CN100569077C - A kind of mixed pesticide of radix euphorbiae lantu chromocor and preparation method thereof - Google Patents
A kind of mixed pesticide of radix euphorbiae lantu chromocor and preparation method thereof Download PDFInfo
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- CN100569077C CN100569077C CNB2007100483191A CN200710048319A CN100569077C CN 100569077 C CN100569077 C CN 100569077C CN B2007100483191 A CNB2007100483191 A CN B2007100483191A CN 200710048319 A CN200710048319 A CN 200710048319A CN 100569077 C CN100569077 C CN 100569077C
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Abstract
The invention provides plant resource mixed pesticide of radix euphorbiae lantu chromocor that a kind of drug effect is good, quick-acting good, the longevity of residure is long, synergy is remarkable, cost is lower, be convenient to promote the use of and preparation method thereof.Being characterized in extracting from the poisonous plant root of langdu root of langdu flavones with insecticidal effect, is main component with the nicotine that extracts in root of langdu flavones, the tobacco, carries out organic assembling through preferred insecticides adjuvant and is processed into.Root of langdu flavones and the nicotine remarkable synergistic function that has been mixed.
Description
One, technical field
The present invention relates to a kind of biopesticide or mixed insecticide that is mixed and makes with root of langdu flavones and nicotine, belong to the biological agricultural medicine of plant resource field.
Two, background technology
Use in a large number owing to height poisons the medicine of learning to farm in China, produced serious social ecological problem, the acute poisoning incident of vegetables, fruit chemical pesticide happens occasionally, agricultural byproducts outlets also has the residual toxicity phenomenon that exceeds standard, and the chronic poisoning that the chemical pesticide contaminated environment may cause especially cancer rate occurred frequently is troubling, other is as chemical pesticide kill pests natural enemy, and the destruction ecological balance etc. presses for the problem of solution especially.The development public nuisance-free agricultural chemicals; preserve the ecological environment. produce pollution-free food; become the problem of people's growing interest, country " 21 centurys 1,600,000,000 population food security " as important realization target, public nuisance-free agricultural chemicals will replace height greatly and poison the medicine of learning to farm to estimate the beginning of next century.
China is research and uses pesticide plant country the earliest.Just once mentioning plants such as the tuber of stemona, black false hellebore, the root of langdu, kuh-seng has insecticidal properties in 1892 kinds of medicines that the Compendium of Material Medica that the Ming Dynasty 24 years Wanli year (1596) Li Shizhen (1518-1593 A.D.) is write is narrated.For many years, the Chinese research personnel study the active component of more than 10 kind of pesticide plants such as tobacco, trifoliate jewelvine, thick fruit chicken, blood rattan, crotons, melia toosendan, China tree and Celastrus angulatus, and develop some plant species source pesticides.
Consult pertinent literature and analysis more as can be known, at present, utilizing Chinese Stellera Root as the existing report of the research of biopesticide.As, Chinese patent 00116146.6 disclosed " preparation method of biological broad spectrum insecticide ", this technology principal character is to be that raw material is produced biological broad spectrum insecticide with Eupatorium adenophorum and Chinese Stellera Root, trifoliate jewelvine; Chinese patent ZL02133971.6 disclosed " euphorbia-one pesticide and preparation method thereof ", be characterized in from Chinese Stellera Root separating, extract have insecticidal effect low polarity to nonpolar root of langdu ketone, be that main component is processed into root of langdu ketone.Root of langdu flavonoids is the composition that has remarkable insecticidal activity in the root of langdu.Root of langdu extract has good insecticidal effect as agricultural chemicals, but its effect is comparatively slow, and often effect is unsatisfactory under low amount of application condition.Nicotine is a kind of alkaloid that extracts from tobacco, be a kind of never poison, to insect stomach toxicity arranged, tag, fumigate, interior suction and food refusal effect. it is good to have quick-acting, easily degraded in environment, characteristics such as insect is difficult for developing immunity to drugs. but because the nicotine high volatility, the field lasting period is short.The present invention utilizes the characteristics of the two action effect and the difference of the mechanism of action, and the development mixed pesticide of radix euphorbiae lantu chromocor so far, is not seen this series products on the market.
