CN103651592B - Containing composition pesticide and the preparation method and application of Dalmatian chrysanthemum and extract from Lantana camara - Google Patents

Containing composition pesticide and the preparation method and application of Dalmatian chrysanthemum and extract from Lantana camara Download PDF

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CN103651592B
CN103651592B CN201310740374.2A CN201310740374A CN103651592B CN 103651592 B CN103651592 B CN 103651592B CN 201310740374 A CN201310740374 A CN 201310740374A CN 103651592 B CN103651592 B CN 103651592B
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dalmatian chrysanthemum
lantana
extract
composition pesticide
hexane
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CN103651592A (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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    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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    • Y02A50/00TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
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Abstract

The present invention relates to the composition pesticide and its preparation method and application containing Dalmatian chrysanthemum and lantana extract, belong to pesticide field.The technical problem to be solved in the present invention is to provide the composition pesticide and its preparation method and application containing Dalmatian chrysanthemum and lantana extract.The composition pesticide containing Dalmatian chrysanthemum and lantana extract of the present invention, its active component is extracted by the crude drug of following weight portion and forms: Dalmatian chrysanthemum 1 part, lantana 0.2 ~ 4 part.After its active component can be mixed by crude drug Dalmatian chrysanthemum and lantana, common extraction forms; Also Dalmatian chrysanthemum can be extracted separately and obtain pyrethrum extract, lantana extracts separately and obtains lantana extract, then is mixed by two kinds of extracts.The present invention can be good at killing Homoptera, Semiptera, lepidoptera pest containing the composition pesticide of Dalmatian chrysanthemum and lantana extract, has positive effect for agricultural production.

Description

Containing composition pesticide and the preparation method and application of Dalmatian chrysanthemum and extract from Lantana camara
Technical field
The present invention relates to the composition pesticide and its preparation method and application containing Dalmatian chrysanthemum and extract from Lantana camara, belong to pesticide field.
Background technology
Dalmatian chrysanthemum is Chrysanthemum herbaceos perennial, inflorescence is containing pyrethrin, arrow pigment (jaceeidin), apiolin, cyanidenon, stilbene dish element-7-gala grain aldehydic acid first stem ether, apiolin-7-glucuronic acid, sesquiterpene lactone: [determine A (tatridinA) in tower, Ta Liding B (taridinB), (llR)-ll, A (llR)-11 is determined in 13 dihydro towers, 13-dihydrotatridin-A] etc., the powder process of Dalmatian chrysanthemum (Chryaanthemumcinerariaefotiumvis) all herbal medicine, can be used for controlling mange outside human body, also cut-flower is used as, flower border is for viewing and admiring, flower dries abrasive dust, insecticide can be made.
Lantana is Lantana herbaceos perennial, herb is containing lantana element (tanacetin), lantana alcohol A, lantana alcohol B (tanacetolA, B), in volatile oil, composition has absinthol, leaf Han viburnitol, flower containing the long pinane-2 of cis, 7-diketone (cislongipinane-2,7-dione).
Inventor finds through a large amount of experiments, lantana and the common extract of Dalmatian chrysanthemum or by extract from Lantana camara and pyrethrum extract mixing, insecticidal active ingredient wherein has synergistic function, can be good at killing Homoptera, Semiptera, lepidoptera pest, for agricultural production, there is positive effect.
Summary of the invention
The technical problem to be solved in the present invention is to provide composition pesticide containing Dalmatian chrysanthemum and extract from Lantana camara and preparation method and application.
The present invention contains the composition pesticide of Dalmatian chrysanthemum and extract from Lantana camara, and its active component is extracted by the crude drug of following weight portion and forms: Dalmatian chrysanthemum 1 part, lantana 0.2 ~ 4 part.Wherein, active component is preferably extracted by the crude drug of following weight portion and forms: Dalmatian chrysanthemum 1 part, lantana 0.5 ~ 2 part; Be more preferably and formed by the crude drug extraction of following weight portion: Dalmatian chrysanthemum 1 part, lantana 0.5 ~ 1.5 part; More preferably extracted by the crude drug of following weight portion and form: Dalmatian chrysanthemum 1 part, lantana 1 part.
Wherein, the Dalmatian chrysanthemum that the present invention adopts and lantana are Chinese herbal medicine, contain the activity of the composition pesticide of Dalmatian chrysanthemum and extract from Lantana camara in order to improve the present invention, the Dalmatian chrysanthemum petal that Dalmatian chrysanthemum is preferably dry, the Leaves of Lantana Camara that lantana is preferably dry.
The present invention contains the composition pesticide of Dalmatian chrysanthemum and extract from Lantana camara, and after its active component can be mixed by crude drug Dalmatian chrysanthemum and lantana, common extraction forms; Also first can be extracted separately by Dalmatian chrysanthemum and obtain pyrethrum extract, lantana is extracted separately and obtains extract from Lantana camara, then is mixed by two kinds of extracts; Wherein, extracting solvent for use is n-hexane-ethanolic solution, and in described n-hexane-ethanolic solution, n-hexane content is 50 ~ 100%v/v, and be preferably 70 ~ 100%v/v, optimum is 100%v/v.
