CN103651632B - Containing the composition pesticide and its preparation method and application of Fructus meliae toosendan and black false hellebore extract - Google Patents

Containing the composition pesticide and its preparation method and application of Fructus meliae toosendan and black false hellebore extract Download PDF

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CN103651632B
CN103651632B CN201310740576.7A CN201310740576A CN103651632B CN 103651632 B CN103651632 B CN 103651632B CN 201310740576 A CN201310740576 A CN 201310740576A CN 103651632 B CN103651632 B CN 103651632B
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fructus meliae
meliae toosendan
black false
false hellebore
extract
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CN103651632A (en
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何其明
唐齐
严寒
苏克跃
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Chengdu new Chaoyang Crop Science Co., Ltd
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Chengdu NewSun Crop Science Co Ltd
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Abstract

The present invention relates to the composition pesticide and its preparation method and application containing Fructus meliae toosendan and black false hellebore extract, belong to pesticide field.The technical problem to be solved in the present invention is, provides a kind of and contains composition pesticide of Fructus meliae toosendan and black false hellebore extract and its preparation method and application.The present invention contains the composition pesticide of Fructus meliae toosendan and black false hellebore extract, and its active component is jointly extracted by the crude drug of following weight portion and forms: Fructus meliae toosendan 1 part, black false hellebore 0.5 ~ 6 part; Further, its active component is jointly extracted by Fructus meliae toosendan and black false hellebore and forms; Or extract by Fructus meliae toosendan the Sichuan chinaberry extract, the black false hellebore that obtain and extract the black false hellebore extract obtained and mix; Or its active component is made up of 1 part of toosendanin and 0.5 ~ 6 part of jervine.The present inventor is through great many of experiments, and toosendanin and jervine have synergistic function, effectively can kill acarina pest as Tetranychus cinnabarinus, yellow tea mite, Panonychus citri etc., thus have positive effect for agricultural production.

Description

Containing the composition pesticide and its preparation method and application of Fructus meliae toosendan and black false hellebore extract
Technical field
The present invention relates to the composition pesticide and its preparation method and application containing Fructus meliae toosendan and black false hellebore extract, belong to pesticide field.
Background technology
Fructus meliae toosendan has another name called FRUCTUS TOOSENDAN, traditional Chinese medicine, is the ripening fruits of Meliaceae deciduous tree toosendanin.Mainly originate in the southern various places of China, superior with the product person in Sichuan, therefore have another name called Fructus meliae toosendan.Fructus meliae toosendan is cold in nature, bitter, is the one of qi-activating drug.Mainly enter Liver Channel, catharsis liver heat, promoting qi circulation and relieving pain, has the function except damp and hot, clearing away the liver-fire, pain relieving, desinsection, is that preparation is efficiently without the important source material of residual hazard free of contamination novel plant class agricultural chemicals.
Black false hellebore taste is worked hard, and has strong emetic action, and rapidly poisoning, symptom comprises Nausea and vomiting, cardioplegia etc.Veratrum alkaloid is through polypide surface or suck and enter digestive system, causes local excitation, causes reflectivity polypide excited, then suppresses polypide sensory nerve ending, through conduction with suppress nervous centralis and cause insect death.
The present inventor is through great many of experiments, other active insecticidal components that toosendanin, jervine are identical with jervine with essential groups have synergistic function, effectively can kill acarina pest as Tetranychus cinnabarinus, yellow tea mite, Panonychus citri etc., thus for agricultural production, there is positive effect.
Summary of the invention
The technical problem to be solved in the present invention is, provides a kind of and contains composition pesticide of Fructus meliae toosendan and black false hellebore extract and its preparation method and application.
The present invention contains the composition pesticide of Fructus meliae toosendan and black false hellebore extract, and its active component is jointly extracted by the crude drug of following weight portion and forms: Fructus meliae toosendan 1 part, black false hellebore 0.5 ~ 6 part; Be preferably Fructus meliae toosendan 1 part, black false hellebore 1 ~ 4 part; Be more preferably Fructus meliae toosendan 1 part, black false hellebore 1 ~ 3 part; More preferably Fructus meliae toosendan 1 part, black false hellebore 2 parts.
Wherein, the Fructus meliae toosendan that the present invention adopts and black false hellebore are Chinese herbal medicine raw material, contain the activity of the composition pesticide of Fructus meliae toosendan and black false hellebore extract in order to improve the present invention, the Fructus meliae toosendan that Fructus meliae toosendan is preferably dry, the black false hellebore rhizome that black false hellebore is preferably dry.
Further, preferably, the present invention jointly to be extracted through ethanolic solution by Fructus meliae toosendan and black false hellebore containing the active component of the composition pesticide of Fructus meliae toosendan and black false hellebore extract and forms; Or the black false hellebore extract that the Sichuan chinaberry extract to be obtained through alcohol extract by Fructus meliae toosendan, black false hellebore obtain through alcohol extract mixes; Described concentration of alcohol is 50 ~ 90%v/v, is preferably 80%v/v.
Wherein, in order to improve the effect of the present invention containing the composition pesticide of Fructus meliae toosendan and black false hellebore extract, the present invention preferably jointly to be extracted through ethanolic solution by Fructus meliae toosendan and black false hellebore containing the active component of the composition pesticide of Fructus meliae toosendan and black false hellebore extract and forms;
Further, in order to improve the activity of the composition pesticide containing Fructus meliae toosendan and black false hellebore extract, be convenient to store and transport, the described composition pesticide containing Fructus meliae toosendan and black false hellebore extract can be prepared as the conventional formulations of pesticide, is preferably microemulsion, soluble concentrate or aqua simultaneously.
Further, in order to improve the stability of the composition pesticide containing Fructus meliae toosendan and black false hellebore extract, described containing in the composition pesticide of Fructus meliae toosendan and black false hellebore extract also comprises auxiliary agent, described auxiliary agent can adopt the usual auxiliaries in composition, as at least one in emulsifier, antifreeze, solvent, defoamer, dispersant, wetting agent, stabilizing agent.
