CN102265906B - Artemisia ordosica Kraschen bactericide and preparation method thereof - Google Patents
Artemisia ordosica Kraschen bactericide and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an Artemisia ordosica Kraschen bactericide, which is prepared by adding auxiliary agents into an Artemisia ordosica Kraschen extract serving as the main component. And the prepared bactericide takes the form of a micro-emulsion or an emulsion in water. The Artemisia ordosica Kraschen bactericide of the invention is safe to the environment. The active compounds in the Artemisia ordosica Kraschen bactericide are naturally existing substances coming from the nature, and form an immanent energy and substance circulating and metabolic path during the long-term evolution process, so application of the Artemisia ordosica Kraschen bactericide leaves no residue and results in little biological concentration. The bactericide is also relatively safe to nontarget organisms. Different from conventional pesticides in terms of the mechanism of action to plant pathogens, the Artemisia ordosica Kraschen bactericide is not easy to develop drug resistance in pathogens after application. Able to prevent and treat the downy mildew and botrytis of fruit trees, vegetables and flowers, the botanical bactericide provided in the invention boasts substantial application and promotion value in organic agricultural product production and is a novel pollution-free bactericide.
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 black sand sagebrush (Artemisia filifolia) of plant that utilizes is bactericide and the method thereof of raw material preparation.
Background technology
Black sand sagebrush (Artemisia filifolia) (
Artemisia ordosicaKrasch.), be the composite family sagebruss, be commonly called as oily wormwood artemisia.Black sand sagebrush (Artemisia filifolia) is undershrub, and plant height 50-80cm belongs to phreatophyte.Main root is thick and most, wooden, root-like stock is sturdy.The acrial part branch is intensive, softness is crawled, be convenient to sand, and holding concurrently again, vegetative period is long, sand-fixing effect is fine.
Black sand sagebrush (Artemisia filifolia) herb all can be used as medicine, and is usually used in scattered inflammatory swelling, the sharp gas of wide chest, desinsection and hemostasis, can treat the diseases such as rheumatic arthritis, parotitis, scabies redness, abdominal distension, intestinal obstruction, renal shutdown.
Its branches and leaves are capable of using as feed, achene edible, medicinal, industrial, and distribution is wide, quantity is large, has important resource value and environmental functional.Energy drought resisting anti-blown sand, weatherproof are one of the important herbage on desert area cold season grassland, also are good sand-fixation plants.Be distributed in the provinces and regions such as the Inner Mongol, Shaanxi, Ningxia, Gansu, Xinjiang.Be in Steppe and desert steppe band, also come across steppification desert band.Be born in mobile, half flow, semifixed to fixing sand ground, be one of the Main Constructive Species of sand ground vegetation and sociales.
The extraction that the at present research of black sand sagebrush (Artemisia filifolia) mainly concentrates on its chemical composition with separate, the black sand sagebrush (Artemisia filifolia) chemical composition of open report is take essential oil and flavonoids as main, flavonoids is with cerasine, isosakuranetin, eriodictyol-7-methyl ether, 5,7,2
＇, 4
＇-tetrahydroxy-6,5
＇-dimethoxy flavones etc. are main, and essential oil is then with fragrant magnolol, and trans-β-ocimene is main; Black sand sagebrush (Artemisia filifolia) plant extract microbic activity mainly contains analgesia and anti-inflammatory activity, hypoglycemic activity, anticonvulsant action, antitumor action, antioxidation activity, diuresis and Antiparasitic Activity etc., according to the data-searching that the applicant does, the black application of sand sagebrush (Artemisia filifolia) extract on agricultural chemicals there is not yet report.
Summary of the invention
The object of the invention is to, provide a kind of black sand sagebrush (Artemisia filifolia) of plant that utilizes for bactericide and the method thereof of raw material preparation, do not contain any chemical pesticide composition, to the people, animal low toxicity, pathogen is difficult for developing immunity to drugs after using.