In order to improve the insecticidal properties of composition pesticide of the present invention, after its active component is preferably and is mixed by Dalmatian chrysanthemum and lantana, common extraction forms.
Further, in order to improve the stability of the composition pesticide containing Dalmatian chrysanthemum and extract from Lantana camara, the present invention contains in the composition pesticide of Dalmatian chrysanthemum and extract from Lantana camara and also comprises auxiliary agent, described auxiliary agent can adopt the usual auxiliaries in agricultural chemicals, 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.; Described 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.
Wherein, stabilizing agent can be 2-expoxy propane, butyl glycidyl ether, isopropyl alcohol, n-butanol, polyethylene glycol etc.
The present invention can be prepared into any one formulation of applicable agricultural use containing the composition pesticide of Dalmatian chrysanthemum and extract from Lantana camara by the method for this area routine, for the ease of storing and transport, can make microemulsion, aqua or soluble concentrate.
Further, the soluble concentrate be preferably made up of the component of following weight portion: Dalmatian chrysanthemum and extract from Lantana camara, 8 parts of emulsifier 1601,10 parts of dimethyl sulfoxide (DMSO)s, 42 parts of ethanol, wherein, Dalmatian chrysanthemum and extract from Lantana camara are that the crude drug extraction of 40 weight portions forms.Dalmatian chrysanthemum and extract from Lantana camara can obtain for Dalmatian chrysanthemum and lantana mix rear common extraction in proportion; Also can take Dalmatian chrysanthemum and lantana in proportion, be mixed to get after extracting separately.
For the ease of storing and transport, extract can be concentrated into not containing n-hexane, obtain concentrate, and then be prepared into various formulation, cycles of concentration can according to needs of production from Row sum-equal matrix.Preferably, Dalmatian chrysanthemum and extract from Lantana camara are prepared from by the following method: crude drug, through extracting and being concentrated into not containing n-hexane, then adds ethanol and makes concentrate weight identical with crude drug weight.
Second technical problem that the present invention solves is to provide the method that preparation contains the composition pesticide of Dalmatian chrysanthemum and extract from Lantana camara.
The preparation method that the present invention contains the composition pesticide of Dalmatian chrysanthemum and extract from Lantana camara is made up of following steps:
A, extraction: take Dalmatian chrysanthemum particle and lantana particle, mixing, solvent is added by solid-liquid ratio 1:3 ~ 12g/ml, extract in 15 ~ 45 DEG C of reduced-pressure backflows, filter, obtain extract, wherein, described solvent is n-hexane-ethanolic solution, and in described n-hexane-ethanolic solution, n-hexane content is 50 ~ 100%v/v; Pressure is 0 ~ 101kPa;
B, preparation: extract is made microemulsion, soluble concentrate or aqua.
Wherein, Dalmatian chrysanthemum particle and lantana particle can adopt commercially available particle, and conventional method pulverizing Dalmatian chrysanthemum petal and Leaves of Lantana Camara also can be adopted to obtain.In order to improve the effect of extraction, simultaneously cost-saving, Dalmatian chrysanthemum particle and lantana 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 Dalmatian chrysanthemum of lg and lantana particle can add 3 ~ 12ml solvent extraction, preferably add 4 ~ 10ml, more preferably add 6ml.
In order to improve dissolution rate, ensure extraction efficiency, in described n-hexane-ethanolic solution, n-hexane content is 70 ~ 100%v/v simultaneously, is preferably 100%v/v.
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 20 ~ 30 DEG C, is more preferably 25 DEG C; Pressure is 0 ~ 101kPa; Reflow's cycle is twice, and each return time is 2.5 hours, and merging filtrate, obtains extract.
The application of the composition pesticide that the present invention also provides the present invention to contain Dalmatian chrysanthemum and extract from Lantana camara in control crop pest.The present invention contains the composition pesticide of Dalmatian chrysanthemum and extract from Lantana camara, to homoptera pest as aphid, scale insect, trialeurodes vaporariorum etc.; Semiptera is as green plant bug etc.; Lepidoptera pest such as cabbage caterpillar, diamond-back moth, prodenia litura etc. have good preventive effect.
In the agricultural production of reality, in order to improve composition pesticide containing Dalmatian chrysanthemum and extract from Lantana camara to the control efficiency of insect pest, the described composition pesticide containing Dalmatian chrysanthemum and extract from Lantana camara is preferably applied to insect pest of the plant initial stage of origination; The present invention can use by common method containing the composition pesticide of Dalmatian chrysanthemum and extract from Lantana camara, sprays on plant leaf surface.Preferably, when using, the present invention is diluted with water to the activity component concentration of crude drug weighing scale as 10 ~ 100ppm containing the composition pesticide of Dalmatian chrysanthemum and extract from Lantana camara, 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 active ingredient concentration is further that 20 ~ 50ppm sprays in plant blade face, and 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.
