CN101779680A - Sargentodoxa cuueata vegetative acaricide and preparation method thereof - Google Patents
Sargentodoxa cuueata vegetative acaricide and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a Sargentodoxa cuueata vegetative acaricide suitable for controlling pest mites on fruit trees, vegetables and other commercial crops as well as a preparation method and application thereof. The Sargentodoxa cuueata vegetative acaricide is prepared by adding a surface active agent, an emulsifying agent, a penetrating agent, a synergistic agent and the like into the effective parts of Sargentodoxa cuueata. The Sargentodoxa cuueata vegetative acaricide has the characteristics of high efficiency, low toxicity, low remnant, harmony with environments and the like.
Description
Patent application of the present invention is for dividing an application, and the original bill application number is 200710178863.8, and the applying date is on December 6th, 2007, and denomination of invention is the achene of Siberian cocklebur, Sargent gloryvine or Osmuncla japonica vegetable miticide and preparation method thereof.
Technical field
The present invention relates to agricultural chemicals and preparation method thereof, particularly relate to botanical acaricide and preparation method thereof.
Background technology
Phytophagous mites is the important harmful mite in the agricultural production, and it has a very wide distribution, and the harm host is many, and it is big that area takes place, and medicine resistance ability is strong, and is serious and restive to the loss that agricultural production causes.At present, the research object of botanical pesticide is based on insect, and the research of mite class is less; In the at present domestic similar research, the product of existing many plant insecticides comes out, but the acaricidal Pesticidal products of plant resource is but reported less.As seen utilize the harm of biopesticide control phytophagous mites, agricultural chemicals is residual in the reduction agricultural product, and research and development pollution-free plant source miticide is extremely urgent.
Summary of the invention
The present invention adopts the method for chemical extraction, extracting from the achene of Siberian cocklebur (Xanthium sibiricum), Sargent gloryvine (Sargentodoxa cuueata) or rhizome of cyrtomium (Osmuncla japonica) complete stool respectively has the achene of Siberian cocklebur, Sargent gloryvine or the rhizome of cyrtomium complete stool active ingredient of lethal effect to the mite class, and is prepared into the plant resource miticide.Achene of Siberian cocklebur complete stool active component of the present invention can be achene of Siberian cocklebur whole strain extract or extract, and achene of Siberian cocklebur whole strain extract preparation technology is selected from one of following method:
A adopts multi-function extractor, and the volume ratio of plant achene of Siberian cocklebur complete stool powder and organic solvent ethanol is 1: 2-8 (preferred 1: 4,1: 5 or 1: 6), and temperature is soaked or cold soaking 4-24 hour, filters, and drying gets achene of Siberian cocklebur whole strain extract;
B adopts multi-function extractor, and the volume ratio of plant achene of Siberian cocklebur complete stool powder and organic solvent ethanol is 1: 2-8 (preferred 1: 4,1: 5 or 1: 6), and diacolation extracts 2-10 time repeatedly, or continuous backflow was extracted 4-24 hour, filter, drying gets achene of Siberian cocklebur whole strain extract.
Achene of Siberian cocklebur complete stool extract preparation technology: with achene of Siberian cocklebur whole strain 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 0.7: 1.5 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 0.8-1g/cm
3(preferred relative density is 0.9123g/cm to the ointment shape
3) achene of Siberian cocklebur complete stool extract.
Acaricidal preparation method: achene of Siberian cocklebur whole strain extract or 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.
Achene of Siberian cocklebur whole strain extract miticide:
Extract 5-32 weight portion
Solvent 35-95 weight portion
Solubilizer 1-30 weight portion
Emulsifier or suspending agent 2-35 weight portion
Synergist 0.5-25 weight portion
Bleeding agent 0.5-20 weight portion.
Achene of Siberian cocklebur complete stool extract miticide:
Extract 3-35 weight portion
Solvent 30-95 weight portion
Solubilizer 1-20 weight portion
Emulsifier or suspending agent 2-20 weight portion
Bleeding agent 0.5-15 weight portion
Synergist 0.5-15 weight portion.
The organic solvent of using among the described achene of Siberian cocklebur whole strain extract preparation method can also be selected from a kind of in chloroform, 30-90 ℃ benzinum, ether, ethyl acetate, n-hexane, cyclohexane, benzene, methyl alcohol, acetone, the cyclohexanone etc. non-limitingly except that ethanol.
Among the described achene of Siberian cocklebur complete stool extract preparation method, used organic solvent can also be selected from a kind of in chloroform, 30-90 ℃ benzinum, ether, ethyl acetate, n-hexane, cyclohexane, benzene, methyl alcohol, acetone, the cyclohexanone etc. non-limitingly except that ethanol.
