CN107484778A - A kind of insecticide containing Tea Saponin and preparation method thereof - Google Patents
A kind of insecticide containing Tea Saponin and preparation method thereof Download PDFInfo
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- CN107484778A CN107484778A CN201710931507.2A CN201710931507A CN107484778A CN 107484778 A CN107484778 A CN 107484778A CN 201710931507 A CN201710931507 A CN 201710931507A CN 107484778 A CN107484778 A CN 107484778A
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- Prior art keywords
- insecticide
- tea saponin
- extract
- safflower
- tea
- Prior art date
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- 239000002917 insecticide Substances 0.000 title claims abstract description 57
- 239000001397 quillaja saponaria molina bark Substances 0.000 title claims abstract description 49
- 229930182490 saponin Natural products 0.000 title claims abstract description 49
- 150000007949 saponins Chemical class 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000000284 extract Substances 0.000 claims abstract description 82
- 244000020518 Carthamus tinctorius Species 0.000 claims abstract description 54
- 235000003255 Carthamus tinctorius Nutrition 0.000 claims abstract description 54
- 235000012771 pancakes Nutrition 0.000 claims abstract description 19
- 239000002904 solvent Substances 0.000 claims abstract description 16
- 239000004094 surface-active agent Substances 0.000 claims abstract description 10
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 90
- 238000000605 extraction Methods 0.000 claims description 41
- 239000000706 filtrate Substances 0.000 claims description 34
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 32
- 239000000243 solution Substances 0.000 claims description 28
- 239000000843 powder Substances 0.000 claims description 24
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 17
- 235000013311 vegetables Nutrition 0.000 claims description 17
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 14
- 239000007864 aqueous solution Substances 0.000 claims description 11
- 239000003960 organic solvent Substances 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 239000012046 mixed solvent Substances 0.000 claims description 7
- 230000006837 decompression Effects 0.000 claims description 4
- 239000008213 purified water Substances 0.000 claims description 4
- 150000002148 esters Chemical class 0.000 claims description 2
- 230000002147 killing effect Effects 0.000 abstract description 13
- 239000000126 substance Substances 0.000 abstract description 9
- 235000013305 food Nutrition 0.000 abstract description 8
- 241000196324 Embryophyta Species 0.000 abstract description 6
- 239000004480 active ingredient Substances 0.000 abstract description 4
- 231100000614 poison Toxicity 0.000 abstract description 4
- 239000003905 agrochemical Substances 0.000 abstract description 3
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- 230000036541 health Effects 0.000 abstract description 3
- 230000009471 action Effects 0.000 abstract description 2
- 230000015556 catabolic process Effects 0.000 abstract description 2
- 238000006731 degradation reaction Methods 0.000 abstract description 2
- 239000002574 poison Substances 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 231100000704 bioconcentration Toxicity 0.000 abstract 1
- 231100000481 chemical toxicant Toxicity 0.000 abstract 1
- 239000003440 toxic substance Substances 0.000 abstract 1
- 238000010992 reflux Methods 0.000 description 19
- 241001122767 Theaceae Species 0.000 description 18
- 230000000052 comparative effect Effects 0.000 description 13
- 238000001914 filtration Methods 0.000 description 13
- 238000010438 heat treatment Methods 0.000 description 12
- 239000003643 water by type Substances 0.000 description 12
- 241000238631 Hexapoda Species 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 241000607479 Yersinia pestis Species 0.000 description 4
- 201000010099 disease Diseases 0.000 description 4
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 4
- 238000005238 degreasing Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- XYIBRDXRRQCHLP-UHFFFAOYSA-N ethyl acetoacetate Chemical compound CCOC(=O)CC(C)=O XYIBRDXRRQCHLP-UHFFFAOYSA-N 0.000 description 3
- 239000000575 pesticide Substances 0.000 description 3