The present invention is mixed by pyrethrum extract and extract from Lantana camara containing the composition pesticide of Dalmatian chrysanthemum and extract from Lantana camara, or mix extraction by Dalmatian chrysanthemum and lantana to form, its preventive effect is far away higher than the extract of single component, particularly extract common after Dalmatian chrysanthemum and lantana mixing, owing to having solubilising, hydrotropy effect between Dalmatian chrysanthemum and lantana, the composition pesticide insecticidal effect made after common extraction is more remarkable.
Compared with prior art, the present invention has the following advantages containing the composition pesticide of Dalmatian chrysanthemum and extract from Lantana camara:
1, the present invention has synergistic function containing the composition pesticide of Dalmatian chrysanthemum and extract from Lantana camara, obvious to the control efficiency of the insects such as Homoptera, Lepidoptera, Semiptera.
2, Dalmatian chrysanthemum of the present invention and lantana mix after jointly extracting or extracting respectively, and the composition pesticide made can improve crop immune system ability while quick-acting tagging, and can significantly improve its vigor.
3, 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.
4, when the present invention uses containing the composition pesticide of Dalmatian chrysanthemum and extract from Lantana camara, valid density is low, with low cost.
Embodiment
The present invention contains the composition pesticide of Dalmatian chrysanthemum and extract from Lantana camara, and its active component is extracted by the crude drug of following weight portion and forms: Dalmatian chrysanthemum 1 part, lantana 0.2 ~ 4 part.Wherein, active component is preferably extracted by the crude drug of following weight portion and forms: Dalmatian chrysanthemum 1 part, lantana 0.5 ~ 2 part; Be more preferably and formed by the crude drug extraction of following weight portion: Dalmatian chrysanthemum 1 part, lantana 0.5 ~ 1.5 part; More preferably extracted by the crude drug of following weight portion and form: Dalmatian chrysanthemum 1 part, lantana 1 part.
Wherein, the Dalmatian chrysanthemum that the present invention adopts and lantana are Chinese herbal medicine, contain the activity of the composition pesticide of Dalmatian chrysanthemum and extract from Lantana camara in order to improve the present invention, the Dalmatian chrysanthemum petal that Dalmatian chrysanthemum is preferably dry, the Leaves of Lantana Camara that lantana is preferably dry.
The present invention contains the composition pesticide of Dalmatian chrysanthemum and extract from Lantana camara, and after its active component can be mixed by crude drug Dalmatian chrysanthemum and lantana, common extraction forms; Also first can be extracted separately by Dalmatian chrysanthemum and obtain pyrethrum extract, lantana is extracted separately and obtains extract from Lantana camara, then is mixed by two kinds of extracts; Wherein, extracting solvent for use is n-hexane-ethanolic solution, and in described n-hexane-ethanolic solution, n-hexane content is 50 ~ 100%v/v, and be preferably 70 ~ 100%v/v, optimum is 100%v/v.
In order to improve the insecticidal properties of composition pesticide of the present invention, after its active component is preferably and is mixed by Dalmatian chrysanthemum and lantana, common extraction forms.
Further, in order to improve the stability of the composition pesticide containing Dalmatian chrysanthemum and extract from Lantana camara, the present invention contains in the composition pesticide of Dalmatian chrysanthemum and extract from Lantana camara and also comprises auxiliary agent, described auxiliary agent can adopt the usual auxiliaries in agricultural chemicals, 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.; Described 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.
Wherein, stabilizing agent can be 2-expoxy propane, butyl glycidyl ether, isopropyl alcohol, n-butanol, polyethylene glycol etc.
The present invention can be prepared into any one formulation of applicable agricultural use containing the composition pesticide of Dalmatian chrysanthemum and extract from Lantana camara by the method for this area routine, for the ease of storing and transport, can make microemulsion, aqua or soluble concentrate.
Further, the soluble concentrate be preferably made up of the component of following weight portion: Dalmatian chrysanthemum and extract from Lantana camara, 8 parts of emulsifier 1601,10 parts of dimethyl sulfoxide (DMSO)s, 42 parts of ethanol, wherein, Dalmatian chrysanthemum and extract from Lantana camara are that the crude drug extraction of 40 weight portions forms.Dalmatian chrysanthemum and extract from Lantana camara can obtain for Dalmatian chrysanthemum and lantana mix rear common extraction in proportion; Also can take Dalmatian chrysanthemum and lantana in proportion, be mixed to get after extracting separately.
For the ease of storing and transport, extract can be concentrated into not containing n-hexane, obtain concentrate, and then be prepared into various formulation, cycles of concentration can according to needs of production from Row sum-equal matrix.Preferably, Dalmatian chrysanthemum and extract from Lantana camara are prepared from by the following method: crude drug, through extracting and being concentrated into not containing n-hexane, then adds ethanol and makes concentrate weight identical with crude drug weight.
Second technical problem that the present invention solves is to provide the method that preparation contains the composition pesticide of Dalmatian chrysanthemum and extract from Lantana camara.