Three. technology contents
The object of the present invention is to provide plant resource mixed pesticide of radix euphorbiae lantu chromocor that a kind of drug effect is good, quick-acting good, the longevity of residure is long, synergy is remarkable, cost is lower, be convenient to promote the use of and preparation method thereof.Remedy single plant extracts as insecticide deficiency in use to reach; Urge the long weak point of mending mutually with being mixed of various plants extract, significantly improve control efficiency, reduce use cost.Being characterized in extracting from the poisonous plant root of langdu root of langdu flavones with insecticidal effect, is main component with the nicotine that extracts in root of langdu flavones, the tobacco, carries out organic assembling through preferred insecticides adjuvant and is processed into.Root of langdu flavones and the nicotine remarkable synergistic function that has been mixed.
Technical scheme of the present invention:
Mixed pesticide of radix euphorbiae lantu chromocor is made up of the composition of following weight ratio:
Root of langdu flavones 10 one 80%
Nicotine 0.1 one 65%
All the other are auxiliary agent.
Said preparation can be made into emulsifiable concentrate, aqua, aqueous emulsion, colloidal suspending agent, soluble powder and wetting powder.To make the cream preparation best results.
Preparation method of the present invention comprises the steps:
A. the extraction of root of langdu flavones: with Chinese Stellera Root clean, pulverize, with ethanol, methyl alcohol, propyl alcohol, acetone, n-hexane, benzinum and or chloroform at least a immersion, repeatedly extract, be concentrated into the root of langdu chromocor extract of flowing soaking paste, extracting temperature is 30-95 ℃, and the time is 4-24 hour.Root of langdu extract flavone Determination on content: with the rutin is standard items, utilize spectrophotometric method to root of langdu extractive total flavone content measure (reference: Wang Guangya chief editor. health food functional component detection method [M]. Beijing: the .2002.1082 of China Light Industry Press～1086.).
B. nicotine preparation: rhizome, leaf with tobacco are raw material, with organic solvent (organic solvent is: ethanol, methyl alcohol, butanols, propyl alcohol, acetone, benzinum and or chloroform at least a) refluxing extraction, filtration.It is standby that extract is evaporated to the liquid extract of setting concentration.In the tobacco extract assay of nicotine adopt the complexometric extraction spectrophotometric method carry out (reference: Wu Suxi etc., the nicotine in the complexometric extraction spectrophotometry tobacco extract, " tobacco science and technology " 2 phases in 2006,33-36).
C. mixed insecticide: (as preparation of B method or commercially available nicotine elaboration: nicotine content 50-98%): the content requirement of the root of langdu flavones of setting in prescription 10 one 80%, nicotine 0.1 one 65% is determined root of langdu extract, tobacco extract proportion of raw materials ratio and is mixed then to measure in the root of langdu extract content of nicotine in flavones, the tobacco extract earlier, mixed raw material drops in the reactor, add other auxiliary agent of setting by prescription, heated and stirred is even, promptly gets root of langdu flavones mixed emulsifiable solution.Wherein temperature of reaction kettle is 45 1 60 ℃, and mixing time is 30 1 60 minutes.
Root of langdu flavones mixed emulsifiable solution preparation of the present invention has kept existing root of langdu preparation to all characteristics that insect showed, but its quick-acting and insecticidal toxicity are significantly increased.Being mixed of root of langdu flavones and nicotine shows tangible coordination synergistic effect.
Mixed pesticide of radix euphorbiae lantu chromocor of the present invention is applicable to pest, is specially adapted to harmful insect, the control of pest mite.
The present invention has the following advantages and effect:
1, after root of langdu flavones and nicotine are mixed, both can overcome the slow shortcoming of root of langdu flavones insecticide effect, can keep the advantage of root of langdu flavones insecticide long action time again; Simultaneously, significantly improve the quick-acting and the insecticidal toxicity of mixed agent.
2, root of langdu flavones and nicotine all are botanical pesticides, and being mixed between them kept botanical pesticide low toxicity, efficient, easily degraded, noresidue, to insect be difficult for developing immunity to drugs, advantage free from environmental pollution.
3, being mixed of root of langdu flavones and nicotine can enlarge the prevention and treatment range to agricultural pest, and can make it to become one is insecticide, is again bactericidal agent, but also is the novel agrochemical formulations of antivirotic.
Four, embodiment
Further the present invention is elaborated below by non-limiting embodiment.Inventive embodiment:
The root of langdu flavones mixed emulsifiable solution agent preparation of embodiment 1.15%
Proportioning components (weight): 10% root of langdu flavones content, 5% nicotine content, surfactant 30%, stabilizing agent 10%, organic solvent 44.8%, pH value conditioning agent 0.2%.