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 xanthium sibiricum miticide is preferably:
Extract 20 weight portions
Toluene 75 weight portions
Polysorbate 3 weight portions
Tea Saponin 4 weight portions
Lauryl sodium sulfate 2.5 weight portions
Azone 1.5 weight portions.
Achene of Siberian cocklebur extract miticide is preferably:
Extract 14 weight portions
Dimethylbenzene 55 weight portions
Sorbierite polyoxy ether 4 weight portions
APEO 5 weight portions
6-vinyl capraldehyde 3 weight portions
Emulsifier BP 2 weight portions.
The present patent application also discloses a kind of Sargent gloryvine active component and miticide, and Sargent gloryvine active component and miticide and above-mentioned achene of Siberian cocklebur active component and acaricidal technical scheme are except that the raw material Sargent gloryvine is different with the achene of Siberian cocklebur, and all the other technical characterictics are identical.Finally collecting chloroform or petroleum ether extraction phase among the Sargent gloryvine complete stool extract preparation technology and being evaporated to relative density is 0.8-1g/cm
3The ointment shape, preferred relative density is 0.9143g/cm
3, get Sargent gloryvine complete stool extract.
The present patent application also discloses a kind of basket fern effective parts and miticide, and basket fern effective parts and miticide and above-mentioned achene of Siberian cocklebur active component and acaricidal technical scheme are except that the raw material rhizome of cyrtomium is different with the achene of Siberian cocklebur, and all the other technical characterictics are identical.Finally collecting chloroform or petroleum ether extraction phase among the rhizome of cyrtomium complete stool extract preparation technology and being evaporated to relative density is 0.85-1g/cm
3The ointment shape, preferred relative density is 0.9214g/cm
3, get rhizome of cyrtomium complete stool extract.
The invention provides a kind of efficient, low toxicity, low-residual, with environment and with other biological harmonious novel biopesticide, 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 the achene of Siberian cocklebur, Sargent gloryvine or rhizome of cyrtomium complete stool 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) achene of Siberian cocklebur, Sargent gloryvine or rhizome of cyrtomium complete stool 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 the achene of Siberian cocklebur, Sargent gloryvine or rhizome of cyrtomium complete stool miticide have significant miticidal effect, have the chemical pesticide characteristics of high efficiency; (4) extraction of active component is simple in the achene of Siberian cocklebur, Sargent gloryvine or the rhizome of cyrtomium complete stool, 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.
The test of experimental example 1 pharmacodynamic study
The achene of Siberian cocklebur, Sargent gloryvine or rhizome of cyrtomium whole strain extract or the extract that obtain by the present invention, standard method-slide method of recommending with reference to FAO carries out biological activity determination to the extract or the extract of the achene of Siberian cocklebur, Sargent gloryvine or rhizome of cyrtomium to the evil mite; 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, select 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 3 row, sticking 10 of every row; Temperature is (25 ± 1) ℃, place 4h in the biochemical incubator about RH85% after, use binocular vision, reject death or inactive individuality; Medicament dilutes 3-5 concentration on the basis of prerun, a 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 three plant species extracts are to Tetranychus cinnabarinus (Teranychus cinnabarinus) miticidal effect
Table 2 three plant species extracts are to Tetranychus cinnabarinus (Teranychus cinnabarinus) toxic effect
The result shows: the acaricidal rate of the extract of three plant species or extract knot Tetranychus cinnabarinus and poisoning rate all level reach more than 85%, the poisoning rate of Sargent gloryvine extract is lower slightly, but also nearly 80%, along with the extract of three plant species or the reduction of extract concentration, its miticidal effect and toxic effect decrease, but the lethality of acarid is still about 50%.This shows that the whole strain extract of the achene of Siberian cocklebur of the present invention, Sargent gloryvine or rhizome of cyrtomium or the miticidal effect of extract are remarkable.
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 50 of female one-tenth mites, place under (25 ± 1) ℃ and let alone the 24h of laying eggs, remove female one-tenth mite, behind the inspection record ovum grain number, place (25 ± 1) ℃ constant incubator, when ovum reaches 36-48h age, measure, soup 5s is respectively handled in the blade immersion of band ovum, 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 to add up and respectively handle lethality, the achene of Siberian cocklebur, Sargent gloryvine and rhizome of cyrtomium complete stool extract kill the ovum effect and see Table 3:
Table 3 three plant species extracts are to the active effect of Tetranychus cinnabarinus (Teranychus cinnabarinus) ovum
The result shows: three plant species extracts all can reach 60% to the poisoning rate of Tetranychus cinnabarinus ovum, and wherein achene of Siberian cocklebur extract can reach 70% to the poisoning rate of Tetranychus cinnabarinus ovum, prove that three plant species extracts are remarkable to the toxic effect of mite 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 three plant species extracts are to the antifeedant activity effect of Tetranychus cinnabarinus (Teranychus cinnabarinus)
The result shows: three plant species extracts are obvious to the antifeedant activity effect of Tetranychus cinnabarinus, to slightly strong if the food refusal rate of mite is compared into the food refusal rate of mite, all can reach more than 70%, wherein achene of Siberian cocklebur extract can reach more than 80% the food refusal rate of Tetranychus cinnabarinus, prove the present invention's three plant species extracts to if mite with become mite that stronger antifeedant activity effect is all arranged.