- WWNNZCOKKKDOPX-UHFFFAOYSA-N N-methylnicotinate Chemical compound C[N+]1=CC=CC(C([O-])=O)=C1 WWNNZCOKKKDOPX-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000006071 cream Substances 0.000 description 2
- 239000012043 crude product Substances 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- IYRMWMYZSQPJKC-UHFFFAOYSA-N kaempferol Chemical compound C1=CC(O)=CC=C1C1=C(O)C(=O)C2=C(O)C=C(O)C=C2O1 IYRMWMYZSQPJKC-UHFFFAOYSA-N 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 230000007096 poisonous effect Effects 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 229930024421 Adenine Natural products 0.000 description 1
- GFFGJBXGBJISGV-UHFFFAOYSA-N Adenine Chemical compound NC1=NC=NC2=C1N=CN2 GFFGJBXGBJISGV-UHFFFAOYSA-N 0.000 description 1
- 240000002791 Brassica napus Species 0.000 description 1
- 235000006008 Brassica napus var napus Nutrition 0.000 description 1
- 241000209507 Camellia Species 0.000 description 1
- 244000025254 Cannabis sativa Species 0.000 description 1
- 235000009024 Ceanothus sanguineus Nutrition 0.000 description 1
- UBSCDKPKWHYZNX-UHFFFAOYSA-N Demethoxycapillarisin Natural products C1=CC(O)=CC=C1OC1=CC(=O)C2=C(O)C=C(O)C=C2O1 UBSCDKPKWHYZNX-UHFFFAOYSA-N 0.000 description 1
- 206010059866 Drug resistance Diseases 0.000 description 1
- GQODBWLKUWYOFX-UHFFFAOYSA-N Isorhamnetin Natural products C1=C(O)C(C)=CC(C2=C(C(=O)C3=C(O)C=C(O)C=C3O2)O)=C1 GQODBWLKUWYOFX-UHFFFAOYSA-N 0.000 description 1
- 241000255777 Lepidoptera Species 0.000 description 1
- 240000003553 Leptospermum scoparium Species 0.000 description 1
- 235000015459 Lycium barbarum Nutrition 0.000 description 1
- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 241000282806 Rhinoceros Species 0.000 description 1
- PEFASEPMJYRQBW-HKWQTAEVSA-N Robinin Chemical compound O[C@@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@H]1OC[C@@H]1[C@H](O)[C@H](O)[C@@H](O)[C@H](OC=2C(C3=C(O)C=C(O[C@H]4[C@@H]([C@H](O)[C@@H](O)[C@H](C)O4)O)C=C3OC=2C=2C=CC(O)=CC=2)=O)O1 PEFASEPMJYRQBW-HKWQTAEVSA-N 0.000 description 1
- 210000001015 abdomen Anatomy 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 229960000643 adenine Drugs 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 230000001887 anti-feedant effect Effects 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- IRUJZVNXZWPBMU-UHFFFAOYSA-N cartap Chemical compound NC(=O)SCC(N(C)C)CSC(N)=O IRUJZVNXZWPBMU-UHFFFAOYSA-N 0.000 description 1
- 239000013043 chemical agent Substances 0.000 description 1
- OEYIOHPDSNJKLS-UHFFFAOYSA-N choline Chemical compound C[N+](C)(C)CCO OEYIOHPDSNJKLS-UHFFFAOYSA-N 0.000 description 1
- 229960001231 choline Drugs 0.000 description 1
- 235000018597 common camellia Nutrition 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- OEBRKCOSUFCWJD-UHFFFAOYSA-N dichlorvos Chemical compound COP(=O)(OC)OC=C(Cl)Cl OEBRKCOSUFCWJD-UHFFFAOYSA-N 0.000 description 1
- 229950001327 dichlorvos Drugs 0.000 description 1
- MCWXGJITAZMZEV-UHFFFAOYSA-N dimethoate Chemical compound CNC(=O)CSP(=S)(OC)OC MCWXGJITAZMZEV-UHFFFAOYSA-N 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 239000000686 essence Substances 0.000 description 1
- 150000002191 fatty alcohols Chemical class 0.000 description 1
- 229930003944 flavone Natural products 0.000 description 1
- 150000002213 flavones Chemical class 0.000 description 1
- 235000011949 flavones Nutrition 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000001990 intravenous administration Methods 0.000 description 1
- -1 is mixed Uniformly Substances 0.000 description 1
- IZQSVPBOUDKVDZ-UHFFFAOYSA-N isorhamnetin Chemical compound C1=C(O)C(OC)=CC(C2=C(C(=O)C3=C(O)C=C(O)C=C3O2)O)=C1 IZQSVPBOUDKVDZ-UHFFFAOYSA-N 0.000 description 1
- 235000008800 isorhamnetin Nutrition 0.000 description 1
- 235000008777 kaempferol Nutrition 0.000 description 1
- MWDZOUNAPSSOEL-UHFFFAOYSA-N kaempferol Natural products OC1=C(C(=O)c2cc(O)cc(O)c2O1)c3ccc(O)cc3 MWDZOUNAPSSOEL-UHFFFAOYSA-N 0.000 description 1
- DDELFAUOHDSZJL-UHFFFAOYSA-N kaempferol 3-O-rutinoside-7-O-rhamnoside Natural products OC1C(O)C(O)C(C)OC1OC1C(O)C(O)C(CO)OC1OC1=C(C=2C=CC(O)=CC=2)OC2=CC(OC3C(C(O)C(O)C(C)O3)O)=CC(O)=C2C1=O DDELFAUOHDSZJL-UHFFFAOYSA-N 0.000 description 1
- PEFASEPMJYRQBW-UHFFFAOYSA-N kaempferol 7-O-alpha-L-rhamnopyradoside 3-O-beta-rutinoside Natural products OC1C(O)C(O)C(C)OC1OCC1C(O)C(O)C(O)C(OC=2C(C3=C(O)C=C(OC4C(C(O)C(O)C(C)O4)O)C=C3OC=2C=2C=CC(O)=CC=2)=O)O1 PEFASEPMJYRQBW-UHFFFAOYSA-N 0.000 description 1
