to make the present invention is easy to understand, and is further elaborated the present invention below in conjunction with specific embodiment.
Following examples of the present invention cypermethrin technical material, deltamethrin original medicine, the former medicine of Biphenthrin, the former medicine of gamma cyhalothrin, the former medicine of indoxacarb, the former medicine of Avermectin, the former medicine of Affirm (Merck Co.), the former medicine of capillary, the former medicine of chlopyrifos, the former medicine of lufenuron, the former medicine of ethiprole, the former medicine of malicious fluorine phosphorus, the former medicine of Fluoxastrobin, epoxiconazole raw drug and other auxiliary agents used is commercial, and is that often kind of medicament is all from the same batch products of same producer.
Embodiment 1
The present embodiment gamma cyhalothrin solid dispersions comprises the former medicine of gamma cyhalothrin, Tween 80 and PEG4000 composition, and three's weight ratio is 10:2:88.
Its preparation method is fusion method: 88gPEG4000 is heated to thawing, then joins in PEG4000 by former for 10g gamma cyhalothrin medicine and 2g Tween 80, is quickly cooled to cold curing.
Gamma cyhalothrin maximum absorption wavelength in methyl alcohol is 220nm.
Solvability detects: get some tool plug conical flasks, add the deionized water of 100mL respectively, add the gamma cyhalothrin solid dispersions (after conversion, gamma cyhalothrin is 0.5mg in proportion) of 5mg again, respectively 25 DEG C of isothermal vibrations 48 hours, after testing, in gamma cyhalothrin solid dispersions, the solvability of gamma cyhalothrin is on average 0.1320mg/L.
By the gamma cyhalothrin solid dispersions (after conversion, gamma cyhalothrin is 2.5g in proportion) of 25g, sodium metnylene bis-naphthalene sulfonate 4g, neopelex 3g, kaolin mends 100g, then co-grinding, is prepared into 2.5% gamma cyhalothrin wetting powder (being called for short medicament 1).
Embodiment 2
The present embodiment gamma cyhalothrin solid dispersions comprises the former medicine of gamma cyhalothrin, Tween 80 and PEG4000 composition, and three's weight ratio is 5:6:89.
Its preparation method is fusion method: 89gPEG4000 is heated to thawing, then joins in PEG4000 by former for 5g gamma cyhalothrin medicine and 6g Tween 80, is quickly cooled to cold curing.
In methyl alcohol, gamma cyhalothrin maximum absorption wavelength is 220nm.
Solvability detects: get some tool plug conical flasks, add the deionized water of 100mL respectively, add the gamma cyhalothrin solid dispersions (after conversion, gamma cyhalothrin is 0.5mg in proportion) of 10mg again, respectively 25 DEG C of isothermal vibrations 48 hours, in gamma cyhalothrin solid dispersions, the solvability of gamma cyhalothrin is on average 0.1432mg/L after testing.
By the gamma cyhalothrin solid dispersions (after conversion, gamma cyhalothrin is 2.5g in proportion) of 50g, sodium metnylene bis-naphthalene sulfonate 4g, neopelex 3g, kaolin mends 100g, then co-grinding, is prepared into 2.5% gamma cyhalothrin wetting powder (being called for short medicament 2).
Comparative example 1: comparative sample 1 is the former medicine of gamma cyhalothrin.
Solubility test method is: get some tool plug conical flasks, add the deionized water of 100mL respectively, then add the former medicine of 0.5mg gamma cyhalothrin, and 25 DEG C of isothermal vibrations 48 hours, the solvability of gamma cyhalothrin was on average 0.005mg/L after testing.
By the gamma cyhalothrin of 2.5g, sodium metnylene bis-naphthalene sulfonate 4g, neopelex 3g, kaolin mends 100g, then co-grinding, is prepared into 2.5% gamma cyhalothrin wetting powder (being called for short medicament 3).
Contrasted from above-mentioned 3 embodiments, the solvability of the gamma cyhalothrin in the solid dispersions of embodiment 1 improves 0.127mg/L relative to the solvability of the gamma cyhalothrin of comparative example 1; The solvability of the gamma cyhalothrin in the solid dispersions of embodiment 2 improves 0.1427mg/L relative to the solvability of the former medicine of the gamma cyhalothrin of comparative example 1.
When preventing and treating cabbage pieris, the dosage of each medicament is 120 grams/acre, and the control efficiency of 7 days investigation each sample after medicine, result is as follows: the control efficiency of medicament 1 is 85.6%, and the control efficiency of medicament 2 is 88.1%, and the control efficiency of medicament 3 is 71.8%.The control efficiency of blank (Tween 80: PEG4000=1:1) is 0.Contrasted from control efficiency, the control efficiency of medicament 1 and medicament 2 respectively higher than the control efficiency of medicament 3 by 13.8%, 16.3%.
Embodiment 3
The present embodiment cypermethrin solid dispersions comprises cypermethrin technical material, polysorbate60 and PEG6000 composition, and three's weight ratio is 10:8:82.
Its preparation method is solvent method: be dissolved in acetone by 10g cypermethrin, 8g polysorbate60 and 82gPEG6000, spraying dry removing acetone.
In methyl alcohol, measure cypermethrin maximum absorption wavelength is 230nm.
Solvability is detected as: get some tool plug conical flasks, add the deionized water of 100mL respectively, add the cypermethrin solid dispersions (after conversion, cypermethrin is 0.5mg in proportion) of 5mg again, respectively 25 DEG C of isothermal vibrations 48 hours, after testing, in cypermethrin solid dispersions, the solvability of cypermethrin is on average 0.2537mg/L.
By 25g cypermethrin solid dispersions (after conversion, cypermethrin is 2.5g in proportion), sodium lignin sulfonate 3g, neopelex 2g, kaolin mends 100g, then co-grinding, is prepared into 2.5% cypermethrin wetting powder (being called for short medicament 4).
Embodiment 4
The present embodiment cypermethrin solid dispersions comprises cypermethrin technical material, polysorbate60 and PEG6000 composition, and three's weight ratio is 4:6:90.
Its preparation method is solvent method: be dissolved in acetone by 4g cypermethrin, 6g polysorbate60 and 90gPEG6000, spraying dry removing acetone.
In methyl alcohol, measure cypermethrin maximum absorption wavelength is 230nm.
Solvability detects: get some tool plug conical flasks, add the deionized water of 100mL respectively, add the cypermethrin solid dispersions (after conversion, cypermethrin is 0.5mg in proportion) of 12.5mg again, respectively 25 DEG C of isothermal vibrations 48 hours, after testing, cypermethrin maximum absorption wavelength is 230nm, and in cypermethrin solid dispersions, the solvability of cypermethrin is on average 0.2844mg/L.
By 62.5g cypermethrin solid dispersions (after conversion, cypermethrin is 2.5g in proportion), sodium lignin sulfonate 3g, neopelex 2g, kaolin mends 100g, then co-grinding, is prepared into 2.5% cypermethrin wetting powder (being called for short medicament 5).
Comparative example 2: comparative sample 2 is cypermethrin technical material.
Solvability detects: get some tool plug conical flasks, add the deionized water of 100mL respectively, then add the comparative sample 2 of 0.5mg, respectively 25 DEG C of isothermal vibrations 48 hours, after testing, and the solvability average out to 0.013mg/L of cypermethrin.
By 2.5g cypermethrin technical material, sodium lignin sulfonate 3g, neopelex 2g, kaolin mends 100g, then co-grinding, is prepared into 2.5% cypermethrin wetting powder (being called for short medicament 6).