For realizing above-mentioned task, the technical scheme that the present invention takes is:
A kind of black sand sagebrush (Artemisia filifolia) bactericide is characterized in that, make should black sand sagebrush (Artemisia filifolia) bactericide be main component and to add auxiliary agent formulated by black sand sagebrush (Artemisia filifolia) extract, the preparation form is microemulsion or aqueous emulsion, wherein:
Described microemulsion is prepared by following raw materials by weight:
Black sand sagebrush (Artemisia filifolia) extract: 10～30%, organic solvent: 0～20%, surfactant: 10～30%, antifreezing agent: 4～10%, surplus is water, the percentage by weight sum of raw material is 100%;
Described aqueous emulsion is prepared by following raw materials by weight:
Black sand sagebrush (Artemisia filifolia) extract: 10%～50%, organic solvent: 0～30%, surfactant: 5%～20%, antifreezing agent: 4%～10%, thickener: 0.2～1%; Surplus is water, and the percentage by weight sum of raw material is 100%.
Described black sand sagebrush (Artemisia filifolia) extract is that root, stem, leaf, the pollen of black sand sagebrush (Artemisia filifolia) is broken, and with extracting solvent extraction, extract obtains through concentrated.
Described organic solvent is one or more the mixture in ethyl acetate, cyclohexanone, ethanol, methyl alcohol, the dimethyl formamide;
Described surfactant is one or more mixture in the addition product, aralkyl phenol polyethenoxy ether formaldehyde condensation products of alkyl benzene sulfonate, alkylphenol polyoxyethylene class, phenethyl phenol polyethenoxy ethers, phenethyl phenol polyethenoxy ether polyoxypropylene ethers and similar substance, castor oil and oxirane;
Described antifreezing agent is ethylene glycol or propane diols;
Described thickener is one or more the mixture in polyvinyl alcohol, xanthans, sodium carboxymethylcellulose, the Magnesiumaluminumsilicate.
The preparation method of above-mentioned black sand sagebrush (Artemisia filifolia) bactericide is characterized in that, carries out according to the following steps:
A, the ordos wormwood root with drying, stem, leaf and pollen are broken, cross 40 mesh sieves;
B, with 3～4 times of ethyl acetate solvents to black sand sagebrush (Artemisia filifolia) crushed material quality, under refluxad extract, extract 60～70 ℃ of temperature, extract 8h;
C, with the method for Vacuum Concentration, will deceive the sand sagebrush (Artemisia filifolia) extract and be concentrated into deceiving the sand sagebrush (Artemisia filifolia) raw meal and mince and wait weight, must deceive the sand sagebrush (Artemisia filifolia) extract;
D, in reactor, will deceive sand sagebrush (Artemisia filifolia) extract, organic solvent, surfactant, antifreezing agent and water mixes according to the bactericidal microemulsion proportional quantity, in reactor, stir transparently, namely get microemulsion through quality inspection;
E. will deceive sand sagebrush (Artemisia filifolia) extract, organic solvent, surfactant, antifreezing agent, thickener and water according to proportional quantity and mix, emulsion dispersion under the effect of high-speed shearing machine through after the quality inspection, is namely made aqueous emulsion.
Black sand sagebrush (Artemisia filifolia) bactericide of the present invention is a kind of novel bactericide, and tomato in plastic greenhouse gray mold and cucumber downy mildew are had preferably control efficiency, is desirable nuisanceless bactericide.
Advantage of the present invention is as follows:
1, black sand sagebrush (Artemisia filifolia) is natural active matter, derives from nature, has formed intrinsic energy and material recycle metabolic pathway in long-term evolutionary process, so use rear noresidue, can not cause biological concentration; Easily degraded in environment is to mammal low toxicities such as people and animals, to pest natural enemy and other beneficial organism safety.
2, the formulation that adopts is mainly microemulsion, aqueous emulsion etc., without aromatic hydrocarbon solvents such as dimethylbenzene, greatly reduces environmental disruption, has reduced in the dispenser process murder by poisoning to operator.
3, photostability raising, lasting period suit, and can reduce dispenser frequency and cost accounting, and be conducive to further alleviate the pressure to environment.
