CN103141523A - Acanthopanax gracilistylus insecticide and its preparation method - Google Patents
Acanthopanax gracilistylus insecticide and its preparation method Download PDFInfo
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- CN103141523A CN103141523A CN2013100480536A CN201310048053A CN103141523A CN 103141523 A CN103141523 A CN 103141523A CN 2013100480536 A CN2013100480536 A CN 2013100480536A CN 201310048053 A CN201310048053 A CN 201310048053A CN 103141523 A CN103141523 A CN 103141523A
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Abstract
The invention discloses an Acanthopanax gracilistylus insecticide and its preparation method. According to the method, the roots and bark of Acanthopanax gracilistylus are mixed and crushed, and after certain processing process, the Acanthopanax gracilistylus insecticide in the form of wettable powder, a microemulsion and the like can be obtained. With a good insecticidal effect, the insecticide developed and prepared by the invention is also safe to the environment, human, livestock, natural enemies of pests and other beneficial organisms, and pests do not have resistance to the insecticide. The insecticide has a simple preparation process and a low cost, thus being suitable for popularization and application.
Description
Technical field
The invention belongs to technical field of pesticide, be specifically related to agricultural chemicals preparation and manufacture field, particularly a kind of plant acanthopanax gracilistylus that utilizes is insecticide and the method thereof of raw material preparation.
Background technology
Compare with the traditional chemical agricultural chemicals, botanical pesticide has raw material to be easy to get, action site is many, pest is difficult for developing immunity to drugs, easily degraded, low-residual, to advantages such as natural enemy insect harm are less and environmentally safe.Filter out the high activity material from natural products, take it as template synthesizing new chemical pesticide, or directly it is developed to efficiently, low toxicity, low-residual, and the natural source pesticidal preparations of environment harmony, become that of novel pesticide initiative is important and one of effective approach is the developing direction of pesticide in future.
China soil is vast, and plant resources is abundant, and the condition of development plant insecticide is richly endowed by nature, and prospect is very wide.According to statistics, approximately there are more than 50 ten thousand kinds of plants in the whole world, nearly more than 30 ten thousand kinds of higher plant, and China existing higher plant 470 sections, more than 3700 belong to, and approximately 30,000 kinds, occupy the third place in the world." Chinese poisonous plant " lists China poisonous plant kind more than 1300 in, and wherein great majority have insecticidal activity, and numerous species is used as the botanical pesticide utilization.
Since the nineties in 20th century, China researcher has carried out more deep investigation to the plant resources that western part has insecticidal activity.Zhang Xing equals to complete in 1998 the screening operation of 475 Plants that gather from the Northwest, has found 128 kinds of activity plant preferably.Zhang Hongli etc. have 87 kinds to mythimna separata, food refusal preferably or toxic effect to be arranged to finding in the screening of the 204 Plants samples that pick up from Qinling Mountain Areas.Zhou Lijuan etc. filter out magnificent wild carraway (Sinacalia tangutica (Maxim.) B.Nord.) from more than 40 kind of endemic plant of China and Taiwania flousiana (Taiwania flousiana Gaussen) kind more than 10 has insecticidal activity preferably.Yao Yingjuan etc. filter out galangal (Alpinia officinarum), yellow ginger (Curcuma longa), cubeb litsen tree (Litsea cubeba), grass-leaved sweetflag (Acorus gramineus) and crotons (Croton tiglium) 5 Plants the corn weevil tool are are obviously walked quickly and kept away and action of contace poison from 21 Plants.Wherein, the research of pesticide plant China tree, Celastrus angulatus and Sabina vulgaris Ant etc. is more deep, and the insecticidal emulsifiable concentrate commercialization take China tree, melia toosendan etc. as principal component.
