CN100384329C - Pesticide containing comptothecin or dreivates of camptothecin, and preparation method - Google Patents
Pesticide containing comptothecin or dreivates of camptothecin, and preparation method Download PDFInfo
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Abstract
The present invention discloses a pesticide containing camptothecin or camptothecin derivatives and a preparation method thereof, particularly a pesticide used for preventing and killing pests such as homoptera, thysanoptera, lepidoptera and coleoptera, and the present invention belongs to the technical field of pesticides. The gpesticide containing camptothecin or camptothecin derivatives is characterized in that the pesticide contains the following components in proportion: 0.01 to 5.00% of camptothecin or the derivative thereof, 0.5 to 20% of emulsifier, 0.5 to 20% of penetrating agent and organic solvent as the rest; additionally, the components in the proportion are mixed to prepare the pesticide, and the components can also be compounded with other known pesticides to prepare mixture pesticides. The pesticide containing camptothecin or camptothecin derivatives has the advantages of high activity, broad disinsection spectrum, environmental protection and no public hazard, and belongs to the field of biotic pesticides.
Description
Technical field
The invention belongs to the insecticide technical field, especially prevent and treat the insecticide of Homoptera, thrips, Lepidoptera and coleopteran pest, be specifically related to a kind of insecticide that contains camptothecine or camptothecin derivative and preparation method thereof.
Background technology
Camptothecine (CPT) is a kind of pyrroles's quinoline alkaloid, and the chemical structure of general formula of camptothecine and derivative thereof is as follows:
O
R7 R8 R9 R10
R6
N O
R5 N O
R4 R3 R2?R1 OH
General formula (I)
Wherein the R1-10 in the chemical constitution represents in hydrogen atom, methyl, ethyl, propyl group, butyl, hydroxyl, nitro, amino, oxygen methyl, first aminooxy group, fluoro ethyl, chloro ethyl, bromoethyl, nitrogen base, silicyl, the alkoxyl one.Camptothecine is mainly derived from the equal camplotheca acuminata of the distinctive plant a kind of jade of China, is separated first by people such as Wall in 1966 to obtain from the camplotheca acuminata bar that China introduces a fine variety.Discover that camptothecine all has certain short term effect to multiple malignant tumours such as head and neck neoplasm, carcinoma of urinary bladder and leukemia.Until 1985, people such as Hsiang find camptothecine and derivative be with topology isomerase (topo I) serve as that the effect target suppresses DNA synthetic bring into play the mechanism of antitumaous effect after, just cause people's attention again.Many derivatives arise at the historic moment, and become the new focus of anticancer area research.So far the derivative of being reported reached seven, 80 kind more than.But all in all, the derivative developed of clinical testing at present mainly contains two classes: a kind of is the research of soluble derivative.The preclinical phase evidence: this analog derivative is a topo I inhibitor preferably, and the solid piece tumour of multiple human body is produced effect.Another kind of is to be the water-insoluble derivative of the camptothecine of representative with 9-nitro and 9-amino.They are higher than the active anticancer of parent compound in evidence.
As seen, camptothecine and derivative thereof have become the focus of medical research as the research of medicine especially antineoplastic, in China's patent information database, be that keyword is searched for the camptothecine, more than 100 relevant patent appears altogether, wherein has only a patent relevant with agricultural chemicals, the patent No. is 91103498 Camptothecines plant insecticide and manufacture method thereof, this invention relates to a kind of Camptothecines plant insecticide and manufacture method thereof, mainly be to contain alkaloidal plant tissue with several, according to camplotheca acuminata 33～36%, horn 3～5%, thunder godvine 7～12%, drooping stringbush flower root and bark 3～6%, herba fibraureae recisae 1～3%, Bothriospermum Chinese 1～2% material coarse cutting such as several plant such as grade, mix by a certain percentage, dry, pulverize, leaching, filter, be mixed.And add additive 5～11%, and water 30～36%, in fact, because above-mentioned alkaloid is natural alkaloid, and all difficulty is dissolved in water, camptothecine especially, this patent exploitativeness is relatively poor, and drug effect is general.