The preparation method that the present invention contains the composition pesticide of Dalmatian chrysanthemum and extract from Lantana camara is made up of following steps:
A, extraction: take Dalmatian chrysanthemum particle and lantana particle, mixing, solvent is added by solid-liquid ratio 1:3 ~ 12g/ml, extract in 15 ~ 45 DEG C of reduced-pressure backflows, filter, obtain extract, wherein, described solvent is n-hexane-ethanolic solution, and in described n-hexane-ethanolic solution, n-hexane content is 50 ~ 100%v/v; Pressure is 0 ~ 101kPa;
B, preparation: extract is made microemulsion, soluble concentrate or aqua.
Wherein, Dalmatian chrysanthemum particle and lantana particle can adopt commercially available particle, and conventional method pulverizing Dalmatian chrysanthemum petal and Leaves of Lantana Camara also can be adopted to obtain.In order to improve the effect of extraction, simultaneously cost-saving, Dalmatian chrysanthemum particle and lantana 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 Dalmatian chrysanthemum of lg and lantana particle can add 3 ~ 12ml solvent extraction, preferably add 4 ~ 10ml, more preferably add 6ml.
In order to improve dissolution rate, ensure extraction efficiency, in described n-hexane-ethanolic solution, n-hexane content is 70 ~ 100%v/v simultaneously, is preferably 100%v/v.
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 20 ~ 30 DEG C, is more preferably 25 DEG C; Pressure is 0 ~ 101kPa; Reflow's cycle is twice, and each return time is 2.5 hours, and merging filtrate, obtains extract.
The application of the composition pesticide that the present invention also provides the present invention to contain Dalmatian chrysanthemum and extract from Lantana camara in control crop pest.The present invention contains the composition pesticide of Dalmatian chrysanthemum and extract from Lantana camara, to homoptera pest as aphid, scale insect, trialeurodes vaporariorum etc.; Semiptera is as green plant bug etc.; Lepidoptera pest such as cabbage caterpillar, diamond-back moth, prodenia litura etc. have good preventive effect.
In the agricultural production of reality, in order to improve composition pesticide containing Dalmatian chrysanthemum and extract from Lantana camara to the control efficiency of insect pest, the described composition pesticide containing Dalmatian chrysanthemum and extract from Lantana camara is preferably applied to insect pest of the plant initial stage of origination; The present invention can use by common method containing the composition pesticide of Dalmatian chrysanthemum and extract from Lantana camara, sprays on plant leaf surface.Preferably, when using, the present invention is diluted with water to the activity component concentration of crude drug weighing scale as 10 ~ 100ppm containing the composition pesticide of Dalmatian chrysanthemum and extract from Lantana camara, 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 active ingredient concentration is further that 20 ~ 50ppm sprays in plant blade face, and 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.
The present invention is mixed by pyrethrum extract and extract from Lantana camara containing the composition pesticide of Dalmatian chrysanthemum and extract from Lantana camara, or mix extraction by Dalmatian chrysanthemum and lantana to form, its preventive effect is far away higher than the extract of single component, particularly extract common after Dalmatian chrysanthemum and lantana mixing, owing to having solubilising, hydrotropy effect between Dalmatian chrysanthemum and lantana, the composition pesticide insecticidal effect made after common extraction is more remarkable.
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 contains the preparation of the composition pesticide of Dalmatian chrysanthemum and extract from Lantana camara
A, extraction: take dry Dalmatian chrysanthemum petal and Leaves of Lantana Camara, mixing, pulverize, cross 80 mesh sieves, add n-hexane-ethanolic solution, refluxing extraction twice, filter, merging filtrate, be concentrated into not containing n-hexane, then adding ethanol makes concentrate weight identical with crude drug weight, obtains extract cm-01 ~ cm-06; Wherein, each parameter is in table 1;
B, preparation: in extract cm-01 ~ cm-06, add auxiliary agent in table 2, stir, must contain the composition pesticide CM-01 ~ CM-06 of Dalmatian chrysanthemum and extract from Lantana camara.
The preparation technology parameter of table 1 Dalmatian chrysanthemum and extract from Lantana camara
Wherein, Dalmatian chrysanthemum petal and Leaves of Lantana Camara are all purchased from Anguo City Zhong Tian prepared slices of Chinese crude drugs Co., Ltd.
Table 2 contains the formula of the composition pesticide of Dalmatian chrysanthemum and extract from Lantana camara
Embodiment 2 contains the preparation of the composition pesticide of Dalmatian chrysanthemum and extract from Lantana camara
A, extraction: take dry Dalmatian chrysanthemum petal, pulverize, cross 80 mesh sieves, add n-hexane-ethanolic solution, refluxing extraction twice, filter, merging filtrate, be concentrated into not containing n-hexane, then adding ethanol makes concentrate weight identical with crude drug weight, obtain extract d1-01 ~ d1-03, wherein, each parameter is in table 3;
Take dry Leaves of Lantana Camara, pulverize, cross 80 mesh sieves, add n-hexane-ethanolic solution, refluxing extraction twice, filters, merging filtrate, is concentrated into not containing n-hexane, then adding ethanol makes concentrate weight identical with crude drug weight, obtains extract d2-01 ~ d2-03, and wherein, each parameter is in table 4;
B, preparation: take Dalmatian chrysanthemum extract, lantana extract and auxiliary agent, stirring and evenly mixing, obtain the composition pesticide CM-07 ~ CM-12 containing Dalmatian chrysanthemum and extract from Lantana camara, wherein, each parameter is in table 5.
