CN101595895A - Amorpha fruticosa plant miticide and preparation method thereof - Google Patents
Amorpha fruticosa plant miticide and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of plant acaricide that is applicable to evil mite on the economic crops such as control fruit tree, vegetables and its production and use, it adds surfactant, emulsifier, bleeding agent, synergist etc. by plant shrubby flase indigo (Amorpha fruticosa) active component makes, have efficient, low toxicity, low-residual, with characteristics such as environment harmony.
Description
Patent application of the present invention is for dividing an application, and the original bill application number is 200710119721.4, and the applying date is on July 31st, 2007, and denomination of invention is Java brucea, fructus gleditsiae or amorpha fruticosa plant miticide and preparation method thereof.
Technical field
The present invention relates to a kind of agricultural chemicals and preparation method thereof, particularly relate to botanical acaricide and preparation method thereof.
Background technology
Phytophagous mites is the important pest 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.The negative effect that chemical control brought is well-known.At present, the research object of botanical pesticide is based on insect, and the research of mite class does not almost have; In the at present domestic similar research, the product of existing many plant insecticides comes out, but the acaricidal Pesticidal products of plant resource does not but appear in the newspapers.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, and extracting from Java brucea, fructus gleditsiae or shrubby flase indigo complete stool has Java brucea, fructus gleditsiae or the shrubby flase indigo complete stool active ingredient of lethal effect to the mite class, and is prepared into the plant resource miticide.
Java brucea complete stool active component of the present invention can be Java brucea whole strain extract or extract, and Java brucea whole strain extract preparation technology is selected from one of following method:
A adopts multi-function extractor, and plant Java brucea complete stool is made powder, with the volume ratio of organic solvent ethanol be 1: 2-8, preferred 1: 4,1: 5 or 1: 6, temperature was soaked or cold soaking 4-24 hour, filter, drying, the Java brucea whole strain extract;
B adopts multi-function extractor, and the volume ratio of plant Java brucea complete stool powder and organic solvent ethanol is 1: 2-8, preferred 1: 4,1: 5 or 1: 6, diacolation extracts 2-10 time repeatedly, or continuous backflow was extracted filtration 4-24 hour, drying gets the Java brucea whole strain extract.
Java brucea complete stool extract preparation technology: with Java brucea 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
3The ointment shape, preferred relative density is Java brucea 0.9242g/cm
3, get Java brucea complete stool extract.
Acaricidal preparation method:, add solubilizer, emulsifier and/or the suspending agent, synergist, the bleeding agent that promote extract or extract to dissolve or suspend therein with ratio in the following order and make miticide with Java brucea whole strain extract or extract dissolution with solvents.
Java brucea whole strain extract miticide:
Extract: 5-35 weight portion
Solvent: 30-95 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
Java brucea complete stool extract miticide:
Extract: 3-30 weight portion
Solvent: 30-90 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 Java brucea whole strain extract preparation method can also be selected from except that ethanol non-limitingly: a kind of in chloroform, 30-90 ℃ benzinum, ether, ethyl acetate, n-hexane, cyclohexane, benzene, methyl alcohol, acetone or the cyclohexanone etc.
Among the described Java brucea complete stool extract preparation method, used organic solvent can also be selected from except that ethanol non-limitingly: a kind of in chloroform, 30-90 ℃ benzinum, ether, ethyl acetate, n-hexane, cyclohexane, benzene, methyl alcohol, acetone or the cyclohexanone etc.
Among the acaricidal preparation method, solvent is selected from a kind of in water, ethanol, methyl alcohol, acetone, cyclohexanone, toluene, dimethylbenzene, benzinum, petroleum aromatic or the purified petroleum benzin; Solubilizer is neopelex, Potassium dodecylbenzenesulfonate, polysorbate, polyethylene glycol, sorbierite polyoxy ether, lignosulfonates, tea is withered or take any in the Chinese honey locust; Synergist is any in Tea Saponin, 2-C1C6H4-N=OCH3SCH3, methylenedioxy benzene derivative, 6-vinyl capraldehyde or 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 or the alkylaryl sulfonates; Bleeding agent is any in emulsifier BP, azone or the triphen phosphorus.