Acanthopanax gracilistylus (Acanthopanax gracilistylus W.W.Smith) is studies on plants of Acanthopanax Miq. in Araliaceae, has another name called slender acanthopanax (Sheng Nong's herbal classic), white le tree (popular name, Guangdong), five Ye Luci, white thorn point (popular name, Sichuan), five leaf wood (new Compendium of Materia Medica).Distribution Area is very wide, be distributed in Central-South, the southwest of China and Shanxi, Shaanxi, Henan, Hubei, Anhui, zhejiang and other places, be born in scrub forest, border, roadside, hillside and village, vertical distribution from the hundreds of rice of height above sea level to more than 1,000 meters, can reach in the western Sichuan of China and northwestern Yunnan Province and pull out several 3000 meters (Chinese Plants will editorial boards of the Chinese Academy of Sciences: " Chinese Plants will ", the 54th volume, Science Press, 1978, P.107-108).Its dry root skin is common Chinese medicine among the people " cortex acanthopanacis ".The medicinal material main product in Hubei, the ground such as Henan, Anhui, excavate root in summer, Qiu Erji, clean, strip the root skin, dry and make.Cortex acanthopanacis has wines used as antirheumatic on the traditional Chinese medical science, filling liver kidney, and the strengthening the bones and muscles function is used for Bi condition, and the muscles and bones impotence is soft, children's's retardation of walking, body void is weak, oedema, beriberi (Chinese Pharmacopoeia Commission: the Pharmacopoeia of the People's Republic of China, the 54th volume, Chemical Industry Press, 2005, P.44).
Acanthopanax gracilistylus mainly contains 4-methoxysalicylaldehyde (4-methoxysalicyl aldehyde), kaurenoic acid (kaurenoic acid), Syringin, the compositions such as Isofraxidin glycosides (isofraxedinoside) and tannin, its root skin contain kaurenoic acid (kaurenoic acid), ligustrin, Isofraxidin glucoside (isofraxedinoside), cupreol, palmitic acid, linoleic acid, vitamin B1 etc.As the common Chinese medicine material, China scientific research personnel mainly concentrates on medicinal active the research of acanthopanax gracilistylus.Dan Baoen etc. find in the research to the cortex acanthopanacis antitumor activity, its antitumor activity be the approximately simple protein composition of 64kDa of a kind of molecular weight; Hui Qiuchan etc. find compound 16-α-hydroxyl-19-dammara alkanoic acid, 16 α H in the acanthopanax gracilistylus stem, and 17-isovaleryloxy-ent-kauran-19-oic acid, dammara alkanoic acid glycosides A, Syringin, laricin all have in various degree inhibitory action to people's lung cancer A549 cell; The people such as Qian Shihui find to have the Acanthopanaxgenin acid and the Acankoreagenin that contain in the acanthopanax gracilistylus branches and leaves and anti-angiogenesis activity antitumor, use with chemotherapy drugs in combination to have synergy.
On agricultural active, the report such as Hu Junhua Cortex Acanthopancis extract is obvious to the bacteriostasis of citrus pathogens penicillium, Penicillium digitatum and Geotrichum candidum, the discovery cortex acanthopanacis such as Wang Gaoxue have certain killing action to the fish Dactylogyrus, but so far there are no to the insecticidal action research of its development system, do not form product and be applied to produce.
Summary of the invention
The object of the invention is to, take acanthopanax gracilistylus as primary raw material, provide high, nuisanceless, the cheap plant insecticide of a kind of insecticidal effect and manufacture method thereof.
In order to realize that above-mentioned task the present invention takes following technical solution:
A kind of acanthopanax gracilistylus insecticide is characterized in that, this acanthopanax gracilistylus insecticide that makes is take the acanthopanax gracilistylus extract as principal component and add auxiliary agent to process, and the preparation form is wetting powder and microemulsion; Wherein:
Described wetting powder is prepared by following raw materials by weight:
The acanthopanax gracilistylus extract: 20%~60%, filler: 30%~74%, surfactant: 1%~25%, the percentage summation of raw material is 100%;
Described microemulsion is prepared by following raw materials by weight:
The acanthopanax gracilistylus extract: 10%~30%, solvent 40%~84%, surfactant 1%~20%, the percentage summation of raw material is 100%.
Above-mentioned filler is that bentonite, imvite, common brick, clay, slag kaolin, diatomite, white carbon, sodium lignin sulfonate, calcium dodecyl benzene sulfonate, granular float stone, perlite, people's granulation load one or more the mixture in body, gangue, vermiculite;
Above-mentioned solvent is ethyl acetate, cyclohexanone, methyl oleate, ethanol, methyl alcohol, acetone, one or more mixtures in dimethyl formamide, normal propyl alcohol, isopropyl alcohol, ethyl acetate and water;
Above-mentioned surfactant is the mixture of one or more in the sub-?phosphate for alkyl benzene sulfonate, alkylphenol polyoxyethylene class, multi-styrene phenol APEO, ethoxylated dodecyl alcohol, polyoxyethylene nonylphenol ether, aliphatic alcohol polyethenoxy base ether, phenethyl phenol polyethenoxy ethers, phenethyl phenol polyethenoxy ether polyoxypropylene ethers, styrene acid APEO, this Pan's series, tween, agricultural the moon.
