CN119423105A - Pesticide mother liquor and application thereof - Google Patents
Pesticide mother liquor and application thereof Download PDFInfo
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- CN119423105A CN119423105A CN202411529124.9A CN202411529124A CN119423105A CN 119423105 A CN119423105 A CN 119423105A CN 202411529124 A CN202411529124 A CN 202411529124A CN 119423105 A CN119423105 A CN 119423105A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
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Abstract
本发明公开了一种杀虫剂母液及其应用，以式I所示的高效拟除虫菊酯作为活性成分制备杀虫剂母液；本发明的母液可加工成蚊香、蝇香、电热蚊香液、电热蚊香片、气雾剂、防蛀片剂或防蚊网，用于防治蚊、蝇、德国小蠊、美洲大蠊、臭虫、蚂蚁、跳蚤、蜜蜂等卫生害虫；本发明的杀虫剂母液，可以降低有机溶剂的使用量，保护环境，同时实现增效减施的目的；另一方面可以用溶剂对母液进行不同比例的稀释，然后加工成相应的剂型，使用方便。 The invention discloses an insecticide mother solution and application thereof. The insecticide mother solution is prepared by taking a high-efficiency pyrethroid shown in formula I as an active ingredient. The mother solution of the invention can be processed into mosquito coils, fly coils, electric mosquito coil liquid, electric mosquito coil tablets, aerosols, moth-proof tablets or mosquito nets, and is used for preventing and controlling mosquitoes, flies, German cockroaches, American cockroaches, bedbugs, ants, fleas, bees and other sanitary pests. The insecticide mother solution of the invention can reduce the usage of organic solvents, protect the environment, and achieve the purpose of increasing efficiency and reducing application. On the other hand, the mother solution can be diluted with a solvent in different proportions, and then processed into corresponding dosage forms, which is convenient to use.
Description
The application relates to a divisional application of Chinese patent application, the original application date is 2022, 07, 13, application number 202210823424.2, the application creation name is an insecticide mother liquor and application thereof, the publication number is CN115669677A, and the applicant puts forward the divisional application.
Technical Field
The invention relates to an insecticide mother liquor and application thereof.
Background
The pyrethroid compound shown in the formula I is a novel sanitary insecticide, has good basic activity for preventing and controlling sanitary pests, and can be prepared according to the following reaction route:
Wherein R is methyl or ethyl, M is sodium or potassium and R1 is hydrogen.
For example, 3-formyl-2, 2-dimethyl cyclopropane carboxylic acid methyl ester (CAS No. 62138-41-4) is used as a starting material, acetonitrile is subjected to condensation reaction for 4 hours under the action of sodium ethoxide at 60 ℃, olefine hydrochloric acid is added to neutralize pH to 8, ethyl acetate and water solution are added, and an oil layer is desolventized to obtain an intermediate 3- (2-cyano-1-vinyl) -2, 2-dimethyl cyclopropane carboxylic acid methyl ester.
Adding 2,3,5, 6-tetrafluorobenzyl alcohol, catalytic amount of tetraisopropyl titanate and toluene solvent into the obtained 3- (2-cyano-1-vinyl) -2, 2-dimethylcyclopropane carboxylic acid methyl ester, slowly heating to reflux to obtain byproduct methanol, controlling in a gas phase, cooling to 0-5 ℃ after the raw materials are completely converted, dropwise adding a small amount of water, separating liquid, and desolventizing to obtain the pyrethroid compound shown in the formula I.
