CN103651633B - Pesticide composition containing lightyellow sophora root and veratrum nigrum extracts, and preparation method and application thereof - Google Patents
Pesticide composition containing lightyellow sophora root and veratrum nigrum extracts, and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to a pesticide composition containing lightyellow sophora root and veratrum nigrum extracts, and a preparation method and application thereof, and belongs to the field of pesticides. In order to solve technical problems, the invention provides the pesticide composition containing the lightyellow sophora root and veratrum nigrum extracts, and the preparation method and application thereof. According to the pesticide composition containing the lightyellow sophora root and veratrum nigrum extracts, active ingredients of the pesticide composition are prepared by extracting 1 weight part of lightyellow sophora root and 0.5 to 8 weight parts of veratrum nigrum together; furthermore, the active ingredients are prepared by extracting the lightyellow sophora root and the veratrum nigrum together through an ethanol solution. The pesticide composition containing the lightyellow sophora root and veratrum nigrum extracts is prepared by mixing the lightyellow sophora root and the veratrum nigrum and extracting together, the content of total alkaloids is greatly increased, and the pesticide composition can well kill Homoptera pests such as aphid, scale insect and whitefly, and Hemiptera pests such as green plant bug, so the pesticide composition has positive significance for agricultural production.
Description
Technical field
The present invention relates to the composition pesticide and its preparation method and application containing kuh-seng and black false hellebore extract, belong to pesticide field.
Background technology
Kuh-seng is the plant that pulse family kuh-seng belongs to.Be distributed in the ground such as each provinces and regions, north and south of Russia, Japan, India, Korea and China's Mainland, be grown on the area of height above sea level 1500 meters, how raw in hillside, sand ground, Cao Po, spinney and near field, at present not yet by artificial introducing and planting.Function cures mainly: heat-clearing and damp-drying drug, desinsection, diuresis.For hot dysentery, have blood in stool, jaundice renal shutdown, leukorrhea with reddish discharge, swelling of vulva pruritus vulvae, eczema, wet sore, pruitus, mange leprosy; Control trichomonas vaginitis outward.
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.General veratrum alkaloid extracting method has ammonia alkali chloroform ultrasonic extraction, water extraction and Alcohol percolation etc., but the method for prior art exists the shortcomings such as seriously polluted, recovery rate is low.
Inventor finds through a large amount of experiments, jointly extract after kuh-seng is mixed with black false hellebore, biology total alkali content significantly rises, kuh-seng add the stripping being conducive to veratrum alkaloid, homoptera pest can well be killed as aphid, scale insect, trialeurodes vaporariorum, Hemipteran pest, as green plant bug etc., thus has positive effect for agricultural production.
Summary of the invention
The technical problem to be solved in the present invention is, provides a kind of and contains composition pesticide of kuh-seng and black false hellebore extract and its preparation method and application.
The present invention contains the composition pesticide of kuh-seng and black false hellebore extract, and its active component is jointly extracted by the crude drug of following weight portion and forms: kuh-seng 1 part, black false hellebore 0.5 ~ 8 part; Be preferably kuh-seng 1 part, black false hellebore 2 ~ 5 parts; More preferably kuh-seng 1 part, black false hellebore 3 ~ 5 parts; Be more preferably kuh-seng 1 part, black false hellebore 4 parts.
Wherein, the kuh-seng that the present invention adopts and black false hellebore are Chinese herbal medicine raw material, contain the activity of the composition pesticide of kuh-seng and black false hellebore extract in order to improve the present invention, the radix sophorae that kuh-seng is preferably dry, the black false hellebore rhizome that black false hellebore is preferably dry.
Further, in order to improve the effect of the present invention containing the composition pesticide of kuh-seng and black false hellebore extract, preferably, the present invention jointly to be extracted through ethanolic solution by kuh-seng and black false hellebore containing the active component of the composition pesticide of kuh-seng and black false hellebore extract and forms; Described ethanol solution concentration >=60%v/v, is preferably absolute ethyl alcohol.