4, the mechanism of action of phytopathogen is different from conventional pesticide, pathogen is difficult for developing immunity to drugs after using.Not only tomato in plastic greenhouse gray mold and cucumber downy mildew are had preferably control efficiency, also common germ has obvious control efficiency on the gourd, fruit and vegetable to outdoor cropping, has very big application and popularization value in organic farm products production.
Embodiment
The applicant is on the basis that various feverfew bactericidal activities are extensively screened; find the bactericidal activity of black sand sagebrush (Artemisia filifolia); its extract shows higher bacteriostatic activity to the various plants disease fungus; can prevent that under condition of living body pathogen to the infecting of crops, having good protective effect to crops.
For a more clear understanding of the present invention and the drug effect of medicament of the present invention, below the specific embodiment of finishing according to technical solution of the present invention that provides by the inventor the present invention is described in further detail, these only are preferably embodiment of the present invention, but are not limited to these embodiment.Need to prove, in following embodiment, organic solvent can be one or more the mixture in ethyl acetate, cyclohexanone, ethanol, methyl alcohol, the dimethyl formamide; Surfactant can be one or more mixture in the addition product, aralkyl phenol polyethenoxy ether formaldehyde condensation products of alkyl benzene sulfonate, alkylphenol polyoxyethylene class, phenethyl phenol polyethenoxy ethers, phenethyl phenol polyethenoxy ether polyoxypropylene ethers and similar substance, castor oil and oxirane; Antifreezing agent can be ethylene glycol or propane diols; Thickener can be one or more the mixture in polyvinyl alcohol, xanthans, sodium carboxymethylcellulose, the Magnesiumaluminumsilicate.
Embodiment 1: the preparation of black sand sagebrush (Artemisia filifolia) extract
Ordos wormwood root, stem, leaf and the pollen of drying is broken, cross 40 mesh sieves.Take by weighing the black sand sagebrush (Artemisia filifolia) crushed material of 100kg in the refluxing extraction still, add ethyl acetate 300kg, be heated to 76 ℃, extract 8h; Filter; Filtrate is concentrated into 100kg, namely gets black sand sagebrush (Artemisia filifolia) extract.
Embodiment 2: the preparation of black sand sagebrush (Artemisia filifolia) extract
Ordos wormwood root, stem, leaf and the pollen of drying is broken, cross 40 mesh sieves.Take by weighing the black sand sagebrush (Artemisia filifolia) crushed material of 100kg in the refluxing extraction still, add methyl alcohol 300kg, be heated to 76 ℃, extract 8h; Filter; Filtrate is concentrated into 100kg, namely gets black sand sagebrush (Artemisia filifolia) extract.
Embodiment 3: the preparation of black sand sagebrush (Artemisia filifolia) disinfectant aqueous emulsion
Take by weighing black sand sagebrush (Artemisia filifolia) extract 25kg, with methyl alcohol 5kg dissolving, under agitation add polyoxyethylene nonylphenol ether phosphate 20kg, stir, add deionized water 50kg, get final product to get the black sand sagebrush (Artemisia filifolia) aqueous emulsion of 100kg
Embodiment 4: the preparation of black sand sagebrush (Artemisia filifolia) bactericide microemulsion
Take by weighing black sand sagebrush (Artemisia filifolia) extract 25kg and 20kg polyoxyethylene nonylphenol ether phosphate, be dissolved in the 5kg methyl alcohol, above solution is heated to 40 ℃ in homogenizer, add deionized water 50kg under the high-speed stirred; Dropwise, stir 45min again, cooling namely gets black sand sagebrush (Artemisia filifolia) bactericidal microemulsion.
EXPERIMENTAL EXAMPLE 1: black sand sagebrush (Artemisia filifolia) extract is to the inhibition determination of activity of phytopathogen
This experiment has been measured black sand sagebrush (Artemisia filifolia) extract active to the inhibition of phytopathogen in vitro, and experimental technique and result of the test are as follows:
1.1 for the examination bacterial classification
Cucumber anthracnose, cucumber downy mildew, graw mold of tomato, early blight of tomato, tomato late blight provide by Nuisanceless Pesticide Research Service Center, Xibei Agroforestry Science and T.
