CN104026159B - A kind of preparation method of plant insecticide - Google Patents
A kind of preparation method of plant insecticide Download PDFInfo
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- CN104026159B CN104026159B CN201410323238.8A CN201410323238A CN104026159B CN 104026159 B CN104026159 B CN 104026159B CN 201410323238 A CN201410323238 A CN 201410323238A CN 104026159 B CN104026159 B CN 104026159B
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- extract
- benzinum
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- giant knotweed
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Abstract
The present invention relates to a kind of preparation method of plant insecticide, be with giant knotweed flower for raw material, pulverize through cracker, extract with methanol eddy, extract is concentrated into dry total extract, and total extract first uses the ultrasonic extraction of benzinum, use the ultrasonic extraction of ether again, obtain ether extract.Wherein ether extract crosses silica gel column chromatography, and with benzinum and acetone mixed solvent wash-out, namely eluent reduced pressure concentration obtains giant knotweed flower pesticide product.This product has good toxic action to lucilia sericata adult.This extract belongs to botanical pesticide, has people, animal safety, free from environmental pollution, not easily causes pesticide resistance, is easy to the advantages such as degraded in natural environment.
Description
(1) technical field
The present invention relates to a kind of preparation method of plant insecticide, belong to botanical pesticide development field.
(2) background technology
Lucilia sericata (Luciliasericata) is namely notorious " mung bean fly ", is a kind of Calliphoridae insect, is distributed widely in the American-European each continent, Asia and Africa except the Antarctic Continent, South America.Lucilia sericata is near settlement and one of field Kinds of Flies, and adult scope of activities is extremely wide, and normal discrepancy crowd lives in concentrated communities part.Larva has corpse feeding habits, is mainly originated in stench corrupt material as places such as corpse, fish, shrimp, rubbish, also can breeds in pig manure and animal feed.Lucilia sericata is very long for breeding period, and female fly is liked laying eggs at places such as running sore, wound, corrupt spoils.The various diseases such as dysentery, typhoid fever, cholera, tuberculosis can be propagated.Also usually attack sheep, birds etc., cause the myiasis of domestic animal and poultry, have very large harm to livestock breeding.The current control to fly class is substantially based on chemical control.As everyone knows, use chemical agent Control pests, be a kind of method that effect and efficiency are all very high, ratio for input and output is also very high.But the high toxicity of the high residue of organochlorine insecticide and some organophosphorus compounds and carbamate insecticide is shown great attention to by people, the particularly puzzlement that brings environmental quality of organochlorine insecticide, causes most attention.
Along with deepening continuously of Pesticide Science research, botanical pesticide achieves tremendous development in recent years, and it has people, animal safety, free from environmental pollution, not easily causes pesticide resistance, is easy to the advantages such as degraded in natural environment.Botanical pesticide mainly comprise extract from plant active component, plant itself and by active structure synthesis compound and derivative.As realized the nimbin that industrialization is produced, the secondary metabolite obtained from Meliaceae plant print chinaberry exactly; Now widely used natural insecticide-chrysanthemum ester insecticide modifies from the pyrethrin feverfew Dalmatian chrysanthemum to develop.Therefore from natural products, find novel agrochemical, become one of initiative and the important channel producing novel pesticide.
Giant knotweed (PolygonumcuspidatumSieb.etZucc.) is polygonaceae giant knotweed platymiscium, main containing Anthraquinones and talan constituents.There is dampness removing removing jaundice, clearing heat and detoxicating, blood stasis removing analgesic, relieving cough and reducing sputum effect.Be mainly used in jaundice with damp-heat pathogen, stranguria with turbid discharge, under band, arthralgia due to wind-dampness, carbuncle sore tumefacting virus, scald, through Bi ， Disorder lump in the abdomen, traumatic injury, the diseases such as cough with lung heat.A kind of common Chinese medicine.But relevant giant knotweed is in botanical pesticide, particularly the insecticidal activity aspect of giant knotweed flower has no report.
(3) summary of the invention
In order to solve the problem, the invention provides a kind of preparation method of plant insecticide; Object is to provide a kind of preparation method of giant knotweed flower extract and the application of extract thereof.