The Fructus Bruceae extract miticide is preferably:
Extract: 15 weight portions
Toluene: 70 weight portions
Polysorbate: 3 weight portions
Tea Saponin: 4 weight portions
Lauryl sodium sulfate: 2.5 weight portions
Azone: 1.5 weight portions
Java brucea extract miticide is preferably:
Extract: 12 weight portions
Dimethylbenzene: 65 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 fructus gleditsiae active component and miticide, and fructus gleditsiae active component and miticide and above-mentioned Java brucea active component and acaricidal technical scheme are except that the raw material fructus gleditsiae is different with Java brucea, 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 relative density 0.8998g/cm among the fructus gleditsiae complete stool extract preparation technology
3
The present patent application also discloses a kind of shrubby flase indigo active component and miticide, and shrubby flase indigo active component and miticide and above-mentioned Java brucea active component and acaricidal technical scheme are except that the raw material shrubby flase indigo is different with Java brucea, 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 relative density 0.9365g/cm among the shrubby flase indigo 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 Java brucea, fructus gleditsiae or shrubby flase indigo 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) Java brucea, fructus gleditsiae or shrubby flase indigo 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 Java brucea, fructus gleditsiae or shrubby flase indigo complete stool miticide have significant miticidal effect, have the chemical pesticide characteristics of high efficiency; (4) extraction of active component is simple in Java brucea, fructus gleditsiae or the shrubby flase indigo 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
By Java brucea, fructus gleditsiae or shrubby flase indigo whole strain extract or 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 urticaes; 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 urticae (Teranychus urticae) miticidal effect
Table 2 three plant species extracts 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 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, Java brucea, fructus gleditsiae or shrubby flase indigo complete stool extract kill the ovum effect and see Table 3.
Table 3 three plant species extracts 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 three plant species extracts are to the antifeedant activity effect of Tetranychus urticae
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 activity
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 (extract or extract)
Following embodiment all can realize the effect of above-mentioned experimental example.
Embodiment
Embodiment 1:
The Java brucea 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 15kg and add toluene 70kg, 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 Java brucea whole strain extract miticide missible oil.
Embodiment 2:
The fructus gleditsiae 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 15kg and add toluene 70kg, 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 fructus gleditsiae whole strain extract miticide missible oil.
Embodiment 3:
The shrubby flase indigo 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 15kg and add toluene 70kg, 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 shrubby flase indigo whole strain extract miticide missible oil.
Embodiment 4:
The Java brucea 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 12kg and add dimethylbenzene 65kg, 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 Java brucea whole strain extract miticide missible oil.
Embodiment 5:
The fructus gleditsiae 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 12kg and add dimethylbenzene 65kg, 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 fructus gleditsiae whole strain extract miticide missible oil.
Embodiment 6:
The shrubby flase indigo 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 12kg and add dimethylbenzene 65kg, 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 shrubby flase indigo whole strain extract miticide missible oil.
Embodiment 7:
The Java brucea 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 18kg and add dimethylbenzene 75kg, add and have in the mixing kettle of agitator and thermometer, under 60 ℃, mixed 2 hours, adding neopelex 10kg, 6-vinyl capraldehyde 3kg, paraoctyl phenol APEO 4kg, azone 1kg mix, and obtain Java brucea whole strain extract miticide missible oil.
Embodiment 8:
The fructus gleditsiae 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 18kg and add dimethylbenzene 75kg, add and have in the mixing kettle of agitator and thermometer, under 60 ℃, mixed 2 hours, adding neopelex 10kg, 6-vinyl capraldehyde 3kg, paraoctyl phenol APEO 4kg, azone 1kg mix, and obtain fructus gleditsiae whole strain extract miticide missible oil.
Embodiment 9:
The shrubby flase indigo 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 18kg and add dimethylbenzene 75kg, add and have in the mixing kettle of agitator and thermometer, under 60 ℃, mixed 2 hours, adding neopelex 10kg, 6-vinyl capraldehyde 3kg, paraoctyl phenol APEO 4kg, azone 1kg mix, and obtain shrubby flase indigo whole strain extract miticide missible oil.
