CN101642138A - Aconitum carmichaeli plant acaricide and preparation method thereof - Google Patents
Aconitum carmichaeli plant acaricide and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a plant acaricide suitable for controlling pest mites on such economic crops as fruit trees and vegetables and a preparation method and application thereof. The plant acaricide is prepared by adding surfactant, emulsifiers, penetrants, synergists and the like into the effective components of Aconitum carmichaeli, and has the characteristics of high efficiency, low toxicity, low residues and accordance with the environment, etc.
Description
Patent application of the present invention is for dividing an application, and the original bill application number is 200710119720.X, and the applying date is on July 31st, 2007, and denomination of invention is black nightshade, the rhizome of Chinese monkshood or Artemesia annua plant acaricide and preparation method thereof.
Technical field
The present invention relates to a kind of agricultural chemicals and preparation method thereof, particularly relate to a kind of miticide and preparation method thereof.
Background technology
" five little insects (tetranychid, coccid, aphid, aleyrodid and thrips) " is the important pests (mite) on the agricultural, and the harm to crop in recent years has the trend that increases the weight of.Use the negative effect that chemical pesticide control brought to receive much attention, thirst for from plant or other biological, screening the activated material of insect, thus the agent for controlling noxious insect pests of exploitation and environment friendliness.Botanical pesticide has advantages such as wide spectrum, low toxicity, safety, contains the acaricidal activity material in many plants, and the acaricidal research and development of plant resource have great importance.Methanolic extract, chloroform extract, ligroin extraction as Chinese Stellera Root in the existing public technology all have biologically active preferably to tetranychus viennensis, root of langdu chloroform is carried in the Chinese Stellera Root may contain noxious material, therefore in systemic action, cause metabolic enzyme activity to raise, but in action of contace poison, the activity of esterase is subjected to inhibition to a certain degree.By repetition test, found that the extract of black nightshade (Solanumnigrum), the rhizome of Chinese monkshood (Aconitum carmichaeli) and argy wormwood plants such as (Artemesia annua) has acaricidal activity preferably.
Summary of the invention
The present invention adopts the method for chemical extraction, and extracting from black nightshade, the rhizome of Chinese monkshood or argy wormwood complete stool has the active substance of lethal effect to the mite class, and is prepared into the plant resource miticide.
Black nightshade complete stool active component of the present invention can be black nightshade whole strain extract or black nightshade complete stool extract, and extract preparation technology is selected from one of following method in the black nightshade complete stool:
A adopts multi-function extractor, and the black nightshade complete stool is made powder, with the volume ratio of organic solvent benzinum be 1: 2-8 (preferred 1: 3 or 1: 5), temperature is soaked or cold soaking 4-48 hour, filter, drying, black nightshade extract;
B adopts multi-function extractor, and the volume ratio of Black Nightshade Herb and organic solvent ethanol is 1: 2-8 (preferred 1: 3 or 1: 5), and diacolation extracts 2-8 time repeatedly, or continuous backflow extracted 4-20 hour, filters, and drying must black nightshade extract.
Black nightshade extract preparation technology: with black nightshade extract of the present invention with dissolve with methanol after, place airtight extractor, adopt liquid-liquid apportion design extraction with chloroform or benzinum solvent with 0.5: 1 ratio of volume ratio and methyl alcohol, with solvent polarity is the extraction order of solvent from small to large, and finally collecting chloroform or petroleum ether extraction phase and being evaporated to relative density is 0.5-1g/cm
3(preferred relative density is 0.8769g/cm to the ointment shape
3) the black nightshade extract.
Acaricidal preparation method: black nightshade extract or black nightshade extract with chloroform, cyclohexane, benzene, dimethylbenzene or the dissolving of ethanol equal solvent, can be in the following order added auxiliary materials such as promoting extract or extract dissolving or the solubilizer, emulsifier and/or the suspending agent that suspend, synergist, bleeding agent therein with ratio and make miticide.
The black nightshade extract miticide:
Extract 2-35 weight portion
Solvent 28-98 weight portion
Solubilizer 0.5-15 weight portion
Emulsifier or suspending agent 0.7-15 weight portion
Synergist 0.4-10 weight portion
Bleeding agent 0.3-8 weight portion
Black nightshade extract miticide:
Extract 2-30 weight portion
Solvent 25-95 weight portion
Solubilizer 0.4-15 weight portion
Emulsifier or suspending agent 0.6-15 weight portion
Synergist 0.5-9 weight portion
Bleeding agent 0.5-8 weight portion
The organic solvent of using among the described black nightshade extract preparation method can also be selected from except that benzinum non-limitingly: a kind of in ethanol, chloroform, 30-90 ℃ benzinum, ether, ethyl acetate, n-hexane, cyclohexane, benzene, methyl alcohol, acetone, the cyclohexanone etc.
Among the described black nightshade extract preparation method, used organic solvent removes benzinum can also be selected from a kind of in ethanol, chloroform, 30-90 ℃ benzinum, ether, methyl alcohol, n-hexane, cyclohexane, benzene, ethyl acetate, acetone, the cyclohexanone.
Among the acaricidal preparation method, solvent is selected from a kind of in water, ethanol, methyl alcohol, acetone, cyclohexanone, toluene, dimethylbenzene, benzinum, petroleum aromatic, the purified petroleum benzin; Solubilizer be neopelex, Potassium dodecylbenzenesulfonate, polysorbate, polyethylene glycol, sorbierite polyoxy ether, lignosulfonates, tea withered, take any in the Chinese honey locust; Synergist is any in Tea Saponin, 2-C1C6H4-N=OCH3SCH3, methylenedioxy benzene derivative, 6-vinyl capraldehyde, the Octachlorodipropyl Ether; Emulsifier is any in C15～17H31～37COONa, odium stearate, lauryl sodium sulfate, N-domiphen, APEO, polyethenoxy ether, paraoctyl phenol APEO, aliphatic alcohol polyethenoxy base ether, aliphatic acid polyethenoxy base ester, the alkylaryl sulfonates; Bleeding agent is any in emulsifier BP, azone, the triphen phosphorus.