1.2 test method
Above-mentioned black sand sagebrush (Artemisia filifolia) microemulsion is adopted the test of exsomatizing of mycelial growth rate method, according to formula calculating inhibiting rate:
Mycelial growth inhibition rate=
* 100%
1.3 result of the test
Measure black sand sagebrush (Artemisia filifolia) microemulsion to the virulence for the examination pathogen with growth rate method, thereby obtained its extract to the virulence for the examination pathogen, the results are shown in Table 1
Table 1: black sand sagebrush (Artemisia filifolia) active substance suppresses the virulence (72h) of mycelial growth
EXPERIMENTAL EXAMPLE 2: black sand sagebrush (Artemisia filifolia) microemulsion field control effectiveness test
2.1 reagent agent
Black sand sagebrush (Artemisia filifolia) aqueous emulsion, Nuisanceless Pesticide Research Service Center, Xibei Agroforestry Science and T provides.
70% aliette mancozeb wettable powder, commercially available.
2.2 for studying thing
Cucumber (
Cucumis sativus Linn.), kind is " grind No. four in Tianjin ".
2.3 controlling object
Cucumber downy mildew (
Pseudoperonospora cubensis).
2.4 the selection in test plot is processed with test
2.4.1 the selection in test plot
This test is located at booth vegetable base, village, Da Zhai, township, Yangling district of Shaanxi Province Yangchuan village to be carried out, spring stubble plastic tent cucumber ground, and cucumber continuous cropping 3 years, soil fertility is medium;
2.4.2 test is processed and Quarter Design
Reagent agent for black sand sagebrush (Artemisia filifolia) aqueous emulsion 100 *, 200 *, 400 *; Contrast medicament 70% aliette MnZn 500 * and blank (clear water) totally five kinds of processing.Every kind of processing area is 27m
2, process the interval randomized arrangement.
2.4.3 application method
By the mu amount of being watered 30kg, carry out foliar spray with the MATABI knapsack hand sprayer.For the first time dispenser on April 18th, 2011, for the second time dispenser on April 25.Temperature is on the low side in the duration of test booth, 28 ℃ of maximum temperatures, 17 ℃ of minimum temperatures.
2.4.4 investigation method
Every residential quarter is got 4 investigation at random, looks into two strains at every, and whole blades are investigated in every strain.Investigation state of an illness radix before the dispenser for the first time carried out efficacy survey in 7 days respectively after 7 days and for the second time dispenser after the dispenser first time, and according to following grade scale record fruit incidence;
Stage division (take blade as unit):
0 grade: without scab;
1 grade: lesion area accounts for below 5% of whole leaf area;
3 grades: lesion area accounts for the 6%-l0% of whole leaf area;
5 grades: lesion area accounts for the 11%-25% of whole leaf area;
7 grades: lesion area accounts for the 26%-50% of whole leaf area;
9 grades: lesion area accounts for more than 50% of whole leaf area.
2.4.5 drug effect computational methods
Drug effect is calculated by formula (1), formula (2):
Disease index=
(1)
Control efficiency (%)=
(2)
In the formula
Disease index before the district's dispenser of CK0-blank;
Disease index after the district's dispenser of CK1-blank;
Disease index before the district's dispenser of PT0-chemicals treatment;
Disease index after the district's dispenser of PT1-chemicals treatment.
2.5 results and analysis
Black sand sagebrush (Artemisia filifolia) aqueous emulsion control plastic tent cucumber downy mildew drug effect the results are shown in Table 2, investigation in 7 days after for the first time dispenser of black sand sagebrush (Artemisia filifolia) aqueous emulsion, black sand sagebrush (Artemisia filifolia) aqueous emulsion 100 *, 200 *, 400 * preventive effect be 62.00%-73.86%, contrast medicament 70% aliette MnZn 500 * preventive effect is 70.81%, three of black sand sagebrush (Artemisia filifolia) aqueous emulsions are processed preventive effect and all reached more than 60%, and are better than preventive effect with contrast medicament 70% aliette MnZn; For the second time the black sand sagebrush (Artemisia filifolia) aqueous emulsion 100 of investigation in 5 days after the dispenser *, 200 * preventive effect is higher than 80%, and is close with contrast medicament 70% aliette MnZn 500 * preventive effect.