Table 3
Table 4
Table 5
Continued 5
Test example 1 the present invention contains the efficiency test of the composition pesticide tea tree tea lesser leafhopper of Dalmatian chrysanthemum and extract from Lantana camara
1, test material
1.1 for studying thing and object: tea tree tea lesser leafhopper
1.2 reagent agent
Product in embodiment: CM-01 ~ CM-12;
Dalmatian chrysanthemum single dose (D1), lantana single dose (D2);
Chemical reagent contrasts: 10% Methomyl imidacloprid wettable powder (CK-01), purchased from Hailir Pharmaceutical Group Co., Ltd.;
Clear water contrast (CK-02).
Wherein, the preparation method of Dalmatian chrysanthemum single dose is: get 40gd1-03, and add 8g emulsifier 1601,10g dimethyl sulfoxide (DMSO), 42g ethanol, stirring and evenly mixing, to obtain final product.
Lantana single dose preparation method is: get 40gd2-03, and add 8g emulsifier 1601,10g dimethyl sulfoxide (DMSO), 42g ethanol, stirring and evenly mixing, to obtain final product.
2, experimental scheme and method
This test 12 medicaments, 2 single dose contrasts, 1 contrast medicament, 1 blank, repeats for three times, Gong48Ge community.Minizone and surrounding all leave isolation strip, plot area 12m 2, community respectively processes randomized arrangement.
Be 50ppm by reagent agent thin up to activity component concentration, spray application to plant blade face, so that water membrane to appear in blade face, not lower of liquid is advisable.
Be fixed the tea lesser leafhopper quantity statistics of blade before the test and listing mark.Within 5 days after dispenser, investigate and record the tea lesser leafhopper number alive on each blade.Calculate Revision insect recluced rate and preventive effect, calculate and adopt following formula:
Ta: the individual amount of survival after treatment region control; Tb: the individual amount of survival before treatment region control
Ca: the individual amount of survival after the control of check plot; Cb: the individual amount of survival before the control of check plot
3, result of the test
Each group is repeated meter of averaging, and calculate Revision insect recluced rate and preventive effect, it the results are shown in Table 6.
Table 6
Test medicine Radix before medicine 5 days borer populations alive after medicine Revision insect recluced rate (%) Preventive effect (%)
CM-01 248 70 71.77 76.59
CM-02 256 53 79.30 82.83
CM-03 214 38 82.24 85.27
CM-04 267 54 79.78 83.23
CM-05 220 50 77.27 81.15
CM-06 215 54 74.88 79.17
CM-07 249 96 61.45 68.03
CM-08 273 88 67.77 73.27
CM-09 284 80 71.83 76.64
CM-10 213 68 68.08 73.53
CM-11 260 90 65.38 71.29
CM-12 275 99 64.00 70.15
D1 228 150 34.21 45.44
D2 292 269 7.88 23.61
CK-01 264 39 85.23 87.75
CK-02 272 328 -20.59 ——
As can be seen from Table 6, product of the present invention has good preventive effect to tea lesser leafhopper, and better, visible than the control efficiency of single pyrethrum extract and extract from Lantana camara, has synergistic function between product compositions of the present invention.And the preventive effect of the product adopting mixing extracting method to make is apparently higher than extracting separately rear blended product, visible mixing extraction contributes to improving dissolution rate, improves insecticide efficiency.In addition, have no during dispenser and have poisoning to show to plant.
Test example 2 the present invention contains the efficiency test of the composition pesticide eggplant aphid of Dalmatian chrysanthemum and extract from Lantana camara
Products C M-01 of the present invention ~ CM-12 is used for preventing and treating eggplant aphid.This test 12 medicaments, 2 single doses, 1 blank, repeats for three times, Gong45Ge community.Minizone and surrounding all leave isolation strip, plot area 10m 2, community respectively processes randomized arrangement.
Be 50ppm by reagent agent thin up to activity component concentration, spray application to plant blade face, so that water membrane to appear in blade face, not lower of liquid is advisable.
Be fixed the Aphed population statistics alive also listing mark of blade before the test.Within 5 days after dispenser, investigate and record the aphid number alive on each blade.Calculate Revision insect recluced rate and preventive effect, calculate and adopt following formula:
Ta: the individual amount of survival after treatment region control; Tb: the individual amount of survival before treatment region control
Ca: the individual amount of survival after the control of check plot; Cb: the individual amount of survival before the control of check plot
Each group is repeated meter of averaging, and calculate Revision insect recluced rate and preventive effect, it the results are shown in Table 7.