Experimental example 2 is compared with disclosed extraction process, and active component that this technology 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 three plant species to Tetranychus cinnabarinus (Teranychus cinnabarinus) active substance
Annotate: A: be the action effect of active component that this technology is carried (extract or extract), B: be the action effect of active component that disclosed technology is carried
The result shows: compare with disclosed existing technology, with the extract of three plant species of extraction process of the present invention preparation or extract the toxic action and the food refusal effect of Tetranychus cinnabarinus all there is remarkable result, the ovicidal rate that technology of the present invention is extracted active component can reach 60%, the acaricidal rate that open technology is extracted active component only about 40%; The food refusal rate that technology of the present invention is extracted active component can reach the openly twice of the food refusal rate of getting active component of technology, proves, the active component of extraction process preparation of the present invention has significant acaricidal rate and food refusal rate.
The following embodiment of the present invention all can realize the effect of above-mentioned experimental example.
Embodiment
Embodiment 1:
Achene of Siberian cocklebur complete stool is cleaned, dried in the shade, grind the back and cross the 40-60 mesh sieve in the ventilation; Plant powder after pulverizing is put into multi-function extractor, extract with the benzinum of 5 times of volumes of plant powder, collection Petroleum ether extraction phase, concentrating under reduced pressure gets extract; Get extract 20kg and add toluene 75kg, add and have in the mixing kettle of agitator and thermometer, under 50 ℃, mixed 1.5 hours, add tween (polysorbate) 3kg, 6-vinyl capraldehyde 4kg, lauryl sodium sulfate 2.5kg, emulsifier BP 1.5kg, mix, obtain achene of Siberian cocklebur whole strain extract miticide missible oil.
Embodiment 2:
As the method for embodiment 1, make Caulis Sargentodoxae extract miticide missible oil.
Embodiment 3:
As the method for embodiment 1, make Rhizoma Osmundae extract miticide missible oil.
Embodiment 4:
Achene of Siberian cocklebur complete stool is cleaned,, ground the back and cross 60 mesh sieves in 45 ℃ of oven dry down; Plant powder after pulverizing is put into multi-function extractor, extract with the chloroform of 4 times of volumes, collection chloroform extraction phase, concentrating under reduced pressure gets extract; Get extract 14kg and add dimethylbenzene 55kg, add and have in the mixing kettle of agitator and thermometer, under 60 ℃, mixed 3 hours, add polyethylene glycol 4kg, Tea Saponin 5kg, paraoctyl phenol APEO 3kg, azone 2kg, mix, obtain achene of Siberian cocklebur whole strain extract miticide missible oil.
Embodiment 5:
As the method for embodiment 4, make Sargent gloryvine whole strain extract miticide missible oil.
Embodiment 6:
As the method for embodiment 4, make rhizome of cyrtomium whole strain extract miticide missible oil.
Embodiment 7:
Achene of Siberian cocklebur complete stool is cleaned,, ground the back and cross 60 mesh sieves in 40 ℃ of oven dry down; Plant powder after pulverizing is put into multi-function extractor, extract with the chloroform of 6 times of volumes, collection chloroform extraction phase, concentrating under reduced pressure gets extract; Get extract 17kg and add dimethylbenzene 80kg, add and have in the mixing kettle of agitator and thermometer, under 60 ℃, mixed 2 hours, adding neopelex 7kg, 6-vinyl capraldehyde 4kg, paraoctyl phenol APEO 2kg, azone 2kg mix, and obtain achene of Siberian cocklebur whole strain extract miticide missible oil.
Embodiment 8:
As the method for embodiment 7, make Sargent gloryvine whole strain extract miticide missible oil.
Embodiment 9:
As the method for embodiment 7, make rhizome of cyrtomium whole strain extract miticide missible oil.