Further, in order to improve the activity of the composition pesticide containing kuh-seng and black false hellebore extract, be convenient to store and transport, the described composition pesticide containing kuh-seng 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 kuh-seng and black false hellebore extract, described containing in the composition pesticide of kuh-seng 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 present invention is made up of the component of following weight portion containing the composition pesticide of kuh-seng and black false hellebore extract: kuh-seng and black false hellebore extract, 8 parts of emulsifier, 602,5 parts of dimethyl sulfoxide (DMSO)s, 37 parts of ethanol; Wherein, kuh-seng and black false hellebore extract are that the crude drug of 50 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, kuh-seng 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, the invention also discloses the preparation method that the present invention contains the composition pesticide of kuh-seng and black false hellebore extract, be made up of following steps:
A, extraction: take kuh-seng particle and black false hellebore particle, mixing, adds ethanolic solution by solid-liquid ratio 1:3 ~ 12g/ml, in 60 ~ 85 DEG C of refluxing extraction, filters, obtains extract; Wherein, ethanol solution concentration >=60%v/v;
B, preparation: extract is made microemulsion, soluble concentrate or aqua.
Wherein, kuh-seng particle and black false hellebore particle can adopt commercially available particle, and conventional method pulverizing radix sophorae and black false hellebore rhizome also can be adopted to obtain.In order to improve the effect of extraction, simultaneously cost-saving, kuh-seng 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 kuh-seng 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 ethanolic solution is preferably absolute ethyl alcohol simultaneously.
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 80 DEG C; Reflow's cycle is twice, and each return time is 2 hours, and merging filtrate, obtains extract.
After the present invention adopts kuh-seng and black false hellebore mixing containing the composition pesticide of kuh-seng and black false hellebore extract, the biology total alkali content jointly extracted in the extract obtained is greater than black false hellebore and extracts separately biology total alkali content in the extract obtained, and the black false hellebore total alkali with insecticidal activity obviously increases.
Further, the invention also discloses the application of composition pesticide in control crop pest containing kuh-seng and black false hellebore extract, wherein, described crop pest is preferably Homoptera, Hemipteran pest; Common homoptera pest is as aphid, trialeurodes vaporariorum etc., and common Hemipteran pest is as green plant bug etc.
In the agricultural production of reality, in order to improve composition pesticide containing kuh-seng and black false hellebore extract to the control efficiency of insect pest, the described composition pesticide containing kuh-seng 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 kuh-seng and black false hellebore extract, sprays on crop blade face.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 kuh-seng and black false hellebore extract, 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 activity component 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.
Beneficial effect of the present invention:
1, kuh-seng of the present invention and the common extract of black false hellebore have synergistic function, and to Homoptera as aphid, scale insect, trialeurodes vaporariorum, the control efficiency of Semiptera as insect pests such as green plant bugs is obvious.
2, the present invention adopts kuh-seng and black false hellebore jointly to extract, and improves black false hellebore total alkali, can improve crop immune system ability, and can significantly improve its vigor while quick-acting tagging.
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, the valid density when composition pesticide containing kuh-seng and black false hellebore extract uses is invented low, with low cost.
Embodiment
The present invention contains the composition pesticide of kuh-seng and black false hellebore extract, and its active component is jointly extracted by the crude drug of following weight portion and forms: kuh-seng 1 part, black false hellebore 0.5 ~ 8 part; Be preferably kuh-seng 1 part, black false hellebore 2 ~ 5 parts; More preferably kuh-seng 1 part, black false hellebore 3 ~ 5 parts; Be more preferably kuh-seng 1 part, black false hellebore 4 parts.
Wherein, the kuh-seng that the present invention adopts and black false hellebore are Chinese herbal medicine raw material, contain the activity of the composition pesticide of kuh-seng and black false hellebore extract in order to improve the present invention, the radix sophorae that kuh-seng is preferably dry, the black false hellebore rhizome that black false hellebore is preferably dry.
Further, in order to improve the effect of the present invention containing the composition pesticide of kuh-seng and black false hellebore extract, preferably, the present invention jointly to be extracted through ethanolic solution by kuh-seng and black false hellebore containing the active component of the composition pesticide of kuh-seng and black false hellebore extract and forms; Described ethanol solution concentration >=60%v/v, is preferably absolute ethyl alcohol.