Contrasted from above-mentioned 3 embodiments, the solvability of the cypermethrin in the solid dispersions of embodiment 3 improves 0.2407mg/L relative to the solvability of the cypermethrin of comparative example 2; The solvability of the cypermethrin in the solid dispersions of embodiment 4 improves 0.2831mg/L relative to the solvability of the cypermethrin technical material of comparative example 2.
When preventing and treating cabbage pieris, the dosage of each medicament is 160 grams/acre, the control efficiency of 7 days investigation each sample after medicine, result is as follows: the control efficiency of medicament 4 is 79.4%, the control efficiency of medicament 5 is 75.9%, the control efficiency of medicament 6 is 64.1%, and the control efficiency of blank (polysorbate60: PEG6000=1:1) is 0.Contrasted from control efficiency, the control efficiency of medicament 4 and medicament 5 respectively higher than the control efficiency of medicament 6 by 15.3%, 11.8%.
Embodiment 5
The present embodiment Biphenthrin solid dispersions comprises the former medicine of Biphenthrin, Tween 80 and PEG12000 composition, and three's weight ratio is 10:8:82.
Its preparation method is solvent method: be dissolved in acetone by 10g Biphenthrin, 8g Tween 80 and 82gPEG12000, spraying dry removing acetone.
In methyl alcohol, measure Biphenthrin maximum absorption wavelength is 240nm.
Solvability detects: get some tool plug conical flasks, add the deionized water of 100mL respectively, add the Biphenthrin solid dispersions (after conversion, Biphenthrin is 0.5mg in proportion) of 5mg again, respectively 25 DEG C of isothermal vibrations 48 hours, in Biphenthrin solid dispersions, the solvability of Biphenthrin is on average 2.4325mg/L after testing.
By 50g Biphenthrin solid dispersions (after conversion, Biphenthrin is 5g in proportion), sodium carboxymethylcellulose 3.5g, neopelex 2g, kaolin mends 100g, then co-grinding, is prepared into 5% Biphenthrin wetting powder (being called for short medicament 7).
Comparative example 3: comparative sample 3 is the former medicine of Biphenthrin.
Solvability detects: get some tool plug conical flasks, add the deionized water of 100mL respectively, then add the comparative sample 2 of 0.5mg, respectively 25 DEG C of isothermal vibrations 48 hours, and the solvability average out to 0.1000mg/L of Biphenthrin after testing.
By 5g Biphenthrin, sodium carboxymethylcellulose 3.5g, neopelex 2g, kaolin mends 100g, then co-grinding, is prepared into 5% Biphenthrin wetting powder (being called for short medicament 8).
Contrasted from above-mentioned 2 embodiments, the solvability of the Biphenthrin in the solid dispersions of the embodiment of the present invention 5 improves 2.3325mg/L relative to the solvability of the Biphenthrin of comparative example 3.
When preventing and treating tea tree smaller green leaf hopper, the dosage of each medicament is 75 grams/acre, the control efficiency of 7 days investigation each sample after medicine, result is as follows: the control efficiency of medicament 7 is 74.7%, the control efficiency of medicament 8 is 62.3%, and the control efficiency of blank (Tween 80: PEG12000=8:82) is 0.Contrasted from control efficiency, the control efficiency of medicament 7 is higher than the control efficiency of medicament 8 by 12.4%.
Embodiment 6
The present embodiment decis solid dispersions comprises deltamethrin original medicine, PLURONICS F87 and PVPK30 composition, and three's weight ratio is 10:10:80.
Its preparation method is solvent method: be dissolved in chloroform by 10g decis, 10g PLURONICS F87 and 80gPVPK30, spraying dry removing chloroform.
In methyl alcohol, measure decis maximum absorption wavelength is 240nm.
Detection method: get some tool plug conical flasks, add the deionized water of 100mL respectively, then the decis solid dispersions (in proportion conversion after decis be 0.5mg) adding 5mg, respectively 25 DEG C of isothermal vibrations 48 hours.The solvability average out to 0.1028mg/L of decis in decis solid dispersions after testing.
By 1g decis solid dispersions (after conversion, decis is 0.1g in proportion), sodium metnylene bis-naphthalene sulfonate 2g, lauryl sodium sulfate 3g, kaolin mends 100g, then co-grinding, is prepared into 0.1% decis wetting powder (being called for short medicament 9).
Embodiment 7
The present embodiment decis solid dispersions comprises deltamethrin original medicine, PLURONICS F87 and PVPK30 composition, and three's weight ratio is 1:1:99.
Its preparation method is solvent method: be dissolved in chloroform by 1g decis, 1g PLURONICS F87 and 99gPVPK30, spraying dry removing chloroform.
In methyl alcohol, measure decis maximum absorption wavelength is 240nm.
Detection method: get some tool plug conical flasks, add the deionized water of 100mL respectively, then the decis solid dispersions (in proportion conversion after decis be 0.5mg) adding 50mg, respectively 25 DEG C of isothermal vibrations 48 hours.After testing, the solvability average out to 0.1341mg/L of decis in decis solid dispersions.
By 10g decis solid dispersions (after conversion, decis is 0.1g in proportion), sodium metnylene bis-naphthalene sulfonate 2g, lauryl sodium sulfate 3g, kaolin mends 100g, then co-grinding, is prepared into 0.1% decis wetting powder (being called for short medicament 10).
Comparative example 4: comparative sample 4 is deltamethrin original medicine
Detection method: get some tool plug conical flasks, add the deionized water of 100mL respectively, then add the comparative sample 3 of 0.5mg, respectively 25 DEG C of isothermal vibrations 48 hours.After testing, the solvability of decis is on average 0.0001mg/L.
By 1g deltamethrin original medicine, sodium metnylene bis-naphthalene sulfonate 2g, lauryl sodium sulfate 3g, kaolin mends 100g, then co-grinding, is prepared into 0.1% decis wetting powder (being called for short medicament 11).
Contrasted from above-mentioned 3 embodiments, the solvability of the decis in the solid dispersions of embodiment 6 and embodiment 7 improves 0.1027mg/L, 0.1340mg/L than the solvability of the decis of comparative example 4 respectively.
When preventing and treating a variety of Chinese cabbage cabbage caterpillar, the dosage of each medicament is 500 grams/acre, the control efficiency of 7 days investigation each sample after medicine, result is as follows: the control efficiency of medicament 9 is 70.9%, the control efficiency of medicament 10 is 71.6%, the control efficiency of medicament 11 is 56.7%, and the control efficiency of blank (PLURONICS F87: PVPK30=1:1) is-3.2%.Contrasted from control efficiency, the control efficiency of medicament 9 and medicament 10 respectively higher than the control efficiency of medicament 11 by 14.2%, 14.9%,
Embodiment 8
The present embodiment Avermectin solid dispersions comprises the former medicine of Avermectin, polysorbas20, PEG20000 and PEG12000 composition, and four weight ratios are 10:6:40:44.
In methyl alcohol, measure Avermectin maximum absorption wavelength is 245nm.
Its preparation method is solvent-fusion method: 40gPEG20000 and 44gPEG12000 is heated to thawing, is dissolved in acetone, joins in the PEG of thawing by 10g Avermectin and 6g polysorbas20, spraying dry removing acetone.
Solvability detects: get some tool plug conical flasks, add the deionized water of 100mL respectively, add the Avermectin solid dispersions (after conversion, Avermectin is 0.5mg in proportion) of 5mg more respectively, respectively 25 DEG C of isothermal vibrations 48 hours, in Avermectin solid dispersions, the solvability of Avermectin is on average 0.2800mg/L after testing.
By 20g Avermectin solid dispersions (after conversion, Avermectin is 2g in proportion), sodium metnylene bis-naphthalene sulfonate 3g, lauryl sodium sulfate 1g, kaolin mends 100g, then co-grinding, is prepared into 2% Avermectin wetting powder (being called for short medicament 12).