Embodiment 10:
Adopting multi-function extractor, is 1: 4 with the volume ratio of achene of Siberian cocklebur complete stool and organic solvent ethanol, mac per hor X, and filtration, drying must achene of Siberian cocklebur whole strain extract; With gained achene of Siberian cocklebur whole strain extract with dissolve with methanol after, place airtight extractor, adopt liquid-liquid apportion design extraction with the benzinum solvent with 0.7: 1.5 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 0.9123g/cm
3, get achene of Siberian cocklebur complete stool extract; After getting achene of Siberian cocklebur complete stool extract 12kg usefulness benzinum 60kg dissolving, injection has the mixing kettle of agitator and thermometer, under 30 ℃, mixed 2 hours, adding polysorbate with ratio in the following order is 4kg, odium stearate 3kg, Tea Saponin 2kg and azone 3kg, makes achene of Siberian cocklebur complete stool extract miticide missible oil.
Embodiment 11:
As the method for embodiment 10, make Sargent gloryvine complete stool extract miticide missible oil.
Embodiment 12:
As the method for embodiment 10, make rhizome of cyrtomium complete stool extract miticide missible oil.
Embodiment 13: the preparation of achene of Siberian cocklebur whole strain extract
Adopting multi-function extractor, is 1: 5 with the volume ratio of achene of Siberian cocklebur complete stool and organic solvent ethanol, and temperature was soaked 10 hours, filtration, and drying must achene of Siberian cocklebur whole strain extract.
Embodiment 14: the preparation of Sargent gloryvine whole strain extract
As the method for embodiment 13, make the Sargent gloryvine whole strain extract.
Embodiment 15: the preparation of rhizome of cyrtomium whole strain extract
As the method for embodiment 13, make the rhizome of cyrtomium whole strain extract.
Embodiment 16: the preparation of achene of Siberian cocklebur whole strain extract
Adopting multi-function extractor, is 1: 4 with the volume ratio of achene of Siberian cocklebur complete stool powder and organic solvent-normal hexane, and diacolation extracts 8 times repeatedly, filtration, and drying must achene of Siberian cocklebur whole strain extract.
Embodiment 17: the preparation of Sargent gloryvine whole strain extract
As the method for embodiment 16, make the Sargent gloryvine whole strain extract.
Embodiment 18: the preparation of rhizome of cyrtomium whole strain extract
As the method for embodiment 16, make the rhizome of cyrtomium whole strain extract.
Embodiment 19: the preparation of achene of Siberian cocklebur complete stool extract
With embodiment 13,16 gained achene of Siberian cocklebur whole strain extracts with dissolve with methanol after, place airtight extractor, adopt liquid-liquid apportion design extraction with the chloroform solvent with 0.7: 1.5 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 0.9123g/cm
3, get achene of Siberian cocklebur complete stool extract.
Embodiment 20: the preparation of Sargent gloryvine complete stool extract
With embodiment 14,17 gained Sargent gloryvine whole strain extracts with dissolve with methanol after, place airtight extractor, adopt liquid-liquid apportion design extraction with the chloroform solvent with 0.7: 1.5 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 Sargent gloryvine 0.9143g/cm
3, get Sargent gloryvine complete stool extract.
Embodiment 21: the preparation of rhizome of cyrtomium complete stool extract
With embodiment 15,18 gained rhizome of cyrtomium whole strain extracts with dissolve with methanol after, place airtight extractor, adopt liquid-liquid apportion design extraction with the chloroform solvent with 0.7: 1.5 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 rhizome of cyrtomium rattan 0.9143g/cm
3, get rhizome of cyrtomium complete stool extract.
Embodiment 22: the preparation of achene of Siberian cocklebur whole strain extract
Adopting multi-function extractor, is 1: 6 with the volume ratio of achene of Siberian cocklebur complete stool powder and organic solvent ethyl acetate, and continuous backflow was extracted 20 hours, filtered, and drying must achene of Siberian cocklebur whole strain extract.
Embodiment 23: the preparation of Sargent gloryvine whole strain extract
As the method for embodiment 22, make the Sargent gloryvine whole strain extract.
Embodiment 24: the preparation of rhizome of cyrtomium whole strain extract
As the method for embodiment 22, make the rhizome of cyrtomium whole strain extract.
Embodiment 25: the preparation of achene of Siberian cocklebur complete stool extract
With the achene of Siberian cocklebur 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 0.7: 1.5 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 0.9123g/cm
3, get achene of Siberian cocklebur complete stool extract.
Embodiment 26: the preparation of Sargent gloryvine complete stool extract
With the Sargent gloryvine 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 0.7: 1.5 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 0.9143g/cm
3, get Sargent gloryvine complete stool extract.
Embodiment 27: the preparation of rhizome of cyrtomium complete stool extract
With the rhizome of cyrtomium 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 0.7: 1.5 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 0.9143g/cm
3, get rhizome of cyrtomium complete stool extract.
