CN104521968A - Plant molluscicide as well as preparation method and application thereof - Google Patents
Plant molluscicide as well as preparation method and application thereof Download PDFInfo
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- CN104521968A CN104521968A CN201510029821.2A CN201510029821A CN104521968A CN 104521968 A CN104521968 A CN 104521968A CN 201510029821 A CN201510029821 A CN 201510029821A CN 104521968 A CN104521968 A CN 104521968A
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Abstract
The invention discloses a plant molluscicide as well as a preparation method and application thereof. The molluscicide consists of the following components in percentage by weight: 1-40% of a mother medicine and 60-99% of an auxiliary agent. The preparation method comprises the following steps: (1) removing grease of tea seed meal; (2) adding tea seed meal powder into a 5-18% sodium hydroxide solution of which the weight is 5-6 times that of the tea seed meal powder, soaking for 4-5 hours at 85-105 DEG C to obtain a soaking solution, then adding alkaline protease which accounts for 5-20% of the soaking solution in weight into the soaking solution, soaking for 10-14 hours at 55-75 DEG C, filtering to obtain a filtrate and a filter cake, and drying the filter cake to obtain the auxiliary agent; (3) neutralizing the filtrate by using 5-10% hydrochloric acid until precipitates cannot be separated out any more, centrifuging, removing supernatant liquid to obtain lower-layer precipitates, and drying the lower-layer precipitates to obtain the mother medicine; and (4) crushing the mother medicine and the auxiliary agent into 100-300 meshes, and then uniformly mixing. The molluscicide disclosed by the invention has the advantages of high efficiency, low toxicity, environmental protection, easiness in degradation, low cost, safety, convenience and the like. The method disclosed by the invention is simple, feasible, simple in technological process, and slight in pollution to the environment.
Description
Technical field
The present invention relates to molluscicide technical field, more specifically relate to a kind of plant molluscacide, also relate to a kind of preparation method of plant molluscacide simultaneously, also relate to a kind of plant molluscacide and preparing the purposes killed in Pomacea canaliculata medicine.
Background technology
Pomacea canaliculata has another name called Ampullaria gigas, apple spiral shell, snow spiral shell, is amphibious freshwater shellfish mollusk, classification belongs to Mollusca, Gastropoda, Mesogastropoda, Ampullariidae, bottle spiral shell genus, originates in South America Amazon River basin.
Be introduced into south China and Southeast Asian countries the eighties.Owing to lacking natural enemy and there is strong adaptability, the strong characteristic such as resistance, high reproductive rate (a female spiral shell can breed 300,000 offsprings for a year), break out in China and tropical and subtropical region, Southeast Asia, current Pomacea canaliculata has invaded China's 13 provinces (city) 246 counties (city), numerous river basins such as the Zhujiang River, the Xijiang River, Xiang River, Ganjiang River, River of Ten Thousand Springs, lake, feed ditch, farmland etc., overflow everywhere, a lot of place is developed into " having water just to have Pomacea canaliculata " and the stage of " current where, and where Pomacea canaliculata is just with ".
Fast about 10 times of Pomacea canaliculata reproduction speed nearly source more local than Rice In Asian Cultivated Rice Tanaka species, very fast at most area formation Natural Population since invasion, serious threat invasion waters, ground and neighbouring bio-diversity, harm the crops (paddy rice, wild rice stem, white lotus etc.) and other water plants, causes huge economic loss.Pomacea canaliculata is one of 100 kinds of pernicious Invasive Alien Species in the world, one of first (16 kinds) Invasive Alien Species (Environmental Protection Administration and the Chinese Academy of Sciences, 2003) that Ye Shi China announces.
Asia agricultural, based on rice cultivation, provides good life condition to Pomacea canaliculata.Soon namely start to nibble the water plants such as drinking water rice after Pomacea canaliculata hatching, the tender part of eating children.Mainly be injured the phase before putting field after rice transplanting.It is eaten the main tiller of paddy rice and effective tiller, causes few seedling to be short of seedling, repeatedly need fill the gaps with seedlings, cause extreme loss.Breeding of domestic Pomacea canaliculata year two eposides now, population density is very huge, and as in Guangxi part districts and cities, the generation density of Pomacea canaliculata in rice field is up to 16.95/square metre; Paddy rice strain rate of being injured is generally 7% ~ 15%, is up to 64%, agricultural production is caused to having a strong impact on.The rice field that Pomacea canaliculata is more, the inevitable significantly underproduction of paddy rice, when rice field Pomacea canaliculata density height, can cause the production loss of more than 50%, serious rice seedling one is eaten up night, need remigrate.Comprise the south east asia of China, be the main product ground of View of World Rice, account for 80% of Gross World Product.In the last few years, the total total 5-6 hundred million mu of paddy rice in these areas, were subject to Pomacea canaliculata serious harm, caused the underproduction 10% ~ 35%.
