CN1810123A - Botanical pesticide prepared with calamus - Google Patents
Botanical pesticide prepared with calamus Download PDFInfo
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- CN1810123A CN1810123A CN 200610001399 CN200610001399A CN1810123A CN 1810123 A CN1810123 A CN 1810123A CN 200610001399 CN200610001399 CN 200610001399 CN 200610001399 A CN200610001399 A CN 200610001399A CN 1810123 A CN1810123 A CN 1810123A
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Abstract
The newly developed botanical pesticide includes pesticide oil emulsion containing calamus extracting concentrate in 0.5-20 wt% and pesticide oil aqua containing calamus extracting concentrate in 0.5-10 wt%. The botanical pesticide has calamus extracting concentrate as effective pesticidal component. The present invention is superior to available chemical pesticides for stored grains, household, vegetable and flower, and has less environmental pollution, high effect, long effective period and broad pesticidal spectrum.
Description
One, technical field:
The present invention relates to a kind of plant resource broad spectrum pesticide, specifically refer to a kind of calamus class plant (rhizoma calami, grass-leaved sweetflag) insecticide of preventing and treating grain storage pest, sanitary insect pest, vegetable-crop pest-insect, flowers insect, formulation comprises missible oil, aqua formulation, belongs to the botanical pesticide field.
Two, background content:
Grain, tobacco, traditional Chinese medicine are in storage, because of insect breeds in a large number, not only can cause the direct quantity loss of reserve, and its ight soil and corpse also can pollute, cause the of inferior quality indirect loss of product qualitative change, sometimes also may spread disease etc., endanger the healthy of people directly or indirectly.According to statistics, the whole world only loss that causes because of insect pest every year of grain storage is about 10% of total output of grain, behind the annual grain harvest of China because grain storage pest causes about 3%～5% loss.Temperate zone and torrid areas loss are bigger.Sanitary insect pest mosquito, fly, cockroach can be propagated various diseases, and it harm takes place not only disturbs people's peacefulness, and has a strong impact on the healthy of people.Vegetable crop, flowers suffer the harm of various insects in process of growth, cause very big economic loss.
The method of at present the most effective and economic control grain storage, tobacco, traditional Chinese medicine insect is the chemical agent fumigating system and uses the chemical protector method, directly enter human body because of grain becomes food, people to the requirement of the residual toxicity of fumigant and protective agent more than crops and forestry medication strictness.Sanitary insect pest, vegetable-crop pest-insect, flowers insect are mainly by chemical pesticide control.Though chemical pesticide has been controlled the generation of insect to a certain extent, many drawbacks have also been brought, as pest resistance to insecticide (Resistance), residue of pesticide (Residue), insect rampant again (Resurgence), i.e. " 3R " problem.The main grain storage pest corn weevil of China, lesser grain borer, the flat ostomatid in long angle etc. have also produced resistance in various degree to pest control phosphorus (protective agent), phosphine (fumigant), and the regional pest resistance coefficient that has is up to 1000 times.Health, vegetables, flowers insect have also produced pesticide resistance in various degree to agricultural chemicals such as some pyrethroid pesticides, organic phosphors.
Along with the growing interest that society that agricultural chemicals caused and ecological problem are subjected to people, the using and act on and be subjected to general query of simple chemical pesticide.80～nineties of 20th century, domestic and international many experts think, the use of chemical pesticide will be walked to be at the end, but the fact shows, in foreseeable future, agricultural chemicals and chemical control method will be substituted fully, will be an inevitable development trend and develop environment amenable botanical pesticide with the usage amount that reduces chemical pesticide.
Along with the proposition of sustainable plant protection theory, research and the application of vegetable insecticide in insect is administered seems more important.Utilize the harmonious botanical pesticide of pesticide plant and secondary metabolite development environment thereof to become one of focus of current insecticide research.The Secondary Metabolism of Plant product be plant long-term with insect coevolution process in resist the insect's food-taking behavior and the chemical substance that produces, these materials can through and being processed into vegetable insecticide.Vegetable insecticide to insect have multiple biologically active, little to natural enemy influence, in environment degraded, insect characteristics such as be difficult for developing immunity to drugs easily, meet of the requirement of sustainable plant protection strategy of new century to pesticidal properties.
In the last few years, the research report that utilizes the pesticide plant pest control was constantly arranged.China is research and uses pesticide plant country the earliest.Since 20th century the '30s, to tobacco, Dalmatian chrysanthemum, trifoliate jewelvine, Celastrus angulatus, Chinese Stellera Root, thick fruit reticulate millettia, goat's horn turn round, Rhododendron molle, crotons, thunder godvine, macleaya cordata, the tuber of stemona, chrysanthemum cuckoo, Africa mountain soya bean, polygonum flaccidum, the fruit of a cubeb litsea tree, China tree, garlic, peppermint, Chinese cassia tree, black pepper, Artemisia scoparia, galangal, kaempferia galamga, argy wormwood etc. carried out certain research.But up to the present, utilize the research of pesticide plant pest control mainly to rest on conceptual phase in the laboratory, the product of formation and practical application thereof are seldom.The vegetable insecticide product of having reported has the plain A biology of 5% Chinese Stellera Root go out aphid agent Ec, 0.1% Chinese azalea extract Ec, 0.5% aqueous matrine solution, 0.2% Celastrus angulatus missible oil, 1.0% macleaya cordata WP, 20% silver medal safe Ec, 20%RAD profit standing grain precious Ec, nimbin preparation Margosan-O etc.Research about calamus class plant (grass-leaved sweetflag, rhizoma calami) and extraction concentrate pest control thereof, (agricultural chemicals such as Xie Hongying, 2004 the 43rd the 8th phases of volume) in the laboratory, studied the biologically active of root of Rhizoma Acori Graminei stem extraction to mythimna separata, the methanolic extract of report grass-leaved sweetflag, reaches about 60% the lethality of tagging of larva up to 91.89% mythimna separata 4 instar larvae food refusal rates.Research about rhizoma calami, grass-leaved sweetflag control grain storage pest, sanitary insect pest, vegetable-crop pest-insect, flowers insect is reported seldom, and is utilized the pesticide product of these plants exploitations and application in practice not to appear in the newspapers as yet.
