CN103828842B - Camellia Leaves extract and Metarhizium anisopliae compounded pesticides and preparation method thereof - Google Patents
Camellia Leaves extract and Metarhizium anisopliae compounded pesticides and preparation method thereof Download PDFInfo
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Abstract
Camellia Leaves extract and Metarhizium anisopliae compounded pesticides and preparation method thereof, described compounded pesticides is 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%.The present invention also comprises the preparation method of described compounded pesticides.The features such as compounded pesticides of the present invention has desinsection spectrum width, activity is high, effect stability, insecticidal effect are fast, pesticide resistance is strong, the longevity of residure is long, environmental influence is little, easy to use; Utilize the present invention, also can improve the added value of oil tea, meanwhile, also can promote the large-scale application of green muscardine fungus.
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 crop loss caused due to pest reaches 15 ~ 25% every year.Use chemical pesticide is the main policies of current Control pests on a large scale.But the desinsection selectivity of chemical pesticide is poor; the field longevity of residure is longer; easily bring out insect to develop immunity to drugs to it simultaneously; particularly chemical residue agricultural chemicals is to the pollution of agricultural product and environment; cause women to miscarry, 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 the chemical pesticide of routine, biopesticide has mode of action uniqueness, prevent object single-minded, to beneficial organism safety such as natural enemies, consumption is little, and degraded is fast, low to people, animal, environmental risks, 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, namely with the environment friendly agricultural of environmentally compatible, mechanism of action uniqueness.
Oil tea (
camelliaOleifera) originate from China, be Theaceae Camellia Plants, in China, there is long cultivation history, 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 chemical composition contained by 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 the desinsection of agricultural chemicals, bactericidal effect, these advantages are that synthetic surfactant institute cannot be by comparison; It is the important natural nonionic green surfactant of Vehicles Collected from Market; Separately as biopesticide, Tea Saponin can be directly used in some disease and insect of control.Meet the sustainable development of current pesticide industry and agriculture environmental protection, have a good application prospect.But this platymiscium complex chemical composition, diverse biological activities, for a long time, the development and application of oil tea does not all relate to pesticide field, and its medical value is left in the basket, and Camellia Leaves drops in oil tea forest land mostly, directly rots and wastes.Also do not report at present and utilize Camellia Leaves to extract plant insecticide, if Camellia Leaves resource can be made full use of, excavate its medical value, develop plant insecticide, it can be made to turn waste into wealth, increase the farmers' income of rural area, be also beneficial to the sound development promoting China's camellia oleiferaindustry, produce good Social benefit and economic benefit.
Green muscardine fungus (
metarhiziumanisopliae) Universal Chinese character name: Metarhizium anisopliae (being called for short green muscardine fungus), belonging to Ascomycota, Hypocreales, Clavicipitaceae, Metarhizium, is 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 propagates in pest population, make insect lethal in pest body.Green muscardine fungus has certain selectivity, to person poultry harmless, also there is free from environmental pollution, noresidue simultaneously, the advantage such as insect can not develop immunity to drugs, microbial inoculum is easily produced, have broad application prospects, the area applying its pest control abroad exceedes white muscardine fungi, and control efficiency can match in excellence or beauty with white muscardine fungi.The subject matter of current white stiff mattress pest control is that green muscardine fungus is used alone, virulence is inadequate, insecticide efficiency is not high, desinsection speed is slower, the weakness such as comparatively large and effect instability affected by environment, have impact on its control efficiency in agriculture and forestry injurious insect, thus limit the large-scale application of such fungus insecticide to a certain extent.
