Background technology
Aphid, two spotted spider mite, fragrant-flowered garlic maggot, Paratrioza sinica, pear sucker, cabbage caterpillar, diamond-back moth, mythimna separata etc. be melon, really, the primary pest on vegetables, flowers, damaging range is wide, difficulty is larger in control.The medicament of these insects of control is mainly chemical agent at present, yet long-term a large amount of chemical medication has caused producing the appearance of the problems such as pesticide resistance, environmental pollution, harm humans health; In addition, the export of farm produce suffers the impact of " green barrier " repeatly, causes country to have to limit the use of many chemical pesticides.From the natural resources treasure-house, finding insecticide active substance, becoming important channel and the study hotspot of novel pesticide initiative.Particularly the science by multiple components composite after, the effect of vegetable source pesticide active substance can significantly improve.
Matrine is by root, stem and the fruit of pulse family Sophora machaka kuh-seng (SophoraflavescensAit), to be extracted a kind of water-soluble alkaloid obtained through strict technique, and outward appearance is the brown homogeneous liquid.Be generally Banlangen, its main component has matrine, oxymatrine, sophocarpine, N-Oxysophocarpine, Sophoridine etc.Wherein the content with matrine and oxymatrine is the highest.
Matrine is the broad spectrum activity plant insecticide, and insect is had to stomach toxicity and action of contace poison.Main Function is in the nervous system of insect, and the sodium-ion channel of insect nerve cell is had to the concentration dependent blocking effect, can cause the nervous centralis paralysis, and then suppress the respiration of insect, makes insect death by suffocation.Can effectively prevent and treat Lepidoptera, Homoptera, coleoptera, acarina pest such as aphid class, stinkbug class, cabbage caterpillar, diamond-back moth, peach fruit borer, rice fulgorid, rice leaf roller, two spotted spider mite etc.
Macleaya cordata alkaloids is the main active of Papaveraceae Macleaya plant macleaya cordata, and it contains multiple single alkali such as sanguinarine, dihydrosanguinarine and dish alkali in the wrong.Wherein sanguinarine mainly is present in the herb of greater celandine, the piece root of corydalis, the herb of macleaya cordata, the acrial part of snowpoppy.The evidences such as Sun Guangzhong, 1% sanguinarine wetting powder has good insect killing effect to the apple Tetranychus urticae, and working concentration is in the time of 2500 times, and 2500 times of liquid phases of 20% pyridaben wetting powder of promoting the use of in control efficiency and production are worked as; Dihydrosanguinarine has higher toxic action to mythimna separata 3 instar larvaes; The LC of the macleaya cordata made by the acidic ethanol extraction method to tested suede tail fly maggot maggot in 3 age
50For 148.75g/L, 95% credibility interval is 122.19g/L-180.94g/L.
The data-searching of doing according to the applicant, at present in matrine and macleaya cordata extracts, the sanguinarine of one of main component is composite or take that matrine, sanguinarine are composite to be mainly contained as basic mixed insecticide: Wang Zhengguo etc. have applied for the patent of jamaicin matrine sterilization and disinsection aqua, publication number is CN1401235, and this invention mainly contains jamaicin 0.5%~2.5% and matrine 0.1~2.0%.The present invention is mainly used in preventing and treating the insects such as mythimna separata and kill bacteria etc.Lv Shilu has applied for the patent of 0.36% matrine water agriculture chemicals and production method thereof, publication number is CN1422531, it is characterized in that vegetable insecticide made by kuh-seng, the tuber of stemona, tobacco, China tree, Dalmatian chrysanthemum compatibility, its compatibility is: kuh-seng: 52.5~72kg, the tuber of stemona: 12~22.5kg, tobacco: 22.5~37.5kg, China tree: 15~37.5kg, Dalmatian chrysanthemum: 4.5-15kg; Described auxiliary agent comprises that turpentine oil, concentration are ethanol, emulsifier, bleeding agent, the preservative of 70 °-95 °, and the charge ratio of auxiliary agent is turpentine oil 10~17.5kg, ethanol 17.5~24kg, emulsifier 5~11.5kg, bleeding agent 2.5~6kg, preservative 0.3~1.3kg; The charge ratio of vegetable insecticide and auxiliary agent is counted 1~1.5:1 by weight ratio.Chen Zhijun etc. have applied for the patent of 0.08% aqueous matrine solution, publication number is CN1171198, by pure natural plant kuh-seng, China tree, tobacco, trifoliate jewelvine, thunder godvine, maple willow, hop, rule grass, mountain flower green pepper, through pulverizing, extraction, concentrated, alcohol precipitation, return and stay, be mixed.Its compatibility is kuh-seng 20%, China tree 20%, tobacco 10%, trifoliate jewelvine 5%, thunder godvine 5%, maple willow 20%, hop 6%, rule grass 4%, mountain flower green pepper 10%.Aqueous matrine solution to Lepidoptera, the Semiptera of vegetables, fruit tree, flowers, forest, field crop, stick up the various pests such as wing, Homoptera obvious control efficiency arranged.Qian Yixin etc. have applied for the patent of matrine-cybermethrin mixed preparation and manufacture method thereof, and publication number is CN1149385, contain matrine 1.0%~10.0%, cypermethrin 0.5%~5.0%, emulsifier 5.0%~8.0%, solvent 77.0%~94.0%.Its production method is: the matrine raw material pulverized, crossed 20~40 mesh sieves, then the raw material powder is mixed with 50% ethanol to infiltrate and dissolve, and refluxing extraction, extract is concentrated through heating evaporation, and obtains matrine; Matrine, cypermethrin, emulsifier, solvent, add reactor to be mixed in proportion, and finally packing, good to control efficiency such as fruit tree, vegetables, cotton aphid, tea tree tea geometrids.Lv Shilu etc. have applied for the patent of 0.36% aqueous matrine solution, publication number CN1276160, by kuh-seng 40%, tobacco 20%, the tuber of stemona 10%, chinaberry 15%, Dalmatian chrysanthemum 5%, catharanthus roseus 4%, thunder godvine 6%, through pulverizing respectively, immersion, boiling extract, filter, concentrated, solution