A preparation method for plant insecticide, is get dry giant knotweed flower, pulverizes, cross 40 mesh sieves with cracker, extract giant knotweed and spend 3 times, each 6h, extract merging with the methanol eddy of 3 ~ 6 times of giant knotweeds flower weight, is concentrated into dry total extract.Then use the ultrasonic extraction total extract of the benzinum of 5 ~ 8 times of total extract weight 3 times, each 0.5h, remove impurity; Use the ultrasonic extraction total extract of the ether of 5 ~ 8 times of total extract weight 3 times again, each 0.5h, merge extract and obtain ether extract.With the acetone solution ether extract of ether extract 1 ~ 3 times of weight, upper silica gel column chromatography (200-300 object silica gel will rinse through the benzinum of 3 column volumes in advance), then wash-out is carried out with benzinum and acetone mixing as eluant, eluent, eluent reduced pressure concentration is dry, obtain giant knotweed flower pesticide product; Described benzinum: the volume ratio of acetone is 50:1 ~ 2:1.
By above-mentioned pesticide product acetone solution, solution preparation becomes a series of liquor strength, evenly be added on 1.8g cotton balls with dropper, then cotton balls is positioned over 50 DEG C of oven dry in baking oven, cotton balls after oven dry by 8ml concentration be again 10% sucrose solution rayon balls is soaked after, be put in 1000ml triangular flask, every bottle graft enters lucilia sericata adult 30.Take acetone soln as contrast, often process repetition 3 times.The lethality of statistics 10h.
At present study more botanical pesticide in the world and mainly contain the compositions such as nimbin, rotenone, pyrethrin, nicotine, matrine, wherein nimbin and pyrethrin and their derivative be with fastest developing speed, product at most, the most successful botanical pesticide of research.But all in all, the investigation and application of botanical pesticide is just in the primary stage (botanical pesticide accounts for about 1% of global agrochemical market) compared with chemical pesticide.Under the food security situation of current rigorous, Devoting Major Efforts To Developing and promote the environmental-friendly plant source pesticide of efficient, micro-poison be ensure food safety, an important channel of agricultural sustainable development.
(4) embodiment
Embodiment 1
Giant knotweed flower insecticide of the present invention is prepared according to the following step:
1. the flower of the giant knotweed after 40 mesh sieves meal 100g was got;
2. by the giant knotweed flower meal methyl alcohol of its 3 times of weight refluxing extraction 3 times under 85 DEG C of conditions, each 6h, merges extract, is evaporated to dry giant knotweed flower total extract 8.4g;
3. by step, 2. middle total extract is first with the ultrasonic extraction of the benzinum of its 5 times of weight 3 times, and each 0.5h, removes impurity; Again with the ultrasonic extraction of the ether of its 5 times of weight 3 times, each 0.5h, merges extract and obtains ether extract;
4. by the step 3. middle 0.29g ether extract obtained 5ml acetone solution also upper silica gel column chromatography, for preventing impurity from disturbing, silicagel column rinses with the benzinum of 150ml in advance.Then be that the benzinum of 20:1 and acetone mixed solution 300ml carry out wash-out by volume ratio, eluent reduced pressure concentration obtains giant knotweed flower pesticide product.
5. get step 4. in the pesticide product acetone of gained be mixed with a series of liquor strength (0.2,0.4,0.8,1.6,3.2mg/ml), be evenly added on 1.8g cotton balls with dropper, then cotton balls is positioned in baking oven and dries (50 DEG C), cotton balls after oven dry is put in 1000ml triangular flask after being soaked by rayon balls with 10% sucrose solution that 8ml concentration is again, and every bottle graft enters lucilia sericata adult 30.Take acetone soln as contrast, often process repetition 3 times.The lethality of statistics 10h.IC after measured
50(lethal concentration of 50) value is 1.3mg/ml.
Example 2
Took the flower of the giant knotweed after 40 mesh sieves meal 150g, by the methyl alcohol of giant knotweed flower meal 5 times of weight refluxing extraction 3 times under 88 DEG C of conditions, each 5h, merges extract, is evaporated to dry giant knotweed flower total extract.