In recent years, the problem that compounded pesticides brings for solution single dose agricultural chemicals has very positive effect.Such as, 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, compare with alone green muscardine fungus and use conveniently, efficacy stability, 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 of composition active principle is different, and insect is not easy to develop immunity to drugs; But this Recompounded pesticide and environment friendly agricultural require certain distance.Chinese invention patent 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; This green muscardine fungus and vegetable insecticide, the composite of chemical insecticide make insect pest greatly reduce, and also greatly can improve by building component the concentration that medicament arrives target, obtain 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, provides a kind of Camellia Leaves extract and green muscardine fungus compounded pesticides, this compounded pesticides desinsection spectrum width, active high, effect stability, and insecticidal effect is fast, and the longevity of residure is long, little to environmental influence, easy to use; And provide an effective way for the utilization of Camellia Leaves resource.
The technical scheme that the present invention solves the employing of its technical problem is:
A kind of Camellia Leaves extract of the present invention 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 extracts: 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 DEG C of (preferably 75 DEG C) 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), after merging 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: add water mixing in step (1) described methyl alcohol 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) extract: in step (2) described methyl alcohol and the acetone extract aqueous solution, add cyclohexane, 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 extraction (preferably 3 hours) layering afterwards in 2 ~ 4 hours is left standstill, get upper strata solvent and carry out decompression distillation recovery cyclohexane mutually, collect lower floor's aqueous phase, repeatedly extract 3 ~ 5 times (preferably 3 times);
(4) reextraction: add carbon tetrachloride in step (3) gained lower floor aqueous phase, add the volume of carbon tetrachloride: the preferred 3:1 of volume=2 ~ 4:1(of lower floor's aqueous phase), stir 5 ~ 10 minutes (preferably 10 minutes), then extraction (preferably 3 hours) layering afterwards in 2 ~ 4 hours is left standstill, take off layer solvent and carry out decompression distillation recovery carbon tetrachloride mutually, obtain lower floor's concentrate, repeatedly extract 3 ~ 5 times (preferably 3 times), after merging 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 the concentration of spore alive is 10
10individual/g ~ 10
12the conidial powder of individual/g.
Further, described surfactant is the mixture of one or more in neopelex, lauryl sodium sulfate, calcium dodecyl benzene sulfonate, polyoxyethylene nonylphenol ether and sorbitol polyoxyethylene ether.
Further, described auxiliary agent is the mixture of one or more in polyvinyl alcohol, MorwetD-400, carboxymethyl cellulose, dispersant Z, calcium lignosulfonate.
Further, described filler is the mixture of one or more in diatomite, bentonite, attapulgite, starch, white carbon and kaolin.
The Camellia Leaves extract of the present invention and the preparation method of Metarhizium anisopliae compounded pesticides: after Camellia Leaves extract extract dry, pulverize through cracker, crosses 200 mesh sieves, then by sieving and Metarhizium anisopliae (
metarhiziumanisopliae), surfactant, auxiliary agent, filler press predetermined quality percentage mixing.
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 superior being oral, non-toxic, overcomes the toxic action of chemical pesticide to human body.
The preparation method of the Camellia Leaves extract of the present invention, adopts mixed solvent to extract and water extraction combined extracting, 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; Achieve recycling of solvent, solvent loss is few simultaneously, and extraction time is short, widely economize energy, 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 compositely making a kind of novel pesticide, and this compounded pesticides has desinsection spectrum width, activity is high, effect stability, insecticidal effect are fast, pesticide resistance is strong, the longevity of residure is long, environmental influence is little, easy to use feature; Test proves, spraying the compounded pesticides of the present invention of dilution 1000 times after 72 hours, average killing rate can reach more than 80%.This compounded pesticides not only can the shortcoming of microbial pesticide quick-acting difference, can also improve the insecticidal activity of plant insecticide.
The Camellia Leaves extract of the present invention 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, the Camellia Leaves resource that mountain area is abundant can be made full use of, solve the problem that current biopesticide lacks, and the development of mountain area economy can be promoted, 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 (
metarhiziumanisopliae) (concentration containing spore of living in conidial powder is 10 to conidial powder
10individual/g) 10%, neopelex 10%, MorwetD-40015%, diatomite 5%.