Embodiment 28: the preparation of achene of Siberian cocklebur whole strain extract
Adopting multi-function extractor, is 1: 4 with the volume ratio of achene of Siberian cocklebur complete stool powder and organic solvent ether, mac per hor X, and filtration, drying must achene of Siberian cocklebur whole strain extract.
Embodiment 29: the preparation of Sargent gloryvine whole strain extract
As the method for embodiment 28, make the Sargent gloryvine whole strain extract.
Embodiment 30: the preparation of rhizome of cyrtomium whole strain extract
As the method for embodiment 28, make the rhizome of cyrtomium whole strain extract.
Embodiment 31: the preparation of achene of Siberian cocklebur whole strain extract
Adopting multi-function extractor, is 1: 6 with the volume ratio of achene of Siberian cocklebur complete stool powder and organic solvent methyl alcohol, and temperature was soaked 20 hours, filtration, and drying must achene of Siberian cocklebur whole strain extract.
Embodiment 32: the preparation of Sargent gloryvine whole strain extract
As the method for embodiment 31, make the Sargent gloryvine whole strain extract.
Embodiment 33: the preparation of rhizome of cyrtomium whole strain extract
As the method for embodiment 31, make the rhizome of cyrtomium whole strain extract.
Embodiment 34: the preparation of achene of Siberian cocklebur whole strain extract
Adopting multi-function extractor, is 1: 5 with the volume ratio of achene of Siberian cocklebur complete stool powder and organic solvent ethyl acetate, and temperature was soaked 10 hours, filtration, and drying must achene of Siberian cocklebur whole strain extract.
Embodiment 35: the preparation of Sargent gloryvine whole strain extract
As the method for embodiment 34, make the Sargent gloryvine whole strain extract.
Embodiment 36: the preparation of rhizome of cyrtomium whole strain extract
As the method for embodiment 34, make the rhizome of cyrtomium whole strain extract.
Embodiment 37: the preparation of achene of Siberian cocklebur whole strain extract
Adopting multi-function extractor, is 1: 4 with the volume ratio of achene of Siberian cocklebur complete stool powder and organic solvent-benzene, and diacolation extracts 5 times repeatedly, filtration, and drying must achene of Siberian cocklebur whole strain extract.
Embodiment 38: the preparation of Sargent gloryvine whole strain extract
As the method for embodiment 37, make the Sargent gloryvine whole strain extract.
Embodiment 39: the preparation of rhizome of cyrtomium whole strain extract
As the method for embodiment 37, make the rhizome of cyrtomium whole strain extract.
Embodiment 40: the preparation of achene of Siberian cocklebur whole strain extract
Adopting multi-function extractor, is 1: 5 with the volume ratio of achene of Siberian cocklebur complete stool powder and organic solvent-acetone, and continuous backflow was extracted 10 hours, filtration, and drying must achene of Siberian cocklebur whole strain extract.
Embodiment 41: the preparation of Sargent gloryvine whole strain extract
As the method for embodiment 39, make the Sargent gloryvine whole strain extract.
Embodiment 42: the preparation of rhizome of cyrtomium whole strain extract
As the method for embodiment 39, make the rhizome of cyrtomium whole strain extract.
Embodiment 43: the preparation of achene of Siberian cocklebur whole strain extract
Adopting multi-function extractor, is 1: 6 with the volume ratio of achene of Siberian cocklebur complete stool powder and organic solvent-normal hexane, and diacolation extracts 3 times repeatedly, filtration, and drying must achene of Siberian cocklebur whole strain extract.
Embodiment 44: the preparation of Sargent gloryvine whole strain extract
As the method for embodiment 42, make the Sargent gloryvine whole strain extract.
Embodiment 45: the preparation of rhizome of cyrtomium whole strain extract
As the method for embodiment 42, make the rhizome of cyrtomium whole strain extract.
Embodiment 46: the preparation of achene of Siberian cocklebur whole strain extract
Adopting multi-function extractor, is 1: 5 with the volume ratio of achene of Siberian cocklebur complete stool powder and organic solvent ethyl acetate, and continuous backflow was extracted 18 hours, filtration, and drying must achene of Siberian cocklebur whole strain extract.
Embodiment 47: the preparation of Sargent gloryvine whole strain extract
As the method for embodiment 45, make the Sargent gloryvine whole strain extract.
Embodiment 48: the preparation of rhizome of cyrtomium whole strain extract
As the method for embodiment 45, make the rhizome of cyrtomium whole strain extract.
Embodiment 49: the preparation of achene of Siberian cocklebur complete stool extract
Behind 30-90 ℃ of petroleum ether dissolution of embodiment 28 gained achene of Siberian cocklebur whole strain extracts usefulness, place airtight extractor, adopt with 0.7: 1.5 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 0.9123g/cm
3, get achene of Siberian cocklebur complete stool extract.