Embodiment 9
The present embodiment Avermectin solid dispersions comprises the former medicine of Avermectin, Tween 80, PEG6000 and PEG12000 composition, and four weight ratios are 5:6:42:47.
Its preparation method is solvent-fusion method: 42gPEG6000 and 47gPEG12000 is heated to thawing, is dissolved in acetone, joins in the PEG of thawing by 5g Avermectin and 6g Tween 80, spraying dry removing acetone.
In methyl alcohol, measure Avermectin maximum absorption wavelength is 245nm.
Solvability detects: get some tool plug conical flasks, add the deionized water of 100mL respectively, add the Avermectin solid dispersions (after conversion, Avermectin is 0.5mg in proportion) of 10mg more respectively, respectively 25 DEG C of isothermal vibrations 48 hours, after testing, Avermectin maximum absorption wavelength 245nm, in Avermectin solid dispersions, the solvability of Avermectin is on average 0.3289mg/L.
By 40g Avermectin solid dispersions (after conversion, Avermectin is 2g in proportion), sodium metnylene bis-naphthalene sulfonate 3g, lauryl sodium sulfate 1g, kaolin mends 100g, then co-grinding, is prepared into 2% Avermectin wetting powder (being called for short medicament 13).
Comparative example 5: the comparative sample 5 of the present embodiment is the former medicine of Avermectin.
Solvability detects: get some tool plug conical flasks, add the deionized water of 100mL respectively, then add 0.5mg comparative sample 5 respectively, and respectively 25 DEG C of isothermal vibrations 48 hours, Avermectin solvability is on average 0.0078mg/L after testing.
By 2g Avermectin, sodium metnylene bis-naphthalene sulfonate 3g, lauryl sodium sulfate 1g, kaolin mends 100g, then co-grinding, is prepared into 2% Avermectin wetting powder (being called for short medicament 14).
Contrasted from above-mentioned 3 embodiments, the solvability of the Avermectin in the solid dispersions of embodiment 8 and embodiment 9 improves 0.2722mg/L, 0.3211mg/L than the solvability of the Avermectin of comparative example 5 respectively.
When preventing and treating paddy rice rice leaf roller, the dosage of each medicament is 40 grams/acre, the control efficiency of 7 days investigation each sample after medicine, result is as follows: the control efficiency of medicament 12 is 76.5%, the control efficiency of medicament 13 is 77.6%, the control efficiency of medicament 14 is 61.2%, and the control efficiency of blank (polysorbas20: PEG20000:PEG12000=1:1:1) is-2.6%.Contrasted from control efficiency, the control efficiency of medicament 12 and medicament 13 respectively higher than the control efficiency of medicament 14 by 15.3%, 16.4%;
Embodiment 10
The present embodiment indoxacarb solid dispersions comprises the former medicine of indoxacarb, Brij35 and PEG4000 composition, and three's weight ratio is 10:2:88.
Its preparation method is fusion method: 88gPEG4000 is heated to thawing, then by 10g indoxacarb with 2g Brij35, mix, join in PEG4000, be quickly cooled to cold curing.
In methyl alcohol, measure indoxacarb maximum absorption wavelength is 325nm.
Solvability detects: get some tool plug conical flasks, add the deionized water of 100mL respectively, add 20mg indoxacarb solid dispersions (in proportion indoxacarb 2mg after conversion) more respectively, respectively 25 DEG C of isothermal vibrations 48 hours, after testing, indoxacarb maximum absorption wavelength is 325nm, and in indoxacarb solid dispersions, the solvability of indoxacarb is on average 9.1320mg/L.
By 50g indoxacarb solid dispersions (after conversion, indoxacarb is 5g in proportion), pull open powder 2g, lauryl sodium sulfate 2g, kaolin mends 100g, then co-grinding, is prepared into 5% indoxacarb wetting powder (being called for short medicament 15).
Embodiment 11
The present embodiment indoxacarb solid dispersions comprises the former medicine of indoxacarb, Brij35 and PEG4000 composition, and three's weight ratio is 10:8:82.
Its preparation method is fusion method: 82gPEG4000 is heated to thawing, then by 10g indoxacarb with 8g Brij35, mix, join in PEG4000, be quickly cooled to cold curing.
In methyl alcohol, measure indoxacarb maximum absorption wavelength is 325nm.
Solvability detects: get some tool plug conical flasks, add the deionized water of 100mL respectively, add 20mg indoxacarb solid dispersions (in proportion indoxacarb 2mg after conversion) more respectively, respectively 25 DEG C of isothermal vibrations 48 hours, in indoxacarb solid dispersions, the solvability of indoxacarb is on average 9.450mg/L after testing.
By 50g indoxacarb solid dispersions (after conversion, indoxacarb is 5g in proportion), pull open powder 2g, lauryl sodium sulfate 2g, kaolin mends 100g, then co-grinding, is prepared into 5% indoxacarb wetting powder (being called for short medicament 16).
Comparative example 6: the comparative sample 6 of the present embodiment is the former medicine of indoxacarb.
Solvability detects: get some tool plug conical flasks, add the deionized water of 100mL respectively, then add 2mg comparative sample 4 respectively, and respectively 25 DEG C of isothermal vibrations 48 hours, the solvability of indoxacarb is on average 0.2000mg/L after testing
By 5g indoxacarb, pull open powder 2g, lauryl sodium sulfate 2g, kaolin mends 100g, then co-grinding, is prepared into 5% indoxacarb wetting powder (being called for short medicament 17).
Contrasted from above-mentioned 3 embodiments, the solvability of the indoxacarb in the solid dispersions of embodiment 10 and embodiment 11 improves 8.9320mg/L, 9.250mg/L than the solvability of the indoxacarb of comparative example 6 respectively.
When preventing and treating wild cabbage diamond-back moth, the dosage of each medicament is 60 grams/acre, the control efficiency of 7 days investigation each sample after medicine, result is as follows: the control efficiency of medicament 15 is 89.2%, the control efficiency of medicament 16 is 87.4%, the control efficiency of medicament 17 is 68.2%, and the control efficiency of blank (Brij35: PEG4000=8:82) is-3.8%.Contrasted from control efficiency, the control efficiency of medicament 15 and medicament 16 respectively higher than the control efficiency of medicament 17 by 21%, 19.2%;
Embodiment 12
The Affirm (Merck Co.) solid dispersions of the present embodiment comprises the former medicine of Affirm (Merck Co.), Emulsifier EL-60 and PVPK90 composition, and three's weight ratio is 10:6:84.
Its preparation method is solvent method: be dissolved in chloroform by 10g Affirm (Merck Co.), 6g Emulsifier EL-60 and 84gPVPK90, spraying dry removing chloroform.
In methyl alcohol, measure Affirm (Merck Co.) maximum absorption wavelength is 245nm.
Solvability detects: get some tool plug conical flasks, add the deionized water of 100mL respectively, add 100mg Affirm (Merck Co.) solid dispersions (after conversion, Affirm (Merck Co.) is 10mg in proportion) more respectively, respectively 25 DEG C of isothermal vibrations 48 hours, in Affirm (Merck Co.) solid dispersions, the average solubility of Affirm (Merck Co.) is 45.5800mg/L after testing.
By 20g Affirm (Merck Co.) solid dispersions (after conversion, Affirm (Merck Co.) is 2g in proportion), sldium lauryl sulfate 4g, lauryl sodium sulfate 1g, kaolin mends 100g, then co-grinding, is prepared into 2% Affirm (Merck Co.) wetting powder (being called for short medicament 18).
