CN103828842A - Sasanqua leaf extract and Metarhizium anisopliae complex insecticide and preparation method thereof - Google Patents
Sasanqua leaf extract and Metarhizium anisopliae complex insecticide and preparation method thereof Download PDFInfo
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- CN103828842A CN103828842A CN201410076112.5A CN201410076112A CN103828842A CN 103828842 A CN103828842 A CN 103828842A CN 201410076112 A CN201410076112 A CN 201410076112A CN 103828842 A CN103828842 A CN 103828842A
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Abstract
The invention relates to a sasanqua leaf extract and Metarhizium anisopliae complex insecticide and a preparation method thereof. The complex insecticide is prepared from the following raw materials in mass percent: 30-60% of a sasanqua leaf extract, 10-30% of Metarhizium anisopliae, 5-20% of a surface active agent, 10-20% of an assistant and 5-15% of filler. The invention also comprises a preparation method of the sasanqua leaf extract and Metarhizium anisopliae complex insecticide. The sasanqua leaf extract and Metarhizium anisopliae complex insecticide has the characteristics of broad insecticidal spectrum, high activity, stable effect, quick insecticidal effect, strong pesticide resistance, long residual life, little environment influence, convenience in use and the like; according to the invention, the additional value of sasanqua is improved, and the large-scale application of green muscardine fungus is promoted.
Description
Technical field
The present invention relates to a kind of plant insecticide and microorganism insecticide compounded pesticides and preparation method thereof, especially relate to a kind of Camellia Leaves extract and Metarhizium anisopliae compounded pesticides and preparation method thereof.
Background technology
At present in the world, the agricultural product loss causing due to pest reaches 15～25% every year.Using on a large scale chemical pesticide is the main policies of current Control pests.But the desinsection selectivity of chemical pesticide is poor; the field longevity of residure is longer; easily bring out insect develops immunity to drugs to it simultaneously; the particularly pollution of residual chemical pesticide to agricultural product and environment; cause women's miscarriage, fetal malformation and bring out the diseases such as the various cancers of the mankind; therefore along with the enhancing of human environment protection consciousness, the biopesticide of high-efficiency low-toxicity has become the developing direction of current agricultural chemicals.For conventional chemical pesticide, biopesticide has mode of action uniqueness, prevent that object is single-minded, to beneficial organism safety such as natural enemies, consumption is little, and degraded is fast, dangerous low to people, animal, ambient wind, being specially adapted to the features such as disease, worm, crop smothering integrated control, is the higher pollution-free pesticide of a kind of safety or public nuisance-free agricultural chemicals, with the environment friendly agricultural of environmentally compatible, mechanism of action uniqueness.
Oil tea (
camellia Oleifera) originate from China, be Theaceae Camellia Plants, there is long cultivation history in China, be mainly distributed in the knob of 17 provinces such as Hunan, Jiangxi, Hubei, Guangxi, Anhui, with Hunan cultivation at most.Oil tea is the world four large woody edible oil source seeds equally celebrated for their achievements with olive, oil palm tree and coconut.Camellia Leaves is the blade of tea oil tree, and the contained chemical composition of Camellia Leaves mainly contains saponins, flavonoids and tannin class, is the raw material of medicine, pesticide industry.Wherein saponins compound is the popular domain of current researches on natural drugs, has multiple pharmacological effect; And Tea Saponin is separately as agricultural agent, can improve desinsection, the bactericidal effect of agricultural chemicals, these advantages be synthetic surfactant cannot be by comparison; It is the important natural nonionic green surfactant of Vehicles Collected from Market; As biopesticide, Tea Saponin can be directly used in some disease and insect of control separately.Meet the sustainable development of current pesticide industry and agriculture environmental protection, have a good application prospect.But this platymiscium complex chemical composition, biologically active is various, for a long time, the development and application of oil tea does not all relate to pesticide field, its medical value is left in the basket, Camellia Leaves drops mostly in oil tea forest land, directly rot and waste.Also do not report at present and utilize Camellia Leaves to extract plant insecticide, if can make full use of Camellia Leaves resource, excavate its medical value, develop plant insecticide, can make it turn waste into wealth, increase the farmers' income of rural area, be also beneficial to the sound development that promotes China's camellia oleiferaindustry, produce good Social benefit and economic benefit.