Wherein, emulsifier can adopt at least one in non-ionic surface active agent and anion surfactant, described non-ionic surface active agent can be dibenzyl xenyl APEO, styryl phenyl APEO, styryl phenyl APEO, phenethyl phenyl polyoxyethylene one polyethenoxy ether, OPEO, alkylphenol polyoxyethylene sulfosuccinate, aliphatic acid polyethenoxy ether, fatty alcohol-polyoxyethylene ether, aliphatic amine polyoxyethylene ether, castor oil ethylene oxide adduct and derivative thereof, at least one in polyol fatty acid ester and ethylene oxide adduct etc. thereof, described anion surfactant is at least one in calcium dodecyl benzene sulfonate, alkylphenol polyoxyethylene phosphate, phenethyl phenol polyethenoxy ether phosphate etc., as emulsifier 500,601p, 602p etc., in addition, commercially available emulsifier production can also be used.
Wherein, solvent can adopt at least one in water, ethanol, isopropyl alcohol, n-butanol, ethyl acetate, butyl acetate, methyl-sulfoxide, turpentine oil, solvent naphtha, 1-METHYLPYRROLIDONE, dimethyl formamide etc.
Wherein, antifreeze can be glycerine, propane diols, ethylene glycol, sodium chloride, calcium chloride, sorbierite etc.
Wherein, defoamer is silicone defoaming agent etc.
Wherein, dispersant is at least one in lignosulfonates, PAA and propionamide copolymer, alkylnaphthalene sulfonate, polycarboxylic acid salt's condensation product, methyl sodiosul foaliphatate etc.
Wherein, wetting agent can be alkyl sulfate, alkylbenzenesulfonate, alkylnaphthalene sulfonate, aliphatic alcohol polyethenoxy base ether, alkylphenol-polyethenoxy base ether, sorbitan fatty acid ester etc.; Described stabilizing agent can be 2-expoxy propane, butyl glycidyl ether, isopropyl alcohol, n-butanol, polyethylene glycol etc.
Further, preferably, the soluble concentrate that the present invention contains the composition pesticide of Fructus meliae toosendan and black false hellebore extract is made up of the component of following weight portion: Fructus meliae toosendan and black false hellebore extract, 15 parts of emulsifier 508,5 parts of emulsifier, 506,20 parts of ethanol, 5 parts of dimethyl sulfoxide (DMSO)s, 5 parts of ethylene glycol, 20 parts of water; Wherein, Fructus meliae toosendan and black false hellebore extract are that the crude drug of 30 weight portions jointly extracts and forms.
For the ease of storing and transport, extract can be concentrated, obtain concentrate, and then be prepared into various formulation, cycles of concentration can according to needs of production from Row sum-equal matrix, preferably, Fructus meliae toosendan is prepared from by the following method with black false hellebore extract: crude drug is through extracting and being concentrated into identical with crude drug weight.
Further, after measured, the present invention has synergistic function containing Fructus meliae toosendan and the toosendanin in the composition pesticide active component of black false hellebore extract, other active insecticidal components that jervine is identical with jervine with essential groups, therefore, the independent extract that the composition pesticide effect prepared by common extract is better than the two mixes the composition pesticide prepared.Meanwhile, through inventor's lot of experiments, find the composition pesticide adopting toosendanin and jervine binary built to obtain, although activity is a little less than extract, but still there is certain activity.Therefore, from cost-saving angle, the active component that the present invention contains the composition pesticide of Fructus meliae toosendan and black false hellebore extract also can be made up of toosendanin and jervine, and wherein, the mass ratio of toosendanin and jervine is 1:0.5 ~ 6, is preferably 1:2.
Further, the invention also discloses the preparation method that the present invention contains the composition pesticide of Fructus meliae toosendan and black false hellebore extract, wherein, according to Fructus meliae toosendan and black false hellebore be raw material prepare the composition pesticide of the present invention containing Fructus meliae toosendan and black false hellebore extract time, can following methods be adopted:
Method (one):
A, extraction: take Fructus meliae toosendan particle and black false hellebore particle, mixing, adds solvent by solid-liquid ratio 1:3 ~ 12g/ml, in 60 ~ 95 DEG C of refluxing extraction, filters, obtains extract;
B, preparation: extract is made microemulsion, soluble concentrate or aqua.
Method (two):
A, extraction: take Fructus meliae toosendan particle, add ethanolic solution by solid-liquid ratio 1:3 ~ 12g/ml, in 60 ~ 95 DEG C of refluxing extraction, filters, obtain Fructus meliae toosendan extract;
Take black false hellebore particle, add ethanolic solution by solid-liquid ratio 1:3 ~ 12g/ml, in 60 ~ 95 DEG C of refluxing extraction, filter, obtain black false hellebore extract;
B, preparation: by Fructus meliae toosendan extract and the mixing of black false hellebore extract, and make microemulsion, soluble concentrate or aqua.
Wherein, in said method () and (two), Fructus meliae toosendan particle and black false hellebore particle can adopt commercially available particle, conventional method also can be adopted to pulverize Fructus meliae toosendan and black false hellebore rhizome obtains.In order to improve the effect of extraction, simultaneously cost-saving, Fructus meliae toosendan particle and black false hellebore particle cross 60 ~ 100 mesh sieves, preferred mistake 80 mesh sieve.
Further, in order to cost-saving, simultaneously also in order to improve extraction efficiency, the solid-liquid ratio in a step is preferably 1:4 ~ 10g/ml, is more preferably 1:6g/ml.Namely the Fructus meliae toosendan of lg and black false hellebore particle add 3 ~ 12ml solvent extraction, preferably add 4 ~ 10ml, more preferably add 6ml.
In order to improve dissolution rate, ensure extraction efficiency, described solvent is preferably the ethanol of 50 ~ 90%v/v simultaneously, is more preferably 80%v/v ethanol.
In order to shorten preparation time, accelerate extraction rate, can stir when adding hot reflux, mixing speed is preferably 80 ~ 100 revs/min.
Further, reflux temperature is preferably 75 ~ 85 DEG C, is more preferably 82 DEG C; Reflow's cycle is twice, and each return time is 2 hours, and merging filtrate obtains corresponding extract.
