CN107660535A - Composition pesticide and its application - Google Patents
Composition pesticide and its application Download PDFInfo
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- CN107660535A CN107660535A CN201610604589.5A CN201610604589A CN107660535A CN 107660535 A CN107660535 A CN 107660535A CN 201610604589 A CN201610604589 A CN 201610604589A CN 107660535 A CN107660535 A CN 107660535A
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- giant knotweed
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N31/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic oxygen or sulfur compounds
- A01N31/08—Oxygen or sulfur directly attached to an aromatic ring system
- A01N31/16—Oxygen or sulfur directly attached to an aromatic ring system with two or more oxygen or sulfur atoms directly attached to the same aromatic ring system
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
- C07C37/685—Processes comprising at least two steps in series
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P7/00—Preparation of oxygen-containing organic compounds
- C12P7/02—Preparation of oxygen-containing organic compounds containing a hydroxy group
- C12P7/22—Preparation of oxygen-containing organic compounds containing a hydroxy group aromatic
Abstract
The invention discloses a kind of composition pesticide and its application, it is related to technical field of pesticide combination.The composition derives from polygonaceae giant knotweed, and the extraction process step of the composition includes：1) extract：Giant knotweed rhizome is crushed to certain particle size, giant knotweed is extracted using Extraction solvent to obtain giant knotweed crude extract；2) handle：By giant knotweed crude extract sour water solution, enzymolysis or the microbial fermentation conversion processing in step 1)；3) separate：Treated giant knotweed crude extract in step 2) is subjected to being partially or wholly separated for resveratrol, the solvent in the residue after separation is partially or completely removed, produces the composition pesticide.The present inventor has found by research, the composition that carbohydrate ligands are converted into the composition that non-carbohydrate ligands obtain by the conversion of sour water solution, enzymolysis or microbial fermentation becomes simple, the stability of each component in composition has been ensured, has improved the utilization rate of Gentrin Knotweed P.E.
Description
Technical field
The present invention relates to a kind of composition pesticide and its application, and it is white by extraction, processing, separation to particularly relate to a kind of giant knotweed
A kind of composition pesticide obtained after veratryl alcohol and its application, belong to technical field of pesticide.
Background technology
As the whole world responds and recognized jointly as countries in the world to resource and the extensive concern of environment, the strategy of sustainable development
Same theme, " organic agriculture ", " pollution-free food " have turned into the direction of agricultural development, and find and develop efficient, less toxic, low-residual
Harmonious biogenic pesticide has progressively turned into the new direction of pesticide research with environment.Currently with the plant of natural secondary metabolite
The development and application of material resource agricultural chemicals are to formulate the important directions and study hotspot of biological pesticide.And extraction in actual production often be present
The problems such as source resource is limited, active effect is unstable.
The rhizome of polygonaceae plant giant knotweed, its main component are Anthraquinones (such as rheum emodin), stilbene compound (such as white black false hellebore
Alcohol), flavone compound, free amino acid, phenolic substance, polysaccharide etc..Natural anthraquinone compound in Gentrin Knotweed P.E can
For the preventing and treating of plant disease, Chinese patent application 201080044771.0 discloses a kind of preparation containing anthraquinone derivative, in
State's patent application 201010103826.2 discloses a kind of composition and its application for being used to prevent and treat the viroses of plant.It is described above
Composition obtain mode be usually：Giant knotweed rhizome is used finite concentration and the organic solvent of ratio in mechanical agitation and added after crushing
Obtained under heat backflow or immersion ultrasound condition.The composition components that this method obtains are complicated, including such as Rhein, rheum emodin,
Chrysophanol, aloe-emodin, resveratrol, Physcion, rheum emodin part sugar, Physcion part sugar, Chrysophanol are matched somebody with somebody
Body sugar, polydatin, tannin and a variety of polysaccharide etc..
But the composition that Gentrin Knotweed P.E is used for controlling plant diseases still at present, there is into more room for promotion, its drug effect
Ability still needs to improve.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of component is relatively easy, drug effect is controllable, and bactericidal effect is good to kill
Bacteria composition and its application.
In order to solve the above technical problems, present invention offer technical scheme is as follows：
A kind of composition pesticide of the present invention, the composition derive from polygonaceae giant knotweed, the preparation technology of the composition
Step includes：
1) extract：Giant knotweed rhizome is crushed to certain particle size, giant knotweed is extracted using Extraction solvent to obtain obtaining giant knotweed
Crude extract；
2) handle：By giant knotweed crude extract sour water solution, enzymolysis or the microbial fermentation conversion processing in step 1)；
3) separate：Giant knotweed crude extract in step 2) is subjected to being partially or wholly separated for resveratrol, after separation
Solvent in residue is partially or completely removed, and produces the composition pesticide.
The present invention is that the active ingredient in giant knotweed is extracted by using water or organic solvent, active ingredient therein
Including materials such as Physcion, rheum emodin, resveratrols, extracting method can use extracting method commonly used in the prior art；
On the other hand, the present invention is handled by the methods of sour water solution, enzymolysis, microbial fermentation, and the carbohydrate ligands in giant knotweed are converted
Resveratrol is converted into for non-carbohydrate ligands, such as polydatin, the component of giant knotweed crude extract is become relatively easy, it is of the invention
Processing method, including sour water solution, enzymolysis, microbial fermentation etc. can be handled using maturation process of the prior art；Furthermore
The method for being used to separate resveratrol in the present invention can be using the maturation process of prior art.