mixing, precipitation, filtration, solvent refluxing, collect mother liquor, adding turpentine oil 29%, ethanol 44%, emulsifier 18%, bleeding agent 8%, preservative 1%, the liquid made in two hours in reaction kettle for reaction, in liquid, contain matrine 0.36%, have good insecticidal effect.Shi Jiansheng has applied for the patent of a kind of vegetable insecticide that contains matrine and its preparation method and application, publication number is CN101156609, in the raw material of this invention, contains the bulk drug of following weight portion: 0.8~1.2 part of 9.0~10.0 parts of kuh-sengs, 1.5~2.0 parts of thunder godvines, 3.2~3.5 parts of black false hellebores, 1.2~1.4 parts of the roots of langdu, 0.8~1.2 part of capsicum annum fasciculatum, 1.2~1.6 parts, tobacco leaf, 0.8~1.2 part of azedarach and the tuber of stemona.The Zhang Wenlong application patent of matrine agent plant pesticide and preparation method thereof of special for killing aphids, publication number is CN101233865, 11~13 parts of Chinese medicine extracts that contain matrine, 10~20 parts of emulsifier, 4~8 parts of bleeding agents, 0.1 part, antioxidant, 57~64 parts of deionized waters, the Chinese medicine extract that this invention contains matrine is for by weight by 15~25 parts of kuh-sengs, 10~17 parts of China trees, 3~4 parts of tarragons, 6~8 parts of Celastrus angulatus, 4~8 parts of trifoliate jewelvines, 2~4 parts of cape jasmines, 7~9 parts of oriental wormwoods, 10~14 parts of gelsemium elegan, 5~7 parts of citrus seeds, 7~10 parts of mixed extracts of Chinese wingnut leaf, in this insecticide, contain 1.3% the superelevation content matrine of having an appointment.The Zhang Wenlong application patent of matrine agent plant pesticide and preparation method thereof of special for killing cabbage worm, publication number is CN101233866, Chinese medicine extract 15-20 part of containing matrine, emulsifier 10-20 part, 4~8 parts of bleeding agents, 0.1 part, antioxidant, 55~60 parts of deionized waters, the Chinese medicine extract that this invention contains matrine is for by weight by kuh-seng 20-30 part, 7~10 parts of Fructus meliae toosendans, 12~19 parts of melia toosendan skins, 10~15 parts of thunder godvines, 18~24 parts of Radix Aconiti Kusnezoffiis, 4~6 parts of the roots of langdu, 6~8 parts of mixed extracts of dried orange peel, in this insecticide, contain 2.0% the superelevation content matrine of having an appointment.Li Jianzhong has applied for a kind of patent that contains the Pesticidal combination of Affirm (Merck Co.) and matrine, publication number is CN1650710, contain the combination of Affirm (Merck Co.) and matrine as active component, wherein, matrine comprises from the Chinese herbal medicine kuh-seng, Sophora alopecuroide, fabaceous of root of subprostrate sophora etc., stem, the a series of alkaloid formulations that extract in fruit, in the composite embodiment of kuh-seng and emamectin-benzoate, refer to mainly take that matrine and oxymatrine thereof are as main, but be not limited to this two kinds of alkaloids, and Affirm (Merck Co.) or its salt: matrine=1:0.01-100.Guo Jiankang has applied for a kind of patent of matrine capsaicin composite pesticide, and publication number is CN1663380, and host has matrine, capsaicine and auxiliary agent formulated, and raw material is commercially available; Production technology cylinder list, namely prepare burden by a certain percentage, by the refinement mixing apparatus, stirs in certain temperature range, and analysis host active constituent content meets the requirements and gets final product.Chen Deshou etc. have applied for the patent of 0.3% matrine insecticide and preparation method thereof, publication number is CN1557156, and this insecticide is by a certain amount of, to add preservative, bleeding agent and auxiliary agent mixing preparation to make by kuh-seng, Lappula echinata, chinaberry, Anemone Vitifolia, Dalmatian chrysanthemum, Chinese honey locust after extracting, concentrating again.Yang Helin has applied for the patent of 0.3% matrine vegetable insecticide (0.3% aqueous matrine solution), publication number is CN101095413, take the Chinese herbal medicine kuh-seng as main, and that joins counts the flavor Chinese herbal medicine with other, through industrialization, extract supernatant, add again the novel agrochemical that various medical, edible auxiliary agents are made.Chen Zhangyan etc. have applied for containing the patent of the composition pesticide of indoxacarb and matrine, publication number is CN101366389, wherein the weight ratio of indoxacarb and matrine is preferably 50:1~1:1,20:1~1:1 more preferably, be particularly preferably 20:1~8:1, this composition pesticide is specially adapted to pest control such as prodenia litura.Zhang Rong etc. have applied for the patent of matrine chlorpyrifos water agent, publication number is CN101422177, it is characterized in that being re-dubbed aqua by chlopyrifos and matrine vegetable extract, the content of its Chlorpyrifos is 1-2mg/L, and the content of matrine vegetable extract is 2-5mg/L.Li Wuliang etc. have applied for the patent of 0.3% matrine compound agent, publication number is CN101449687, it is characterized in that take that natural plants is main body, comprise traditional Chinese medicine more than five kinds, formulated by the extraction of the techniques such as immersion, boiling, filtration, plant resource raw material used and content (weight) are: kuh-seng 35%~45%, south tongue rattan 10%~15%, chinaberry 12%~18%, radix aconiti agrestis 10%~15%, hairyvein agrimony 8%~13%; Nicotiniana rustica 11%~16%, also can increase by hundred steps 2%~5%, thunder godvine 2%~5%, above-mentioned raw materials extract and the preparation of dilution emulsifier.Wang Yingzi has applied for the compounded pesticides of Osthole and matrine and the patent of application thereof, publication number is CN101589716, in complex composition, the weight ratio of Osthole and two kinds of compositions of matrine is 4:1~1:4, preferred proportion is 1:1~1:4, optimal proportion is 1:2, after Osthole and matrine compound, is applied to prevent and treat the grape green plant bug.Xu Qiyun etc. have applied for a kind of patent of matrine composition, publication number is