Table 2: black sand sagebrush (Artemisia filifolia) aqueous emulsion is to the control efficiency of plastic tent cucumber downy mildew
EXPERIMENTAL EXAMPLE 3: black sand sagebrush (Artemisia filifolia) microemulsion field control effectiveness test
3.1 reagent agent
Black sand sagebrush (Artemisia filifolia) microemulsion: Nuisanceless Pesticide Research Service Center, Xibei Agroforestry Science and T provides.
Sukeling: 50% wetting powder, SUMITOMO CHEMICAL chemistry strain formula can product.
3.2 for studying thing and controlling object
For studying thing: tomato (Lycopersicum esculentum Mill).
Controlling object: graw mold of tomato.
3.3 the selection in test plot is processed with test
3.3.1 the selection in test plot
This test is located at booth vegetable base, village, Da Zhai, township, Yangling district of Shaanxi Province Yangchuan village to be carried out, spring stubble tomato in plastic greenhouse ground, and tomato continuous cropping 3 years, soil fertility is medium;
3.3.2 test is processed and Quarter Design
Reagent agent for black sand sagebrush (Artemisia filifolia) microemulsion 100 *, 200 *, 400 *; Contrast medicament Sukeling 1000 * and blank (clear water) totally five kinds of processing.Every kind of processing area is 27m
2, process the interval randomized arrangement.
3.3.3 application method
By the mu amount of being watered 30kg, carry out foliar spray with the MATABI knapsack hand sprayer.For the first time dispenser on February 17th, 2011, for the second time dispenser on February 22.Temperature is on the low side in the duration of test booth, 22 ℃ of maximum temperatures, 12 ℃ of minimum temperatures.Humidity is high in the canopy.
3.3.4 investigation method
5 samplings of every processing diagonal, every is selected 3 strains at random, totally 15 strains, every strain is selected 3 fruits at random from upper.Investigation state of an illness radix before the dispenser for the first time carried out efficacy survey in 5 days respectively after 5 days and for the second time dispenser after the dispenser first time, and according to following grade scale record fruit incidence;
The killed stage division of tamato fruit (take fruit as unit):
0 grade: without scab;
1 grade: residual petal morbidity or column cap morbidity;
3 grades: overstate that sheet rots or the column cap morbidity spreads to areola section;
5 grades: there is the spot of infiltration in areola section without mould layer;
7 grades: there is mould layer in areola section but does not expand to other positions;
9 grades: mould layer expands to other positions of fruit.
3.3.5 drug effect computational methods
Drug effect is calculated by formula (1), formula (2):
Disease index=
(1)
Control efficiency (%)=
(2)
In the formula:
Disease index before the district's dispenser of CK0-blank;
Disease index after the district's dispenser of CK1-blank;
Disease index before the district's dispenser of PT0-chemicals treatment;
Disease index after the district's dispenser of PT1-chemicals treatment.
3.4 results and analysis
Black sand sagebrush (Artemisia filifolia) microemulsion is prevented and treated tomato in plastic greenhouse gray mold drug effect and be the results are shown in Table 3, investigation in 7 days after for the first time dispenser of black sand sagebrush (Artemisia filifolia) microemulsion, black sand sagebrush (Artemisia filifolia) microemulsion 100 *, 200 *, 400 * preventive effect be 51.12%-69.47%, contrast medicament Sukeling 1000 * preventive effect is 66.86%, and is better than preventive effect with contrast medicament aliette MnZn; The black sand sagebrush (Artemisia filifolia) microemulsion 100 * preventive effect of investigation in 5 days is higher than 80% after for the second time dispenser, and is close with contrast medicament Sukeling 1000 * preventive effect.
Table 3: black sand sagebrush (Artemisia filifolia) microemulsion is to the control efficiency of tomato in plastic greenhouse grey mold
Comprehensive field control effectiveness test; black sand sagebrush (Artemisia filifolia) bactericide is when preventing and treating tomato in plastic greenhouse gray mold and cucumber downy mildew; suitable with contrast medicament Sukeling; simultaneously; plant resource kills equal agent and has certain lasting period; and environmentally friendly, therefore very applicable in protection ground growing vegetables, have very large application and popularization value.