The manufacture method of above-mentioned acanthopanax gracilistylus insecticide is characterized in that, adopts following steps:
A. acanthopanax gracilistylus root skin is mixed, the meal that is crushed to 1~5mm with the plant tissue cracker minces;
B. the meal of steps A gained is minced and adopt the solvent method lixiviate, extracting temperature is 50~80 ℃, and extraction time is 6~12 hours, extract through Vacuum Concentration to being equivalent to 1kg dry powder/kg concentrate;
C. with the concentrate of step B gained, mix in the still that is mixed according to formula ratio and filler and surfactant, after namely get the acanthopanax gracilistylus wettable powder for disinsection.
D. with the concentrate of step B gained, in the still that is mixed, the still temperature that is mixed is 35-60 ℃ according to formula ratio and solvent and surfactant, and mixing time is 30 minutes, namely gets the acanthopanax gracilistylus pest killing micro emulsion after stirring.
The made acanthopanax gracilistylus insecticide of the present invention has the following advantages:
1. to lepidoptera pest, especially diamond-back moth, have very strong antifeedant activity, and insecticidal effect is high;
2. contained bioactive ingredients is complicated, and insect should not develop immunity to drugs to it;
3. to environment, people, animal, pest natural enemy and other beneficial organism safety;
4. after using, noresidue is poisoned;
Aboundresources, manufacture method simple, with low cost, be suitable for promoting the use of.
Embodiment
Acanthopanax gracilistylus insecticide of the present invention is take acanthopanax gracilistylus root skin as raw material, obtains the acanthopanax gracilistylus extract through traditional solvent method lixiviate, adds auxiliary agent at the acanthopanax gracilistylus extract, through certain process, makes acanthopanax gracilistylus wetting powder and microemulsion.
Wetting powder is prepared by following raw materials by weight: the acanthopanax gracilistylus extract: 20%~60%, and filler 30%~74%, surfactant 1%~25%, the summation of raw material is 100%;
Microemulsion: acanthopanax gracilistylus extract 10%~30%, solvent 40%~84%, surfactant 1%~20%, the summation of raw material is 100%.
Its manufacture method is:
The acquisition of A, acanthopanax gracilistylus extract:
Acanthopanax gracilistylus root skin is mixed, and the meal that is crushed to 1~5mm with the plant tissue cracker minces.The meal of gained is minced with conventional solvent method lixiviate, extraction solvent is any one or a few in ethanol, ethyl acetate, chloroform, benzinum, water, extracting temperature is 50~80 ℃, extraction time is 6~12 hours, extract to being equivalent to 1kg dry powder/kg concentrate, namely obtains the acanthopanax gracilistylus extract through Vacuum Concentration.
The preparation of B, acanthopanax gracilistylus insecticide
Acanthopanax gracilistylus extract and solvent or filler and surfactant are mixed with the pesticidal preparations such as microemulsion and wetting powder, are used for pest control.
In above-mentioned various formulation, the percentage by weight of each raw material is:
Formulation | Acanthopanax gracilistylus extract % | Filler or solvent % | Surfactant % |
Wetting powder | 20~60 | 30~74 | 1~25 |
Microemulsion | 10~30 | 40~84 | 1~20 |
In wetting powder preparation, filler used is that bentonite, imvite, common brick, clay, slag kaolin, diatomite, white carbon, sodium lignin sulfonate, calcium dodecyl benzene sulfonate, granular float stone, perlite, people's granulation load one or more the mixture in body, gangue, vermiculite;
Solvent for use is ethyl acetate, cyclohexanone, methyl oleate, ethanol, methyl alcohol, acetone, one or more mixtures in dimethyl formamide, normal propyl alcohol, isopropyl alcohol, ethyl acetate and water;
Surfactant used is the mixture of one or more in the sub-?phosphate for alkyl benzene sulfonate, alkylphenol polyoxyethylene class, multi-styrene phenol APEO, ethoxylated dodecyl alcohol, polyoxyethylene nonylphenol ether, aliphatic alcohol polyethenoxy base ether, phenethyl phenol polyethenoxy ethers, phenethyl phenol polyethenoxy ether polyoxypropylene ethers, styrene acid APEO, this Pan's series, tween, agricultural the moon.