Summary of the invention
For overcoming problems of the prior art, the present invention aims to provide a kind of active high, exploitativeness is good and good drug efficacy, insecticidal spectrum are wide insecticide that contains camptothecine or camptothecin derivative and preparation method thereof.
Described a kind of insecticide that contains camptothecine or camptothecin derivative is characterized in that containing: camptothecine or derivatives thereof 0.01～5.00%, and emulsifier 0.5～20%, bleeding agent 0.5～20%, surplus is an organic solvent.
Described a kind of insecticide that contains camptothecine or camptothecin derivative, it is characterized in that containing: camptothecine or derivatives thereof 0.05～2.5% is preferably 0.1～1%; Emulsifier 1～10% is preferably 2～5%; Bleeding agent 1～10% is preferably 2～5%.Described camptothecine or derivatives thereof is one or more the mixture in the camptothecine or derivatives thereof, promptly contains the compound in a kind of general formula (I) at least.
Described a kind of insecticide that contains camptothecine or camptothecin derivative is characterized in that containing: insecticide 2～40% is preferably 5～20%, more preferably 8～15%.Described insecticide is present known insecticide.
Described a kind of insecticide that contains camptothecine or camptothecin derivative, it is characterized in that: described camptothecin derivative is 9-nitrocamptothecin, 9-aminocamptothecin, 10-hydroxycamptothecine, 10,11-methylene-dioxy-camptothecine, Fluoroethylcamptothederivatives, 10-alkoxy camptothecin or 9-nitro-20-camptothecine.
Described a kind of insecticide that contains camptothecine or camptothecin derivative is characterized in that: described organic solvent is one or more the mixture in dimethyl sulfoxide (DMSO), dimethyl formamide, propyl alcohol, isopropyl alcohol, ethylene glycol, ethanol, methyl alcohol, ether, chloroform toluene, acetone, benzene,toluene,xylene and the propylene glycol.
Described a kind of insecticide that contains camptothecine or camptothecin derivative, it is characterized in that: described emulsifier is anion surfactant, non-ionic surface active agent or its mixture, is preferably one or more the mixture in Tween-80, OP-10, the calcium dodecyl benzene sulfonate.
Described a kind of insecticide that contains camptothecine or camptothecin derivative is characterized in that: described bleeding agent is a penetrating agent JFC, i.e. fatty alcohol ethylene oxide condensate, perhaps azone.
Described a kind of insecticide that contains camptothecine or camptothecin derivative is characterized in that: described insecticide is fluorine worm nitrile, Imidacloprid, buprofezin, desinsection list, chlopyrifos, carbosulfan, sumicidin or Avermectin.
Described a kind of method for producing insecticide that contains camptothecine or camptothecin derivative is characterized in that comprising the following steps:
1) in reactor or agitator tank, adds solvent by said ratio, in this solvent, add the camptothecine or derivatives thereof, be heated to 20～60 ℃ and constantly stirring, to dissolving fully;
2) add emulsifier again, after stirring, add bleeding agent or high bleeding agent, stir, get finished product, promptly contain the insecticide of camptothecine or camptothecin derivative.
Described a kind of method for producing insecticide that contains camptothecine or camptothecin derivative is characterized in that comprising the following steps:
1) in reactor or agitator tank, adds solvent by said ratio, in this solvent, add the camptothecine or derivatives thereof, be heated to 20～60 ℃ and constantly stirring, after the dissolving, add insecticide more extremely fully, stir;
2) add emulsifier again, after stirring, add bleeding agent, stir, get finished product, promptly contain the insecticide of camptothecine or camptothecin derivative.
Described a kind of insecticide that contains camptothecine or camptothecin derivative is by the camptothecine to natural extract, and camptothecine is carried out the camptothecin derivative of structure of modification, carries out the processing of insecticide formulation, have greater activity, and exploitativeness is good; Because the insecticidal spectrum of camptothecine and derivative thereof is very wide, comprises homoptera pest, thrips, lepidoptera pest, coleopteran pest, and has a plurality of different mechanism of action, is difficult for developing immunity to drugs; The own toxicity of camptothecine and derivative thereof is little, even use under extremely low concentration, as less than 1ppm, all has good insecticidal effect, and as seen, described insecticide insecticidal spectrum is wide, good drug efficacy and environmental protection and public nuisance free.