Pomacea canaliculata feeding habits are mixed, harm lotus rhizome, and young spiral shell can gnaw the lotus leaf in floating agio face at the bottom of leaf, and cause lotus leaf blade bore a hole or incise, time serious, blade is gnawed riddled with gaping wounds, is difficult to detach the water surface.Pomacea canaliculata also endangers the various water plants such as daffodil, orchid, becomes a great trouble evil in southern china waters.In addition, Pomacea canaliculata reproduction speed is exceedingly fast, and survival ability is extremely strong, and the existence of the aquatic shellfish of serious harm, threatens local bio-diversity, destroys the formation of food chain and causes serious harm to original aquatic ecological balance.Pomacea canaliculata directly endangers except causing above these, also can cause indirect hazard, the wound taken food become multiple germ invasion passage, bring out various disease occur and popular.Pomacea canaliculata is also the vector of pipe strongylid, echinostoma revolutum, can cause and bite acid meningitis; A large amount of spiral shell shells in paddy field can scratch sole, human body of causing harm.At present, spiral shell evil has become a subject matter of harm China ecotope, and effectively controlling spiral shell evil is ensure one of normal key link of producing of China's agricultural.
The control of spiral shell evil is a complicated comprehensive management engineering, mainly comprises chemical control (as agricultural chemicals goes out spiral shell), biological control (as putting duck in a suitable place to breed) and manually pick up spiral shell plucking the means such as ovum.
In the preventing and controlling of current spiral shell evil, chemical control is widely used, and chemical molluscacide has become the Main Means addressed this problem.Control Pomacea canaliculata chemicals has four kinds of active ingredients both at home and abroad at present: bayluscid, the methaldehyde, fentin acetate and penta sodium pentachlorophenate.These four kinds control Pomacea canaliculatas kill the shortcoming of preparation and present situation as following table:
Wherein three kinds of preparations are because toxicity is large, the residence time long, easily cause the fatal drawbacks such as person poultry poisoning, and are prohibited from using, and a kind ofly discharge a large amount of carcinogen, use procedure quality because of production process and biologically logically to kill, expensive, and use is restricted.In traditional farming is produced, Ye You peasant household uses the custom of tea seed cake control paddy rice Pomacea canaliculata, but in actual use, also exist such as usage amount excessive (mu 20-30Kg), high cost, sn ail control effect bad, use the problems such as inconvenience.
Therefore, be badly in need of development safe and efficient, easily degrade, to environment low-residual, pollution-free, molluscacide cheap and easy to use.
Summary of the invention
For solving above-mentioned prior art Problems existing, the invention provides a kind of plant molluscacide, this molluscacide formula is reasonable, is a kind of novel molluscacide, has efficient, low toxicity, environmental protection, easily degraded, the advantage such as with low cost and safe and convenient to use.
Present invention also offers a kind of preparation method of plant molluscacide, the method is simple, technological process is simple, process conditions are simple and easy to control, rich raw material resource and cheap, agents useful for same and equipment are easy to get and with low cost, and in technical process, do not have waste liquid and discardedly to produce, and environmental pollution is little.
Invention further provides a kind of plant molluscacide and killing the purposes in Pomacea canaliculata and oncomelania, Pomacea canaliculata killed by this molluscacide and oncomelania is effective, and killing rate reaches more than 81%.
A kind of plant molluscacide, comprises the component of following percentage by weight:
Weight percentages of components
Female medicine (the being called for short female medicine) 1-40% of spiral shell prestige
The tea dregs of rice extract solid residue (abbreviation auxiliary agent) 60-99% after the female medicine of spiral shell prestige.
A kind of plant molluscacide, comprises the component of following percentage by weight:
Weight percentages of components
The female medicine 2-20% of spiral shell prestige
The tea dregs of rice extract the solid residue 80-98% after the female medicine of spiral shell prestige.
A kind of plant molluscacide, comprises the component of following percentage by weight:
Weight percentages of components
The female medicine 3-10% of spiral shell prestige
The tea dregs of rice extract the solid residue 90-97% after the female medicine of spiral shell prestige.
A kind of plant molluscacide, comprises the component of following percentage by weight:
Weight percentages of components
The female medicine 8% of spiral shell prestige
The tea dregs of rice extract the solid residue 92% after the female medicine of spiral shell prestige.