Below the embodiment that the inventor provides:
The preparation of embodiment 1:55% acanthopanax gracilistylus wetting powder
Filler White Carbon black 30kg is added in cone-type mixer, by high pressure nozzle, 55kg acanthopanax gracilistylus extract (concentrate) is sprayed in blender, fully mix; Add dodecyl sodium sulfate 10kg, aliphatic alcohol polyethenoxy base ether 5kg fully mixes, and can make 55% acanthopanax gracilistylus wetting powder again.Dispersed in the water of preparation, dilution is stable, cold and hot storage stability meets the commercially available agricultural chemical preparation and must ask.
The preparation of embodiment 2:20% acanthopanax gracilistylus microemulsion
Take acanthopanax gracilistylus concentrate 20kg, be dissolved in 30kg ethyl acetate, then add the 15kg calcium dodecyl benzene sulfonate, the 5kg polyoxyethylene nonylphenol ether, mixed under high-speed stirred, be heated to 40 ℃ of left and right; Drip deionized water 30kg under high-speed stirred, control the rate of addition of water, make temperature remain on 40 ℃ of left and right; Water dropwises, and is warming up to 50 ℃, stirs 1 hour, makes 20% acanthopanax gracilistylus microemulsion 100kg.The stability of preparation, outward appearance etc. meet the requirement of commodity preparation.
Embodiment 3: the indoor biological activity determination of acanthopanax gracilistylus extract to diamond-back moth and mythimna separata 3 instar larvaes
This measuring the cytotoxicity of acanthopanax gracilistylus acetone extract to diamond-back moth and mythimna separata 3 instar larvaes, experimental technique and result of the test are as follows:
1, for the examination insect
Mythimna separata (Mythimna separata W.), diamond-back moth (Plutella xylostella L.) are indoor (T (25 ± 1) ℃, RH=75% ± 5%, D/L=12h/12h) raise population, provided by Nuisanceless Pesticide Research Service Center, Xibei Agroforestry Science and T, choose that Individual Size is consistent, 3 instar larvaes of bouncing are for examination.
2, test method
Cytotoxicity is measured and is adopted leaflet dish additive process.Fresh wild cabbage or maize leaf are cut into leaflet dish (maize leaves 1cm * 1cm, cabbage leaves 0.5cm * 0.5cm), be placed in the test plant extract and flood 2~3s, naturally after drying, put into culture dish (D=9cm) or plastic culture box (H=7.5cm, D=5cm) in, the examination worm of the hungry 4h of access.Every processing repeats 3 times, and 10 examination worms of every repetition are take acetone treatment as contrast.Check result after processing 48 and 72h, and the statistics lethality (death standard: the aphagia of examination worm, that touches is motionless).The lethality of mythimna separata and diamond-back moth is calculated with following formula.
3, result of the test
Adopt leaflet dish additive process, system measurement the cytotoxicity of acanthopanax gracilistylus acetone extract to mythimna separata and diamond-back moth 3 instar larvaes, added up the lethality of 48h and 72h, and tried to achieve the virulence curve, the results are shown in Table 1 and table 2.
Table 1: the cytotoxicity of acanthopanax gracilistylus extract to mythimna separata and diamond-back moth 3 instar larvaes
Table 2: the acanthopanax gracilistylus extract is to diamond-back moth and mythimna separata 3 instar larvae toxicity test results
By table 2 data as can be known, Cortex Acanthopancis extract will be significantly higher than it to the cytotoxicity of mythimna separata to the cytotoxicity of diamond-back moth.
The field control effect of 4: two kinds of acanthopanax gracilistylus preparation diamond-back moths of embodiment
1, reagent agent
55% acanthopanax gracilistylus wetting powder, the 20% acanthopanax gracilistylus microemulsion of preparation embodiment preparation, Nuisanceless Pesticide Research Service Center, Xibei Agroforestry Science and T provides.
20% fenvalerate missible oil, commercially available.
2, for studying thing
Wild cabbage.
3, controlling object
Diamond-back moth (Plutella xylostella L.).