In the preparation technology of above-mentioned composition, giant knotweed can be crushed to 5~200 mesh, for acid-hydrolyzed sour addition,
Addition for the enzyme of enzymolysis can with the standard empirical of those skilled in the art according to the activity etc. of the hydrolysis properties of acid, enzyme
To know, culture and fermentation condition for the microorganism of microbial fermentation also need the characteristic according to microorganism with art technology
The standard empirical of personnel can be known.
Composition of the present invention derives from polygonaceae plant giant knotweed, and used extracting mode is：Giant knotweed rhizome is crushed
To after certain particle size, microbial fermentation or acid, enzyme hydrolysis are first passed through, carbohydrate ligands in giant knotweed are converted into non-carbohydrate ligands, then use
Conventional Extraction solvent is extracted, and improves the utilization ratio of Gentrin Knotweed P.E, then for this extract, will wherein have height
The resveratrol of economic value and medical value is partially or wholly separated, the composition obtained after separation, is the present invention
The composition.The composition can use in liquid form, further can also exist in solid form, the composition
In material mainly in the form of its non-carbohydrate ligands exist, there is higher bioactivity applied to control of plant disease.
In the processing step：It is hydrochloric acid for acid-hydrolyzed acid, sulfuric acid, phosphoric acid, nitric acid, carbonic acid, hypochlorous acid, high chlorine
Acid, citric acid, the one or more of acetic acid；Enzyme for enzymolysis is cellulase, plant extraction complex enzymes, amylase, pectin
Enzyme, beta-glucosidase it is one kind of multiple；Bacterium for microbial fermentation conversion is saccharomycete, aspergillus niger, the one of endogenetic fungus
Kind is a variety of.
Further, the solvent for extracting giant knotweed crude extract is the one or two of water or organic solvent, described organic
Solvent is the one of alcohols solvent, ketones solvent, esters solvent, chloroform, carbon tetrachloride and C5~C20 straight or branched varsols
Kind is a variety of.
Further, the alcohols solvent be it is a kind of in methanol, ethanol, isobutanol, n-butanol, n-hexyl alcohol, n-octyl alcohol or
It is a variety of；The ketones solvent is acetone；；The esters solvent is ethyl acetate, butyl acetate；C5~C20 straight chains or branch
Catenanes solvent is that benzene, n-hexane or petroleum ether are one or more.
Preferably, the processing mode of the separation resveratrol is pH regulations, soda acid processing, column chromatography, macroreticular resin
The one or more therein such as absorption, extraction, UF membrane, recrystallization.
Pesticidal preparations auxiliary element can also be contained in the bactericidal composition of the present invention, the content of the composition pesticide is
0.01%~90%, the formulation for being adapted to agriculturally use can be made, the formulation of the bactericidal composition is suspending agent, dry suspension
Agent, oil-suspending agent, water dispersible granules, wettable powder or suspension seed-coating agent.
The bactericidal composition of the present invention can be prepared into any one formulation of suitable agricultural use with known method, than
Preferable formulation is dry suspending agent (DF), oil-suspending agent, aqueous emulsion, microemulsion, wettable powder (WP), water dispersible granules
(WDG), suspending agent (SC), seed treatment or suspension seed-coating agent etc..
A wettable powders (WP), be can be dispersed in water solid powder preparation.Wettable powder of the present invention except
Into active compound plus such as outside white carbon, precipitated calcium carbonate, clay, diatomite, attapulgite diluent or inert substance, also from
Subtype or nonionic surface active agent (wetting agent, dispersant), wetting agent is for example, alkylbenzenesulfonate (DBS-Na), alkyl
Naphthalene sulfonate (pull open powder), alkylphenol-polyethenoxy base ether sulfate, alkylphenol-polyethenoxy base ether formaldehyde condensation products sulfate,
Aliphatic alcohol sulfate, fatty alcohol ethylene oxide adduct sulfonate, alkyl amide taurate, aliphatic alcohol polyethenoxy base ether
(JFC), content 0.1~30%；Dispersant such as naphthalene sulfonate, naphthalene or alkyl naphthalene formaldehyde condensate sulfonates (NO, NN0, MF), wood
Quality and its derivative sulfonate (M-9, POLYFON etc.), polyoxyethylene poly-oxygen propylene aether block copolymer, alkyl phenol polyoxy second
Alkene ether formaldehyde condensation products sulfate (SOPA), PVA, CMC content 0.1~30%；Also containing penetrating agent JFC, azone, thiophene ketone,
One or more materials among penetrant t, content 0.3~30%；Stabilizer, foam inhibitor, anticaking agent etc. can also be contained
Other auxiliary agents.
B water dispersible granules (WDG), be can be comparatively fast disintegrated in water, the scattered granule for forming higher suspension dispersion.By
The key element such as the auxiliary agent such as active component, wetting agent, dispersant, interleaving agent, disintegrant, stabilizer, adhesive and carrier forms.It is helped
Agent and carrier, and the compound method of precursor (preformed objects before granulation) are analogous to wettable powder and suspending agent substantially.
C suspending agents (SC), it is the not dispersion of water soluble solid agricultural chemicals or immiscible liquids agricultural chemicals in water or oil.By activity
Composition, auxiliary agent (wetting dispersing agent, thickener, stabilizer, pH adjusting agent, defoamer, antifreezing agent) are made through soybean dietary fiber.