The pyrethroid compound of the formula I with a corresponding configuration can be obtained by taking cyclopropane carboxylic acid esters with different single configurations as starting materials, for example, methyl (1R, 3R) -3-formyl-2, 2-dimethylcyclopropane carboxylate (CAS number 27335-33-7) is used as the starting materials for synthesis, the product of the chrysanthemic acid part 1R,3R is obtained, distributed crystallization is carried out, and double bond CN group Z and E isomers are separated, so that single 2,3,4, 5-tetrafluorobenzyl- (1R, 3R) -3- [ (1Z) -2-cyano-1-vinyl ] -2, 2-dimethylcyclopropylcarboxylate or 2,3,4, 5-tetrafluorobenzyl- (1R, 3R) -3- [ (1E) -2-cyano-1-vinyl ] -2, 2-dimethylcyclopropylcarboxylate can be obtained. With methyl (1R, 3S) -3-formyl-2, 2-dimethylcyclopropanecarboxylate (CAS No. 55701-02-5), 2,3,4, 5-tetrafluorobenzyl- (1R, 3S) -3- (-2-cyano-1-vinyl) -2, 2-dimethylcyclopropylcarboxylate or 2,3,4, 5-tetrafluorobenzyl- (1R, 3S) -3- [ (1Z) -2-cyano-1-vinyl ] -2, 2-dimethylcyclopropylcarboxylate or 2,3,4, 5-tetrafluorobenzyl- (1R, 3S) -3- [ (1E) -2-cyano-1-vinyl ] -2, 2-dimethylcyclopropylcarboxylate can be obtained.
However, the preparation of the pyrethroid compound shown in I can be applied to the process of preparing a formulation for controlling sanitary pests. On the other hand, in the prior art, odorless kerosene is generally used for dissolving and diluting the hygienic pyrethroid crude drug, but because the kerosene has lower solubility to the compound of the formula I, a large amount of kerosene is needed, and the problem of solvent waste exists, and the invention researches the compound mother liquor of the formula I and the application thereof in order to solve the problem.
Disclosure of Invention
The invention aims to solve the technical problems of the prior art and provides an insecticide mother liquor and application thereof, wherein the insecticide mother liquor is prepared by taking high-efficiency pyrethroid shown in a formula I as an active ingredient, and can be processed into mosquito-repellent incense, fly incense, electrothermal mosquito-repellent incense liquid, electrothermal mosquito-repellent incense sheet, aerosol, mothproof tablet or mosquito-repellent net, and is used for preventing and controlling sanitary pests such as mosquitoes, flies, german cockroaches, american cockroaches, bed bugs, ants, fleas, bees and the like.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
The pesticide mother solution comprises a component A and a component B, wherein the total weight of the component A and the component B accounts for 90% -99.99% of the total weight of the pesticide mother solution, and the balance is other components, and the component A accounts for 0.1% -30% of the total weight of the component A and the component B;
the component A is a compound shown in a formula I;
the component B is a solvent;
In the above technical scheme, the component A preferably accounts for 5% -20% of the total weight of the component A and the component B.
In the above technical scheme, the component A is any one or more than two of 2,3,4, 5-tetrafluorobenzyl-3- [ -2-cyano-1-vinyl ] -2, 2-dimethylcyclopropylcarboxylate, preferably 2,3,4, 5-tetrafluorobenzyl- (1R, 3S) -3- [ (1Z) -2-cyano-1-vinyl ] -2, 2-dimethylcyclopropylcarboxylate, 2,3,4, 5-tetrafluorobenzyl- (1S, 3R) -3- [ (1Z) -2-cyano-1-vinyl ] -2, 2-dimethylcyclopropylcarboxylate, 2,3,4, 5-tetrafluorobenzyl- (1R, 3R) -3- [ (1Z) -2-cyano-1-vinyl ] -2, 2-dimethylcyclopropylcarboxylate and 2,3,4, 5-tetrafluorobenzyl- (1S, 3S) -3- [ (1Z) -2-cyano-1-vinyl ] -2, 2-dimethylcyclopropylcarboxylate.
In the above technical scheme, the component A is preferably 2,3,4, 5-tetrafluorobenzyl- (1R, 3S) -3- [ (1Z) -2-cyano-1-vinyl ] -2, 2-dimethylcyclopropylcarboxylate.
The component B is selected from C8-18 alkane solvents, deionized water, dodecylbenzene, decaalkylbenzene, N-dimethyl-sunflower amide and other amide solvents, gamma-butyrolactone, methyl oleate, isopropyl tridecanoate, isopropyl myristate, isopropyl palmitate, isopropyl phenylacetate, ethyl phenylacetate, N-butyl myristate and other monocarboxylic acid ester solvents, diisopropyl glutarate, diisopropyl adipate, diisobutyl adipate and other dicarboxylic acid ester solvents, tributyl citrate, tributyl acetylcitrate and other tricarboxylic acid ester solvents, triethylene glycol monobutyl ether, diethylene glycol monobutyl ether, propylene glycol methyl ether and other alcohol ether solvents, C2-8 alcohol solvents, and a mixture of any one or two or more of the compounds shown in the formula II and the compounds shown in the formula III in any proportion;
Wherein R1 and R2 are both C1-C10 alkyl groups.