Further, in order to improve the activity of the composition pesticide containing kuh-seng and black false hellebore extract, be convenient to store and transport, the described composition pesticide containing kuh-seng 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 kuh-seng and black false hellebore extract, described containing in the composition pesticide of kuh-seng 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 present invention is made up of the component of following weight portion containing the composition pesticide of kuh-seng and black false hellebore extract: kuh-seng and black false hellebore extract, 8 parts of emulsifier, 602,5 parts of dimethyl sulfoxide (DMSO)s, 37 parts of ethanol; Wherein, kuh-seng and black false hellebore extract are that the crude drug of 50 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, kuh-seng 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, the invention also discloses the preparation method that the present invention contains the composition pesticide of kuh-seng and black false hellebore extract, be made up of following steps:
A, extraction: take kuh-seng particle and black false hellebore particle, mixing, adds ethanolic solution by solid-liquid ratio 1:3 ~ 12g/ml, in 60 ~ 85 DEG C of refluxing extraction, filters, obtains extract; Wherein, ethanol solution concentration >=60%v/v;
B, preparation: extract is made microemulsion, soluble concentrate or aqua.
Wherein, kuh-seng particle and black false hellebore particle can adopt commercially available particle, and conventional method pulverizing radix sophorae and black false hellebore rhizome also can be adopted to obtain.In order to improve the effect of extraction, simultaneously cost-saving, kuh-seng 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 kuh-seng 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 ethanolic solution is preferably absolute ethyl alcohol simultaneously.
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 80 DEG C; Reflow's cycle is twice, and each return time is 2 hours, and merging filtrate, obtains extract.
After the present invention adopts kuh-seng and black false hellebore mixing containing the composition pesticide of kuh-seng and black false hellebore extract, the biology total alkali content jointly extracted in the extract obtained is greater than black false hellebore and extracts separately biology total alkali content in the extract obtained, and the black false hellebore total alkali with insecticidal activity obviously increases.
Further, the invention also discloses the application of composition pesticide in control crop pest containing kuh-seng and black false hellebore extract, wherein, described crop pest is preferably Homoptera, Hemipteran pest; Common homoptera pest is as aphid, trialeurodes vaporariorum etc., and common Hemipteran pest is as green plant bug etc.
In the agricultural production of reality, in order to improve composition pesticide containing kuh-seng and black false hellebore extract to the control efficiency of insect pest, the described composition pesticide containing kuh-seng 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 kuh-seng and black false hellebore extract, sprays on crop blade face.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 kuh-seng and black false hellebore extract, 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 activity component 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.
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 kuh-seng and black false hellebore extract
A, extraction: take dry radix sophorae and black false hellebore rhizome, mixing, pulverizes, and crosses 80 mesh sieves, adds ethanolic solution, refluxing extraction twice, filters, merging filtrate, concentrated, makes extract weight equal the weight of crude drug, obtains extract kl-01 ~ kl-06; Wherein, each parameter is in table 1;
B, preparation: in extract kl-01 ~ kl-06, add auxiliary agent in table 2, stir, must contain the composition pesticide KL-01 ~ KL-06 of kuh-seng and black false hellebore extract.
Table 1
Wherein, the kuh-seng 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 contains the formula of the composition pesticide of kuh-seng and black false hellebore extract
Continued 2
Test example 1 the present invention contains the composition pesticide orange caterpillar efficiency test of kuh-seng and black false hellebore extract
1 test material
1.1 for studying thing and object: orange caterpillar
1.2 medicament
Test medicine: KL-01 ~ KL-06;
Contrast medicament: D-01(single matrine); D-02(jervine single dose); D-03 (oxymatrine single dose);
Wherein, single matrine formula is: matrine 10g, No. 100 solvent naphtha 10g, 10g emulsifier 1601,3g emulsifier 1602,2g emulsifier 500,5g ethylene glycol, the yellow collagen of 0.1g, 59.9g water;
Jervine single dose formulations is: jervine 10g, No. 100 solvent naphtha 10g, 10g emulsifier 1601,3g emulsifier 1602,2g emulsifier 500,5g ethylene glycol, the yellow collagen of 0.1g, 59.9g water;
Oxymatrine single dose formulations is: oxymatrine 10g, No. 100 solvent naphtha 10g, 10g emulsifier 1601,3g emulsifier 1602,2g emulsifier 500,5g ethylene glycol, the yellow collagen of 0.1g, 59.9g water;
CK-01 (10% Methomyl Imidacloprid built agent, purchased from Hailir Pharmaceutical Group Co., Ltd.);
CK-02(clear water contrasts).