Green muscardine fungus (
metarhizium anisopliae) Universal Chinese character name: Metarhizium anisopliae (being called for short green muscardine fungus), belong to Ascomycota, Hypocreales, Clavicipitaceae, Metarhizium, be a kind of insect pathogenic bacteria of wide spectrum.Green muscardine fungus is a class disinsection fungal that can parasitize various pests, enters in pest body by body surface invasion effect, constantly increases breeding by consuming nutrition, mechanical penetration, generation toxin, and constantly in pest population, propagate in pest body, makes insect lethal.Green muscardine fungus has certain selectivity, to person poultry harmless, also have that free from environmental pollution, noresidue, insect can not be developed immunity to drugs simultaneously, the easily advantage such as production of microbial inoculum, have broad application prospects, the area of applying abroad its pest control exceedes white muscardine fungi, and control efficiency can match in excellence or beauty with white muscardine fungi.The subject matter of white stiff mattress pest control is at present that green muscardine fungus is used separately, virulence is inadequate, insecticide efficiency is not high, desinsection speed is slower, the weakness such as large and effect affected by environment is unstable, affect its control efficiency in agriculture and forestry injurious insect, thereby limited to a certain extent the large-scale application of such fungus insecticide.
In recent years, the problem that compounded pesticides brings for solution single dose agricultural chemicals has very positive effect.For example, CN200910225149.9 discloses a kind of green muscardine fungus complex insecticidal composition and application thereof, the active ingredient of composition is Metarhizium anisopliae and a kind of anabasine insecticide, wherein in composition the content of green muscardine fungus be 1～10,000,000,000 spore/gram, the content of anabasine insecticide is 10～200 grams/kilogram, and all the other are agricultural chemicals auxiliary element.The complex composition of this green muscardine fungus and chemical pesticide, relatively uses conveniently with alone green muscardine fungus, efficacy stability, and quick-acting is good; Compared with alone chemical pesticide, the lasting period is long, reduces the usage amount of chemical pesticide, reduces environmental pollution; The mechanism of action difference of composition active principle, insect is not easy to develop immunity to drugs; But this Recompounded pesticide and environment friendly agricultural require to have certain distance.China's invention training application 201310480725.0 discloses a kind of insecticides, and this insecticides comprises the raw material of following weight portion: Tea Saponin 25-30 part; Green muscardine fungus 15-20 part; Teflubenzuron 6-9 part; Building component 10-13 part; Emulsifier 5-7 part; The composite of this green muscardine fungus and vegetable insecticide, chemical insecticide greatly reduces insect pest, and also can greatly improve the concentration of medicament arrival target by building component, obtains better insecticidal effect.Wherein Teflubenzuron is process for preparation of benzoylurea compounds, although be a kind of important high-efficient low toxicity insecticide, this Recompounded pesticide and environment friendly agricultural still have certain distance.
summary of the invention
The technical problem to be solved in the present invention is, a kind of Camellia Leaves extract and green muscardine fungus compounded pesticides are provided, and this compounded pesticides desinsection spectrum width is active high, effect stability, and insecticidal effect is fast, and the longevity of residure is long, little to environmental influence, easy to use; And for the utilization of Camellia Leaves resource provides an effective way.
The technical scheme that the present invention solves its technical problem employing is:
The present invention's a kind of Camellia Leaves extract and Metarhizium anisopliae compounded pesticides, be made up of the raw material of following mass percent: Camellia Leaves extract 30～60%; Metarhizium anisopliae 10～30%; Surfactant 5～20%; Auxiliary agent 10～20%; Filler 5～15%.
Further, described Camellia Leaves extract and Metarhizium anisopliae compounded pesticides, be made up of the raw material of following mass percent: Camellia Leaves extract 60%; Metarhizium anisopliae 10%; Surfactant 10%; Auxiliary agent 15%; Filler 5%.
Further, described Camellia Leaves extract and Metarhizium anisopliae compounded pesticides, the described raw material by following mass percent is made: Camellia Leaves extract 40%; Metarhizium anisopliae 20%; Surfactant 20%; Auxiliary agent 10%; Filler 10%.
Further, described Camellia Leaves extract adopts following methods to make:
(1) mixed solvent extract: by Camellia Leaves after drying, pulverize through cracker, cross 200 mesh sieves, to the preferred 2:1 of sieving volume ratio: 1～3:1() methyl alcohol and acetone mixed extract be heated to 65～80 ℃ of (preferably 75 ℃) refluxing extraction 2～4 times (preferably 3 times), add the volume (ml) of methyl alcohol and acetone mixed extract: the preferred 8:1 of quality (g)=7～9:1(of sieving) at every turn, each extraction time is 2～4 hours (preferably 3 hours), merge after each extract, carry out decompression distillation with Rotary Evaporators and remove methyl alcohol and acetone, until methyl alcohol and acetone all volatilize, obtain methyl alcohol and acetone extract medicinal extract, methyl alcohol and the recover acetone of volatilization recycle,
(2) water extraction: mix to adding water in the described methyl alcohol of step (1) and acetone extract medicinal extract, add the volume (ml) of water: methyl alcohol and the preferred 3:1 of acetone extract medicinal extract quality (g)=2～4:1();
(3) extraction: add cyclohexane in the described methyl alcohol of step (2) and the acetone extract aqueous solution, add the volume of cyclohexane: the preferred 3:1 of volume=2～4:1(of methyl alcohol and the acetone extract aqueous solution), stir 5～10 minutes (preferably 10 minutes), then leave standstill extraction (preferably 3 hours) rear layering in 2～4 hours, get upper strata solvent phase and carry out decompression distillation recovery cyclohexane, collect lower floor's water, repeatedly extract 3～5 times (preferably 3 times), merge lower floor's water of each extraction;
(4) reextraction: add carbon tetrachloride in step (3) gained lower layer of water phase amalgamation liquid, add the volume of carbon tetrachloride: the preferred 3:1 of volume=2～4:1(of lower layer of water phase amalgamation liquid), stir 5～10 minutes (preferably 10 minutes), then leave standstill extraction (preferably 3 hours) rear layering in 2～4 hours, take off layer solvent phase and carry out decompression distillation recovery carbon tetrachloride, obtain lower floor's concentrate, repeatedly extract 3～5 times (preferably 3 times), merge after lower floor's concentrate of each extraction, carry out decompression distillation and remove remaining carbon tetrachloride, obtain Camellia Leaves extract medicinal extract, be Camellia Leaves extract.