Wetting dispersing agent can be naphthalene or alkyl naphthalene formaldehyde condensate sulfonates (NO, NN0, MF), lignin and its derivative sulfonate
(M-9, POLYFON etc.), alkylphenol-polyethenoxy base ether sulfonate, polyoxyethylene polyoxypropylene base ether block copolymers, alkyl
Phenol polyethenoxy base phosphate, carboxymethyl cellulose (CMC), polyvinylpyrrolidone (PVP), polyethylene glycol (PEG), condensation phosphorus
One or more in hydrochlorate etc., content 0.1~12%；Thickener and stabilizer can be xanthan gum (XG), polyvinyl alcohol
(PVA), the one or more in Magnesiumaluminumsilicate etc., content 0.05~0.5%；PH adjusting agent and defoamer optionally can add in right amount
Add.
D dry suspending agents (Dry Flowable, abbreviation DF), it is that can be comparatively fast disintegrated in water, scattered form higher suspension and disperse
The granule of system.Preparation method：The preparation obtained by the dehydration of suspending agent.Its auxiliary agent and carrier, and precursor (dehydrate
Preceding preformed objects) compound method it is consistent with suspending agent.
Bactericidal composition of the present invention is applied to prepare the pesticidal preparations of controlling plant diseases.Particularly useful for making
Prevent and treat powdery mildew, downy mildew, gray mold, early blight, scab, rust, spot defoliation, rot, rice blast, ring spot,
Droop, anthracnose, sclerotiniose etc.；Bacterial disease bacterial angular leaf spot, canker, bacterial wilt, bacterial stripe etc.；Disease
Application in the virus disease such as pesticidal preparations of tobacco mosaic virus disease, tomato virus disease.
The beneficial effects of the present invention are：
(1) the present inventor has found by research, is converted by sour water solution, enzymolysis or microbial fermentation by carbohydrate ligands
The composition for being converted into the composition that non-carbohydrate ligands obtain becomes simple, while by the white black false hellebore with economic value and medical value
Alcohol extracting is taken out, and makes the certain stability contorting of the realizations such as ratio, the purity of extraction components, has ensured the steady of each component in composition
It is qualitative, the utilization rate of Gentrin Knotweed P.E is improved, and finally obtain composition bactericidal effect and become more preferable；
(2) composition of the polygonaceae plant giant knotweed after handling, extracting separation resveratrol is used to prevent plant disease, its
Component derives from natural plants, degradable in nature, pollution-free, to people and livestock safety, has less toxic, low-residual
Feature, meet the developing direction of modern biotechnology agricultural chemicals, to developing green agriculture, promoting the sustainable development of agricultural production has weight
Economy, society and the environmental benefit wanted；
(3) Pesticide use that the composition is used in agricultural production, improves the resource utilization of giant knotweed, reduces life
Cost is produced, realizes making full use of for resource.
Embodiment
To make the technical problem to be solved in the present invention, technical scheme and advantage clearer, specific embodiment will be used below
It is described in detail, but the present invention is limited to absolutely not these examples.As described below is only the preferable embodiment of the present invention, only to
The present invention is explained, therefore can not be interpreted as the limitation to the scope of the claims of the present invention.It is it should be pointed out that all the present invention's
All any modification, equivalent and improvement done within spirit and principle etc., should be included in the scope of the protection.
Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Embodiment 1:
(1) crush：Giant knotweed raw material is crushed to 8-10 mesh, it is standby；
(2) extract：By solid-to-liquid ratio 5:Refluxing extraction 3 times at 80 DEG C of the ethanol solution of 1 addition 70%, first 1.5 hours twice,
1 hour for the third time, merge extract solution and be concentrated under reduced pressure, reclaim ethanol in extract solution, obtain Gentrin Knotweed P.E concentrate；
(3) digest：Gentrin Knotweed P.E concentrate is sent into fermentation tank, with hydrolyzing fermented by biological enzyme 4 days under the conditions of warm water,
In the fermentation step, the addition for hydrolyzing biology enzyme is 0.5%, and the temperature control of fermentation process is at 35 DEG C；
(4) it will be extracted three times with the ethyl acetate of 3 times of amounts by the Gentrin Knotweed P.E of enzymolysis, collect extract and raffinate
Liquid；
(5) once concentrate：Acetic acid ethyl acetate extract is concentrated under reduced pressure and filtered under the conditions of 70 DEG C, reclaims ethyl acetate,
Obtain medicinal extract；
(6) secondary concentration：The methanol of addition 60% is dissolved in the medicinal extract after once concentrating, then is filtered, and is received
Collect much filtrate, take filtrate to be concentrated, reclaim the methanol in filtrate, must be precipitated, precipitated through drying by plate-frame filtering after standing
Crush to obtain resveratrol finished product, content 92.4%；
(7) after the plate-frame filtering, resveratrol is realized and is kept completely separate substantially, and obtained filtrate is carried out under the conditions of 60 DEG C
Concentration, merge 4) in raffinate and 6) in much filtrate through drying, crush after giant knotweed extraction composition finished product, (wherein white black false hellebore
1.07%) alcohol residual content is.
