CN101449686B - Nux vomica or cortex dictamni botanical acaricide and preparation method thereof - Google Patents
Nux vomica or cortex dictamni botanical acaricide and preparation method thereof Download PDFInfo
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- CN101449686B CN101449686B CN2007101788642A CN200710178864A CN101449686B CN 101449686 B CN101449686 B CN 101449686B CN 2007101788642 A CN2007101788642 A CN 2007101788642A CN 200710178864 A CN200710178864 A CN 200710178864A CN 101449686 B CN101449686 B CN 101449686B
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Abstract
The invention relates to a botanical acaricide for prevent acarid of economic crops of fruit trees and vegetables and the like and usage thereof, which is prepared by adding surfactant, emulsifying agent, characterized by high efficiency, low toxicity, low residual, being harmonious with environment and the like.
Description
Technical field
The present invention relates to a kind of agricultural chemicals and preparation method thereof, particularly relate to a kind of miticide and preparation method thereof.
Background technology
Phytophagous mites is the important pest mite in the agricultural production, and is because medicine resistance ability is strong, 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 is less; In the at present domestic similar research, the product of existing many plant insecticides comes out, but the acaricidal Pesticidal products report of plant resource is less.Therefore, 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 vomiting nut (Strychnos nux-vomica) or the root bark of shaggy-fruited dittany (Dictamnus dasycarpus) complete stool respectively has the vomiting nut or the root bark of shaggy-fruited dittany complete stool active ingredient of lethal effect to the mite class, and is prepared into the plant resource miticide.
Vomiting nut complete stool active component of the present invention can be vomiting nut whole strain extract or extract, and vomiting nut whole strain extract preparation technology is selected from one of following method:
A adopts multi-function extractor, and plant vomiting nut 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 vomiting nut whole strain extract;
B adopts multi-function extractor, and the volume ratio of plant vomiting nut 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 vomiting nut whole strain extract.
Vomiting nut complete stool extract preparation technology: with vomiting nut 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 0.8: 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 0.78-1g/cm
3The ointment shape, preferred relative density is vomiting nut 0.9546g/cm
3, get vomiting nut complete stool extract.
Acaricidal preparation method: vomiting nut whole strain extract or extract are dissolved with chloroform, cyclohexane, benzene, dimethylbenzene or alcohol solvent, 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.
Vomiting nut whole strain extract miticide:
Extract 5-36 weight portion
Solvent 30-95 weight portion
Solubilizer 1-40 weight portion
Emulsifier or suspending agent 2-350 weight portion
Synergist 0.5-30 weight portion
Bleeding agent 0.5-28 weight portion.
Vomiting nut complete stool extract miticide:
Extract 3-30 weight portion
Solvent 30-95 weight portion
Solubilizer 1-30 weight portion
Emulsifier or suspending agent 2-32 weight portion
Bleeding agent 0.5-28 weight portion
Synergist 0.5-25 weight portion.
The organic solvent of using among the described vomiting nut 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, the cyclohexanone etc.
Among the described vomiting nut 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, 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, 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 Semen Strychni extract miticide is preferably:
Extract 18 weight portions
Toluene 70 weight portions
Polysorbate 5 weight portions
Tea Saponin 4 weight portions
Lauryl sodium sulfate 5 weight portions
Azone 3 weight portions.
Vomiting nut extraction thing miticide is preferably:
Extract 14 weight portions
Dimethylbenzene 65 weight portions
Sorbierite polyoxy ether 3.5 weight portions
APEO 4 weight portions
6-vinyl capraldehyde 2.5 weight portions
Emulsifier BP 2.5 weight portions.