The component B in the technical scheme is preferably N, N-dimethyl-sunflower amide, gamma-butyrolactone, diisopropyl adipate, tributyl citrate, acetyl tributyl citrate and isopropyl myristate.
In the above-mentioned embodiments, the C8-18 alkane solvent is preferably any one of D60 (Exxon Mobil petrochemical company), D80 (Exxon Mobil petrochemical company), D100 (Exxon Mobil petrochemical company), D110 (Exxon Mobil petrochemical company), isopar-E (Exxon Mobil petrochemical company), isopar-G (Exxon Mobil petrochemical company), isopar-H (Exxon Mobil petrochemical company), isopar-L (Exxon Mobil petrochemical company), isopar-M (Exxon Mobil petrochemical company), octane, nonane, quinine, undecane, dodecane, tridecane, tetradecane, pentadecane, hexadecane, and mixtures of two or more of them in any ratio.
In the above technical scheme, the alcohol solvent of C2-8 is preferably one or a mixture of two or more of ethanol, isopropanol, n-propanol, n-butanol, sec-butanol, tert-butanol, n-pentanol and its isomer, n-hexanol and its isomer, n-heptanol and its isomer, n-octanol and its isomer in any proportion.
In the technical scheme, the other components are any one or a mixture of two of a synergistic agent and a phenol antioxidant in any proportion.
In the technical scheme, the synergist is preferably 0.01% -8% of the total weight of the pesticide mother liquor, and the synergist is preferably any one of self-oxidized piperonyl butoxide, synergistic amine or triphenyl phosphate.
In the above technical scheme, the phenol antioxidant preferably accounts for 0.05% -2% of the total weight of the pesticide mother liquor, and the phenol antioxidant preferably is a mixture formed by mixing any one, two or more of 2, 6-di-tert-butyl-4-methylphenol, beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) isooctyl propionate, butyl hydroxyanisole, beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) n-stearyl propionate.
The invention also provides application of the pesticide mother liquor in preventing and controlling sanitary pests.
In the technical scheme, the sanitary insect pests refer to mosquitoes, flies, german cockroaches, american cockroaches, bed bugs, ants, fleas, bees and the like.
In the above technical scheme, the sanitary insect pest is preferably culex pallidum, culex tiredness, culex trilobus, aedes albopictus, aedes aegypti, anopheles sinensis, albopictus, midge, fly, chrysomyia megacephala, lucilia sericata, aeruginosa, liriomyza sativae, campylomyza sativae, german cockroach, american cockroach, bed bug, ant, flea, bee, wasp and the like.
In the technical scheme, the pesticide mother liquor is used in the mode of diluting odorless kerosene or C8-C18 alkane solvent by 1-100 times according to the weight ratio to prepare mosquito-repellent incense, fly incense, electric mosquito-repellent incense liquid, electric mosquito-repellent incense sheet, aerosol, mothproof tablet or mosquito-repellent net for use when preventing and controlling sanitary pests.
In the above technical scheme, the C8-C18 alkane solvent is selected from any one of D60 (elkesen mobil petrochemical company), D80 (elkesen mobil petrochemical company), D100 (elkesen mobil petrochemical company), D110 (elkesen mobil petrochemical company), isopar-E (elkesen mobil petrochemical company), isopar-G (elkesen mobil petrochemical company), isopar-H (elkesen mobil petrochemical company), isopar-L (elkesen mobil petrochemical company), isopar-M (elkesen mobil petrochemical company), octane, nonane, quiniane, undecane, dodecane, tridecane, tetradecane, pentadecane, hexadecane, heptadecane, octadecane, and a mixture of two or more of them in any proportion.
The pesticide mother liquor can reduce the use amount of the organic solvent, protect the environment and realize the aims of synergy and application reduction, and on the other hand, the pesticide mother liquor can be diluted with the solvent according to different proportions and then processed into corresponding dosage forms, so that the pesticide is convenient to use.