Percentage composition in the present specification is the weight percentage of pure material.
Embodiment
Now describe preferred embodiment of the present invention in detail, and the beneficial effect of this embodiment is described by test.
Embodiment 1
(1) drop into 100L ethanol in reactor or agitator tank, add the 60L calcium dodecyl benzene sulfonate, after the stirring, add 40L OP-10, stir, promptly compound emulsifying agent is standby.
(2) in another reactor or agitator tank, drop into the 400L dimethyl sulfoxide (DMSO), adding 0.5kg purity is 90% camptothecine, be heated to 35 ℃ and constantly stirring, after camptothecine dissolves fully, add above-mentioned compound emulsifying agent 20L, after stirring, add 15L JFC and 5L azone, stir, final products.
Embodiment 2
The purity that is added be 90%-camptothecine is 2kg, other conditions are identical with embodiment 1.
Embodiment 3
The purity that is added is that 90% camptothecine is 5kg, and other conditions are identical with embodiment 1.
Embodiment 4
In reactor or agitator tank, drop into 400L mixed solvent (methyl alcohol+ethanol, 1: 1) add 0.2kg purity greater than 90% 9-aminocamptothecin, after stirring dissolving fully, add 1.8kg purity greater than 90% above fluorine worm nitrile, after the stirring and dissolving, add the 30L Tween-80 and stir, add 10L JFC and 1L azone, stir, final products.
Embodiment 5
In reactor or agitator tank, drop into the 400L isopropanol solvent, add 1.0kg purity greater than 90% 9-aminocamptothecin, after stirring dissolving fully, add 1.0kg purity greater than 90% above Imidacloprid, after the stirring and dissolving, add the 40L Tween-80 and stir, add 20L JFC and 1L azone, stir, final products.
Embodiment 6
In reactor or agitator tank, drop into the 400L alcohol solvent, add 2.0kg purity greater than 90% 9-aminocamptothecin, after stirring dissolving fully, add 20kg purity greater than 90% above carbosulfan, after the stirring and dissolving, add the 40L Tween-80 and stir, add 20L JFC and 1L azone, stir, final products.
Embodiment 7
(1) drop into the 100L dimethyl formamide in reactor or agitator tank, add the 40L calcium dodecyl benzene sulfonate, after the stirring, add 30L OP-10 and 30L Tween-80 and stir, promptly compound emulsifying agent is standby.
(2) in another reactor or agitator tank, drop into the 400L dimethyl sulfoxide (DMSO), add 0.3kg purity and be 90% 20 (s)-camptothecines and 0.2kg purity and be 90% 10-hydroxycamptothecine, be heated to 35 ℃ and constantly stirring, fully after the dissolving, add above-mentioned compound emulsifying agent 20L, after stirring, add 5L JFC and 2L azone, stir, final products.
Embodiment 8
The purity that is added is that 90% camptothecine is 1.0kg, and purity is that 90% 10-hydroxycamptothecine is 1.0kg, and other conditions are identical with embodiment 7.
Embodiment 9
The purity that is added is that 90% camptothecine is 2.0kg, and purity is that 90% 10-hydroxycamptothecine is 2.0kg, and other conditions are identical with embodiment 7.
The embodiment 1 control paddy rice rice lice test of pesticide effectiveness and result
Be the control efficiency of 1 pair of paddy rice rice of clear and definite embodiment lice, working concentration and to the safety of paddy rice etc. has carried out the sub-district test of pesticide effectiveness in August, 2005 in the single cropping late rice in Lanxi, Zhejiang, and final report is as follows as a result:
1. material and method
1.1 reagent agent
The insecticide that embodiment 1 is prepared
1.2 contrast medicament
The clean WP of 10% aphid lice is produced by Kesheng Group Co., Ltd., Jiangsu Prov., and is commercially available
1.3 trial crops and controlling object
Trial crops is the single cropping late rice, and kind is D excellent 527; Controlling object is a paddy rice rice lice,
White back of the body rice lice Sogatella furcifera (Horvath)
Brown back rice plant hopper Nilaparvata lugens (Stdl)
Small brown-back rice plant-hopper Laodelphax striatellus (Fallen)
1.4 experimental scheme and method
1.4.1 the field design: test is carried out in the paddy field at the living family of Lanxi City Yongchang subdistrict office Bai Huang village Wu Bai, 6 processing are established in test, be respectively: 500 times, 1000 times, 2000 times, 4000 times of the insecticide dilutions of embodiment 1 preparation, the clean WP20g/667m of contrast medicament 10% aphid lice
2, repeat 3 times, totally 18 sub-districts, the sub-district area is 30m
2, district's group randomized arrangement is established guard row all around.