Further, described Metarhizium anisopliae is that the concentration of spore alive is 10
10individual/g～10
12the conidial powder of individual/g.
Further, described surfactant is one or more the mixture in neopelex, lauryl sodium sulfate, calcium dodecyl benzene sulfonate, polyoxyethylene nonylphenol ether and sorbitol polyoxyethylene ether.
Further, described auxiliary agent is one or more the mixture in polyvinyl alcohol, Morwet D-400, carboxymethyl cellulose, dispersant Z, calcium lignosulfonate.
Further, described filler is one or more the mixture in diatomite, bentonite, attapulgite, starch, white carbon and kaolin.
The present invention's Camellia Leaves extract and the preparation method of Metarhizium anisopliae compounded pesticides: by after Camellia Leaves extract extract dry, pulverize through cracker, cross 200 mesh sieves, then by sieving and Metarhizium anisopliae (
metarhizium anisopliae), surfactant, auxiliary agent, filler mix by predetermined quality percentage.
Research shows, the theasaponin insecticide duration of efficacy in Camellia Leaves extract exceedes other plant type insecticide and chemical pesticide, has high efficiency, with other agriculture chemical compounding, can also save 50% ~ 70% of former medicine.Tea Saponin is compared with other chemical pesticide, and an outstanding feature, is exactly to the oral avirulence of superior being, has overcome the toxic action of chemical pesticide to human body.
The preparation method of the present invention's Camellia Leaves extract, adopts mixed solvent to extract and combines extraction with water extraction, cyclohexane, carbon tetrachloride reextraction, each several part extract is through decompression distillation, in gained Camellia Leaves extract, Tea Saponin purity is higher, and color and luster is better, and quality is higher; Realized recycling of solvent, solvent loss is few simultaneously, and extraction time is short, saves widely the energy, and simple and reliable process is easy to realize industrialization.
The present invention utilizes Camellia Leaves extract (plant insecticide) and green muscardine fungus (microorganism insecticide) to carry out composite a kind of novel pesticide of making, and this compounded pesticides has desinsection spectrum width, active high, effect stability, insecticidal effect is fast, pesticide resistance is strong, the longevity of residure is long, environmental influence is little, easy to use feature; Evidence, at the compounded pesticides of the present invention that sprays 1000 times of dilutions, after 72 hours, average killing rate can reach more than 80%.This compounded pesticides not only can the poor shortcoming of microbial pesticide quick-acting, can also improve the insecticidal activity of plant insecticide.
The present invention's Camellia Leaves extract and Metarhizium anisopliae compounded pesticides can be used for the control of fruit tree, vegetables, tealeaves, sugarcane or the economic crops insect such as melon.Utilize the present invention, can make full use of the abundant Camellia Leaves resource in mountain area, solve the problem that current biopesticide lacks, and can promote the development of mountain area economy, meanwhile, also can promote the large-scale application of green muscardine fungus.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
embodiment 1
The present embodiment compounded pesticides is formulated by the raw material of following mass percent: Camellia Leaves extract 60%, Metarhizium anisopliae (
metarhizium anisopliae) (concentration that contains the spore of living in conidial powder is 10 to conidial powder
10individual/g) 10%, neopelex 10%, Morwet D-400 15%, diatomite 5%.