Three, summary of the invention:
The invention discloses a kind of novel plant insecticide emulsifiable concentrate and aqua by calamus medicinal plant (rhizoma calami, grass-leaved sweetflag) development.Extract concentrate content by calamus and be processed into 0.5%-20% calamus missible oil and 0.5-10% calamus aqua, platymiscium pesticide field.The insecticidal activity thing is that calamus is extracted concentrate (main insecticidal active ingredient comprises asarone, acorone etc.) in the product.Product of the present invention has overcome " 3R " problem that present grain storage pest, sanitary insect pest, vegetable-crop pest-insect, flowers insect widely apply chemical insecticide to bring in control, can guarantee that environmental pollution is little, but control efficiency reaches 80-100%, wherein the grain storage pest lasting period was reached more than 1 year, be the wide spectrum novel plant insects medicament of above-mentioned sustainable pest management.
A kind of vegetable source pesticide agent emulsifiable solution, contain is 0.5～20 by weight: 100: 2～5 calamus class plant roots and stems extracts concentrate, solvent, emulsifier, wherein said extraction concentrate extracts calamus class plant roots and stems and obtains for extracting solvent or steam distillation by alcohols or ethers or ketone or esters solvent, solvent is 70%～100% ethanol, and emulsifier is OP～10 or OP～15 or farming breast 100.The vegetable source pesticide agent emulsifiable solution can use 2.5% decis, 10% Imidacloprid as synergist, and the weight ratio that calamus class plant roots and stems extracts concentrate, solvent, emulsifier and synergist is 0.5～20: 100: 2～5: 0.05～1.
The vegetable source pesticide agent emulsifiable solution, it is characterized in that: containing weight ratio is 4: 100: 3: 1 calamus class plant roots and stems extracts concentrate, solvent, emulsifier, synergist, solvent is 70～100% ethanol, emulsifier is OP～10 or OP～15, and synergist is 2.5% decis, 10% Imidacloprid.
A kind of plant insecticide aqua, contain is 0.5～10 by weight: 100: 0.5～1 calamus class plant roots and stems extracts concentrate, aqueous solvent and preservative, and described extraction concentrate extracts solvent extraction calamus class plant roots and stems by water or steam distillation or alcohols and obtains.
The plant insecticide aqua, extracting concentrate is to adopt steam distillation or alcohols solvent to extract calamus class plant roots and stems to obtain, extracting concentrate, aqueous solvent and preservative is 10: 100: 0.5 by weight.
The described plant insecticide aqua of vegetable source pesticide agent emulsifiable solution or claim 5, described calamus class plant roots and stems extracts in the concentrate, comprises as the main effectively asarone 65%～80% of insecticidal constituent, acorone 12.5%～18.5%.
The application method of described vegetable source pesticide agent emulsifiable solution of claim 1 or the described plant insecticide aqua of claim 5 adopts spraying, ultra low volume spraying or mixes the grain use, is used to prevent and treat grain storage pest, sanitary insect pest, vegetable-crop pest-insect or flowers insect.
The preparation method of vegetable source pesticide agent emulsifiable solution, calamus class plant roots and stems is extracted concentrate, solvent, emulsifier by 0.5～20: 100: 2～5 weight ratio is prepared, wherein said extraction concentrate extracts calamus class plant roots and stems and obtains for extracting solvent or steam distillation by alcohols or ethers or ketone or esters solvent, solvent is 70%～100% ethanol, and emulsifier is OP～10 or OP～15 or farming breast 100.
The preparation method of vegetable source pesticide agent emulsifiable solution, calamus class plant roots and stems is extracted concentrate, solvent, emulsifier, synergist by 4: 100: 3: 1 weight ratio is configured, solvent is 70～100% ethanol, emulsifier is OP～10 or OP～15, and synergist is 2.5% decis or 10% Imidacloprid.
A kind of preparation method of plant insecticide aqua, calamus class plant roots and stems is extracted concentrate, aqueous solvent and preservative by 0.5～10: 100: 0.5～1 weight ratio is prepared, and described extraction concentrate is obtained by water or steam distillation or alcohols extraction solvent extraction calamus class plant roots and stems.
The preparation method of plant insecticide aqua is characterized in that: described extraction concentrate is to adopt steam distillation or alcohols solvent to extract calamus class plant roots and stems to obtain, and the weight ratio of extracting concentrate, aqueous solvent and preservative is 10: 100: 0.5.
Advantage of the present invention:
1, prescription is novel: calamus plant missible oil and aqua, new effective prescription that its characteristics have been to adopt pesticide plant extraction concentrate and synergist to be mixed and to use, active component extracts and adopts ethanol to make to extract solvent, missible oil also adopts ethanol to make solvent, adopt methanol extraction and the preparation agricultural chemicals is commonly used at present solvent xylene to compare with Xie Hongying etc. (2004), to human and environment safety.
2, high-efficiency low-toxicity, to the person poultry safety: the control efficiency to grain storage pest, vegetable-crop pest-insect, sanitary insect pest and flowers insect reaches 100%, and the grain storage pest lasting period was reached more than 1 year.