Further, the invention also discloses the application of composition pesticide in control crop pest containing Fructus meliae toosendan and black false hellebore extract, wherein, described crop pest is preferably acarina pest; Common acarina pest has Panonychus citri, Tetranychus cinnabarinus, yellow tea mite etc.
In the agricultural production of reality, in order to improve composition pesticide containing Fructus meliae toosendan and black false hellebore extract to the control efficiency of insect pest, the described composition pesticide containing Fructus meliae toosendan and black false hellebore extract is preferably applied to crop pest initial stage of origination; The present invention can use by common method containing the composition pesticide of Fructus meliae toosendan and black false hellebore extract, sprays on crop blade face.Preferably, the composition pesticide containing Fructus meliae toosendan and black false hellebore extract as the present invention adopts Fructus meliae toosendan and black false hellebore extraction to be prepared from, be diluted with water to when then using with the activity component concentration of crude drug weighing scale as 10 ~ 100ppm, namely the composition pesticide that 1g crude drug is obtained after extracting, when using, be diluted with water to 10kg, then its activity component concentration equals 100ppm; Preferably being diluted to further with the activity component concentration of crude drug weighing scale is that 20 ~ 50ppm sprays in plant blade face.When the present invention containing the composition pesticide of Fructus meliae toosendan and black false hellebore extract adopt toosendanin and jervine composite as active component time, being then diluted with water to activity component concentration in composition pesticide when using is 10 ~ 100ppm; Preferably being diluted to jervine concentration is further that 20 ~ 50ppm sprays in plant blade face.When spraying, so that water membrane to appear in blade face, not lower of liquid is advisable; Secondary dispenser is carried out, the preferred continuous administration of a season crop 2 ~ 3 times after being preferable over 3 ~ 5 days.
Beneficial effect of the present invention:
1, Fructus meliae toosendan of the present invention and the common extract of black false hellebore have synergistic function, obvious to the control efficiency of acarina pest.
2, the present invention adopts Fructus meliae toosendan and black false hellebore jointly to extract, improve other active insecticidal components content that toosendanin, jervine and essential groups are identical with jervine, crop immune system ability can be improved while quick-acting tagging, and its vigor can be significantly improved.
3, in the present invention, toosendanin and jervine have synergistic function.
4, the present invention take Chinese herbal medicine as raw material, thus there is not Pesticide Residue, and insect is difficult to produce resistance; Be used alone compared with chemical source agricultural chemicals, environmentally friendly.
5, the valid density when composition pesticide containing Fructus meliae toosendan and black false hellebore extract uses is invented low, with low cost.
Embodiment
The present invention contains the composition pesticide of Fructus meliae toosendan and black false hellebore extract, and its active component is jointly extracted by the crude drug of following weight portion and forms: Fructus meliae toosendan 1 part, black false hellebore 0.5 ~ 6 part; Be preferably Fructus meliae toosendan 1 part, black false hellebore 1 ~ 4 part; Be more preferably Fructus meliae toosendan 1 part, black false hellebore 1 ~ 3 part; More preferably Fructus meliae toosendan 1 part, black false hellebore 2 parts.
Wherein, the Fructus meliae toosendan that the present invention adopts and black false hellebore are Chinese herbal medicine raw material, contain the activity of the composition pesticide of Fructus meliae toosendan and black false hellebore extract in order to improve the present invention, the Fructus meliae toosendan that Fructus meliae toosendan is preferably dry, the black false hellebore rhizome that black false hellebore is preferably dry.
Further, preferably, the present invention jointly to be extracted through ethanolic solution by Fructus meliae toosendan and black false hellebore containing the active component of the composition pesticide of Fructus meliae toosendan and black false hellebore extract and forms; Or the black false hellebore extract that the Sichuan chinaberry extract to be obtained through alcohol extract by Fructus meliae toosendan, black false hellebore obtain through alcohol extract mixes; Described concentration of alcohol is 50 ~ 90%v/v, is preferably 80%v/v.
Wherein, in order to improve the effect of the present invention containing the composition pesticide of Fructus meliae toosendan and black false hellebore extract, the present invention preferably jointly to be extracted through ethanolic solution by Fructus meliae toosendan and black false hellebore containing the active component of the composition pesticide of Fructus meliae toosendan and black false hellebore extract and forms;
Further, in order to improve the activity of the composition pesticide containing Fructus meliae toosendan and black false hellebore extract, be convenient to store and transport, the described composition pesticide containing Fructus meliae toosendan and black false hellebore extract can be prepared as the conventional formulations of pesticide, is preferably microemulsion, soluble concentrate or aqua simultaneously.
Further, in order to improve the stability of the composition pesticide containing Fructus meliae toosendan and black false hellebore extract, described containing in the composition pesticide of Fructus meliae toosendan and black false hellebore extract also comprises auxiliary agent, described auxiliary agent can adopt the usual auxiliaries in composition, as at least one in emulsifier, antifreeze, solvent, defoamer, dispersant, wetting agent, stabilizing agent.
Wherein, emulsifier can adopt at least one in non-ionic surface active agent and anion surfactant, described non-ionic surface active agent can be dibenzyl xenyl APEO, styryl phenyl APEO, styryl phenyl APEO, phenethyl phenyl polyoxyethylene one polyethenoxy ether, OPEO, alkylphenol polyoxyethylene sulfosuccinate, aliphatic acid polyethenoxy ether, fatty alcohol-polyoxyethylene ether, aliphatic amine polyoxyethylene ether, castor oil ethylene oxide adduct and derivative thereof, at least one in polyol fatty acid ester and ethylene oxide adduct etc. thereof, described anion surfactant is at least one in calcium dodecyl benzene sulfonate, alkylphenol polyoxyethylene phosphate, phenethyl phenol polyethenoxy ether phosphate etc., as emulsifier 500,601p, 602p etc., in addition, commercially available emulsifier production can also be used.
Wherein, solvent can adopt at least one in water, ethanol, isopropyl alcohol, n-butanol, ethyl acetate, butyl acetate, methyl-sulfoxide, turpentine oil, solvent naphtha, 1-METHYLPYRROLIDONE, dimethyl formamide etc.
Wherein, antifreeze can be glycerine, propane diols, ethylene glycol, sodium chloride, calcium chloride, sorbierite etc.
