CN101336644A - Plant insecticide prepared by humulus and its preparing process horehound - Google Patents
Plant insecticide prepared by humulus and its preparing process horehound Download PDFInfo
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- CN101336644A CN101336644A CNA2008100138092A CN200810013809A CN101336644A CN 101336644 A CN101336644 A CN 101336644A CN A2008100138092 A CNA2008100138092 A CN A2008100138092A CN 200810013809 A CN200810013809 A CN 200810013809A CN 101336644 A CN101336644 A CN 101336644A
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- humulus grass
- plant insecticide
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Abstract
The invention provides a botanical pesticide made from Japanese Hop and a preparation method thereof. The botanical pesticide with required concentration can be prepared by the following steps:drying root, stem, leaf or whole plant of Japanese Hop in shade; grinding and drying to obtain dry Japanese Hop powder; extracting with 10 times by mass of acetone as an extraction solvent; decompress concentrating and drying to obtain a dry extract sample; extracting with petroleum ether, trichloromethane and ethyl acetate which have different polarity; Dissolving petroleum ether extract with acetone. According to the invention, the botanical pesticide has the advantages of wide material source, low production cost, favorable comprehensive insect control effect, no environmental pollution and low residual in production, no harm to crops and safety for human beings and animals. In a word, it is a nuisance-free botanical pesticide.
Description
Technical field
The present invention relates to plant insecticide of humulus grass exploitation and preparation method thereof, belong to the botanical pesticide technical field, be exclusively used in the humulus grass and be developed as plant insecticide.
Background technology
Along with the raising day by day of environmental protection cry, a large amount of uses of high toxicity agricultural chemicals have caused worldwide extensive concern to the negative effect that agricultural production and ecotope cause.For environment and the agriculture sustainable development of protecting human survival; the development of agricultural chemicals is subjected to environment and ecological restriction with use with strictness; botanical pesticide because of its have nuisanceless, the mode of action is unique, with advantages such as the good and development cost of environment compatibility are low, be the focus of China's chemistry of pesticide and pesticide toxicology research so utilize the abundant plant resource explorations of China to study novel pesticide always.
The humulus grass is named again and uproots plants after their edible portions have been harvested, and for the dry aerial parts of moraceae plants humulus grass Humulus Scandens (Lour) Merr. etc., its stolon growth spreads rapidly, often is wrapped on crops or the fruit tree, has a strong impact on the growth of other plant.Be annual or perennial evergreen voluble herb, it is many to reach 4m.The close living delavay raspberry herb of stem branch and petiole, the stem light green has vertical rib.The nearly kidney shape pentagon of leaf, diameter 7～10cm, palmate 5 drastic cracks, rare is 3 or 7 to split, anxious point of tip or point gradually, the base portion heart, there is the rough sawn tooth at the edge, the leaf two coarse bristle of looking unfamiliar, fall flowering, spend little, the fruit ear green, similar pinecone shape, achene is spherical little flat.The property happiness half cloudy environment, cold-resistant, drought resisting, happiness fertilizer, well-drained rich soil, the rapid humulus grass of growth rate adaptability is strong, various environment are suitable growth all, the whole nation is widely distributed, aboundresources, raw material are easy to get, stable yield has good industrialization prospect.。Herb contains cyanidenon, glycoside, choline, asparagine and volatile oil, tanning, resin; Cone contains humulone and lupulones; Leaf contains cosmosiin, Vitex negundo var cannabifolia element.Have clearing hectic heat, the treating stranguria function of detoxifcation, be used to the polydipsia of generating heat, the hectic fever hectic fever due to yin, frequent micturition is anxious logical; Pruitus is controlled in external application.Except that Xinjiang and Qinghai, all there is distribution in urban district, national each province, and at part provinces and regions hyoscine.Hubei Tujia is called " big half-capitate hemiboea herb ", also is used for the treatment of urinary tract infections, diarrhoea, accumulation of food in the stomach and intes tine due to indigestion, cough heating; The external application treating snakebite.Zhuang is called " thunder ", washes the affected part with the herb decocting and controls eczema.The method of this extraction provided by the invention and separation and purification humulus grass insecticidal active ingredient belongs to initiative.
Summary of the invention
Technical problem: the purpose one of this research provides a kind of safe, economic and non-harmful natural plants insecticide and preparation method thereof, the 2nd, this plant resources of development and use humulus grass.