Embodiment 50: the preparation of Sargent gloryvine complete stool extract
Behind 30-90 ℃ of petroleum ether dissolution of embodiment 29 gained Sargent gloryvine whole strain extracts usefulness, place airtight extractor, adopt with 0.7: 1.5 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 0.9143g/cm
3, get Sargent gloryvine complete stool extract.
Embodiment 51: the preparation of rhizome of cyrtomium complete stool extract
Behind 30-90 ℃ of petroleum ether dissolution of embodiment 30 gained rhizome of cyrtomium whole strain extracts usefulness, place airtight extractor, adopt with 0.7: 1.5 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 0.9143g/cm
3, get rhizome of cyrtomium complete stool extract.
Embodiment 52: the preparation of achene of Siberian cocklebur complete stool extract
With embodiment 31 gained achene of Siberian cocklebur whole strain extracts with dissolve with ethanol after, place airtight extractor, adopt liquid-liquid apportion design extraction with the chloroform solvent with 0.7: 1.5 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 0.9123g/cm
3, get achene of Siberian cocklebur complete stool extract.
Embodiment 53: the preparation of Sargent gloryvine complete stool extract
With embodiment 32 gained Sargent gloryvine whole strain extracts with dissolve with ethanol after, place airtight extractor, adopt liquid-liquid apportion design extraction with the chloroform solvent with 0.7: 1.5 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 0.9143g/cm
3, get Sargent gloryvine complete stool extract.
Embodiment 54: the preparation of rhizome of cyrtomium complete stool extract
With embodiment 33 gained rhizome of cyrtomium whole strain extracts with dissolve with ethanol after, place airtight extractor, adopt liquid-liquid apportion design extraction with the chloroform solvent with 0.7: 1.5 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 0.9143g/cm
3, get rhizome of cyrtomium complete stool extract.
Embodiment 55: the preparation of achene of Siberian cocklebur complete stool extract
With embodiment 34 gained achene of Siberian cocklebur whole strain extracts with acetic acid ethyl dissolution after, place airtight extractor, adopt liquid-liquid apportion design extraction with the benzinum solvent with 0.7: 1.5 ratio of volume ratio and ethyl acetate, final collection petroleum ether extraction phase also is evaporated to the ointment shape, and relative density is 0.9123g/cm
3, get achene of Siberian cocklebur complete stool extract.
Embodiment 56: the preparation of Sargent gloryvine complete stool extract
With embodiment 35 gained Sargent gloryvine whole strain extracts with acetic acid ethyl dissolution after, place airtight extractor, adopt liquid-liquid apportion design extraction with the benzinum solvent with 0.7: 1.5 ratio of volume ratio and ethyl acetate, final collection petroleum ether extraction phase also is evaporated to the ointment shape, and relative density is 0.9143g/cm
3, get Sargent gloryvine complete stool extract.
Embodiment 57: the preparation of rhizome of cyrtomium complete stool extract
With embodiment 36 gained rhizome of cyrtomium whole strain extracts with acetic acid ethyl dissolution after, place airtight extractor, adopt liquid-liquid apportion design extraction with the benzinum solvent with 0.7: 1.5 ratio of volume ratio and ethyl acetate, final collection petroleum ether extraction phase also is evaporated to the ointment shape, and relative density is 0.9143g/cm
3, get rhizome of cyrtomium complete stool extract.
Embodiment 58: the preparation of achene of Siberian cocklebur complete stool extract
With embodiment 37 gained achene of Siberian cocklebur whole strain extracts with dissolve with methanol after, place airtight extractor, adopt liquid-liquid apportion design extraction with the chloroform solvent with 0.7: 1.5 ratio of volume ratio and methyl alcohol, finally collect the chloroform extraction phase and be evaporated to the ointment shape, relative density is 0.9143g/cm
3, get achene of Siberian cocklebur complete stool extract.
Embodiment 59: the preparation of Sargent gloryvine complete stool extract
With embodiment 38 gained Sargent gloryvine whole strain extracts with dissolve with methanol after, place airtight extractor, adopt liquid-liquid apportion design extraction with the chloroform solvent with 0.7: 1.5 ratio of volume ratio and methyl alcohol, finally collect the chloroform extraction phase and be evaporated to the ointment shape, relative density is 0.9123g/cm
3, get Sargent gloryvine complete stool extract.
Embodiment 60: the preparation of rhizome of cyrtomium complete stool extract
With embodiment 39 gained rhizome of cyrtomium whole strain extracts with dissolve with methanol after, place airtight extractor, adopt liquid-liquid apportion design extraction with the chloroform solvent with 0.7: 1.5 ratio of volume ratio and methyl alcohol, finally collect the chloroform extraction phase and be evaporated to the ointment shape, relative density is 0.9123g/cm
3, get rhizome of cyrtomium complete stool extract.