Embodiment 10:
Adopting multi-function extractor, is 1: 4 with the volume ratio of Java brucea complete stool and organic solvent ethanol, mac per hor X, and filtration, drying must the Java brucea whole strain extract; The Java brucea 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 0.9286g/cm
3, get Java brucea complete stool extract; After getting Java brucea complete stool extract 7kg usefulness benzinum 50kg dissolving, injection has the mixing kettle of agitator and thermometer, under 30 ℃, mixed 2 hours, adding polysorbate with ratio in the following order is 3.5kg, odium stearate 2.5kg, Tea Saponin 1.5kg and azone 2kg, makes Java brucea complete stool extract miticide missible oil.
Embodiment 11:
Adopting multi-function extractor, is 1: 4 with the volume ratio of fructus gleditsiae complete stool and organic solvent ethanol, mac per hor X, and filtration, drying must the fructus gleditsiae whole strain extract; The fructus gleditsiae 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 0.9286g/cm
3, get fructus gleditsiae complete stool extract; After getting fructus gleditsiae complete stool extract 7kg usefulness benzinum 50kg dissolving, injection has the mixing kettle of agitator and thermometer, under 30 ℃, mixed 2 hours, adding polysorbate with ratio in the following order is 3.5kg, odium stearate 2.5kg, Tea Saponin 1.5kg and azone 2kg, makes fructus gleditsiae complete stool extract miticide missible oil.
Embodiment 12:
Adopting multi-function extractor, is 1: 4 with the volume ratio of shrubby flase indigo complete stool and organic solvent ethanol, mac per hor X, and filtration, drying must the shrubby flase indigo whole strain extract; The shrubby flase indigo 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 0.9286g/cm
3, get shrubby flase indigo complete stool extract; After getting shrubby flase indigo complete stool extract 7kg usefulness benzinum 50kg dissolving, injection has the mixing kettle of agitator and thermometer, under 30 ℃, mixed 2 hours, adding polysorbate with ratio in the following order is 3.5kg, odium stearate 2.5kg, Tea Saponin 1.5kg and azone 2kg, makes shrubby flase indigo complete stool extract miticide missible oil.
Embodiment 13: the preparation of Java brucea whole strain extract
Adopt multi-function extractor, the volume ratio of powder of Java brucea complete stool and organic solvent ethanol is 1: 2, and temperature was soaked 8 hours, filters, and drying gets the Java brucea whole strain extract.
Embodiment 14: the preparation of fructus gleditsiae whole strain extract
As the method for embodiment 13, make the fructus gleditsiae whole strain extract.
Embodiment 15: the preparation of shrubby flase indigo whole strain extract
As the method for embodiment 13, make the shrubby flase indigo whole strain extract.
Embodiment 16: the preparation of Java brucea whole strain extract
Adopt multi-function extractor, the volume ratio of powder of Java brucea complete stool and organic solvent ethanol is 1: 3, and cold soaking 24 hours filters, and drying gets the Java brucea whole strain extract.
Embodiment 17: the preparation of fructus gleditsiae whole strain extract
As the method for embodiment 16, make the fructus gleditsiae whole strain extract.
Embodiment 18: the preparation of shrubby flase indigo whole strain extract
As the method for embodiment 16, make the shrubby flase indigo whole strain extract.
Embodiment 19: the preparation of Java brucea whole strain extract
Adopt multi-function extractor, the volume ratio of powder of Java brucea complete stool and organic solvent ethanol is 1: 4, and temperature was soaked 10 hours, filters, and drying gets the Java brucea whole strain extract.
Embodiment 20: the preparation of fructus gleditsiae whole strain extract
As the method for embodiment 19, make the fructus gleditsiae whole strain extract.
Embodiment 21: the preparation of shrubby flase indigo whole strain extract
As the method for embodiment 19, make the shrubby flase indigo whole strain extract.
Embodiment 22: the preparation of Java brucea whole strain extract
Adopt multi-function extractor, the volume ratio of powder of Java brucea complete stool and organic solvent ethanol is 1: 2, and temperature was soaked 12 hours, filters, and drying gets the Java brucea whole strain extract.
Embodiment 23: the preparation of fructus gleditsiae whole strain extract
As the method for embodiment 22, make the fructus gleditsiae whole strain extract.
Embodiment 24: the preparation of shrubby flase indigo whole strain extract
As the method for embodiment 22, make the shrubby flase indigo whole strain extract.
