CN105076234A - Preparation process of botanical insecticide capable of preventing and treating maize weevil - Google Patents
Preparation process of botanical insecticide capable of preventing and treating maize weevil Download PDFInfo
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- CN105076234A CN105076234A CN201510511002.1A CN201510511002A CN105076234A CN 105076234 A CN105076234 A CN 105076234A CN 201510511002 A CN201510511002 A CN 201510511002A CN 105076234 A CN105076234 A CN 105076234A
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- red clover
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- 0 COc(cc1)ccc1C1=COc2cc(O)ccc2C1=* Chemical compound COc(cc1)ccc1C1=COc2cc(O)ccc2C1=* 0.000 description 1
- TZBJGXHYKVUXJN-UHFFFAOYSA-N Oc(cc1)ccc1C1=COc2cc(O)cc(O)c2C1=O Chemical compound Oc(cc1)ccc1C1=COc2cc(O)cc(O)c2C1=O TZBJGXHYKVUXJN-UHFFFAOYSA-N 0.000 description 1
Abstract
The invention discloses a botanical insecticide capable of preventing and treating maize weevil. The main ingredient of the botanical insecticide capable of preventing and treating maize weevil is a trifolium pratense extract. A trifolium pratense botanical pesticide provided by the invention has obvious contact toxicity on stored grain insects, is beneficial to human health, is environment-friendly and is low in pesticide resistance generation possibility. In addition, the botanical insecticide is rich in plant resources and simple in preparation process and has favorable development and application prospects in the aspect of protecting the grain safety.
Description
Technical field
The present invention relates to its preparation technology of plant insecticide of a kind of control of maize elephant, belong to biological pesticide technical field.
Background technology
Grain is important strategic materials, has important effect to economic development, national security and social stability.In the cereal that the whole world newly gathers in the crops every year, the significant loss caused because of storage pest is about 15%, and some developing countries do not catch up with because of technical merit, human and material resources less investment, not in time, the loss caused is up to 25% [1-2] for early prevention and treatment measures.China be in the world topmost product grain and consumption big country, in recent years, the grain annual production of China has reached 5,000 hundred million kilograms, and quantity in stock accounts for the over half of annual production.Grain storage pest not only causes mass loss, also reduces the edible quality of grain storage, processing quality, kind quality and technological quality; Shorten warehouse service life; Propagate pathogenic microorganisms, harm people's is healthy simultaneously.
Plant insecticide has draws materials easily, processes easy to use, can pest control and low to people, animal toxicity effectively, and the feature of use safety, can not pollute grain and environment, not killed natural enemies, insect not easily develops immunity to drugs.It had both been applicable to the grain storage of large-scale national treasury, was applicable to again peasant household's small lot grain storage.Therefore, effective plant insecticide is found significant for the control carrying out reserves insect.
Corn weevil is one of most important kind in grain storage pest, and under current means of prevention, antichemical protection agent and fumigant create stronger resistance.In the study on prevention of grain storage pest, vegetable insecticide rises for the research of the target pests such as corn weevil.Find in early-stage Study, the various plants such as composite family, Lauraceae, Cupressaceae all have corn weevil certain to walk quickly and keep away, contact toxicity.But because plant resources is abundant not, or activity is not very desirable, a lot of research fails to obtain further achievement, and does not mostly all determine active chemical components wherein.
Summary of the invention
The invention provides the plant insecticide of a kind of control of maize elephant of good disinsection effect;
Another object of the present invention is to provide the preparation method of the plant insecticide of above-mentioned control of maize elephant.
Object of the present invention carrys out specific implementation by the following technical programs:
A plant insecticide for control of maize elephant, its main component is red clover extract.
Preferably, the plant insecticide of control of maize elephant, its main component is one or more the combination in the ethyl acetate extract extract of red clover extract, petroleum ether part extract or aqueous phase position extract.
Best, the plant insecticide of control of maize elephant, its main component is the ethyl acetate extract extract of red clover extract.Through experimental verification, the ethyl acetate extract extract adopting red clover extract is the plant insecticide of main component as control of maize elephant, compared with the better effects if of other parts extract.
The main active of the plant insecticide of control of maize elephant is onocerin and genistein.
The preparation technology of the plant insecticide of above-mentioned control of maize elephant, the preparation method of described red clover extract is as follows:
Gather fresh red clover Plant aboveground position, dry in the shade after pulverizing, add ethanol water, ultrasonic or heating and refluxing extraction, extract reduced pressure concentration obtains medicinal extract, then dries at ventilation lucifugal place, obtained red clover extract, i.e. red clover extract according to claim 1.
Preferably, described ethanol water, addition is 10-50 times of dry powder volume, and ethanol water concentration is 20-100wt%; Ultrasonic or heating and refluxing extraction 10-90 minute.