- 235000012054 meals Nutrition 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- UXOUKMQIEVGVLY-UHFFFAOYSA-N morin Natural products OC1=CC(O)=CC(C2=C(C(=O)C3=C(O)C=C(O)C=C3O2)O)=C1 UXOUKMQIEVGVLY-UHFFFAOYSA-N 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 150000002966 pentacyclic triterpenoids Chemical class 0.000 description 1
- 239000000419 plant extract Substances 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- PEFASEPMJYRQBW-XMWKPCQISA-N robinin Natural products O(C[C@@H]1[C@H](O)[C@H](O)[C@@H](O)[C@H](OC2=C(c3ccc(O)cc3)Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@@H](O)[C@@H](C)O4)c3)C2=O)O1)[C@H]1[C@@H](O)[C@@H](O)[C@@H](O)[C@H](C)O1 PEFASEPMJYRQBW-XMWKPCQISA-N 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/02—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms
- A01N43/04—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom
- A01N43/14—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom six-membered rings
- A01N43/16—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom six-membered rings with oxygen as the ring hetero atom
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
- A01N65/08—Magnoliopsida [dicotyledons]
- A01N65/20—Fabaceae or Leguminosae [Pea or Legume family], e.g. pea, lentil, soybean, clover, acacia, honey locust, derris or millettia
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Zoology (AREA)
- Agronomy & Crop Science (AREA)
- Plant Pathology (AREA)
- Dentistry (AREA)
- Wood Science & Technology (AREA)
- Environmental Sciences (AREA)
- Biotechnology (AREA)
- Microbiology (AREA)
- Mycology (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Pest Control & Pesticides (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a kind of insecticide containing Tea Saponin, the insecticide is made up of the component of following percentage by weight：Tea Saponin 1.5~2.0%, safflower dish extract 0.8~1.2%, surfactant 1.0~1.3%, surplus is solvent；And provide its preparation method.The active ingredient of insecticide of the present invention is extracted to obtain from tea-seed pancake and safflower dish, is a kind of plant insecticide, and environmental pollution is small, environment-friendly；Preparation method is simple compared with chemical insecticide, avoids a large amount of difficult degradations, the generation of toxic chemical substance in chemical synthesis；The insecticide easily biological-degradable of the present invention, greatly reduces residual quantity of the agricultural chemicals on plant, avoids bioconcentration from being endangered by food chain to caused by health；Killing ability to Parametrites theae is remarkably reinforced after Tea Saponin and safflower dish extract are used in combination, and produces food refusal and action of contace poison to Parametrites theae, 72h killing rates are up to more than 65%.
Description
Technical field
The invention belongs to technical field of insecticide, in particular it relates to which a kind of contain the insecticide of Tea Saponin and its preparation side
Method.
Background technology
Chemical insecticide is a kind of poisonous chemical agent, with the pest and disease damages of crops, trees just can be killed on a small quantity, or it is right
Material impact occurs for the physiologically active of pest and disease damage.The advantages of chemical insecticide is that use cost is low, quick, wide in variety, preventing and treating
Object is wide.For shortcoming to be polluted to environment, the agricultural chemicals of residual causes the residual in food by the inspissation of food chain
Accumulation, it is enriched with vivo after people is edible, threatens the health and lives of the mankind, easily trigger major disease, such as cancer；Insect is easy
Produce drug resistance.
Parametrites theae, Lepidoptera, Jian Chi moths section, host have tea, oil tea and camellia, mainly eat into young sprout at the top of food tea tree with larva
Cause harm, cause young sprout withered, influence tea yield.Medicine currently used for Parametrites theae preventing and treating mainly has 40% Rogor, 80% enemy
1500 times of liquid of dichlorvos emulsion, 1500 times of liquid of 2.5% 3000 times of uranus missible oil liquid and 50% Padan's pulvis, these medicines are generally deposited
The shortcomings that chemical insecticide described above.