2 experimental scheme
2.1 chemicals treatment
By table 2 Chinese medicine thin up, after dilution, activity component concentration is in table 3, and spray application to plant blade face, so that water membrane to appear in blade face, not lower of liquid is advisable.
Table 3
| Numbering | Active component | Activity component concentration/ppm |
| KL-01 | kl-01 | 50 |
| KL-02 | kl-02 | 50 |
Continued 3
| KL-03 | kl-03 | 50 |
| KL-04 | kl-04 | 50 |
| KL-05 | kl-05 | 50 |
| KL-06 | kl-06 | 50 |
| D-01 | Matrine | 50 |
| D-02 | Jervine | 50 |
| D-03 | Oxymatrine | 50 |
| CK-01 | 10% Methomyl Imidacloprid built agent | 50 |
| CK-02 | Clear water contrasts | -- |
2.2 Quarter Design
This test 6 medicaments, 4 contrast medicaments, 1 blank, repeats for three times, Gong33Ge community.Minizone and surrounding all leave isolation strip, plot area 20m
2, community respectively processes randomized arrangement.
3 test results and analysis
3.1 test data
Be fixed the Aphed population statistics also listing mark of blade before the test, and five days after dispenser add up population number respectively, each group is repeated to average, and adopts following formulae discovery Revision insect recluced rate and preventive effect, the results are shown in Table 4.
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 4
| Test medicine | Radix before medicine | Five days borer populations alive after medicine | Revision insect recluced rate | Preventive effect |
| KL-01 | 155 | 33 | 78.71% | 83.11% |
| KL-02 | 174 | 35 | 79.89% | 84.04% |
Continued 4
| KL-03 | 163 | 24 | 85.28% | 88.32% |
| KL-04 | 187 | 21 | 88.77% | 91.09% |
| KL-05 | 192 | 23 | 88.02% | 90.50% |
| KL-06 | 148 | 18 | 87.84% | 90.35% |
| D-01 | 172 | 168 | 2.33% | 22.50% |
| D-02 | 151 | 92 | 39.07% | 51.66% |
| D-03 | 147 | 139 | 5.44% | 24.98% |
| CK-01 | 175 | 15 | 91.43% | 93.20% |
| CK-02 | 169 | 213 | -26.04% | —— |
3.2 result of the test
As shown in Table 4, the present invention contains in the composition pesticide orange caterpillar test of kuh-seng and black false hellebore extract, and KL-04 pharmacy control efficacy is best, reach 91.09%, all the other experimental group preventive effects have all remained on more than 83%, and control efficiency is excellent, performance is stable, and to contrast pharmacy control efficacy suitable with chemical source; Meanwhile, jointly extract after kuh-seng and black false hellebore mixing, have synergistic function, successful is better than jervine single dose, single matrine and oxymatrine single dose.
3.3 interpretation of result
This result of the test show that the composition pesticide containing kuh-seng and black false hellebore extract of variable concentrations has all remained on more than 83% to the preventive effect of orange caterpillar, and KL-04 medicament reaches 91.09%, and preventive effect performance is relatively stable, suitable with chemical source agricultural chemicals preventive effect.