Table 7
Test medicine Radix before medicine 5 days borer populations alive after medicine Revision insect recluced rate (%) Preventive effect (%)
CM-01 411 91 77.86 81.37
CM-02 438 63 85.62 87.90
CM-03 446 52 88.34 90.19
CM-04 478 65 86.40 88.56
CM-05 417 72 82.73 85.47
CM-06 462 89 80.74 83.79
CM-07 477 154 67.71 72.83
CM-08 492 126 74.39 78.45
CM-09 440 99 77.50 81.06
CM-10 465 117 74.84 78.83
CM-11 478 135 71.76 76.23
CM-12 468 144 69.23 74.11
D1 413 250 39.47 49.06
D2 449 382 14.92 28.40
CK-02 409 486 -18.83 ——
As can be seen from Table 7, product of the present invention has good preventive effect to aphid, and better, visible than the control efficiency of single pyrethrum extract and extract from Lantana camara, has synergistic function between product compositions of the present invention.And the preventive effect of the product adopting mixing extracting method to make is apparently higher than extracting separately rear blended product, visible mixing extraction contributes to improving dissolution rate, improves insecticide efficiency.In addition, have no during dispenser and have poisoning to show to plant.
Test example 3 the present invention contains the efficiency test of the composition pesticide grape green plant bug of Dalmatian chrysanthemum and extract from Lantana camara
Products C M-01 of the present invention ~ CM-12 is used for preventing and treating grape green plant bug.This test 12 medicaments, 2 single doses, 1 blank, repeats for three times, Gong45Ge community.Minizone and surrounding all leave isolation strip, plot area 20m 2, community respectively processes randomized arrangement.
Be 50ppm by reagent agent thin up to activity component concentration, spray application to plant blade face, so that water membrane to appear in blade face, not lower of liquid is advisable.
Be fixed the green plant bug quantity statistics alive of blade before the test and listing mark.Within 5 days after dispenser, investigate and record the green plant bug number alive on each blade.Calculate Revision insect recluced rate and preventive effect, calculate and adopt following formula:
Ta: the individual amount of survival after treatment region control; Tb: the individual amount of survival before treatment region control
Ca: the individual amount of survival after the control of check plot; Cb: the individual amount of survival before the control of check plot
Each group is repeated meter of averaging, and calculate Revision insect recluced rate and preventive effect, its result is as shown in table 8.
Table 8
Test medicine Radix before medicine 5 days borer populations alive after medicine Revision insect recluced rate (%) Preventive effect (%)
CM-01 311 64 79.42 82.75
CM-02 321 49 84.74 87.21
CM-03 338 40 88.17 90.08
CM-04 337 53 84.27 86.82
CM-05 384 68 82.29 85.16
CM-06 361 70 80.61 83.75
CM-07 308 91 70.45 75.23
CM-08 391 90 76.98 80.71
CM-09 376 84 77.66 81.27
CM-10 343 81 76.38 80.21
CM-11 351 88 74.93 78.99
CM-12 394 105 73.35 77.66
D1 340 209 38.53 48.48
D2 362 315 12.98 27.06
Continued 8
CK-02 373 445 -19.30 ——
As can be seen from Table 8, product of the present invention has good preventive effect to green plant bug, and better, visible than the control efficiency of single pyrethrum extract and extract from Lantana camara, has synergistic function between product compositions of the present invention.And the preventive effect of the product adopting mixing extracting method to make is apparently higher than extracting separately rear blended product, visible mixing extraction contributes to improving dissolution rate, improves insecticide efficiency.In addition, have no during dispenser and have poisoning to show to plant.
Test example 4 the present invention contains the efficiency test of the composition pesticide a variety of Chinese cabbage diamond-back moth of Dalmatian chrysanthemum and extract from Lantana camara
Products C M-01 of the present invention ~ CM-12 is used for preventing and treating a variety of Chinese cabbage diamond-back moth.This test 12 medicaments, 2 single doses, 1 blank, repeats for three times, Gong45Ge community.Minizone and surrounding all leave isolation strip, plot area 10m 2, community respectively processes randomized arrangement.
Be 50ppm by reagent agent thin up to activity component concentration, spray application to plant blade face, so that water membrane to appear in blade face, not lower of liquid is advisable.
Be fixed the diamond-back moth quantity statistics alive of blade before the test and listing mark.Within 5 days after dispenser, investigate and record the diamond-back moth number alive on each blade.Calculate Revision insect recluced rate and preventive effect, calculate and adopt following formula:
Ta: the individual amount of survival after treatment region control; Tb: the individual amount of survival before treatment region control
Ca: the individual amount of survival after the control of check plot; Cb: the individual amount of survival before the control of check plot
Each group is repeated meter of averaging, and calculate Revision insect recluced rate and preventive effect, its result is as shown in table 9.
Table 9
Test medicine Radix before medicine 5 days borer populations alive after medicine Revision insect recluced rate (%) Preventive effect (%)
CM-01 322 67 79.19 82.20
CM-02 315 44 86.03 88.05
CM-03 361 41 88.64 90.28
CM-04 308 40 87.01 88.89
CM-05 347 56 83.86 86.19
CM-06 391 73 81.33 84.03
CM-07 341 102 70.09 74.41
CM-08 368 86 76.63 80.01
Continued 9
CM-09 329 69 79.03 82.06
CM-10 334 75 77.54 80.79
CM-11 383 97 74.67 78.33
CM-12 320 89 72.19 76.21
D1 372 250 32.80 42.51
D2 394 346 12.18 24.88
CK-02 361 422 -16.90 ——
As can be seen from Table 9, product of the present invention has good preventive effect to diamond-back moth, and better, visible than the control efficiency of single pyrethrum extract and extract from Lantana camara, has synergistic function between product compositions of the present invention.And the preventive effect of the product adopting mixing extracting method to make is apparently higher than extracting separately rear blended product, visible mixing extraction contributes to improving dissolution rate, improves insecticide efficiency.In addition, have no during dispenser and have poisoning to show to plant.