The content of the invention
First purpose of the present invention is to overcome drawbacks described above, there is provided a kind of insecticide containing Tea Saponin, this is killed
The active ingredient of worm agent is plant extracts, has the advantages of environmental pollution is small, degradable.
Second object of the present invention is to provide above-mentioned method for producing insecticide.
This what the 3rd purpose is to provide the application of above-mentioned insecticide.
The purpose of the present invention implements by the following technical programs：
A kind of insecticide containing Tea Saponin, the insecticide are made up of the component of following percentage by weight：Tea Saponin 1.5
~2.0%, safflower dish extract 0.8~1.2%, surfactant 1.0~1.3%, surplus are solvent.
Preferably, the insecticide is made up of the component of following percentage by weight：Tea Saponin 1.8%, safflower dish
Extract 1.0%, surfactant 1.1%, surplus are solvent.
Further, the surfactant includes C8-C10 AEOs.
Further, the solvent is the aqueous solution of 8~10wt% containing esters.
The above-mentioned method for producing insecticide containing Tea Saponin, specifically comprises the following steps：
(1) preparation of Tea Saponin
Tea-seed pancake crushes, and carries out secondary back extraction to tea-seed pancake powder with ethanol water, extract solution is concentrated under reduced pressure
Medicinal extract is made, dissolved in purified water is added into the medicinal extract, then with ether and ethyl acetate mixed extractant solvent, collects organic
Solvent layer solution, anhydrous magnesium sulfate is added into obtained organic solvent layer solution, is stood after stirring, filtered, obtain
Filtrate decompression concentration, dry, obtain Tea Saponin；
(2) preparation of safflower dish extract
Safflower vegetable plot upper part is dried, and crushes, secondary back extraction, extract solution are carried out to safflower vegetable powder with ethanol water
It is concentrated under reduced pressure and medicinal extract is made, dissolved in purified water is added into the medicinal extract, is then extracted with ethyl acetate, collects ethyl acetate
Layer, anhydrous magnesium sulfate is added to ethyl acetate layer, is stood after stirring, is filtered, obtained filtrate decompression is concentrated, dried, and is obtained
Safflower dish extract；
(3) preparation of insecticide
The Tea Saponin that step (1) obtains and the safflower dish extract that step (2) obtains are taken, is sequentially added in solvent, is mixed
Uniformly, surfactant is then added, is sufficiently mixed uniformly, produces insecticide.
Further, in the step (1), volume fraction of ethanol 50~70% in the ethanol water；
Ethanol water volume is 8~10 times of tea-seed pancake powder weight when extracting for the first time, and extraction time is 4~6h,
Ethanol water volume is 6~8 times of tea-seed pancake powder weight during second of extraction, and extraction time is 2~3h；
Described be concentrated under reduced pressure is carried out under -0.07~-0.08Mpa.
Further, in the step (1), the dosage of pure water is 8~10 times of medicinal extract weight；
The volume ratio of the in the mixed solvent ether and ethyl acetate is 1：3~4；
Mixed extractant solvent 3~4 times, the dosage of mixed solvent is 3~4 times of medicinal extract weight during extraction；
The time of repose is 20~24h.
Further, in the step (2), volume fraction of ethanol 50~70% in the ethanol water；
Ethanol water volume is 8~10 times of safflower vegetable powder weight when extracting for the first time, and extraction time is 3~5h, the
Ethanol water volume is 6~8 times of tea-seed pancake powder weight during second extraction, and extraction time is 2~3h；
Described be concentrated under reduced pressure is carried out under -0.07~-0.08Mpa.
Further, in the step (2), the dosage of pure water is 8~10 times of medicinal extract weight；
Extraction is carried out 3~4 times, and the dosage of ethyl acetate is 3~4 times of medicinal extract weight during extraction；
The time of repose is 20~24h.
The above-mentioned insecticide containing Tea Saponin is used to prevent and treat Parametrites theae.
Tea Saponin also known as TS, it is from plant of theaceae seed, as extracted in the tea cake after tea seed cake, tea seeds oil expression
Vegetable insecticide, active ingredient belongs to pentacyclic triterpenoid, and bitter is pungent, the organic solvent such as soluble in water, alcohols, right
Insect, which has, to tag and Antifeedant Effects.Tea Saponin or a kind of natural nonionic surface active agent, there is good emulsification, divide
The functions such as scattered, foaming, moistening.