3, insect is difficult for developing immunity to drugs: because main component comprises in calamus missible oil and the aqua: vegetative insecticidal material, synergist, taken into full account the synergy of extracting each active ingredient in the concentrate, and various active ingredients are to the mechanism of action difference of insect, the action target difference, the active stack in back makes insect be difficult to develop immunity to drugs so be mixed.
4, insecticidal spectrum is extensive: calamus missible oil and aqua are for answering the broad spectrum activity vegetable insecticide, to grain storage primary insect corn weevil, lesser grain borer, gelechiid, later stage property insect saw-toothed grain beetle, the flat ostomatid in long angle, red flour beetle etc., to sanitary insect pest mosquito, fly class, cockroach, flour mite, food leaf, thorn to vegetables, flowers are inhaled class, and boring the moth class pest all has fine control efficiency.Xie Hongying etc. (2004) only in laboratory research to the biologically active of mythimna separata.
5, cost economy: the easy artificial cultivation of calamus class plant, big, the cost economy of biomass, and environmental pollution is little in production processing and the use.Reduce cost, also reduced pollution on the environment simultaneously greatly.
6, easy and simple to handle: the vegetable matter in calamus missible oil and the aqua is for slightly carrying concentrate, and extraction process is simple, and is easy to operate, for batch production production provides possibility.Missible oil and aqua can be processed as pulvis, when grain puts in storage, admix grain with conveyer belt, do not need additionally to increase operation, and also fit and apply in peasant household; Missible oil and aqua can directly be converted water spray when control sanitary insect pest, vegetable-crop pest-insect and flowers insect, using method is also very easy.
Four, embodiment:
The preparation method and the analysis of effective component method of calamus (rhizoma calami, grass-leaved sweetflag) vegetable insecticide are as follows:
(1) vegetable material is prepared: calamus class (rhizoma calami, grass-leaved sweetflag) rhizome is dried or dries in 50～60 ℃ of baking ovens, make water content reach 10～12%, pulverize standby then.
(2) extract: utilize steam distillation from plant drymeal, to extract, or press plant drymeal and solvent (preferred 95% ethanol, benzinum) 1: the part by weight of 5-8, place lucifuge dark place (25～30 ℃) to soak 2h, putting into extraction vessel then at room temperature is extracted into colourless, extracting temperature is 60～95 ℃, filters out solvent then and obtains crude extract;
(3) concentrate: crude extract at room temperature concentrates with Rotary Evaporators, is concentrated into solvent-free oozing again, with extract put into fume hood 1d to the constant weight till, promptly get and extract concentrate, extract concentrate and be contained in the brown bottle, place 4 ℃ of refrigerators standby.
(4) isolation and purification of insecticidal active ingredient in the extraction concentrate:
1. different solvents extraction: utilize benzinum, ethanol, chloroform, ethyl acetate, water different parts extract to carry out biological activity determination.
2. the first column chromatography of calamus (rhizoma calami, grass-leaved sweetflag) petroleum ether extract, secondary chromatography, first column chromatography condition: eluent: benzinum-ethanol, gradient elution (100: 0; 95: 5; 90: 10; 75: 25; 50: 50; 0: 100); Secondary column chromatography condition: eluent, benzinum-ethyl acetate, gradient elution (125: 1; 75: 1; 25: 1; 10: 1; 1: 1).
3. component thin-layer chromatography: can obtain two active principles (monomer).
4. utilize gas-chromatography and standard specimen, operational procedure is carried out active component evaluation and assay thereof routinely, containing main effectively insecticidal constituent in calamus (rhizoma calami, grass-leaved sweetflag) ethanol, benzinum, the steam distillation extraction concentrate is asarone 65～80%, acorone 12.5～18.5%
(5) calamus (rhizoma calami, grass-leaved sweetflag) plant missible oil, aqua quality testing:
1. missible oil and aqua outward appearance
Observe with ocular estimate.Under the room temperature, range estimation should be single-phase transparency liquid.
2. emulsifying effectiveness and emulsion stability is measured
The tool plug graduated cylinder that will be incorporated with 200ml standard hard water (342mg/l) (standard hard water is with reference to " analysis of agricultural drugs " described method preparation) places 30 ± 1 ℃ water bath with thermostatic control, after treating temperature stabilization, freely drip from liquid level 1cm place with pipette, extract missible oil 1ml, observe emulsifying effectiveness and emulsion stability from top and side then.Emulsifying effectiveness divides dispersive property and two aspects of colostrum attitude of missible oil, and its evaluation index is identical, is divided into 5 grades, is specially:
The I level: after splashing into missible oil in the water, can automatically be dispersed into rapidly and be with blue vaporific dispersion, stirring can be light blue or shallow white clear solution a little.
The II level: after splashing into missible oil in the water, can automatically be dispersed into the blue vaporific dispersion of band fluorescence rapidly, stirring can be blue translucent solution a little;
III level: be white in color vaporific after splashing into missible oil in the water or strip disperses, be creamy white after the stirring slightly with the opaque solution of fluorescence;
The IV level: the small oil droplet that is white in color after splashing into missible oil in the water sinks, and opaque emulsion is white in color after the stirring;
V: be big grain oil droplet after dissolving in missible oil in the water and sink rapidly, be emulsion after the stirring, but very fast grease and the precipitation separated out again.
In the above-mentioned standard, the I-III level is qualified, and IV, V are defective.
Adopt domestic prescriptive procedure: the GB/T-1603-2001 standard is carried out, and adds 30 ± 2 ℃ of standard hard water of 100ml in the 250ml beaker, with pipette, extract missible oil sample, under continuous condition of stirring, adds slowly in the hard water, makes it be made into 100ml emulsion.After adding missible oil, continue slowly to stir 30 seconds with the speed of 2～3r/s, immediately emulsion is moved in the 100ml graduated cylinder of cleaning, drying, graduated cylinder is put in the water bath with thermostatic control, observe at 25～30 ℃ of down static 1h, if last no oil slick, following nothing precipitation or heavy oil, wall built-up qualified stability then not, otherwise be defective.