Embodiment 13
The Affirm (Merck Co.) solid dispersions of the present embodiment comprises the former medicine of Affirm (Merck Co.), polysorbate60 and PVPK90 composition, and three's weight ratio is 5:6:89.
Its preparation method is solvent method: be dissolved in chloroform by 5g Affirm (Merck Co.), 6g polysorbate60 and 89gPVPK90, spraying dry removing chloroform.
In methyl alcohol, measure Affirm (Merck Co.) maximum absorption wavelength is 245nm.
Solvability detects: get some tool plug conical flasks, add the deionized water of 100mL respectively, add 200mg Affirm (Merck Co.) solid dispersions (after conversion, Affirm (Merck Co.) is 10mg in proportion) more respectively, respectively 25 DEG C of isothermal vibrations 48 hours, in Affirm (Merck Co.) solid dispersions, the average solubility of Affirm (Merck Co.) is 48.4412mg/L after testing.
By 40g Affirm (Merck Co.) solid dispersions (after conversion, Affirm (Merck Co.) is 2g in proportion), sldium lauryl sulfate 4g, lauryl sodium sulfate 1g, kaolin mends 100g, then co-grinding, is prepared into 2% Affirm (Merck Co.) wetting powder (being called for short medicament 19).
Comparative example 7: the comparative sample 7 of the present embodiment is the former medicine of Affirm (Merck Co.).
Solvability detects: get some tool plug conical flasks, add the deionized water of 100mL respectively, then add the Affirm (Merck Co.) of 10mg respectively, and respectively 25 DEG C of isothermal vibrations 48 hours, the solvability of Affirm (Merck Co.) is on average 9.0000mg/L after testing.
By 2g Affirm (Merck Co.), sldium lauryl sulfate 4g, lauryl sodium sulfate 1g, kaolin mends 100g, then co-grinding, is prepared into 2% Affirm (Merck Co.) wetting powder (being called for short medicament 20).
Contrasted from above-mentioned 3 embodiments, the solvability of the former medicine of the Affirm (Merck Co.) in the solid dispersions of embodiment 18 and embodiment 19 improves 36.5800mg/L, 39.4412mg/L than the solvability of the Affirm (Merck Co.) of comparative example 7 respectively.
When preventing and treating paddy rice rice leaf roller, the dosage of each medicament is 50 grams/acre, the control efficiency of 7 days investigation each sample after medicine, result is as follows: the control efficiency of medicament 18 is 82.7%, the control efficiency of medicament 19 is 84.5%, the control efficiency of medicament 20 is 67.3%, and the control efficiency of blank 1 (Emulsifier EL-60: PVPK90=6:84) is 0, and the control efficiency of blank 2 (polysorbate60: PVPK90=6:89) is 0%.Contrasted from control efficiency, the control efficiency of medicament 15 and medicament 16 respectively higher than the control efficiency of medicament 17 by 15.4%, 17.2%;
Embodiment 14
The present embodiment capillary solid dispersions comprises the former medicine of capillary, Tween 80 and PEG6000 composition, and three's weight ratio is 10:8:82.
Its preparation method is solvent method: be dissolved in acetone by 10g capillary, 8g Tween 80 and 82gPEG6000, spraying dry removing acetone.
In methyl alcohol, measure capillary maximum absorption wavelength is 205nm.
Solvability detects: get some tool plug conical flasks, add the deionized water of 100mL respectively, add the capillary solid dispersions (after conversion, capillary is 0.5mg in proportion) of 5mg again, respectively 25 DEG C of isothermal vibrations 48 hours, in capillary solid dispersions, the solvability of capillary is on average 2.7345mg/L after testing.
By 60g capillary solid dispersions (after conversion, capillary is 6g in proportion), alkyl benzene calcium sulfonate 2.4g, lauryl sodium sulfate 3g, kaolin mends 100g, then co-grinding, is prepared into 6% capillary wetting powder (being called for short medicament 21).
Embodiment 15
The present embodiment capillary solid dispersions comprises the former medicine of capillary, Tween 80 and PEG6000 composition, and three's weight ratio is 10:10:80.
Its preparation method is solvent method: be dissolved in acetone by 10g capillary, 10g Tween 80 and 80gPEG6000, spraying dry removing acetone.
In methyl alcohol, measure capillary maximum absorption wavelength is 205nm.
Solvability detects: get some tool plug conical flasks, add the deionized water of 100mL respectively, add the capillary solid dispersions (after conversion, capillary is 0.5mg in proportion) of 5mg again, respectively 25 DEG C of isothermal vibrations 48 hours, in capillary solid dispersions, the solvability of capillary is on average 2.9860mg/L after testing.
By 60g capillary solid dispersions (after conversion, capillary is 6g in proportion), alkyl benzene calcium sulfonate 2.4g, lauryl sodium sulfate 3g, kaolin mends 100g, then co-grinding, is prepared into 6% capillary wetting powder (being called for short medicament 22).
Comparative example 8: the comparative sample 8 of the present embodiment is the former medicine of capillary.
Solvability detects: get some tool plug conical flasks, add the deionized water of 100mL respectively, then add the comparative sample 2 of 0.5mg, respectively 25 DEG C of isothermal vibrations 48 hours, and the solvability average out to 0.1300mg/L of capillary after testing.
By 6g capillary, alkyl benzene calcium sulfonate 2.4g, lauryl sodium sulfate 3g, kaolin mends 100g, then co-grinding, is prepared into 6% capillary wetting powder (being called for short medicament 23).
Contrasted from above-mentioned 3 embodiments, the solvability of the capillary in the solid dispersions of embodiment 14 and embodiment 15 improves 2.6045mg/L than the solvability of the capillary of comparative example 8 respectively; 2.8560mg/L.
When preventing and treating wild cabbage diamond-back moth, the dosage of each medicament is 45 grams/acre, the control efficiency of 7 days investigation each sample after medicine, result is as follows: the control efficiency of medicament 21 is 87.3%, the control efficiency of medicament 22 is 86.6%, the control efficiency of medicament 23 is 64.2%, and the control efficiency of blank (Tween 80: PEG6000=1:1) is 0.Contrasted from control efficiency, the control efficiency of medicament 21 and medicament 22 respectively higher than the control efficiency of medicament 23 by 23.1%, 22.4%;
Embodiment 16
The present embodiment chlopyrifos solid dispersions comprises the former medicine of chlopyrifos, Emulsifier EL-60 and PVPK90 composition, and three's weight ratio is 10:7:83.
Its preparation method is solvent method: be dissolved in chloroform by 10g chlopyrifos, 7g Emulsifier EL-60 and 83gPVPK90, spraying dry removing chloroform.
In methyl alcohol, measure chlopyrifos maximum absorption wavelength is 230nm.
Solvability detects: get some tool plug conical flasks, add the deionized water of 100mL respectively, add 100mg chlopyrifos solid dispersions (after conversion, chlopyrifos is 10mg in proportion) more respectively, respectively 25 DEG C of isothermal vibrations 48 hours, the average solubility of chlopyrifos solid dispersions Chlorpyrifos is 31.4468mg/L after testing.
By 80g chlopyrifos solid dispersions (after conversion, chlopyrifos is 8g in proportion), sodium lignin sulfonate 2.4g, lauryl sodium sulfate 3g, kaolin mends 100g, then co-grinding, is prepared into 8% chlopyrifos wetting powder (being called for short medicament 24).
Embodiment 17
The present embodiment chlopyrifos solid dispersions comprises the former medicine of chlopyrifos, Emulsifier EL-60 and PVPK90 composition, and three's weight ratio is 10:10:80.
Its preparation method is solvent method: be dissolved in chloroform by 10g chlopyrifos, 10g Emulsifier EL-60 and 80gPVPK90, spraying dry removing chloroform.