The present patent application also discloses a kind of root bark of shaggy-fruited dittany active component and miticide, root bark of shaggy-fruited dittany active component and miticide adopt the technical scheme identical with above-mentioned vomiting nut to be prepared from, and wherein finally collecting chloroform or petroleum ether extraction phase among the root bark of shaggy-fruited dittany complete stool extract preparation technology and being evaporated to relative density is 0.8-1g/cm
3The ointment shape, preferred relative density is 0.9128g/cm
3, get root bark of shaggy-fruited dittany 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 vomiting nut or root bark of shaggy-fruited dittany 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) vomiting nut or root bark of shaggy-fruited dittany 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 vomiting nut or root bark of shaggy-fruited dittany complete stool miticide have significant miticidal effect, have the chemical pesticide characteristics of high efficiency; (4) extraction of active component is simple in vomiting nut or the root bark of shaggy-fruited dittany 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 vomiting nut or root bark of shaggy-fruited dittany whole strain extract or extract that the present invention obtains, standard method one slide method of recommending with reference to FAO carries out biological activity determination to the vomiting nut or the root bark of shaggy-fruited dittany 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 liang plant species extract is to Tetranychus cinnabarinus (Teranychus cinnabarinus) miticidal effect
| Concentration | Corrected mortality | |
| Vomiting nut | The root bark of shaggy-fruited dittany | |
| 300× 600× 900× | 88.35±4.23a 68.54±2.76b 45.81±4.43c | 82.58±4.32a 64.27±3.54b 41.42±4.22c |
Table 2 liang plant species extract is to Tetranychus cinnabarinus (Teranychus cinnabarinus) toxic effect
| Concentration | Corrected mortality | |
| Vomiting nut | The root bark of shaggy-fruited dittany | |
| 400× 800× 1200× | 81.31±2.76a 61.33±3.76b 50.89±4.28c | 71.54±4.78a 52.44±3.88b 47.98±4.24c |
The result shows: the acaricidal rate of the extract of two plant species or extract knot Tetranychus cinnabarinus and poisoning rate all level reach more than 80%, the poisoning rate of root bark of shaggy-fruited dittany extract is lower slightly, but also reach more than 70%, along with the extract of two plant species or the reduction of extract concentration, its miticidal effect and toxic effect decrease, but the lethality of acarid is still about 45%.This shows that the whole strain extract of the vomiting nut of the present invention or the root bark of shaggy-fruited dittany 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, vomiting nut, the root bark of shaggy-fruited dittany and shrubby flase indigo complete stool extract kill the ovum effect and see Table 3.
Table 3 liang plant species extract is to the active effect of Tetranychus cinnabarinus (Teranychus cinnabarinus) ovum
| Concentration | Corrected mortality | |
| Vomiting nut | The root bark of shaggy-fruited dittany | |
| 400× 800× 1200× | 71.01±4.11a 65.42±3.44b 42.37±4.55c | 67.37±2.87a 57.79±4.31b 38.67±3.27c |
The result shows: two plant species extracts all can reach 65% to the poisoning rate of Tetranychus cinnabarinus ovum, and wherein vomiting nut extraction thing can reach more than 70% the poisoning rate of Tetranychus cinnabarinus ovum, proves that two 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 liang plant species extract is to the antifeedant activity effect of Tetranychus cinnabarinus (Teranychus cinnabarinus)
| Handle | Vomiting nut | The root bark of shaggy-fruited dittany | |
| If mite | 300× 600× 900× | 76.55±4.31a 59.33±4.12b 39.34±3.18c | 70.32±3.67a 53.99±4.44b 41.65±3.21c |
| Become mite | 300× 600× 900× | 70.55±2.49a 58.32±4.37b 41.33±2.68c | 67.32±3.87a 53.66±4.32b 36.97±2.78c |
The result shows: two 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 about 70%, prove the present invention's two 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 Tetranychus cinnabarinus (Teranychus cinnabarinus) active substance of two plant species
| Project | Vomiting nut | The root bark of shaggy-fruited dittany | |
| Egg mortality 500 * | A B | 71.01±4.11a 35.70±4.52b | 67.37±2.87a 36.34±2.95b |
| Food refusal rate 300 * | A B | 70.55±2.49a 33.21±3.76b | 67.32±3.87a 27.89±4.02b |
Annotate: A: be the action effect of active component that this technology is carried, 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 two 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 about 70%, the acaricidal rate that open technology is extracted active component only about 35%; 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.