Embodiment 61: the acaricidal preparation of xanthium sibiricum
Embodiment 13,16,22 or 28 achene of Siberian cocklebur whole strain extract prepare miticide in following ratio
Extract 20kg
Toluene 75kg
Polysorbate 3kg
Tea Saponin 4kg
Lauryl sodium sulfate 2.5kg
Azone 1.5kg.
Embodiment 62: the acaricidal preparation of Caulis Sargentodoxae extract
Embodiment 14,17,23 or 29 Sargent gloryvine whole strain extract prepare miticide in following ratio
Extract 20kg
Toluene 75kg
Polysorbate 3kg
Tea Saponin 4kg
Lauryl sodium sulfate 2.5kg
Azone 1.5kg.
Embodiment 63: the acaricidal preparation of Rhizoma Osmundae extract
Embodiment 15,18,24 or 30 rhizome of cyrtomium whole strain extract prepare miticide in following ratio
Extract 20kg
Toluene 75kg
Polysorbate 3kg
Tea Saponin 4kg
Lauryl sodium sulfate 2.5kg
Azone 1.5kg.
Embodiment 64: the acaricidal preparation of xanthium sibiricum
Embodiment 31,34,37 or 40 achene of Siberian cocklebur whole strain extract prepare miticide in following ratio
Extract 30kg
Acetone 60kg
Polyethylene glycol 5kg
6-vinyl capraldehyde 10kg
N-domiphen 5kg
Triphen phosphorus 5kg.
Embodiment 65: the acaricidal preparation of Caulis Sargentodoxae extract
Embodiment 32,35,38 or 41 Sargent gloryvine whole strain extract prepare miticide in following ratio
Extract 30kg
Acetone 60kg
Polyethylene glycol 5kg
6-vinyl capraldehyde 10kg
N-domiphen 5kg
Triphen phosphorus 5kg.
Embodiment 66: the acaricidal preparation of Rhizoma Osmundae extract
Embodiment 33,36,39 or 42 rhizome of cyrtomium whole strain extract prepare miticide in following ratio
Extract 30kg
Acetone 60kg
Polyethylene glycol 5kg
6-vinyl capraldehyde 10kg
N-domiphen 5kg
Triphen phosphorus 5kg.
Embodiment 67: the acaricidal preparation of achene of Siberian cocklebur extract
Embodiment 19,25 or 49 achene of Siberian cocklebur complete stool extract prepare miticide in following ratio
Extract 14kg
Dimethylbenzene 55kg
Sorbierite polyoxy ether 4kg
APEO 5kg
6-vinyl capraldehyde 3kg
Emulsifier BP 2kg.
Embodiment 68: the acaricidal preparation of Sargent gloryvine extract
Embodiment 20,26 or 50 Sargent gloryvine complete stool extract prepare miticide in following ratio
Extract 14kg
Dimethylbenzene 55kg
Sorbierite polyoxy ether 4kg
APEO 5kg
6-vinyl capraldehyde 3kg
Emulsifier BP 2kg.
Embodiment 69: the acaricidal preparation of rhizome of cyrtomium extract
Embodiment 21,27 or 51 rhizome of cyrtomium complete stool extract prepare miticide in following ratio
Extract 14kg
Dimethylbenzene 55kg
Sorbierite polyoxy ether 4kg
APEO 5kg
6-vinyl capraldehyde 3kg
Emulsifier BP 2kg.
Embodiment 70: the acaricidal preparation of achene of Siberian cocklebur extract
Embodiment 52,55 or 58 achene of Siberian cocklebur complete stool extract prepare miticide in following ratio
Extract 30kg
Cyclohexanone 60kg
Polyethylene glycol 12kg
Paraoctyl phenol APEO 3kg
Octachlorodipropyl Ether 10kg
Triphen phosphorus 5kg.
Embodiment 71: the acaricidal preparation of Sargent gloryvine extract
Embodiment 53,56 or 59 Sargent gloryvine complete stool extract prepare miticide in following ratio
Extract 30kg
Cyclohexanone 60kg
Polyethylene glycol 12kg
Paraoctyl phenol APEO 3kg
Octachlorodipropyl Ether 10kg
Triphen phosphorus 5kg.
Embodiment 72: the acaricidal preparation of rhizome of cyrtomium extract
Embodiment 54,57 or 60 rhizome of cyrtomium complete stool extract prepare miticide in following ratio
Extract 30kg
Cyclohexanone 60kg
Polyethylene glycol 12kg
Paraoctyl phenol APEO 3kg
Octachlorodipropyl Ether 10kg
Triphen phosphorus 5kg.