In methyl alcohol, measure chlopyrifos maximum absorption wavelength is 230nm.
Solvability detects: get some tool plug conical flasks, add the deionized water of 100mL respectively, add 100mg chlopyrifos solid dispersions (after conversion, chlopyrifos is 10mg in proportion) more respectively, respectively 25 DEG C of isothermal vibrations 48 hours, the average solubility of chlopyrifos solid dispersions Chlorpyrifos is 32.5680mg/L after testing.
By 80g chlopyrifos solid dispersions (after conversion, chlopyrifos is 8g in proportion), sodium lignin sulfonate 2.4g, lauryl sodium sulfate 3g, kaolin mends 100g, then co-grinding, is prepared into 8% chlopyrifos wetting powder (being called for short medicament 25).
Comparative example 9: the comparative sample 9 of the present embodiment is the former medicine of chlopyrifos.
Solvability detects: get some tool plug conical flasks, add the deionized water of 100mL respectively, then add the chlopyrifos of 10mg respectively, and respectively 25 DEG C of isothermal vibrations 48 hours, the solvability of chlopyrifos is on average 1.2125mg/L after testing.
By 8g chlopyrifos, sodium lignin sulfonate 2.4g, lauryl sodium sulfate 3g, kaolin mends 100g, then co-grinding, is prepared into 8% chlopyrifos wetting powder (being called for short medicament 26).
Contrasted from above-mentioned 3 embodiments, the solvability of the former medicine of the chlopyrifos in the solid dispersions of embodiment 16 and embodiment 17 improves 30.2343mg/L, 31.3555mg/L than the solvability of the chlopyrifos of comparative example 9 respectively.
When preventing and treating paddy rice rice leaf roller, the dosage of each medicament is 300 grams/acre, the control efficiency of 7 days investigation each sample after medicine, result is as follows: the control efficiency of medicament 24 is 80.5%, the control efficiency of medicament 25 is 79.1%, the control efficiency of medicament 26 is 61.2%, and the control efficiency of blank (Emulsifier EL-60: PVPK90=1:1) is 0.Contrasted from control efficiency, the control efficiency of medicament 24 and medicament 25 respectively higher than the control efficiency of medicament 26 by 19.3%, 17.9%;
Embodiment 18
The present embodiment lufenuron solid dispersions comprises the former medicine of lufenuron, Tween 80 and PEG6000 composition, and three's weight ratio is 8:4:88.
Its preparation method is solvent method: be dissolved in chloroform by 8g lufenuron, 4g Tween 80 and 88gPEG6000, spraying dry removing chloroform.
Lufenuron maximum absorption wavelength in methyl alcohol is 220nm.
Solvability detects: get some tool plug conical flasks, add the deionized water of 100mL respectively, add the lufenuron solid dispersions (after conversion, lufenuron is 0.5mg in proportion) of 5mg again, respectively 25 DEG C of isothermal vibrations 48 hours, after testing, in lufenuron solid dispersions, the solvability of lufenuron is on average 0.1366mg/L.
By 50g lufenuron solid dispersions (after conversion, lufenuron is 4g in proportion), pull open powder 2g, lauryl sodium sulfate 3g, kaolin mends 100g, then co-grinding, is prepared into 4% lufenuron wetting powder (being called for short medicament 27).
Embodiment 19
The present embodiment lufenuron solid dispersions comprises the former medicine of lufenuron, Tween 80 and PEG6000 composition, and three's weight ratio is 10:10:80.
Its preparation method is solvent method: be dissolved in chloroform by 10g lufenuron, 10g Tween 80 and 80gPEG6000, spraying dry removing chloroform.
Lufenuron maximum absorption wavelength in methyl alcohol is 220nm.
Solvability detects: get some tool plug conical flasks, add the deionized water of 100mL respectively, add the lufenuron solid dispersions (after conversion, lufenuron is 0.5mg in proportion) of 5mg again, respectively 25 DEG C of isothermal vibrations 48 hours, after testing, in lufenuron solid dispersions, the solvability of lufenuron is on average 0.1465mg/L.
By 40g lufenuron solid dispersions (after conversion, lufenuron is 4g in proportion), pull open powder 2g, lauryl sodium sulfate 3g, kaolin mends 100g, then co-grinding, is prepared into 4% lufenuron wetting powder (being called for short medicament 28).
Comparative example 10: the comparative sample 10 of the present embodiment is the former medicine of lufenuron.
Solubility test method is: get some tool plug conical flasks, add the deionized water of 100mL respectively, then add the former medicine of 0.5mg lufenuron, and 25 DEG C of isothermal vibrations 48 hours, the solvability of lufenuron was on average 0.0054mg/L after testing.
By 4g lufenuron, pull open powder 2g, lauryl sodium sulfate 3g, kaolin mends 100g, then co-grinding, is prepared into 4% lufenuron wetting powder (being called for short medicament 29).
Contrasted from above-mentioned 3 embodiments, the solvability of the lufenuron in the solid dispersions of embodiment 18 and embodiment 19 improves 0.1312mg/L, 0.1411mg/L than the solvability of the lufenuron of comparative example 10 respectively.
When preventing and treating Laphygma exigua Hubner, the dosage of each medicament is 50 grams/acre, the control efficiency of 7 days investigation each sample after medicine, result is as follows: the control efficiency of medicament 27 is 91.8%, the control efficiency of medicament 28 is 89.3%, the control efficiency of medicament 29 is 70.2%, and the control efficiency of blank (Tween 80: PEG6000=1:1) is 0.Contrasted from control efficiency, the control efficiency of medicament 27 and medicament 28 respectively higher than the control efficiency of medicament 29 by 21.6%, 19.1%;
Embodiment 20
The present embodiment ethiprole solid dispersions comprises the former medicine of ethiprole, Emulsifier EL-60 and PVPK90 composition, and three's weight ratio is 10:5:85.
Its preparation method is solvent method: be dissolved in chloroform by 10g ethiprole, 5g Emulsifier EL-60 and 85gPVPK90, spraying dry removing chloroform.
In methyl alcohol, measure ethiprole maximum absorption wavelength is 240nm.
Solvability detects: get some tool plug conical flasks, add the deionized water of 100mL respectively, add 100mg ethiprole solid dispersions (after conversion, ethiprole is 10mg in proportion) more respectively, respectively 25 DEG C of isothermal vibrations 48 hours, in ethiprole solid dispersions, the average solubility of ethiprole is 38.7850mg/L after testing.
By 50g ethiprole solid dispersions (after conversion, ethiprole is 5g in proportion), sodium metnylene bis-naphthalene sulfonate 2g, lauryl sodium sulfate 2g, kaolin mends 100g, then co-grinding, is prepared into 5% ethiprole wetting powder (being called for short medicament 30).
Embodiment 21
The present embodiment ethiprole solid dispersions comprises the former medicine of ethiprole, Emulsifier EL-60 and PVPK90 composition, and three's weight ratio is 10:10:80.
Its preparation method is solvent method: be dissolved in chloroform by 10g ethiprole, 10g Emulsifier EL-60 and 80gPVPK90, spraying dry removing chloroform.
In methyl alcohol, measure ethiprole maximum absorption wavelength is 240nm.
Solvability detects: get some tool plug conical flasks, add the deionized water of 100mL respectively, add 100mg ethiprole solid dispersions (after conversion, ethiprole is 10mg in proportion) more respectively, respectively 25 DEG C of isothermal vibrations 48 hours, in ethiprole solid dispersions, the average solubility of ethiprole is 40.8867mg/L after testing.