Wherein, defoamer is silicone defoaming agent etc.
Wherein, dispersant is at least one in lignosulfonates, PAA and propionamide copolymer, alkylnaphthalene sulfonate, polycarboxylic acid salt's condensation product, methyl sodiosul foaliphatate etc.
Wherein, wetting agent can be alkyl sulfate, alkylbenzenesulfonate, alkylnaphthalene sulfonate, aliphatic alcohol polyethenoxy base ether, alkylphenol-polyethenoxy base ether, sorbitan fatty acid ester etc.; Described stabilizing agent can be 2-expoxy propane, butyl glycidyl ether, isopropyl alcohol, n-butanol, polyethylene glycol etc.
Further, preferably, the soluble concentrate that the present invention contains the composition pesticide of Fructus meliae toosendan and black false hellebore extract is made up of the component of following weight portion: Fructus meliae toosendan and black false hellebore extract, 15 parts of emulsifier 508,5 parts of emulsifier, 506,20 parts of ethanol, 5 parts of dimethyl sulfoxide (DMSO)s, 5 parts of ethylene glycol, 20 parts of water; Wherein, Fructus meliae toosendan and black false hellebore extract are that the crude drug of 30 weight portions jointly extracts and forms.
For the ease of storing and transport, extract can be concentrated, obtain concentrate, and then be prepared into various formulation, cycles of concentration can according to needs of production from Row sum-equal matrix, preferably, Fructus meliae toosendan is prepared from by the following method with black false hellebore extract: crude drug is through extracting and being concentrated into identical with crude drug weight.
Further, after measured, the present invention has synergistic function containing Fructus meliae toosendan and the toosendanin in the composition pesticide active component of black false hellebore extract, other active insecticidal components that jervine is identical with jervine with essential groups, therefore, the independent extract that the composition pesticide effect prepared by common extract is better than the two mixes the composition pesticide prepared.Meanwhile, through inventor's lot of experiments, find the composition pesticide adopting toosendanin and jervine binary built to obtain, although activity is a little less than extract, but still there is certain activity.Therefore, from cost-saving angle, the active component that the present invention contains the composition pesticide of Fructus meliae toosendan and black false hellebore extract also can be made up of toosendanin and jervine, and wherein, the mass ratio of toosendanin and jervine is 1:0.5 ~ 6, is preferably 1:2.
Further, the invention also discloses the preparation method that the present invention contains the composition pesticide of Fructus meliae toosendan and black false hellebore extract, wherein, according to Fructus meliae toosendan and black false hellebore be raw material prepare the composition pesticide of the present invention containing Fructus meliae toosendan and black false hellebore extract time, can following methods be adopted:
Method (one):
A, extraction: take Fructus meliae toosendan particle and black false hellebore particle, mixing, adds solvent by solid-liquid ratio 1:3 ~ 12g/ml, in 60 ~ 95 DEG C of refluxing extraction, filters, obtains extract;
B, preparation: extract is made microemulsion, soluble concentrate or aqua.
Method (two):
A, extraction: take Fructus meliae toosendan particle, add ethanolic solution by solid-liquid ratio 1:3 ~ 12g/ml, in 60 ~ 95 DEG C of refluxing extraction, filters, obtain Fructus meliae toosendan extract;
Take black false hellebore particle, add ethanolic solution by solid-liquid ratio 1:3 ~ 12g/ml, in 60 ~ 95 DEG C of refluxing extraction, filter, obtain black false hellebore extract;
B, preparation: by Fructus meliae toosendan extract and the mixing of black false hellebore extract, and make microemulsion, soluble concentrate or aqua.
Wherein, in said method () and (two), Fructus meliae toosendan particle and black false hellebore particle can adopt commercially available particle, conventional method also can be adopted to pulverize Fructus meliae toosendan and black false hellebore rhizome obtains.In order to improve the effect of extraction, simultaneously cost-saving, Fructus meliae toosendan particle and black false hellebore particle cross 60 ~ 100 mesh sieves, preferred mistake 80 mesh sieve.
Further, in order to cost-saving, simultaneously also in order to improve extraction efficiency, the solid-liquid ratio in a step is preferably 1:4 ~ 10g/ml, is more preferably 1:6g/ml.Namely the Fructus meliae toosendan of lg and black false hellebore particle add 3 ~ 12ml solvent extraction, preferably add 4 ~ 10ml, more preferably add 6ml.
In order to improve dissolution rate, ensure extraction efficiency, described solvent is preferably the ethanol of 50 ~ 90%v/v simultaneously, is more preferably 80%v/v ethanol.
In order to shorten preparation time, accelerate extraction rate, can stir when adding hot reflux, mixing speed is preferably 80 ~ 100 revs/min.
Further, reflux temperature is preferably 75 ~ 85 DEG C, is more preferably 82 DEG C; Reflow's cycle is twice, and each return time is 2 hours, and merging filtrate obtains corresponding extract.
Further, the invention also discloses the application of composition pesticide in control crop pest containing Fructus meliae toosendan and black false hellebore extract, wherein, described crop pest is preferably acarina pest; Common acarina pest has Panonychus citri, Tetranychus cinnabarinus, yellow tea mite etc.
In the agricultural production of reality, in order to improve composition pesticide containing Fructus meliae toosendan and black false hellebore extract to the control efficiency of insect pest, the described composition pesticide containing Fructus meliae toosendan and black false hellebore extract is preferably applied to crop pest initial stage of origination; The present invention can use by common method containing the composition pesticide of Fructus meliae toosendan and black false hellebore extract, sprays on crop blade face.Preferably, the composition pesticide containing Fructus meliae toosendan and black false hellebore extract as the present invention adopts Fructus meliae toosendan and black false hellebore extraction to be prepared from, be diluted with water to when then using with the activity component concentration of crude drug weighing scale as 10 ~ 100ppm, namely the composition pesticide that 1g crude drug is obtained after extracting, when using, be diluted with water to 10kg, then its activity component concentration equals 100ppm; Preferably being diluted to further with the activity component concentration of crude drug weighing scale is that 20 ~ 50ppm sprays in plant blade face.When the present invention containing the composition pesticide of Fructus meliae toosendan and black false hellebore extract adopt toosendanin and jervine composite as active component time, being then diluted with water to activity component concentration in composition pesticide when using is 10 ~ 100ppm; Preferably being diluted to jervine concentration is further that 20 ~ 50ppm sprays in plant blade face.When spraying, so that water membrane to appear in blade face, not lower of liquid is advisable; Secondary dispenser is carried out, the preferred continuous administration of a season crop 2 ~ 3 times after being preferable over 3 ~ 5 days.