By the total extract ultrasonic extraction of the benzinum of its 6 times of weight 3 times, each 0.5h, removes impurity; Again with the ultrasonic extraction of the ether of its 6 times of weight 3 times, each 0.5h, merges extract and obtains ether extract; Get 0.44g ether extract 6ml acetone solution and upper silica gel column chromatography, for preventing impurity from disturbing, silicagel column rinses with the benzinum of 150ml in advance.Then be that the benzinum of 5:1 and acetone mixed solution 300ml carry out wash-out by volume ratio, eluent reduced pressure concentration obtains giant knotweed flower pesticide product.This product acetone is mixed with a series of liquor strength (0.2,0.4,0.8,1.6,3.2mg/ml), be evenly added on 1.8g cotton balls with dropper, then cotton balls is positioned over 50 DEG C of oven dry in baking oven, cotton balls after oven dry by 8ml concentration be again 10% sucrose solution rayon balls is soaked after, be put in 1000ml triangular flask, every bottle graft enters lucilia sericata adult 30.Take acetone soln as contrast, often process repetition 3 times.The lethality of statistics 10h.IC after measured
50(lethal concentration of 50) value is 1.7mg/ml.
Claims (1)
1. a preparation method for plant insecticide, is characterized in that getting dry giant knotweed flower, pulverizes, cross 40 mesh sieves with cracker, extracts giant knotweed and spends 3 times, each 6h, extract merging with the methanol eddy of 3 ~ 6 times of giant knotweeds flower weight, is concentrated into dry total extract; Then use the ultrasonic extraction total extract of the benzinum of 5 ~ 8 times of total extract weight 3 times, each 0.5h, remove impurity; Remove total extract after impurity 3 times with ultrasonic extraction of the ether of 5 ~ 8 times of total extract weight again, each 0.5h, merges extract and obtains ether extract; With the acetone solution ether extract of ether extract 1 ~ 3 times of weight, upper silica gel column chromatography, 200-300 object silicagel column will rinse through the benzinum of 3 column volumes in advance, then wash-out is carried out with benzinum and acetone mixing as eluant, eluent, eluent reduced pressure concentration is dry, obtain giant knotweed flower pesticide product; Described benzinum: the volume ratio of acetone is 50:1 ~ 2:1.
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| CN201410323238.8A CN104026159B (en) | 2014-07-08 | 2014-07-08 | A kind of preparation method of plant insecticide |
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| CN201410323238.8A CN104026159B (en) | 2014-07-08 | 2014-07-08 | A kind of preparation method of plant insecticide |
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| CN104026159A CN104026159A (en) | 2014-09-10 |
| CN104026159B true CN104026159B (en) | 2016-03-30 |
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| CN107595714A (en) * | 2017-10-31 | 2018-01-19 | 广东丸美生物技术股份有限公司 | A kind of Gentrin Knotweed P.E and preparation method thereof and the application in cosmetics |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1450077A (en) * | 2003-04-22 | 2003-10-22 | 上海大学 | Method for extracting polygonum cuspidatum tannic acid |
| WO2007145655A1 (en) * | 2006-06-09 | 2007-12-21 | Guthy-Renker Corporation | Pain relief composition |
| CN101397242A (en) * | 2007-09-28 | 2009-04-01 | 张博钧 | Technique for extracting and purifying resveratrol from fresh giant knotweed rhizome |
| CN101870640A (en) * | 2010-07-08 | 2010-10-27 | 贵州师范大学 | Method for preparing resveratrol extract from giant knotweed and product |
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2014
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1450077A (en) * | 2003-04-22 | 2003-10-22 | 上海大学 | Method for extracting polygonum cuspidatum tannic acid |
| WO2007145655A1 (en) * | 2006-06-09 | 2007-12-21 | Guthy-Renker Corporation | Pain relief composition |
| CN101397242A (en) * | 2007-09-28 | 2009-04-01 | 张博钧 | Technique for extracting and purifying resveratrol from fresh giant knotweed rhizome |
| CN101870640A (en) * | 2010-07-08 | 2010-10-27 | 贵州师范大学 | Method for preparing resveratrol extract from giant knotweed and product |
Non-Patent Citations (2)
| Title |
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| 从虎杖中同时提取分离白藜芦醇和蒽醌类工艺研究;徐顶巧 等;《食品与发酵工业》;20120630;第38卷(第6期);224-228 * |
| 静态顶空进样气质联用法测定虎杖花地头香成分;孙印石 等;《中药材》;20120229;第35卷(第2期);241-243 * |
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