Test example 5 the present invention contains the efficiency test of the composition pesticide cucumber beet snout moth's larva of Dalmatian chrysanthemum and extract from Lantana camara
Products C M-01 of the present invention ~ CM-12 is used for prevent and treat cucumber beet snout moth's larva.This test 12 medicaments, 2 single doses, 1 blank, repeats for three times, Gong45Ge community.Minizone and surrounding all leave isolation strip, plot area 10m 2, community respectively processes randomized arrangement.
Be 50ppm by reagent agent thin up to activity component concentration, spray application to plant blade face, so that water membrane to appear in blade face, not lower of liquid is advisable.
Be fixed the beet snout moth's larva quantity statistics alive of blade before the test and listing mark.Within 5 days after dispenser, investigate and record the beet snout moth's larva number alive on each blade.Calculate Revision insect recluced rate and preventive effect, calculate and adopt following formula:
Ta: the individual amount of survival after treatment region control; Tb: the individual amount of survival before treatment region control
Ca: the individual amount of survival after the control of check plot; Cb: the individual amount of survival before the control of check plot
Each group is repeated meter of averaging, and calculate Revision insect recluced rate and preventive effect, its result is as shown in table 10.
Table 10
Test medicine Radix before medicine 5 days borer populations alive after medicine Revision insect recluced rate (%) Preventive effect (%)
CM-01 344 75 78.20 81.67
CM-02 358 51 85.75 88.02
Continued 10
CM-03 312 35 88.78 90.57
CM-04 307 41 86.64 88.77
CM-05 363 59 83.75 86.34
CM-06 339 61 82.01 84.87
CM-07 341 107 68.62 73.62
CM-08 360 92 74.44 78.52
CM-09 385 85 77.92 81.44
CM-10 374 93 75.13 79.10
CM-11 364 99 72.80 77.14
CM-12 355 100 71.83 76.32
D1 391 245 37.34 47.33
D2 330 307 6.97 21.80
CK-02 327 389 -18.96 ——
As can be seen from Table 10, product of the present invention has good preventive effect to beet snout moth's larva, and better, visible than the control efficiency of single pyrethrum extract and extract from Lantana camara, has synergistic function between product compositions of the present invention.And the preventive effect of the product adopting mixing extracting method to make is apparently higher than extracting separately rear blended product, visible mixing extraction contributes to improving dissolution rate, improves insecticide efficiency.In addition, have no during dispenser and have poisoning to show to plant.

Claims (22)

1. contain the composition pesticide of Dalmatian chrysanthemum and lantana extract, it is characterized in that, jointly extract through n-hexane-ethanolic solution after its active component is mixed by the crude drug of following weight portion and form: Dalmatian chrysanthemum 1 part, lantana 0.2 ~ 4 part;
Extraction step is: take Dalmatian chrysanthemum and lantana, and mixing, adds solvent by solid-liquid ratio 1:3 ~ 12g/ml, extract in 15 ~ 45 DEG C of reduced-pressure backflows, filter, obtain extract, wherein, described solvent is n-hexane-ethanolic solution, and in described n-hexane-ethanolic solution, n-hexane content is 50 ~ 100%v/v; Pressure is 0-101kPa.
2. the composition pesticide containing Dalmatian chrysanthemum and lantana extract according to claim 1, is characterized in that, its active component is extracted by the crude drug of following weight portion and forms: Dalmatian chrysanthemum 1 part, lantana 0.5 ~ 2 part.
3. the composition pesticide containing Dalmatian chrysanthemum and lantana extract according to claim 2, is characterized in that, its active component is extracted by the crude drug of following weight portion and forms: Dalmatian chrysanthemum 1 part, lantana 0.5 ~ 1.5 part.
4. the composition pesticide containing Dalmatian chrysanthemum and lantana extract according to claim 3, is characterized in that, its active component is extracted by the crude drug of following weight portion and forms: Dalmatian chrysanthemum 1 part, lantana 1 part.
5. the composition pesticide containing Dalmatian chrysanthemum and lantana extract according to any one of Claims 1 to 4, is characterized in that: in described n-hexane-ethanolic solution, n-hexane content is 70 ~ 100%v/v.
6. the composition pesticide containing Dalmatian chrysanthemum and lantana extract according to claim 5, is characterized in that: in described n-hexane-ethanolic solution, n-hexane content is 100%v/v.
7. the composition pesticide containing Dalmatian chrysanthemum and lantana extract according to any one of Claims 1 to 4, is characterized in that: the described composition pesticide containing Dalmatian chrysanthemum and lantana extract is microemulsion, aqua or soluble concentrate.