1.4.2 overview experimental field:
Experimental field soil property is a sandy loam, pH value 5.8, and the content of organic matter 2.95%, middle fertility, the paddy rice growing way is good, tests and does not use any insecticide in preceding 20 days.
1.4.3 spraying time and method
Test in medication on August 14, average every clump of this moment about 15 of worms are arranged, based on 1-2 age.Dispenser adopts workers and peasants-16 type manual sprayer slightly to spray, and rolls over every 667m
2Use amount of liquid medicine 50kg.
1.4.4 investigation content and method
Test respectively at medicine before, behind the medicine 1 day, 5 days, 15 days, straight line sampling of jumping in every sub-district is clapped and is looked into 20 clumps, the total borer population of record rice lice, calculate insect population go down rate, proofread and correct preventive effect.Also investigate the worm amount of small brown rice planthopper behind the medicine in 5 days, calculated preventive effect.And carry out the new multipole of Deng Kenshi poor (DMRT) significance analysis.Test is also estimated behind medicine and has been investigated the influence of dispenser to paddy growth each investigation day, and safety is investigated.
2. result of the test
2.1 correction preventive effect to total rice lice
Behind the medicine 1 day, proofread and correct preventive effects for 500 times, 1000 times, 2000 times, 4000 times of the insecticide of embodiment 1 preparation and be respectively 82.28%, 69.64%, 51.63%, 38.41%, the clean WP20g/667m of contrast medicament 10% aphid lice
2Proofreading and correct preventive effect is 54.92%.Through significance analysis, the clean WP20g/667m of 10% aphid lice
2Significantly be worse than 500 times, 1000 times of insecticide of embodiment 1 preparation, be better than 4000 times of processing of the insecticide of embodiment 1 preparation, with 2000 times of no significant differences.
Behind the medicine 5 days, each was handled preventive effect and all peaks, and proofreaies and correct preventive effects for 500 times, 1000 times, 2000 times, 4000 times of the insecticide of embodiment 1 preparation and is respectively 96.06%, 83.33%, 68.05%, 55.40%, the clean WP20g/667m of contrast medicament 10% aphid lice
2Proofreading and correct preventive effect is 73.41%.Through significance analysis, the clean WP20g/667m of contrast medicament 10% aphid lice
2Significantly be better than 4000 times of processing of the insecticide of embodiment 1 preparation,, but be lower than 500 times and 1000 times of insecticide that embodiment 1 prepares with 2000 times of no significant differences of the insecticide of embodiment 1 preparation.
Behind the medicine 15 days, each was handled preventive effect and all descends rapidly, and wherein the decrease speed of the insecticide of embodiment 1 preparation is faster than the contrast medicament.Proofread and correct preventive effect for 500 times, 1000 times, 2000 times, 4000 times of the insecticide 1 of embodiment preparation and be respectively 67.59%, 54.25%, 43.60%, 32.54%, the clean WP20g/667m of contrast medicament 10% aphid lice
2Proofreading and correct preventive effect is 54.36%.Through significance analysis, the clean WP20g/667m of 10% aphid lice
2Significantly be better than 2000 times, 4000 times processing of the insecticide of embodiment 1 preparation, suitable with 1000 times of processing, but not as 500 times of processing.