Described Camellia Leaves extract is prepared from accordance with the following methods:
(1) mixed solvent extract: by Camellia Leaves after drying, pulverize with cracker, cross 200 mesh sieves, sieving is added to methyl alcohol and acetone mixed extract (methyl alcohol and acetone volume ratio 8:1), be heated to 75 ℃ of refluxing extraction 3 times, add the volume (ml) of methyl alcohol and acetone mixed extract: quality (the g)=8:1 of sieving at every turn, each extraction time is 3 hours, merge after each extract, carry out decompression distillation with Rotary Evaporators and remove methyl alcohol and acetone, until methyl alcohol and acetone all volatilize, obtain methyl alcohol and acetone extract medicinal extract; Methyl alcohol and the recover acetone utilization of volatilization;
(2) water extraction: mix to adding water in the described methyl alcohol of step (1) and acetone extract medicinal extract, obtain methyl alcohol and the acetone extract aqueous solution, the quality of the water adding is equivalent to 3 times of medicinal extract quality;
(3) extraction: add cyclohexane in the described methyl alcohol of step (2) and the acetone extract aqueous solution, add the volume of cyclohexane to be equivalent to 3 times of the volumes of methyl alcohol and the acetone extract aqueous solution, stir 10 minutes, then leave standstill extraction layering after 3 hours, get upper strata solvent phase and carry out decompression distillation recovery cyclohexane, collect lower floor's water, repeatedly extract 3 times, merge lower floor's water of each extraction;
(4) reextraction: add carbon tetrachloride in step (3) gained lower layer of water phase amalgamation liquid, add the volume of carbon tetrachloride to be equivalent to 3 times of the volumes of lower layer of water phase amalgamation liquid, stir 10 minutes, then leave standstill extraction layering after 3 hours, take off layer solvent phase and carry out decompression distillation recovery carbon tetrachloride, obtain lower floor's concentrate, repeatedly extract 3 times, merge after lower floor's concentrate of each extraction, carry out decompression distillation and remove remaining carbon tetrachloride, obtain Camellia Leaves extract medicinal extract, dry, be Camellia Leaves extract.
The present embodiment compounded pesticides preparation: described Camellia Leaves extract is pulverized with cracker, is crossed 200 mesh sieves, by the Camellia Leaves extract powder of described mistake 200 mesh sieves and Metarhizium anisopliae (
metarhizium anisopliae) (concentration that contains the spore of living in conidial powder is 10 to conidial powder
12individual/g), neopelex, Morwet D-400, diatomite mix.
The present embodiment Camellia Leaves extract and Metarhizium anisopliae compounded pesticides desinsection drug effect are as shown in table 1-3.
(1) toxic action to prodenia litura
Embodiment 1 compounded pesticides water is pressed after different multiples (1000 times, 1500 times, 2000 times) dilution, be sprayed onto cabbage leaves surface, then the prodenia litura living is raised and on cabbage leaves, carried out the test of insecticide effect, in triplicate, separately establish 3 groups of control groups: control group 1: do not spray embodiment 1 compounded pesticides; Control group 2: the Camellia Leaves extract insecticide (specifically formula: Camellia Leaves extract extract powder, neopelex, Morwet D-400, diatomite by mass percentage 70:10:15:5 mix) that sprays 1000 times of dilutions; Control group 3: spray dilution 1000 times Metarhizium anisopliae insecticide (specifically formula: Metarhizium anisopliae (
metarhizium anisopliae) (concentration of the spore of living is 10 to conidial powder
12individual/g), neopelex, Morwet D-400, diatomite by mass percentage 70:10:15:5 mix).In the different time, insecticidal effect is added up respectively, be the results are shown in Table 1.
As shown in Table 1, spraying embodiment 1 compounded pesticides dilution after 72 hours, the compounded pesticides of different extension rates reaches more than 61.3% the average killing rate of prodenia litura, and the compounded pesticides that especially dilutes 1000 times is the highest to the average killing rate of prodenia litura, can reach 80.0%; And the killing rate of control group 2 and 3 is starkly lower than the embodiment of the present invention compounded pesticides of 1000 times of dilutions.
(2) toxic action to black bean aphid
Embodiment 1 compounded pesticides is pressed after different multiples (1000 times, 1500 times, 2000 times) dilution, be sprayed onto and be cut into the basically identical broad bean seedling surface of length, the black bean aphid of living is raised and in broad bean seedling fragment, carried out the test of insecticide effect, in triplicate, separately establish 3 groups of control groups: control group 1: do not spray embodiment 1 compounded pesticides; Control group 2: the Camellia Leaves extract insecticide (specifically formula: Camellia Leaves extract extract powder, neopelex, Morwet D-400, diatomite by mass percentage 70:10:15:5 mix) that sprays 1000 times of dilutions; Control group 3: spray dilution 1000 times Metarhizium anisopliae insecticide (specifically formula: Metarhizium anisopliae (
metarhizium anisopliae) (concentration of the spore of living is 10 to conidial powder
12individual/g), neopelex, Morwet D-400, diatomite by mass percentage 70:10:15:5 mix).In the different time, insecticidal effect is added up respectively, be the results are shown in Table 2.