Technical scheme: the plant insecticide of humulus grass exploitation is characterized in that this plant insecticide is to be prepared from by the following method:
(1) pulverize: dry in the shade after the humulus grass is cleaned, oven dry is pulverized the back and is crossed 40 mesh sieves, obtains humulus grass dry powder;
(2) extract: the dry powder that weighing prepares, the benzinum, benzene, chloroform, ethyl acetate, acetone, the ethanol that are equipped with about 10 times of quality extract as extracting solvent, get each solvent crude extract;
(3) concentrate: utilize active the tracking to determine the optimum extraction solvent, then the optimum solvent extract is evaporated to the thick paste shape in rotary evaporator, obtain paste extract;
(4) extraction: paste extract is molten with 10 times of hydro-thermals, extract with polarity different organic solvent benzinum, chloroform, ethyl acetate then, get the different medicinal extract of polarity, utilize active the tracking to determine best extractant again.
Best extract is promptly obtained the plant insecticide of desired concn with the proper amount of acetone dissolving.
The optimum extraction solvent is an acetone among the above-mentioned preparation method; Best extractant is a chloroform.
Beneficial effect: plant insecticide of humulus grass provided by the present invention exploitation and preparation method thereof is compared with existing method, has the following advantages;
(1) be raw material with the sweeping humulus grass that distributes, raw material sources are wide, and are cheap, and production cost is low, and production technology is simple, is suitable for various large-scale production.
(2) the desinsection resultant effect is good.Experiment showed, that this medicament all has desirable control efficiency to diamond-back moth, cotten aphid.
(3) preparation method is simple, and dna purity is higher
(4) non-environmental-pollution in the production, low-residual, harmless to crop, to the person poultry safety, be a kind of nuisance-free plant insecticide, can be used for the production of organic food.
(5) fully developed widespread this plant resources of humulus grass.
Embodiment
Adopt cold-maceration extraction, concentrated, the liquid-liquid extraction of rotary evaporation.
(1) raw material is handled: gather fresh humulus grass, dry in the shade and put to constant temperature oven after cleaning and dry by the fire to the material embrittlement under 50 ℃, with multifunctional crusher it is pulverized, and make dry powder by 40 mesh sieves, be sealed in the plastic sack standby;
(2) extract: accurately take by weighing dry powder 20g or take by weighing as required, soak 4-5d/ time down in 25 ℃ with the different solvent of 6 kinds of polarity such as benzinum, benzene, chloroform, ethyl acetate, acetone, ethanol respectively, continuous lixiviate 3 times merges 3 times filtrate for later use;
(3) concentrate: extract is evaporated to the thick paste shape in rotary evaporator, obtains paste extract, press 1g dry powder/mL concentration, get the different solvents crude extract, place 4 ℃ of refrigerators to preserve standby mensuration desinsection biologically actives each extract acetone diluted;
(4) extraction: behind the selected good optimum extraction solvent of desinsection biologicall test, extract in a large number with said method with this solvent, get optimum solvent extract dry sample, the distilled water that this dry sample is added 10 times of amounts, thermosol, pack in the separatory funnel, adopt liquid-liquid apportion design, respectively extract 3 times with benzinum, chloroform, ethyl acetate successively.At last these extracts and remaining aqueous solution are evaporated to the thick paste shape, and weigh, get the different medicinal extract of polarity.Best extract is promptly got the plant insecticide of desired concn with the proper amount of acetone dissolving.
Select the embodiment of optimum extraction solvent to see embodiment 1,2,3; Select the embodiment of best extractant to see embodiment 4.
Embodiment 1 each crude extract is to the action of contace poison of diamond-back moth examination worm
Cabbage leaves is put into insect box in right amount, get 30 of diamond-back moth examination in 2 ages worms, place and soak the worm cover, immerse respectively in the different solvent crude extract of polarity, take out after 6 seconds, polypide is dried to be placed on the cabbage leaves and feeds, and immerses in the aqueous acetone solution of corresponding concentration in contrast with the examination worm respectively, repeat 3 times, write down 24,48 hours examination worm lethality.
Can get by result's (seeing Table 1): in 6 kinds of solvent extraction liquid, benzinum, benzene, chloroform extract insecticidal activity are relatively poor, and all below 30%, and acetone, ethanol, acetic acid ethyl acetate extract are better active, especially best with acetone extract, 48h examination worm lethality reaches 86.7%.