CN101647459, take matrine and anabasine insecticide as main, form with auxiliary agent and excipients, be mixed with microemulsion, aqueous emulsion, suspending agent, water dispersible granules, wetting powder, missible oil.Wherein the mass percent of matrine and anabasine insecticide is 30:1-1:100, can be used for preventing and treating rice fulgorid, trialeurodes vaporariorum, aphid, paddy stem borer, striped rice borer, thrips, Lissorhoptrus oryzophilus Kuschel, rice gall midge.Xu Qiyun etc. have applied for a kind of Pesticidal combination of capillary and matrine and patent of application thereof of containing, publication number is CN101884339A, take capillary and matrine insecticide as main, with auxiliary agent and excipient, form, be mixed with microemulsion, aqueous emulsion, suspending agent, water dispersible granules, wetting powder, missible oil.Wherein the mass percent of capillary and matrine insecticide is 300:1-10:1, is preferably 49:1-29:1, can be used for preventing and treating diamond-back moth, prodenia litura, phyllotreta striolata, rice fulgorid, trialeurodes vaporariorum, aphid, thrips, rice gall midge and phytophagy tetranychid.Hu Qiongbo etc. have applied for the patent of destruxins and matrine compound desinsection host and insecticide, publication number is CN101773129A, described compounded pesticides comprises host and assistant agent, and the weight percentage of host and assistant agent is respectively 1%~30% and 70%~99%.Described compound insecticidal host is the mixture prepared according to the part by weight of 1:0.25~50 by destruxins and matrine.Described destruxins is pure substance or the mixture that contains destruxins A, B, C, D, E, and described matrine is pure substance or the mixture that contains Banlangen.Hu Zhiquan etc. have applied for the patent of a kind of nicotine matrine agent plant pesticide and preparation method thereof, publication number is CN101926372A, by comprising what following raw material made: 5~10 parts of vomiting nuts, 10~15 parts of monkshoods, 3~6 parts of rhizoma arisaematis, 2~5 parts of the roots of langdu, 5~10 parts of monkshoods, 5~15 parts of Chinese blister beetles, 6~10 parts of YEYUTOUs, give birth to 5~10 parts of the tuber of pinellia, 5~10 parts of wartwort, 5~10 parts of crotons, 5~10 parts of the roots of Beijing euphorbia, 5~10 parts of azedaraches, 3~6 parts of Rhododendron molles, 5~10 parts of Java brucea, 5~10 parts of stone-like omphalias, 5~10 parts of kongpo monkshood roots, 5~10 parts of peach leaves, the nicotine of 5~10 parts of yellow Teng's roots and effective dose, Banlangen, count by weight.Ge Yaolun etc. have applied for a kind of patent that contains the Pesticidal combination of Nitenpyram and matrine, publication number is CN102302018A, its active ingredient is matrine and Nitenpyram, and the percentage by weight of two kinds of active ingredients is 0.01-15:80-1, and preferred weight percent is 5~0.1:5~50; In Pesticidal combination, the total quality percentage composition of active ingredient is 1%~90%, be preferably 5%~50%, all the other are in agricultural chemicals, to allow to use and the acceptable auxiliary element, can be prepared into aqua, missible oil, suspending agent, soluble concentrate, wetting powder, water dispersible granules by known method.
Making a general survey of above-mentioned patent documentation, is mostly to be mixed with matrine or sanguinarine and plant extracts or agricultural chemicals, and patent documentation and product that matrine and Macleaya cordata alkaloids are mixed are had no to open report so far.
Summary of the invention
The object of the invention is to, provide a kind of and take botanical components matrine and Macleaya cordata alkaloids and be the preparation method of insecticide active substance and synergism compound preparation thereof, be mainly used in the control melon, really, the pest such as the aphid on vegetables, two spotted spider mite, fragrant-flowered garlic maggot, Paratrioza sinica, pear sucker, cabbage caterpillar, diamond-back moth, mythimna separata.
In order to realize above-mentioned task, the present invention takes following technical solution to be achieved:
A kind of plant resource compound synergic insecticide that contains matrine and Macleaya cordata alkaloids, it is characterized in that, this plant resource synergistic complex insecticide made is main component by matrine and Macleaya cordata alkaloids and adds additive compound to form, and the preparation form is environment-friendly type missible oil, microemulsion or aqueous emulsion; Wherein:
Described environment-friendly type missible oil is prepared by following raw materials by weight:
Matrine: 0.1~20%, Macleaya cordata alkaloids: 0.1~20%, emulsifier: 5~15%, synergist: 0~20%, surplus is organic solvent, the percentage by weight sum of raw material is 100%;
Described aqua is prepared by following raw materials by weight:
Matrine: 0.1~20%, Macleaya cordata alkaloids: 0.1~20%, organic solvent: 0~20%, surfactant: 5~20%, synergist: 0~20%, antifreezing agent: 0~10%, surplus is water, the percentage by weight sum of raw material is 100%.
Described soluble liquid is prepared by following raw materials by weight:
Matrine: 0.1~20%, Macleaya cordata alkaloids: 0.1~20%, surfactant: 5~20%, synergist: 0~20%, surplus is organic solvent, the percentage by weight sum of raw material is 100%.
Described organic solvent is one or more the mixture in ethyl acetate, cyclohexanone, methyl oleate, ethanol, methyl alcohol, acetone, dimethyl formamide;
Described emulsifier is one or more the mixture in alkyl benzene sulfonate, alkylphenol polyoxyethylene class, phenethyl phenol polyethenoxy ethers, phenethyl phenol polyethenoxy ether polyoxypropylene ethers, this Pan's series, tween;
Described surfactant is one or more mixture in the addition product, aralkyl phenol polyethenoxy ether formaldehyde condensation products of alkyl benzene sulfonate, alkylphenol polyoxyethylene class, phenethyl phenol polyethenoxy ethers, phenethyl phenol polyethenoxy ether polyoxypropylene ethers, castor oil and oxirane;
Described synergist is one or more the mixture in organosilicon, Butacide, Octacide 264, alkyl carbonate, azone;
Described antifreezing agent is ethylene glycol or propane diols.