Below in conjunction with embodiment, the specific embodiment of the present invention is further described, does not therefore limit the present invention among described scope of embodiments.
Embodiment 1 the present invention contains the preparation of the composition pesticide of Fructus meliae toosendan and black false hellebore extract
A, extraction: take dry Fructus meliae toosendan and black false hellebore rhizome, mixing, pulverizes, and crosses 80 mesh sieves, adds solvent, refluxing extraction twice, filters, merging filtrate, concentrated, makes extract weight equal the weight of crude drug, obtains extract cl-01 ~ cl-06; Wherein, each parameter is in table 1;
B, preparation: in extract cl-01 ~ cl-06, add auxiliary agent in table 2, stir, must contain the composition pesticide CL-01 ~ CL-06 of Fructus meliae toosendan and black false hellebore extract.
Table 1
Wherein, the Fructus meliae toosendan used in the present invention and black false hellebore are all purchased from Anguo City Zhong Tian prepared slices of Chinese crude drugs Co., Ltd.
Table 2
Embodiment 2 the present invention contains the preparation of the composition pesticide of Fructus meliae toosendan and black false hellebore extract
A, extraction: take dry Fructus meliae toosendan, pulverize, and crosses 80 mesh sieves, add solvent, refluxing extraction twice, filters, merging filtrate, and concentrated, make extract weight equal the weight of crude drug, obtain extract d1-01 ~ d1-03, wherein, each parameter is in table 3;
Take dry black false hellebore rhizome, pulverize, cross 80 mesh sieves, add solvent, refluxing extraction twice, filter, merging filtrate, concentrated, make extract weight equal the weight of crude drug, obtain extract d2-01 ~ d2-03, wherein, each parameter is in table 4;
B, preparation: take Fructus meliae toosendan extract, black false hellebore extract and auxiliary agent, stirring and evenly mixing, obtain the composition pesticide CL-07 ~ CL-12 containing Fructus meliae toosendan and black false hellebore extract, wherein, each parameter is in table 5.
Table 3
Continued 3
Table 4
Table 5
Embodiment 3 the present invention contains the preparation of the composition pesticide of Fructus meliae toosendan and black false hellebore extract
Take toosendanin and jervine and auxiliary agent according to proportioning in table 6, mixing, stir, stirring and evenly mixing, obtains the composition pesticide CL-13 ~ CL-18 containing Fructus meliae toosendan and black false hellebore extract.
Table 6
Continued 6
Wherein, toosendanin and jervine are all purchased from Xi'an Lin He Bioisystech Co., Ltd.
Test example 1 the present invention contains the composition pesticide eggplant Tetranychus cinnabarinus efficiency test of Fructus meliae toosendan and black false hellebore extract
1 test material
1.1 for studying thing and object: eggplant Tetranychus cinnabarinus
1.2 medicament
Test medicine: CL-01 ~ CL-18;
Fructus meliae toosendan single dose (D1); Toosendanin single dose (D2); Black false hellebore single dose (D3); Jervine single dose (D4);
Contrast medicament: 1.5% abamectin emulsifiable concentrate (CK-01), purchased from Hailir Pharmaceutical Group Co., Ltd.;
Clear water contrast (CK-02).
Wherein, the preparation method of Fructus meliae toosendan single dose is: the d1-04 getting 30g, and add 15g emulsifier 508,5g emulsifier 506,20g ethanol, 5g dimethyl sulfoxide (DMSO), 5g ethylene glycol, 20g water, stirring and evenly mixing, to obtain final product.
Black false hellebore single dose preparation method is: the d2-04 getting 30g, and add 15g emulsifier 508,5g emulsifier 506,20g ethanol, 5g dimethyl sulfoxide (DMSO), 5g ethylene glycol, 20g water, stirring and evenly mixing, to obtain final product.
The preparation method of toosendanin single dose is: the toosendanin getting 30g, and add 15g emulsifier 508,5g emulsifier 506,20g ethanol, 5g dimethyl sulfoxide (DMSO), 5g ethylene glycol, 20g water, stirring and evenly mixing, to obtain final product.
Jervine single dose preparation method is: the jervine getting 30g, and add 15g emulsifier 508,5g emulsifier 506,20g ethanol, 5g dimethyl sulfoxide (DMSO), 5g ethylene glycol, 20g water, stirring and evenly mixing, to obtain final product.
2, experimental scheme and method
This test 18 medicaments, 4 single dose contrasts, 1 contrast medicament, 1 blank, repeats for three times, Gong72Ge community.Minizone and surrounding all leave isolation strip, plot area 12m 2, community respectively processes randomized arrangement.
By medicament CL-01 ~ CL-12, D1, D3 thin up to the activity component concentration of crude drug weighing scale for 50ppm; Be 50ppm by CL-13 ~ CL-18, D2, D4 thin up to activity component concentration; Contrast medicament CK-02 thin up is 50ppm to activity component concentration; And spray application to plant blade face, so that water membrane to appear in blade face, not lower of liquid is advisable.
Be fixed the eggplant Tetranychus cinnabarinus quantity statistics of blade before the test and listing mark.Within 5 days after dispenser, investigate and record the Tetranychus cinnabarinus number alive on each blade, each group is repeated meter of averaging, and calculate Revision insect recluced rate and preventive effect, it the results are shown in Table 7.
In formula:
Borer population alive before PT0---chemicals treatment district medicine;
PT1---borer population of living after chemicals treatment district medicine;
Borer population alive before CK0---blank district medicine;
CK1---borer population of living after blank district medicine.