As shown in Table 2, spraying embodiment 1 compounded pesticides after 72 hours, the compounded pesticides of different extension rates reaches more than 65.3% the average killing rate of black bean aphid, and the compounded pesticides that especially dilutes 1000 times is the highest to the average killing rate of black bean aphid, can reach 82.0%; And the killing rate of control group 2 and 3 is starkly lower than the embodiment of the present invention compounded pesticides of 1000 times of dilutions.
(3) toxic action to mythimna separata
Embodiment 1 compounded pesticides is pressed after different multiples (1000 times, 1500 times, 2000 times) dilution, be sprayed onto and be cut into the basically identical maize seedling surface of length, the mythimna separata living is raised and in maize seedling fragment, carries out the test of insecticide effect, in triplicate, separately establish 3 groups of control groups: control group 1: do not spray embodiment 1 compounded pesticides; Control group 2: the Camellia Leaves extract insecticide (specifically formula: Camellia Leaves extract extract powder, neopelex, Morwet D-400, diatomite by mass percentage 70:10:15:5 mix) that sprays 1000 times of dilutions; Control group 3: spray dilution 1000 times Metarhizium anisopliae insecticide (specifically formula: Metarhizium anisopliae (
metarhizium anisopliae) (concentration of the spore of living is 10 to conidial powder
12individual/g), neopelex, Morwet D-400, diatomite by mass percentage 70:10:15:5 mix).In the different time, insecticidal effect is added up respectively, be the results are shown in Table 3.
As shown in Table 3, spraying embodiment 1 compounded pesticides dilution after 72 hours, the compounded pesticides of different extension rates reaches more than 63.3% the average killing rate of mythimna separata, and the compounded pesticides that especially dilutes 1000 times is the highest to the average killing rate of mythimna separata, can reach 81.3%; And the killing rate of control group 2 and 3 is starkly lower than the embodiment of the present invention compounded pesticides of 1000 times of dilutions.
embodiment 2
The difference of the present embodiment and embodiment 1 is: each material quality component proportion is: Camellia Leaves extract extract powder 40%, Metarhizium anisopliae (
metarhizium anisopliae) (concentration that contains the spore of living in conidial powder is 10 to conidial powder
10individual/g) 20%, sorbitol polyoxyethylene ether 20%, carboxymethyl cellulose 10%, bentonite 10%.
The present embodiment Camellia Leaves extract and Metarhizium anisopliae compounded pesticides desinsection drug effect are as shown in Table 4-6.
(1) toxic action to prodenia litura
Embodiment 2 insecticide waters are pressed after different multiples (1000 times, 1500 times, 2000 times) dilution, be sprayed onto cabbage leaves surface, then the prodenia litura living is raised and on cabbage leaves, carried out the test of insecticide effect, in triplicate, separately establish 3 groups of control groups: control group 1: do not spray embodiment 2 compounded pesticides; Control group 2: the Camellia Leaves extract insecticide (specifically formula: Camellia Leaves extract extract powder, sorbitol polyoxyethylene ether, carboxymethyl cellulose, bentonite by mass percentage 60:20:10:10 mix) that sprays 1000 times of dilutions; Control group 3: spray dilution 1000 times Metarhizium anisopliae insecticide (specifically formula: Metarhizium anisopliae (
metarhizium anisopliae) (concentration of the spore of living is 10 to conidial powder
12individual/g), sorbitol polyoxyethylene ether, carboxymethyl cellulose, bentonite by mass percentage 60:20:10:10 mix).In the different time, insecticidal effect is added up respectively, be the results are shown in Table 4.
As shown in Table 4, spraying embodiment 2 compounded pesticides dilutions after 72 hours, the compounded pesticides of different extension rates reaches more than 65.3% the average killing rate of prodenia litura, and the compounded pesticides that especially dilutes 1000 times is the highest to the average killing rate of prodenia litura, can reach 82.7%; And the killing rate of control group 2 and 3 is starkly lower than the embodiment of the present invention compounded pesticides of 1000 times of dilutions.
(2) toxic action to black bean aphid
Embodiment 2 compounded pesticides are pressed after different multiples (1000 times, 1500 times, 2000 times) dilution, be sprayed onto and be cut on the basically identical broad bean seedling surface of length, the black bean aphid of living is raised and in broad bean seedling fragment, carried out the test of insecticide effect, in triplicate, separately establish 3 groups of control groups: control group 1: do not spray embodiment 2 compounded pesticides; Control group 2: the Camellia Leaves extract insecticide (specifically formula: Camellia Leaves extract extract powder, sorbitol polyoxyethylene ether, carboxymethyl cellulose, bentonite by mass percentage 60:20:10:10 mix) that sprays 1000 times of dilutions; Control group 3: spray dilution 1000 times Metarhizium anisopliae insecticide (specifically formula: Metarhizium anisopliae (
metarhizium anisopliae) (concentration of the spore of living is 10 to conidial powder
12individual/g), sorbitol polyoxyethylene ether, carboxymethyl cellulose, bentonite by mass percentage 60:20:10:10 mix).In the different time, insecticidal effect is added up respectively, be the results are shown in Table 5.