Test example 2 the present invention tests containing the composition pesticide eggplant trialeurodes vaporariorum preventive effect of kuh-seng and black false hellebore extract
Product K L-01 of the present invention ~ KL-06 is used for preventing and treating eggplant trialeurodes vaporariorum.This test 6 medicaments, 3 single doses, 1 blank, repeats for three times, Gong30Ge community.Minizone and surrounding all leave isolation strip, and plot area 10m2, 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 trialeurodes vaporariorum quantity statistics alive of blade before the test and listing mark.Within five days after dispenser, investigate and record the trialeurodes vaporariorum quantity alive on each blade, each group is repeated to average, and adopts following formulae discovery Revision insect recluced rate and preventive effect, the results are shown in Table 5.
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 5
| Test medicine | Radix before medicine | Five days borer populations alive after medicine | Revision insect recluced rate | Preventive effect |
| KL-01 | 182 | 55 | 69.78% | 75.36% |
| KL-02 | 179 | 51 | 71.51% | 76.77% |
| KL-03 | 167 | 44 | 73.65% | 78.52% |
| KL-04 | 188 | 41 | 78.19% | 82.22% |
| KL-05 | 152 | 39 | 74.34% | 79.08% |
| KL-06 | 161 | 47 | 70.81% | 76.19% |
| D-01 | 154 | 143 | 7.14% | 24.28% |
| D-02 | 119 | 72 | 39.50% | 50.66% |
| D-03 | 183 | 175 | 4.37% | 22.02% |
| CK-02 | 190 | 233 | -22.63% | —— |
As can be seen from Table 5, the present invention is excellent to trialeurodes vaporariorum control efficiency containing the composition pesticide of kuh-seng and black false hellebore extract, and all more than 75%, the highest preventive effect reaches 82.22%, and control efficiency is excellent, and performance is stable, and to contrast pharmacy control efficacy suitable with chemical source; Meanwhile, jointly extract after kuh-seng and black false hellebore mixing, have synergistic function, successful is better than jervine single dose, single matrine and oxymatrine single dose.
Test example 3 the present invention tests containing the composition pesticide grape green plant bug preventive effect of kuh-seng and black false hellebore extract
Product K L-01 of the present invention ~ KL-06 is used for preventing and treating grape green plant bug.This test 6 medicaments, 3 single doses, 1 blank, repeats for three times, Gong30Ge 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 green plant bug quantity statistics alive of blade before the test and listing mark.Within five days after dispenser, investigate and record the green plant bug quantity alive on each blade, each group is repeated to average, and adopts following formulae discovery Revision insect recluced rate and preventive effect, the results are shown in Table 6.
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 6
| Test medicine | Radix before medicine | Five days borer populations alive after medicine | Revision insect recluced rate | Preventive effect |
| KL-01 | 210 | 62 | 70.48% | 75.90% |
| KL-02 | 226 | 65 | 71.24% | 76.52% |
| KL-03 | 201 | 55 | 72.64% | 77.66% |
| KL-04 | 192 | 45 | 76.56% | 80.87% |
| KL-05 | 198 | 54 | 72.73% | 77.74% |
| KL-06 | 237 | 68 | 71.31% | 76.58% |
| D-01 | 217 | 197 | 9.22% | 25.90% |
| D-02 | 222 | 121 | 45.50% | 55.51% |
| D-03 | 209 | 192 | 8.13% | 25.01% |
| CK-02 | 231 | 283 | -22.51% | —— |
As can be seen from Table 6, the present invention is excellent to green plant bug control efficiency containing the composition pesticide of kuh-seng and black false hellebore extract, and all more than 75%, the highest preventive effect reaches 80.87%, and control efficiency is excellent, and performance is stable, and to contrast pharmacy control efficacy suitable with chemical source; Meanwhile, jointly extract after kuh-seng and black false hellebore mixing, have synergistic function, successful is better than jervine single dose, single matrine and oxymatrine single dose.