2.2 preventive effect to small brown rice planthopper
Behind the medicine 5 days, 500 times, 1000 times, 2000 times, 4000 times preventive effects of the insecticide of embodiment 1 preparation were respectively 96.27%, 85.43%, 67.42%, 38.78%, the clean WP20g/667m of contrast medicament 10% aphid lice
2Preventive effect is 88.60%, through significance analysis, above-mentioned medicament to the preventive effect of small brown-back rice plant-hopper except that 2000 times and 4000 times of the insecticide of embodiment 1 preparation hang down, the correction preventive effect of 5 days total rice lices is approaching behind 1000 times of processing and the medicine, but 500 times effect of the insecticide of embodiment 1 preparation obviously is better than contrasting medicament.
2.3 safety: each investigation day range estimation behind the medicine, medicament does not have any harmful effect to paddy growth.
It is basic identical with the insecticide that embodiment 1 prepares that the insecticide of embodiment 2, embodiment 3 preparations carries out the result of the test of the above-mentioned control paddy rice rice lice test of pesticide effectiveness.
Embodiment 1 control eggplant palm thrips result of the test
Handle:
1. reagent agent: embodiment 1 prepared insecticide dilutes 500 times
2. contrast medicament: 750 times of clean WP of 10% aphid lice
3. control efficiency
Roll over every mu and use amount of liquid medicine 75kg, 1,3,7,15 day investigation worm amount before the medicine, behind the medicine, every processing random inspection 50 leaves.The results are shown in following table:
Conclusion
Draw according to result of the test, the insecticide of embodiment 1 preparation has the better prevention effect to palm thrips, and the effect that the clean dilution of insecticidal effect that the dilution of embodiment 1 is 500 times and 10% aphid lice is 750 times is suitable.But after the dispenser medicament lasting period not long, recommend in the production using dosage for dilution 500-1000 doubly.
It is basic identical that embodiment 2, embodiment 3 prepared insecticides carry out the insecticide of the result of the test of above-mentioned control palm thrips field control effectiveness test and embodiment 1 preparation.
The control efficiency of 4 pairs of rice-stem borer medicines of embodiment
The insecticide of embodiment 4 preparations is to the control efficiency of paddy rice rice lice, every 667m
2Dosage and to the safety of paddy rice etc. was carried out the 8-9 month in 2005 the sub-district test of pesticide effectiveness in single late rice in Lanxi, Zhejiang, final report is as follows as a result:
1 material and method
1.1 reagent agent
The insecticide of embodiment 4 preparations
1.2 contrast medicament
The special SC of 5% sharp strength is produced by Bayer Hangzhou crop science Co., Ltd, and is commercially available
1.3 trial crops and controlling object
Trial crops is: late hybrid rice " two excellent trainings nine "; Controlling object is: paddy rice three generations striped rice borer (end peak), Cnaphalocrocis medinalis Guenee.
1.4 experimental scheme and method
1.4.1 the field design: test is carried out in single late rice at the living family of Lanxi City Yongchang town Bai Huang village Wu Bai.6 processing are established in test: the insecticide that is respectively embodiment 4 preparations dilutes 500 times, 1000 times, 2000 times, 4000 times, the special SC35ml/667m of contrast medicament 5% sharp strength
2And blank clear water contrast.Repeat, count 18 sub-districts, sub-district area 20m for 3 times
2, district's group randomized arrangement is established guard row all around.
1.4.2 overview experimental field:
Experimental field soil property is on the husky earth, pH value 6.2, and the content of organic matter 2.95%, middle fertility, sowing on May 26, June 18 transplanted, and the experimental field fertility is even, and rice seedling growing way balance is tested and was not used any insecticide in preceding 20 days.
1.4.3 spraying time and method
Test in medication for the first time on August 31, this moment, the peak was incubated for three generations striped rice borer (end peak) ovum in the field, and the field has the high instar larvae of a small amount of previous generation to exist.7 days range estimation fields still have adult to exist behind the medicine, so dispenser on the same day second.Dispenser adopts workers and peasants-16 type manual sprayer slightly to spray, and rolls over every 667m
2Use amount of liquid medicine 37.5kg.