3. cold storage of missible oil and aqua and heat endurance check
Cold storage detects: the missible oil and the aqua sample that prepare are placed 7h in 0 ℃ refrigerator, 14h takes out observations, less than precipitating or oil slick, or small amount of precipitate or oil slick is only arranged but the sample that at room temperature can die away in the 1d is qualified.
Heat storage check: get missible oil and the aqua sample that 30ml prepares and respectively be divided in 3 10ml tool plug scale test tubes, seal.Place 54 ± 2 ℃ insulating box, take out test behind the 14d, the transparent homogeneous of preparation, there is not precipitation, color then is qualified than dark a little monochromatic transparency liquid before storing, and then insect carried out toxicity test, to investigate the influence of temperature, therefrom understand the time limit that it can be remained valid under normal temperature to the medicament insecticidal activity.
Cold storage and heat storage missible oil sample also all need be by the tests of above-mentioned emulsifying effectiveness and emulsion stability.
4. the formulation of pH value: carry out according to GB/1601-1993 agricultural chemicals pH value assay method.
The saturated calomel electrode of Delta320-SPH is inserted 0.05mol/l potassium hydrogen phthalate solution, adopt some calibration methods to proofread and correct, use the distilled water cleaning electrode.
Take by weighing sample 1g in beaker, add 99ml water, vigorous stirring 1min, static 1min.
Electrode is put into sample to be tested solution, measure its pH value.At least parallel determination is three times, and the measurement result difference should be got the pH value of its arithmetic mean of instantaneous value as this sample less than 0.1.
5. moisture determination: measure according to the international analysis of agricultural drugs committee of association (CIPAC) agricultural chemicals determination of moisture method.
The preparation and the efficiency test of calamus class (rhizoma calami, grass-leaved sweetflag) insecticide emulsifiable concentrate and aqua product are as follows:
Vegetable source pesticide agent emulsifiable solution active component is extracted by alcohols, ethers equal solvent, contain calamus class (rhizoma calami, grass-leaved sweetflag) plant roots and stems and extract concentrate, solvent (70～100% ethanol), emulsifier (OP-10, OP-15, farming breast 100), synergist (2.5% decis or 10% Imidacloprid) is 0.5～20: 100: 2～5: 0.05--1 by weight.
The active component of plant insecticide aqua is extracted by steam distillation and alcohols solvent, contain calamus class (rhizoma calami, grass-leaved sweetflag) rhizome and extract concentrate, aqueous solvent, preservative (sorbic acid or diacetic acid), its weight ratio is 0.5～10: 100: 0.5～1.0.
Calamus (rhizoma calami, grass-leaved sweetflag) rhizome steam distillation or alcohols or ethers etc. extract in the concentrate, and main effectively insecticidal constituent comprises asarone and acorone, wherein preferred asarone 65%～80%, calamus cave 12.5%～18.5%.
The embodiment of optimizing is exemplified below:
Embodiment 1:
The preparation of rhizoma calami missible oil: to the preparation of preferred rhizoma calami missible oil, adopt rhizoma calami rhizome 95% alcohol extract concentrate, solvent (95% ethanol), emulsifier op-10, synergist 2.5% decis or 10% Imidacloprid, be 4: 100: 3 by weight: 1 makes missible oil.
Embodiment 2:
Grass-leaved sweetflag emulsifiable concentrate formulation and ratio are the same, utilize grass-leaved sweetflag to replace rhizoma calami.
Embodiment 3:
The preparation of rhizoma calami aqua: adopt rhizoma calami rhizome steam distillation or 95% alcohol extract concentrate, aqueous solvent, preservative sorbic acid to make aqua by weight 10: 100: 0.5.
Embodiment 4:
The prescription and the ratio of grass-leaved sweetflag aqua are the same, utilize grass-leaved sweetflag to replace rhizoma calami.。The quality testing result of calamus (rhizoma calami, grass-leaved sweetflag) missible oil and aqua is as follows:
As embodiment 1 and 2 calamus missible oil and embodiment 3 and 4 calamus aquas:
| Formulation | Embodiment 1 and 2 calamus missible oil | Embodiment 3 and 4 calamus aquas |
| Test item | Testing result | |
| Emulsifying dispersivity | Emulsified state: stir a little, be blue translucent milky liquid dispersity: can automatically disperse rapidly, evaluation criterion is II level (qualified) | |
| Missible oil and/or aqua stability | No oil slick, heavy oil, precipitation are separated out, and stability meets | Do not have precipitation and separate out, stability meets |
| Low-temperature stability | 0 ± 1 ℃ of cold storage 7d takes out not have and freezes phenomenon | 0 ± 1 ℃ of cold storage 7d takes out not have and freezes phenomenon |
| Heat temperature stability | Place under 54 ± 2 ℃, the transparent homogeneous of preparation does not have precipitation and oil slick, and color is than dark a little before storing. | Place under 54 ± 2 ℃, the transparent homogeneous of preparation does not have precipitation, and color is than dark a little before storing. |
It is qualified that the missible oil of other content of calamus plant and aqua also are through quality testing.
The insecticidal activity analysis that calamus class (rhizoma calami, grass-leaved sweetflag) rhizome different solvents extracts concentrate is compared as follows:
Plant drymeal is dried, pulverized to calamus class (rhizoma calami, grass-leaved sweetflag) rhizome put into container under 50～60 ℃ of temperature, respectively with 95% ethanol or benzinum or acetone or ethyl acetate immersion, put into then and extract still and be extracted into colourlessly, obtain crude extract.Crude extract concentrates with Rotary Evaporators, is concentrated into solvent-free oozing again, and promptly gets and extracts concentrate, uses for biological activity determination.