Described Camellia Leaves extract is prepared from accordance with the following methods:
(1) mixed solvent extracts: by Camellia Leaves after drying, pulverize with cracker, cross 200 mesh sieves, methyl alcohol and acetone mixed extract (methyl alcohol and acetone volume ratio 8:1) are added to sieving, be heated to 75 DEG C 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, after merging 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; The methyl alcohol of volatilization and recover acetone utilize;
(2) water extraction: add water mixing in step (1) described methyl alcohol and acetone extract medicinal extract, and obtain methyl alcohol and the acetone extract aqueous solution, the quality of the water added is equivalent to 3 times of medicinal extract quality;
(3) extract: in step (2) described methyl alcohol and the acetone extract aqueous solution, add cyclohexane, add cyclohexane volume be equivalent to the volume 3 times of methyl alcohol and the acetone extract aqueous solution, stir 10 minutes, then extraction layering after 3 hours is left standstill, get upper strata solvent and carry out decompression distillation recovery cyclohexane mutually, collect lower floor's aqueous phase, repeatedly extract 3 times;
(4) reextraction: add carbon tetrachloride in step (3) gained lower floor aqueous phase, add carbon tetrachloride volume be equivalent to the volume 3 times of lower floor's aqueous phase, stir 10 minutes, then leave standstill extraction layering after 3 hours, take off layer solvent and carry out decompression distillation recovery carbon tetrachloride mutually, obtain lower floor's concentrate, repeatedly extract 3 times, after merging 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.
Prepared by the present embodiment compounded pesticides: pulverized by described Camellia Leaves extract cracker, crosses 200 mesh sieves, by the Camellia Leaves extract powder of described mistake 200 mesh sieve and Metarhizium anisopliae (
metarhiziumanisopliae) (concentration containing spore of living in conidial powder is 10 to conidial powder
12individual/g), neopelex, MorwetD-400, diatomite mixing.
The present embodiment Camellia Leaves extract and Metarhizium anisopliae compounded pesticides desinsection drug effect are as shown shown in 1-3.
(1) to the toxic action of prodenia litura
After embodiment 1 compounded pesticides use water being pressed different multiples (1000 times, 1500 times, 2000 times) dilution, be sprayed onto cabbage leaves surface, then the prodenia litura lived is raised and carry out the test of insecticide effect on cabbage leaves, in triplicate, 3 groups of control groups are separately established: control group 1: do not spray embodiment 1 compounded pesticides; Control group 2: the Camellia Leaves extract insecticide (specifically filling a prescription: the 70:10:15:5 mixing by mass percentage of Camellia Leaves extract extract powder, neopelex, MorwetD-400, diatomite) spraying dilution 1000 times; Control group 3: spray dilution 1000 times Metarhizium anisopliae insecticide (specifically fill a prescription: Metarhizium anisopliae (
metarhiziumanisopliae) (concentration of spore of living is 10 to conidial powder
12individual/g), neopelex, MorwetD-400, diatomite by mass percentage 70:10:15:5 mixing).In the different time, insecticidal effect is added up respectively, the results are shown in Table 1.
Table 1 embodiment 1 compounded pesticides is to the toxic effect of prodenia litura
As shown in Table 1, at sprinkling embodiment 1 compounded pesticides dilution after 72 hours, the average killing rate of compounded pesticides to prodenia litura of different extension rate reaches more than 61.3%, and the average killing rate of compounded pesticides to prodenia litura especially diluting 1000 times is the highest, 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 dilution 1000 times.
(2) to the toxic action of black bean aphid
After embodiment 1 compounded pesticides being pressed 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 in broad bean seedling fragment, carries out the test of insecticide effect, in triplicate, 3 groups of control groups are separately established: control group 1: do not spray embodiment 1 compounded pesticides; Control group 2: the Camellia Leaves extract insecticide (specifically filling a prescription: the 70:10:15:5 mixing by mass percentage of Camellia Leaves extract extract powder, neopelex, MorwetD-400, diatomite) spraying dilution 1000 times; Control group 3: spray dilution 1000 times Metarhizium anisopliae insecticide (specifically fill a prescription: Metarhizium anisopliae (
metarhiziumanisopliae) (concentration of spore of living is 10 to conidial powder
12individual/g), neopelex, MorwetD-400, diatomite by mass percentage 70:10:15:5 mixing).In the different time, insecticidal effect is added up respectively, the results are shown in Table 2.