Table 7
Test medicine Radix before medicine Five days borer populations alive after medicine Revision insect recluced rate (%) Preventive effect (%)
CL-01 361 111 69.25 74.32
CL-02 355 98 72.39 76.94
CL-03 349 90 74.21 78.46
CL-04 386 96 75.13 79.23
CL-05 399 108 72.93 77.39
CL-06 347 96 72.33 76.89
CL-07 371 157 57.68 64.66
CL-08 326 135 58.59 65.41
CL-09 309 119 61.49 67.84
Continued 7
CL-10 385 138 64.16 70.06
CL-11 366 139 62.02 68.28
CL-12 346 138 60.12 66.69
CL-13 351 97 72.36 76.92
CL-14 328 84 74.39 78.61
CL-15 375 93 75.20 79.29
CL-16 386 87 77.46 81.18
CL-17 342 85 75.15 79.24
CL-18 318 82 74.21 78.46
D1 325 211 35.08 45.78
D2 339 194 42.77 52.21
D3 384 235 38.80 48.89
D4 357 178 50.14 58.36
CK-01 356 76 78.65 82.17
CK-02 304 364 -19.74 ——
3.2 result of the test
As shown in Table 7, the present invention has good preventive effect containing the composition pesticide of Fructus meliae toosendan and black false hellebore extract to Tetranychus cinnabarinus.
The preventive effect of the composition pesticide (CL-01 ~ CL-06) adopting common extracting method to make is apparently higher than the composition pesticide (CL-07 ~ CL-012) be mixed to get after extracting separately, and visible common extraction contributes to improving dissolution rate, improves insecticide efficiency; And the control efficiency of black false hellebore single dose D3 that the Fructus meliae toosendan single dose D1 be prepared from than single Sichuan chinaberry extract and black false hellebore extract are prepared from is good, visible, has synergistic function between product compositions of the present invention.
Meanwhile, adopt the preventive effect of toosendanin and the composite composition pesticide (CL-13 ~ CL-18) obtained of jervine also apparently higher than toosendanin single dose D2 and jervine single dose D4, visible, toosendanin and jervine is composite has synergistic function.
In addition, have no during dispenser and have poisoning to show to plant.
Test example 2 the present invention contains the composition pesticide panonychus citri efficiency test of Fructus meliae toosendan and black false hellebore extract
Products C L-01 of the present invention ~ CL-18 is used for preventing and treating panonychus citri.This test 18 medicaments, 4 single dose contrasts, 1 blank, repeats for three times, Gong69Ge community.Minizone and surrounding all leave isolation strip, plot area 12m 2, community respectively processes randomized arrangement.
By medicament CL-01 ~ CL-12, D1, D3 thin up to the activity component concentration of crude drug weighing scale for 50ppm; Be 50ppm by CL-13 ~ CL-18, D2, D4 thin up to activity component concentration; And spray application to plant blade face, so that water membrane to appear in blade face, not lower of liquid is advisable.
Be fixed the Panonychus citri quantity statistics alive of blade before the test and listing mark.Within 5 days after dispenser, investigate and record the Panonychus citri number alive on each blade, each group is repeated meter of averaging, and calculate Revision insect recluced rate and preventive effect, it the results are shown in Table 8.
In formula:
Borer population alive before PT0---chemicals treatment district medicine;
PT1---borer population of living after chemicals treatment district medicine;
Borer population alive before CK0---blank district medicine;
CK1---borer population of living after blank district medicine.
Table 8
Test medicine Radix before medicine Five days borer populations alive after medicine Revision insect recluced rate (%) Preventive effect (%)
CL-01 411 122 70.32 73.27
CL-02 425 120 71.76 74.58
CL-03 392 103 73.72 76.34
CL-04 406 89 78.08 80.26
CL-05 414 99 76.09 78.47
CL-06 456 127 72.15 74.92
CL-07 471 182 61.36 65.21
CL-08 485 177 63.51 67.14
CL-09 492 171 65.24 68.71
CL-10 422 137 67.54 70.77
CL-11 405 136 66.42 69.76
Continued 8
CL-12 441 156 64.63 68.15
CL-13 438 109 75.11 77.59
CL-14 486 110 77.37 79.62
CL-15 454 99 78.19 80.37
CL-16 419 87 79.24 81.30
CL-17 428 103 75.93 78.33
CL-18 440 103 76.59 78.92
D1 408 256 37.25 43.50
D2 471 253 46.28 51.63
D3 466 271 41.85 47.64
D4 428 209 51.17 56.03
CK-02 452 502 -11.06 ——
As shown in Table 8, the present invention has good preventive effect containing the composition pesticide of Fructus meliae toosendan and black false hellebore extract to Tetranychus cinnabarinus.
The preventive effect of the composition pesticide (CL-01 ~ CL-06) adopting common extracting method to make is apparently higher than the composition pesticide (CL-07 ~ CL-012) be mixed to get after extracting separately, and visible common extraction contributes to improving dissolution rate, improves insecticide efficiency; And the control efficiency of black false hellebore single dose D3 that the Fructus meliae toosendan single dose D1 be prepared from than single Sichuan chinaberry extract and black false hellebore extract are prepared from is good, visible, has synergistic function between product compositions of the present invention.
Meanwhile, adopt the preventive effect of toosendanin and the composite composition pesticide (CL-13 ~ CL-18) obtained of jervine also apparently higher than toosendanin single dose D2 and jervine single dose D4, visible, toosendanin and jervine is composite has synergistic function.
In addition, have no during dispenser and have poisoning to show to plant.
Test example 3 the present invention contains the composition pesticide tealeaves yellow tea mite efficiency test of Fructus meliae toosendan and black false hellebore extract
Products C L-01 of the present invention ~ CL-18 is used for preventing and treating tealeaves yellow tea mite.This test 18 medicaments, 4 single dose contrasts, 1 blank, repeats for three times, Gong69Ge community.Minizone and surrounding all leave isolation strip, plot area 12m 2, community respectively processes randomized arrangement.
By medicament CL-01 ~ CL-12, D1, D3 thin up to the activity component concentration of crude drug weighing scale for 50ppm; Be 50ppm by CL-13 ~ CL-18, D2, D4 thin up to activity component concentration; And spray application to plant blade face, so that water membrane to appear in blade face, not lower of liquid is advisable.