Following embodiment all can realize the effect of above-mentioned experimental example.
Embodiment
Embodiment 1:
The vomiting nut 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 18kg and add toluene 70kg, add and have in the mixing kettle of agitator and thermometer, under 50 ℃, mixed 1.5 hours, add tween (polysorbate) 5kg, 6-vinyl capraldehyde 4kg, lauryl sodium sulfate 5kg, emulsifier BP 3kg, mix, obtain vomiting nut whole strain extract miticide missible oil.
Embodiment 2:
As the method for embodiment 1, make Cortex Dictamni extract miticide missible oil.
Embodiment 3:
The vomiting nut 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 65kg, add and have in the mixing kettle of agitator and thermometer, under 60 ℃, mixed 3 hours, add polyethylene glycol 3.5kg, Tea Saponin 4kg, paraoctyl phenol APEO 2.5kg, azone 2.5kg, mix, obtain vomiting nut whole strain extract miticide missible oil.
Embodiment 4:
As the method for embodiment 3, make Cortex Dictamni extract miticide missible oil.
Embodiment 5:
The vomiting nut 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 15kg and add dimethylbenzene 70kg, add and have in the mixing kettle of agitator and thermometer, under 60 ℃, mixed 2 hours, adding neopelex 8kg, 6-vinyl capraldehyde 4kg, paraoctyl phenol APEO 5kg, azone 3kg mix, and obtain vomiting nut whole strain extract miticide missible oil.
Embodiment 6:
As the method for embodiment 5, make Cortex Dictamni extract miticide missible oil.
Embodiment 7:
Adopting multi-function extractor, is 1: 4 with the volume ratio of vomiting nut complete stool and organic solvent ethanol, mac per hor X, and filtration, drying must the vomiting nut whole strain extract; The vomiting nut 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 0.9546g/cm
3, get vomiting nut complete stool extract; After getting vomiting nut complete stool extract 10kg 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 vomiting nut complete stool extract miticide missible oil.
Embodiment 8:
Adopting multi-function extractor, is 1: 4 with the volume ratio of root bark of shaggy-fruited dittany complete stool and organic solvent ethanol, mac per hor X, and filtration, drying must root bark of shaggy-fruited dittany whole strain extract; Root bark of shaggy-fruited dittany 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 0.9128g/cm
3, get root bark of shaggy-fruited dittany complete stool extract; After getting root bark of shaggy-fruited dittany complete stool extract 10kg 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 root bark of shaggy-fruited dittany complete stool extract miticide missible oil.
Embodiment 9:
The preparation of vomiting nut whole strain extract
Adopt multi-function extractor, plant vomiting nut complete stool made powder, with the volume ratio of organic solvent ethanol be 1: 4, temperature was soaked 10 hours, filter, drying, the vomiting nut whole strain extract.
Embodiment 10:
The preparation of root bark of shaggy-fruited dittany whole strain extract
Method as embodiment 9 makes root bark of shaggy-fruited dittany whole strain extract.
Embodiment 11:
The preparation of vomiting nut whole strain extract
Adopting multi-function extractor, is 1: 4 with the volume ratio of vomiting nut complete stool powder and organic solvent-normal hexane, and diacolation extracts 8 times repeatedly, filtration, and drying must the vomiting nut whole strain extract.
Embodiment 12:
The preparation of root bark of shaggy-fruited dittany whole strain extract
Method as embodiment 11 makes root bark of shaggy-fruited dittany whole strain extract.
Embodiment 13:
The preparation of vomiting nut complete stool extract
With embodiment 9,11 gained vomiting nut 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 0.9546g/cm
3, get vomiting nut complete stool extract.
Embodiment 14:
The preparation of root bark of shaggy-fruited dittany complete stool extract
With embodiment 10,12 gained root bark of shaggy-fruited dittany 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 0.9128g/cm
3, get root bark of shaggy-fruited dittany complete stool extract.