Embodiment 25: the preparation of Java brucea whole strain extract
Adopt multi-function extractor, the volume ratio of powder of Java brucea complete stool and organic solvent ethanol is 1: 3, and cold soaking 18 hours filters, and drying gets the Java brucea whole strain extract.
Embodiment 26: the preparation of fructus gleditsiae whole strain extract
As the method for embodiment 25, make the fructus gleditsiae whole strain extract.
Embodiment 27: the preparation of shrubby flase indigo whole strain extract
As the method for embodiment 25, make the shrubby flase indigo whole strain extract.
Embodiment 28: the preparation of Java brucea whole strain extract
The volume ratio of Java brucea complete stool powder and organic solvent ethanol is 1: 3, and diacolation extracts 6 times repeatedly, filters, and drying gets the Java brucea whole strain extract.
Embodiment 29: the preparation of fructus gleditsiae whole strain extract
As the method for embodiment 28, make the fructus gleditsiae whole strain extract.
Embodiment 30: the preparation of shrubby flase indigo whole strain extract
As the method for embodiment 28, make the shrubby flase indigo whole strain extract.
Embodiment 31: the preparation of Java brucea whole strain extract
The volume ratio of Java brucea complete stool powder and organic solvent ethanol is 1: 3, and continuous backflow was extracted 8 hours, filters, and drying gets the Java brucea whole strain extract.
Embodiment 32: the preparation of fructus gleditsiae whole strain extract
As the method for embodiment 31, make the fructus gleditsiae whole strain extract.
Embodiment 33: the preparation of shrubby flase indigo whole strain extract
As the method for embodiment 31, make the shrubby flase indigo whole strain extract.
Embodiment 34: the preparation of Java brucea whole strain extract
The volume ratio of Java brucea complete stool powder and organic solvent ethanol is 1: 2, and diacolation extracts 4 times repeatedly, filters, and drying gets the Java brucea whole strain extract.
Embodiment 35: the preparation of fructus gleditsiae whole strain extract
As the method for embodiment 34, make the fructus gleditsiae whole strain extract.
Embodiment 36: the preparation of shrubby flase indigo whole strain extract
As the method for embodiment 34, make the shrubby flase indigo whole strain extract.
Embodiment 37: the preparation of Java brucea whole strain extract
The volume ratio of Java brucea complete stool powder and organic solvent ethanol is 1: 2, and continuous backflow was extracted 10 hours, filters, and drying gets the Java brucea whole strain extract.
Embodiment 38: the preparation of fructus gleditsiae whole strain extract
As the method for embodiment 37, make the fructus gleditsiae whole strain extract.
Embodiment 39: the preparation of shrubby flase indigo whole strain extract
As the method for embodiment 37, make the shrubby flase indigo whole strain extract.
Embodiment 40: the preparation of Java brucea whole strain extract
The volume ratio of Java brucea complete stool powder and organic solvent ethanol is 1: 4, and diacolation extracts 8 times repeatedly, filters, and drying gets the Java brucea whole strain extract.
Embodiment 41: the preparation of fructus gleditsiae whole strain extract
As the method for embodiment 40, make the fructus gleditsiae whole strain extract.
Embodiment 42: the preparation of shrubby flase indigo whole strain extract
As the method for embodiment 40, make the shrubby flase indigo whole strain extract.
Embodiment 43: the preparation of Java brucea whole strain extract
The volume ratio of Java brucea complete stool powder and organic solvent ethanol is 1: 4, and continuous backflow was extracted 4 hours, filters, and drying gets the Java brucea whole strain extract.
Embodiment 44: the preparation of fructus gleditsiae whole strain extract
As the method for embodiment 43, make the fructus gleditsiae whole strain extract.
Embodiment 45: the preparation of shrubby flase indigo whole strain extract
As the method for embodiment 43, make the shrubby flase indigo whole strain extract.
Embodiment 46: the preparation of Java brucea whole strain extract
The volume ratio of Java brucea complete stool powder and organic solvent ethanol is 1: 4, and diacolation extracts 10 times repeatedly, filters, and drying gets the Java brucea whole strain extract.
Embodiment 47: the preparation of fructus gleditsiae whole strain extract
As the method for embodiment 46, make the fructus gleditsiae whole strain extract.