Detailed Description
The following detailed description of the technical scheme of the present invention is provided, but the present invention is not limited to the following descriptions:
The preparation method of the dosage form in each embodiment of the invention comprises the steps of mixing the component A, the component B and other components according to a certain proportion at room temperature or under the condition of heating to prepare corresponding mother liquor.
The invention is illustrated below with reference to specific examples.
Formulation example 1:
0.5g of 2,3,4, 5-tetrafluorobenzyl-3- [ (1Z) -2-cyano-1-vinyl ] -2, 2-dimethylcyclopropylcarboxylate ((1R, 3S), (1S, 3R), (1R, 3R), (1S, 3S) four isomers each accounting for 25%), piperonyl butoxide 1g, isopropyl myristate make up to 100g, giving a 0.5% mother liquor.
Formulation example 2:
0.5g of 2,3,4, 5-tetrafluorobenzyl- (1R, 3S) -3- [ (1Z) -2-cyano-1-vinyl ] -2, 2-dimethylcyclopropylcarboxylate, 1g of piperonyl butoxide, and 100g of isopropyl myristate were added to give a 0.5% mother liquor.
Formulation example 3:
0.5g of 2,3,4, 5-tetrafluorobenzyl- (1R, 3S) -3- [ (1Z) -2-cyano-1-vinyl ] -2, 2-dimethylcyclopropylcarboxylate, 1g of piperonyl butoxide, and 100g of dodecylbenzene were added to give a 0.5% mother liquor.
Formulation example 4:
0.5g of 2,3,4, 5-tetrafluorobenzyl- (1R, 3S) -3- [ (1Z) -2-cyano-1-vinyl ] -2, 2-dimethylcyclopropylcarboxylate, 1g of piperonyl butoxide and 100g of diisopropyl adipate were added to give a 0.5% mother liquor.
Formulation example 5:
5g of 2,3,4, 5-tetrafluorobenzyl-3- [ (1Z) -2-cyano-1-vinyl ] -2, 2-dimethylcyclopropylcarboxylate ((1R, 3S): (1S, 3R) =4:1), β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid isooctyl ester 0.5g, N-dimethylsunflower amide 5g, diisobutyl adipate up to 100g give a 5% mother liquor.
Formulation example 6:
6g of 2,3,4, 5-tetrafluorobenzyl- (1R, 3S) -3- [ (1Z) -2-cyano-1-vinyl ] -2, 2-dimethylcyclopropylcarboxylate, 0.2g of 2, 6-di-tert-butyl-4-methylphenol, diisopropyl adipate up to 100g, give a 6% mother liquor.
Formulation example 7:
5g of tributyl 2,3,4, 5-tetrafluorobenzyl citrate-3- [ (1Z) -2-cyano-1-vinyl ] -2, 2-dimethylcyclopropylcarboxylate ((1R, 3S): (1S, 3R) =5:1), piperonyl butoxide 3g, tributyl citrate 20g, isopropyl myristate make up to 100g, giving a 5% mother liquor.
Formulation example 8:
5g of 2,3,4, 5-tetrafluorobenzyl-3- [ (1Z) -2-cyano-1-vinyl ] -2, 2-dimethylcyclopropylcarboxylate ((1R, 3S): (1S, 3R) =3:1), 1g of piperonyl butoxide, and 100g of isopropyl myristate were supplemented to give a 5% mother liquor.
Formulation example 9:
0.1g of 2,3,4, 5-tetrafluorobenzyl-3- [ (1Z) -2-cyano-1-vinyl ] -2, 2-dimethylcyclopropylcarboxylate ((1R, 3S), (1S, 3R), (1R, 3R), (1S, 3S) four isomers each accounting for 25%), synergistic amine 0.01g, butyl hydroxy anisole 0.1g, D110 g, tributyl citrate make up to 100g, giving a 0.1% mother liquor.
Formulation example 10:
10g of 2,3,4, 5-tetrafluorobenzyl- (1R, 3S) -3- [ (1Z) -2-cyano-1-vinyl ] -2, 2-dimethylcyclopropylcarboxylate, 1g of 2, 6-di-tert-butyl-4-methylphenol, 20g of deionized water and 100g of triethylene glycol monobutyl ether were added to give a 10% mother liquor.