Table 2 embodiment 1 compounded pesticides is to the toxic effect of black bean aphid
As shown in Table 2, at sprinkling embodiment 1 compounded pesticides after 72 hours, the average killing rate of compounded pesticides to black bean aphid of different extension rate reaches more than 65.3%, and the average killing rate of compounded pesticides to black bean aphid especially diluting 1000 times is the highest, 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 dilution 1000 times.
(3) to the toxic action of mythimna separata
After embodiment 1 compounded pesticides being pressed 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 lived is raised in maize seedling fragment, carries out the test of insecticide effect, in triplicate, 3 groups of control groups are separately established: control group 1: do not spray embodiment 1 compounded pesticides; Control group 2: the Camellia Leaves extract insecticide (specifically filling a prescription: the 70:10:15:5 mixing by mass percentage of Camellia Leaves extract extract powder, neopelex, MorwetD-400, diatomite) spraying dilution 1000 times; Control group 3: spray dilution 1000 times Metarhizium anisopliae insecticide (specifically fill a prescription: Metarhizium anisopliae (
metarhiziumanisopliae) (concentration of spore of living is 10 to conidial powder
12individual/g), neopelex, MorwetD-400, diatomite by mass percentage 70:10:15:5 mixing).In the different time, insecticidal effect is added up respectively, the results are shown in Table 3.
Table 3 embodiment 1 compounded pesticides is to the toxic effect of mythimna separata
As shown in Table 3, at sprinkling embodiment 1 compounded pesticides dilution after 72 hours, the average killing rate of compounded pesticides to mythimna separata of different extension rate reaches more than 63.3%, and the average killing rate of compounded pesticides to mythimna separata especially diluting 1000 times is the highest, 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 dilution 1000 times.
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 (
metarhiziumanisopliae) (concentration containing 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) to the toxic action of prodenia litura
After embodiment 2 insecticide use water being pressed different multiples (1000 times, 1500 times, 2000 times) dilution, be sprayed onto cabbage leaves surface, then the prodenia litura lived is raised and carry out the test of insecticide effect on cabbage leaves, in triplicate, 3 groups of control groups are separately established: control group 1: do not spray embodiment 2 compounded pesticides; Control group 2: the Camellia Leaves extract insecticide (specifically filling a prescription: the 60:20:10:10 mixing by mass percentage of Camellia Leaves extract extract powder, sorbitol polyoxyethylene ether, carboxymethyl cellulose, bentonite) spraying dilution 1000 times; Control group 3: spray dilution 1000 times Metarhizium anisopliae insecticide (specifically fill a prescription: Metarhizium anisopliae (
metarhiziumanisopliae) (concentration of spore of living is 10 to conidial powder
12individual/g), sorbitol polyoxyethylene ether, carboxymethyl cellulose, bentonite by mass percentage 60:20:10:10 mixing).In the different time, insecticidal effect is added up respectively, the results are shown in Table 4.
Table 4 embodiment 2 compounded pesticides is to the toxic effect of prodenia litura
As shown in Table 4, at sprinkling embodiment 2 compounded pesticides dilution after 72 hours, the average killing rate of compounded pesticides to prodenia litura of different extension rate reaches more than 65.3%, and the average killing rate of compounded pesticides to prodenia litura especially diluting 1000 times is the highest, 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 dilution 1000 times.