The mensuration of action of contace poison: adopt the filter paper medicine embrane method, according to the volume ratio of extracting concentrate weight and solution, with acetone each is extracted concentrate and be made into 0.50,0.25 respectively, the soup of 0.13g/ml, on the culture dish chassis of diameter 9cm, put into the identical circular filter paper of area, on filter paper, splash into plant extract concentrate acetone diluted liquid 1ml, be equivalent to complete absorptive amount 7.86 on the filter paper respectively, 3.93,1.97mg/cm
2, filter paper absorbs fully to dripping soup.Splash into equivalent acetone as blank at another filter paper with diameter.For the examination insect main grain storage pest lesser grain borer adult is arranged, the female aphid of the virginopara of vegetable-crop pest-insect cabbage caterpillar, vegetable aphid, every processing 3 times repeats, and whenever repeats to insert for 30 of examination insects.Because corundum Sitophilusspp. imago, Groton bug adult, diamondback moth larvae are active, for preventing to escape, the test of tagging of these three kinds of insects is carried out in Cans, but every cm
2Medicine carrying amount on the area be provided with test with culture dish identical.(27 ± 1 ℃ of temperature, relative moisture 75 ± 5%) in the insectary is put in each processing, check the effect of once tagging, observe 96h continuously, the calculation correction lethality every 24h.Give birth to survey and the results are shown in Table 1.
Each of table 1 rhizoma calami rhizome different solvents extraction concentrate processing is for examination insect 96h post-equalization lethality
(％)
| Extract | Concentration (mg/cm 2) | Corundum Sitophilusspp. imago | The lesser grain borer adult | The Groton bug adult | Diamondback moth larvae | Cabbage caterpillar | Vegetable aphid |
| 95% ethanol extract | 7.86 | 100％ | 100％ | 100％ | 100％ | 100％ | 100％ |
| Ligroin extraction | 7.86 | 100％ | 100％ | 100％ | 100％ | 100％ | 100％ |
| Acetone extract | 7.86 | 91.11％ | 90.5％ | 92.5％ | 91.8％ | 91.5％ | 92.3％ |
| Ethyl acetate extract | 7.86 | 93.33％ | 92.5％ | 91.8％ | 92.3％ | 94.2％ | 95.1％ |
Find out by table 1, the rhizoma calami rhizome all has very strong contact toxicity by the extraction concentrate of above-mentioned 4 kinds of solvents to 6 kinds of insects for examination, behind the processing 96h, reaches 90.5～100% for the corrected mortality that tries insect, wherein the activity of 95% ethanol and Petroleum ether extraction is the highest, handles the death entirely of 96h insect.So preferred alcohol, benzinum are as the extraction solvent of rhizoma calami rhizome.
With with above-mentioned same quadrat method, steam distillation is extracted concentrate, 70% ethanol, absolute ethyl alcohol rhizoma calami are extracted concentrate and above-mentioned 6 kinds of insects are carried out contact toxicity measure, handle 96h after, each also all reaches 100% for examination insect corrected mortality.Use steam distillation, 70% ethanol, 95% ethanol, absolute ethyl alcohol and benzinum extract the grass-leaved sweetflag rhizome, use with above-mentioned and with quadrat method above-mentioned 6 kinds of insects are carried out contact toxicity mensuration, and each is for the also all whole death of examination insect behind the processing 96h.Compare with other people research, Xie Hongying etc. (2004) report that according to laboratory research the grass-leaved sweetflag methanolic extract reaches 60% to the lethality of tagging of armyworm larvae, methyl alcohol is big to people's toxicity, environmental pollution is serious, methanolic extract is to the lethality only about 60% of tagging of armyworm larvae, and the present invention adopts steam distillation and ethanol as calamus class (rhizoma calami, grass-leaved sweetflag) extraction of active ingredients solvent, and not only insecticidal activity improves greatly, and to human and environment safety.
Calamus class (rhizoma calami, grass-leaved sweetflag) plant insecticide agent emulsifiable solution and aqua can adopt spraying, ultralow molten amount spraying and mix grain and use, prevent and treat main grain storage pest (corn weevil, lesser grain borer, gelechiid, Indian meal moth, red flour beetle, the flat ostomatid in long angle, saw-toothed grain beetle, booklice, flour mite etc.), sanitary insect pest (mosquito, fly class, cockroach, bedbug, flour mite) and vegetables, the food leaf class of flowers, thorn suction class, brill moth class pest, calamus insecticide emulsifiable concentrate and aqua product are as follows to various insect application technologies and control efficiency:
(1) the grass-leaved sweetflag missible oil of the control rhizoma calami missible oil of grain storage pest: embodiment 1 and embodiment 2 press grain weight 3 using dosages of design (dosing/grain weight) be 10mg/kg, 20mg/kg, 30mg/kg), and establish blank, utilize rice chaff for carrier fully and the paddy mix, every Treatment Design repeats for 3 times, handle the back and inserted insect in every month and observed the insect lethality, represent control efficiency (table 2) with the insect corrected mortality.
(2) control sanitary insect pest: to the control test of mosquito, family's rope, Groton bug adult, at gauze cage (50 * 50 * 50cm
3) in carry out, insert above-mentionedly in every cage for each 30 of examination adults, the rhizoma calami missible oil of embodiment 1 and the grass-leaved sweetflag missible oil of embodiment 2 respectively are provided with promptly 1: 1000 times of 3 concentration gradient (consumption/water of medicine), 1: 2000 times, 1: 4000 times; The % grass-leaved sweetflag aqua of the rhizoma calami aqua of embodiment 3 and embodiment 4 is with 1: 500 times, and 1: 1000 times, 1: 2000 times of spraying.And compare with clear water spraying, 3 repetition are established in every processing, handle back 24h, 48h, and 72h investigates the insect lethality, represents control efficiency (seeing Table 3) with corrected mortality.