Formulation example 11:
5g of 2,3,4, 5-tetrafluorobenzyl-3- [ (1Z) -2-cyano-1-vinyl ] -2, 2-dimethylcyclopropylcarboxylate ((1R, 3S): (1S, 3R) =6:1), n-octadecyl β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate 0.5g, N-dimethylsunflower amide 10g, ethyl phenylacetate 10g, diisobutyl adipate up to 100g, giving a 5% mother liquor.
Formulation example 12:
27g of 2,3,4, 5-tetrafluorobenzyl- (1R, 3S) -3- [ (1Z) -2-cyano-1-vinyl ] -2, 2-dimethylcyclopropylcarboxylate, 5g of synergistic amine, 2g of 2, 6-di-tert-butyl-4-methylphenol and up to 100g of isopropyl tridecanoate give a 27% mother liquor.
Formulation example 13:
10g of 2,3,4, 5-tetrafluorobenzyl- (1R, 3S) -3- [ (1Z) -2-cyano-1-vinyl ] -2, 2-dimethylcyclopropylcarboxylate, 1g of 2, 6-di-tert-butyl-4-methylphenol, and the balance of isopropyl tridecanoate to 100g gave a 10% mother liquor.
Formulation example 14:
10g of 2,3,4, 5-tetrafluorobenzyl- (1R, 3S) -3- [ (1Z) -2-cyano-1-vinyl ] -2, 2-dimethylcyclopropylcarboxylate, 1g of 2, 6-di-tert-butyl-4-methylphenol, and tributyl citrate up to 100g give a 10% mother liquor.
Formulation example 15:
10g of 2,3,4, 5-tetrafluorobenzyl- (1S, 3S) -3- [ (1Z) -2-cyano-1-vinyl ] -2, 2-dimethylcyclopropylcarboxylate, 1g of 2, 6-di-tert-butyl-4-methylphenol, and the balance of isopropyl tridecanoate to 100g gave a 10% mother liquor.
Formulation example 16:
6g of isooctyl 2,3,4, 5-tetrafluorobenzyl- (1R, 3S) -3- [ (1Z) -2-cyano-1-vinyl ] -2, 2-dimethylcyclopropylcarboxylate, β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate 0.2g, diisopropyl adipate up to 100g, give a 6% mother liquor.
Formulation example 17:
6g of n-stearyl 2,3,4, 5-tetrafluorobenzyl- (1R, 3S) -3- [ (1Z) -2-cyano-1-vinyl ] -2, 2-dimethylcyclopropylcarboxylate, β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate 0.2g, diisopropyl adipate up to 100g gave a 6% mother liquor.
Formulation example 18:
20g of n-stearyl 2,3,4, 5-tetrafluorobenzyl- (1R, 3S) -3- [ (1Z) -2-cyano-1-vinyl ] -2, 2-dimethylcyclopropylcarboxylate, β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate 0.4g, diisopropyl adipate up to 100g, giving a 20% mother liquor.
Formulation example 19:
16g of 2,3,4, 5-tetrafluorobenzyl- (1R, 3S) -3- [ (1Z) -2-cyano-1-vinyl ] -2, 2-dimethylcyclopropylcarboxylate, 1g of 2, 6-di-tert-butyl-4-methylphenol, 45g of isopropyl tridecanoate, diisopropyl adipate up to 100g, give a 16% mother liquor.
Formulation example 20:
6g of 2,3,4, 5-tetrafluorobenzyl- (1R, 3S) -3- [ (1Z) -2-cyano-1-vinyl ] -2, 2-dimethylcyclopropylcarboxylate, 0.2g of 2, 6-di-tert-butyl-4-methylphenol, and the balance of dodecylbenzene to 100g gave a 6% mother liquor.
Formulation example 21:
6g of 2,3,4, 5-tetrafluorobenzyl- (1R, 3S) -3- [ (1Z) -2-cyano-1-vinyl ] -2, 2-dimethylcyclopropylcarboxylate, 0.2g of 2, 6-di-tert-butyl-4-methylphenol, and the tributyl acetylcitrate make up to 100g, giving a 6% mother liquor.