A preparation method for plant molluscacide, comprises the steps:
1) grease residual in the tea dregs of rice is removed with solvent naphtha;
2) the tea dregs of rice after degreasing are shattered, obtain tea dregs of rice powder, then tea dregs of rice powder to be joined weight be the 5-6 concentration doubly of tea dregs of rice grain weight amount is in the sodium hydroxide solution of 5%-18%, 4-5 hour is soaked under 85 DEG C of-105 DEG C of conditions, obtain soak, the alkali protease that weight is soak weight 5-20% is added again in soak, soak 10-14 hour under 55 DEG C of-75 DEG C of conditions after, filter, obtain filtrate and filter cake, by filtration cakes torrefaction, obtain the solid residue after the female medicine of tea dregs of rice extraction spiral shell prestige;
3) by filtrate mass percentage concentration be the hydrochloric acid neutralization of 5%-10%, until no longer separate out precipitation, centrifugal, obtain lower sediment after removing supernatant liquor, lower sediment is dry, obtain the female medicine of spiral shell prestige;
4) take the solid residue after the female medicine of spiral shell prestige and the female medicine of tea dregs of rice extraction spiral shell prestige according to above-mentioned weight proportion, mix after the solid residue after female for spiral shell prestige medicine and the tea dregs of rice are extracted the female medicine of spiral shell prestige is crushed to 100-300 order.
Improve technique scheme, described solvent naphtha is No. 6 solvent naphthas; The tea dregs of rice after degreasing are shattered to 100-300 order; In the described tea dregs of rice, the content of pentacyclic triterpene is 8%-12%; Step 3) in supernatant liquor recycled in step 2) in, for preparing sodium hydroxide solution.
A kind of plant molluscacide is killing the purposes in Pomacea canaliculata.This molluscacide Pomacea canaliculata method of going out comprises the steps:
1) molluscacide is taken, wherein consumption (representing with M) (gram)=spiral shell prestige concentration (representing with A1) × rice field depth of water (representing with H) (centimetre) × rice field area (representing with S) (hectare) of active ingredient spiral shell prestige, wherein spiral shell prestige concentration is 90 ~ 150g.ai/ha, i.e. M=A*H*S, can be converted into A2 (g/m
3), A2=M/ (S*10
4* H*10
-2)=M/S*10
2* H, according to the actual conditions in rice field, the depth of water is generally 3-6 centimetre, and the depth of water is preferably 5 centimetres.
2) be that molluscacide consumption 300-400 water-soluble solution doubly is evenly sprayed in rice field afterwards by molluscacide quality, in actual mechanical process, also every mu of dosage can mix 8-12 kilogram of fine sand and apply, keep water level in paddy field to stablize 2-4 days, suitably can increase and decrease the dosage of molluscacide according to spiral shell evil degree and weather condition.
Compared with prior art, its beneficial effect and advantage are in the present invention:
1, the raw material of this molluscicide is the tea dregs of rice after tea seed squeezes edible oil, and be natural organic substance, toxicity is low, and natural degradation is fast, has infertile field effect, produces and the equal environmentally safe of use procedure, and aboundresources, and cheap, per ton only have about thousand yuan.
2, effective medicinal ingredient of this molluscicide is the spiral shell prestige in the female medicine of spiral shell prestige, because the cost of the female medicine of spiral shell prestige is very high, and the female survival dose of spiral shell prestige seldom just has good curative effect, and the solid residue after the female medicine of tea dregs of rice extraction spiral shell prestige is natural organic substance, and toxicity is low, natural degradation is fast, molluscicide can be processed into together with the female medicine of auxiliary agent and spiral shell prestige, not only can kill the Pomacea canaliculata in farmland, also there is infertile field function, easy degraded, little on environmental organism impact.
3, this molluscicide and existing market stub kill compared with the agent of spiral shell preparation Niclosamide ethanolamine salt wettable powder, preventive effect is suitable, reduce the toxic action to fish, increase the reaction time (slow down or eliminate and cause harm) being strayed into the aquaculture districts such as fish pond because using this molluscacide, and production cost only has 1/3rd of bayluscid, cost performance is better than niclosamidum greatly; Compared with Seed of Camellia Sinensis plant molluscicide, avoid proposing Tea Saponin with tea seed cake for many years and to go out the traditional approach of spiral shell, and dosage comparatively Tea Saponin significantly reduce, the spiral shell cost that goes out is low, effective.
4, this molluscicide is easily degraded, and environmental pollution is little, and to people and other biological safe and harmless.This molluscicide carries out per os to mouse, tests through skin test, and Acute inhalation all belongs to lower toxicity; This molluscicide, to the test of cavy sensitization contact, is weak sensitization; This molluscicide is non-stimulated to rabbit skin, stimulates be respectively slight excitant to rabbit eyes.
5, the preparation method of this molluscicide is simple, has increased substantially the content of spiral shell prestige in the female medicine of spiral shell prestige, and spiral shell prestige content about 50% in the female medicine of spiral shell prestige of gained, significantly shortens the time of preparing the female medicine of spiral shell prestige, save the cost preparing the female medicine of spiral shell prestige.
In a word, this molluscicide had both breached the restraining factors that plant is in the past gone out in Pomacea canaliculata research, solve again existing chemistry to go out the bottleneck of Pomacea canaliculata medicament, have efficient, low toxicity, environmental protection, easily degraded, the advantage such as with low cost and safe and convenient to use, suit large area to popularize application.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1
A kind of plant molluscacide, it is made up of the component of following percentage by weight:
The female medicine 8% of spiral shell prestige
The tea dregs of rice extract the solid residue 92% after the female medicine of spiral shell prestige.