Embodiment 48: the preparation of shrubby flase indigo whole strain extract
As the method for embodiment 46, make the shrubby flase indigo whole strain extract.
Embodiment 49: the preparation of Java brucea whole strain extract
The volume ratio of Java brucea complete stool powder and organic solvent ethanol is 1: 4, and continuous backflow was extracted 6 hours, filters, and drying gets the Java brucea whole strain extract.
Embodiment 50: the preparation of fructus gleditsiae whole strain extract
As the method for embodiment 49, make the fructus gleditsiae whole strain extract.
Embodiment 51: the preparation of shrubby flase indigo whole strain extract
As the method for embodiment 49, make the shrubby flase indigo whole strain extract.
Embodiment 52: the preparation of Java brucea complete stool extract
With embodiment 13 Java brucea 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 0.8997g/cm
3, get Java brucea complete stool extract.
Embodiment 53: the preparation of fructus gleditsiae complete stool extract
With the method that embodiment 14 gained fructus gleditsiae whole strain extracts are pressed embodiment 52, making relative density is 0.9132g/cm
3Fructus gleditsiae complete stool extract.
Embodiment 54: the preparation of shrubby flase indigo complete stool extract
With the method that embodiment 15 gained shrubby flase indigo whole strain extracts are pressed embodiment 52, making relative density is 0.9088g/cm
3Shrubby flase indigo complete stool extract.
Embodiment 55: the preparation of Java brucea complete stool extract
With embodiment 16 Java brucea whole strain extracts 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, use column chromatography method, with solvent polarity is the extraction order of solvent from small to large, chromatography, separation, purifying are repeatedly continuously finally collected petroleum ether extraction mutually and be evaporated to the ointment shape, and relative density is 0.9132g/cm
3, get Java brucea complete stool extract active component.
Embodiment 56: the preparation of fructus gleditsiae complete stool extract
With the method that embodiment 17 gained fructus gleditsiae whole strain extracts are pressed embodiment 55, making relative density is 0.8979g/cm
3Fructus gleditsiae complete stool extract.
Embodiment 57: the preparation of shrubby flase indigo complete stool extract
With the method that embodiment 18 gained shrubby flase indigo whole strain extracts are pressed embodiment 55, making relative density is 0.8798g/cm
3Shrubby flase indigo complete stool extract.
Embodiment 58: the acaricidal preparation of Java brucea whole strain extract
Embodiment 13,16,19,22 or 25 Java brucea whole strain extracts prepare miticide in following ratio.
Extract: 30kg
Acetone 60kg
Polyethylene glycol: 15kg
6-vinyl capraldehyde: 2kg
Paraoctyl phenol APEO: 20kg
Emulsifier BP: 1kg.
Embodiment 59: the acaricidal preparation of fructus gleditsiae whole strain extract
Embodiment 14,17,20,23 or 26 fructus gleditsiae whole strain extracts prepare miticide in following ratio.
Extract: 30kg
Acetone 60kg
Polyethylene glycol: 15kg
6-vinyl capraldehyde: 2kg
Paraoctyl phenol APEO: 20kg
Emulsifier BP: 1kg.
Embodiment 60: the acaricidal preparation of shrubby flase indigo whole strain extract
Embodiment 15,18,21,24 or 27 shrubby flase indigo whole strain extracts prepare miticide in following ratio.
Extract: 30kg
Acetone 60kg
Polyethylene glycol: 15kg
6-vinyl capraldehyde: 2kg
Paraoctyl phenol APEO: 20kg
Emulsifier BP: 1kg.
Embodiment 61: the acaricidal preparation of Java brucea whole strain extract
Embodiment 28,31,34,37,40,43,46 or 49 Java brucea whole strain extracts prepare miticide in following ratio.
Extract: 7kg
Cyclohexanone: 80kg
Neopelex: 8kg
Tea Saponin: 10kg
N-domiphen: 2kg
Triphen phosphorus: 15kg.
Embodiment 62: the acaricidal preparation of fructus gleditsiae whole strain extract
Embodiment 29,32,35,38,41,44,47 or 50 fructus gleditsiae whole strain extracts prepare miticide in following ratio.
Extract: 7kg
Cyclohexanone: 80kg
Neopelex: 8kg
Tea Saponin: 10kg
N-domiphen: 2kg
Triphen phosphorus: 15kg.