(2) to the toxic action of black bean aphid
After embodiment 2 compounded pesticides being pressed different multiples (1000 times, 1500 times, 2000 times) dilution, be sprayed onto and be cut into the basically identical broad bean seedling of length on the surface, the black bean aphid of living is raised in broad bean seedling fragment, carries out the test of insecticide effect, in triplicate, 3 groups of control groups are separately established: control group 1: do not spray embodiment 2 compounded pesticides; Control group 2: the Camellia Leaves extract insecticide (specifically filling a prescription: the 60:20:10:10 mixing by mass percentage of Camellia Leaves extract extract powder, sorbitol polyoxyethylene ether, carboxymethyl cellulose, bentonite) spraying dilution 1000 times; Control group 3: spray dilution 1000 times Metarhizium anisopliae insecticide (specifically fill a prescription: Metarhizium anisopliae (
metarhiziumanisopliae) (concentration of spore of living is 10 to conidial powder
12individual/g), sorbitol polyoxyethylene ether, carboxymethyl cellulose, bentonite by mass percentage 60:20:10:10 mixing).In the different time, insecticidal effect is added up respectively, the results are shown in Table 5.
Table 5 embodiment 2 compounded pesticides is to the toxic effect of black bean aphid
As shown in Table 5, at sprinkling embodiment 2 compounded pesticides after 72 hours, the average killing rate of compounded pesticides to black bean aphid of different extension rate reaches more than 64.7%, and the average killing rate of compounded pesticides to black bean aphid especially diluting 1000 times is the highest, 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 dilution 1000 times.
(3) to the toxic action of mythimna separata
After embodiment 2 compounded pesticides being pressed 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 lived is raised in maize seedling fragment, carries out the test of insecticide effect, in triplicate, 3 groups of control groups are separately established: control group 1: do not spray embodiment 2 compounded pesticides; Control group 2: the Camellia Leaves extract insecticide (specifically filling a prescription: the 60:20:10:10 mixing by mass percentage of Camellia Leaves extract extract powder, sorbitol polyoxyethylene ether, carboxymethyl cellulose, bentonite) spraying dilution 1000 times; Control group 3: spray dilution 1000 times Metarhizium anisopliae insecticide (specifically fill a prescription: Metarhizium anisopliae (
metarhiziumanisopliae) (concentration of spore of living is 10 to conidial powder
12individual/g), sorbitol polyoxyethylene ether, carboxymethyl cellulose, bentonite by mass percentage 60:20:10:10 mixing).In the different time, insecticidal effect is added up respectively, the results are shown in Table 6.
Table 6 embodiment 2 compounded pesticides is to the toxic effect of mythimna separata
As shown in Table 6, at sprinkling embodiment 2 compounded pesticides dilution after 72 hours, the average killing rate of compounded pesticides to mythimna separata of different extension rate reaches more than 66.0%, and the average killing rate of compounded pesticides to mythimna separata especially diluting 1000 times is the highest, 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 dilution 1000 times.
embodiment 3
The difference of the present embodiment and embodiment 1 is: each material quality component proportion is: by 200 mesh sieve Camellia Leaves extract extract powders 30%, Metarhizium anisopliae (
metarhiziumanisopliae) (concentration containing 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 shown in 7-9.
(1) to the toxic action of prodenia litura
After embodiment 3 compounded pesticides use water being pressed different multiples (1000 times, 1500 times, 2000 times) dilution, be sprayed onto cabbage leaves surface, then the prodenia litura lived is raised and carry out the test of insecticide effect on cabbage leaves, in triplicate, 3 groups of control groups are separately established: control group 1: do not spray embodiment 3 compounded pesticides; Control group 2: the Camellia Leaves extract insecticide (specifically filling a prescription: the 60:5:20:15 mixing by mass percentage of Camellia Leaves extract extract powder, polyoxyethylene nonylphenol ether, dispersant Z, white carbon) spraying dilution 1000 times; Control group 3: spray dilution 1000 times Metarhizium anisopliae insecticide (specifically fill a prescription: Metarhizium anisopliae (
metarhiziumanisopliae) (concentration of spore of living is 10 to conidial powder
10individual/g), polyoxyethylene nonylphenol ether, dispersant Z, white carbon by mass percentage 60:5:20:15 mixing).In the different time, insecticidal effect is added up respectively, the results are shown in Table 7.