By 50g ethiprole solid dispersions (after conversion, ethiprole is 5g in proportion), sodium metnylene bis-naphthalene sulfonate 2g, lauryl sodium sulfate 2g, kaolin mends 100g, then co-grinding, is prepared into 5% ethiprole wetting powder (being called for short medicament 31).
Comparative example 11: the comparative sample 11 of the present embodiment is the former medicine of ethiprole.
Solvability detects: get some tool plug conical flasks, add the deionized water of 100mL respectively, then add the ethiprole of 10mg respectively, and respectively 25 DEG C of isothermal vibrations 48 hours, the solvability of ethiprole is on average 1.9000mg/L after testing.
By 5g ethiprole, sodium metnylene bis-naphthalene sulfonate 2g, lauryl sodium sulfate 2g, kaolin mends 100g, then co-grinding, is prepared into 5% ethiprole wetting powder (being called for short medicament 32).
Contrasted from above-mentioned 3 embodiments, the solvability of the former medicine of the ethiprole in the solid dispersions of embodiment 20 and embodiment 21 improves 36.8850mg/L, 38.9867mg/L than the solvability of the ethiprole of comparative example 11 respectively.
When chrysanthemum noctuid is viewed and admired in control, the dosage of each medicament is 45 grams/acre, the control efficiency of 7 days investigation each sample after medicine, result is as follows: the control efficiency of medicament 30 is 93.5%, the control efficiency of medicament 31 is 91.8%, the control efficiency of medicament 32 is 77.2%, and the control efficiency of blank (Emulsifier EL-60: PVPK90=1:1) is 0.Contrasted from control efficiency, the control efficiency of medicament 30 and medicament 31 respectively higher than the control efficiency of medicament 32 by 16.3%, 14.6%;
Embodiment 22
The present embodiment poison fluorine phosphorus solid dispersions comprises the former medicine of malicious fluorine phosphorus, Emulsifier EL-60 and PVPK90 composition, and three's weight ratio is 10:4:86.
Its preparation method is solvent method: be dissolved in chloroform by 10g poison fluorine phosphorus, 4g Emulsifier EL-60 and 86gPVPK90, spraying dry removing chloroform.
In methyl alcohol, measure malicious fluorine phosphorus maximum absorption wavelength is 270nm.
Solvability detects: get some tool plug conical flasks, add the deionized water of 100mL respectively, add 100mg poison fluorine phosphorus solid dispersions (after conversion, malicious fluorine phosphorus is 10mg in proportion) more respectively, respectively 25 DEG C of isothermal vibrations 48 hours, the average solubility of the poisoning fluorine phosphorus of malicious fluorine phosphorus solid dispersions is 221.6832mg/L after testing.
By 40g poison fluorine phosphorus solid dispersions (after conversion, malicious fluorine phosphorus is 4g in proportion), sodium metnylene bis-naphthalene sulfonate 3.5g, lauryl sodium sulfate 1g, kaolin mends 100g, then co-grinding, is prepared into 4% malicious fluorine phosphorus wetting powder (being called for short medicament 33).
Embodiment 23
The present embodiment poison fluorine phosphorus solid dispersions comprises the former medicine of malicious fluorine phosphorus, Emulsifier EL-60 and PVPK90 composition, and three's weight ratio is 10:10:80.
Its preparation method is solvent method: be dissolved in chloroform by 10g poison fluorine phosphorus, 10g Emulsifier EL-60 and 80gPVPK90, spraying dry removing chloroform.
In methyl alcohol, measure malicious fluorine phosphorus maximum absorption wavelength is 270nm.
Solvability detects: get some tool plug conical flasks, add the deionized water of 100mL respectively, add 100mg poison fluorine phosphorus solid dispersions (after conversion, malicious fluorine phosphorus is 10mg in proportion) more respectively, respectively 25 DEG C of isothermal vibrations 48 hours, the average solubility of the poisoning fluorine phosphorus of malicious fluorine phosphorus solid dispersions is 233.5000mg/L after testing.
By 40g poison fluorine phosphorus solid dispersions (after conversion, malicious fluorine phosphorus is 4g in proportion), sodium metnylene bis-naphthalene sulfonate 3.5g, lauryl sodium sulfate 1g, kaolin mends 100g, then co-grinding, is prepared into 4% malicious fluorine phosphorus wetting powder (being called for short medicament 34).
Comparative example 12: the comparative sample 12 of the present embodiment is the former medicine of malicious fluorine phosphorus.
Solvability detects: get some tool plug conical flasks, add the deionized water of 100mL respectively, then add the malicious fluorine phosphorus of 10mg respectively, and respectively 25 DEG C of isothermal vibrations 48 hours, the solvability of malicious fluorine phosphorus is on average 39.2000mg/L after testing.
By 4g poison fluorine phosphorus, sodium metnylene bis-naphthalene sulfonate 3.5g, lauryl sodium sulfate 1g, kaolin mends 100g, then co-grinding, is prepared into 4% malicious fluorine phosphorus wetting powder (being called for short medicament 35).
Contrasted from above-mentioned 3 embodiments, the solvability of the former medicine of malicious fluorine phosphorus in the solid dispersions of embodiment 22 and embodiment 23 improves 181.4832mg/L, 193.3000mg/L than the solvability of the malicious fluorine phosphorus of comparative example 12 respectively.
When water prevention rice black streak dwarf, the dosage of each medicament is 350 grams/acre, the control efficiency of 14 days investigation each sample after medicine, result is as follows: the control efficiency of medicament 33 is 74.6%, the control efficiency of medicament 34 is 76.3%, the control efficiency of medicament 35 is 63.4%, and the control efficiency of blank (Emulsifier EL-60: PVPK90=1:1) is 0.Contrasted from control efficiency, the control efficiency of medicament 33 and medicament 34 respectively higher than the control efficiency of medicament 35 by 11.2%, 12.9%;
Embodiment 24
The present embodiment Fluoxastrobin solid dispersions comprises the former medicine of Fluoxastrobin, polysorbas20, PEG4000 and PEG6000 composition, and four weight ratios are 10:4:42:44.
Its preparation method is solvent-fusion method: 42gPEG4000 and 44gPEG6000 is heated to thawing, is dissolved in acetone, joins in the PEG of thawing by 10g Fluoxastrobin and 4g polysorbas20, spraying dry removing acetone.
In methyl alcohol, measure Fluoxastrobin maximum absorption wavelength is 254nm.
Solvability detects: get some tool plug conical flasks, add the deionized water of 100mL respectively, add the Fluoxastrobin solid dispersions (after conversion, Fluoxastrobin is 0.5mg in proportion) of 5mg more respectively, respectively 25 DEG C of isothermal vibrations 48 hours, in Fluoxastrobin solid dispersions, the solvability of Fluoxastrobin is on average 68.9822mg/L after testing.
By 50g Fluoxastrobin solid dispersions (after conversion, Fluoxastrobin is 5g in proportion), sodium metnylene bis-naphthalene sulfonate 3g, lauryl sodium sulfate 1.5g, kaolin mends 100g, then co-grinding, is prepared into 5% Fluoxastrobin wetting powder (being called for short medicament 36).
Embodiment 25
The present embodiment Fluoxastrobin solid dispersions comprises the former medicine of Fluoxastrobin, polysorbas20 and PEG4000 composition, and four weight ratios are 10:10:80.
Its preparation method is solvent-fusion method: 80gPEG4000 is heated to thawing, is dissolved in acetone, joins in the PEG of thawing by 10g Fluoxastrobin and 10g polysorbas20, spraying dry removing acetone.
In methyl alcohol, measure Fluoxastrobin maximum absorption wavelength is 254nm.