Embodiment 2:
(1) crush：Giant knotweed raw material is crushed to 8-10 mesh, it is standby；
(2) extract：By solid-to-liquid ratio 5:Refluxing extraction 3 times at 80 DEG C of the ethanol solution of 1 addition 70%, first 1.5 hours twice,
1 hour for the third time, merge extract solution and be concentrated under reduced pressure, reclaim ethanol in extract solution, obtain Gentrin Knotweed P.E concentrate；
(3) acidolysis：Gentrin Knotweed P.E concentrate is sent into hydrolytic decomposition pot, watery hydrochloric acid catalytic reaction 6h is added, in the acidolysis
In step, sour addition is 1.5%, and the temperature control of acidolysis is 60 DEG C；
(4) Gentrin Knotweed P.E Jing Guo acidolysis is extracted three times with the ethyl acetate of 3 times of amounts, collects extract and raffinate
Liquid；
(5) once concentrate：Acetic acid ethyl acetate extract is concentrated under reduced pressure and filtered under the conditions of 70 DEG C, reclaims ethyl acetate,
Obtain medicinal extract；
(6) secondary concentration：The methanol of addition 60% is dissolved in the medicinal extract after once concentrating, then is filtered, and is received
Collect much filtrate, take filtrate to be concentrated, reclaim the methanol in filtrate, must be precipitated, precipitated through drying by plate-frame filtering after standing
Crush to obtain resveratrol finished product, content 88.3%；
(7) after the plate-frame filtering, resveratrol is realized and is kept completely separate substantially, and obtained filtrate is carried out under the conditions of 60 DEG C
Concentration, merge 4) in raffinate and 6) in much filtrate through drying, crush after giant knotweed extraction composition finished product, (wherein white black false hellebore
1.32%) alcohol residual content is
Embodiment 3:
(1) crush：Giant knotweed raw material is crushed to 8-10 mesh, it is standby；
(2) extraction extraction three times, 0.5 hour every time, obtains extract solution under the conditions of adding 55 DEG C of the ethyl acetate of 3 times of amounts；
(3) extract solution is concentrated under reduced pressure recycling design, adds the water of 2 times of amounts, add the aspergillus niger 1% that cell age is 40h,
40 DEG C ferment 48 hours, obtain zymotic fluid；
(4) dichloromethane of 6 times of amounts of Gentrin Knotweed P.E raw material weight after fermentation of Aspergillus niger is extracted and stirred
10h, temperature are 30 DEG C；
(5) filter, concentrate：Extract solution is filtered, is concentrated and dried to obtain crude extract solid, then with the dissolving of saturation isobutanol and mistake
Filter, obtains filtrate；
(6) by 5) gained filtrate adsorbed with polyamide, collect efflux after the completion of absorption, then with 70% methanol
Polymeric adsorbent is eluted, collects eluent, eluent is concentrated to be drying to obtain resveratrol crude product, content 75.9%；
(7) by 6) in the concentrated drying of efflux and with 5) in filter cake obtain giant knotweed extraction composition finished product through drying and crushing
(wherein resveratrol residual content is 1.8%).
Embodiment 4:
(1) giant knotweed will be dried and is crushed to 60-80 mesh；
(2) giant knotweed after crushing is extracted with the acetone of 8 times of amounts and stirs 10h, temperature is 40 DEG C, and extract solution is dense through depressurizing
Retract and receive acetone, obtain giant knotweed crude extract；
(3) water of 2 times of amounts, 0.2% cellulase and pectase (ratio 4 are added in giant knotweed crude extract:1) 40
DEG C stirring enzymolysis 5h obtain zymotic fluid；
(4) concentrate：Zymotic fluid is concentrated to give concentrate；
(5) extract and separate：By concentrate petroleum ether extraction untill petroleum ether layer is closely colourless, extract is collected, will
Extract is in 45 DEG C of distillation and concentrations to dry.Dry is dissolved in isometric ethyl acetate and water again, resveratrol is dissolved in second
Acetoacetic ester, fill post：A certain amount of silica gel is fitted into beaker to be placed in baking oven, after 105 DEG C activate 2h, taking-up is cooled to room temperature and refilled
Post.Pillar is grown using dry-packing to 15cm, slowly strikes to solid.Then petroleum ether-ethyl acetate (5 is used：5) elute, until
Untill having solution outflow.Chromatography：Acetic acid ethyl acetate extract is poured slowly into silicagel column, eluted with petroleum ether-ethyl acetate, is controlled
Flow velocity processed collects eluent in 1.0-2.0/min, equal portions method.Examine：Take 2-3 drop eluents to be put into clean surface plate, add
Enter 2-5 drop ammoniacal liquor, solution reddens, proved with the presence of RV.Dry：Eluent containing resveratrol is sent into rotation
(recovery organic solvent is for recycling) in evaporimeter, is evaporated under reduced pressure, obtains concentrate.Crystallization：Concentrate is put into refrigerator (-
15 DEG C), crystallized after standing 20-24h, obtain white crystal, it is vacuum dried, obtain RV product, content 91.7%.
(6) by 5) in raffinate and concentrated dry giant knotweed extraction composition finished product (the wherein resveratrol of efflux
0.58%) residual content is.
Embodiment 5:
(1) giant knotweed will be dried and is crushed to 60-80 mesh；
(2) dichloromethane of 6 times of the giant knotweed raw material weight amount after drying and crushing are extracted and stirs 8h and obtain giant knotweed and slightly carried
Thing, temperature are 30 DEG C；
(3) by giant knotweed crude extract concentration and recovery solvent, the water of 2 times of amounts is added, 1.5% acetum is in 60 DEG C of hydrolysis
10h obtains hydrolyzate；
(4) add at 50 DEG C of the saturation isobutanol of 3 times of amounts after stirring 6h and filter in acid hydrolysis liquid, obtain filtrate；
(5) by 4) gained filtrate adsorbed with polyamide, collect efflux after the completion of absorption, then with 70% methanol
Polymeric adsorbent is eluted, collects eluent, eluent is concentrated to be drying to obtain resveratrol crude product, content 62.7%；
(6) by 5) in the concentrated drying of efflux and with 4) in filter cake obtain giant knotweed extraction composition finished product through drying and crushing
(wherein resveratrol residual content is 1.74%).