Claims (2)
1. a black sand sagebrush (Artemisia filifolia) bactericide is characterized in that, the preparation form that should deceive the sand sagebrush (Artemisia filifolia) bactericide that makes is microemulsion or aqueous emulsion, wherein:
Described aqueous emulsion with methyl alcohol 5kg dissolving, under agitation adds polyoxyethylene nonylphenol ether phosphate 20kg by black sand sagebrush (Artemisia filifolia) extract 25kg, stirs, and adds deionized water 50kg, namely gets the black sand sagebrush (Artemisia filifolia) aqueous emulsion of 100kg;
Described microemulsion is dissolved in the 5kg methyl alcohol by black sand sagebrush (Artemisia filifolia) extract 25kg and 20kg polyoxyethylene nonylphenol ether phosphate, and above solution is heated to 40 ℃ in homogenizer, adds deionized water 50kg under the high-speed stirred; Dropwise, stir 45min again, cooling namely gets black sand sagebrush (Artemisia filifolia) bactericidal microemulsion;
Described black sand sagebrush (Artemisia filifolia) extract adopts root, stem, leaf, the flower of black sand sagebrush (Artemisia filifolia) to be raw material, extracts with ethyl acetate solvent or methyl alcohol, and extract obtains through concentrated.
2. the preparation method of black sand sagebrush (Artemisia filifolia) bactericide claimed in claim 1, it is characterized in that, described aqueous emulsion is by black sand sagebrush (Artemisia filifolia) extract 25kg, dissolve with methyl alcohol 5kg, under agitation add polyoxyethylene nonylphenol ether phosphate 20kg, stir, add deionized water 50kg, namely get the black sand sagebrush (Artemisia filifolia) aqueous emulsion of 100kg;
Described microemulsion is dissolved in the 5kg methyl alcohol by black sand sagebrush (Artemisia filifolia) extract 25kg and 20kg polyoxyethylene nonylphenol ether phosphate, and above solution is heated to 40 ℃ in homogenizer, adds deionized water 50kg under the high-speed stirred; Dropwise, stir 45min again, cooling namely gets black sand sagebrush (Artemisia filifolia) bactericidal microemulsion.
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| CN104351262B (en) * | 2014-09-29 | 2015-12-30 | 北京农学院 | Pilose gerbera herb extract and preparation method thereof and application |
| CN104430625A (en) * | 2014-11-12 | 2015-03-25 | 苏州市新巷农艺科技园 | Method for preparing special environment-friendly bactericide for flowers and plants |
| CN104705350B (en) * | 2015-04-10 | 2017-06-16 | 兰州大学 | A kind of white sand parthenium extract and its preparation method and application |
| CN109169644A (en) * | 2018-09-07 | 2019-01-11 | 东北农业大学 | A kind of argy wormwood microemulsion and preparation method thereof |
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| CN1814064A (en) * | 2005-11-28 | 2006-08-09 | 蓝子花 | Collateral-flow-activating pain-relieving ointment of semen Artemisiae ordosicae for treating affection by dampness |
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|---|---|---|---|---|
| CN1814064A (en) * | 2005-11-28 | 2006-08-09 | 蓝子花 | Collateral-flow-activating pain-relieving ointment of semen Artemisiae ordosicae for treating affection by dampness |
Non-Patent Citations (2)
| Title |
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| 赵东保,等.黑沙蒿黄酮类化学成分研究.《中国中药杂志》.2005,第30卷(第18期),第1430-1432页. |
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Effective date of registration: 20141230 Address after: 712100, Shaanxi Yangling Demonstration Zone Industrial Park Yang Yang Road West of the south side Patentee after: Yangling Fu Ji Biological Technology Co. Ltd. Address before: 712100 Shaanxi Province, Xi'an city Yangling District Tai Road No. 3 demonstration Patentee before: Yangling Nongkeda Research & Development Center of Biorational Pesticide |