The black nightshade extract miticide is preferably:
Extract 15 weight portions
Cyclohexanone 65 weight portions
Tween 80 1.5 weight portions
Tea Saponin 3.0 weight portions
Polyethenoxy ether 1.5 weight portions
Emulsifier BP 2.5 weight portions
Black nightshade extract miticide is preferably:
Extract 12 weight portions
Dimethylbenzene 55 weight portions
Sorbierite polyoxy ether 2.0 weight portions
6-vinyl capraldehyde 3.0 weight portions
Lauryl sodium sulfate 2.5 weight portions
Azone 3.0 weight portions
The present patent application also discloses a kind of rhizome of Chinese monkshood active component and miticide, and rhizome of Chinese monkshood active component and miticide and above-mentioned black nightshade active component and acaricidal technical scheme are except that the raw material rhizome of Chinese monkshood is different with black nightshade, and all the other technical characterictics are identical.Final relative density of collecting chloroform or petroleum ether extraction phase and concentrating under reduced pressure can also be preferably 0.8988g/cm among the rhizome of Chinese monkshood complete stool extract preparation technology
3
The present patent application also discloses a kind of argy wormwood active component and miticide, and argy wormwood active component and miticide and above-mentioned black nightshade active component and acaricidal technical scheme are except that the raw material argy wormwood is different with black nightshade, and all the other technical characterictics are identical.Final relative density of collecting chloroform or petroleum ether extraction phase and concentrating under reduced pressure can also be preferably 0.9081g/cm among the argy wormwood complete stool extract preparation technology
3
The invention provides a kind of efficient, low toxicity, low-residual, with novel biopesticide of environment and and association biological with other, it all has far reaching significance to environmental protection and the pesticide resistance that solves the evil mite.Compare with pesticides prepared by chemistry, the present invention has following characteristics and advantage:
(1) because black nightshade, the rhizome of Chinese monkshood or argy wormwood are the plant of occurring in nature, so its extract is easy to decompose under field conditions (factors), to environment and ecosystem safety on every side, do not have problem of environmental pollution.(2) black nightshade, the rhizome of Chinese monkshood or argy wormwood miticide are a kind of multicomponent mixtures, and the mite class is had a plurality of action sites, therefore are difficult for developing immunity to drugs.(3) experiment showed, that black nightshade, the rhizome of Chinese monkshood or argy wormwood miticide have significant miticidal effect, have the characteristics of chemical pesticide produce effects.(4) extraction of active ingredients is simple in black nightshade, the rhizome of Chinese monkshood or the argy wormwood, very helps carrying out suitability for industrialized production.
Following experimental example or embodiment are used to further specify but are not limited to the present invention.
Experimental example 1
By black nightshade, the rhizome of Chinese monkshood or biennial wormwood extract and black nightshade, the rhizome of Chinese monkshood or argy wormwood extract that the present invention obtains, standard method-slide method of recommending with reference to FAO carries out biological activity determination to pest mites such as tetranychus viennensis, Tetranychus cinnabarinus and truncate leaf mites; Method is long for two-sided tape being cut into 2-3cm, is attached to an end of slide, throws off the scraps of paper on the adhesive tape with tweezers, selects the female one-tenth mite that size is consistent, body colour is bright-coloured, action is active with No. zero writing brush, its back is bonded on the two-sided tape every sticking 30; In temperature is (25 ± 1) ℃, place 4h in the biochemical incubator about RH85% after, use binocular vision, reject death or inactive individuality; End that will band mite slide immerses in the soup, takes out after shaking 5s gently, blots mite body and unnecessary soup thereof on every side with blotting paper rapidly; Place biochemical incubator, use the binocular check result behind the 24h; Touch the mite body with writing brush, motionless person is death with the mite foot; 3 repetitions of each concentration the results are shown in following table 1-2:
Table 1 black nightshade extract, rhizome of Chinese monkshood extract and biennial wormwood extract are to Tetranychus urticae (Teranychus urticae) miticidal effect
Table 2 black nightshade extract, rhizome of Chinese monkshood extract and argy wormwood extract are to the Tetranychus urticae toxic effect
Ovicidal action is also improved with reference to the blade residual hazard method (Leaf-residue method) that FAO recommends, gather fresh ground beans blade, petiole is clipped 0.5cm, and on petiole, wrap wet cotton balls, being placed on water planting supports on the platform, every blade connects 30 of female one-tenth mites, places under (25 ± 1) ℃ and lets alone the 24h of laying eggs, and removes female one-tenth mite, behind the inspection record ovum grain number, place (25 ± 1) ℃ constant incubator, measure when ovum reaches 36～48h age, blade that will the band ovum immerses respectively handles soup 5s, be placed on the blotting paper then and dry in the shade, put back to water planting and support on the platform, treat the hatching of control group ovum and grow the as for mite stage, check that statistics respectively handles lethality; The Walnut Leaves extract kills the ovum effect and sees Table 3:
Table 3 black nightshade extract, rhizome of Chinese monkshood extract and argy wormwood extract are to the active effect of Tetranychus urticae ovum
After antifeedant activity test is cleaned ground beans blade, blot water, overleaf along a side (about 0.01ml/cm of arteries and veins in the leaf
2) coat sample for examination, opposite side distilled water is done contrast; 30 head lobe mites are connected on the leaf back, and the glass collar with diameter 5cm covers then, and leaf Zhong Mai both sides processing area and contrast area are equated; Check behind the 24h that leaf Zhong Mai both sides tetranychid perches number, the tetranychid that dwells on Ye Zhongmai and glass collar wall does not count; Each 30 of examination worms, triplicate handled;
Food refusal rate (%)=[(check plot tetranychid number-treatment region tetranychid number)/sum] * 100% the results are shown in Table 4:
Table 4 black nightshade extract, rhizome of Chinese monkshood extract and argy wormwood extract are to the antifeedant activity effect of Tetranychus urticae
Experimental example 2 is compared with disclosed extraction process, and active component that technology of the present invention is carried has preferably ovum and antifeedant activity extremely, the results are shown in Table 5:
The different extraction processes of table 5 are to the comparison of black nightshade, the rhizome of Chinese monkshood and argy wormwood activity
Annotate: A: be the action effect of active component that technology of the present invention is carried (extract or extract), B: be the action effect of active component that disclosed technology is carried (extract or extract)
Embodiment all can realize above-mentioned effect below the present invention.