Table 7 embodiment 3 compounded pesticides is to the toxic effect of prodenia litura
As shown in Table 7, at sprinkling embodiment 3 compounded pesticides dilution after 72 hours, the average killing rate of compounded pesticides to prodenia litura of different extension rate reaches more than 60.0%, and the average killing rate of compounded pesticides to prodenia litura especially diluting 1000 times is the highest, 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 dilution 1000 times.
(2) to the toxic action of black bean aphid
After embodiment 3 compounded pesticides being pressed different multiples (1000 times, 1500 times, 2000 times) dilution, be sprayed onto and be cut into the basically identical broad bean seedling of length on the surface, the black bean aphid of living is raised in broad bean seedling fragment, carries out the test of insecticide effect, in triplicate, 3 groups of control groups are separately established: control group 1: do not spray embodiment 3 compounded pesticides; Control group 2: the Camellia Leaves extract insecticide (specifically filling a prescription: the 60:5:20:15 mixing by mass percentage of Camellia Leaves extract extract powder, polyoxyethylene nonylphenol ether, dispersant Z, white carbon) spraying dilution 1000 times; Control group 3: spray dilution 1000 times Metarhizium anisopliae insecticide (specifically fill a prescription: Metarhizium anisopliae (
metarhiziumanisopliae) (concentration of spore of living is 10 to conidial powder
10individual/g), polyoxyethylene nonylphenol ether, dispersant Z, white carbon by mass percentage 60:5:20:15 mixing).In the different time, insecticidal effect is added up respectively, the results are shown in Table 8.
Table 8 embodiment 3 compounded pesticides is to the toxic effect of black bean aphid
As shown in Table 8, at sprinkling embodiment 3 compounded pesticides after 72 hours, the average killing rate of compounded pesticides to black bean aphid of different extension rate reaches more than 58.7%, and the average killing rate of compounded pesticides to black bean aphid especially diluting 1000 times is the highest, 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 dilution 1000 times.
(3) to the toxic action of mythimna separata
After embodiment 3 compounded pesticides being pressed 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 lived is raised in maize seedling fragment, carries out the test of insecticide effect, in triplicate, 3 groups of control groups are separately established: control group 1: do not spray embodiment 3 compounded pesticides; Control group 2: the Camellia Leaves extract insecticide (specifically filling a prescription: the 60:5:20:15 mixing by mass percentage of Camellia Leaves extract extract powder, polyoxyethylene nonylphenol ether, dispersant Z, white carbon) spraying dilution 1000 times; Control group 3: spray dilution 1000 times Metarhizium anisopliae insecticide (specifically fill a prescription: Metarhizium anisopliae (
metarhiziumanisopliae) (concentration of spore of living is 10 to conidial powder
10individual/g), polyoxyethylene nonylphenol ether, dispersant Z, white carbon by mass percentage 60:5:20:15 mixing).In the different time, insecticidal effect is added up respectively, the results are shown in Table 9.
Table 9 embodiment 3 compounded pesticides is to the toxic effect of mythimna separata
As shown in Table 9, at sprinkling embodiment 3 compounded pesticides dilution after 72 hours, the average killing rate of compounded pesticides to mythimna separata of different extension rate reaches more than 60.7%, and the average killing rate of compounded pesticides to mythimna separata especially diluting 1000 times is the highest, 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 dilution 1000 times.