Formulation example 22:
0.5g of 2,3,4, 5-tetrafluorobenzyl-3- [ -2-cyano-1-vinyl ] -2, 2-dimethylcyclopropylcarboxylate, 1g of piperonyl butoxide, and up to 100g of diisopropyl adipate give a 0.5% mother liquor.
Formulation example 23 (different from formulation example 13 active ingredient):
10g of 2,3,4, 5-tetrafluorobenzyl-3- [ -2-cyano-1-vinyl ] -2, 2-dimethylcyclopropylcarboxylate, 1g of 2, 6-di-tert-butyl-4-methylphenol, and up to 100g of isopropyl tridecanoate were added to give a 10% mother liquor.
Formulation example 24:
6g of 2,3,4, 5-tetrafluorobenzyl-3- [ -2-cyano-1-vinyl ] -2, 2-dimethylcyclopropylcarboxylate, 0.2g of 2, 6-di-tert-butyl-4-methylphenol, and diisopropyl adipate up to 100g gave a 6% mother liquor.
Formulation example 25:
16g of 2,3,4, 5-tetrafluorobenzyl-3- [ -2-cyano-1-vinyl ] -2, 2-dimethylcyclopropylcarboxylate, 1g of 2, 6-di-tert-butyl-4-methylphenol, 45g of isopropyl tridecanoate, diisopropyl adipate up to 100g, give a 16% mother liquor.
The test materials in the drug effect embodiment of the invention comprise culex light color, female adults which do not suck blood after the emergence of the culex light color and the female adults are 3 to 5 days, houseflies, adults which are the adults after the emergence of the culex light color and the female adults and the male adults are the adults after the emergence of the culex light color and the female adults are the adults after the emergence of the culex light color and the age of 10 to 15 days.
Pharmacodynamic example 1:
To a mixture of 99.96g of corn starch, carbon powder and wood powder (1:5:4) was added 120g of water and kneaded to form, and then dried to form a mosquito-repellent incense base material (diameter 12.0cm, thickness 4mm, pair of weights 40 g)
The mother liquor of formulation example 1, formulation example 2, formulation example 4 and formulation example 22 was sprayed 4g onto the above mosquito-repellent incense base material to obtain 0.05% of mosquito-repellent incense coil I, mosquito-repellent incense coil II, mosquito-repellent incense coil III and mosquito-repellent incense coil V, respectively.
0.5G of 2,3,4, 5-tetrafluorobenzyl- (1R, 3S) -3- [ (1Z) -2-cyano-1-vinyl ] -2, 2-dimethylcyclopropylcarboxylate, 1g of oxidized piperonyl butoxide and 100g of odorless kerosene are complemented to obtain a 0.5% mother liquor, 4g of the mother liquor is taken and sprayed on the mosquito-repellent incense base material, and the mosquito-repellent incense coil IV is coiled.
The disc type mosquito-repellent incense I-IV is subjected to drug effect comparison according to GBT 13917.4-2009 sanitary pesticide indoor efficacy test for pesticide registration and evaluation part 4, namely mosquito-repellent incense. A cylindrical device is used. 30 mosquitoes are sucked, and the rubber plug (H) is plugged from the central round hole of the original plate (F) below the cylinder. After the tested mosquito resumes normal activity, randomly taking a section of mosquito-repellent incense to be tested, horizontally mounting on a mosquito-repellent incense frame, pre-igniting for 5min at the other position, moving to a cylinder for smoking for 1min, immediately removing the mosquito-repellent incense, plugging a rubber plug (H), timing, and recording the number of knocked-down tested insects at regular intervals. The observation time period was 20min. The test should be repeated three times or more, and the mosquito-repellent incense for repeated test should be randomly taken. After each test, the test device should be cleaned. The test results are shown in the following table:
| Mosquito-repellent incense | Concentration w/w | Culex light color KT50 (min) |
| Disc type mosquito-repellent incense I | 0.05% | 3.8 |
| Disc type mosquito-repellent incense II | 0.05% | 2.6 |
| Disc type mosquito-repellent incense III | 0.05% | 2.3 |
| Disc type mosquito-repellent incense IV | 0.05% | 3.4 |
| Disc type mosquito-repellent incense V | 0.05% | 3.1 |
Drug efficacy example 2:
The preparation example, odorless kerosene and propane-butane were mixed at room temperature in a certain ratio and added to a tank equipped with a control valve, and a propellant was added under pressure to the tank through the control valve.