1.4.4 investigation content and method
Tested September 30 and gathered in the crops preceding 7 days, 10 samplings of every sub-district straight line parallel jump, 2 clumps every, investigate 20 clumps altogether, investigation is put down in writing investigation strain number, the strain number of causing harm, is calculated cause harm rate, seedling protecting effect, and shells and look into record borer population alive, calculates the worm preventive effect of living, and carry out the new multipole of Deng Kenshi poor (DMRT) significance analysis, computational methods are carried out according to the GB/T17980.1-2000 regulation.The influence of dispenser to paddy growth investigated in also each dispenser behind medicine of test, an investigation day range estimation, and safety is investigated.
2. result of the test
500 times, 1000 times, 2000 times, 4000 times in the insecticide of 2.1 seedling protecting effect: embodiment 4 preparations, preventive effect is respectively: 85.78%, 78.19%, 66.03%, 52.72%, the special SC35ml/667m of contrast medicament 5% sharp strength
2For: 92.96%, through arcsine conversion significance analysis, all there were significant differences between each was handled exists.
500 times, 1000 times, 2000 times, 4000 times in the insecticide of worm preventive effect: embodiment 4 preparations 2.2 live, preventive effect is respectively: 87.69%, 78.11%, 66.29%, 52.42%, the special SC35ml/667m of contrast medicament 5% sharp strength
2For: 95.03%, through arcsine conversion significance analysis, all there were significant differences between each was handled exists.The worm preventive effect of living is approaching with seedling protecting effect.
2.2 safety: each dispenser behind the medicine, investigation day range estimation, medicament does not have any harmful effect to paddy growth.
3. brief summary and analysis
3.1 result of the test shows: in this experimental condition and amount ranges, the insecticide of embodiment 4 preparations is to rice safety, though preventive effect is inferior to the special SC35ml/667m of 5% sharp strength
2, but under the situation that paddy rice three generations striped rice borer in this year (end peak) is retransmitted and single cropping rice later stage rice plant is tall and big, prevent and treat, 500 times, 1000 times of working concentrations, the worm preventive effect of living, protect the leaf effect near or surpass 80%, can on producing, promote the use of.
3.2 test shows simultaneously: from overall preventive effect and Bao Ye effect, the high more preventive effect of insecticide concentration of embodiment 4 preparations is good more in this test, and the high concentration preventive effect is significantly higher than low concentration.Therefore, use general available 500 times of this chemical control rice-stem borer in the production, prevent and treat with sufficient water yield even spraying, and according to preventing and treating once every 7 days for the striped rice borer peak phase, control several times continuously according to the rice seedling size.
It is basic identical with the insecticide that embodiment 4 prepares that embodiment 5, embodiment 6 prepared insecticides carry out the result of the test of control efficiency test of above-mentioned rice-stem borer medicine.
The report of 7 pairs of controls of embodiment cabbage caterpillar field control effectiveness test
1. experimental condition:
Test and Selection is carried out in Linan, Zhejiang.The test vegetables are wild cabbage, and be early stage vegetative period, and growing way is relatively more consistent.Test all sub-district rich water quality management unanimities.
2. test is handled:
2.1 experimental scheme and arrangement:
Test medicine is the insecticide of embodiment 7 preparations; The contrast medicament is 4.5% r.
Following 5 kinds of processing are established in test:
A. the insecticide dilution of embodiment 7 preparations is 500 times; B. the insecticide dilution of embodiment 7 preparations is 1000 times; C. the insecticide dilution of embodiment 7 preparations is 2000 times; D.4.5% 45 milliliters/667m of r
2E. blank.
4 repetitions, totally 20 sub-districts are respectively established in above-mentioned 5 processing.About 17 square metres of sub-district area.Arrange all sub-districts district's group at random.
2.2 dispenser
At cabbage caterpillar 2-3 instar larvae occurrence in peak period, various medicaments are converted water respectively by the dosage of experimental scheme be made into even soup, with manual sprayer soup evenly is sprayed onto on the vegetables blade, dispenser is once during the whole test.
3. investigation records and measuring method
3.1 meteorological data:
Duration of test: no rain, 25 ℃ of mean temperature of air, 34 ℃ of the maximum air temperatures, minimum 23 ℃.
3.2 control time, number of times and method
Dispenser eve is carried out the radix investigation, carries out efficacy survey behind the medicine in 1 day, 3 days, 7 days respectively.Method: investigate the larva quantity that the cabbage caterpillar in all dish strains lives in each sub-district.Be calculated as follows control efficiency, adopt " DMRT " method to measure the preventive effect significance of difference between processing.