Embodiment 63: the acaricidal preparation of shrubby flase indigo whole strain extract
Embodiment 30,33,36,39,42,45,48 or 51 shrubby flase indigo whole strain extracts prepare miticide in following ratio.
Extract: 7kg
Cyclohexanone: 80kg
Neopelex: 8kg
Tea Saponin: 10kg
N-domiphen: 2kg
Triphen phosphorus: 15kg.
Embodiment 64: the acaricidal preparation of Java brucea extract
Embodiment 52 Java brucea complete stool extracts prepare miticide in following ratio.
Extract: 25kg
Benzinum: 45kg
Potassium dodecylbenzenesulfonate: 15kg
Octachlorodipropyl Ether: 5kg
Polyethenoxy ether: 4kg
Azone: 1kg.
Embodiment 65: the acaricidal preparation of fructus gleditsiae extract
Embodiment 53 fructus gleditsiae complete stool extracts prepare miticide in following ratio.
Extract: 25kg
Benzinum: 45kg
Potassium dodecylbenzenesulfonate: 15kg
Octachlorodipropyl Ether: 5kg
Polyethenoxy ether: 4kg
Azone: 1kg.
Embodiment 66: the acaricidal preparation of shrubby flase indigo extract
Embodiment 54 shrubby flase indigo complete stool extracts prepare miticide in following ratio.
Extract: 25kg
Benzinum: 45kg
Potassium dodecylbenzenesulfonate: 15kg
Octachlorodipropyl Ether: 5kg
Polyethenoxy ether: 4kg
Azone: 1kg.
Embodiment 67: the acaricidal preparation of Java brucea extract
Embodiment 55 Java brucea complete stool extracts prepare miticide in following ratio.
Extract: 10kg
Toluene: 70kg
Sorbierite polyoxy ether: 3kg
Odium stearate: 8kg
Azone: 7kg
Methylenedioxy benzene derivative: 2kg.
Embodiment 68: the acaricidal preparation of fructus gleditsiae extract
Embodiment 56 fructus gleditsiae complete stool extracts prepare miticide in following ratio.
Extract: 10kg
Toluene: 70kg
Sorbierite polyoxy ether: 3kg
Odium stearate: 8kg
Azone: 7kg
Methylenedioxy benzene derivative: 2kg.
Embodiment 69: the acaricidal preparation of shrubby flase indigo extract
Embodiment 57 shrubby flase indigo complete stool extracts prepare miticide in following ratio.
Extract: 10kg
Toluene: 70kg
Sorbierite polyoxy ether: 3kg
Odium stearate: 8kg
Azone: 7kg
Methylenedioxy benzene derivative: 2kg.
Claims (10)
1, plant shrubby flase indigo active component is characterized in that this active component is to be made by one of following method:
A adopts multi-function extractor, and plant shrubby flase indigo complete stool is made powder, with the volume ratio of organic solvent ethanol be 1: 2-8, temperature is soaked or cold soaking 4-24 hour, filter, drying, the shrubby flase indigo whole strain extract;
B adopts multi-function extractor, and the volume ratio of plant shrubby flase indigo 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 shrubby flase indigo whole strain extract.
2, the full pearl extract of shrubby flase indigo as claimed in claim 1 is characterized in that making that the volume ratio of shrubby flase indigo powder and ethanol is 1: 4 in the full pearl extract of the shrubby flase indigo method, 1: 5 or 1: 6.
3, shrubby flase indigo active component as claimed in claim 1 or 2 is characterized in that this shrubby flase indigo active component is to be made by following method:
With the shrubby flase indigo 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 ointment shape gets shrubby flase indigo complete stool extract.