The above-mentioned plant resource compound synergic method for producing insecticide that contains matrine and Macleaya cordata alkaloids is characterized in that the preparation form made is environment-friendly type missible oil, aqua or soluble liquid; Wherein:
The preparation method of environment-friendly type missible oil is: according to formula ratio, matrine, Macleaya cordata alkaloids, emulsifier, organic solvent, synergist are mixed, stir in reactor, get product through quality inspection;
The preparation method of aqua is: according to formula ratio, matrine, Macleaya cordata alkaloids, organic solvent, surfactant, synergist, antifreezing agent and water are mixed, in reactor, stir transparently, after quality inspection, make finished product;
The preparation method of soluble liquid is: according to formula ratio, matrine, Macleaya cordata alkaloids, surfactant, synergist and organic solvent are mixed, in reactor, stir transparently, after quality inspection, make finished product.
The plant resource compound synergic insecticide that contains matrine and Macleaya cordata alkaloids of the present invention is a kind of novel insecticide, can prevent and treat melon, really, the pest such as the aphid on vegetables, flowers, two spotted spider mite, fragrant-flowered garlic maggot, Paratrioza sinica, pear sucker, cabbage caterpillar, diamond-back moth, mythimna separata, has higher control efficiency, in organic farm products production, having very big application and popularization value, is desirable novel non-pollution insecticide.
Advantage of the present invention is as follows:
1. matrine and Macleaya cordata alkaloids are natural active matter, easily degraded in environment, and to mammal low toxicities such as people and animals, to pest natural enemy and other beneficial organism safety, and insect is difficult for developing immunity to drugs to it.
2. the formulation adopted is mainly environment-friendly type missible oil, aqua, soluble liquid etc., without aromatic hydrocarbon solvents such as dimethylbenzene, greatly reduces the destruction to environment, has reduced in the dispenser process murder by poisoning to operator.
3. photostability improves, the lasting period is suitable, can reduce dispenser frequency and cost accounting, and be conducive to further alleviate the pressure to environment.
4, various to the insect mode of action, to the Main Agricultural insects such as aphid, two spotted spider mite, Paratrioza sinica, pear sucker have stomach toxicity, avoid keep away, isoreactivity is grown in food refusal, inhibition, and mostly be slow and regulate effect of growth and development, meet sustainable pest management and administer strategy.
5. aphid, two spotted spider mite, fragrant-flowered garlic maggot, Paratrioza sinica, pear sucker, cabbage caterpillar, diamond-back moth, mythimna separata are had to food refusal, cytotoxicity and control efficiency, can obtain larger economy, society and ecological benefits.
Embodiment
The applicant is through studying matrine and Macleaya cordata alkaloids, determine that both are after rationally composite, the environment-friendly type missible oil, aqua or the soluble liquid that by adding auxiliary agent, are processed into, for preventing and treating various agricultural insect, evil mite, especially for aphid, two spotted spider mite, fragrant-flowered garlic maggot, Paratrioza sinica, pear sucker, cabbage caterpillar etc., has good control efficiency.
The plant resource compound synergic insecticide that contains matrine and Macleaya cordata alkaloids of the present invention, take matrine and Macleaya cordata alkaloids is active component, add a certain proportion of solvent and cosolvent and other insecticides adjuvant, carry out formulation, can make environment-friendly type missible oil, aqua or soluble liquid.Wherein, matrine consumption by weight percentage 0.1~20%, Macleaya cordata alkaloids consumption by weight percentage 0.1~20%, all the other are auxiliary agents.
Evidence through the inventor, in the plant resource compound synergic insecticide that contains matrine and Macleaya cordata alkaloids of the present invention, matrine and Macleaya cordata alkaloids part by weight are between 2:1~1:5 to be suitable, be mainly used in the control melon, really, the pest such as the aphid on vegetables, flowers, two spotted spider mite, fragrant-flowered garlic maggot, pear sucker, cabbage caterpillar, diamond-back moth, mythimna separata.
1. environment-friendly type missible oil: matrine consumption by weight 0.1~20%, Macleaya cordata alkaloids consumption by weight 0.1~20%, all the other are auxiliary agents, auxiliary agent comprises: emulsifier, organic solvent, synergist.
Emulsifier: 5~15%, be one or more the mixture in alkyl benzene sulfonate, alkylphenol polyoxyethylene class, phenethyl phenol polyethenoxy ethers, phenethyl phenol polyethenoxy ether polyoxypropylene ethers and similar substance thereof, this Pan series, tween;
Synergist: 0~20%, be one or more the mixture in organosilicon, Butacide, Octacide 264, alkyl carbonate, azone;
Surplus is together to 100% of organic solvent: be one or more the mixture in ethyl acetate, acetone, ethanol.
2. aqua: matrine content by weight 0.1~20%, Macleaya cordata alkaloids 0.1~20%; All the other are auxiliary agents, and auxiliary agent comprises: surfactant, organic solvent, synergist, antifreezing agent and water.
Surfactant: 5~20%, be one or more mixture in the addition product of alkyl phosphate class, alkylphenol polyoxyethylene phosphoric acid ester, aralkyl phenol polyethenoxy ether phosphoric acid ester, aliphatic acid polyethenoxy ether class, phenethyl phenol polyethenoxy ethers, phenethyl phenol polyethenoxy ether polyoxypropylene ethers and analog, castor oil and oxirane, aralkyl phenol polyethenoxy ether formaldehyde condensation products;
Organic solvent: 0~20%, be one or more mixture in methyl alcohol, cyclohexanone, dimethyl formamide, dimethyl sulfoxide (DMSO), ethyl acetate, acetone, ethanol;
Synergist: 0~20%, be one or more the mixture in organosilicon, Butacide, Octacide 264, alkyl carbonate, azone;
Antifreezing agent: 0~10%, be any of ethylene glycol or propane diols;
Surplus water polishing to 100%.