Test example 4 the present invention tests containing the composition pesticide oranges and tangerines cottonycushion scale preventive effect of kuh-seng and black false hellebore extract
Product K L-01 of the present invention ~ KL-06 is used for preventing and treating oranges and tangerines cottonycushion scale.This test 6 medicaments, 3 single doses, 1 blank, repeats for three times, Gong30Ge 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 cottonycushion scale quantity statistics alive of blade before the test and listing mark.Within five days after dispenser, investigate and record the cottonycushion scale quantity alive on each blade, each group is repeated to average, and adopts following formulae discovery Revision insect recluced rate and preventive effect, 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 |
| KL-01 | 89 | 31 | 65.17% | 72.94% |
| KL-02 | 67 | 21 | 68.66% | 75.65% |
| KL-03 | 86 | 26 | 69.77% | 76.51% |
| KL-04 | 79 | 20 | 74.68% | 80.33% |
| KL-05 | 92 | 24 | 73.91% | 79.73% |
| KL-06 | 86 | 23 | 73.26% | 79.22% |
| D-01 | 77 | 74 | 3.90% | 25.34% |
| D-02 | 95 | 54 | 43.16% | 55.84% |
Continued 7
| D-03 | 88 | 81 | 7.95% | 28.49% |
| CK-02 | 94 | 121 | -28.72% | —— |
As can be seen from Table 7, the present invention is excellent to oranges and tangerines cottonycushion scale control efficiency containing the composition pesticide of kuh-seng and black false hellebore extract, and all more than 72%, the highest preventive effect reaches 80.33%, and control efficiency is excellent, and performance is stable, and to contrast pharmacy control efficacy suitable with chemical source; Meanwhile, jointly extract after kuh-seng and black false hellebore mixing, have synergistic function, successful is better than jervine single dose, single matrine and oxymatrine single dose.
Test example 5 the present invention contains biology total alkali assay in the composition pesticide of kuh-seng and black false hellebore extract
1,1g black false hellebore is pulverized, cross 80 mesh sieves, add 100ml absolute ethyl alcohol and stirring, rotating speed 90 turns/min, and carry twice altogether in 80 DEG C of backflows, each two hours, merge extract altogether, be concentrated into 25ml, obtain extract 1.
2, by 1g black false hellebore, the mixing of 1g kuh-seng, pulverize, cross 80 mesh sieves, add 100ml absolute ethyl alcohol and stirring, rotating speed 90 turns/min, and carry twice altogether in 80 DEG C of backflows, each two hours, merge extract altogether, be concentrated into 25ml, obtain extract 2.
3, by 1g black false hellebore, the mixing of 3g kuh-seng, pulverize, cross 80 mesh sieves, add 100ml absolute ethyl alcohol and stirring, rotating speed 90 turns/min, and carry twice altogether in 80 DEG C of backflows, each two hours, merge extract altogether, be concentrated into 25ml, obtain extract 3.
By HPLC-ESI MS technology, the alkaloid of black false hellebore in above-mentioned 3 extracts is studied, measurement result is in table 8, wherein, Mass Spectrometry Conditions: mass spectrum spray voltage 5.0kV, metal capillary temperature 250 DEG C, METAL HEATING PROCESS capillary voltage is-10V, and shell gas is N2, adopt negative ion mode, sweep limits is: (m/z) 50 ~ 2000; The online condition of liquid matter: Waters600 liquid chromatogram (Waters, US); Automatic sampler (Agilent company of the U.S., 1100 series); 2000 type ELSD detectors (Alltech company of the U.S.); Capcell Pak C
18chromatographic column 4.6mm × 250mm, column temperature 35 DEG C, drift tube temperature: 85 DEG C; Mobile phase: A: water (0.2% acetic acid), B: acetonitrile, linear gradient elution, Mobile phase B: 25 ~ 52%, 45min, sample introduction 10 μ L.