Solvability detects: get some tool plug conical flasks, add the deionized water of 100mL respectively, add the Fluoxastrobin solid dispersions (after conversion, Fluoxastrobin is 0.5mg in proportion) of 5mg more respectively, respectively 25 DEG C of isothermal vibrations 48 hours, in Fluoxastrobin solid dispersions, the solvability of Fluoxastrobin is on average 70.8720mg/L after testing.
By 50g Fluoxastrobin solid dispersions (after conversion, Fluoxastrobin is 5g in proportion), sodium metnylene bis-naphthalene sulfonate 3g, lauryl sodium sulfate 1.5g, kaolin mends 100g, then co-grinding, is prepared into 5% Fluoxastrobin wetting powder (being called for short medicament 37).
Embodiment 26
The present embodiment Fluoxastrobin solid dispersions comprises the former medicine of Fluoxastrobin, Tween 80, PEG4000 and PEG6000 composition, and four weight ratios are 10:4:42:44.
Its preparation method is solvent-fusion method: 42gPEG4000 and 44gPEG6000 is heated to thawing, is dissolved in acetone, joins in the PEG of thawing by 10g Fluoxastrobin and 4g Tween 80, spraying dry removing acetone.
In methyl alcohol, measure Fluoxastrobin maximum absorption wavelength is 254nm.
Solvability detects: get some tool plug conical flasks, add the deionized water of 100mL respectively, add the Fluoxastrobin solid dispersions (after conversion, Fluoxastrobin is 0.5mg in proportion) of 5mg more respectively, respectively 25 DEG C of isothermal vibrations 48 hours, in Fluoxastrobin solid dispersions, the solvability of Fluoxastrobin is on average 30.2514mg/L after testing.
By 50g Fluoxastrobin solid dispersions (after conversion, Fluoxastrobin is 5g in proportion), sodium metnylene bis-naphthalene sulfonate 3g, lauryl sodium sulfate 1.5g, kaolin mends 100g, then co-grinding, is prepared into 5% Fluoxastrobin wetting powder (being called for short medicament 38).
Embodiment 27
The present embodiment Fluoxastrobin solid dispersions comprises the former medicine of Fluoxastrobin, Tween 80 and PEG4000 composition, and four weight ratios are 10:10:80.
Its preparation method is solvent-fusion method: 80gPEG4000 is heated to thawing, is dissolved in acetone, joins in the PEG of thawing by 10g Fluoxastrobin and 10g Tween 80, spraying dry removing acetone.
In methyl alcohol, measure Fluoxastrobin maximum absorption wavelength is 245nm.
Solvability detects: get some tool plug conical flasks, add the deionized water of 100mL respectively, add the Fluoxastrobin solid dispersions (after conversion, Fluoxastrobin is 0.5mg in proportion) of 5mg more respectively, respectively 25 DEG C of isothermal vibrations 48 hours, in Fluoxastrobin solid dispersions, the solvability of Fluoxastrobin is on average 32.5266mg/L after testing.
By 50g Fluoxastrobin solid dispersions (after conversion, Fluoxastrobin is 5g in proportion), sodium metnylene bis-naphthalene sulfonate 3g, lauryl sodium sulfate 1.5g, kaolin mends 100g, then co-grinding, is prepared into 5% Fluoxastrobin wetting powder (being called for short medicament 39).
Comparative example 13: the comparative sample 13 of the present embodiment is the former medicine of Fluoxastrobin.
Solvability detects: get some tool plug conical flasks, add the deionized water of 100mL respectively, then add 0.5mg comparative sample 5 respectively, and respectively 25 DEG C of isothermal vibrations 48 hours, Fluoxastrobin solvability is on average 2.0411mg/L after testing.
By 5g Fluoxastrobin, sodium metnylene bis-naphthalene sulfonate 3g, lauryl sodium sulfate 1.5g, kaolin mends 100g, then co-grinding, is prepared into 5% Fluoxastrobin wetting powder (being called for short medicament 40).
Contrasted from above-mentioned 5 embodiments, the solvability of the Fluoxastrobin in the solid dispersions of embodiment 24, embodiment 25, embodiment 26 and embodiment 27 improves 66.9411mg/L, 68.8309mg/L, 28.2103mg/L, 30.4855mg/L relative to the solvability of the Fluoxastrobin of comparative example 13.
When the water prevention rice sheath blight, the dosage of each medicament is 120 grams/acre, the control efficiency of 14 days investigation each sample after medicine, result is as follows: the control efficiency of medicament 36 is 85.1%, the control efficiency of medicament 37 is 83.6%, the control efficiency of medicament 38 is 84.1%, the control efficiency of medicament 39 is 81.8%, the control efficiency of medicament 40 is 62.7%, blank 1 (polysorbas20: PEG4000:PEG6000=1:1:1), blank 2 (polysorbas20: PEG4000=1:1), blank 3 (Tween 80: PEG4000:PEG6000=1:1:1), the control efficiency of blank 4 (Tween 80: PEG4000=1:8) is 0.Contrasted from control efficiency, the control efficiency of medicament 36, medicament 37, medicament 38, medicament 39 respectively higher than the control efficiency of medicament 40 by 22.4%, 20.9%, 21.4%, 19.1%;
Embodiment 28
The present embodiment epoxiconazole solid dispersions comprises epoxiconazole raw drug, Tween 80 and PEG6000 composition, and three's weight ratio is 8:4:88.
Its preparation method is solwution method: be dissolved in chloroform by 8g epoxiconazole, 4g Tween 80 and 88gPEG6000, spraying dry removing chloroform.
Epoxiconazole maximum absorption wavelength in methyl alcohol is 205nm.
Solvability detects: get some tool plug conical flasks, add the deionized water of 100mL respectively, add the epoxiconazole solid dispersions (after conversion, epoxiconazole is 0.5mg in proportion) of 5mg again, respectively 25 DEG C of isothermal vibrations 48 hours, after testing, in epoxiconazole solid dispersions, the solvability of epoxiconazole is on average 70.5638mg/L.
By 50g epoxiconazole solid dispersions (after conversion, epoxiconazole is 4g in proportion), sodium metnylene bis-naphthalene sulfonate 3g, lauryl sodium sulfate 1.5g, kaolin mends 100g, then co-grinding, is prepared into 4% epoxiconazole wetting powder (being called for short medicament 41).
Embodiment 29
The present embodiment epoxiconazole solid dispersions comprises epoxiconazole raw drug, Tween 80 and PEG6000 composition, and three's weight ratio is 10:10:80.
Its preparation method is solwution method: be dissolved in chloroform by 10g epoxiconazole, 10g Tween 80 and 80gPEG6000, spraying dry removing chloroform.
Epoxiconazole maximum absorption wavelength in methyl alcohol is 205nm.
Solvability detects: get some tool plug conical flasks, add the deionized water of 100mL respectively, add the epoxiconazole solid dispersions (after conversion, epoxiconazole is 0.5mg in proportion) of 5mg again, respectively 25 DEG C of isothermal vibrations 48 hours, after testing, in epoxiconazole solid dispersions, the solvability of epoxiconazole is on average 72.6680mg/L.
By 40g epoxiconazole solid dispersions (after conversion, epoxiconazole is 4g in proportion), sodium metnylene bis-naphthalene sulfonate 3g, lauryl sodium sulfate 1.5g, kaolin mends 100g, then co-grinding, is prepared into 4% epoxiconazole wetting powder (being called for short medicament 42).
Comparative example 14: the comparative sample 14 of the present embodiment is epoxiconazole raw drug.
Solubility test method is: get some tool plug conical flasks, add the deionized water of 100mL respectively, then add 0.5mg epoxiconazole raw drug, and 25 DEG C of isothermal vibrations 48 hours, the solvability of epoxiconazole was on average 8.4221mg/L after testing.