3. soluble liquid: matrine content by weight 0.1~20%, Macleaya cordata alkaloids 0.1~20%; All the other are auxiliary agents, and auxiliary agent comprises: surfactant, organic solvent, synergist and organic solvent.
Surfactant: 5~20%, be one or more mixture in the addition product of alkyl phosphate class, alkylphenol polyoxyethylene phosphoric acid ester, aralkyl phenol polyethenoxy ether phosphoric acid ester, aliphatic acid polyethenoxy ether class, phenethyl phenol polyethenoxy ethers, phenethyl phenol polyethenoxy ether polyoxypropylene ethers and analog, castor oil and oxirane, aralkyl phenol polyethenoxy ether formaldehyde condensation products;
Synergist: 0~20%, be one or more the mixture in organosilicon, Butacide, Octacide 264, alkyl carbonate, azone;
Organic solvent: be one or more mixture polishing to 100% in methyl alcohol, cyclohexanone, dimethyl formamide, dimethyl sulfoxide (DMSO), ethyl acetate, acetone, ethanol;
The above-mentioned production method that contains the plant resource compound synergic insecticide of matrine and Macleaya cordata alkaloids is:
1) environment-friendly type missible oil: raw material, by formula weighing medicament, is added successively to mixing, and stirs in reactor, after quality inspection, finally make finished product.
2) aqua: raw material, by the formula weighing, is added to mixing successively, stir transparently in reactor, after quality inspection, finally make finished product.
3) soluble liquid: raw material, by the formula weighing, is added to mixing successively, stir transparently in reactor, after quality inspection, finally make finished product.
In order better to understand essence of an invention, below with embodiment, describe the technology contents of invention in detail, but the content of invention is not limited to these embodiment.
EXPERIMENTAL EXAMPLE:
1, matrine and Macleaya cordata alkaloids are composite to the indoor co-toxicity research of flowering plant aphid
1.1 materials and methods
1.1.1 examination worm
Flowering plant aphid is mainly that cotten aphid Aphis gossypii is indoor for many generations to raise with the flowers seedling, laboratory picking aphid of the same size.
1.1.2 reagent agent
A.3.0% matrine mother liquor; B.20.0% Macleaya cordata alkaloids mother liquor; Biochemical Co., Ltd provides by Shanxi moral prestige.
1.2 assay method
The method that adopts NY/T1154.7-2006 to recommend, two-sided tape is cut into to the long segment of 3cm and is attached to slide one end, then with tweezers, tear the scraps of paper on viscose glue off, choose basically identical, the healthy aphid of Individual Size, with little writing brush, provoke, be attached to its back on viscose glue and its feeler and foot are not stuck, sticky 30 of every slide.First in the moisturizing condition, transfer 4h, check with bitubular anatomical lens, the aphid of checkmating is chosen and discards, then mends sticky.The slide that then will be stained with aphid soaks and into the liquidly shakes gently, through 5 seconds take out with blotting paper, suck the viscose glue surface and around liquid, every processing repeats for 4 times, 30 of every repetitions, and establish the corresponding organic solvent that does not contain medicament and process in contrast.
1.3 co-toxicity evaluation
Give birth to the survey method the same.By the SunShi method, obtain the co-toxicity coefficient (CTC value) of various complex preparations, and with the CTC value, pass judgment on the synergistic effect of mixture.This patent is thought: as CTC > be synergistic effect 120 the time, CTC<80 o'clock are antagonism, 80<CTC<120 are summation action, CTC > remarkable synergistic effect 200 o'clock arranged.
1.4 results and analysis
The method that adopts NY/T1154.7-2006 to recommend has been measured matrine and Macleaya cordata alkaloids to the indoor virulence of flowering plant aphid, the results are shown in Table 1.
Table 1 matrine, Macleaya cordata alkaloids and mixture thereof the virulence to flowering plant aphid
As can be seen from Table 1, matrine and Macleaya cordata alkaloids and mixture thereof are to flowering plant aphid LC
50Be respectively 7.60mg/L, 19.92mg/L, 13.93mg/L, 12.68mg/L, 10.17mg/L, 11.92mg/L and 10.07mg/L, wherein to be mixed to the flowering plant aphid co-toxicity coefficient at 1: 3 be 139.34 for matrine and Macleaya cordata alkaloids, be greater than 120, has obvious synergistic effect, all the other proportionings are mixed the flowering plant aphid co-toxicity coefficient are respectively to 112.60,118.62,108.39 and 109.24, all be less than matrine and Macleaya cordata alkaloids and be mixed at 1: 3 to the flowering plant aphid co-toxicity coefficient.This shows that matrine and Macleaya cordata alkaloids are mixed flowering plant aphid is had to certain synergistic effect at 1: 3.
2, matrine and Macleaya cordata alkaloids are measured the synergy of Radix Folium Allii tuberosi maggot indoor virulence
2.1 materials and methods
2.1.1 examination worm
Fragrant-flowered garlic maggot (Bradysia odoriphaga Yan et Zhang) is indoor to be raised with the leek seedling, laboratory picking 5 day old larva of the same size.
2.1.2 reagent agent
A.3.0% matrine mother liquor; B.20.0% Macleaya cordata alkaloids mother liquor; Biochemical Co., Ltd provides by Shanxi moral prestige.
2.2 assay method
Adopt medicine embrane method.During mensuration, get the 1ml liquid in dactylethrae, rotate dactylethrae and make liquid evenly coat inside pipe wall, often in vitro connect 10 left and right of leek root maggot larva after the acetone volatilization, be placed in insectary and raise, every processing repeats for 4 times, 30 of every repetitions.
2.3 results and analysis
Adopt medicine embrane method to measure matrine and Macleaya cordata alkaloids to the indoor virulence of leek root maggot, the results are shown in Table 2.