The preparation method of above-mentioned plant molluscacide, comprises the steps:
1) content choosing pentacyclic triterpene is the tea dregs of rice of 8%-12%, removes grease (fat content is lower than 2%) residual in the tea dregs of rice with No. 6 solvent naphthas.
2) the tea dregs of rice after degreasing are shattered, obtain tea dregs of rice powder, then tea dregs of rice powder to be joined weight be the concentration of 5.5 times of tea dregs of rice grain weight amount is in the sodium hydroxide solution of 12%, soaks 4.5 hours, obtain soak under 95 DEG C of conditions, the alkali protease that weight is soak weight 12.5% is added again in soak, soak under 60 DEG C of conditions after 12 hours, filter, obtain filtrate and filter cake, by filtration cakes torrefaction, obtain the solid residue after the female medicine of tea dregs of rice extraction spiral shell prestige.
3) by filtrate quality percentage concentration be 7.5% hydrochloric acid neutralization, until no longer separate out precipitation, centrifugal, obtain lower sediment after removing supernatant liquor, lower sediment is dry, obtain the female medicine of spiral shell prestige.
4) solid residue after the female medicine of spiral shell prestige and the female medicine of tea dregs of rice extraction spiral shell prestige is taken according to above-mentioned weight proportion, mix after solid residue after female for spiral shell prestige medicine and the tea dregs of rice are extracted the female medicine of spiral shell prestige is crushed to 200 orders, obtain this molluscicide, after testing, wherein the mass percentage of spiral shell prestige is 4%.
Its preparation process is identical with embodiment 1.
Following test is carried out with molluscacide prepared by the present embodiment 1:
Test one, the indoor security when stubble trial crops is tested
Reagent agent: molluscacide prepared by the present embodiment 1
Dosage is arranged: 400 grams/acre, 800 grams/acre, 1600 grams/acre
For studying thing: Wu Xiang is glutinous 8333, military fortune No. 7, round-grained rice, new two excellent No. 6
Controlling object: Pomacea canaliculata (Pomacea canaliculata)
Application method: spraying, metered dose process rice seedling.
Investigation method: by symptom and the degree of five point sampling investigation records poisoning.
Result of the test:
In whole process of the test, do not observe the symptom that poisoning appears in crop, therefore this medicament is safe to working as stubble trial crops.
Test two: environmental organism toxicity and safety evaluatio are tested
Reagent agent: molluscacide prepared by the present embodiment 1.
One, toxicity in fish and safety evaluatio are tested
1, fingerling is tested
Test fingerling is zebra fish (Brachydanio rerio H.B), and average body long (connecting tail) 3.5cm, average weight is about 0.4g, and by Nanjing, Confucian scholar provides in aquarium.Raise and train one week in indoor before test, raise and train period zebra fish growth normally, without dead, all healthy anosis, in the same size.Test stops feeding the previous day, also not feeding in test.
2, test method
Test water is that test chamber is the glass jar of 25 liters through depositing and the aeration dechlorination process running water of more than 24 hours.First by prerun determination toxic effect scope, during normal assays within the scope of this differential liquid that some groups of variable concentrations are set according to a certain percentage, separately establish a blank group, repeated test 3 times.Concrete scheme is: in 6 glass jars, prepare the molluscacide liquid that 10 liters of concentration are 0mg/l, 0.04mg/l, 0.10mg/l, 0.15mg/l, 0.2mg/l and 0.4mg/l respectively, and in 6 glass jars, drop into zebra fish 10 respectively, regulate the room temperature and make water temperature remain on about 20 DEG C.
Experiment adopts the semi-static method changing a liquid every 24 hours.In test, timing measures dissolved oxygen and the pH value of test solution in each cylinder.Experiment lasts 96 hours, the poisoning symptom of Continuous Observation record 24,48,72 and 96 hours zebra fishs and death figure, in time removes dead fish, and show that plant molluscacide prepared by embodiment 1 is to the half lethal concentration LC of zebra fish according to result of the test
50value.
Test shows, after zebra fish contact liquid, low concentration group frequently turns around, and moves about fast, and oral area opening and closing rapidly, aobvious state short of breath; High concentration group rubs head, whipping, play rolling, and look turns white, abdomen swelling, and after 20-30 minute, the bottom of lying on one's side, twitches spasm, death of struggling rapidly.
Result of the test is as following table:
Plant molluscacide prepared by table 1 the present embodiment is to the toxicity of zebra fish
Try to achieve the LC of zebra fish 96h thus
50for 0.15mg/l, 95% is crediblely limited to 0.14-0.17mg/l.