Embodiment 15:
The preparation of vomiting nut whole strain extract
Adopting multi-function extractor, is 1: 6 with the volume ratio of vomiting nut complete stool powder and organic solvent ethyl acetate, and continuous backflow was extracted 20 hours, filtered, and drying must the vomiting nut whole strain extract.
Embodiment 16: the preparation of root bark of shaggy-fruited dittany whole strain extract
As the method for embodiment 15, make root bark of shaggy-fruited dittany whole strain extract.
Embodiment 17: the preparation of vomiting nut complete stool extract
With the vomiting nut whole strain extract of embodiment 15 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 vomiting nut 0.9546g/cm
3, get vomiting nut complete stool extract.
Embodiment 18: the preparation of root bark of shaggy-fruited dittany complete stool extract
With the root bark of shaggy-fruited dittany whole strain extract of embodiment 16 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 root bark of shaggy-fruited dittany 0.9128g/cm
3, get root bark of shaggy-fruited dittany complete stool extract.
Embodiment 19: the preparation of Semen Strychni extract
Adopting multi-function extractor, is 1: 5 with the volume ratio of vomiting nut complete stool powder and organic solvent ether, mac per hor X, and filtration, drying must the vomiting nut whole strain extract.
Embodiment 20: the preparation of Cortex Dictamni extract
As the method for embodiment 19, make root bark of shaggy-fruited dittany whole strain extract.
Embodiment 21: the preparation of vomiting nut whole strain extract
Adopting multi-function extractor, is 1: 6 with the volume ratio of vomiting nut complete stool powder and organic solvent methyl alcohol, and temperature was soaked 20 hours, filtration, and drying must the vomiting nut whole strain extract.
Embodiment 22: the preparation of Cortex Dictamni extract
As the method for embodiment 21, make root bark of shaggy-fruited dittany whole strain extract.
Embodiment 23: the preparation of vomiting nut whole strain extract
Adopting multi-function extractor, is 1: 6 with the volume ratio of vomiting nut complete stool powder and organic solvent ethyl acetate, and temperature was soaked 10 hours, filtration, and drying must the vomiting nut whole strain extract.
Embodiment 24: the preparation of Cortex Dictamni extract
As the method for embodiment 23, make root bark of shaggy-fruited dittany whole strain extract.
The preparation of tuber of stemona whole strain extract
Embodiment 25: the preparation of vomiting nut whole strain extract
Adopting multi-function extractor, is 1: 4 with the volume ratio of vomiting nut complete stool powder and organic solvent-benzene, and diacolation extracts 5 times repeatedly, filtration, and drying must the vomiting nut whole strain extract.
Embodiment 26: the preparation of Cortex Dictamni extract
As the method for embodiment 25, make root bark of shaggy-fruited dittany whole strain extract.
Embodiment 27: the preparation of vomiting nut whole strain extract
Adopting multi-function extractor, is 1: 5 with the volume ratio of vomiting nut complete stool powder and organic solvent-acetone, and continuous backflow was extracted 10 hours, filtration, and drying must the vomiting nut whole strain extract.
Embodiment 28: the preparation of Cortex Dictamni extract
As the method for embodiment 27, make root bark of shaggy-fruited dittany whole strain extract.
Embodiment 29: the preparation of vomiting nut whole strain extract
Adopting multi-function extractor, is 1: 6 with the volume ratio of vomiting nut complete stool powder and organic solvent-normal hexane, and diacolation extracts 3 times repeatedly, filtration, and drying must the vomiting nut whole strain extract.
Embodiment 30: the preparation of Cortex Dictamni extract
As the method for embodiment 29, make root bark of shaggy-fruited dittany whole strain extract.
Embodiment 31: the preparation of vomiting nut whole strain extract
Adopting multi-function extractor, is 1: 5 with the volume ratio of vomiting nut complete stool powder and organic solvent ethyl acetate, and continuous backflow was extracted 18 hours, filtration, and drying must the vomiting nut whole strain extract.
Embodiment 32: the preparation of Cortex Dictamni extract
As the method for embodiment 31, make root bark of shaggy-fruited dittany whole strain extract.