Above-mentioned with the preparation technology of the plant insecticide of the extract of the red clover extract control of maize elephant that is main component, comprise the steps:
1) preparation of red clover extract;
2) preparation at red clover different activities position
A. the preparation of red clover petroleum ether part extract: by the water-soluble solution of red clover extract, add benzinum again, thermal agitation, stratification, supernatant is petroleum ether layer, and lower aqueous solution benzinum re-extract 2-5 time, merges petroleum ether layer, reduced pressure concentration, obtained red clover petroleum ether part extract;
B. the preparation of red clover ethyl acetate extract extract: add ethyl acetate in the aqueous solution after petroleum ether extraction, thermal agitation, stratification, supernatant is ethyl acetate layer, lower aqueous solution ethyl acetate re-extract 2-5 time, combined ethyl acetate layer, reduced pressure concentration, obtained red clover ethyl acetate extract extract;
C. the preparation of red clover aqueous phase position extract: by remaining aqueous solution after extraction into ethyl acetate, reduced pressure concentration, obtained red clover aqueous phase position extract.
Preferably, described step 2) step a in, the red clover extract distilled water of its 2-20 times volume dissolves.
Preferably, described step 2) step a in, add the benzinum of red clover extract 2-10 times of volume.
Preferably, described step 2) step b in, add the ethyl acetate of aqueous solution 2-10 times volume in the aqueous solution after petroleum ether extraction.
The plant insecticide of control of maize elephant provided by the invention, the vegetable material of employing is red clover, and it is the multi-functional good forage of pulse family, has extensive plantation in the whole world.The isoflavones components wherein contained, has estrogen-like action, and for treatment diabetes, cancer, particularly women's phase syndrome, has positive effect.The ethyl acetate extract utilizing this plant to prepare is at 49 μ g/cm
2concentration under, just up to more than 80%, good development prospect can be had to the contact toxicity of corn weevil.
The present invention simultaneously also its main active clear and definite is onocerin and genistein.Through experimental verification, red clover ethyl acetate extract has extraordinary insecticidal activity.Utilize the separation means such as column chromatography chromatogram, recrystallization, be separated from ethyl acetate extract and obtain two kinds of compounds.Measured by Modern spectroscopy technology, identify that these two compounds are isoflavonoid, be respectively onocerin (formononetin, hereinafter referred to as FOR) and genistein (genistein, hereinafter referred to as GEN).Activity determination result shows, these two compounds also have obvious contact toxicity to reserves insect, LC
50be respectively 0.295 and 0.273 μm of ol/cm
2.
Red clover botanical pesticide provided by the invention, not only has obvious action of contace poison to grain storage pest, not easily develops immunity to drugs, and environmentally friendly, harmless.In addition, this plant resources enriches, and preparation technology is simple, in protection grain security, have good development prospect.
Embodiment
First it may be noted that embodiments of the invention only disclose preferred embodiment several, not should be appreciated that paired restriction of the invention process, protection scope of the present invention is still as the criterion with the content disclosed in claims.
The preparation at embodiment 1 red clover different activities position
1, the preparation of red clover extract: the position, ground gathering fresh red clover plant, dries in the shade, and pulverizes.Add 20 times of volume ethanol, ultrasonic extraction 30 minutes, repeat extraction 3 times.By Extraction solvent reduced pressure concentration, obtain medicinal extract, at ventilation lucifugal place, dry, obtain red clover extract.
2, the preparation at red clover different activities position: get obtained red clover extract 20g, dissolves with the distilled water 100mL of 5 times of volumes, and add 3 times in aqueous to the benzinum 300mL of aqueous solution volume, thermal agitation, stratification, supernatant is petroleum ether layer; Re-extract 3 times, merges petroleum ether layer, reduced pressure concentration, obtained red clover petroleum ether part.To add the ethyl acetate 300mL of 3 times of volumes, thermal agitation in remaining aqueous solution after petroleum ether extraction, stratification, supernatant is ethyl acetate layer, re-extract 3 times, combined ethyl acetate layer, reduced pressure concentration, obtained red clover ethyl acetate extract.Remaining aqueous solution after extracting, reduced pressure concentration, obtained red clover aqueous phase position.
Embodiment 2 different activities position is to the insecticidal activity of corn weevil
Namely insecticide obtains preparation: take the benzinum of above-mentioned preparation, ethyl acetate and aqueous phase different activities site material 10-15mg, the acetone solution added respectively containing 10% distilled water is mixed with the mother liquor of 12.5mg/mL concentration, with distilled water, mother liquor is diluted to successively the solution of 6.25,3.125,1.25 and 0.625mg/mL again, add the surfactant JFC (C7 ~ C9 alkanol APEO) of medicine liquid volume 1%, mix and obtain insecticide.Different component insecticide to the contact efficacy of corn weevil in table 1.