(333mg dry powder/mL) is to the action of contace poison of diamond-back moth for table 1 different solvents crude extract
Embodiment 2 each crude extract are to the food refusal effect of diamond-back moth examination worm
With card punch fresh cabbage leaves being broken into diameter is 3 centimetres leaf dish, put into 100mg/mL again and soak i.e. taking-up in 8 seconds for the acetone soln that tries the extraction sample, after treating that the leaf dish dries, put it into (interior pad filter paper in the culture dish of 9 centimetres of diameters, adding a small amount of distilled water preserves moisture), each culture dish is put into 3 and is handled leaf dish (contrast is 5), inserts 2 hours diamond-back moth examination in 2 ages worm of 2 hunger.Every processing repeats 10 times, calculates the food refusal rate with squared paper measuring and calculating leaf dish area in 24,48 hours.
Can be analyzed by the result and to draw, each extract is all not high to the antifeedant activity of diamond-back moth under for examination concentration, all below 30%.
Table 2 different solvents extract is to the food refusal effect (%) of diamond-back moth
Embodiment 3 each crude extract are to the action of contace poison of aphid
Adopt and carry aphid blade infusion process.Cultivate cotton seedling in the greenhouse with nutrient solution, every glass two strain, connect aptery one-tenth aphid in the every strain of cotyledon period and count head, treat nearly hundred of two leaf period natural propagations, reject younger ones in an age group if aphid, if only surplus 3 ages are aphid and aptery one-tenth aphid, to be diluted to variable concentrations with 0.1% lauryl sodium sulfate aqueous solution (this solution has emulsification to extract) for the examination extract, take out cotton seedling and in soup, dipped for 5 seconds, inhale the unnecessary soup of defoliation edge with blotting paper, the aphid number of counting immediately on the cauline leaf is insect population radix before handling, every glass is a repetition, and every processing repeats 3 times, is contrast with the acetone soln after diluting with 0.1% lauryl sodium sulfate aqueous solution, in handling back 24,48h record survival aphid number calculates aphid lethality (%).
Each solvent crude extract all has the effect of well tagging (the results are shown in Table 3) to cotten aphid.Acetone, ethanol, ethyl acetate, chloroform crude extract are under 50mg/mL concentration, preventive effect is all more than 59.6%, also active best with the acetone crude extract wherein, 24h, 48h cotton aphid mortality are respectively 76.8%, 85.6% under the 50mg/mL concentration, and cotton aphid mortality is respectively 82.6%, 92.5% under the 100mg/mL concentration.
6 kinds of solvent extraction liquid of table 3 are to the action of contace poison of aphid
Embodiment 4 each extract are to the action of contace poison of diamond-back moth
After going out humulus grass optimum extraction solvent and be acetone by above experimental selection,, adopt liquid liquid apportion design that active ingredient is carried out separation and purification then with a large amount of effective component extractings of acetone, three kinds of solvent extracts, diamond-back moth contact toxicity assay method is the same.
As can be seen from Table 4, the best extractant of humulus grass active ingredient is a chloroform, contains a small amount of active ingredient in the petroleum ether extraction liquid, contains effective composition in the acetic acid ethyl acetate extract hardly.When concentration was 25mg/mL, chloroform, benzinum and acetic acid ethyl acetate extract diamond-back moth 48h lethality were respectively 76.7%, 20.0% and 10.0%.
Table 4 different solvents extract is to the action of contace poison of diamond-back moth
Comprehensively show: humulus grass dry powder acetone crude extract all has good contact toxicity to diamond-back moth, cotten aphid, is ethanol, ethyl acetate crude extract secondly; In further separation and purification active component process, best extractant is a chloroform, and concentration diamond-back moth 48h lethality when 50mg/mL can reach 93.3%.
Claims (4)
1, plant insecticide of humulus grass exploitation and preparation method thereof is characterized in that this plant insecticide is to be prepared from by the following method:
(1) pulverize: dry in the shade after the humulus grass is cleaned, oven dry is pulverized the back and is crossed 40 mesh sieves, obtains humulus grass dry powder;
(2) extract: the dry powder that weighing prepares, the benzinum, benzene, chloroform, ethyl acetate, acetone, the ethanol that are equipped with quality and are 10 times extract as extracting solvent, extract;
(3) concentrate: extract is evaporated to the thick paste shape in rotary evaporator, obtains paste extract;
(4) extraction: medicinal extract is molten with 10 times of hydro-thermals, adopts liquid-liquid apportion design to select for use benzinum, chloroform, ethyl acetate to extract, and gets the different medicinal extract of polarity;
(5) take by weighing the medicinal extract acetone solution, can be made into the plant insecticide of desired concn.
2, according to the plant insecticide of the described humulus grass of claim 1 exploitation, it is characterized in that the dry powder raw material can be selected independent Radix humuli scandentis, humulus grass blade or humulus blade of grass sheet for use, also can select humulus grass complete stool.