As shown in Table 5, spraying embodiment 2 compounded pesticides after 72 hours, the compounded pesticides of different extension rates reaches more than 64.7% the average killing rate of black bean aphid, and the compounded pesticides that especially dilutes 1000 times is the highest to the average killing rate of black bean aphid, can reach 83.3%; And the killing rate of control group 2 and 3 is starkly lower than the embodiment of the present invention compounded pesticides of 1000 times of dilutions.
(3) toxic action to mythimna separata
Embodiment 2 compounded pesticides are pressed after different multiples (1000 times, 1500 times, 2000 times) dilution, be sprayed onto and be cut into the basically identical maize seedling surface of length, the mythimna separata living is raised and in maize seedling fragment, carries out the test of insecticide effect, in triplicate, separately establish 3 groups of control groups: control group 1: do not spray embodiment 2 compounded pesticides; Control group 2: the Camellia Leaves extract insecticide (specifically formula: Camellia Leaves extract extract powder, sorbitol polyoxyethylene ether, carboxymethyl cellulose, bentonite by mass percentage 60:20:10:10 mix) that sprays 1000 times of dilutions; Control group 3: spray dilution 1000 times Metarhizium anisopliae insecticide (specifically formula: Metarhizium anisopliae (
metarhizium anisopliae) (concentration of the spore of living is 10 to conidial powder
12individual/g), sorbitol polyoxyethylene ether, carboxymethyl cellulose, bentonite by mass percentage 60:20:10:10 mix).In the different time, insecticidal effect is added up respectively, be the results are shown in Table 6.
As shown in Table 6, spraying embodiment 2 compounded pesticides dilutions after 72 hours, the compounded pesticides of different extension rates reaches more than 66.0% the average killing rate of mythimna separata, and the compounded pesticides that especially dilutes 1000 times is the highest to the average killing rate of mythimna separata, can reach 83.3%; And the killing rate of control group 2 and 3 is starkly lower than the embodiment of the present invention compounded pesticides of 1000 times of dilutions.
embodiment 3
The difference of the present embodiment and embodiment 1 is: each material quality component proportion is: will cross 200 mesh sieve Camellia Leaves extract extract powders 30%, Metarhizium anisopliae (
metarhizium anisopliae) (concentration that contains the spore of living in conidial powder is 10 to conidial powder
10individual/g) 30%, polyoxyethylene nonylphenol ether 5%, dispersant Z20%, white carbon 15%.
The present embodiment Camellia Leaves extract and Metarhizium anisopliae compounded pesticides desinsection drug effect are as shown in table 7-9.
(1) toxic action to prodenia litura
Embodiment 3 compounded pesticides waters are pressed after different multiples (1000 times, 1500 times, 2000 times) dilution, be sprayed onto cabbage leaves surface, then the prodenia litura living is raised and on cabbage leaves, carried out the test of insecticide effect, in triplicate, separately establish 3 groups of control groups: control group 1: do not spray embodiment 3 compounded pesticides; Control group 2: the Camellia Leaves extract insecticide (specifically formula: Camellia Leaves extract extract powder, polyoxyethylene nonylphenol ether, dispersant Z, white carbon by mass percentage 60:5:20:15 mix) that sprays 1000 times of dilutions; Control group 3: spray dilution 1000 times Metarhizium anisopliae insecticide (specifically formula: Metarhizium anisopliae (
metarhizium anisopliae) (concentration of the spore of living is 10 to conidial powder
10individual/g), polyoxyethylene nonylphenol ether, dispersant Z, white carbon by mass percentage 60:5:20:15 mix).In the different time, insecticidal effect is added up respectively, be the results are shown in Table 7.
As shown in Table 7, spraying embodiment 3 compounded pesticides dilutions after 72 hours, the compounded pesticides of different extension rates reaches more than 60.0% the average killing rate of prodenia litura, and the compounded pesticides that especially dilutes 1000 times is the highest to the average killing rate of prodenia litura, can reach 78.7%; And the killing rate of control group 2 and 3 is starkly lower than the embodiment of the present invention compounded pesticides of 1000 times of dilutions.