Claims (15)
1. a Camellia Leaves extract and Metarhizium anisopliae compounded pesticides, it is characterized in that, 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%;
Described Camellia Leaves extract adopts following methods to make:
(1) mixed solvent extracts: after being dried by Camellia Leaves, pulverize with cracker, cross 200 mesh sieves, 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 DEG C of refluxing extraction 2 ~ 4 times, add the volume ml of methyl alcohol and acetone mixed extract: the quality g=7 ~ 9:1 of sieving at every turn, each extraction time is 2 ~ 4 hours, after merging 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, the methyl alcohol of volatilization and recover acetone utilize,
(2) water extraction: add water mixing in step (1) described methyl alcohol and acetone extract medicinal extract, obtains 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) extract: in step (2) described methyl alcohol and the acetone extract aqueous solution, add cyclohexane, the volume of added cyclohexane: the volume=2 ~ 4:1 of methyl alcohol and the acetone extract aqueous solution, stir 5 ~ 10 minutes, then extraction layering after 2 ~ 4 hours is left standstill, get upper strata solvent and carry out decompression distillation recovery cyclohexane mutually, collect lower floor's aqueous phase, repeatedly extract 3 ~ 5 times;
(4) reextraction: add carbon tetrachloride in step (3) gained lower floor aqueous phase, the volume of added carbon tetrachloride: the volume=2 ~ 4:1 of lower floor's aqueous phase, stir 5 ~ 10 minutes, then extraction layering after 2 ~ 4 hours is left standstill, take off layer solvent and carry out decompression distillation recovery carbon tetrachloride mutually, obtain lower floor's concentrate, repeatedly extract 3 ~ 5 times, after merging 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;
Described surfactant is the mixture of one or more in neopelex, lauryl sodium sulfate, calcium dodecyl benzene sulfonate, polyoxyethylene nonylphenol ether and sorbitol polyoxyethylene ether;
Described filler is the mixture of one or more in diatomite, bentonite, attapulgite, starch, white carbon and kaolin;
Described auxiliary agent is the mixture of one or more in polyvinyl alcohol, MorwetD-400, carboxymethyl cellulose, calcium lignosulfonate.
2. Camellia Leaves extract as claimed in claim 1 and Metarhizium anisopliae compounded pesticides, is characterized in that, 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%.
3. Camellia Leaves extract as claimed in claim 1 and Metarhizium anisopliae compounded pesticides, is characterized in that, be 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. Camellia Leaves extract according to claim 1 and Metarhizium anisopliae compounded pesticides, it is characterized in that, described step (1), in described methyl alcohol and acetone mixed extract, the volume ratio of methyl alcohol and acetone is 2:1, be heated to 75 DEG C of refluxing extraction 3 times, add the volume ml of methyl alcohol and acetone mixed extract: the quality g=8:1 of sieving at every turn, each extraction time is 3 hours, after merging 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.
5. according to the Camellia Leaves extract one of Claims 1 to 4 Suo Shu and Metarhizium anisopliae compounded pesticides, it is characterized in that, described step (2), add water mixing in step (1) described methyl alcohol and acetone extract medicinal extract, add the volume ml of water: methyl alcohol and acetone extract medicinal extract quality g=3:1.
6. according to the Camellia Leaves extract one of Claims 1 to 4 Suo Shu and Metarhizium anisopliae compounded pesticides, it is characterized in that, described step (3), in step (2) described methyl alcohol and the acetone extract aqueous solution, add cyclohexane, the volume of added cyclohexane: the volume=3:1 of methyl alcohol and the acetone extract aqueous solution, stir 10 minutes, then extraction layering after 3 hours is left standstill, get upper strata solvent and carry out decompression distillation recovery cyclohexane mutually, collect lower floor's aqueous phase, repeatedly extract 3 times.
7. Camellia Leaves extract according to claim 5 and Metarhizium anisopliae compounded pesticides, it is characterized in that, described step (3), in step (2) described methyl alcohol and the acetone extract aqueous solution, add cyclohexane, the volume of added cyclohexane: the volume=3:1 of methyl alcohol and the acetone extract aqueous solution, stir 10 minutes, then extraction layering after 3 hours is left standstill, get upper strata solvent and carry out decompression distillation recovery cyclohexane mutually, collect lower floor's aqueous phase, repeatedly extract 3 times.