Be fixed the yellow tea mite quantity statistics alive of blade before the test and listing mark.Within 5 days after dispenser, investigate and record the yellow tea mite number alive on each blade, each group is repeated meter of averaging, and calculate Revision insect recluced rate and preventive effect, it the results are shown in Table 9.
In formula:
Borer population alive before PT0---chemicals treatment district medicine;
PT1---borer population of living after chemicals treatment district medicine;
Borer population alive before CK0---blank district medicine;
CK1---borer population of living after blank district medicine.
Table 9
Test medicine Radix before medicine Five days borer populations alive after medicine Revision insect recluced rate (%) Preventive effect (%)
CL-01 194 62 68.04 72.69
CL-02 147 44 70.07 74.42
CL-03 151 38 74.83 78.49
CL-04 137 29 78.83 81.91
CL-05 181 46 74.59 78.28
CL-06 190 50 73.68 77.51
CL-07 111 50 54.95 61.51
CL-08 155 65 58.06 64.16
CL-09 192 74 61.46 67.06
CL-10 133 45 66.17 71.09
CL-11 156 56 64.10 69.32
CL-12 178 66 62.92 68.31
CL-13 185 48 74.05 77.83
CL-14 138 35 74.64 78.33
Continued 9
CL-15 159 39 75.47 79.04
CL-16 167 38 77.25 80.56
CL-17 205 51 75.12 78.74
CL-18 160 42 73.75 77.57
D1 192 130 32.29 42.14
D2 185 110 40.54 49.19
D3 188 119 36.70 45.91
D4 105 55 47.62 55.24
CK-02 141 165 -17.02 ——
As shown in Table 9, the present invention has good preventive effect containing the composition pesticide of Fructus meliae toosendan and black false hellebore extract to Tetranychus cinnabarinus.
The preventive effect of the composition pesticide (CL-01 ~ CL-06) adopting common extracting method to make is apparently higher than the composition pesticide (CL-07 ~ CL-012) be mixed to get after extracting separately, and visible common extraction contributes to improving dissolution rate, improves insecticide efficiency; And the control efficiency of black false hellebore single dose D3 that the Fructus meliae toosendan single dose D1 be prepared from than single Sichuan chinaberry extract and black false hellebore extract are prepared from is good, visible, has synergistic function between product compositions of the present invention.
Meanwhile, adopt the preventive effect of toosendanin and the composite composition pesticide (CL-13 ~ CL-18) obtained of jervine also apparently higher than toosendanin single dose D2 and jervine single dose D4, visible, toosendanin and jervine is composite has synergistic function.
In addition, have no during dispenser and have poisoning to show to plant.

Claims (25)

1. contain the composition pesticide of Fructus meliae toosendan and black false hellebore extract, it is characterized in that, its active component is extracted by the crude drug of following weight portion and forms: Fructus meliae toosendan 1 part, black false hellebore 0.5 ~ 6 part; Its extracting method is: take Fructus meliae toosendan particle and black false hellebore particle, and mixing, adds solvent by solid-liquid ratio 1:3 ~ 12g/ml, and in 60 ~ 95 DEG C of refluxing extraction, filter, obtain extract, wherein, described solvent is organic solvent or water; Described organic solvent is methyl alcohol, ethanol, ethyl acetate, acetone, chloroform.
2. the composition pesticide containing Fructus meliae toosendan and black false hellebore extract according to claim 1, its active component is extracted by the crude drug of following weight portion and forms: Fructus meliae toosendan 1 part, black false hellebore 1 ~ 4 part.
3. the composition pesticide containing Fructus meliae toosendan and black false hellebore extract according to claim 2, its active component is extracted by the crude drug of following weight portion and forms: Fructus meliae toosendan 1 part, black false hellebore 1 ~ 3 part.
4. the composition pesticide containing Fructus meliae toosendan and black false hellebore extract according to claim 3, its active component is extracted by the crude drug of following weight portion and forms: Fructus meliae toosendan 1 part, black false hellebore 2 parts.
5. the composition pesticide containing Fructus meliae toosendan and black false hellebore extract according to any one of Claims 1 to 4, is characterized in that: its active component is jointly extracted by Fructus meliae toosendan and black false hellebore and forms.
6. the composition pesticide containing Fructus meliae toosendan and black false hellebore extract according to any one of Claims 1 to 4, is characterized in that: the described composition pesticide containing Fructus meliae toosendan and black false hellebore extract is microemulsion, soluble concentrate or aqua.
7. the composition pesticide containing Fructus meliae toosendan and black false hellebore extract according to claim 5, is characterized in that: the described composition pesticide containing Fructus meliae toosendan and black false hellebore extract is microemulsion, soluble concentrate or aqua.
8. the composition pesticide containing Fructus meliae toosendan and black false hellebore extract according to any one of Claims 1 to 4, it is characterized in that: described containing in the composition pesticide of Fructus meliae toosendan and black false hellebore extract also comprises auxiliary agent, and described auxiliary agent is at least one in emulsifier, antifreeze, solvent, defoamer, dispersant, wetting agent, stabilizing agent.
9. the composition pesticide containing Fructus meliae toosendan and black false hellebore extract according to claim 5, it is characterized in that: described containing in the composition pesticide of Fructus meliae toosendan and black false hellebore extract also comprises auxiliary agent, and described auxiliary agent is at least one in emulsifier, antifreeze, solvent, defoamer, dispersant, wetting agent, stabilizing agent.
10. the composition pesticide containing Fructus meliae toosendan and black false hellebore extract according to claim 6, it is characterized in that: described containing in the composition pesticide of Fructus meliae toosendan and black false hellebore extract also comprises auxiliary agent, and described auxiliary agent is at least one in emulsifier, antifreeze, solvent, defoamer, dispersant, wetting agent, stabilizing agent.
11. composition pesticides containing Fructus meliae toosendan and black false hellebore extract according to claim 7, it is characterized in that: described containing in the composition pesticide of Fructus meliae toosendan and black false hellebore extract also comprises auxiliary agent, and described auxiliary agent is at least one in emulsifier, antifreeze, solvent, defoamer, dispersant, wetting agent, stabilizing agent.