The each alkaloidal relative abundance of table 8
| Alkaloid title | [M＋H](m/z) | Extract 1 | Extract 2 | Extract 3 |
| veralosidine | 414 | 7.06 | 9.69 | 10.27 |
| veramarine | 430 | 3.07 | 3.15 | 3.31 |
| protoverutridne | 594 | 5.03 | 5.99 | 5.59 |
| germidine | 636 | 6.18 | 11.55 | 10.27 |
| germerine | 694 | 12.92 | 25.08 | 25.13 |
| dideacetylprotoveratrineA | 710 | 23.01 | 33.75 | 33.41 |
| germitrine | 736 | 29.73 | 50.21 | 65.82 |
Continued 8
| germinalinine | 752 | 42.13 | 54.69 | 74.81 |
| Protoveratrine B | 810 | 31.52 | 40.77 | 46.69 |
| Etilline | 414 | 20.51 | 26.37 | 29.81 |
| Neogermidine | 636 | 11.16 | 13.45 | 15.94 |
| Verzine | 398 | 14.32 | 15.97 | 19.24 |
By table 8, we can find out, each veratrine composition detection content increases with kuh-seng adding proportion and increases, that is, black false hellebore is extracted after mixing with kuh-seng jointly, and the black false hellebore total alkali stripping quantity with insecticidal activity obviously increases.
Claims (2)
1. containing the composition pesticide of kuh-seng and black false hellebore extract, it is characterized in that, its active component jointly to be extracted through ethanolic solution by the crude drug of following weight portion and forms: kuh-seng 1 part, black false hellebore 0.5 ~ 8 part.
2. the composition pesticide containing kuh-seng and black false hellebore extract according to claim 1, is characterized in that, its active component jointly to be extracted through ethanolic solution by the crude drug of following weight portion and forms: kuh-seng 1 part, black false hellebore 2 ~ 5 parts.
3
.composition pesticide containing kuh-seng and black false hellebore extract according to claim 2, is characterized in that, its active component jointly to be extracted through ethanolic solution by the crude drug of following weight portion and forms: kuh-seng 1 part, black false hellebore 3 ~ 5 parts.
4
.composition pesticide containing kuh-seng and black false hellebore extract according to claim 3, is characterized in that, its active component jointly to be extracted through ethanolic solution by the crude drug of following weight portion and forms: kuh-seng 1 part, black false hellebore 4 parts.
5
.the composition pesticide containing kuh-seng and black false hellebore extract according to any one of Claims 1 to 4, is characterized in that: described ethanol solution concentration>=60%v/v.
6
.the composition pesticide containing kuh-seng and black false hellebore extract according to claim 5, is characterized in that: described ethanolic solution is absolute ethyl alcohol.
7
.the composition pesticide containing kuh-seng and black false hellebore extract according to any one of Claims 1 to 4, is characterized in that: the described composition pesticide containing kuh-seng and black false hellebore extract is microemulsion, soluble concentrate or aqua.
8
.the composition pesticide containing kuh-seng and black false hellebore extract according to claim 5, is characterized in that: the described composition pesticide containing kuh-seng and black false hellebore extract is microemulsion, soluble concentrate or aqua.
9
.the composition pesticide containing kuh-seng and black false hellebore extract according to claim 6, is characterized in that: the described composition pesticide containing kuh-seng and black false hellebore extract is microemulsion, soluble concentrate or aqua.
10
.the composition pesticide containing kuh-seng 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 kuh-seng 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
.the composition pesticide containing kuh-seng and black false hellebore extract according to claim 5, it is characterized in that: described containing in the composition pesticide of kuh-seng 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
.the composition pesticide containing kuh-seng and black false hellebore extract according to claim 6, it is characterized in that: described containing in the composition pesticide of kuh-seng 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.
13
.the composition pesticide containing kuh-seng and black false hellebore extract according to claim 7, it is characterized in that: described containing in the composition pesticide of kuh-seng 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.
14
.the composition pesticide containing kuh-seng and black false hellebore extract according to claim 8, it is characterized in that: described containing in the composition pesticide of kuh-seng 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.
15
.the composition pesticide containing kuh-seng and black false hellebore extract according to claim 9, it is characterized in that: described containing in the composition pesticide of kuh-seng 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.
16
.the composition pesticide containing kuh-seng and black false hellebore extract according to claim 13, it is characterized in that, described soluble concentrate is made up of the component of following weight portion: kuh-seng and black false hellebore extract, 8 parts of emulsifier, 602,5 parts of dimethyl sulfoxide (DMSO)s, 37 parts of ethanol; Wherein, kuh-seng and black false hellebore extract are that the crude drug of 50 weight portions jointly extracts and forms.