The separating technology of resveratrol may be referred to maturation process of the prior art in above-described embodiment.
Comparative example 1：
(1) crush：Giant knotweed will be dried and be crushed to 60-80 mesh；
(2) extract：Raw material after crushing is extracted 3 times with 75% ethanol of 8 times of amounts of raw material weight, temperature is 75 DEG C；
(3) concentrate, filter：Extract solution is concentrated, filtered；
(4) by 3) adsorbed with DM-130 model resins, resin is cleaned to efflux to be colourless with deionized water, then
Eluted by several times with the ethanol solution of 10% ethanol, 20% ethanol, 40% ethanol, 60% ethanol, 100% various concentrations successively
Separation, 60% ethanolic moiety is concentrated under reduced pressure, and it is powdered to be sprayed to, and resveratrol weight content sum is 3.8%；
(5) ethanol eluate of 10% ethanol, 20% ethanol, 40% ethanol, 100% concentration is mixed, through being concentrated under reduced pressure
The concentrate of Gentrin Knotweed P.E is obtained, it is spray-dried to obtain Gentrin Knotweed P.E solid powder；
Comparative example 2：
(1) crush：Dry giant knotweed is crushed to 60-80 mesh；
(2) extract：The giant knotweed powder after crushing is taken to be extracted 3 times with 75% alcohol reflux, temperature is 75 DEG C；It is preceding to extract twice
Time is 2h, third time extraction time 1h；
(3) filtering and concentrating：By the extract solution filtering and concentrating of step (2), the concentrate of Gentrin Knotweed P.E, concentrate warp are obtained
It is spray-dried to obtain Gentrin Knotweed P.E solid powder；
Comparative example 3：
Commercially available Gentrin Knotweed P.E (Nanjing Ze Lang bio tech ltd, 25kg/ buckets).
The composition pesticide obtained by above-described embodiment, can be by adding conventional agriculturally acceptable carrier and helping
It is as follows that agent is prepared into agriculturally available formulation, section Example：
Embodiment 6：5% soluble concentrate
5 parts of 1 composition of Example by weight, is dissolved in 10 parts of propylene glycol monomethyl ethers, adds 8 castor oil polyoxyethylenes
Ether, 77 parts of water are well mixed and stirred, and produce 5% soluble concentrate.
Embodiment 7：5% aqua
5 parts of 2 composition of Example by weight, it is dissolved in 10 parts of ethanol, 5 parts of phenethyl phenol polyethenoxy ethers, 80 parts of water
It is well mixed and stirs, produces 5% aqua.
Embodiment 8：5% microemulsion
5 parts of 3 composition of Example by weight, 6 parts of 1-METHYLPYRROLIDONEs, 2 parts of cyclohexanone, 10 parts of methanol, 8 part ten
Dialkyl benzene sulfonate, 69 parts of water are mixed and stirred for uniformly, producing 5% microemulsion.
Embodiment 9：10% oil-suspending agent
10 parts of 4 composition of Example by weight, 6 parts of AEOs, 6 castor oil polyoxyethylene ethers, 2 parts
Organobentonite, 66 methyl oleates mixing, uniformly and stirs, is sanded and produces 10% oil-suspending agent.
Embodiment 10：20% aqueous suspension agent
20 parts of 5 composition of Example by weight, 3 parts of APES sulfonate, 3 parts of acrylic acid-acrylics
Sour hydroxypropyl ester copolymer, 0.2 part of xanthans, 0.5 part of sodium benzoate, 5 parts of ethylene glycol, 74.3 parts of water mixing, it is sanded and produces 20%
Aqueous suspension agent.
Embodiment 11：30% missible oil
30 parts of 1 composition of Example by weight, 8 parts of phenethyl phenol polyethenoxy ethers, 4 parts of DBSAs
Salt, 58 parts of dimethylbenzene, mixed dissolution simultaneously stir, and produce 30% missible oil.
Embodiment 12：70% water dispersible granules
70 parts of 3 composition of Example by weight, 5 parts of dodecane sulfonate formaldehyde condensations, 4 parts of alkylbenzoic acids
Sodium, 4 parts of property lignin, 17 parts of kaolin mix, again through air-flow crushing after mechanical crushing, through being granulated and drying after being well mixed
70% water dispersible granules.
Embodiment 13：85% wettable powder
85 parts of 5 composition of Example by weight, 4 parts of dodecylbenzoic sodium, 4 parts of APEO formaldehyde condensations
Thing, 7 parts of white carbon mixing, 85% wettable powder is obtained through mechanical crushing through air-flow crushing again.
Test example 1：Present composition Antifungal Activity in Vitro detects
Will be for examination target bacterium botrytis cinerea (Botrytis cinerea), cucumber cucumber anthracnose
(Colletotrichum orbiculare), Alternaria mali (Alternaria alternaria), rape sclerotium
Germ (Sclerotinia sclerotiorum), Phyllosticta musarum (Macrophoma musae), Pyricularia oryzae
18 kinds of pathogens such as (Magnaporthe grisea) are connected on PDA plate, are placed in preculture 5d in 25 ± 1 DEG C of incubators.