Table 2 matrine, Macleaya cordata alkaloids and mixture thereof the virulence to the leek root maggot
As can be seen from Table 2, matrine and Macleaya cordata alkaloids and mixture thereof are to leek root maggot LC
50Be respectively 84.78mg/L, 60.01mg/L, 57.45mg/L, 71.23mg/L, 51.37mg/L, 54.30mg/L and 59.16mg/L, wherein to be mixed to leek root maggot co-toxicity coefficient be 125.50 for matrine and Macleaya cordata alkaloids 1:3, be greater than 120, has obvious synergistic effect, all the other proportionings are mixed leek root maggot co-toxicity coefficient are respectively to 109.80,93.01,121.80 and 117.70, all be less than matrine and Macleaya cordata alkaloids and be mixed at 1: 3 to leek root maggot co-toxicity coefficient.This shows that matrine and Macleaya cordata alkaloids are mixed the leek root maggot is had to certain synergistic effect at 1: 3.
3, matrine and Macleaya cordata alkaloids are measured the synergy of Paratrioza sinica indoor virulence
3.1 materials and methods
3.1.1 examination worm
Paratrioza sinica Paratrioza sinica picks up from field, laboratory picking examination of the same size worm.
3.1.2 reagent agent
A.3.0% matrine mother liquor; B.20.0% Macleaya cordata alkaloids mother liquor; Biochemical Co., Ltd provides by Shanxi moral prestige.
3.2 assay method
The method that adopts NY/T1154.7-2006 to recommend, two-sided tape is cut into to the long segment of 3cm and is attached to slide one end, then with tweezers, tear the scraps of paper on viscose glue off, choose basically identical, the healthy examination worm of Individual Size, with little writing brush, provoke, be attached to its back on viscose glue and its feeler and foot are not stuck, sticky 30 of every slide.First in the moisturizing condition, transfer 4h, check with bitubular anatomical lens, the examination worm of checkmating is chosen and discards, then mends sticky.The slide that then will be stained with the examination worm soaks and into the liquidly shakes gently, through 5 seconds take out with blotting paper, suck the viscose glue surface and around liquid, every processing repeats for 4 times, 30 of every repetitions, and establish the corresponding organic solvent that does not contain medicament and process in contrast.
3.3 results and analysis
The method that adopts NY/T1154.7-2006 to recommend has been measured matrine and Macleaya cordata alkaloids to the indoor virulence of Paratrioza sinica, the results are shown in Table 3.
Table 3 matrine, Macleaya cordata alkaloids and mixture thereof the virulence to Paratrioza sinica
As can be seen from Table 3, matrine and Macleaya cordata alkaloids and mixture thereof are to Paratrioza sinica LC
50Be respectively 11.46mg/L, 52.81mg/L, 26.37mg/L, 20.11mg/L, 15.51mg/L, 20.08mg/L and 12.99mg/L, wherein to be mixed to the Paratrioza sinica co-toxicity coefficient at 1: 3 be 137.79 for matrine and Macleaya cordata alkaloids, be greater than 120, has obvious synergistic effect, all the other proportionings are mixed the Paratrioza sinica co-toxicity coefficient are respectively to 112.07,112.76,97.08 and 127.58, all be less than matrine and Macleaya cordata alkaloids and be mixed at 1: 3 to the Paratrioza sinica co-toxicity coefficient.This shows that matrine and Macleaya cordata alkaloids are mixed Paratrioza sinica is had to certain synergistic effect at 1: 3.
The preparation of Preparation Example 1:30% matrine Macleaya cordata alkaloids environment-friendly type missible oil
Under 20~25 ℃, get 30 parts of matrine Macleaya cordata alkaloids (the composite ratio of matrine and Macleaya cordata alkaloids is 1:3), on the said mixture basis, add successively 10 parts of organosilicons, 7 parts of neopelexes and 1 part of OPEO and 2 parts of phenethyl phenol polyethenoxy polyethenoxy ethers, with ethanol+ethyl acetate+dimethyl formamide (6:3.5:0.5), complement to 100 parts, with 800~1000 rev/mins of mixing speeds, stirred 10~30 minutes, can make 30% matrine Macleaya cordata alkaloids environment-friendly type missible oil.
The preparation of Preparation Example 2:20% matrine Macleaya cordata alkaloids environment-friendly type missible oil
Under 20~25 ℃, get 20 parts of matrine Macleaya cordata alkaloids (the composite ratio of matrine and Macleaya cordata alkaloids is 1:3), on the said mixture basis, add successively 8 parts of organosilicons, 5 parts of neopelexes and 1 part of OPEO and 2 parts of phenethyl phenol polyethenoxy polyethenoxy ethers, with ethanol+ethyl acetate+dimethyl formamide (7:2.8:0.2), complement to 100 parts, with 800~1000 rev/mins of mixing speeds, stirred 10~30 minutes, can make 20% matrine Macleaya cordata alkaloids environment-friendly type missible oil.
The preparation of Preparation Example 3:10% matrine Macleaya cordata alkaloids environment-friendly type missible oil
Under 20~25 ℃, get 10 parts of matrine Macleaya cordata alkaloids (the composite ratio of matrine and Macleaya cordata alkaloids is 1:3), on the said mixture basis, add successively 6 parts of organosilicons, 4 parts of neopelexes and 1 part of OPEO and 1 part of phenethyl phenol polyethenoxy polyethenoxy ether, with ethanol+ethyl acetate+dimethyl formamide (6:3.5:0.5), complement to 100 parts, with 800~1000 rev/mins of mixing speeds, stirred 10~30 minutes, can make 10% matrine Macleaya cordata alkaloids environment-friendly type missible oil.
The preparation of Preparation Example 4:20% matrine Macleaya cordata alkaloids aqua
Under 20~25 ℃, get 20 parts of matrine Macleaya cordata alkaloids (the composite ratio of matrine and Macleaya cordata alkaloids is 1:3), in said mixture, add successively 1 part of organosilicon, 7 parts of polyoxyethylene nonylphenol ether, 4 parts of polyoxyethylene nonylphenol ether phosphates, 5 parts of glycerine, mix rear solution polishing to 100 part, with 100~200 rev/mins of mixing speeds, stirred 10~30 minutes, can make 20% matrine Macleaya cordata alkaloids aqua.