From table 1, the activity at our known red clover ethyl acetate and aqueous phase position is all higher than petroleum ether part.Wherein, at 49 μ g/cm
2under concentration, after 96h process, ethyl acetate extract is to the contact toxicity of corn weevil just up to 82%, and the activity of aqueous phase is 59%.In addition, aqueous phase position has better activity, and the ratio also for improving water in extract and dosing in further development and application red clover insecticide process provides possibility, is conducive to reducing producing and use cost, and safer environmental protection.
Table 1 red clover different activities position is to the contact toxicity of corn weevil
The tracking of embodiment 3 insecticidal active compound is separated
Activity Results shows, red clover ethyl acetate extract activity is the strongest.Therefore, further separation and purification has been carried out to ethyl acetate extract.Get ethyl acetate extract 10g, sample is mixed with silica gel 10g, upper 100g silicagel column, use benzinum 300mL successively, benzinum: acetone (100:1) solution 300mL, benzinum: acetone (50:1) solution 300mL, benzinum: acetone (10:1) solution 500mL, benzinum: acetone (2:1) solution 300mL, benzinum: acetone (1:1) solution 300mL, acetone 100mL wash-out, is compared by thin-layer chromatographic analysis, merge similar compositions, obtain A-H8 component.Carry out repeatedly continuous print silica gel column chromatography to wherein component D to be separated, utilize sephadex to carry out purifying, recrystallization obtains compound F 17-hydroxy-corticosterone OR.Carry out repeatedly continuous print silica gel column chromatography to wherein component E to be separated, utilize sephadex to carry out purifying, obtain compound GEN.
Utilize nuclear magnetic resonance technique and mass spectrum, identify that these two active components are respectively onocerin (Formononetin) and genistein (Genistein), chemical structural formula is:
Its structured data is as follows:
FOR: colourless acicular crystal.ESI-MS provides [M+H]
+m/z269.0805.
1H-NMR(400M，DMSO-d
6)δ：8.34(1H,s,H-2),7.97(1H,d,J＝8.0Hz,H-5),7.51(2H,d,J＝8.0Hz,H-2’,H-6’),6.98(2H,d,J＝8.0Hz,H-3’,H-5’),6.93(1H,dd,J＝8.0,4.0Hz,H-6),6.87(1H,d,J＝4.0Hz,H-8),3.79(3H,s,4’-OCH
3)。
GEN: colourless acicular crystal.ESI-MS provides [M+H]
+m/z271.0440.
1H-NMR(400M，DMSO-d
6)δ：12.96(1H,s,5-OH),10.88(1H,s,7-OH),9.58(1H,s,4’-OH),8.32(1H,s,H-2),7.38(2H,d,J＝12.0Hz,H-2’,H-6’),6.82(2H,d,J＝12.0Hz,H-3’,H-5’),6.39(1H,brs,H-8),6.23(1H,brs,H-6)。
Active testing result shows (table 2), and compound F 17-hydroxy-corticosterone OR and GEN all has obvious contact toxicity to corn weevil, after their process corn weevil 96h (table 3), and LC
50be respectively 79.06 μ g/cm
2(0.295 μm of ol/cm
2) and 73.83 μ g/cm
2(0.273 μm of ol/cm
2).Compared with ethyl acetate extract, activity is more weak, and this phenomenon is followed the tracks of separation at vegetable active and detected also comparatively common.These two compounds possible mix in certain proportion in plant extracts, have synergistic effect, thus the insecticidal activity that performance is stronger.
Table 2 red clover reactive compound is to the contact toxicity of corn weevil
Table 3 reactive compound is to the contact toxicity of corn weevil process after 96 hours
From above example, the insecticide utilizing red clover to prepare has good contact toxicity to corn weevil, especially ethyl acetate extract, and preparation technology is simple, and cost is cheap.Meanwhile, red clover, as the plant resource health care medicinal useful to human body, food security has advantageous advantage.Prepared by the present invention red clover insecticide by grain reserves, transport in there is important application prospect.
Finally being also pointed out that any entity or individual use or implement technical scheme of the present invention is all to infringement of the present invention, and any entity or individual, without the permission of the applicant, can not implement this patent separately.And any entity or individual are subject to inspiration of the present invention or implement through simple adjustment, also should think the protection domain of this patent.
Claims (10)
1. a plant insecticide for control of maize elephant, is characterized in that: its main component is red clover extract.
2. the plant insecticide of control of maize elephant according to claim 1, is characterized in that: its main component is one or more the combination in the ethyl acetate extract extract of red clover extract, petroleum ether part extract or aqueous phase position extract.
3. the plant insecticide of control of maize elephant according to claim 2, is characterized in that: its main component is the ethyl acetate extract extract of red clover extract.