5% soluble concentrate that embodiment 1 to embodiment 5 and comparative example 1 are configured to the eligible compositions of comparative example 3, point
Preparation 4g also known as is taken, 200mL is settled to using sterilized water.Then PDA culture medium is dissolved, by decoction and PDA culture medium 1:9 is mixed
Close the band poison flat board for uniformly (v/v) being made that extension rate is 500 times.Then with a diameter of 5mm card punch close to bacterium colony side
Beaten on the same circumference of edge and take bacteria cake (ensureing that the cell age for examination germ of same repetition is identical), and with transfer needle in aseptic condition
It is lower by pure culture biscuits involvng inoculation to malicious culture medium flat plate center, mycelia is face-down, and sets not dosing flat board and compare, and is placed under dark and trains
Support, often processing is repeated 3 times measure.
When blank control bacteria cake grows to flat-plate bacterial colony edge, each concentration processing colony diameter is recorded, calculates medicament to target
Mark the inhibiting rate of bacterium.Bacteriostasis rate %=(blank colony diameter-processing bacterium colony is straight)/(blank colony diameter-bacteria cake diameter) ×
100。
As a result prove that embodiment 1-5 and the soluble concentrate of comparative example 1-3 eligible compositions 5% have necessarily to 18 kinds of target bacterium
Bacteriostatic activity, while composition activity described in embodiment 1-5 is substantially better than comparative example 1-3 compositions.Sterilization is obtained through glycolysis
Composition activity is much better than without composition bacteriostatic activity described in glycolysis.
The eligible compositions Antifungal Activity in Vitro of the present invention of table 1
The present inventor, which studies, to be found, the bacteriostatic activity of composition pesticide prepared by the present invention, the selection with formulation
There is no too big difference, by testing discovery repeatedly, composition pesticide of the invention is far longer than pair to the inhibitory activity of pathogen
The bacteriostatic activity of comparative compositions.
Test example 2:The present composition is to powdery mildew of cucumber pot experiment
Experiment is using People's Republic of China (PRC) agricultural industry criteria NY/T 1156.11-2008 preventing and treating cucurbits powdery mildew experiments
Method.It will be sowed after excellent No. 1 presoaking and germinating in cucumber susceptible variety Tianjin, 20-25 DEG C of greenhouse cultivation cucumber is unearthed standby to the 2-3 leaf phases
With.5% aqua that embodiment 1 to embodiment 5, comparative example 1, comparative example 2, the eligible compositions of comparative example 3 are configured to is configured to
Extension rate is standby for the decoction 200m of 500 times of liquid, is uniformly sprayed decoction in blade face to whole wettings using raw spray tower of surveying,
5 basins, 4 repetitions are often handled, and sets the processing for not containing effect composition containing only solvent and surfactant and makees blank control.Medicament
After processing 24 hours, with sprayer, even spraying is inoculated with cucumber powdery mildew's pathogen spore suspension on cucumber leaves.
The collocation method of spore suspension：With the pure water for adding a small amount of Tween 80, Powdery Mildew plant leaf blade will be covered with
On Fresh spores elute, filtered with double gauze, be made 1 × 105Individual spore/mL suspension.Often processing sprays
100ml spore suspensions, the cucumber plant after inoculation is placed under conditions of 20 DEG C -25 DEG C of temperature and cultivated.
When blank control disease leaf rate reaches more than 50%, incidence is managed in classification investigation everywhere, investigates every true leaf disease
Level index.Grade scale is：
0 grade：It is disease-free；
1 grade：Lesion area accounts for less than the 5% of full wafer leaf area；
3 grades：Lesion area accounts for the 5%-25% of full wafer leaf area；
5 grades：Lesion area accounts for below the 25%-50% of full wafer leaf area；
7 grades：Lesion area accounts for below the 50%-75% of full wafer leaf area；
9 grades：Lesion area accounts for more than the 75% of full wafer leaf area；
According to survey data result, the disease index and prevention effect of each processing are counted.
Each processing disease index and preventive effect are calculated by formula (1), formula (2), as a result retains 2 significant digits.
In formula：X --- disease index；
Ni --- the sick numbers of sheets at different levels；
I --- with respect to value of series；
N --- investigation total number of sheets.
In formula：
P --- prevention effect, unit are percentage (%)；
CK --- blank control disease index；
PT --- chemicals treatment disease index.
It is preferable to powdery mildew of cucumber active effect with composition described in embodiment 1 to embodiment 5 from result.
Composition active effect described in embodiment 1 to embodiment 5 is superior to described in comparative example 1, comparative example 2 and comparative example 3
Composition active effect.
2 eligible compositions of the present invention of table are to the potted plant active effect of powdery mildew of cucumber
Test example 3：The present composition is to powdery mildew of cucumber field control effectiveness test
Test medicine：The aqueous suspension agent of eligible compositions 20% of the present invention, comparison medicament：25% trazodone wettable powder.
Test site and kind：This experiment is located at Mianyang City Fucheng District Feng Gu towns Hui Longgou villages cucumber in solar-greenhouse Tanaka.
Experimental cultivar is excellent No. 1 of Tianjin, and cucumber is in harvesting initial stage during experiment, and powdery mildew of cucumber sporadicly starts to fall ill.