The preparation of Preparation Example 5:10% matrine Macleaya cordata alkaloids aqua
Under 20~25 ℃, get 10 parts of matrine Macleaya cordata alkaloids (the composite ratio of matrine and Macleaya cordata alkaloids is 1:3), in said mixture, add successively 1 part of organosilicon, 5 parts of polyoxyethylene nonylphenol ether, 3 parts of polyoxyethylene nonylphenol ether phosphates, 4 parts of glycerine, mix rear solution polishing to 100 part, with 100~200 rev/mins of mixing speeds, stirred 10~30 minutes,, can make 10% matrine Macleaya cordata alkaloids aqua.
The preparation of Preparation Example 6:5% matrine Macleaya cordata alkaloids aqua
Under 20~25 ℃, get 5 parts of matrine Macleaya cordata alkaloids (the composite ratio of matrine and Macleaya cordata alkaloids is 1:3), in said mixture, add successively 1 part of organosilicon, 3 parts of polyoxyethylene nonylphenol ether, 1 part of polyoxyethylene nonylphenol ether phosphate, 2 parts of glycerine, mix rear solution polishing to 100 part, with 100~200 rev/mins of mixing speeds, stirred 10~30 minutes,, can make 5% matrine Macleaya cordata alkaloids aqua.
The preparation of Preparation Example 7:20% matrine Macleaya cordata alkaloids soluble liquid
Under 20~25 ℃, get 20 parts of matrine Macleaya cordata alkaloids (the composite ratio of matrine and Macleaya cordata alkaloids is 1:3), in said mixture, add successively 7 parts of polyoxyethylene nonylphenol ether, 4 parts of polyoxyethylene nonylphenol ether phosphates, 5 parts of organic solvent polishings to 100 part of glycerine, after mixing, stirred 10~30 minutes with 100~200 rev/mins of mixing speeds, can make 20% matrine Macleaya cordata alkaloids soluble liquid.
The preparation of Preparation Example 8:10% matrine Macleaya cordata alkaloids soluble liquid
Under 20~25 ℃, get 10 parts of matrine Macleaya cordata alkaloids (the composite ratio of matrine and Macleaya cordata alkaloids is 1:3), in said mixture, add successively 5 parts of polyoxyethylene nonylphenol ether, 3 parts of polyoxyethylene nonylphenol ether phosphates, 4 parts of organic solvent polishings to 100 part of glycerine, after mixing, stirred 10~30 minutes with 100~200 rev/mins of mixing speeds, can make 15% matrine Macleaya cordata alkaloids soluble liquid.
The preparation of Preparation Example 9:5% matrine Macleaya cordata alkaloids soluble liquid
Under 20~25 ℃, get 5 parts of matrine Macleaya cordata alkaloids (the composite ratio of matrine and Macleaya cordata alkaloids is 1:3), in said mixture, add successively 3 parts of polyoxyethylene nonylphenol ether, 1 part of polyoxyethylene nonylphenol ether phosphate, 2 parts of organic solvent polishings to 100 part of glycerine, after mixing, stirred 10~30 minutes with 100~200 rev/mins of mixing speeds, can make 5% matrine Macleaya cordata alkaloids soluble liquid.
The field control effectiveness test of 1: nine Plants source synergistic complex insecticide of checking embodiment to two spotted spider mite
The field efficacy situation of the nine Plants source synergistic complex insecticides that prepare for clear and definite embodiment, the applicant carried out the drug effect test of field zone of control citrus red mite to this medicament at Shaanxi Province's Hanzhong City in 2011.
1, reagent agent
20% matrine Macleaya cordata alkaloids soluble liquid, medicament code name KXK1;
10% matrine Macleaya cordata alkaloids soluble liquid, medicament code name KXK2;
5% matrine Macleaya cordata alkaloids soluble liquid, medicament code name KXK3;
20% matrine Macleaya cordata alkaloids aqua, medicament code name KXS1;
10% matrine Macleaya cordata alkaloids aqua, medicament code name KXS2;
5% matrine Macleaya cordata alkaloids aqua, medicament code name KXS3;
30% matrine Macleaya cordata alkaloids environment-friendly type missible oil, medicament code name KXR1;
20% matrine Macleaya cordata alkaloids environment-friendly type missible oil, medicament code name KXR2;
10% matrine Macleaya cordata alkaloids environment-friendly type missible oil, medicament code name KXR3;
20% pyridaben wetting powder, Shanxi Hengtian Chemical Industry Co., Ltd..
2, test article
3 of syringes (10ml), two of knapsack sprayers, drop (300), 1 of Enamel jar (1000ml), 3 of pencils, 1 of minute book, pulling needle is some, and one one, camera.
3, for studying thing
Oranges and tangerines.
4, experimental scheme and method
Small plot experiment is randomized arrangement, repeats 3 Ci, community areas depending on actual conditions.By 500,1000,1500 times of liquid measures of reagent agent, carry out the blade face conventional spray, 20% 2500 times of pyridabens liquid carries out the blade face conventional spray for the contrast medicament, and establishes the clear water contrast.Investigation complete stool worm amount.Investigation insect population radix before medicine, investigation in 1,3,7 day borer population alive after medicine.By worm amount before and after each chemicals treatment dispenser, calculate the insect population decline rate, district compares with blank, calculates the control efficiency of each chemicals treatment, and carries out significance test by " DMRT " method.Calculate the insect population decline rate and proofread and correct preventive effect, computing formula is as follows:
In formula, Ta: insect population number after chemicals treatment, Tb: insect population number before chemicals treatment, Ca: insect population number after control treatment, Cb: insect population number before control treatment.
5, result of the test and statistics
Adopt conventional spray-on process to matrine and 9 kinds of built agents of Macleaya cordata alkaloids alkali, the field efficacy of two spotted spider mite to be tested, the results are shown in Table 4.