Embodiment
Embodiment 1:
The black nightshade complete stool is cleaned, dried in the shade, grind the back and cross 40 mesh sieves in the ventilation; Plant powder after pulverizing is put into multi-function extractor, extract with the benzinum (30-90 ℃) of 5 times of volumes of its powder, collection Petroleum ether extraction phase, concentrating under reduced pressure gets extract; Getting extract 15kg adding toluene 65kg adding has in the mixing kettle of agitator and thermometer, under 40 ℃, mixed 1.5 hours, add odium stearate 1.5kg, 3.0kg Tween 80, neopelex 1.5kg, chlorine ketone 2.5kg, mix, obtain black nightshade extract miticide missible oil.
Embodiment 2:
Rhizome of Chinese monkshood complete stool is cleaned, dried in the shade, grind the back and cross 40 mesh sieves in the ventilation; Plant powder after pulverizing is put into multi-function extractor, extract with the benzinum (30-90 ℃) of 5 times of volumes of its powder, collection Petroleum ether extraction phase, concentrating under reduced pressure gets extract; Getting extract 15kg adding toluene 65kg adding has in the mixing kettle of agitator and thermometer, under 40 ℃, mixed 1.5 hours, add odium stearate 1.5kg, 3.0kg Tween 80, neopelex 1.5kg, chlorine ketone 2.5kg, mix, obtain rhizome of Chinese monkshood extract miticide missible oil.
Embodiment 3:
The argy wormwood complete stool is cleaned, dried in the shade, grind the back and cross 40 mesh sieves in the ventilation; Plant powder after pulverizing is put into multi-function extractor, extract with the benzinum (30-90 ℃) of 5 times of volumes of its powder, collection Petroleum ether extraction phase, concentrating under reduced pressure gets extract; Getting extract 15kg adding toluene 65kg adding has in the mixing kettle of agitator and thermometer, under 40 ℃, mixed 1.5 hours, add odium stearate 1.5kg, 3.0kg Tween 80, neopelex 1.5kg, chlorine ketone 2.5kg, mix, obtain biennial wormwood extract miticide missible oil.
Embodiment 4:
The black nightshade complete stool is cleaned, under 20-30 ℃, dried, grind the back and cross 40 mesh sieves; Plant powder after pulverizing is put into multi-function extractor, extract with the chloroform of 7 times of volumes, concentrating under reduced pressure gets extract; Getting extract 12kg part adding dimethylbenzene 55kg adding has in the mixing kettle of agitator and thermometer, under 40 ℃, mixed 3 hours, adding odium stearate 2.0kg, Tween 80 are 3kg, neopelex 2.5kg, chlorine ketone 3.0kg, mix, obtain black nightshade whole strain extract miticide missible oil.
Embodiment 5:
Rhizome of Chinese monkshood complete stool is cleaned, under 20-30 ℃, dried, grind the back and cross 40 mesh sieves; Plant powder after pulverizing is put into multi-function extractor, extract with the chloroform of 7 times of volumes, concentrating under reduced pressure gets extract; Getting extract 12kg part adding dimethylbenzene 55kg adding has in the mixing kettle of agitator and thermometer, under 40 ℃, mixed 3 hours, adding odium stearate 2.0kg, Tween 80 are 3kg, neopelex 2.5kg, chlorine ketone 3.0kg, mix, obtain rhizome of Chinese monkshood whole strain extract miticide missible oil.
Embodiment 6:
The argy wormwood complete stool is cleaned, under 20-30 ℃, dried, grind the back and cross 40 mesh sieves; Plant powder after pulverizing is put into multi-function extractor, extract with the chloroform of 7 times of volumes, concentrating under reduced pressure gets extract; Getting extract 12kg part adding dimethylbenzene 55kg adding has in the mixing kettle of agitator and thermometer, under 40 ℃, mixed 3 hours, adding odium stearate 2.0kg, Tween 80 are 3kg, neopelex 2.5kg, chlorine ketone 3.0kg, mix, obtain argy wormwood whole strain extract miticide missible oil.
Embodiment 7:
The black nightshade complete stool is cleaned, dried in the shade, grind the back and cross 40 mesh sieves in the ventilation; Plant powder after pulverizing is put into multi-function extractor, extract with 7 times of volumes methanol, concentrating under reduced pressure gets extract; After getting extract 9kg adding methyl alcohol 45kg, inject the mixing kettle that has agitator and thermometer, under 40 ℃, mixed 3 hours, the adding Tween 80 is to mix behind 3.5kg, the chlorine ketone 3kg, makes black nightshade whole strain extract miticide missible oil.
Embodiment 8:
Rhizome of Chinese monkshood complete stool is cleaned, dried in the shade, grind the back and cross 40 mesh sieves in the ventilation; Plant powder after pulverizing is put into multi-function extractor, extract with 7 times of volumes methanol, concentrating under reduced pressure gets extract; After getting extract 9kg adding methyl alcohol 45kg, inject the mixing kettle that has agitator and thermometer, under 40 ℃, mixed 3 hours, the adding Tween 80 is to mix behind 3.5kg, the chlorine ketone 3kg, makes rhizome of Chinese monkshood whole strain extract miticide missible oil.
Embodiment 9:
The argy wormwood complete stool is cleaned, dried in the shade, grind the back and cross 40 mesh sieves in the ventilation; Plant powder after pulverizing is put into multi-function extractor, extract with 7 times of volumes methanol, concentrating under reduced pressure gets extract; After getting extract 9kg adding methyl alcohol 45kg, inject the mixing kettle that has agitator and thermometer, under 40 ℃, mixed 3 hours, the adding Tween 80 is to mix behind 3.5kg, the chlorine ketone 3kg, makes argy wormwood whole strain extract miticide missible oil.