By 4g epoxiconazole, sodium metnylene bis-naphthalene sulfonate 3g, lauryl sodium sulfate 1.5g, kaolin mends 100g, then co-grinding, is prepared into 4% epoxiconazole wetting powder (being called for short medicament 43).
Contrasted from above-mentioned 3 embodiments, the solvability of the epoxiconazole in the solid dispersions of embodiment 28 and embodiment 29 improves 62.1417mg/L, 64.2459mg/L relative to the solvability of the epoxiconazole of comparative example 14.
When the water prevention rice sheath blight, the dosage of each medicament is 150 grams/acre, the control efficiency of 10 days investigation each sample after medicine, result is as follows: the control efficiency of medicament 41 is 86.3%, the control efficiency of medicament 42 is 84.2%, the control efficiency of medicament 43 is 67.5%, and the control efficiency of blank 1 (Tween 80: PEG6000=1:1) is 0.Contrasted from control efficiency, the control efficiency of medicament 41, medicament 42 respectively higher than the control efficiency of medicament 43 by 18.8%, 16.7%;
Above embodiment is only in order to illustrate technical scheme of the present invention and unrestricted; those skilled in the art is to be understood that; do not departing from the purpose and scope of the invention, can modify to technical scheme of the present invention or equivalent replacement, it all should be encompassed in protection scope of the present invention.
Claims (10)
1. a solid dispersions for indissoluble agricultural chemicals, is characterized in that, solid dispersions is made up of indissoluble agricultural chemicals, solubilizer and macromolecule carrier, and three's weight ratio is 1 ~ 10:1 ~ 10:80 ~ 98.
2. the solid dispersions of indissoluble agricultural chemicals according to claim 1, is characterized in that, described indissoluble agricultural chemicals is selected from the one in the insecticide of slightly solubility, bactericide.
3. the solid dispersions of indissoluble agricultural chemicals according to claim 2, it is characterized in that, described insecticide is cypermethrin, decis, Biphenthrin, gamma cyhalothrin, indoxacarb, Avermectin, Affirm (Merck Co.), capillary, chlopyrifos, lufenuron, ethiprole.
4. the solid dispersions of indissoluble agricultural chemicals according to claim 2, is characterized in that, described bactericide is malicious fluorine phosphorus, Fluoxastrobin, epoxiconazole.
5., according to the solid dispersions of the arbitrary described indissoluble agricultural chemicals of claim 1-4, it is characterized in that, described solubilizer comprises: polysorbas20, polysorbate60, Tween 80, PLURONICS F87, Brij35, Emulsifier EL-60.
6. according to the solid dispersions of the arbitrary described indissoluble agricultural chemicals of claim 1-4, it is characterized in that, described macromolecule carrier comprises: polyethylene glycol, poly-(NVP).
7. the solid dispersions of indissoluble agricultural chemicals according to claim 5, is characterized in that, described macromolecule carrier comprises: polyethylene glycol, poly-(NVP).
8. the solid dispersions of indissoluble agricultural chemicals according to claim 6, is characterized in that, described polyethylene glycol is PEG4000, PEG6000, PEG12000, PEG20000; Described poly-(NVP) is PVPK30 and PVPK90.
9. a preparation method for the solid dispersions of the indissoluble agricultural chemicals as described in as arbitrary in claim 1-8, is characterized in that, by solvent method, fusion method, solvent-fusion method preparation.
10. a pesticidal preparations, is characterized in that, described pesticidal preparations comprises the solid dispersions of the arbitrary described indissoluble agricultural chemicals of claim 1-8, insecticides adjuvant and agricultural chemicals auxiliary element.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105724373A (en) * | 2016-04-28 | 2016-07-06 | 福建农林大学 | Emamectin benzoate binary joint carrier solid dispersion and preparation method thereof |
| WO2018215883A1 (en) * | 2017-05-25 | 2018-11-29 | Upl Ltd | A stable agrochemical composition and process thereof |
| CN113287608A (en) * | 2021-05-11 | 2021-08-24 | 浙江工业大学 | Drug solubilization system and application thereof in pesticide preparation |
| JP2022505538A (en) * | 2018-10-24 | 2022-01-14 | シンジェンタ パーティシペーションズ アーゲー | New Abamectin Soluble Concentrated Composition (SL) |
| CN115644191A (en) * | 2022-07-09 | 2023-01-31 | 浙江工业大学 | Preparation method of bifenthrin emulsion |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1465485B1 (en) * | 2001-11-07 | 2006-04-26 | Basf Aktiengesellschaft | Nanoparticles comprising a crop protection agent |
| CN101489535A (en) * | 2006-07-13 | 2009-07-22 | 荷兰联合利华有限公司 | Improvements relating to nanodispersions |
| CN102176822A (en) * | 2008-10-08 | 2011-09-07 | 詹森药业有限公司 | High solid dispersions comprising biocides |
| CN104798772A (en) * | 2015-03-13 | 2015-07-29 | 中国农业科学院农业环境与可持续发展研究所 | Pesticide nano-solid dispersion and preparation method thereof |
-
2015
- 2015-10-12 CN CN201510653729.3A patent/CN105145553A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1465485B1 (en) * | 2001-11-07 | 2006-04-26 | Basf Aktiengesellschaft | Nanoparticles comprising a crop protection agent |
| CN101489535A (en) * | 2006-07-13 | 2009-07-22 | 荷兰联合利华有限公司 | Improvements relating to nanodispersions |
| CN102176822A (en) * | 2008-10-08 | 2011-09-07 | 詹森药业有限公司 | High solid dispersions comprising biocides |
| CN104798772A (en) * | 2015-03-13 | 2015-07-29 | 中国农业科学院农业环境与可持续发展研究所 | Pesticide nano-solid dispersion and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 张炳盛，黄敏琪: "《中药药剂学》", 28 February 2013 * |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105724373A (en) * | 2016-04-28 | 2016-07-06 | 福建农林大学 | Emamectin benzoate binary joint carrier solid dispersion and preparation method thereof |
| CN105724373B (en) * | 2016-04-28 | 2018-06-15 | 福建农林大学 | A kind of emamectin benzoate binary combination carrier solids dispersion and preparation method thereof |
| WO2018215883A1 (en) * | 2017-05-25 | 2018-11-29 | Upl Ltd | A stable agrochemical composition and process thereof |
| CN111405848A (en) * | 2017-05-25 | 2020-07-10 | Upl有限公司 | Stable agrochemical compositions and methods thereof |
| EP3629733A4 (en) * | 2017-05-25 | 2021-03-10 | UPL Ltd | A stable agrochemical composition and process thereof |
| JP2022505538A (en) * | 2018-10-24 | 2022-01-14 | シンジェンタ パーティシペーションズ アーゲー | New Abamectin Soluble Concentrated Composition (SL) |
| JP7429230B2 (en) | 2018-10-24 | 2024-02-07 | シンジェンタ パーティシペーションズ アーゲー | Novel Abamectin Soluble Concentrate Composition (SL) |
| CN113287608A (en) * | 2021-05-11 | 2021-08-24 | 浙江工业大学 | Drug solubilization system and application thereof in pesticide preparation |
| CN113287608B (en) * | 2021-05-11 | 2022-05-17 | 浙江工业大学 | Drug solubilization system and application thereof in pesticide preparation |
| CN115644191A (en) * | 2022-07-09 | 2023-01-31 | 浙江工业大学 | Preparation method of bifenthrin emulsion |
| CN115644191B (en) * | 2022-07-09 | 2024-04-30 | 浙江工业大学 | Preparation method of bifenthrin emulsion |
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