(3) control vegetables and flowers insect: to the control test of the little Macrosiphus spp of chrysanthemum on vegetable-crop pest-insect vegetable aphid, diamondback moth larvae, cabbage caterpillar and the flowers, will be potted plant for vegetables, the flowers of examination, every basin inserts above-mentioned for 30 of examination insects, and covers with sarong.With 1: 1000 times of each dilute with water of grass-leaved sweetflag missible oil of rhizoma calami missible oil among the embodiment 1 and embodiment 2,1: 2000 times, 1: 4000 times of spraying, the rhizoma calami aqua of embodiment 3 and the grass-leaved sweetflag aqua of embodiment 4 are with 1: 500 times, 1: 1000 times, 1: 2000 times of spraying, and add a small amount of synergist, compare with the clear water spraying.3 repetitions are established in every processing, handle back 24h, 48h, and 72h investigation insect lethality is represented control efficiency (table 4) with corrected mortality.
Table 2 calamus missible oil is to the control efficiency of main grain storage pest corn weevil
| Reagent agent | Dosage (mg/kg) | Insect corrected mortality % | |||||||||||
| After handling January | After February | After March | After April | After May | After June | After July | After August | After September | After October | After November | After December | ||
| Embodiment 1 missible oil | 10 | 85.4 | 85.2 | 85.1 | 85.1 | 85.0 | 85.0 | 85.0 | 84.8 | 84.7 | 84.5 | 84.5 | 84.4 |
| 20 | 100.0 | 100.0 | 100.0 | 100.0 | 100.0 | 100.0 | 100.0 | 100.0 | 98.7 | 98.6 | 98.6 | 98.5 | |
| 30 | 100.0 | 100.0 | 100.0 | 100.0 | 100.0 | 100.0 | 100.0 | 100.0 | 99.8 | 99.6 | 99.6 | 99.4 | |
| Embodiment 2 missible oil | 10 | 85.3 | 85.1 | 85.1 | 85.0 | 85.0 | 84.9 | 84.8 | 84.6 | 84.5 | 84.4 | 84.2 | 84.2 |
| 20 | 100.0 | 100.0 | 100.0 | 100.0 | 100.0 | 100.0 | 100.0 | 98.9 | 98.6 | 98.5 | 98.2 | 98.0 | |
| 30 | 100.0 | 100.0 | 100.0 | 100.0 | 100.0 | 100.0 | 100.0 | 99.9 | 99.7 | 99.5 | 99.4 | 99.2 | |
Found out after the rhizoma calami missible oil of embodiment 1 and the grass-leaved sweetflag missible oil of embodiment 2 are mixed grain with 10～30mg/kg dosage, corn weevil is all had desirable control efficiency by table 2, preventive effect can reach 84.2～100%.From preventive effect, safety and economic integrated survey, the preferred using dosage of 20mg/kg handles that control efficiency still reaches 98.0～98.5% after 1 year.Adopt said method that grain storage pest lesser grain borer, gelechiid, Indian meal moth, red flour beetle, booklice, flour mite are prevented and treated test, handle after 12 months, the control efficiency of two kinds of missible oil is all more than 95.0%.
Table 3 calamus missible oil and aqua are to the control efficiency of main sanitary insect pest
| Reagent agent | Concentration | Mosquito corrected mortality % | Adult housefly corrected mortality % | Groton bug corrected mortality % | ||||||
| 24h | 48h | 72h | 24h | 48h | 72h | 24h | 48h | 72h | ||
| Embodiment 1 missible oil | 1∶1000 | 88.5 | 95.2 | 100.0 | 88.4 | 95.0 | 100.0 | 87.6 | 92.3 | 100.0 |
| 1∶2000 | 88.3 | 94.9 | 100.0 | 88.1 | 94.8 | 100.0 | 86.7 | 90.8 | 100.0 | |
| 1∶4000 | 67.8 | 72.5 | 86.5 | 66.9 | 71.8 | 85.8 | 65.7 | 70.6 | 84.7 | |
| Embodiment 2 missible oil | 1∶1000 | 87.6 | 95.0 | 100.0 | 88.2 | 94.8 | 100.0 | 86.8 | 91.5 | 100.0 |
| 1∶2000 | 88.2 | 94.6 | 100.0 | 88.0 | 94.5 | 100.0 | 85.6 | 90.5 | 100.0 | |
| 1∶4000 | 66.7 | 71.8 | 85.7 | 65.8 | 70.6 | 85.2 | 65.5 | 70.3 | 84.2 | |
| Embodiment 3 aquas | 1∶500 | 88.6 | 96.1 | 100.0 | 88.3 | 95.8 | 100.0 | 87.9 | 93.5 | 100.0 |
| 1∶1000 | 88.4 | 95.9 | 100.0 | 88.2 | 95.6 | 100.0 | 87.4 | 92.8 | 100.0 | |
| 1∶2000 | 71.5 | 77.2 | 87.4 | 70.9 | 76.8 | 87.2 | 70.5 | 78.4 | 86.5 | |
| Embodiment 4 aquas | 1∶500 | 88.4 | 95.8 | 100.0 | 88.2 | 95.7 | 100.0 | 86.8 | 93.3 | 100.0 |
| 1∶1000 | 88.3 | 95.5 | 100.0 | 87.8 | 95.3 | 100.0 | 87.2 | 92.4 | 100.0 | |
| 1∶2000 | 70.8 | 76.7 | 86.8 | 70.5 | 76.5 | 86.5 | 70.2 | 78.3 | 86.3 | |
As shown in Table 3,1000～4000 times of calamus missible oil and aqua all have very high killing effect with 500～2000 times of liquid spraying backs to mosquito, housefly, cockroach.Take all factors into consideration from control efficiency, safety and economy, but 1: 1000 times of spraying control of the calamus aqua of 1: 2000 times of the calamus missible oil of preferred embodiment 1 or 2 or embodiment 3 or 4.