Claims (10)
1. plant Sargent gloryvine active component is characterized in that this active component is to be made by one of following method:
A adopts multi-function extractor, and the volume ratio of plant Sargent gloryvine complete stool powder and organic solvent ethanol is 1: 2-8, and temperature is soaked or cold soaking 4-24 hour, filters, and drying gets the Sargent gloryvine whole strain extract;
B adopts multi-function extractor, and the volume ratio of plant Sargent gloryvine complete stool powder and organic solvent ethanol is 1: 2-8, and diacolation extracts 2-10 time repeatedly, or continuous backflow extracted 4-24 hour, filters, and drying must the Sargent gloryvine whole strain extract.
2. Sargent gloryvine active component as claimed in claim 1 is characterized in that making that the volume ratio of Sargent gloryvine powder and ethanol is 1: 4 in the Sargent gloryvine active component method, 1: 5 or 1: 6.
3. Sargent gloryvine active component as claimed in claim 1 or 2 is characterized in that this Sargent gloryvine active component is to be made by following method:
With the Sargent gloryvine whole strain extract with dissolve with methanol after, place airtight extractor, adopt liquid-liquid apportion design extraction with chloroform or benzinum solvent with 0.7: 1.5 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 0.8-1g/cm
3The Sargent gloryvine complete stool extract of ointment shape.
4. Sargent gloryvine active component as claimed in claim 1 or 2 is made acaricidal preparation method, it is characterized in that this method is: the full pearl extract of Sargent gloryvine with chloroform, methyl alcohol, cyclohexane, benzene, dimethylbenzene or alcohol solvent dissolving, can be added solubilizer, emulsifier and/or the suspending agent, synergist, the bleeding agent auxiliary material that promote extract to dissolve or suspend therein with ratio in the following order and makes the extract miticide;
Extract 5-32 weight portion
Solvent 35-95 weight portion
Solubilizer 1-30 weight portion
Emulsifier or suspending agent 2-35 weight portion
Synergist 0.5-25 weight portion
Bleeding agent 0.5-20 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 Sargent gloryvine active component as described in the claim 3, it is characterized in that this method is: the full pearl extract of Sargent gloryvine 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 3-35 weight portion
Solvent 30-95 weight portion
Solubilizer 1-20 weight portion
Emulsifier or suspending agent 2-20 weight portion
Bleeding agent 0.5-15 weight portion
Synergist 0.5-15 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.
6. Sargent gloryvine 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, n-hexane, cyclohexane, benzene, ethyl acetate, methyl alcohol, acetone or the cyclohexanone.
7. as Sargent gloryvine 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, n-hexane, cyclohexane, benzene, ethyl acetate, acetone or the cyclohexanone.
8. the application of Sargent gloryvine active component as claimed in claim 1 or 2 in the preparation miticide.
9. the application of Sargent gloryvine active component as claimed in claim 3 in the preparation miticide.
10. the application of the full pearl of Sargent gloryvine in the preparation miticide farm chemical.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103340219A (en) * | 2013-07-18 | 2013-10-09 | 奉节县瑞康中药材种植有限公司 | Chinese herbal medicine pesticide and preparation method thereof |
| CN110100846A (en) * | 2019-06-15 | 2019-08-09 | 李钟� | A kind of production method that can trap and kill acarid |
| CN111771888A (en) * | 2020-08-11 | 2020-10-16 | 四川农业大学 | Application of plant resistance inducer containing sargentgloryvine stem polysaccharide in preventing plant diseases |
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| CN1082817A (en) * | 1993-08-25 | 1994-03-02 | 薛永宏 | Chinese herbal medicine insecticide and leach extraction method thereof |
| CN1149962A (en) * | 1995-11-13 | 1997-05-21 | 吴黎明 | Biological inactivator for snail and schistosome |
| CN1150938C (en) * | 2002-11-28 | 2004-05-26 | 贵州安泰药业有限公司 | Capsule for treating gynaecologic inflammation, and its prepn. process |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103340219A (en) * | 2013-07-18 | 2013-10-09 | 奉节县瑞康中药材种植有限公司 | Chinese herbal medicine pesticide and preparation method thereof |
| CN110100846A (en) * | 2019-06-15 | 2019-08-09 | 李钟� | A kind of production method that can trap and kill acarid |
| CN111771888A (en) * | 2020-08-11 | 2020-10-16 | 四川农业大学 | Application of plant resistance inducer containing sargentgloryvine stem polysaccharide in preventing plant diseases |
| CN111771888B (en) * | 2020-08-11 | 2021-05-14 | 四川农业大学 | Application of plant resistance inducer containing sargentgloryvine stem polysaccharide in preventing plant diseases |
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