Safflower dish, belong to pulse family, safflower colza, containing a variety of flavones ingredients：Quercetinglycosides, apiolin, Isorhamnetin, wood
Rhinoceros grass element, robinin, Kaempferol, additionally contains the compositions such as trigonelline, choline, adenine, simple safflower dish extract
Killing ability is weaker.
AEO (AEO), belongs to nonionic surfactant, be by polyethylene glycol and fatty alcohol condensation and
Into ether.
The present invention is carried out refluxing extraction to tea-seed pancake and safflower dish respectively, is prepared into using ethanol water as solution
To Tea Saponin and the crude product of safflower dish extract, using the crude product of Tea Saponin and safflower dish extract as insecticide it is effective into
Point, killing ability to insect Parametrites theae is remarkably reinforced after Tea Saponin and safflower dish extract are used in combination.
The invention has the advantages that：
(1) active ingredient of insecticide of the present invention is extracted to obtain from tea-seed pancake and safflower dish, is a kind of vegetable source pesticide
Agent, environmental pollution is small, environment-friendly；
(2) preparation method is simple compared with chemical insecticide, avoids a large amount of difficult degradation, poisonous chemicals in chemical synthesis
The generation of matter；
(3) insecticide easily biological-degradable of the invention, greatly reduces residual quantity of the agricultural chemicals on plant, avoids biological richness
Collection acts through food chain and endangered to caused by health；
(4) the killing ability after Tea Saponin and safflower dish extract are used in combination to Parametrites theae is remarkably reinforced, to Parametrites theae
Food refusal and action of contace poison are produced, 72h killing rates are up to more than 65%.
Embodiment
The preferred embodiments of the present invention are illustrated below, it will be appreciated that preferred embodiment described herein is only used
In the description and interpretation present invention, it is not intended to limit the present invention.
Raw material in the embodiment of the present invention is that market can obtain product.
Embodiment 1
A kind of method for producing insecticide, preparation method are as follows：
(1) tea-seed pancake after degreasing of extracting oil is crushed, weighs tea seed cake powder 200g, be put into refluxing extraction equipment, add
Enter 1800g 60vt% ethanol waters, to tea-seed pancake powder heating and refluxing extraction 5h, filtrate is collected by filtration, add again into filter residue
Enter 1400g 60vt% ethanol waters, filtrate is collected by filtration in heating and refluxing extraction 3h, and filtrate merges to obtain tea seed extract solution.
Extract solution heats concentration under the conditions of -0.07~-0.08Mpa and medicinal extract is made, and the pure water of 10 times of its weight is added into medicinal extract
Dissolving, then with volume ratio 1:4 ether and ethyl acetate mixed extractant solvent, extract 4 times, each mixed solvent dosage is leaching
3 times of cream weight.Organic solvent layer solution is collected, is merged, is added anhydrous magnesium sulfate into organic solvent layer solution, stir
After stand 24h, filter, collect filtrate, filtrate is concentrated under reduced pressure under the conditions of -0.07~-0.08Mpa, is dried to solid-like, obtains tea
Saponin.
(2) safflower vegetable plot upper part is dried, crushes, weigh safflower vegetable powder 200g, be put into refluxing extraction equipment, added
1800g 60vt% ethanol waters, to safflower vegetable powder heating and refluxing extraction 4h, filtrate is collected by filtration, is added into filter residue
Filtrate is collected by filtration in 1400g 60vt% ethanol waters, heating and refluxing extraction 3h, and filtrate merges to obtain safflower dish extract solution.Carry
Take liquid to heat concentration under the conditions of -0.07~-0.08Mpa and medicinal extract is made, the pure water-soluble of 10 times of its weight is added into medicinal extract
Solution, is then extracted with ethyl acetate, and extracts 4 times, and each ethyl acetate dosage is 3 times of medicinal extract weight.Collect ethyl acetate layer,
Merge, add anhydrous magnesium sulfate, 24h is stood after stirring, filter, collect filtrate, filtrate is in -0.07~-0.08Mpa conditions
Under be concentrated under reduced pressure, be dried to solid-like, obtain safflower dish extract.
(3) Tea Saponin 1.8g and safflower dish extract 1.0g obtained above is weighed, sequentially adds 96.1g second containing 10wt%
In the aqueous solution of acetoacetic ester, it is well mixed, then adds 1.1g C8-C10 AEOs, is sufficiently mixed uniformly, i.e.,
Obtain insecticide.