4. the plant insecticide of control of maize elephant according to claim 3, is characterized in that: main active is onocerin and genistein.
5. the preparation technology of the plant insecticide of control of maize elephant according to claim 1, is characterized in that: the preparation method of described red clover extract is as follows:
Gather fresh red clover Plant aboveground position, dry in the shade after pulverizing, add ethanol water, ultrasonic or heating and refluxing extraction, extract reduced pressure concentration obtains medicinal extract, then dries at ventilation lucifugal place, obtained red clover extract, i.e. red clover extract according to claim 1.
6. the preparation technology of the plant insecticide of control of maize elephant according to claim 5, is characterized in that: described ethanol water, and addition is 10-50 times of dry powder volume, and ethanol water concentration is 20-100wt%; Ultrasonic or heating and refluxing extraction 10-90 minute.
7. the preparation technology of the plant insecticide of the control of maize elephant according to Claims 2 or 3, is characterized in that: comprise the steps:
1) preparation of red clover extract;
2) preparation at red clover different activities position
A. the preparation of red clover petroleum ether part extract: by the water-soluble solution of red clover extract, add benzinum again, thermal agitation, stratification, supernatant is petroleum ether layer, and lower aqueous solution benzinum re-extract 2-5 time, merges petroleum ether layer, reduced pressure concentration, obtained red clover petroleum ether part extract;
B. the preparation of red clover ethyl acetate extract extract: add ethyl acetate in the aqueous solution after petroleum ether extraction, thermal agitation, stratification, supernatant is ethyl acetate layer, lower aqueous solution ethyl acetate re-extract 2-5 time, combined ethyl acetate layer, reduced pressure concentration, obtained red clover ethyl acetate extract extract;
C. the preparation of red clover aqueous phase position extract: by remaining aqueous solution after extraction into ethyl acetate, reduced pressure concentration, obtained red clover aqueous phase position extract.
8. the preparation technology of the plant insecticide of control of maize elephant according to claim 7, is characterized in that: described step 2) step a in, the red clover extract distilled water of its 2-20 times volume dissolves.
9. the preparation technology of the plant insecticide of control of maize elephant according to claim 7, is characterized in that: described step 2) step a in, add the benzinum of red clover extract 2-10 times of volume.
10. the preparation technology of the plant insecticide of control of maize elephant according to claim 7, is characterized in that: described step 2) step b in, add the ethyl acetate of aqueous solution 2-10 times volume in the aqueous solution after petroleum ether extraction.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112790199A (en) * | 2019-11-14 | 2021-05-14 | 兰州大学 | Botanical insecticide for preventing and treating corn weevil and preparation process thereof |
| CN113994966A (en) * | 2021-10-22 | 2022-02-01 | 上海市农业科学院 | Application of genistein in preparation of insect virus synergist and synergist |
Citations (3)
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|---|---|---|---|---|
| WO2006048201A1 (en) * | 2004-11-03 | 2006-05-11 | Universita' Degli Studi Di Milano | Clover extracts for the preparation of insecticidal agents |
| CN101547605A (en) * | 2006-11-29 | 2009-09-30 | 拜尔农作物科学股份公司 | Insecticidal active ingredient combinations (formononetins + insecticides) |
| CN101610672A (en) * | 2007-01-16 | 2009-12-23 | 先正达参股股份有限公司 | Pesticide combination |
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2015
- 2015-08-19 CN CN201510511002.1A patent/CN105076234B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006048201A1 (en) * | 2004-11-03 | 2006-05-11 | Universita' Degli Studi Di Milano | Clover extracts for the preparation of insecticidal agents |
| CN101547605A (en) * | 2006-11-29 | 2009-09-30 | 拜尔农作物科学股份公司 | Insecticidal active ingredient combinations (formononetins + insecticides) |
| CN101610672A (en) * | 2007-01-16 | 2009-12-23 | 先正达参股股份有限公司 | Pesticide combination |
Non-Patent Citations (1)
| Title |
|---|
| S.F.WANG ETAL: ""ROLE OF ISOFLAVONOIDS IN RESISTANCE OF SUBTERRANEAN CLOVER TRIFOLIATES TO THE REDLEGGED EARTH MITE HALOTYDEUS DESTRUCTOR"", 《JOURNAL OF CHEMICAL ECOLOGY》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112790199A (en) * | 2019-11-14 | 2021-05-14 | 兰州大学 | Botanical insecticide for preventing and treating corn weevil and preparation process thereof |
| CN113994966A (en) * | 2021-10-22 | 2022-02-01 | 上海市农业科学院 | Application of genistein in preparation of insect virus synergist and synergist |
| CN113994966B (en) * | 2021-10-22 | 2023-03-10 | 上海市农业科学院 | Application of genistein in preparation of insect virus synergist and synergist |
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