8. according to the Camellia Leaves extract one of Claims 1 to 4 Suo Shu and Metarhizium anisopliae compounded pesticides, it is characterized in that, described step (4), carbon tetrachloride is added in step (3) gained lower floor aqueous phase, add the volume of carbon tetrachloride: the volume=3:1 of lower floor's aqueous phase, stir 10 minutes, then extraction layering after 3 hours is left standstill, take off layer solvent and carry out decompression distillation recovery carbon tetrachloride mutually, obtain lower floor's concentrate, repeatedly extract 3 times, after merging lower floor's concentrate of each extraction, carry out decompression distillation and remove remaining carbon tetrachloride, obtain Camellia Leaves extract medicinal extract.
9. Camellia Leaves extract according to claim 5 and Metarhizium anisopliae compounded pesticides, it is characterized in that, described step (4), carbon tetrachloride is added in step (3) gained lower floor aqueous phase, add the volume of carbon tetrachloride: the volume=3:1 of lower floor's aqueous phase, stir 10 minutes, then extraction layering after 3 hours is left standstill, take off layer solvent and carry out decompression distillation recovery carbon tetrachloride mutually, obtain lower floor's concentrate, repeatedly extract 3 times, after merging lower floor's concentrate of each extraction, carry out decompression distillation and remove remaining carbon tetrachloride, obtain Camellia Leaves extract medicinal extract.
10. Camellia Leaves extract according to claim 6 and Metarhizium anisopliae compounded pesticides, it is characterized in that, described step (4), carbon tetrachloride is added in step (3) gained lower floor aqueous phase, add the volume of carbon tetrachloride: the volume=3:1 of lower floor's aqueous phase, stir 10 minutes, then extraction layering after 3 hours is left standstill, take off layer solvent and carry out decompression distillation recovery carbon tetrachloride mutually, obtain lower floor's concentrate, repeatedly extract 3 times, after merging lower floor's concentrate of each extraction, carry out decompression distillation and remove remaining carbon tetrachloride, obtain Camellia Leaves extract medicinal extract.
11., according to the Camellia Leaves extract one of Claims 1 to 4 Suo Shu and Metarhizium anisopliae compounded pesticides, is characterized in that, described Metarhizium anisopliae is the concentration of spore alive is 10
10individual/g ~ 10
12the conidial powder of individual/g.
12. Camellia Leaves extract according to claim 5 and Metarhizium anisopliae compounded pesticides, is characterized in that, described Metarhizium anisopliae is the concentration of spore alive is 10
10individual/g ~ 10
12the conidial powder of individual/g.
13. Camellia Leaves extract according to claim 6 and Metarhizium anisopliae compounded pesticides, is characterized in that, described Metarhizium anisopliae is the concentration of spore alive is 10
10individual/g ~ 10
12the conidial powder of individual/g.
14. Camellia Leaves extract according to claim 7 and Metarhizium anisopliae compounded pesticides, is characterized in that, described Metarhizium anisopliae is the concentration of spore alive is 10
10individual/g ~ 10
12the conidial powder of individual/g.
The preparation method of 15. 1 kinds of Camellia Leaves extracts as described in one of claim 1 ~ 14 and Metarhizium anisopliae compounded pesticides, it is characterized in that, after Camellia Leaves extract extract dry, pulverize through cracker, cross 200 mesh sieves, then by sieving and Metarhizium anisopliae (
metarhiziumanisopliae), surfactant, auxiliary agent, filler press predetermined quality percentage mixing.
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| CN106359466A (en) * | 2016-08-19 | 2017-02-01 | 管天球 | Oil tea camellia leaf bio-pesticide and preparation method thereof |
| CN107788033A (en) * | 2017-10-30 | 2018-03-13 | 江西省长实竹子科技有限公司 | One vegetative insecticide and preparation method thereof |
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