Table 4: the field control effectiveness test result of nine Plants insecticides to two spotted spider mite
Annotate: 1. in the table, data are the mean value of 3 repetitions; 2. in " preventive effect " hurdle, after ordered series of numbers, the identical lowercase person of mark is illustrated in variance analysis (DMRT method), on 5% level without significant difference.Table 6 is same.
As can be seen from the above table, under 500 times of 9 medicine based on herbs, after 1 day, preventive effect is all more than 75%, and after 3 days, pharmacy control efficacy rises to more than 85%, and after 7 days, KXS-1, KXS-2, KXR-1, KXK-1 reach respectively 100%, 98.63%, 96.62% and 94.58%; Under 1000 times of processing, 3 days and 7 days preventive effects (except KXR-3, KXK-3 and KXS-3 preventive effect when the 3d is 79.36%, 75.21% and 74.87%) have also all reached more than 80%, and this may be that slow characteristic due to botanical components determines.Under 1500 times of concentration for the treatment of, during 7d, the preventive effect of nine kinds of medicaments is all more than 75%.In general, in 9 medicine based on herbs, take the control efficiency of medicament KXS-1, KXS-2, KXR-1 and KXK-1 than other medicaments as good.
2: nine Plants source synergistic complex insecticide control apple yellow aphid field control effectiveness tests of checking embodiment
The method that the applicant investigated the evidence of a case to demonstrate,prove embodiment 1 in 2011 at Shaanxi plain boiled water is prevented and treated above-mentioned nine kinds of reagent agents the drug effect test of field zone of apple yellow aphid, and the contrast medicament is 20% Imidacloprid missible oil, test of pesticide effectiveness result such as table 5:
Table 5: the field control effectiveness test result of nine Plants insecticides to apple yellow aphid
As can be seen from the above table, under 500 times of 9 medicine based on herbs, after 1 day, preventive effect is all more than 75%, and after 3 days, pharmacy control efficacy rises to more than 85%, and after 7 days, KXS-1, KXS-2, KXK-1, KXR-1 reach respectively 95.99%, 92.67%, 96.74% and 97.90%; Under 1000 times of processing, preventive effect in the time of 3 days of 9 medicaments (except the preventive effect of KXK-3 and KXS-3 is respectively 71.35% and 72.19%) is all more than 76%, and the preventive effect in the time of 7 days is all more than 82%, the slow characteristic of botanical components performance more obvious.In general, in 9 medicine based on herbs, take the control efficiency of medicament KXS-1, KXS-2, KXK-1, KXR-1 than other medicaments as good.
3: nine Plants source synergistic complex insecticide control Paratrioza sinica field control effectiveness tests of checking embodiment
The applicant has carried out the drug effect test of field zone of nine Plants source synergistic complex insecticide control Paratrioza sinicas at Yinchuan of Ningxia Province in 2011.
1, reagent agent
20% matrine Macleaya cordata alkaloids soluble liquid, medicament code name KXK1;
10% matrine Macleaya cordata alkaloids soluble liquid, medicament code name KXK2;
5% matrine Macleaya cordata alkaloids soluble liquid, medicament code name KXK3;
20% matrine Macleaya cordata alkaloids aqua, medicament code name KXS1;
10% matrine Macleaya cordata alkaloids aqua, medicament code name KXS2;
5% matrine Macleaya cordata alkaloids aqua, medicament code name KXS3;
30% matrine Macleaya cordata alkaloids environment-friendly type missible oil, medicament code name KXR1;
20% matrine Macleaya cordata alkaloids environment-friendly type missible oil, medicament code name KXR2;
10% matrine Macleaya cordata alkaloids environment-friendly type missible oil, medicament code name KXR3;
4.5% efficient cyhalothrin emulsifiable concentrate, Jiangsu Yangnong Chemical Group Co., Ltd.
2, test article
3 of syringes (10ml), two of knapsack sprayers, drop (300), 1 of Enamel jar (1000ml), 3 of pencils, 1 of minute book, pulling needle is some, and one one, camera.
3, for studying thing
Matrimony vine
4, experimental scheme and method
The cultivation condition of testing all communities comprises that land type, cultivation management, matrimony vine kind and upgrowth situation etc. are all consistent.At a time when test, Paratrioza sinica 2-3 contains the phase in age, carries out the blade face conventional spray by 500,1000,1500 times of liquid measures of reagent agent, and 4.5% 3000 times of efficient cyhalothrin emulsifiable concentrates liquid carries out the blade face conventional spray for the contrast medicament, and establishes the clear water contrast.3 repetitions, every repetition area 20m are established in test
2, randomized arrangement.5 orientation of every strain investigation, each orientation adopts five point samplings, and 5 blades of random searching, record and calculate every 100 blade ovum amounts, respectively at 3d, 7d, 10d before the spray medicine and after the spray medicine, investigate, and the statistics ovum number of living, calculate control efficiency.Computing formula is with checking embodiment 1.Test of pesticide effectiveness result is as shown in table 6:
The field control effectiveness test result of table 6 nine Plants insecticides to Paratrioza sinica
As can be seen from the above table, under 500 times of 9 medicine based on herbs, after 1 day, preventive effect is all more than 70%, and after 3 days, pharmacy control efficacy rises to more than 85%, and after 7 days, KXS-1, KXS-2, KXK-1, KXR-1 reach respectively 93.49%, 92.54%, 92.71% and 95.13%; Under 1000 times of processing, the preventive effect of 9 medicaments in the time of 3 days is all more than 76%, and the preventive effect in the time of 7 days is all more than 82%, and it is more obvious that the slow characteristic of botanical components shows.In general, in 9 medicine based on herbs, take the control efficiency of medicament KXS-1, KXS-2, KXK-1, KXR-1 than other medicaments as good.
The field experiment result of comprehensive above three tables, nine Plants insecticides, in field trial, have all shown slow, and quick-acting is not as chemical agent.Analyze reason, this may be that the essence of effect is just because of the result of Multiple components interaction by the constituent decision of active substance of plant complexity.In addition, plant insecticide has certain lasting period (7~9 days), and to non-target organism and environmental friendliness, therefore very applicable in economic crops and Organic Food Development, have very large application and popularization value.