Aerosol I0.5% 2,3,4, 5-tetrafluorobenzyl- (1R, 3S) -3- [ (1Z) -2-cyano-1-vinyl ] -2, 2-dimethylcyclopropylcarboxylate was prepared by mixing 5g of formulation example 13,45g of odorless kerosene at room temperature into a tank equipped with a control valve, and adding 50g of propane propellant under pressure to the tank via the control valve.
Aerosol II 0.5%2,3,4, 5-tetrafluorobenzyl- (1R, 3S) -3- [ (1Z) -2-cyano-1-vinyl ] -2, 2-dimethylcyclopropylcarboxylate was prepared by mixing 5g of formulation example 14,45g of odorless kerosene at room temperature into a tank equipped with a control valve, and adding 50g of propane propellant under pressure to the tank via the control valve.
Aerosol III 0.5%2,3,4, 5-tetrafluorobenzyl- (1S, 3S) -3- [ (1Z) -2-cyano-1-vinyl ] -2, 2-dimethylcyclopropylcarboxylate was prepared by mixing 5g of the formulation example 15,45g of odorless kerosene at room temperature into a tank equipped with a control valve, and adding 50g of propane propellant under pressure to the tank via the control valve.
Aerosol IV 0.5% of the formula A is obtained by mixing 5g of the formulation example 23,45g of odorless kerosene at room temperature in a tank equipped with a control valve and adding 50g of a butane propellant under pressure to the tank via the control valve.
Control aerosol 0.5g of 2,3,4, 5-tetrafluorobenzyl- (1R, 3S) -3- [ (1Z) -2-cyano-1-vinyl ] -2, 2-dimethylcyclopropylcarboxylate, 0.05g of 2, 6-di-tert-butyl-4-methylphenol, and odorless kerosene were made up to 50g, dissolved by heating, cooled to room temperature and then added to a tank equipped with a control valve, and 50g of a propane-butane propellant was added to the tank under pressure via the control valve to give 0.5% of 2,3,4, 5-tetrafluorobenzyl- (1R, 3S) -3- [ (1Z) -2-cyano-1-vinyl ] -2, 2-dimethylcyclopropylcarboxylate.
The test method refers to the test and evaluation of the indoor efficacy of the sanitary pesticide for pesticide registration of GB/T13917.2-2009, part 2, aerosol method, and adopts a cylinder device for mosquitoes and flies. The specific method is that the test insects (30 flies or 30 mosquitoes) are put into a jar, after the test insects return to normal activities, the aerosol cylinder to be tested is in a horizontal shape, the nozzle is vertical downwards and is aligned to the spraying hole, the medicine (1.0+/-0.1G) is sprayed, and the round hole is immediately plugged by a rubber plug (G). 1min, the pulling plate (A) is pulled out, the time is immediately counted, and the number of knocked-down insects is recorded at regular intervals. And (3) transferring the knocked-down test insects to a clean insect raising cage for 20min, recovering the raising standard, feeding with 5% sugar cotton balls, checking the dead insects for 24h, and calculating the number of the non-knocked-down test insects according to the living insects. The test should be repeated three times or more. At the end of each test, the test device should be cleaned.
Cockroach adopts a cylinder device without a pulling plate. Placing 20 German cockroaches on the upper part of the inner wall, coating vaseline on the upper part of the inner wall, sealing the inner wall with a B barrel with a 12-mesh iron screen, placing the aerosol barrel horizontally after the test insects return to normal activities, vertically aligning the spray nozzle downwards with the spray hole on E, spraying the medicament (1.0+/-0.1G), immediately plugging the round hole with a rubber plug (G), starting timing, recording the number of knocked-down test insects at regular intervals, transferring all the test insects into a cleaning vessel for 20min, returning to standard feeding, feeding with a mixed feed block and a soaked cotton ball, and checking the number of dead insects for 72 h. The test should be repeated three times or more. At the end of each test, the test apparatus should be cleaned and the detailed results are shown in the following table:
drug efficacy example 3:
16.7g of the preparation example 6,40g of D100 and 43.3g of D110 are fully and uniformly mixed, filtered, filled and matched with an inner plug and a wood fiber core rod to obtain the electrothermal mosquito-repellent incense liquid I.