12. composition pesticides containing Fructus meliae toosendan and black false hellebore extract according to claim 6, it is characterized in that, described soluble concentrate is made up of the component of following weight portion: Fructus meliae toosendan and black false hellebore extract, 15 parts of emulsifier 508,5 parts of emulsifier, 506,20 parts of ethanol, 5 parts of dimethyl sulfoxide (DMSO)s, 5 parts of ethylene glycol, 20 parts of water; Wherein, Fructus meliae toosendan and black false hellebore extract are that the crude drug of 30 weight portions jointly extracts and forms; Fructus meliae toosendan is prepared from by the following method with black false hellebore extract: crude drug is through extracting and being concentrated into identical with crude drug weight.
13. composition pesticides containing Fructus meliae toosendan and black false hellebore extract according to claim 7, it is characterized in that, described soluble concentrate is made up of the component of following weight portion: Fructus meliae toosendan and black false hellebore extract, 15 parts of emulsifier 508,5 parts of emulsifier, 506,20 parts of ethanol, 5 parts of dimethyl sulfoxide (DMSO)s, 5 parts of ethylene glycol, 20 parts of water; Wherein, Fructus meliae toosendan and black false hellebore extract are that the crude drug of 30 weight portions jointly extracts and forms; Fructus meliae toosendan is prepared from by the following method with black false hellebore extract: crude drug is through extracting and being concentrated into identical with crude drug weight.
14. composition pesticides containing Fructus meliae toosendan and black false hellebore extract according to claim 10, it is characterized in that, described soluble concentrate is made up of the component of following weight portion: Fructus meliae toosendan and black false hellebore extract, 15 parts of emulsifier 508,5 parts of emulsifier, 506,20 parts of ethanol, 5 parts of dimethyl sulfoxide (DMSO)s, 5 parts of ethylene glycol, 20 parts of water; Wherein, Fructus meliae toosendan and black false hellebore extract are that the crude drug of 30 weight portions jointly extracts and forms; Fructus meliae toosendan is prepared from by the following method with black false hellebore extract: crude drug is through extracting and being concentrated into identical with crude drug weight.
15. composition pesticides containing Fructus meliae toosendan and black false hellebore extract according to claim 11, it is characterized in that, described soluble concentrate is made up of the component of following weight portion: Fructus meliae toosendan and black false hellebore extract, 15 parts of emulsifier 508,5 parts of emulsifier, 506,20 parts of ethanol, 5 parts of dimethyl sulfoxide (DMSO)s, 5 parts of ethylene glycol, 20 parts of water; Wherein, Fructus meliae toosendan and black false hellebore extract are that the crude drug of 30 weight portions jointly extracts and forms; Fructus meliae toosendan is prepared from by the following method with black false hellebore extract: crude drug is through extracting and being concentrated into identical with crude drug weight.
16. containing the composition pesticide of Fructus meliae toosendan and black false hellebore extract, and it is characterized in that: its active component is made up of toosendanin and jervine, wherein, the mass ratio of toosendanin and jervine is 1:0.5 ~ 6; Its extracting method is: take toosendanin and jervine, and mixing, adds solvent by solid-liquid ratio 1:3 ~ 12g/ml, and in 60 ~ 95 DEG C of refluxing extraction, filter, obtain extract, wherein, described solvent is organic solvent or water; Described organic solvent is methyl alcohol, ethanol, ethyl acetate, acetone, chloroform.
17. composition pesticides containing Fructus meliae toosendan and black false hellebore extract according to claim 16, is characterized in that: the mass ratio of toosendanin and jervine is 1:2.
The preparation method containing the composition pesticide of Fructus meliae toosendan and black false hellebore extract described in 18. any one of claim 1 ~ 15, is characterized in that being made up of following steps:
A, extraction: take Fructus meliae toosendan particle and black false hellebore particle, mixing, adds solvent by solid-liquid ratio 1:3 ~ 12g/ml, and in 60 ~ 95 DEG C of refluxing extraction, filter, obtain extract, wherein, described solvent is organic solvent or water;
B, preparation: extract is made microemulsion, soluble concentrate or aqua.
19. preparation methods containing the composition pesticide of Fructus meliae toosendan and black false hellebore extract according to claim 18, it is characterized in that: in described a step, Fructus meliae toosendan particle and black false hellebore particle cross 60 ~ 100 mesh sieves; Solid-liquid ratio is 1:4 ~ 10g/ml; Organic solvent is methyl alcohol, ethanol, ethyl acetate, acetone, chloroform; Reflux temperature is 75 ~ 85 DEG C; Reflow's cycle is twice, and merging filtrate, obtains extract.
20. preparation methods containing the composition pesticide of Fructus meliae toosendan and black false hellebore extract according to claim 19, it is characterized in that: in described a step, Fructus meliae toosendan particle and black false hellebore particle cross 80 mesh sieves; Solid-liquid ratio is 6g/ml; Organic solvent is the ethanol of 50 ~ 90%v/v; Reflux temperature is 82 DEG C.
21. preparation methods containing the composition pesticide of Fructus meliae toosendan and black false hellebore extract according to claim 20, is characterized in that: described organic solvent is 80%v/v ethanol.
The application of the composition pesticide containing Fructus meliae toosendan and black false hellebore extract described in 22. any one of claim 1 ~ 15 in control crop pest, is characterized in that: described insect pest is acarina pest; During application, be diluted with water to the activity component concentration of crude drug weighing scale as 10 ~ 100ppm.
23. application of composition pesticide in control crop pest containing Fructus meliae toosendan and black false hellebore extract according to claim 22, is characterized in that: during application, are diluted with water to the activity component concentration of crude drug weighing scale as 20 ~ 50ppm.
The application of the composition pesticide containing Fructus meliae toosendan and black false hellebore extract described in 24. claims 16 or 17 in control crop pest, is characterized in that: described insect pest is acarina pest; During application, to be diluted with water to active component be concentration is 10 ~ 100ppm.
The 25. described application of composition pesticides in control crop pest containing Fructus meliae toosendan and black false hellebore extract according to claim 24, is characterized in that: during application, and to be diluted with water to active component be concentration is 20 ~ 50ppm.
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