Embodiment 10:
Adopting multi-function extractor, is 1: 4 with the volume ratio of black nightshade complete stool and organic solvent ethanol, and temperature was soaked 10 hours, filtration, and drying respectively must the black nightshade whole strain extract; The extract of black nightshade complete stool with dissolve with methanol after, place airtight extractor, adopt liquid-liquid apportion design extraction with the benzinum solvent with 0.5: 1 ratio of volume ratio and methyl alcohol, with solvent polarity is the extraction order of solvent from small to large, final collection petroleum ether extraction phase also is evaporated to the ointment shape, gets black nightshade complete stool extract; After getting black nightshade complete stool extract 7kg usefulness benzinum 40kg dissolving, inject the mixing kettle that has agitator and thermometer, under 30 ℃, mixed 2 hours,, adding Tween 80 with ratio in the following order is 3.0kg, odium stearate 2.0kg, azone 4kg, makes black nightshade complete stool extract miticide missible oil.
Embodiment 11:
Adopting multi-function extractor, is 1: 4 with the volume ratio of rhizome of Chinese monkshood complete stool and organic solvent ethanol, and temperature was soaked 10 hours, filtration, and drying must rhizome of Chinese monkshood whole strain extract; The extract of rhizome of Chinese monkshood complete stool with dissolve with methanol after, place airtight extractor, adopt liquid-liquid apportion design extraction with the benzinum solvent with 0.5: 1 ratio of volume ratio and methyl alcohol, with solvent polarity is the extraction order of solvent from small to large, final collection petroleum ether extraction phase also is evaporated to the ointment shape, gets rhizome of Chinese monkshood complete stool extract; After getting rhizome of Chinese monkshood complete stool extract 7kg usefulness benzinum 40kg dissolving, inject the mixing kettle that has agitator and thermometer, under 30 ℃, mixed 2 hours,, adding Tween 80 with ratio in the following order is 3.0kg, odium stearate 2.0kg, azone 4kg, makes rhizome of Chinese monkshood complete stool extract miticide missible oil.
Embodiment 12:
Adopting multi-function extractor, is 1: 4 with the volume ratio of argy wormwood complete stool and organic solvent ethanol, and temperature was soaked 10 hours, filtration, and drying must the argy wormwood whole strain extract; The extract of argy wormwood complete stool with dissolve with methanol after, place airtight extractor, adopt liquid-liquid apportion design extraction with the benzinum solvent with 0.5: 1 ratio of volume ratio and methyl alcohol, with solvent polarity is the extraction order of solvent from small to large, final collection petroleum ether extraction phase also is evaporated to the ointment shape, gets argy wormwood complete stool extract; After getting argy wormwood complete stool extract 7kg usefulness benzinum 40kg dissolving, inject the mixing kettle that has agitator and thermometer, under 30 ℃, mixed 2 hours,, adding Tween 80 with ratio in the following order is 3.0kg, odium stearate 2.0kg, azone 4kg, makes wormwood artemisia complete stool extract miticide missible oil.
Embodiment 13: the preparation of black nightshade whole strain extract
Adopting multi-function extractor, is 1: 5 with the volume ratio of black nightshade complete stool and organic solvent ethanol, and temperature was soaked 10 hours, filtration, and drying must the black nightshade whole strain extract.
Embodiment 14: the preparation of rhizome of Chinese monkshood whole strain extract
Adopting multi-function extractor, is 1: 5 with the volume ratio of rhizome of Chinese monkshood complete stool and organic solvent ethanol, and temperature was soaked 10 hours, filtration, and drying must rhizome of Chinese monkshood whole strain extract.
Embodiment 15: the preparation of argy wormwood whole strain extract
Adopting multi-function extractor, is 1: 5 with the volume ratio of argy wormwood complete stool and organic solvent ethanol, and temperature was soaked 10 hours, filtration, and drying must the argy wormwood whole strain extract.
Embodiment 16: the preparation of black nightshade whole strain extract
Adopting multi-function extractor, is 1: 3 with the volume ratio of black nightshade complete stool powder and organic solvent-normal hexane, and diacolation extracts 8 times repeatedly, filtration, and drying must the black nightshade whole strain extract.
Embodiment 17: the preparation of rhizome of Chinese monkshood whole strain extract
Adopting multi-function extractor, is 1: 3 with the volume ratio of rhizome of Chinese monkshood complete stool powder and organic solvent-normal hexane, and diacolation extracts 8 times repeatedly, filtration, and drying must rhizome of Chinese monkshood whole strain extract.
Embodiment 18: the preparation of argy wormwood whole strain extract
Adopting multi-function extractor, is 1: 3 with the volume ratio of argy wormwood complete stool powder and organic solvent-normal hexane, and diacolation extracts 8 times repeatedly, filtration, and drying must the argy wormwood whole strain extract.
Embodiment 19: the preparation of black nightshade complete stool extract
With embodiment 13,16 gained black nightshade whole strain extracts with dissolve with methanol after, place airtight extractor, adopt liquid-liquid apportion design extraction with the chloroform solvent with 0.5: 1 ratio of volume ratio and methyl alcohol, with solvent polarity is the extraction order of solvent from small to large, final collection chloroform extraction phase also is evaporated to the ointment shape, and relative density is 0.8647g/cm
3, get black nightshade complete stool extract.
Embodiment 20: the preparation of rhizome of Chinese monkshood complete stool extract
With embodiment 14,17 gained rhizome of Chinese monkshood whole strain extracts with dissolve with methanol after, place airtight extractor, adopt liquid-liquid apportion design extraction with the chloroform solvent with 0.5: 1 ratio of volume ratio and methyl alcohol, with solvent polarity is the extraction order of solvent from small to large, final collection chloroform extraction phase also is evaporated to the ointment shape, and relative density is 0.8356g/cm
3, get rhizome of Chinese monkshood complete stool extract.
Embodiment 21: the preparation of argy wormwood complete stool extract
With embodiment 15,18 gained argy wormwood whole strain extracts with dissolve with methanol after, place airtight extractor, adopt liquid-liquid apportion design extraction with the chloroform solvent with 0.5: 1 ratio of volume ratio and methyl alcohol, with solvent polarity is the extraction order of solvent from small to large, final collection chloroform extraction phase also is evaporated to the ointment shape, and relative density is 0.8897g/cm
3, get argy wormwood complete stool extract.