Experimental design and method：Experiment sets 20% composition aqueous suspension agent, 300 times of liquid, 500 times of liquid, 700 times of liquid totally three altogether
Individual concentration, using 25% triazolone, 1000 times of liquid as comparison medicament, separately set blank control.Random district's groups arrangement, is repeated 3 times, small
Area area 15m2, are routinely sprayed with knapsack sprayer in experiment and on May 6th, 2016, mu water consumption 60kg, and applied in the 1st time
7 days after medicine, i.e. heavy dressing on May 13 1 time.20 plants of the fixed point investigation per cell, the sick level index of every plant of blade of middle and upper part 10 is recorded,
And calculate prevention effect.
Powdery mildew of cucumber grading index is：
0 grade：It is disease-free；
1 grade：Lesion area accounts for less than the 5% of full wafer leaf area；
3 grades：Lesion area accounts for the 5%-25% of full wafer leaf area；
5 grades：Lesion area accounts for below the 25%-50% of full wafer leaf area；
7 grades：Lesion area accounts for below the 50%-75% of full wafer leaf area；
9 grades：Lesion area accounts for more than the 75% of full wafer leaf area；
Disease index (%)=[(the sick numbers of sheets at different levels × relative value of series)/(investigation total number of sheets × 9)] × 100
Prevention effect (%)=[1- (CK0Sick index × Pt1Sick index)/(CK1Sick index × Pt0Sick index)] × 100
There is result to understand that the present composition has excellent prevention effect to powdery mildew of cucumber, better than comparison medicament three
Oxazolone.Embodiment 3 and the eligible compositions active effect of embodiment 5 are substantially better than comparative example 1, comparative example 2 and comparative example 3 and obtain group
Compound active effect.Medicament is to cucumber growth safety, no poisoning, the preventing and treating available for field powdery mildew of cucumber.
The aqueous suspension agent of eligible compositions 20% of the present invention of table 3 is to powdery mildew of cucumber field efficacy
Test example 4：The present composition is to the potted plant test of pesticide effectiveness of tobacco virus
Test medicine：The oil-suspending agent of eligible compositions 10% of the present invention, comparison medicament：20% Moroxydine Hydrochloride (Jiangxi standing grain
Beneficial chemical industry).
Experimental design and method：Experiment sets 10% composition altogether 2000 times of liquid of suspending agent, 1500 times of liquid, 1000 times of liquid three
Individual dosage, using 20% Moroxydine Hydrochloride, 400 times of liquid as comparison medicament, separately set blank control.Use by above-mentioned 5 processing is dense
Spend and spraying treatment is carried out to the tobacco cultivated to the 3-4 leaf phases, often handle 20 plants, 4 repetitions.CMV poison source tobacco leaf is taken after 24h by cigarette
Leaf and distilled water mass ratio 1：40 ratio prepares CMV diseases juice (now with the current).The sick juice prepared is connect using friction
Kind method is inoculated on tobacco leaf.About 5~7 days after dispenser, respectively investigate dispenser and non-dispenser blade on withered spot number and
Chlorisis spot number, using the leaf of non-dispenser as control, suppression of the antivirotic to CMV is inoculated with after antivirotic and dispenser are applied after statistics inoculation
Effect processed.
In formula：
P --- prevention effect, unit are percentage (%)；
CK --- blank control withered spot mean number；
PT --- chemicals treatment withered spot mean number.
There is result to understand (table 4), the present composition has certain prevention effect to tobacco virus.Embodiment 1 and
The eligible compositions active effect of embodiment 2 is substantially better than comparative example 1, comparative example 2 and the eligible compositions active effect of comparative example 3.
Preventing and treating available for field cucumber tobacco virus.
The oil-suspending agent of 4 present composition of table 10% is to the potted plant prevention effect of tobacco virus
The present composition of test example 5 is to bacterial wilt of tomato prevention effect
Test medicine：The microemulsion of eligible compositions 5% of the present invention, comparison medicament：Streptomycin sulphate.
Experimental design and method：It will be stored in through Pathogenicity Strain of Pseudomonas Solanacearum (Ralstoniasolanacearum)
In closed sterile distilled water, room temperature storage is standby.After tomato seeds are sterilized, 2~3d of vernalization in 25 DEG C of incubators, broadcast after budding
Kind is in the vermiculite nutritive cube (10.0cm × 10.0cm) of sterilizing, 2 plants/alms bowl.It is standby during tomato seedling culture to 2~3 leaf phase.Will
The aqueous solution of 5% microemulsion of composition 400 and clear water (CK) carry out root irrigation, 20mL/ strains to tomato seedling, and each processing repeats 3
It is secondary.With root filling bacterium method inoculation Ralstonia solanacearum is hindered after 48h, bacteria suspension concentration is 108Cfu/mL, inoculum concentration are 5mL/ strains., will after inoculation
Tomato is placed in into 30 DEG C of greenhouses, moisturizing culture.21d records incidence after inoculation, calculates the incidence of disease and relative control effect.
The incidence of disease × 100 of relative control effect (%)=(incidence of disease of the incidence of disease-processing of control)/control
There is result to understand (table 5), the present composition has certain prevention effect to bacterial wilt of tomato.The institute of embodiment 4
Obtain composition active effect and be substantially better than comparative example 1, comparative example 2 and the eligible compositions active effect of comparative example 3.
The microemulsion of 5 present composition of table 50% is to bacterial wilt of tomato prevention effect
Note:Data above is the average value of 3 repetitions.
Above-mentioned test example only lists the disease-controlling effect of part composition pesticide of the present invention, invention of the invention
People is caused by testing discovery, composition pesticide of the invention repeatedly to a variety of pathogens (including the pathogen enumerated in table 1)
Disease be respectively provided with obvious prevention effect, and prevention effect is substantially better than the prevention effect of existing Gentrin Knotweed P.E.