The drug effect computing formula:
Control efficiency (%)=[1-(ck
0Borer population * pt lives
1Borer population alive)/(ck
1Borer population * pt lives
0The borer population of living)] * 100 formulas in: ck
0Be the borer population of living before the medicine of check plot; Ck
1Be the borer population of living behind the medicine of check plot; Pt
0Be the borer population of living before the treatment region medicine; Pt
1Be the borer population of living behind the treatment region medicine.
3.3 other influences to crop
Whether the viewing test medicament produces poisoning to the test vegetables, and makes record.
4. result and analysis
4.1 control efficiency to the vegetables cabbage caterpillar
The insecticide of embodiment 7 preparations has the better prevention effect to cabbage caterpillar.Dilute 2000 times, dilute 1000 times, dilute 500 times, 1 day preventive effect is respectively 74.55%, 85.34%, 93.35% behind the medicine; 3 days preventive effect is respectively 82.94%, 92.51%, 95.58% behind the medicine; 7 days preventive effect is respectively 94.98%, 96.63%, 98.57% behind the medicine; 45 milliliters/667m of contrast medicament 4.5% r
21 day, 3 days, 7 days preventive effect is respectively 86.02%, 93.49%, 98.89% behind the medicine.
The result of variance analysis shows, behind (1) medicine 1 day, 1000 times of the insecticide dilutions of embodiment 7 preparations, the preventive effect of 500 times of two processing of dilution were suitable, and the difference between the preventive effect is not remarkable; And the preventive effect of 2000 times of the insecticide dilutions of embodiment 7 preparation significantly is worse than 45 milliliters/667m of contrast medicament 4.5% r
2Preventive effect.(2) behind the medicine 3 days, 7 days, three in the insecticide of embodiment 7 preparations was handled 45 milliliters/667m of preventive effect and contrast medicament 4.5% r
2Preventive effect suitable, three's difference is not remarkable;
4.2 side effect to vegetables
In the process of the test, undiscovered test medicine produces the phenomenon of poisoning to a variety of Chinese cabbage.
5. conclusion
Draw according to result of the test, the insecticide of embodiment 7 preparations has the better prevention effect to cabbage caterpillar, is particularly useful for the production of various organic food.But the medicament effect is slower after the dispenser, recommends using dosage for 800-1500 times of dilution in the production, uses before 3 length of times the cabbage caterpillar larva.
It is basic identical that embodiment 8, embodiment 9 prepared insecticides carry out the insecticide of the result of the test of above-mentioned control cabbage caterpillar field control effectiveness test and embodiment 7 preparations.
Embodiment 7 control cotton aphid result of the tests
Handle:
1. reagent agent: embodiment 7 prepared insecticides dilute 500 times, 1000 times
2. contrast medicament: 1000 times of 20% carbosulfan EC
3. control efficiency
3 days investigation worm amounts before the medicine, behind the medicine, every processing random inspection 50 leaves.
The results are shown in following table:
Conclusion
Draw according to result of the test, the insecticide of embodiment 7 preparations has the better prevention effect to cotton aphid, and the insecticidal effect that the dilution of embodiment 7 is 500 times is more effective than 1000 times of 20% carbosulfans; But the insecticidal effect that the dilution of embodiment 7 is 1000 times than the weak effect of 1000 times of 20% carbosulfans a bit; After the dispenser medicament lasting period not long, recommend in the production using dosage for dilution 500-1000 doubly.
It is basic identical that embodiment 8, embodiment 9 prepared insecticides carry out the insecticide of the result of the test of above-mentioned control cotton aphid field control effectiveness test and embodiment 7 preparations.