Table 4 calamus missible oil and aqua are to the control efficiency of main vegetables, flowers insect
| Reagent agent | Concentration | Vegetable aphid corrected mortality % | Diamondback moth larvae corrected mortality % | Cabbage caterpillar corrected mortality % | The little long tube aphid of chrysanthemum corrected mortality % | ||||||||
| 24h | 48h | 72h | 24h | 48h | 72h | 24h | 48h | 72h | 24h | 48h | 72h | ||
| Embodiment 1 missible oil | 1∶1000 | 85.2 | 95.6 | 100.0 | 84.9 | 93.7 | 100.0 | 85.1 | 95.4 | 100.0 | 85.3 | 95.5 | 100.0 |
| 1∶2000 | 85.0 | 95.2 | 100.0 | 84.7 | 92.5 | 100.0 | 84.9 | 94.8 | 100.0 | 85.1 | 94.2 | 100.0 | |
| 1∶4000 | 73.5 | 81.6 | 89.5 | 70.8 | 80.7 | 85.3 | 71.9 | 82.3 | 87.8 | 74.2 | 82.1 | 89.2 | |
| Embodiment 2 missible oil | 1∶1000 | 85.1 | 95.4 | 100.0 | 82.6 | 92.8 | 100.0 | 84.8 | 95.3 | 100.0 | 85.2 | 95.4 | 100.0 |
| 1∶2000 | 84.6 | 95.1 | 100.0 | 84.3 | 92.4 | 100.0 | 84.5 | 94.2 | 100.0 | 84.9 | 93.7 | 100.0 | |
| 1∶4000 | 72.8 | 80.9 | 89.2 | 70.5 | 80.3 | 85.1 | 71.5 | 81.6 | 87.5 | 74.0 | 81.4 | 88.6 | |
| Embodiment 3 aquas | 1∶500 | 87.8 | 96.5 | 100.0 | 85.6 | 95.2 | 100.0 | 87.5 | 95.8 | 100.0 | 87.5 | 96.3 | 100.0 |
| 1∶1000 | 87.5 | 95.7 | 100.0 | 85.4 | 93.8 | 100.0 | 87.4 | 95.5 | 100.0 | 86.9 | 95.8 | 100.0 | |
| 1∶2000 | 72.8 | 82.5 | 85.6 | 71.5 | 80.5 | 84.7 | 72.5 | 81.6 | 85.3 | 72.5 | 82.3 | 85.5 | |
| Embodiment 4 aquas | 1∶500 | 86.9 | 95.4 | 100.0 | 85.1 | 95.0 | 100.0 | 86.7 | 94.8 | 100.0 | 85.6 | 95.5 | 100.0 |
| 1∶1000 | 86.7 | 95.2 | 100.0 | 84.5 | 93.6 | 100.0 | 85.5 | 94.5 | 100.0 | 85.5 | 93.5 | 100.0 | |
| 1∶2000 | 71.6 | 80.5 | 83.5 | 71.3 | 79.5 | 82.4 | 72.1 | 81.5 | 85.1 | 71.5 | 80.2 | 83.3 |
Table 4 shows, 1000～4000 times of calamus missible oil and aqua use 500～2000 times of liquid sprayings, main vegetables and flowers insect all there is certain control efficiency, wherein embodiment 1 and 2 calamus missible oil use 1000～2000 times of liquid sprayings, the insect lethality all can reach 100% after handling 72h, embodiment 3 and 4 calamus aqua use 500～1000 times of liquid sprayings, handle 72h after the insect lethality also all reach 100%.
Though to description references of the present invention exemplifying embodiment, it will be understood by those skilled in the art that under the situation that does not break away from the spirit and scope of the present invention, can make multiple modification to it.Within each exemplifying embodiment and the spirit and scope of the present invention that its obvious modification is all belonged in the claim to be proposed.
Claims (17)
1. vegetable source pesticide agent emulsifiable solution, contain is 0.5～20 by weight: 100: 2～5 calamus class plant roots and stems extracts concentrate, solvent, emulsifier, wherein said extraction concentrate extracts calamus class plant roots and stems and obtains for extracting solvent or steam distillation by alcohols or ethers or ketone or esters solvent, solvent is 70%～100% ethanol, and emulsifier is OP～10 or OP～15 or farming breast 100.
2. vegetable source pesticide agent emulsifiable solution according to claim 1, can use 2.5% decis, 10% Imidacloprid as synergist, the weight ratio that calamus class plant roots and stems extracts concentrate, solvent, emulsifier and synergist is 0.5～20: 100: 2～5: 0.05～1.
3. vegetable source pesticide agent emulsifiable solution according to claim 1, it is characterized in that: containing weight ratio is 4: 100: 3: 1 calamus class plant roots and stems extracts concentrate, solvent, emulsifier, synergist, solvent is 70～100% ethanol, emulsifier is OP～10 or OP～15, and synergist is that 2.5% decis, 10% is than worm quinoline.
4. vegetable source pesticide agent emulsifiable solution according to claim 1 is characterized in that: missible oil product solvent for use is 95% ethanol, and emulsifier is OP～10 or OP～15.