17
.the composition pesticide containing kuh-seng and black false hellebore extract according to claim 14, it is characterized in that, described soluble concentrate is made up of the component of following weight portion: kuh-seng and black false hellebore extract, 8 parts of emulsifier, 602,5 parts of dimethyl sulfoxide (DMSO)s, 37 parts of ethanol; Wherein, kuh-seng and black false hellebore extract are that the crude drug of 50 weight portions jointly extracts and forms.
18
.the composition pesticide containing kuh-seng and black false hellebore extract according to claim 15, it is characterized in that, described soluble concentrate is made up of the component of following weight portion: kuh-seng and black false hellebore extract, 8 parts of emulsifier, 602,5 parts of dimethyl sulfoxide (DMSO)s, 37 parts of ethanol; Wherein, kuh-seng and black false hellebore extract are that the crude drug of 50 weight portions jointly extracts and forms.
19
.the composition pesticide containing kuh-seng and black false hellebore extract according to claim 16, it is characterized in that, described kuh-seng 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.
20
.the composition pesticide containing kuh-seng and black false hellebore extract according to claim 17, it is characterized in that, described kuh-seng 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.
21
.the composition pesticide containing kuh-seng and black false hellebore extract according to claim 18, it is characterized in that, described kuh-seng 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.
22
.the preparation method containing the composition pesticide of kuh-seng and black false hellebore extract described in any one of claim 1 ~ 21, is characterized in that being made up of following steps:
A, extraction: take kuh-seng particle and black false hellebore particle, mixing, adds ethanolic solution by solid-liquid ratio 1:3 ~ 12g/ml, in 60 ~ 85 DEG C of refluxing extraction, filters, obtains extract; Wherein, ethanol solution concentration >=60%v/v;
B, preparation: extract is made microemulsion, soluble concentrate or aqua.
23
.the preparation method containing the composition pesticide of kuh-seng and black false hellebore extract according to claim 22, it is characterized in that: in described a step, kuh-seng particle and black false hellebore particle cross 60 ~ 100 mesh sieves; Solid-liquid ratio is 1:4 ~ 10g/ml; Ethanolic solution is absolute ethyl alcohol; Reflux temperature is 75 ~ 85 DEG C; Reflow's cycle is twice, and merging filtrate, obtains extract.
24
.the preparation method containing the composition pesticide of kuh-seng and black false hellebore extract according to claim 23, it is characterized in that: in described a step, kuh-seng particle and black false hellebore particle cross 80 mesh sieves; Solid-liquid ratio is 6g/ml; Reflux temperature is 80 DEG C.
25
.the composition pesticide containing kuh-seng and black false hellebore extract described in any one of claim 1 ~ 21 is preventing and treating the application in crop pest.
26
.the application of composition pesticide in control crop pest containing kuh-seng and black false hellebore extract according to claim 25, is characterized in that: described insect pest is Homoptera, Hemipteran pest; During application, be diluted with water to the activity component concentration of crude drug weighing scale as 10 ~ 100ppm.
27
.the application of composition pesticide in control crop pest containing kuh-seng and black false hellebore extract according to claim 26, is characterized in that: during application, is diluted with water to the activity component concentration of crude drug weighing scale as 20 ~ 50ppm.
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| CN100998341A (en) * | 2006-12-25 | 2007-07-18 | 南风云 | Plant insecticide and its preparing method |
| CN101036477A (en) * | 2007-03-13 | 2007-09-19 | 太原同康泰生物科技有限公司 | Chinese herbal medicine combined pesticide and method for preparing the same |
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| CN100998341A (en) * | 2006-12-25 | 2007-07-18 | 南风云 | Plant insecticide and its preparing method |
| CN101036477A (en) * | 2007-03-13 | 2007-09-19 | 太原同康泰生物科技有限公司 | Chinese herbal medicine combined pesticide and method for preparing the same |
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| 植物源农药防治烟草病虫害;章新军等;《烟草科技》;20060620(第6期);第58-60页；第1.1节、第1.2节、第3节、表2和表3 * |
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