Claims (7)
1. insecticide that contains camptothecine or camptothecin derivative is characterized in that containing: camptothecine or derivatives thereof 0.01～5.00%, and emulsifier 0.5～20%, bleeding agent 0.5～20%, surplus is an organic solvent;
Described camptothecin derivative is 9-nitrocamptothecin, 9-aminocamptothecin, 10-hydroxycamptothecine, 10,11-methylene-dioxy-nitrocamptothecin, Fluoroethylcamptothederivatives, 10-alkoxy camptothecin or 9-nitro-20-camptothecine;
Described emulsifier is one or more the mixture in Tween-80, OP-10, the calcium dodecyl benzene sulfonate;
Described bleeding agent is JFC or azone;
Described organic solvent is one or more the mixture in dimethyl sulfoxide (DMSO), dimethyl formamide, propyl alcohol, isopropyl alcohol, ethylene glycol, ethanol, methyl alcohol, ether, chloroform toluene, acetone, benzene,toluene,xylene and the propylene glycol.
2. a kind of insecticide that contains camptothecine or camptothecin derivative as claimed in claim 1 is characterized in that containing: camptothecine or derivatives thereof 0.05～2.5%, emulsifier 1～10%, bleeding agent 1～10%.
3. a kind of insecticide that contains camptothecine or camptothecin derivative as claimed in claim 1 is characterized in that containing: camptothecine or derivatives thereof 0.1～1%, emulsifier 2～5%, bleeding agent 2～5%.
4. a kind of insecticide that contains camptothecine or camptothecin derivative as claimed in claim 1 is characterized in that also containing insecticide fluorine worm nitrile, Imidacloprid or carbosulfan 2～40%.
5. a kind of insecticide that contains camptothecine or camptothecin derivative as claimed in claim 4 is characterized in that containing fluorine worm nitrile, Imidacloprid or carbosulfan 5～20%.
6. a kind of insecticide that contains camptothecine or camptothecin derivative as claimed in claim 4 is characterized in that containing fluorine worm nitrile, Imidacloprid or carbosulfan 8～15%.
7. as claim 1 or 2 or 3 described a kind of method for producing insecticide that contain camptothecine or camptothecin derivative, it is characterized in that comprising the following steps:
1) in reactor or agitator tank, adds solvent by said ratio, in this solvent, add the camptothecine or derivatives thereof, be heated to 20～60 ℃ and constantly stirring, to dissolving fully;
2) add emulsifier again, after stirring, add bleeding agent or high bleeding agent, stir, get finished product, promptly contain the insecticide of camptothecine or camptothecin derivative.
8. as claim 4 or 5 or 6 described a kind of method for producing insecticide that contain camptothecine or camptothecin derivative, it is characterized in that comprising the following steps:
1) in reactor or agitator tank, adds solvent by said ratio, in this solvent, add the camptothecine or derivatives thereof, be heated to 20～60 ℃ and constantly stirring, after the dissolving, add insecticide more extremely fully, stir;
2) add emulsifier again, after stirring, add bleeding agent, stir, get finished product, promptly contain the insecticide of camptothecine or camptothecin derivative.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1843128B (en) * | 2006-05-17 | 2011-05-25 | 浙江林学院 | Method for directly processing pesticide using Camptotheca acuminata |
| CN100579372C (en) * | 2006-05-31 | 2010-01-13 | 浙江林学院 | Agricultural bactericide containing camptothecin or camptothecin derivative and application thereof |
| CN100592871C (en) * | 2008-03-14 | 2010-03-03 | 浙江林学院 | Insecticide composition and its processing method |
| CN102764216A (en) * | 2012-07-20 | 2012-11-07 | 福建金雷防虫害技术有限公司 | Natural plant innoxious mosquito expelling perfume |
| CN103275095B (en) * | 2013-05-08 | 2015-07-22 | 中国农业科学院植物保护研究所 | 10-hydroxycamptothecine derivatives and applications thereof |
| CN104725390B (en) * | 2013-12-20 | 2017-04-05 | 兰州大学 | A kind of camptothecine compounds and preparation method thereof and the purposes in pesticide |
| CN103931667B (en) * | 2014-04-08 | 2015-09-09 | 许银亚 | Frankincense vaporizer mosquito liquid |
| CN105010427A (en) * | 2015-04-30 | 2015-11-04 | 新昌县大成生物科技有限公司 | Botanical rice thrips repellent |
| CN110037042B (en) * | 2019-05-15 | 2021-01-01 | 江苏省中国科学院植物研究所 | Application of camptothecin in preventing and treating rice blast |
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