Embodiment 22: the preparation of black nightshade whole strain extract
Adopting multi-function extractor, is 1: 6 with the volume ratio of black nightshade complete stool powder and organic solvent ethyl acetate, and continuous backflow was extracted 10 hours, filtered, and drying must the black nightshade whole strain extract.
Embodiment 23: the preparation of rhizome of Chinese monkshood whole strain extract
Adopting multi-function extractor, is 1: 6 with the volume ratio of rhizome of Chinese monkshood complete stool powder and organic solvent ethyl acetate, and continuous backflow was extracted 10 hours, filtered, and drying must rhizome of Chinese monkshood whole strain extract.
Embodiment 24: the preparation of argy wormwood whole strain extract
Adopting multi-function extractor, is 1: 6 with the volume ratio of argy wormwood complete stool powder and organic solvent ethyl acetate, and continuous backflow was extracted 10 hours, filtered, and drying must the argy wormwood whole strain extract.
Embodiment 25: the preparation of black nightshade complete stool extract
With the black nightshade whole strain extract of embodiment 22 gained with dissolve with methanol after, place airtight extractor, adopt liquid-liquid apportion design extraction with the chloroform solvent with 0.5: 1 ratio of volume ratio and methyl alcohol, with solvent polarity is the extraction order of solvent from small to large, final collection petroleum ether extraction phase also is evaporated to the ointment shape, and relative density is 0.8567g/cm
3, get black nightshade complete stool extract.
Embodiment 26: the preparation of rhizome of Chinese monkshood complete stool extract
Respectively with the rhizome of Chinese monkshood whole strain extract of embodiment 23 gained with dissolve with methanol after, place airtight extractor, adopt liquid-liquid apportion design extraction with the chloroform solvent with 0.5: 1 ratio of volume ratio and methyl alcohol, with solvent polarity is the extraction order of solvent from small to large, final collection petroleum ether extraction phase also is evaporated to the ointment shape, and relative density is 0.8326g/cm
3, get rhizome of Chinese monkshood complete stool extract.
Embodiment 27: the preparation of argy wormwood complete stool extract
Respectively with the argy wormwood whole strain extract of embodiment 24 gained with dissolve with methanol after, place airtight extractor, adopt liquid-liquid apportion design extraction with the chloroform solvent with 0.5: 1 ratio of volume ratio and methyl alcohol, with solvent polarity is the extraction order of solvent from small to large, final collection petroleum ether extraction phase also is evaporated to the ointment shape, and relative density is 0.8791g/cm
3, get argy wormwood complete stool extract.
Embodiment 28: the preparation of black nightshade whole strain extract
Adopting multi-function extractor, is 1: 3 with the volume ratio of black nightshade complete stool powder and organic solvent ether, cold soaking 20 hours, and filtration, drying must the black nightshade whole strain extract.
Embodiment 29: the preparation of rhizome of Chinese monkshood whole strain extract
Adopting multi-function extractor, is 1: 3 with the volume ratio of rhizome of Chinese monkshood complete stool powder and organic solvent ether, cold soaking 20 hours, and filtration, drying must rhizome of Chinese monkshood whole strain extract.
Embodiment 30: the preparation of argy wormwood whole strain extract
Adopting multi-function extractor, is 1: 3 with the volume ratio of argy wormwood complete stool powder and organic solvent ether, cold soaking 20 hours, and filtration, drying must the argy wormwood whole strain extract.
Embodiment 31: the preparation of black nightshade whole strain extract
Adopting multi-function extractor, is 1: 6 with the volume ratio of black nightshade complete stool powder and organic solvent methyl alcohol, and temperature was soaked 10 hours, filtration, and drying must the black nightshade whole strain extract.
Embodiment 32: the preparation of rhizome of Chinese monkshood whole strain extract
Adopting multi-function extractor, is 1: 6 with the volume ratio of rhizome of Chinese monkshood complete stool powder and organic solvent methyl alcohol, and temperature was soaked 10 hours, filtration, and drying must rhizome of Chinese monkshood whole strain extract.
Embodiment 33: the preparation of argy wormwood whole strain extract
Adopting multi-function extractor, is 1: 6 with the volume ratio of argy wormwood complete stool powder and organic solvent methyl alcohol, and temperature was soaked 10 hours, filtration, and drying must the argy wormwood whole strain extract.
Embodiment 34: the preparation of black nightshade whole strain extract
Adopting multi-function extractor, is 1: 7 with the volume ratio of black nightshade complete stool powder and organic solvent ethyl acetate, mac per hor X, and filtration, drying must the black nightshade whole strain extract.
Embodiment 35: the preparation of rhizome of Chinese monkshood whole strain extract
Adopting multi-function extractor, is 1: 7 with the volume ratio of rhizome of Chinese monkshood complete stool powder and organic solvent ethyl acetate, mac per hor X, and filtration, drying must rhizome of Chinese monkshood whole strain extract.
Embodiment 36: the preparation of argy wormwood whole strain extract
Adopting multi-function extractor, is 1: 7 with the volume ratio of argy wormwood complete stool powder and organic solvent ethyl acetate, mac per hor X, and filtration, drying must the argy wormwood whole strain extract.
Embodiment 37: the preparation of black nightshade whole strain extract
Adopting multi-function extractor, is 1: 4 with the volume ratio of black nightshade complete stool powder and organic solvent-benzene, and diacolation extracts 5 times repeatedly, filtration, and drying must the black nightshade whole strain extract.
Embodiment 38: the preparation of rhizome of Chinese monkshood whole strain extract
Adopting multi-function extractor, is 1: 4 with the volume ratio of rhizome of Chinese monkshood complete stool powder and organic solvent-benzene, and diacolation extracts 5 times repeatedly, filtration, and drying must rhizome of Chinese monkshood whole strain extract.
Embodiment 39: the preparation of argy wormwood whole strain extract
Adopting multi-function extractor, is 1: 4 with the volume ratio of argy wormwood complete stool powder and organic solvent-benzene, and diacolation extracts 5 times repeatedly, filtration, and drying must the argy wormwood whole strain extract.
Embodiment 40: the preparation of black nightshade whole strain extract
Adopting multi-function extractor, is 1: 5 with the volume ratio of black nightshade complete stool powder and organic solvent-acetone, and continuous backflow was extracted 10 hours, filtration, and drying must the black nightshade whole strain extract.