Embodiment 2
A kind of method for producing insecticide, preparation method are as follows：
(1) tea-seed pancake after degreasing of extracting oil is crushed, weighs tea seed cake powder 200g, be put into refluxing extraction equipment, add
Enter 1600g 70vt% ethanol waters, to tea-seed pancake powder heating and refluxing extraction 6h, filtrate is collected by filtration, add again into filter residue
Enter 1600g 50vt% ethanol waters, filtrate is collected by filtration in heating and refluxing extraction 2h, and filtrate merges to obtain tea seed extract solution.
Extract solution heats concentration under the conditions of -0.07~-0.08Mpa and medicinal extract is made, and the pure water of 10 times of its weight is added into medicinal extract
Dissolving, then with volume ratio 1:3 ether and ethyl acetate mixed extractant solvent, extract 3 times, each mixed solvent dosage is leaching
4 times of cream weight.Organic solvent layer solution is collected, is merged, is added anhydrous magnesium sulfate into organic solvent layer solution, stir
After stand 24h, filter, collect filtrate, filtrate is concentrated under reduced pressure under the conditions of -0.07~-0.08Mpa, is dried to solid-like, obtains tea
Saponin.
(2) safflower vegetable plot upper part is dried, crushes, weigh safflower vegetable powder 200g, be put into refluxing extraction equipment, added
1600g 70vt% ethanol waters, to safflower vegetable powder heating and refluxing extraction 5h, filtrate is collected by filtration, is added into filter residue
Filtrate is collected by filtration in 1600g 50vt% ethanol waters, heating and refluxing extraction 2h, and filtrate merges to obtain safflower dish extract solution.Carry
Take liquid to heat concentration under the conditions of -0.07~-0.08Mpa and medicinal extract is made, the pure water-soluble of 10 times of its weight is added into medicinal extract
Solution, is then extracted with ethyl acetate, and extracts 3 times, and each ethyl acetate dosage is 4 times of medicinal extract weight.Collect ethyl acetate layer,
Merge, add anhydrous magnesium sulfate, 24h is stood after stirring, filter, collect filtrate, filtrate is in -0.07~-0.08Mpa conditions
Under be concentrated under reduced pressure, be dried to solid-like, obtain safflower dish extract.
(3) Tea Saponin 1.8g and safflower dish extract 1.0g obtained above is weighed, sequentially adds 96.1g second containing 10wt%
In the aqueous solution of acetoacetic ester, it is well mixed, then adds 1.1g C8-C10 AEOs, is sufficiently mixed uniformly, i.e.,
Obtain insecticide.
Embodiment 3
A kind of method for producing insecticide, preparation method are as follows：
(1) tea-seed pancake after degreasing of extracting oil is crushed, weighs tea seed cake powder 200g, be put into refluxing extraction equipment, add
Enter 2000g 50vt% ethanol waters, to tea-seed pancake powder heating and refluxing extraction 4h, filtrate is collected by filtration, add again into filter residue
Enter 1200g 70vt% ethanol waters, filtrate is collected by filtration in heating and refluxing extraction 3h, and filtrate merges to obtain tea seed extract solution.
Extract solution heats concentration under the conditions of -0.07~-0.08Mpa and medicinal extract is made, and the pure water-soluble of 8 times of its weight is added into medicinal extract
Solution, then with volume ratio 1:4 ether and ethyl acetate mixed extractant solvent, extract 4 times, each mixed solvent dosage is medicinal extract
3 times of weight.Organic solvent layer solution is collected, merges, anhydrous magnesium sulfate is added into organic solvent layer solution, after stirring
20h is stood, filtering, collects filtrate, filtrate is concentrated under reduced pressure under the conditions of -0.07~-0.08Mpa, is dried to solid-like, obtains tea soap
Element.
(2) safflower vegetable plot upper part is dried, crushes, weigh safflower vegetable powder 200g, be put into refluxing extraction equipment, added
2000g 50vt% ethanol waters, to safflower vegetable powder heating and refluxing extraction 3h, filtrate is collected by filtration, is added into filter residue
Filtrate is collected by filtration in 1200g 70vt% ethanol waters, heating and refluxing extraction 3h, and filtrate merges to obtain safflower dish extract solution.Carry
Take liquid to heat concentration under the conditions of -0.07~-0.08Mpa and medicinal extract is made, the pure water-soluble of 8 times of its weight is added into medicinal extract
Solution, is then extracted with ethyl acetate, and extracts 4 times, and each ethyl acetate dosage is 3 times of medicinal extract weight.Collect ethyl acetate layer,
Merge, add anhydrous magnesium sulfate, 20h is stood after stirring, filter, collect filtrate, filtrate is in -0.07~-0.08Mpa conditions
Under be concentrated under reduced pressure, be dried to solid-like, obtain safflower dish extract.