5. plant insecticide aqua, contain is 0.5～10 by weight: 100: 0.5～1 calamus class plant roots and stems extracts concentrate, aqueous solvent and preservative, and described extraction concentrate extracts solvent extraction calamus class plant roots and stems by water or steam distillation or alcohols and obtains.
6. plant insecticide aqua according to claim 5, it is characterized in that: described extraction concentrate is to adopt steam distillation or alcohols solvent to extract calamus class plant roots and stems to obtain, and extracting concentrate, aqueous solvent and preservative is 10: 100: 0.5 by weight.
7. plant insecticide aqua according to claim 4 is characterized in that: described preservative is a sorbic acid, diacetic acid.
8. the described plant insecticide aqua of vegetable source pesticide agent emulsifiable solution according to claim 1 or claim 5, described calamus class plant roots and stems extracts in the concentrate, comprise as the main effectively asarone 65%～80% of insecticidal constituent, acorone 12.5%～18.5%.
9. the application method of described vegetable source pesticide agent emulsifiable solution of claim 1 or the described plant insecticide aqua of claim 5 adopts spraying, ultra low volume spraying or mixes the grain use, is used to prevent and treat grain storage pest, sanitary insect pest, vegetable-crop pest-insect or flowers insect.
10. application method according to claim 9, it is characterized in that being used to prevent and treat grain storage pest, utilize rice chaff, diatom great soil group to be carrier, described missible oil or described aqua and carrier and grain are mixed and stirred, by extracting the concentrate using dosage is 5～25mg/kg grain, all insects of shelf time in control storage paddy, wheat, corn, jowar, the beans.
11. application method according to claim 9, it is characterized in that adopting spray method to use for 1000～4000 times described missible oil or the dilution of described aqua, or described missible oil or described aqua directly carried out ultra low volume spraying, mosquito, fly class, cockroach, bedbug, the flour mite of control sanitary insect pest, or food leaf class, thorn suction class, the brill moth class various pests of preventing and treating vegetables, flowers.
12. the preparation method of a vegetable source pesticide agent emulsifiable solution, calamus class plant roots and stems is extracted concentrate, solvent, emulsifier by 0.5～20: 100: 2～5 weight ratio is prepared, wherein said extraction concentrate extracts calamus class plant roots and stems and obtains for extracting solvent or steam distillation by alcohols or ethers or ketone or esters solvent, solvent is 70%～100% ethanol, and emulsifier is OP～10 or OP～15 or farming breast 100.
13. the preparation method of vegetable source pesticide agent emulsifiable solution according to claim 12, calamus class plant roots and stems is extracted concentrate, solvent, emulsifier, synergist by 4: 100: 3: 1 weight ratio is configured, solvent is 70～100% ethanol, emulsifier is OP～10 or OP～15, and synergist is 2.5% decis or 10% Imidacloprid.
14. the preparation method of a plant insecticide aqua, calamus class plant roots and stems is extracted concentrate, aqueous solvent and preservative by 0.5～10: 100: 0.5～1 weight ratio is prepared, and described extraction concentrate is obtained by water or steam distillation or alcohols extraction solvent extraction calamus class plant roots and stems.
15. the preparation method of plant insecticide aqua according to claim 14, it is characterized in that: described extraction concentrate is to adopt steam distillation or alcohols solvent to extract calamus class plant roots and stems to obtain, and the weight ratio of extracting concentrate, aqueous solvent and preservative is 10: 100: 0.5.
16. according to one of one of described vegetable source pesticide agent emulsifiable solution of one of claim 1 to 4 or claim 5 to 7 described plant insecticide aqua or claim 13 to 15 described preparation method, described extraction solvent is ethanol or benzinum or acetone or ethyl acetate.
17., it is characterized in that described calamus class plant is rhizoma calami or grass-leaved sweetflag according to one of one of described vegetable source pesticide agent emulsifiable solution of one of claim 1 to 3 or claim 4 to 7 described plant insecticide aqua or claim 13 to 14 described preparation method.
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| CN103053628A (en) * | 2012-03-22 | 2013-04-24 | 华南农业大学 | Plant source solenopsis invicta bait formulation |
| CN103535390A (en) * | 2013-09-27 | 2014-01-29 | 江志鑫 | Insecticidal composition |
| CN104397056A (en) * | 2014-10-30 | 2015-03-11 | 咸宁市幕山茶业有限公司 | Method for controlling chili acanthocoris scaber by using plant-sourced pesticide |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1312008A (en) * | 2001-02-13 | 2001-09-12 | 赵大奇 | Botanical insecticide and its production process |
| KR20040089051A (en) * | 2004-09-08 | 2004-10-20 | 차민철 | Fungi-free extract of the leaf and root of calamus which treats amnesia, improves one's memory, puts someone at ease and removes fatigue |
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- 2006-01-20 CN CNB2006100013990A patent/CN100431422C/en not_active Expired - Fee Related
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103053628A (en) * | 2012-03-22 | 2013-04-24 | 华南农业大学 | Plant source solenopsis invicta bait formulation |
| CN103053628B (en) * | 2012-03-22 | 2018-03-30 | 华南农业大学 | A kind of plant source fire ant bait agent |
| CN103535390A (en) * | 2013-09-27 | 2014-01-29 | 江志鑫 | Insecticidal composition |
| CN104397056A (en) * | 2014-10-30 | 2015-03-11 | 咸宁市幕山茶业有限公司 | Method for controlling chili acanthocoris scaber by using plant-sourced pesticide |
| CN105165921A (en) * | 2015-09-14 | 2015-12-23 | 陈永强 | Mould-proof repellent mat for files and preparation method thereof |
| CN107156207A (en) * | 2017-06-01 | 2017-09-15 | 磐安县派普特生物科技有限公司 | A kind of vegetable source natural insecticide and preparation method thereof |
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