4, experimental scheme and method
Small plot experiment is randomized arrangement, repeats residential quarter area depending on actual conditions 3 times.Carry out the blade face conventional spray with reagent agent 500,750,1000 times of liquid measures, 1000 times of liquid of common insecticide carry out the blade face conventional spray for the contrast medicament, and establish the clear water contrast.Adopt the investigation method of deciding strain, every residential quarter investigation 4~6 points, every some investigation 10 strains.Investigation insect population radix before every medicine, 3,7,14 days investigation insect population quantity after medicine.Calculate insect population decline rate and preventive effect, computing formula is as follows:
Data are processed and are adopted SPSS17.0 software, calculate control efficiency, and analyze the significance of difference between respectively processing.
5, experimental result and statistics
Measure 55% acanthopanax gracilistylus wetting powder and 20% acanthopanax gracilistylus microemulsion to the control efficiency of diamond-back moth, the results are shown in Table 3.
The preventive effect of two kinds of acanthopanax gracilistylus preparations of table 3 to diamond-back moth
Annotate: in table, data are the mean value of 3 repetitions; In " preventive effect " hurdle, refer to be remarkable difference on α=0.05 level with different letters after the ordered series of numbers mark.
As known from Table 5, acanthopanax gracilistylus wetting powder and microemulsion are to the better control efficiency of the equal tool of diamond-back moth, and between different preparations, preventive effect difference is not obvious, and effect is best in 500 times of situations of dilution.But after dispenser 7 days, the preventive effect statistical analysis difference of 500 times of medicament dilutions and 750 times is not remarkable, considers practical application, and when diluting 750 times, less expensive is effective.
Claims (3)
1. an acanthopanax gracilistylus insecticide, is characterized in that, this acanthopanax gracilistylus insecticide that makes is take the acanthopanax gracilistylus extract as principal component and add auxiliary agent to process, and the preparation form is wetting powder and microemulsion; Wherein:
Described wetting powder is prepared by following raw materials by weight:
The acanthopanax gracilistylus extract: 20%~60%, filler: 30%~74%, surfactant: 1%~25%, the percentage summation of raw material is 100%;
Described microemulsion is prepared by following raw materials by weight:
The acanthopanax gracilistylus extract: 10%~30%, solvent 40%~84%, surfactant 1%~20%, the percentage summation of raw material is 100%.
2. acanthopanax gracilistylus insecticide as claimed in claim 1 is characterized in that:
Described filler is that bentonite, imvite, common brick, clay, slag kaolin, diatomite, white carbon, sodium lignin sulfonate, calcium dodecyl benzene sulfonate, granular float stone, perlite, people's granulation load one or more the mixture in body, gangue, vermiculite;
Described solvent is ethyl acetate, cyclohexanone, methyl oleate, ethanol, methyl alcohol, acetone, one or more mixtures in dimethyl formamide, normal propyl alcohol, isopropyl alcohol, ethyl acetate and water;
Described surfactant is the mixture of one or more in the sub-?phosphate for alkyl benzene sulfonate, alkylphenol polyoxyethylene class, multi-styrene phenol APEO, polyoxyethylene nonylphenol ether, aliphatic alcohol polyethenoxy base ether, ethoxylated dodecyl alcohol, phenethyl phenol polyethenoxy ethers, phenethyl phenol polyethenoxy ether polyoxypropylene ethers, styrene acid APEO, this Pan's series, tween, agricultural the moon.
3. the manufacture method of the described acanthopanax gracilistylus insecticide of claim 1 or 2, is characterized in that, adopts following steps:
A. acanthopanax gracilistylus root skin is mixed, the meal that is crushed to 1~5mm with the plant tissue cracker minces;
B. the meal of steps A gained is minced and adopt the solvent method lixiviate, extraction solvent is any one or a few in ethanol, ethyl acetate, chloroform, benzinum, water, extracting temperature is 50~80 ℃, extraction time is 6~12 hours, extract through Vacuum Concentration to being equivalent to 1kg dry powder/kg concentrate;
C. with the concentrate of step B gained, mix in the still that is mixed according to formula ratio and filler and surfactant, after namely get the acanthopanax gracilistylus wettable powder for disinsection.
E. with the concentrate of step B gained, in the still that is mixed, the still temperature that is mixed is 35-60 ℃ according to formula ratio and solvent and surfactant, and mixing time is 30 minutes, namely gets the acanthopanax gracilistylus pest killing micro emulsion after stirring.
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Cited By (1)
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Application publication date: 20130612 |