(3) Tea Saponin 1.8g and safflower dish extract 1.0g obtained above is weighed, sequentially adds 96.1g second containing 8wt%
In the aqueous solution of acetoacetic ester, it is well mixed, then adds 1.1g C8-C10 AEOs, is sufficiently mixed uniformly, i.e.,
Obtain insecticide.
Embodiment 4
The insecticide preparation method of the present embodiment is substantially the same manner as Example 1, is distinguished as in the present embodiment step (3), tea
The amount of saponin is 2.0g, and the amount of safflower dish extract is 0.8g, and the dosage of C8-C10 AEOs is 1.0g, is contained
The amount of the aqueous solution of 10wt% ethyl acetate is 96.2g.
Embodiment 5
The insecticide preparation method of the present embodiment is substantially the same manner as Example 1, is distinguished as in the present embodiment step (3), tea
The amount of saponin is 1.5g, and the amount of safflower dish extract is 1.2g, and the dosage of C8-C10 AEOs is 1.3g, is contained
The amount of the aqueous solution of 10wt% ethyl acetate is 96.0g.
Comparative example 1
This comparative example is distinguished as with embodiment 1：This comparative example does not include the step of embodiment 1 (2)；In step (3), this is right
Ratio is free of safflower dish extract, and the amount of the aqueous solution of the ethyl acetate containing 10wt% is 97.1g.
Comparative example 2
This comparative example is distinguished as with embodiment 1：This comparative example does not include the step of embodiment 1 (2)；In step (3), this is right
Ratio is free of safflower dish extract, and the amount of Tea Saponin is 2.5g, and the amount of the aqueous solution of the ethyl acetate containing 10wt% is 96.4g.
Comparative example 3
This comparative example is distinguished as with embodiment 1：This comparative example does not include the step of embodiment 1 (1)；In step (3), this is right
Ratio is free of Tea Saponin, and the amount of the aqueous solution of the ethyl acetate containing 10wt% is 97.9g.
Comparative example 4
This comparative example is distinguished as with embodiment 1：This comparative example does not include the step of embodiment 1 (1)；In step (3), this is right
Ratio is free of Tea Saponin, and the amount of safflower dish extract is 1.5g, and the amount of the aqueous solution of the ethyl acetate containing 10wt% is 97.4g.
The prevention and control of plant diseases, pest control is tested
1st, test material
Insect selects Parametrites theae.
Insecticide selects insecticide made from above-described embodiment 1-5 and comparative example 1-4.
2nd, test method
30 Parametrites theaes are put into each culture dish, and are put into appropriate And Development of Tea Shoot leaf.Using drop method, micro intravenous drip is used
Insecticide is dropped in Parametrites theae belly back by device, and every kind of insecticide experiment is repeated 3 times, while carries out check experiment.
With the activity of observation post administration Parametrites theae, meal situation, 24h, 48h, 72h statistics death toll, corrected mortality is calculated.
It the results are shown in Table 1.
Killing effect of the different insecticides of table 1 to Parametrites theae
As shown in Table 1, when Tea Saponin and safflower dish extract are used alone, there are certain food refusal and killing to Parametrites theae
Effect, the killing effect of Tea Saponin is higher than safflower dish extract, but the two killing effect is relatively low.
The obvious reduction of activity of rear Parametrites theae is used in combination in Tea Saponin and safflower dish extract, eating to be decreased obviously, right
The killing effect of insect significantly improves, and the killing effect of wherein embodiment 1 is optimal, and 72h Mortality of insect is up to 68.89%.
The plant insecticide of the present invention can be used in combination with chemical pesticide, can also be first using the insecticide pair of the present invention
Pest killing, then further killed with chemical pesticide again.
The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention, although with reference to foregoing reality
Apply example the present invention is described in detail, for those skilled in the art, it still can be to foregoing each implementation
Technical scheme described in example is modified, or carries out equivalent substitution to which part technical characteristic.All essences in the present invention
God any modification, equivalent substitution and improvements made etc., should be included in the scope of the protection with principle.
Claims (10)
1. a kind of insecticide containing Tea Saponin, it is characterised in that the insecticide is made up of the component of following percentage by weight：
Tea Saponin 1.5~2.0%, safflower dish extract 0.8~1.2%, surfactant 1.0~1.3%, surplus is solvent.