8. the composition pesticide containing Dalmatian chrysanthemum and lantana extract according to claim 5, is characterized in that: the described composition pesticide containing Dalmatian chrysanthemum and lantana extract is microemulsion, aqua or soluble concentrate.
9. the composition pesticide containing Dalmatian chrysanthemum and lantana extract according to claim 6, is characterized in that: the described composition pesticide containing Dalmatian chrysanthemum and lantana extract is microemulsion, aqua or soluble concentrate.
10. the composition pesticide containing Dalmatian chrysanthemum and lantana extract according to any one of Claims 1 to 4, it is characterized in that: described containing in the composition pesticide of Dalmatian chrysanthemum and lantana 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 Dalmatian chrysanthemum and lantana extract according to claim 5, it is characterized in that: described containing in the composition pesticide of Dalmatian chrysanthemum and lantana 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 Dalmatian chrysanthemum and lantana extract according to claim 6, it is characterized in that: described containing in the composition pesticide of Dalmatian chrysanthemum and lantana extract also comprises auxiliary agent, and described auxiliary agent is at least one in emulsifier, antifreeze, solvent, defoamer, dispersant, wetting agent, stabilizing agent.
13. composition pesticides containing Dalmatian chrysanthemum and lantana extract according to claim 7, it is characterized in that: described containing in the composition pesticide of Dalmatian chrysanthemum and lantana extract also comprises auxiliary agent, and described auxiliary agent is at least one in emulsifier, antifreeze, solvent, defoamer, dispersant, wetting agent, stabilizing agent.
14. composition pesticides containing Dalmatian chrysanthemum and lantana extract according to claim 8, it is characterized in that: described containing in the composition pesticide of Dalmatian chrysanthemum and lantana extract also comprises auxiliary agent, and described auxiliary agent is at least one in emulsifier, antifreeze, solvent, defoamer, dispersant, wetting agent, stabilizing agent.
15. composition pesticides containing Dalmatian chrysanthemum and lantana extract according to claim 9, it is characterized in that: described containing in the composition pesticide of Dalmatian chrysanthemum and lantana extract also comprises auxiliary agent, and described auxiliary agent is at least one in emulsifier, antifreeze, solvent, defoamer, dispersant, wetting agent, stabilizing agent.
16. composition pesticides containing Dalmatian chrysanthemum and lantana extract according to claim 15, it is characterized in that: described soluble concentrate is made up of the component of following weight portion: Dalmatian chrysanthemum and lantana extract, 8 parts of emulsifier, 1601,10 parts of dimethyl sulfoxide (DMSO)s, 42 parts of ethanol; Wherein, Dalmatian chrysanthemum and lantana extract be 40 weight portions crude drug extract form; Dalmatian chrysanthemum and lantana extract are prepared from by the following method: crude drug, through extracting and being concentrated into not containing n-hexane, then adds ethanol and makes concentrate weight identical with crude drug weight.
17. prepare the method containing the composition pesticide of Dalmatian chrysanthemum and lantana extract described in claim 1-4, any one of 7-16, it is characterized in that being made up of following steps:
A, extraction: take Dalmatian chrysanthemum particle and lantana particle, mixing, solvent is added by solid-liquid ratio 1:3 ~ 12g/ml, extract in 15 ~ 45 DEG C of reduced-pressure backflows, filter, obtain extract, wherein, described solvent is n-hexane-ethanolic solution, and in described n-hexane-ethanolic solution, n-hexane content is 50 ~ 100%v/v; Pressure is 0-101kPa;
B, preparation: extract is made microemulsion, soluble concentrate or aqua.
18. preparations according to claim 17 contain the method for the composition pesticide of Dalmatian chrysanthemum and lantana extract, and it is characterized in that: in described a step, Dalmatian chrysanthemum particle and lantana particle cross 60 ~ 100 mesh sieves; Solid-liquid ratio is 1:4 ~ 10g/ml; In described n-hexane-ethanolic solution, n-hexane content is 70 ~ 100%v/v; Reflux temperature is 20 ~ 30 DEG C; Reflow's cycle is twice, and merging filtrate, obtains extract.
19. preparations according to claim 18 contain the method for the composition pesticide of Dalmatian chrysanthemum and lantana extract, and it is characterized in that: in described a step, Dalmatian chrysanthemum particle and lantana particle cross 80 mesh sieves; Solid-liquid ratio is 1:6g/ml; In described n-hexane-ethanolic solution, n-hexane content is 100%v/v; Reflux temperature is 25 DEG C.
The composition pesticide containing Dalmatian chrysanthemum and lantana extract described in 20. any one of claim 1 ~ 16 is preventing and treating the application in crop pest.
21. application of composition pesticide in control crop pest containing Dalmatian chrysanthemum and lantana extract according to claim 20, is characterized in that: described insect pest is Homoptera, Lepidoptera, Hemipteran pest; During application, be diluted with water to the activity component concentration of crude drug weighing scale as 10 ~ 100ppm.
22. application of composition pesticide in control crop pest containing Dalmatian chrysanthemum and lantana extract according to claim 21, is characterized in that: during application, are diluted with water to the activity component concentration of crude drug weighing scale as 20 ~ 50ppm.
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