Described above is the preferred embodiment of the present invention, it is noted that for those skilled in the art
For, on the premise of principle of the present invention is not departed from, some improvements and modifications can also be made, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (9)
1. a kind of composition pesticide, it is characterised in that the composition derives from polygonaceae giant knotweed, the preparation technology of the composition
Step includes：
1) extract：Giant knotweed rhizome is crushed to certain particle size, giant knotweed is extracted using Extraction solvent to obtain giant knotweed crude extract；
2) handle：By giant knotweed crude extract sour water solution, enzymolysis or the microbial fermentation conversion processing in step 1)；
3) separate：Treated giant knotweed crude extract in step 2) is subjected to being partially or wholly separated for resveratrol, to separation
The solvent in residue afterwards is partially or completely removed, and produces the composition pesticide.
2. composition pesticide according to claim 1, it is characterised in that in the processing step：For acid-hydrolyzed acid
For the one or more in hydrochloric acid, sulfuric acid, phosphoric acid, carbonic acid, hypochlorous acid, perchloric acid, nitric acid, citric acid, acetic acid；For enzymolysis
Enzyme is the one or more in cellulase, plant extraction complex enzymes, amylase, pectase, beta-glucosidase；For micro- life
The bacterium of thing microbe conversion is the one or more in saccharomycete, aspergillus niger, endogenetic fungus.
3. composition pesticide according to claim 1, it is characterised in that for extract the solvent of giant knotweed crude extract for water or
The one or two of organic solvent.
4. composition pesticide according to claim 3, it is characterised in that the organic solvent is alcohols solvent, ketone is molten
Agent, esters solvent, chloroform, the one or more of carbon tetrachloride and C5~C20 straight or branched varsols.
5. composition pesticide according to any one of claims 1 to 4, it is characterised in that the processing of the separation resveratrol
Mode is that direct concentration, pH regulations, soda acid processing, column chromatography, macroporous resin adsorption, extraction, UF membrane or recrystallization are therein
It is one or more.
6. composition pesticide according to any one of claims 1 to 5, it is characterised in that also contain in the bactericidal composition
Pesticidal preparations auxiliary element, the content of the composition pesticide is 0.01%~90%, so that the agent for being adapted to agriculturally use is made
Type.
7. composition pesticide according to claim 6, it is characterised in that the pesticidal preparations auxiliary element is agriculturally may be used
The carrier and auxiliary agent of receiving；The formulation of the bactericidal composition is soluble concentrate, aqua, aqueous suspension agent, dry suspending agent, oil suspension
In agent, wettable powder, water dispersible granules, missible oil, microemulsion, suspension seed-coating agent.
8. application of any described composition pesticide of claim 1 to 7 in the pesticidal preparations for preparing controlling plant diseases.
9. the application of composition pesticide according to claim 8, it is characterised in that prepare preventing and treating powdery mildew, downy mildew,
Gray mold, early blight, scab, rust, spot defoliation, rice blast, rot, ring spot, droop, anthracnose, sclerotium
Disease；Bacterial disease includes bacterial angular leaf spot, canker, bacterial wilt, bacterial stripe；Virus disease includes Tobacco mosaic
Virosis, tomato virus disease pesticidal preparations in application.
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| CN201610604589.5A CN107660535A (en) | 2016-07-27 | 2016-07-27 | Composition pesticide and its application |
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| CN201610604589.5A CN107660535A (en) | 2016-07-27 | 2016-07-27 | Composition pesticide and its application |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111763140A (en) * | 2020-07-07 | 2020-10-13 | 东明格鲁斯生物科技有限公司 | Method for extracting resveratrol from giant knotweed rhizome |
| CN113575621A (en) * | 2021-08-31 | 2021-11-02 | 王浦 | Botanical pesticide for preventing and treating cucumber mosaic virus and preparation method thereof |
| CN115176820A (en) * | 2022-07-08 | 2022-10-14 | 沈阳药科大学 | Polygonum cuspidatum silver ion disinfectant and preparation method and application thereof |
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| CN104341277A (en) * | 2014-11-18 | 2015-02-11 | 白心亮 | Method for extracting resveratrol from Polygonum cuspidatum |
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| CN104341277A (en) * | 2014-11-18 | 2015-02-11 | 白心亮 | Method for extracting resveratrol from Polygonum cuspidatum |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111763140A (en) * | 2020-07-07 | 2020-10-13 | 东明格鲁斯生物科技有限公司 | Method for extracting resveratrol from giant knotweed rhizome |
| CN111763140B (en) * | 2020-07-07 | 2022-08-26 | 东明格鲁斯生物科技有限公司 | Method for extracting resveratrol from giant knotweed rhizome |
| CN113575621A (en) * | 2021-08-31 | 2021-11-02 | 王浦 | Botanical pesticide for preventing and treating cucumber mosaic virus and preparation method thereof |
| CN113575621B (en) * | 2021-08-31 | 2022-03-22 | 王浦 | Botanical pesticide for preventing and treating cucumber mosaic virus and preparation method thereof |
| CN115176820A (en) * | 2022-07-08 | 2022-10-14 | 沈阳药科大学 | Polygonum cuspidatum silver ion disinfectant and preparation method and application thereof |
| CN115176820B (en) * | 2022-07-08 | 2023-10-24 | 沈阳药科大学 | Polygonum cuspidatum silver ion disinfectant, and preparation method and application thereof |
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Application publication date: 20180206 |