Embodiment 41: the preparation of rhizome of Chinese monkshood whole strain extract
Adopting multi-function extractor, is 1: 5 with the volume ratio of rhizome of Chinese monkshood complete stool powder and organic solvent-acetone, and continuous backflow was extracted 10 hours, filtration, and drying must rhizome of Chinese monkshood whole strain extract.
Embodiment 42: the preparation of argy wormwood whole strain extract
Adopting multi-function extractor, is 1: 5 with the volume ratio of argy wormwood complete stool powder and organic solvent-acetone, and continuous backflow was extracted 10 hours, filtration, and drying must the argy wormwood whole strain extract.
Embodiment 43: the preparation of black nightshade whole strain extract
Adopting multi-function extractor, is 1: 6 with the volume ratio of black nightshade complete stool powder and organic solvent-normal hexane, and diacolation extracts 3 times repeatedly, filtration, and drying must the black nightshade whole strain extract.
Embodiment 44: the preparation of rhizome of Chinese monkshood whole strain extract
Adopting multi-function extractor, is 1: 6 with the volume ratio of rhizome of Chinese monkshood complete stool powder and organic solvent-normal hexane, and diacolation extracts 3 times repeatedly, filtration, and drying must rhizome of Chinese monkshood whole strain extract.
Embodiment 45: the preparation of argy wormwood whole strain extract
Adopting multi-function extractor, is 1: 6 with the volume ratio of argy wormwood complete stool powder and organic solvent-normal hexane, and diacolation extracts 3 times repeatedly, filtration, and drying must the argy wormwood whole strain extract.
Embodiment 46: the preparation of black nightshade whole strain extract
Adopting multi-function extractor, is 1: 7 with the volume ratio of black nightshade complete stool powder and organic solvent ethyl acetate, and continuous backflow was extracted 18 hours, filtration, and drying must the black nightshade whole strain extract.
Embodiment 47: the preparation of rhizome of Chinese monkshood whole strain extract
Adopting multi-function extractor, is 1: 7 with the volume ratio of rhizome of Chinese monkshood complete stool powder and organic solvent ethyl acetate, and continuous backflow was extracted 18 hours, filtration, and drying must rhizome of Chinese monkshood whole strain extract.
Embodiment 48: the preparation of argy wormwood whole strain extract
Adopting multi-function extractor, is 1: 7 with the volume ratio of argy wormwood complete stool powder and organic solvent ethyl acetate, and continuous backflow was extracted 18 hours, filtration, and drying must the argy wormwood whole strain extract.
Embodiment 49: the preparation of black nightshade complete stool extract
Behind 30-90 ℃ of petroleum ether dissolution of embodiment 28 gained black nightshade whole strain extracts usefulness, place airtight extractor, adopt with 0.5: 1 ratio of volume ratio and 30-90 ℃ of benzinum with the benzinum solvent that liquid-liquid apportion design extraction is final collects petroleum ether extraction mutually and be evaporated to the ointment shape, relative density is 0.8419g/cm
3, get black nightshade complete stool extract.
Embodiment 50: the preparation of rhizome of Chinese monkshood complete stool extract
Behind 30-90 ℃ of petroleum ether dissolution of embodiment 29 gained rhizome of Chinese monkshood whole strain extracts usefulness, place airtight extractor, adopt with 0.5: 1 ratio of volume ratio and 30-90 ℃ of benzinum with the benzinum solvent that liquid-liquid apportion design extraction is final collects petroleum ether extraction mutually and be evaporated to the ointment shape, relative density is 0.8378g/cm
3, get rhizome of Chinese monkshood complete stool extract.
Embodiment 51: the preparation of argy wormwood complete stool extract
Behind 30-90 ℃ of petroleum ether dissolution of embodiment 30 gained argy wormwood whole strain extracts usefulness, place airtight extractor, adopt with 0.5: 1 ratio of volume ratio and 30-90 ℃ of benzinum with the benzinum solvent that liquid-liquid apportion design extraction is final collects petroleum ether extraction mutually and be evaporated to the ointment shape, relative density is 0.8791g/cm
3, get argy wormwood complete stool extract.
Embodiment 52: the preparation of black nightshade complete stool extract
With embodiment 31 gained black nightshade whole strain extracts with dissolve with ethanol after, place airtight extractor, adopt liquid-liquid apportion design extraction with the chloroform solvent with 0.5: 1 ratio of volume ratio and ethanol, with solvent polarity is the extraction order of solvent from small to large, final collection chloroform extraction phase also is evaporated to the ointment shape, and relative density is 0.7998g/cm
3, get black nightshade complete stool extract.
Embodiment 53: the preparation of rhizome of Chinese monkshood complete stool extract
With embodiment 32 gained rhizome of Chinese monkshood whole strain extracts with dissolve with ethanol after, place airtight extractor, adopt liquid-liquid apportion design extraction with the chloroform solvent with 0.5: 1 ratio of volume ratio and ethanol, with solvent polarity is the extraction order of solvent from small to large, final collection chloroform extraction phase also is evaporated to the ointment shape, and relative density is 0.8826g/cm
3, get rhizome of Chinese monkshood complete stool extract.
Embodiment 54: the preparation of argy wormwood complete stool extract
With embodiment 33 gained argy wormwood whole strain extracts with dissolve with ethanol after, place airtight extractor, adopt liquid-liquid apportion design extraction with the chloroform solvent with 0.5: 1 ratio of volume ratio and ethanol, with solvent polarity is the extraction order of solvent from small to large, final collection chloroform extraction phase also is evaporated to the ointment shape, and relative density is 0.8148g/cm
3, get argy wormwood complete stool extract.
Embodiment 55: the preparation of black nightshade complete stool extract
With embodiment 34 gained black nightshade whole strain extracts with acetic acid ethyl dissolution after, place airtight extractor, adopt liquid-liquid apportion design extraction with the benzinum solvent with 0.5: 1 ratio of volume ratio and ethyl acetate, final collection petroleum ether extraction phase also is evaporated to the ointment shape, and relative density is 0.8122g/cm
3, get black nightshade complete stool extract.