According to agricultural chemicals to toxicity in fish grade scale, 96hLC
50value > 10.0mg/l's is low toxicity, and 1.0-10.0mg/l is poisoning, and 0.l-1.0mg/l is high poison, and < 0.1mg/l is severe toxicity.But this is visible, plant molluscacide prepared by the present embodiment is high poison to fish.Because this medicine is directly used in water body or waterside beach and hillside fields, and working concentration is higher than LC
50value, therefore comparatively large to fish risk, the impact on fish should be kept a close eye on.
Two, birds toxicity and safety evaluatio are tested
1, bird kind is tested
Test bird kind is Japanese quail (Coturnix coturnix japonica), is provided by Agricultural University Of Nanjing chicken farm.Select 30 day age, about body weight 100g, the quail of bouncing is for examination.Precuring one week under laboratory test condition before test, during precuring, quail all grows normally, anosis nothing death.
2, test method
Laboratory's temperature 20 DEG C ~ 25 DEG C, room ventilation printing opacity.Feed adopts into quail feed, feeds with clear water simultaneously.Quail is often organized 10 (male and female half and half) in test, fasting overnight before test, only for clear water.By the first prerun of formal test condition before test, obtain the toxic effect scope of agricultural chemicals to quail.Differential according to a certain percentage within the scope of this during formal test some concentration for the treatment of are set, and establish a blank group, repeated test 3 times.Concrete scheme: medicament is mixed with respectively the molluscacide liquid that concentration is 0mg/ml, 0.12mg/ml, 0.24mg/ml, 0.48mg/ml, 0.72mg/ml and 1.2mg/ml, then carries out contamination process by every 100g body weight quail perfusion 0.5ml.
The per os contamination administration by gavage that test adopts disposable dosage directly to inject, the quail after process is raised according to a conventional method, observed and recorded quail poisoning symptom and death condition, and test lasts 7 days.The medial lethal dose LD50 value of embodiment 1 plant molluscacide to quail is drawn according to result of the test.
Test shows, after quail contamination, low concentration group poisoning symptom is not obvious; High concentration group gets rid of head, and neck stretches indefinite, pouts opening and closing and does not stop, and venturi is sobbed and spoken, and hooks before tail, and wing is sagging, and feather is fluffy messy, and after 20 hours, minority is dead.
Result of the test is as following table:
Plant molluscacide prepared by table 2 the present embodiment is to the toxicity of quail
Try to achieve the LC of quail 7d thus
50> 60mg/kg body weight.
According to the toxic grade criteria for classifying of agricultural chemicals to bird, LD
50the agricultural chemicals of >500mg/kg body weight is low-toxin farm chemicals, and the agricultural chemicals of 50-500mg/kg body weight is medium toxic pesticides, and the agricultural chemicals of 10-50mg/kg body weight is high-toxic pesticide, and the agricultural chemicals of <10mg/kg body weight is highly toxic pesticide.In this test, 60mg/kg body weight is the highest configurable concentration, and when this concentration, the lethality of bird is only 20%.But this is visible, plant molluscacide prepared by the present embodiment is poisoning to birds, because this medicine is not use with granular form, therefore little to the actual Harmfulness analyse of bird.
Three, shrimps toxicity and safety evaluatio are tested
1, shrimp species are tested
Test shrimp species are that freshwater shrimp (Macrobrachium nipponensis de Haan) becomes shrimp, average weight 2.0g.Raise and train two days in indoor before test, raise and train period freshwater shrimp growth normally; None is dead.Test with shrimp all healthy anosis, in the same size.Test stops feeding the previous day, also not feeding in test.
2, test method
Test water is through depositing and the aeration dechlorination process running water of more than 24 hours.Test chamber is the glass jar of 25 liters.First by prerun determination toxic effect scope, during normal assays within the scope of this differential liquid that some groups of variable concentrations are set according to a certain percentage, separately establish a blank group, repeated test 3 times.Concrete scheme is: in 6 glass jars, prepare the molluscacide liquid that 20 liters of concentration are 0mg/l, 1mg/l, 2mg/l, 3mg/l, 5mg/l and 10mg/l respectively, and in 6 glass jars, drop into freshwater shrimp 10 respectively, regulate the room temperature and make water temperature remain on about 20 DEG C.
Test adopts the semi-static method changing a liquid every 24 hours.In test, timing measures dissolved oxygen and the pH value of test solution in each cylinder.Test lasts 96 hours, and the poisoning symptom of Continuous Observation record 24,48,72 and 96 h run biology and death figure, remove died in time.Plant molluscacide prepared by the present embodiment is obtained to the half lethal concentration LC of freshwater shrimp by probabilistic method
50value.
Test shows, after freshwater shrimp contact liquid, the freshwater shrimp of low concentration group is originally movable swashs play, and up and down in experimental liquid, swimming foot is agitated rapidly, aobvious dysphoria state, and after 1-2 hour, major part can return to normal condition; High on the freshwater shrimp head of high concentration group, hook before tail, thorax abdomen is recessed, and together, body bobbing porpoising, after 8-10 hour, major part rubs tail play, and foot is waved in side, struggles dead in clustering.