3, according to the plant insecticide of the described humulus grass of claim 1 exploitation, it is characterized in that the optimum extraction solvent is an acetone among the preparation method.
4, according to the plant insecticide of the described humulus grass of claim 1 exploitation, it is characterized in that best extractant is a chloroform among the preparation method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100138092A CN101336644A (en) | 2008-01-04 | 2008-01-04 | Plant insecticide prepared by humulus and its preparing process horehound |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CNA2008100138092A CN101336644A (en) | 2008-01-04 | 2008-01-04 | Plant insecticide prepared by humulus and its preparing process horehound |
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| CN101336644A true CN101336644A (en) | 2009-01-07 |
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| CNA2008100138092A Pending CN101336644A (en) | 2008-01-04 | 2008-01-04 | Plant insecticide prepared by humulus and its preparing process horehound |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103621585A (en) * | 2013-12-23 | 2014-03-12 | 滨州市智和生产力促进中心 | Pesticide for killing aphides and preparation method thereof |
| CN104086322A (en) * | 2014-06-17 | 2014-10-08 | 沈阳药科大学 | Biologic pesticide |
| CN104920480A (en) * | 2015-06-03 | 2015-09-23 | 杜杭华 | Botanical insecticide and preparation method thereof |
| CN105475385A (en) * | 2016-01-28 | 2016-04-13 | 济南思拓新源医药科技有限公司 | Method for preparing Chinese-chive-maggot-preventing pesticide through biogas slurry |
| CN106613155A (en) * | 2016-11-22 | 2017-05-10 | 蚌埠市涂山绿园蔬菜科研专业合作社 | Fragrant-flowered garlic planting method |
| CN109392959A (en) * | 2018-11-15 | 2019-03-01 | 乐山师范学院 | It is a kind of to prevent and treat natural drug composition and its application for occupying bamboo puppet angle aphid |
| CN113785845A (en) * | 2021-09-18 | 2021-12-14 | 河南省林业科学研究院 | Plant extract with antibacterial effect and application thereof |
| RU2786708C1 (en) * | 2021-11-23 | 2022-12-23 | федеральное государственное бюджетное образовательное учреждение высшего образования "Мичуринский государственный аграрный университет" | Method for producing a powder from dried cones of humulus lupulus in the uhf field |
-
2008
- 2008-01-04 CN CNA2008100138092A patent/CN101336644A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103621585A (en) * | 2013-12-23 | 2014-03-12 | 滨州市智和生产力促进中心 | Pesticide for killing aphides and preparation method thereof |
| CN103621585B (en) * | 2013-12-23 | 2015-03-11 | 滨州市智和生产力促进中心 | Pesticide for killing aphides and preparation method thereof |
| CN104086322A (en) * | 2014-06-17 | 2014-10-08 | 沈阳药科大学 | Biologic pesticide |
| CN104086322B (en) * | 2014-06-17 | 2016-03-02 | 沈阳药科大学 | A kind of biological pesticide |
| CN104920480A (en) * | 2015-06-03 | 2015-09-23 | 杜杭华 | Botanical insecticide and preparation method thereof |
| CN104920480B (en) * | 2015-06-03 | 2018-04-13 | 周瑜 | A kind of plant insecticide and preparation method thereof |
| CN105475385A (en) * | 2016-01-28 | 2016-04-13 | 济南思拓新源医药科技有限公司 | Method for preparing Chinese-chive-maggot-preventing pesticide through biogas slurry |
| CN105475385B (en) * | 2016-01-28 | 2018-08-17 | 芜湖航天特种电缆厂股份有限公司 | A method of preparing the pesticide of prevention bradysia odoriphaga using biogas slurry |
| CN106613155A (en) * | 2016-11-22 | 2017-05-10 | 蚌埠市涂山绿园蔬菜科研专业合作社 | Fragrant-flowered garlic planting method |
| CN109392959A (en) * | 2018-11-15 | 2019-03-01 | 乐山师范学院 | It is a kind of to prevent and treat natural drug composition and its application for occupying bamboo puppet angle aphid |
| CN113785845A (en) * | 2021-09-18 | 2021-12-14 | 河南省林业科学研究院 | Plant extract with antibacterial effect and application thereof |
| RU2786708C1 (en) * | 2021-11-23 | 2022-12-23 | федеральное государственное бюджетное образовательное учреждение высшего образования "Мичуринский государственный аграрный университет" | Method for producing a powder from dried cones of humulus lupulus in the uhf field |
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Open date: 20090107 |