And (2) fully and uniformly mixing 10g of preparation example 18,20g D130 and 70g D110, filtering, filling, and matching with an inner plug and a ceramic core rod to obtain the electrothermal mosquito-repellent incense liquid II.
16.7G of preparation example 20,40g of D100 and 43.3g of D110 are fully and uniformly mixed, filtered, filled and matched with an inner plug and a wood fiber core rod to obtain the electrothermal mosquito-repellent incense liquid III.
16.7G of preparation example 21,40g of D100 and 43.3g of D110 are fully and uniformly mixed, filtered, filled and matched with an inner plug and a wood fiber core rod to obtain the electrothermal mosquito-repellent incense liquid IV.
16.7G of preparation example 24,40g of D100 and 43.3g of D110 are fully and uniformly mixed, filtered, filled and matched with an inner plug and a wood fiber core rod to obtain the electrothermal mosquito-repellent incense liquid V.
The test method refers to the test and evaluation of the indoor efficacy of sanitary pesticide for GBT 13917.6-2009 pesticide registration, part 6, namely electric mosquito repellent liquid, a cylinder device is adopted, wherein 30 tested mosquitoes are sucked in each test, and the test device is put into a central round hole of a circular plate (F) to plug a rubber plug (H). After the test insects return to normal activities, a heater which is continuously electrified to the corresponding time interval point and carries electric heating mosquito repellent liquid to be tested is placed below the central space of the circular plate (F), the central hole is closed, fumigated and killed for 1min, the rubber plug (H) is immediately plugged, timing is carried out, and the number of the knocked-down test insects is recorded at regular intervals. The observation time was 20min. The test should be repeated three times and more. At the end of each test, the test device should be cleaned.
Control sample 1:0.31% tetrafluoro methyl ether electric mosquito repellent liquid (commercially available)
Pharmacodynamic example 4:
electric mosquito-repellent incense sheet I62.5 g of preparation example 19,37.5g D110 were thoroughly and uniformly mixed, filtered, and then 100mg of a base material (a fiber board of a compressed pulp and cotton linter mixture: 2.5cm x 1.5cm, thickness 0.3 cm) was sucked and uniformly impregnated to obtain an electric mosquito-repellent incense sheet.
Electric mosquito-repellent incense sheet II 62.5g of preparation example 25,37.5g of D110 were thoroughly and uniformly mixed, filtered, and then 100mg of a base material (a fiber board of a compressed pulp and cotton linter mixture: 2.5cm x 1.5cm, thickness 0.3 cm) was sucked and uniformly impregnated to obtain an electric mosquito-repellent incense sheet.
The test method refers to the test and evaluation of the indoor efficacy of the sanitary pesticide for GBT 13917.5-2009 pesticide registration, the 5 th part is an electric heating mosquito-repellent incense sheet, a cylinder device is adopted, 30 tested mosquitoes are sucked in each test, and the tested mosquitoes are put in the center round hole of the circular plate (F) to plug the rubber plug (H). After the insect is tested to resume normal activity, a heater which is continuously electrified to a corresponding time interval point and carries the electric mosquito-repellent incense sheet to be tested (an iron wire net is placed above the heater) is placed below the central space of the circular plate (F), the central circular hole is fastened, fumigated and killed for 1min, a rubber plug (H) is immediately plugged, timing is carried out, and the number of the knocked-down mosquitoes is recorded at regular intervals. The observation time was 20min. The test should be repeated three times and more. At the end of each test, the test device should be cleaned.
Control sample 25 mg propargyl pyrethrin+5 mg tetrafluoromethyl ether pyrethrin electric mosquito repellent tablet (commercially available)
The foregoing examples are merely illustrative of the technical concept and technical features of the present invention, and are not intended to limit the scope of the present invention. All equivalent changes or modifications made according to the essence of the present invention should be included in the scope of the present invention.
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