Result of the test is as following table:
Plant molluscacide prepared by table 2 the present embodiment is to the toxicity of freshwater shrimp
Try to achieve the LC of zebra fish 96h thus
50for 6.28mg/l, 95% is crediblely limited to 3.53-11.2mg/l.
According to the grade scale of China's agricultural chemicals to aquatic toxicity, 96h LC
50value >10.0mg/l's is low toxicity, and 1.0-10.0mg/l is poisoning, and 0.1-1.0mg/l is high poison, and <0.1mg/l is severe toxicity.But this is visible, plant molluscacide prepared by the present embodiment is poisoning to shrimps, and the working concentration that method is killed in leaching is 0.2mg/l, is less than the LC of this medicine prawn
50value, the practical risk of prawn is less; Spray method, the actual working concentration of powder injection process is 100mg/l, be greater than LC
5010 times that are worth, when therefore using, shrimps are had a big risk, the impact of prawn should be kept a close eye on.
In sum, the toxicity of plant molluscacide of the present invention to environmental organism reaches criterion of acceptability.During actual use, fish, shrimp are had a big risk, lower to bird risk, keep a close eye on the hydrobiological impact such as fish, shrimp.
Embodiment 10:
A kind of plant molluscacide, it is made up of the component of following percentage by weight:
The female medicine 20% of spiral shell prestige
The tea dregs of rice extract the solid residue 80% after the female medicine of spiral shell prestige.
The preparation method of above-mentioned plant molluscacide, comprises the steps:
1) content choosing pentacyclic triterpene is the tea dregs of rice of 8%-12%, removes grease (fat content is lower than 2%) residual in the tea dregs of rice with No. 6 solvent naphthas.
2) the tea dregs of rice after degreasing are shattered, obtain tea dregs of rice powder, then tea dregs of rice powder to be joined weight be the concentration of 5 times of tea dregs of rice grain weight amount is in the sodium hydroxide solution of 18%, soaks 4 hours, obtain soak under 105 DEG C of conditions, the alkali protease that weight is soak weight 5% is added again in soak, soak under 55 DEG C of conditions after 14 hours, filter, obtain filtrate and filter cake, by filtration cakes torrefaction, obtain the solid residue after the female medicine of tea dregs of rice extraction spiral shell prestige;
3) by filtrate mass percentage concentration be 5% hydrochloric acid neutralization, until no longer separate out precipitation, centrifugal, obtain lower sediment after removing supernatant liquor, lower sediment is dry, obtain the female medicine of spiral shell prestige;
4) take the solid residue after the female medicine of spiral shell prestige and the female medicine of tea dregs of rice extraction spiral shell prestige according to above-mentioned weight proportion, mix after the solid residue after female for spiral shell prestige medicine and the tea dregs of rice are extracted the female medicine of spiral shell prestige is crushed to 200 orders, obtain this molluscicide.
Embodiment 11:
A kind of plant molluscacide, it is made up of the component of following percentage by weight:
The female medicine 40% of spiral shell prestige
The tea dregs of rice extract the solid residue 60% after the female medicine of spiral shell prestige.
The preparation method of above-mentioned plant molluscacide, comprises the steps:
1) content choosing pentacyclic triterpene is the tea dregs of rice of 8%-12%, removes grease (fat content is lower than 2%) residual in the tea dregs of rice with No. 6 solvent naphthas;
2) the tea dregs of rice after degreasing are shattered, obtain tea dregs of rice powder, then tea dregs of rice powder to be joined weight be the concentration of 6 times of tea dregs of rice grain weight amount is in the sodium hydroxide solution of 5%, soaks 4 hours, obtain soak under 85 DEG C of conditions, the alkali protease that weight is soak weight 20% is added again in soak, soak under 75 DEG C of conditions after 10 hours, filter, obtain filtrate and filter cake, by filtration cakes torrefaction, obtain the solid residue after the female medicine of tea dregs of rice extraction spiral shell prestige;
3) by filtrate mass percentage concentration be 10% hydrochloric acid neutralization, until no longer separate out precipitation, centrifugal, obtain lower sediment after removing supernatant liquor, lower sediment is dry, obtain the female medicine of spiral shell prestige;
4) take the solid residue after the female medicine of spiral shell prestige and the female medicine of tea dregs of rice extraction spiral shell prestige according to above-mentioned weight proportion, mix after the solid residue after female for spiral shell prestige medicine and the tea dregs of rice are extracted the female medicine of spiral shell prestige is crushed to 300 orders, obtain this molluscicide.
Embodiment 12:
A kind of plant molluscacide, it is made up of the component of following percentage by weight:
The female medicine 10% of spiral shell prestige
The tea dregs of rice extract the solid residue 90% after the female medicine of spiral shell prestige.