A. the extraction of root of langdu flavones: with the Chinese Stellera Root root pulverize, the vicious root powder of preparation winter daphne 50kg, add 95% ethanol (or methyl alcohol, propyl alcohol, acetone) 80L, 85 ℃ of lixiviate 12h, solvent is reclaimed in the filter back, medicinal extract 5200g; Add absolute ethyl alcohol 5200mL dissolving, admix an amount of diatomite, volatilize ethanol, get 5h with the benzinum apple in apparatus,Soxhlet's, decompression and solvent recovery gets extract 2100g.Measure root of langdu flavones content.
B. producing of nicotine: rhizome, leaf with tobacco are raw material, use the organic solvent refluxing extraction, filter.It is standby that extract is evaporated to the liquid extract of setting concentration.Measure the content of nicotine in the preparation.
C. mixed insecticide: measure in the root of langdu extract content of nicotine in flavones, the tobacco extract earlier, the root of langdu flavones of setting by prescription, nicotine content requirement are determined root of langdu extract, tobacco extract proportion of raw materials ratio and are mixed then, mixed raw material drops in the reactor, add other auxiliary agent of setting by prescription, heated and stirred is even, promptly gets root of langdu flavones mixed emulsifiable solution.Wherein temperature of reaction kettle is 50 ℃, and mixing time is 40 minutes.
The root of langdu flavones mixed emulsifiable solution agent preparation of embodiment 2.25%
Proportioning components (weight): 20% root of langdu flavones content, 5% nicotine content, surfactant 25%, stablize 15%, organic solvent 34.8%, pH value conditioning agent 0.2%.
A. the extraction of root of langdu flavones: with the Chinese Stellera Root root pulverize, the vicious root powder of preparation winter daphne 50kg, directly in apparatus,Soxhlet's, get 2-10h with benzinum or carrene or n-hexane, chloroform apple, decompression and solvent recovery, extract 1850g.Measure root of langdu flavones content.
B. nicotine-containing solution is produced: rhizome, leaf with tobacco are raw material, use the organic solvent refluxing extraction, filter.It is standby that extract is evaporated to the liquid extract of setting concentration.
C. mixed insecticide: measure in the root of langdu extract content of nicotine in flavones, the tobacco extract earlier, the root of langdu flavones of setting by prescription, nicotine content requirement are determined root of langdu extract, tobacco extract proportion of raw materials ratio and are mixed then, mixed raw material drops in the reactor, add other auxiliary agent of setting by prescription, heated and stirred is even, promptly gets root of langdu flavones mixed emulsifiable solution.Wherein temperature of reaction kettle is 60 ℃, and mixing time is 50 minutes.
The root of langdu flavones mixed emulsifiable solution agent preparation of embodiment 3.30%
Proportioning components (weight): 27% root of langdu flavones content, 3% nicotine content, surfactant 20%, stabilizing agent 10%, organic solvent 39.8%, pH value conditioning agent 0.2%
Mixed insecticide: root of langdu flavones, commercially available nicotine (nicotine content 65%) with as above embodiment 1 or 2 preparations are raw material, measure the content of flavones in the root of langdu extract earlier, the root of langdu flavones of setting by prescription, nicotine content requirement are determined root of langdu extract, nicotine proportion of raw materials ratio and are mixed then, mixed raw material drops in the reactor, add other auxiliary agent of setting by prescription, heated and stirred is even, promptly gets root of langdu flavones mixed emulsifiable solution.Wherein temperature of reaction kettle is 60 ℃, and mixing time is 50 minutes.
The root of langdu flavones mixed emulsifiable solution agent preparation of embodiment 4.45%
Proportioning components (weight): 43% root of langdu flavones content, 2% nicotine content, surfactant 15%, stabilizing agent 10%, organic solvent 29.8%, pH value conditioning agent 0.2%
Mixed insecticide: root of langdu flavones, nicotine with as above embodiment 1 or 2 preparations are raw material, the content of nicotine in flavones, the tobacco extract in elder generation's mensuration root of langdu extract, the root of langdu flavones of setting by prescription, nicotine content requirement are determined root of langdu extract, tobacco extract proportion of raw materials ratio and are mixed then, mixed raw material drops in the reactor, add other auxiliary agent of setting by prescription, heated and stirred is even, promptly gets root of langdu flavones mixed emulsifiable solution.Wherein temperature of reaction kettle is 60 ℃, and mixing time is 60 minutes.
Relevant auxiliary agent component is selected as follows in the foregoing description prescription:
Surfactant can be selected for use: tween, sapn, OP-10, sell pool, rare, the sldium lauryl sulfate of polyoxy second; Stabilizing agent can be selected for use: epoxidized vegetable oil;
Organic solvent can be selected for use: dimethylbenzene, methyl alcohol, ethanol, butanone;
The PH conditioning agent can be selected for use: sodium hydroxid, acetic acid;
Preservative is selected for use: benzoic acid is received.