Embodiment 33: the preparation of vomiting nut complete stool extract
Behind 30-90 ℃ of petroleum ether dissolution of embodiment 19 gained vomiting nut 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 0.9546g/cm
3, get vomiting nut complete stool extract.
Embodiment 34: the preparation of Cortex Dictamni extract
Behind 30-90 ℃ of petroleum ether dissolution of embodiment 20 gained root bark of shaggy-fruited dittany 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 0.9128g/cm
3, get root bark of shaggy-fruited dittany complete stool extract.
Embodiment 35: the preparation of vomiting nut complete stool extract
With embodiment 21 gained vomiting nut 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 0.9546g/cm
3, get vomiting nut complete stool extract.
Embodiment 36: the preparation of root bark of shaggy-fruited dittany complete stool extract
With embodiment 22 gained root bark of shaggy-fruited dittany 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 0.9128g/cm
3, get root bark of shaggy-fruited dittany complete stool extract.
Embodiment 37: the preparation of vomiting nut complete stool extract
With embodiment 23 gained vomiting nut 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 0.9546g/cm
3, get vomiting nut complete stool extract.
Embodiment 38: the preparation of root bark of shaggy-fruited dittany complete stool extract
With embodiment 24 gained root bark of shaggy-fruited dittany 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 0.9128g/cm
3, get root bark of shaggy-fruited dittany complete stool extract.
Embodiment 39: the preparation of vomiting nut complete stool extract
With embodiment 25 gained vomiting nut 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 0.9546g/cm
3, get vomiting nut complete stool extract.
Embodiment 40: the preparation of root bark of shaggy-fruited dittany complete stool extract
With embodiment 26 gained root bark of shaggy-fruited dittany 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 0.9128g/cm
3, get root bark of shaggy-fruited dittany complete stool extract.
Embodiment 41: the acaricidal preparation of Semen Strychni extract
Embodiment 9,11,15 or 19 vomiting nut whole strain extract prepare miticide in following ratio
Extract 18kg
Toluene 70kg
Polysorbate 5kg
Tea Saponin 4kg
Lauryl sodium sulfate 5kg
Azone 3kg.
Embodiment 42: the acaricidal preparation of Cortex Dictamni extract
Embodiment 10,12,16 or 20 root bark of shaggy-fruited dittany whole strain extract prepare miticide in following ratio
Extract 18kg
Toluene 70kg
Polysorbate 5kg
Tea Saponin 4kg
Lauryl sodium sulfate 5kg
Azone 3kg.
Embodiment 43: the acaricidal preparation of Semen Strychni extract
Embodiment 21,23,25,27,29 or 31 vomiting nut whole strain extracts prepare miticide in following ratio
Extract 30kg
Acetone 70kg
Polyethylene glycol 15kg
6-vinyl capraldehyde 14kg
Paraoctyl phenol APEO 18kg
Emulsifier BP 12kg.
Embodiment 44: the acaricidal preparation of Cortex Dictamni extract
Embodiment 22,24,26,28,30 or 32 root bark of shaggy-fruited dittany whole strain extracts prepare miticide in following ratio
Extract 30kg
Acetone 70kg
Polyethylene glycol 15kg
6-vinyl capraldehyde 14kg
Paraoctyl phenol APEO 18kg
Emulsifier BP 12kg.
Embodiment 45: the acaricidal preparation of vomiting nut extraction thing
Embodiment 13,17 or 33 vomiting nut complete stool extracts prepare miticide in following ratio
Extract 14kg
Dimethylbenzene 65kg
Sorbierite polyoxy ether 3.5kg
APEO 4kg
6-vinyl capraldehyde 2.5kg
Emulsifier BP 2.5kg.
Embodiment 46: the acaricidal preparation of fresh hide extract
Embodiment 14,18 or 34 root bark of shaggy-fruited dittany complete stool extracts prepare miticide in following ratio
Extract 14kg
Dimethylbenzene 65kg
Sorbierite polyoxy ether 3.5kg
APEO 4kg
6-vinyl capraldehyde 2.5kg
Emulsifier BP 2.5kg.