The preparation method of above-mentioned plant molluscacide, comprises the steps:
1) content choosing pentacyclic triterpene is the tea dregs of rice of 8%-12%, removes grease (fat content is lower than 2%) residual in the tea dregs of rice with No. 6 solvent naphthas;
2) the tea dregs of rice after degreasing are shattered, obtain tea dregs of rice powder, then tea dregs of rice powder to be joined weight be the concentration of 6 times of tea dregs of rice grain weight amount is in the sodium hydroxide solution of 10%, soaks 4.2 hours, obtain soak under 90 DEG C of conditions, the alkali protease that weight is soak weight 9% is added again in soak, soak under 60 DEG C of conditions after 11.5 hours, filter, obtain filtrate and filter cake, by filtration cakes torrefaction, obtain the solid residue after the female medicine of tea dregs of rice extraction spiral shell prestige;
3) by filtrate mass percentage concentration be 7% hydrochloric acid neutralization, until no longer separate out precipitation, centrifugal, obtain lower sediment after removing supernatant liquor, lower sediment is dry, obtain the female medicine of spiral shell prestige;
4) take the solid residue after the female medicine of spiral shell prestige and the female medicine of tea dregs of rice extraction spiral shell prestige according to above-mentioned weight proportion, mix after the solid residue after female for spiral shell prestige medicine and the tea dregs of rice are extracted the female medicine of spiral shell prestige is crushed to 250 orders, obtain this molluscicide.
Embodiment 13:
The plant molluscacide prepared for embodiment 1 below kills Pomacea canaliculata effect test, elaborates to the purposes of this microflora molluscacide.
Reagent agent: molluscacide prepared by the present embodiment 1.
Test reference standard: Toxicity Determination kills method with reference to the indoor harmacological effect evaluation leaching of agricultural chemicals inspection (raw survey) letter [2005] No. 77 agriculture chemical registration health molluscacide test of pesticide effectiveness methods and evaluation (trying) and GB/T17322.1-1998 agriculture chemical registration hygienic insecticide.Pesticide field efficacy medicine test criterion (two) the 81st part molluscicide control paddy rice Pomacea canaliculata standard.
One, laboratory test
Experimental condition: indoor temperature: 26 ± 1 DEG C, relative moisture: 60 ± 5%.
Pomacea canaliculata is originated: Huanggang City, the Hubei Province Yingshan County Fan family chews the Pomacea canaliculata in new bridge village of township ChunHui Group paddy field.
Test method
1) Pomacea canaliculata is placed in laboratory aquarium, mix green vegetable leaf with cooperation chicken feed and raise, select the long 2.5-3.5cm of body, be quick on the draw, disease-free, unabroken spiral shell is tested.
2) the female medicinal acetonitrile of spiral shell prestige embodiment 1 prepared dissolves, and is diluted to 0.05 μ g/mL, 0.10 μ g/mL, 0.20 μ g/mL, 0.40 μ g/mL and 0.80 μ g/mL respectively, and is placed in 5 beakers respectively with the 0.1%Triton X-100 aqueous solution; The former medicinal acetonitrile of 98% bayluscid is dissolved, 0.05 μ g/mL, 0.10 μ g/mL, 0.20 μ g/mL, 0.40 μ g/mL and 0.80 μ g/mL is diluted to the 0.1%Triton X-100 aqueous solution, and be placed in 5 beakers respectively, separately establish a blank group.In each beaker, throw Pomacea canaliculata 10, throw after spiral shell and remove liquid after 48h, get Pomacea canaliculata clear water and rinse to be placed in plate for 3 times and add a little clear water, observe oncomelania 48 hours, stretch dimple and creep for spiral shell of living, remaining with breaking method qualification into pieces anyway.Repeated test three times.
Result of the test is as following table:
This molluscacide of table 4 is to paddy rice Pomacea canaliculata virulence situation
The former medicine of table 5 bayluscid is to paddy rice Pomacea canaliculata virulence situation
As seen from the above table, the consumption of the former medicine of 98% bayluscid on plant molluscacide of the present invention and market is suitable with preventive effect.
Two, outdoor field trial
Test site: the late rice in face village of Long Gang village, Pu Miao town, Yongning District, Nanning City.
Field trial field situation: in the experimental field in low-lying, close ditch, Pomacea canaliculata harm is heavier.Rice cropping mode is for transplanting, and transplanting the date is August 8, and Rice Cropping specification is 6.5cm × 4.5cm, every root and stem of certain plants 3-4 seedling.During test, after paddy rice transplanting 2 days, breeding time was the phase of turning green, the field depth of water 4 ~ 6 centimetres.
Test method
1) Qu Sige community (rice field without Pomacea canaliculata harm), 4 square metres, every community, every community interpolation planting paddy rice 120 clumps of paddy rice, minizone is built ridge and is separated, arrange a blank district again, each minizone plastic film is separated, test repetition 4 times.