Embodiment 56: the preparation of rhizome of Chinese monkshood complete stool extract
With embodiment 35 gained rhizome of Chinese monkshood whole strain extracts with acetic acid ethyl dissolution after, place airtight extractor, adopt liquid-liquid apportion design extraction with the benzinum solvent with 0.5: 1 ratio of volume ratio and ethyl acetate, final collection petroleum ether extraction phase also is evaporated to the ointment shape, and relative density is 0.8623g/cm
3, get rhizome of Chinese monkshood complete stool extract.
Embodiment 57: the preparation of argy wormwood complete stool extract
With embodiment 36 gained argy wormwood whole strain extracts with acetic acid ethyl dissolution after, place airtight extractor, adopt liquid-liquid apportion design extraction with the benzinum solvent with 0.5: 1 ratio of volume ratio and ethyl acetate, final collection petroleum ether extraction phase also is evaporated to the ointment shape, and relative density is 0.7989g/cm
3, get argy wormwood complete stool extract.
Embodiment 58: the preparation of black nightshade complete stool extract
With embodiment 37 gained black nightshade whole strain extracts with dissolve with methanol after, place airtight extractor, adopt liquid-liquid apportion design extraction with the chloroform solvent with 0.5: 1 ratio of volume ratio and methyl alcohol, finally collect the chloroform extraction phase and be evaporated to the ointment shape, relative density is 0.8811g/cm
3, get black nightshade complete stool extract.
Embodiment 59: the preparation of rhizome of Chinese monkshood complete stool extract
With embodiment 38 gained rhizome of Chinese monkshood whole strain extracts with dissolve with methanol after, place airtight extractor, adopt liquid-liquid apportion design extraction with the chloroform solvent with 0.5: 1 ratio of volume ratio and methyl alcohol, finally collect the chloroform extraction phase and be evaporated to the ointment shape, relative density is 0.8478g/cm
3, get rhizome of Chinese monkshood complete stool extract.
Embodiment 60: the preparation of argy wormwood complete stool extract
With embodiment 39 gained argy wormwood whole strain extracts with dissolve with methanol after, place airtight extractor, adopt liquid-liquid apportion design extraction with the chloroform solvent with 0.5: 1 ratio of volume ratio and methyl alcohol, finally collect the chloroform extraction phase and be evaporated to the ointment shape, relative density is 0.8769g/cm
3, get argy wormwood complete stool extract.
Embodiment 61: the acaricidal preparation of black nightshade extract
Embodiment 13,16,22 or 28 black nightshade whole strain extract prepare miticide in following ratio
Extract 15kg
Cyclohexanone 65kg
Tween 80 1.5kg
Tea Saponin 3.0kg
Polyethenoxy ether 1.5kg
Emulsifier BP 2.5kg.
Embodiment 62: the acaricidal preparation of rhizome of Chinese monkshood extract
Embodiment 14,17,23 or 29 rhizome of Chinese monkshood whole strain extract prepare miticide in following ratio
Extract 15kg
Cyclohexanone 65kg
Tween 80 1.5kg
Tea Saponin 3.0kg
Polyethenoxy ether 1.5kg
Emulsifier BP 2.5kg.
Embodiment 63: the acaricidal preparation of biennial wormwood extract
Embodiment 15,18,24 or 30 argy wormwood whole strain extract prepare miticide in following ratio
Extract 15kg
Cyclohexanone 65kg
Tween 80 1.5kg
Tea Saponin 3.0kg
Polyethenoxy ether 1.5kg
Emulsifier BP 2.5kg.
Embodiment 64: the acaricidal preparation of black nightshade extract
Embodiment 31,34,37,40,43 or 46 black nightshade whole strain extracts prepare miticide in following ratio
Extract 14kg
Cyclohexanone 60kg
Neopelex 4kg
Tea Saponin 3kg
N-domiphen 4kg
Triphen phosphorus 2kg.
Embodiment 65: the acaricidal preparation of rhizome of Chinese monkshood extract
Embodiment 32,35,38,41,44 or 47 rhizome of Chinese monkshood whole strain extracts prepare miticide in following ratio
Extract 14kg
Cyclohexanone 60kg
Neopelex 4kg
Tea Saponin 3kg
N-domiphen 4kg
Triphen phosphorus 2kg.
Embodiment 66: the acaricidal preparation of biennial wormwood extract
Embodiment 33,36,39,42,45 or 48 argy wormwood whole strain extracts prepare miticide in following ratio
Extract 14kg
Cyclohexanone 60kg
Neopelex 4kg
Tea Saponin 3kg
N-domiphen 4kg
Triphen phosphorus 2kg.
Embodiment 67: the acaricidal preparation of black nightshade extract
Embodiment 19,25 or 49 black nightshade complete stool extracts prepare miticide in following ratio
Extract 12kg
Dimethylbenzene 55kg
Sorbierite polyoxy ether 2.0kg
6-vinyl capraldehyde 3.0kg
Lauryl sodium sulfate 2.5kg
Azone 3.0kg.
Embodiment 68: the acaricidal preparation of rhizome of Chinese monkshood extract
Embodiment 20,26 or 50 rhizome of Chinese monkshood complete stool extracts prepare miticide in following ratio
Extract 12kg
Dimethylbenzene 55kg
Sorbierite polyoxy ether 2.0kg
6-vinyl capraldehyde 3.0kg
Lauryl sodium sulfate 2.5kg
Azone 3.0kg.
Embodiment 69: the acaricidal preparation of argy wormwood extract
Embodiment 21,27 or 51 argy wormwood complete stool extracts prepare miticide in following ratio
Extract 12kg
Dimethylbenzene 55kg
Sorbierite polyoxy ether 2.0kg
6-vinyl capraldehyde 3.0kg
Lauryl sodium sulfate 2.5kg
Azone 3.0kg.
Embodiment 70: the acaricidal preparation of black nightshade extract
Embodiment 52,55 or 58 black nightshade complete stool extracts prepare miticide in following ratio
Extract 8kg
Toluene 44kg
Sorbierite polyoxy ether 5kg
Odium stearate 12kg
Azone 4kg
Methylenedioxy benzene 3kg.