(2) toxic action to black bean aphid
Embodiment 3 compounded pesticides are pressed after different multiples (1000 times, 1500 times, 2000 times) dilution, be sprayed onto and be cut on the basically identical broad bean seedling surface of length, the black bean aphid of living is raised and in broad bean seedling fragment, carried out the test of insecticide effect, in triplicate, separately establish 3 groups of control groups: control group 1: do not spray embodiment 3 compounded pesticides; Control group 2: the Camellia Leaves extract insecticide (specifically formula: Camellia Leaves extract extract powder, polyoxyethylene nonylphenol ether, dispersant Z, white carbon by mass percentage 60:5:20:15 mix) that sprays 1000 times of dilutions; Control group 3: spray dilution 1000 times Metarhizium anisopliae insecticide (specifically formula: Metarhizium anisopliae (
metarhizium anisopliae) (concentration of the spore of living is 10 to conidial powder
10individual/g), polyoxyethylene nonylphenol ether, dispersant Z, white carbon by mass percentage 60:5:20:15 mix).In the different time, insecticidal effect is added up respectively, be the results are shown in Table 8.
As shown in Table 8, spraying embodiment 3 compounded pesticides after 72 hours, the compounded pesticides of different extension rates reaches more than 58.7% the average killing rate of black bean aphid, and the compounded pesticides that especially dilutes 1000 times is the highest to the average killing rate of black bean aphid, can reach 78.0%; And the killing rate of control group 2 and 3 is starkly lower than the embodiment of the present invention compounded pesticides of 1000 times of dilutions.
(3) toxic action to mythimna separata
Embodiment 3 compounded pesticides are pressed after different multiples (1000 times, 1500 times, 2000 times) dilution, be sprayed onto and be cut into the basically identical maize seedling surface of length, the mythimna separata living is raised and in maize seedling fragment, carries out the test of insecticide effect, in triplicate, separately establish 3 groups of control groups: control group 1: do not spray embodiment 3 compounded pesticides; Control group 2: the Camellia Leaves extract insecticide (specifically formula: Camellia Leaves extract extract powder, polyoxyethylene nonylphenol ether, dispersant Z, white carbon by mass percentage 60:5:20:15 mix) that sprays 1000 times of dilutions; Control group 3: spray dilution 1000 times Metarhizium anisopliae insecticide (specifically formula: Metarhizium anisopliae (
metarhizium anisopliae) (concentration of the spore of living is 10 to conidial powder
10individual/g), polyoxyethylene nonylphenol ether, dispersant Z, white carbon by mass percentage 60:5:20:15 mix).In the different time, insecticidal effect is added up respectively, be the results are shown in Table 9.
As shown in Table 9, spraying embodiment 3 compounded pesticides dilutions after 72 hours, the compounded pesticides of different extension rates reaches more than 60.7% the average killing rate of mythimna separata, and the compounded pesticides that especially dilutes 1000 times is the highest to the average killing rate of mythimna separata, can reach 79.3%; And the killing rate of control group 2 and 3 is starkly lower than the embodiment of the present invention compounded pesticides of 1000 times of dilutions.
Claims (10)
1. a Camellia Leaves extract and Metarhizium anisopliae compounded pesticides, it is characterized in that, made by the raw material of following mass percent: Camellia Leaves extract 30～60%, Metarhizium anisopliae 10～30%, surfactant 5～20%, auxiliary agent 10～20%, filler 5～15%.
2. described Camellia Leaves extract as claimed in claim 1 and Metarhizium anisopliae compounded pesticides, is characterized in that, is made up: Camellia Leaves extract 60% of the raw material of following mass percent; Metarhizium anisopliae 10%; Surfactant 10%; Auxiliary agent 15%; Filler 5%.
3. described Camellia Leaves extract as claimed in claim 1 and Metarhizium anisopliae compounded pesticides, it is characterized in that, described Camellia Leaves extract and Metarhizium anisopliae compounded pesticides, is characterized in that, is made up of the raw material of following mass percent: Camellia Leaves extract 40%; Metarhizium anisopliae 20%; Surfactant 20%; Auxiliary agent 10%; Filler 10%.
4. according to Camellia Leaves extract and Metarhizium anisopliae compounded pesticides described in claim 1 or 2 or 3, it is characterized in that, described Camellia Leaves extract adopts following methods to make:
(1) mixed solvent extracts: after Camellia Leaves is dried, pulverize with cracker, add methyl alcohol and acetone mixed extract, in described methyl alcohol and acetone mixed extract, the volume ratio of methyl alcohol and acetone is 1～3:1, be heated to 65～80 ℃ of refluxing extraction 2～4 times, add the volume (ml) of methyl alcohol and acetone mixed extract: quality (g)=7～9:1 of sieving at every turn, each extraction time is 2～4 hours, merge after each extract, carry out decompression distillation with Rotary Evaporators and remove methyl alcohol and acetone, until methyl alcohol and acetone all volatilize, obtain methyl alcohol and acetone extract medicinal extract, methyl alcohol and the recover acetone utilization of volatilization,
(2) water extraction: mix to adding water in the described methyl alcohol of step (1) and acetone extract medicinal extract, obtain methyl alcohol and the acetone extract aqueous solution, add the volume (ml) of water: methyl alcohol and acetone extract medicinal extract quality (g)=2～4:1;
(3) extraction: add cyclohexane in the described methyl alcohol of step (2) and the acetone extract aqueous solution, add the volume of cyclohexane: the volume=2～4:1 of methyl alcohol and the acetone extract aqueous solution, stir 5～10 minutes, then leave standstill extraction layering after 2～4 hours, get upper strata solvent phase and carry out decompression distillation recovery cyclohexane, collect lower floor's water, repeatedly extract 3～5 times, merge lower floor's water of each extraction;
(4) reextraction: add carbon tetrachloride in step (3) gained lower layer of water phase amalgamation liquid, add the volume of carbon tetrachloride: the volume=2～4:1 of lower layer of water phase amalgamation liquid, stir 5～10 minutes, then leave standstill extraction layering after 2～4 hours, take off layer solvent phase and carry out decompression distillation recovery carbon tetrachloride, obtain lower floor's concentrate, repeatedly extract 3～5 times, merge after lower floor's concentrate of each extraction, carry out decompression distillation and remove remaining carbon tetrachloride, obtain Camellia Leaves extract medicinal extract, dry, obtain Camellia Leaves extract.