2) gather the spiral shell alive in ditch and rice field, precuring 48 hours, 80 spiral shells of the same size are put in dispenser first 1 hour every artificial community.To put after spiral shell 1 hour, after water base the clarification in rice field.Three communities are by experimental scheme spiral shell prestige consumption (spiral shell prestige consumption is amounted to into molluscacide consumption) for 90g.ai/ha, 120g.ai/ha, 150g.ai/ha evenly impose molluscacide prepared by embodiment 1 wherein, more evenly impose 50% Niclosamide ethanolamine salt wettable powder agent to another community by experimental scheme bayluscid consumption (bayluscid consumption is amounted to into Niclosamide ethanolamine salt wettable powder agent) 600g.ai/ha.After dispenser keep within more than 2 days, do not pour water, not draining in 7 days.Within after dispenser 2 days, 7 days, check once the dead spiral shell number of visible work in each community, within after medicine 14 days, find out all spiral shells of putting in a suitable place to breed, check dead spiral shell number of living (inadequate 80 calculate by escaping), and check that paddy rice is subject to Pomacea canaliculata Harm.
Result of the test is as following table:
The outdoor site test results situation of table 6
The results of analysis of variance shows: 150g.ai/ha process and 120g.ai/ha process field efficacy, and two process preventive effects are suitable.120g.ai/ha process preventive effect and 90g.ai/ha process field efficacy, each sky after medicine, 120g.ai/ha process preventive effect is significantly better than 90g.ai/ha process preventive effect, after its Chinese medicine 14 days, and difference reaches pole significance level.Compared with bayluscid, when identical preventive effect, the consumption of plant molluscacide of the present invention is 1.87 times of 50% Niclosamide ethanolamine salt wettable powder agent consumption, but the cost of this plant molluscacide only has 1/3rd of 50% Niclosamide ethanolamine salt wettable powder agent, and this plant molluscacide is very easy to degraded, almost pollution-free to environment, in general, this plant molluscacide is better than 50% Niclosamide ethanolamine salt wettable powder agent greatly.
In sum: it is very good that plant molluscacide of the present invention kills Pomacea canaliculata effect, and cost is low, almost environmentally safe.
Claims (10)
1. a plant molluscacide, is characterized in that the component comprising following percentage by weight:
The female medicine 1-40% of spiral shell prestige
The tea dregs of rice extract the solid residue 60-99% after the female medicine of spiral shell prestige.
2. plant molluscacide according to claim 1, is characterized in that:
The female medicine 2-20% of spiral shell prestige
The tea dregs of rice extract the solid residue 80-98% after the female medicine of spiral shell prestige.
3. plant molluscacide according to claim 1, is characterized in that:
The female medicine 3-10% of spiral shell prestige
The tea dregs of rice extract the solid residue 90-97% after the female medicine of spiral shell prestige.
4. plant molluscacide according to claim 1, is characterized in that:
The female medicine 8% of spiral shell prestige
The tea dregs of rice extract the solid residue 92% after the female medicine of spiral shell prestige.
5. a preparation method for plant molluscacide according to claim 1, is characterized in that comprising the steps:
1) grease residual in the tea dregs of rice is removed with solvent naphtha;
2) the tea dregs of rice after degreasing are shattered, obtain tea dregs of rice powder, then tea dregs of rice powder to be joined weight be the 5-6 concentration doubly of tea dregs of rice grain weight amount is in the sodium hydroxide solution of 5%-18%, 4-5 hour is soaked under 85 DEG C of-105 DEG C of conditions, obtain soak, the alkali protease that weight is soak weight 5-20% is added again in soak, soak 10-14 hour under 55 DEG C of-75 DEG C of conditions after, filter, obtain filtrate and filter cake, by filtration cakes torrefaction, obtain the solid residue after the female medicine of tea dregs of rice extraction spiral shell prestige;
3) by filtrate mass percentage concentration be the hydrochloric acid neutralization of 5%-10%, until no longer separate out precipitation, centrifugal, obtain lower sediment after removing supernatant liquor, lower sediment is dry, obtain the female medicine of spiral shell prestige;
4) take the solid residue after the female medicine of spiral shell prestige and the female medicine of tea dregs of rice extraction spiral shell prestige according to weight proportion described in claim 1, mix after the solid residue after female for spiral shell prestige medicine and the tea dregs of rice are extracted the female medicine of spiral shell prestige is crushed to 100-300 order.
6. the preparation method of plant molluscacide according to claim 5, is characterized in that: described solvent naphtha is No. 6 solvent naphthas.
7. the preparation method of plant molluscacide according to claim 5, is characterized in that: shatter the tea dregs of rice after degreasing to 100-300 order.
8. the preparation method of plant molluscacide according to claim 5, is characterized in that: in the described tea dregs of rice, the content of pentacyclic triterpene is 8%-12%.
9. the preparation method of plant molluscacide according to claim 5, is characterized in that: step 3) in supernatant liquor recycled in step 2) in, for preparing sodium hydroxide solution.
10. a plant molluscacide according to claim 1 is killing the purposes in Pomacea canaliculata.
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Application publication date: 20150422 |