Embodiment 71: the acaricidal preparation of rhizome of Chinese monkshood extract
Embodiment 53,56 or 59 rhizome of Chinese monkshood complete stool extracts prepare miticide in following ratio
Extract 8kg
Toluene 44kg
Sorbierite polyoxy ether 5kg
Odium stearate 12kg
Azone 4kg
Methylenedioxy benzene 3kg.
Embodiment 72: the acaricidal preparation of argy wormwood extract
Embodiment 54,57 or 60 argy wormwood complete stool extracts prepare miticide in following ratio
Extract 8kg
Toluene 44kg
Sorbierite polyoxy ether 5kg
Odium stearate 12kg
Azone 4kg
Methylenedioxy benzene 3kg.
Claims (10)
1, plant rhizome of Chinese monkshood active component is characterized in that this active component is to be made by one of following method:
A adopts multi-function extractor, and rhizome of Chinese monkshood complete stool is made powder, with the volume ratio of organic solvent benzinum be 1: 2-8, temperature is soaked or cold soaking 4-48 hour, filter, drying, rhizome of Chinese monkshood extract;
B adopts multi-function extractor, and the volume ratio of rhizome of Chinese monkshood powder and organic solvent ethanol is 1: 2-8, and diacolation extracts 2-8 time repeatedly, or continuous backflow extracted 4-20 hour, filters, and drying must rhizome of Chinese monkshood extract.
2, the full pearl extract of the rhizome of Chinese monkshood as claimed in claim 1 is characterized in that making that the volume ratio of rhizome of Chinese monkshood powder and ethanol is 1: 3 or 1: 5 in the full pearl extract of the rhizome of Chinese monkshood method.
3, rhizome of Chinese monkshood active component as claimed in claim 1 or 2 is characterized in that this rhizome of Chinese monkshood active component is to be made by following method:
With rhizome of Chinese monkshood extract with dissolve with methanol after, place airtight extractor, adopt liquid-liquid apportion design extraction with chloroform or benzinum solvent with 0.5: 1 ratio of volume ratio and methyl alcohol, with solvent polarity is the extraction order of solvent from small to large, and finally collecting chloroform or petroleum ether extraction phase and being evaporated to relative density is 0.5-1g/cm
3The rhizome of Chinese monkshood extract of ointment shape.
4, rhizome of Chinese monkshood active component as claimed in claim 1 or 2 is made acaricidal preparation method, it is characterized in that this method is: rhizome of Chinese monkshood extract with chloroform, methyl alcohol, cyclohexane, benzene, dimethylbenzene or alcohol solvent dissolving, can be added the extract dissolving with ratio or solubilizer, emulsifier or the suspending agent, synergist, the bleeding agent auxiliary material that suspend are made the extract miticide in the following order therein;
Extract 2-35 weight portion
Solvent 28-98 weight portion
Solubilizer 0.5-15 weight portion
Emulsifier or suspending agent 0.7-15 weight portion
Synergist 0.4-10 weight portion
Bleeding agent 0.3-8 weight portion;
Among the acaricidal preparation method, solvent is selected from a kind of in water, ethanol, methyl alcohol, acetone, cyclohexanone, toluene, dimethylbenzene, benzinum, petroleum aromatic, the purified petroleum benzin; Solubilizer be neopelex, Potassium dodecylbenzenesulfonate, polysorbate, polyethylene glycol, sorbierite polyoxy ether, lignosulfonates, tea withered, take any in the Chinese honey locust; Synergist is any in Tea Saponin, 2-C1C6H4-N=OCH3SCH3, methylenedioxy benzene derivative, 6-vinyl capraldehyde, the Octachlorodipropyl Ether; Emulsifier is any in C15～17H31～37COONa, odium stearate, lauryl sodium sulfate, N-domiphen, APEO, polyethenoxy ether, paraoctyl phenol APEO, aliphatic alcohol polyethenoxy base ether, aliphatic acid polyethenoxy base ester, the alkylaryl sulfonates; Bleeding agent is any in emulsifier BP, azone or the triphen phosphorus.
5, make acaricidal preparation method as rhizome of Chinese monkshood active component as described in the claim 3: rhizome of Chinese monkshood extract with chloroform, cyclohexane, benzene, dimethylbenzene or the dissolving of ethanol equal solvent, is added solubilizer, emulsifier and/or suspending agent, synergist with ratio, the bleeding agent auxiliary material is made the extract miticide in the following order therein;
Extract 2-30 weight portion
Solvent 25-95 weight portion
Solubilizer 0.4-15 weight portion
Emulsifier or suspending agent 0.6-15 weight portion
Synergist 0.5-9 weight portion
Bleeding agent 0.5-8 weight portion.
6, rhizome of Chinese monkshood active component as claimed in claim 1 or 2 is characterized in that wherein said organic solvent ethanol is by a kind of replacement in chloroform, 30-90 ℃ benzinum, ether, ethyl acetate, n-hexane, cyclohexane, benzene, methyl alcohol, acetone or the cyclohexanone.
7, as rhizome of Chinese monkshood active component as described in the claim 3, it is characterized in that wherein said organic solvent methyl alcohol is by a kind of replacement in chloroform, 30-90 ℃ benzinum, ether, ethyl acetate, n-hexane, cyclohexane, benzene, acetone or the cyclohexanone.
8, the application of rhizome of Chinese monkshood active component as claimed in claim 1 or 2 in the preparation miticide.
9, the application of rhizome of Chinese monkshood active component as claimed in claim 3 in the preparation miticide.
10, the application of the full pearl of the rhizome of Chinese monkshood in the preparation miticide farm chemical.
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| CN200910162504A CN101642138A (en) | 2007-07-31 | 2007-07-31 | Aconitum carmichaeli plant acaricide and preparation method thereof |
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| CN102047884A (en) * | 2010-10-20 | 2011-05-11 | 华南理工大学 | Aconitine plant source insecticidal micro emulsion and preparation method thereof |
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| CN102047884A (en) * | 2010-10-20 | 2011-05-11 | 华南理工大学 | Aconitine plant source insecticidal micro emulsion and preparation method thereof |
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