5. Camellia Leaves extract according to claim 4 and Metarhizium anisopliae compounded pesticides, it is characterized in that, described step (1), after Camellia Leaves is dried, pulverize with cracker, cross 200 mesh sieves, in sieving, add methyl alcohol and acetone mixed extract, in described methyl alcohol and acetone mixed extract, the volume ratio of methyl alcohol and acetone is 2:1, be heated to 75 ℃ of refluxing extraction 3 times, add the volume (ml) of methyl alcohol and acetone mixed extract: quality (the g)=8:1 of sieving at every turn, each extraction time is 3 hours, merge after each extract, carry out decompression distillation with Rotary Evaporators and remove methyl alcohol and acetone, until methyl alcohol and acetone all volatilize, obtain methyl alcohol and acetone extract medicinal extract.
6. according to the Camellia Leaves extract described in claim 4 or 5 and Metarhizium anisopliae compounded pesticides, it is characterized in that, described step (2), mix to adding water in the described methyl alcohol of step (1) and acetone extract medicinal extract, add the volume (ml) of water: methyl alcohol and acetone extract medicinal extract quality (g)=3:1.
7. according to the Camellia Leaves extract one of claim 4～6 Suo Shu and Metarhizium anisopliae compounded pesticides, it is characterized in that, described step (3), in the described methyl alcohol of step (2) and the acetone extract aqueous solution, add cyclohexane, add the volume of cyclohexane: the volume=3:1 of methyl alcohol and the acetone extract aqueous solution, stir 10 minutes, then leave standstill extraction layering after 3 hours, get upper strata solvent phase and carry out decompression distillation recovery cyclohexane, collect lower floor's water, repeatedly extract 3 times, merge lower floor's water of each extraction.
8. according to the Camellia Leaves extract one of claim 4～7 Suo Shu and Metarhizium anisopliae compounded pesticides, it is characterized in that, described step (4), in step (3) gained lower layer of water phase amalgamation liquid, add carbon tetrachloride, add the volume of carbon tetrachloride: the volume=3:1 of lower layer of water phase amalgamation liquid, stir 10 minutes, then leave standstill extraction layering after 3 hours, take off layer solvent phase and carry out decompression distillation recovery carbon tetrachloride, obtain lower floor's concentrate, repeatedly extract 3 times, merge after lower floor's concentrate of each extraction, carry out decompression distillation and remove remaining carbon tetrachloride, obtain Camellia Leaves extract medicinal extract.
9. according to the Camellia Leaves extract one of claim 1～8 Suo Shu and Metarhizium anisopliae compounded pesticides, it is characterized in that, described Metarhizium anisopliae is that the concentration of spore alive is 10
10individual/g～10
12the conidial powder of individual/g;
Described surfactant is one or more the mixture in neopelex, lauryl sodium sulfate, calcium dodecyl benzene sulfonate, polyoxyethylene nonylphenol ether and sorbitol polyoxyethylene ether; Described auxiliary agent is one or more the mixture in polyvinyl alcohol, Morwet D-400, carboxymethyl cellulose, dispersant Z, calcium lignosulfonate; Described filler is one or more the mixture in diatomite, bentonite, attapulgite, starch, white carbon and kaolin.
10. a Camellia Leaves extract as described in one of claim 1～9 and the preparation method of Metarhizium anisopliae compounded pesticides, it is characterized in that, by after Camellia Leaves extract extract dry, pulverize through cracker, cross 200 mesh sieves, then by sieving and Metarhizium anisopliae (
metarhizium anisopliae), surfactant, auxiliary agent, filler mix by predetermined quality percentage.
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| GB2577250A (en) * | 2018-09-14 | 2020-03-25 | Bionema Ltd | Insect-pathogenic fungus, spores, composition and use of same |
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