4, shrubby flase indigo active component as claimed in claim 1 or 2 is made acaricidal preparation method, it is characterized in that this method is:, add solubilizer, emulsifier and/or the suspending agent, synergist, the bleeding agent that promote extract to dissolve or suspend therein with ratio in the following order and make miticide with shrubby flase indigo whole strain extract or extract chloroform, cyclohexane, benzene, dimethylbenzene or dissolve with ethanol;
Shrubby flase indigo whole strain extract miticide:
Extract: 5-35 weight portion
Solvent: 30-95 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
Above-mentioned solvent is selected from a kind of in water, ethanol, methyl alcohol, acetone, cyclohexanone, toluene, dimethylbenzene, benzinum, petroleum aromatic or the purified petroleum benzin; Solubilizer is neopelex, Potassium dodecylbenzenesulfonate, polysorbate, polyethylene glycol, sorbierite polyoxy ether, lignosulfonates, tea is withered or take any in the Chinese honey locust; Synergist is any in Tea Saponin, 2-C1C6H4-N=OCH3SCH3, methylenedioxy benzene derivative, 6-vinyl capraldehyde or 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 or the alkylaryl sulfonates; Bleeding agent is any in emulsifier BP, azone or the triphen phosphorus.
5, shrubby flase indigo active component as claimed in claim 3 is made acaricidal preparation method, it is characterized in that this method is:, add solubilizer, emulsifier and/or the suspending agent, synergist, the bleeding agent that promote extract to dissolve or suspend therein with ratio in the following order and make miticide with shrubby flase indigo whole strain extract or extract chloroform, cyclohexane, benzene, dimethylbenzene or dissolve with ethanol;
Shrubby flase indigo complete stool extract miticide:
Extract: 3-30 weight portion
Solvent: 30-90 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
Above-mentioned solvent is selected from a kind of in water, ethanol, methyl alcohol, acetone, cyclohexanone, toluene, dimethylbenzene, benzinum, petroleum aromatic or the purified petroleum benzin; Solubilizer is neopelex, Potassium dodecylbenzenesulfonate, polysorbate, polyethylene glycol, sorbierite polyoxy ether, lignosulfonates, tea is withered or take any in the Chinese honey locust; Synergist is any in Tea Saponin, 2-C1C6H4-N=OCH3SCH3, methylenedioxy benzene derivative, 6-vinyl capraldehyde or 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 or the alkylaryl sulfonates; Bleeding agent is any in emulsifier BP, azone or the triphen phosphorus.
6, shrubby flase indigo active component as claimed in claim 1 or 2 is characterized in that a kind of replacement in wherein said organic solvent ethanol chloroform, 30-90 ℃ benzinum, ether, ethyl acetate, n-hexane, cyclohexane, benzene, methyl alcohol, acetone or the cyclohexanone.
7, shrubby flase indigo active component as claimed in claim 3 is characterized in that a kind of replacement in wherein said organic solvent ethanol chloroform, 30-90 ℃ benzinum, ether, ethyl acetate, n-hexane, cyclohexane, benzene, methyl alcohol, acetone or the cyclohexanone etc.
8, the application of shrubby flase indigo active component as claimed in claim 1 or 2 in the preparation miticide.
9, the application of shrubby flase indigo active component as claimed in claim 3 in the preparation miticide.
10, the application of the full pearl of shrubby flase indigo in the preparation miticide farm chemical.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101606304A CN101595895B (en) | 2007-07-31 | 2007-07-31 | Amorpha fruticosa plant miticide and preparation method thereof |
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| CN2009101606304A CN101595895B (en) | 2007-07-31 | 2007-07-31 | Amorpha fruticosa plant miticide and preparation method thereof |
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| CNB2007101197214A Division CN100553453C (en) | 2007-07-31 | 2007-07-31 | Java brucea botanical acaricide and preparation method thereof |
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| CN101595895B CN101595895B (en) | 2012-08-22 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102687733A (en) * | 2012-05-03 | 2012-09-26 | 上海交通大学 | Black locust plant acaricide, preparation method and application thereof |
| CN107736386A (en) * | 2017-10-17 | 2018-02-27 | 张锡林 | A kind of composition pesticide |
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2007
- 2007-07-31 CN CN2009101606304A patent/CN101595895B/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102687733A (en) * | 2012-05-03 | 2012-09-26 | 上海交通大学 | Black locust plant acaricide, preparation method and application thereof |
| CN102687733B (en) * | 2012-05-03 | 2014-06-18 | 上海交通大学 | Black locust plant acaricide, preparation method and application thereof |
| CN107736386A (en) * | 2017-10-17 | 2018-02-27 | 张锡林 | A kind of composition pesticide |
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| CN101595895B (en) | 2012-08-22 |
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