2. the insecticide according to claim 1 containing Tea Saponin, it is characterised in that the insecticide is by following weight hundred
The component of ratio is divided to be made：Tea Saponin 1.8%, safflower dish extract 1.0%, surfactant 1.1%, surplus is solvent.
3. the insecticide according to claim 1 or 2 containing Tea Saponin, it is characterised in that the surfactant includes
C8-C10 AEOs.
4. the insecticide according to claim 1 or 2 containing Tea Saponin, it is characterised in that the solvent be containing esters 8~
The 10wt% aqueous solution.
5. the method for producing insecticide containing Tea Saponin described in claim any one of 1-4, it is characterised in that specifically include
Following steps：
(1) preparation of Tea Saponin
Tea-seed pancake crushes, and carries out secondary back extraction to tea-seed pancake powder with ethanol water, extract solution, which is concentrated under reduced pressure, to be made
Medicinal extract, dissolved in purified water is added into the medicinal extract, then with ether and ethyl acetate mixed extractant solvent, collect organic solvent
Layer solution, adds anhydrous magnesium sulfate into obtained organic solvent layer solution, is stood after stirring, and filters, obtained filtrate
It is concentrated under reduced pressure, dries, obtains Tea Saponin；
(2) preparation of safflower dish extract
Safflower vegetable plot upper part is dried, and is crushed, and secondary back extraction, extract solution decompression are carried out to safflower vegetable powder with ethanol water
Medicinal extract is made in concentration, and dissolved in purified water is added into the medicinal extract, is then extracted with ethyl acetate, and collects ethyl acetate layer, to
Ethyl acetate layer adds anhydrous magnesium sulfate, is stood after stirring, and filters, and obtained filtrate decompression is concentrated, dried, and obtains safflower dish
Extract；
(3) preparation of insecticide
The Tea Saponin that step (1) obtains and the safflower dish extract that step (2) obtains are taken, is sequentially added in solvent, is well mixed,
Then surfactant is added, is sufficiently mixed uniformly, produces insecticide.
6. the method for producing insecticide according to claim 5 containing Tea Saponin, it is characterised in that the step (1)
In, volume fraction of ethanol 50~70% in the ethanol water；
Ethanol water volume is 8~10 times of tea-seed pancake powder weight when extracting for the first time, and extraction time is 4~6h, second
Ethanol water volume is 6~8 times of tea-seed pancake powder weight during secondary extraction, and extraction time is 2~3h；
Described be concentrated under reduced pressure is carried out under -0.07~-0.08Mpa.
7. the method for producing insecticide according to claim 5 containing Tea Saponin, it is characterised in that the step (1)
In, the dosage of pure water is 8~10 times of medicinal extract weight；
The volume ratio of the in the mixed solvent ether and ethyl acetate is 1：3~4；
Mixed extractant solvent 3-4 times, the dosage of mixed solvent is 3~4 times of medicinal extract weight during extraction；
The time of repose is 20~24h.
8. the method for producing insecticide according to claim 5 containing Tea Saponin, it is characterised in that the step (2)
In, volume fraction of ethanol 50~70% in the ethanol water；
Ethanol water volume is 8~10 times of safflower vegetable powder weight when extracting for the first time, and extraction time is 3~5h, second
Ethanol water volume is 6~8 times of tea-seed pancake powder weight during extraction, and extraction time is 2~3h；
Described be concentrated under reduced pressure is carried out under -0.07~-0.08Mpa.
9. the method for producing insecticide according to claim 5 containing Tea Saponin, it is characterised in that the step (2)
In, the dosage of pure water is 8~10 times of medicinal extract weight；
Extraction is carried out 3~4 times, and the dosage of ethyl acetate is 3~4 times of medicinal extract weight during extraction；
The time of repose is 20~24h.
10. the insecticide containing Tea Saponin described in claim any one of 1-4 is used to prevent and treat Parametrites theae.
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Effective date of registration: 20240304 Address after: No. 1, West 1st Lane, Yuejiang Road, Guyi Town, Sanjiang County, Liuzhou City, Guangxi Zhuang Autonomous Region, 545500 Patentee after: Guangxi Sanjiang Dongzhixiang Biotechnology Co.,Ltd. Country or region after: China Address before: 545500 Dazhai Tun, Dazhu Village, Guyi Town, Sanjiang County, Liuzhou City, Guangxi Zhuang Autonomous Region Patentee before: SANJIANG DAOXIANGSHAN TEA OIL ECOLOGICAL DEVELOPMENT CO.,LTD. Country or region before: China |