Embodiment 47: the acaricidal preparation of vomiting nut extraction thing
Embodiment 35,37 or 39 vomiting nut complete stool extracts prepare miticide in following ratio
Extract 25kg
Benzinum 60kg
Potassium dodecylbenzenesulfonate 10kg
Octachlorodipropyl Ether 7kg
Polyethenoxy ether 8kg
Azone 5kg.
Embodiment 48: the acaricidal preparation of root bark of shaggy-fruited dittany extract
Embodiment 36,38 or 40 root bark of shaggy-fruited dittany complete stool extracts prepare miticide in following ratio
Extract 25kg
Benzinum 60kg
Potassium dodecylbenzenesulfonate 10kg
Octachlorodipropyl Ether 7kg
Polyethenoxy ether 8kg
Azone 5kg.
Claims (8)
1. plant vomiting nut 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 vomiting nut 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 vomiting nut whole strain extract;
B adopts multi-function extractor, and the volume ratio of plant vomiting nut 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 vomiting nut whole strain extract;
With the vomiting nut whole strain extract with dissolve with methanol after, place airtight extractor, adopt liquid-liquid apportion design extraction with chloroform or benzinum solvent with 0.8: 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 0.78-1g/cm
3The vomiting nut complete stool extract of ointment shape.
2. vomiting nut active component as claimed in claim 1 is characterized in that making that the volume ratio of vomiting nut powder and ethanol is 1: 4 in the vomiting nut active component method, 1: 5 or 1: 6.
3. vomiting nut active component as claimed in claim 1 or 2 is made acaricidal preparation method, it is characterized in that this method is: vomiting nut whole strain extract or extract are dissolved with chloroform, cyclohexane, benzene, dimethylbenzene or alcohol solvent, 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;
Extract 5-36 weight portion
Solvent 30-95 weight portion
Solubilizer 1-40 weight portion
Emulsifier or suspending agent 2-350 weight portion
Synergist 0.5-30 weight portion
Bleeding agent 0.5-28 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, the triphen phosphorus.
4. vomiting nut 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.
5. the preparation method of a vomiting nut active component is characterized in that this method is one of following method:
A adopts multi-function extractor, and the volume ratio of plant vomiting nut 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 vomiting nut whole strain extract;
B adopts multi-function extractor, and the volume ratio of plant vomiting nut 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 vomiting nut whole strain extract;
With the vomiting nut whole strain extract with dissolve with methanol after, place airtight extractor, adopt liquid-liquid apportion design extraction with chloroform or benzinum solvent with 0.8: 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 0.78-1g/cm
3The vomiting nut complete stool extract of ointment shape.
6. as the preparation method of vomiting nut active component as described in the claim 5, it is characterized in that the volume ratio of vomiting nut powder and ethanol is 1: 4 in this method, 1: 5 or 1: 6.
7. as the preparation method of vomiting nut active component as described in claim 5 or 6, it is characterized in that wherein said organic solvent except that ethanol by a kind of replacement in chloroform, 30-90 ℃ benzinum, ether, ethyl acetate, n-hexane, cyclohexane, benzene, methyl alcohol, acetone or the cyclohexanone.
8. the application of vomiting nut active component as claimed in claim 1 or 2 in the preparation miticide.
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| CN 200910162506 Division CN101766196B (en) | 2007-12-06 | 2007-12-06 | Dictamnus dasycarpus vegetable acaricide and preparation method thereof |
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| CN1394485A (en) * | 2002-08-22 | 2003-02-05 | 王广勇 | Nuisance-free plant pesticide and its insecticidal organic fertilizer |
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| CN1394485A (en) * | 2002-08-22 | 2003-02-05 | 王广勇 | Nuisance-free plant pesticide and its insecticidal organic fertilizer |
Non-Patent Citations (2)
| Title |
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| 李旭涛.中草药防治蜂螨.《养蜂科技》.1994,(第5期), * |
| 段晓颖.正交试验法优选马钱子醇提工艺研究.《中国现代应用药学杂志》.2007,第24卷(第5期), * |
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