Virulence test embodiment 1
25% root of langdu flavones mixed emulsifiable solution agent toxicity test: the mensuration of carrying out 25% mixed agent synergy degree with Tetranychus urticae (Tetranychus urticae Koch).The results are shown in Table 1.The co-toxicity coefficient of 25% root of langdu flavones mixed emulsifiable solution agent of the present invention is remarkable synergistic effect greater than 200.
Virulence test embodiment 2
45% root of langdu flavones mixed emulsifiable solution agent toxicity test: the mensuration of carrying out 45% mixed agent synergy degree with Tetranychus urticae (Tetranychus urticae Koch).The results are shown in Table 1.The co-toxicity coefficient of 45% root of langdu flavones mixed emulsifiable solution agent of the present invention is remarkable synergistic effect greater than 200.
Table 1 toxicity test
| Reagent agent altogether | Regression equation | Correlation coefficient | LC50(mg/L) | Co-toxicity coefficient |
| 25% root of langdu flavones mixed emulsifiable solution | y＝0.8099x+1.3374 | 0.9433 | 10.5312 | 443.55 |
| 45% root of langdu flavones mixed emulsifiable solution | Y＝2.0151+2.5120 | 0.9532 | 13.5606 | 210.15 |
Claims (5)
1. mixed pesticide of radix euphorbiae lantu chromocor is characterized in that this insecticide is made up of the composition of following percentage by weight:
Root of langdu flavones 10-80%
Nicotine 0.1-65%
All the other are auxiliary agent.
2. mixed pesticide of radix euphorbiae lantu chromocor according to claim 1 is characterized in that: this insecticide is diluted to the spray agent that contains root of langdu flavones 10-1000PPM and nicotine 1-1000PPM concentration.
3. mixed pesticide of radix euphorbiae lantu chromocor according to claim 1 is characterized in that: this insecticide is prepared into emulsion, aqua, aqueous emulsion, colloidal suspending agent, soluble powder or wetting powder.
4. the preparation method of a mixed pesticide of radix euphorbiae lantu chromocor is characterized in that:
(1) extraction of root of langdu flavones: with Chinese Stellera Root clean, pulverize, with at least a immersion in ethanol, methyl alcohol, propyl alcohol, acetone, n-hexane, benzinum and the chloroform, repeatedly extract, be concentrated into the root of langdu chromocor extract of flowing soaking paste, extracting temperature is 30-95 ℃, and the time is 4-24 hour;
(2) preparation of nicotine: rhizome, leaf with tobacco are raw material, use the organic solvent refluxing extraction, filter, and it is standby that extract is evaporated to the liquid extract of setting concentration;
(3) measure the content of nicotine in the commercially available nicotine elaboration of flavones, tobacco extract or nicotine content 50-98% in the root of langdu extract: the content requirement of root of langdu flavones 10-80 weight %, the nicotine 0.1-65 weight % that sets in prescription is determined root of langdu extract, tobacco extract proportion of raw materials ratio and is mixed then, mixed raw material drops in the reactor, add the surplus auxiliary agent of setting by prescription, heated and stirred is even, promptly get root of langdu flavones mixed emulsifiable solution, wherein temperature of reaction kettle is 45-60 ℃, and mixing time is 30-60 minute;
(4) described prescription is set at: root of langdu flavones 10-80 weight %, nicotine 0.1-65 weight % and surplus auxiliary agent.
5. the purposes of mixed pesticide of radix euphorbiae lantu chromocor according to claim 1, it is characterized in that: this insecticide is applicable to the control of pest mite.
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| CN100569077C true CN100569077C (en) | 2009-12-16 |
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| CN101843267A (en) * | 2010-05-20 | 2010-09-29 | 北京绿神保科技有限公司 | High-efficiency nontoxic insecticide and preparation method thereof |
| CN103004854A (en) * | 2013-01-04 | 2013-04-03 | 句容市农业技术推广中心 | Allyl isothiocyanate and nicotine compound insecticide and application thereof |
| FR3018821A1 (en) | 2014-03-24 | 2015-09-25 | Agronomique Inst Nat Rech | NOVEL O-ALPHA-GLUCOSYL FLAVONOIDS ON CYCLE B, PROCESS FOR OBTAINING AND USES |
| CN104642409A (en) * | 2015-01-12 | 2015-05-27 | 无锡双喜金阳生物科技有限公司 | Method for preventing and treating dendrobe sooty mould |
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