CN107484778B - Insecticide containing tea saponin and preparation method thereof - Google Patents
Insecticide containing tea saponin and preparation method thereof Download PDFInfo
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- CN107484778B CN107484778B CN201710931507.2A CN201710931507A CN107484778B CN 107484778 B CN107484778 B CN 107484778B CN 201710931507 A CN201710931507 A CN 201710931507A CN 107484778 B CN107484778 B CN 107484778B
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- 241001122767 Theaceae Species 0.000 title claims abstract description 55
- 239000002917 insecticide Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000001397 quillaja saponaria molina bark Substances 0.000 title abstract description 40
- 229930182490 saponin Natural products 0.000 title abstract description 40
- 150000007949 saponins Chemical class 0.000 title abstract description 40
- 239000000575 pesticide Substances 0.000 claims abstract description 42
- 244000020518 Carthamus tinctorius Species 0.000 claims abstract description 35
- 235000003255 Carthamus tinctorius Nutrition 0.000 claims abstract description 30
- 229940119485 safflower extract Drugs 0.000 claims abstract description 15
- 239000002904 solvent Substances 0.000 claims abstract description 9
- 239000004094 surface-active agent Substances 0.000 claims abstract description 9
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 108
- 239000000284 extract Substances 0.000 claims description 85
- 235000018597 common camellia Nutrition 0.000 claims description 47
- 239000000706 filtrate Substances 0.000 claims description 47
- 239000000243 solution Substances 0.000 claims description 46
- 240000001548 Camellia japonica Species 0.000 claims description 44
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 44
- 238000000605 extraction Methods 0.000 claims description 36
- 238000001914 filtration Methods 0.000 claims description 30
- 239000000843 powder Substances 0.000 claims description 30
- 239000007864 aqueous solution Substances 0.000 claims description 29
- 238000010438 heat treatment Methods 0.000 claims description 27
- 238000010992 reflux Methods 0.000 claims description 27
- 238000002156 mixing Methods 0.000 claims description 25
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 21
- 238000001035 drying Methods 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 16
- 239000008213 purified water Substances 0.000 claims description 16
- 239000012046 mixed solvent Substances 0.000 claims description 15
- 239000003960 organic solvent Substances 0.000 claims description 13
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 150000002191 fatty alcohols Chemical class 0.000 claims description 8
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 8
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 7
- 241000628997 Flos Species 0.000 claims description 5
- 238000005238 degreasing Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 238000003825 pressing Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 4
- 150000002148 esters Chemical class 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 235000013311 vegetables Nutrition 0.000 claims description 2
- 241000209507 Camellia Species 0.000 claims 3
- 238000007605 air drying Methods 0.000 claims 1
- 238000010298 pulverizing process Methods 0.000 claims 1
- 230000002147 killing effect Effects 0.000 abstract description 17
- 239000000126 substance Substances 0.000 abstract description 10
- 235000013305 food Nutrition 0.000 abstract description 5
- 239000004480 active ingredient Substances 0.000 abstract description 4
- 230000001887 anti-feedant effect Effects 0.000 abstract description 4
- 241000526900 Camellia oleifera Species 0.000 abstract description 3
- 241000282414 Homo sapiens Species 0.000 abstract description 3
- 230000009471 action Effects 0.000 abstract description 3
- 231100000481 chemical toxicant Toxicity 0.000 abstract description 3
- 230000006378 damage Effects 0.000 abstract description 3
- 238000003912 environmental pollution Methods 0.000 abstract description 3
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- 239000003440 toxic substance Substances 0.000 abstract description 3
- 241000196324 Embryophyta Species 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 17
- 241000607479 Yersinia pestis Species 0.000 description 9
- 238000005303 weighing Methods 0.000 description 9
- 241000238631 Hexapoda Species 0.000 description 4
- 239000003921 oil Substances 0.000 description 4
- 201000010099 disease Diseases 0.000 description 3
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- MWDZOUNAPSSOEL-UHFFFAOYSA-N kaempferol Natural products OC1=C(C(=O)c2cc(O)cc(O)c2O1)c3ccc(O)cc3 MWDZOUNAPSSOEL-UHFFFAOYSA-N 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 235000009024 Ceanothus sanguineus Nutrition 0.000 description 2
- 240000003553 Leptospermum scoparium Species 0.000 description 2
- 235000015459 Lycium barbarum Nutrition 0.000 description 2
- WWNNZCOKKKDOPX-UHFFFAOYSA-N N-methylnicotinate Chemical compound C[N+]1=CC=CC(C([O-])=O)=C1 WWNNZCOKKKDOPX-UHFFFAOYSA-N 0.000 description 2
- 239000012043 crude product Substances 0.000 description 2
- 229940079593 drug Drugs 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
- 239000002736 nonionic surfactant Substances 0.000 description 2
- -1 pentacyclic triterpenoid compounds Chemical class 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
- 241001184747 Caloptilia theivora Species 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
- 239000005947 Dimethoate Substances 0.000 description 1
- 206010059866 Drug resistance Diseases 0.000 description 1
- 241000220485 Fabaceae Species 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
- 241001676573 Minium Species 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- ZVOLCUVKHLEPEV-UHFFFAOYSA-N Quercetagetin Natural products C1=C(O)C(O)=CC=C1C1=C(O)C(=O)C2=C(O)C(O)=C(O)C=C2O1 ZVOLCUVKHLEPEV-UHFFFAOYSA-N 0.000 description 1
- HWTZYBCRDDUBJY-UHFFFAOYSA-N Rhynchosin Natural products C1=C(O)C(O)=CC=C1C1=C(O)C(=O)C2=CC(O)=C(O)C=C2O1 HWTZYBCRDDUBJY-UHFFFAOYSA-N 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
- 241000256251 Spodoptera frugiperda Species 0.000 description 1
- 210000001015 abdomen Anatomy 0.000 description 1
- 229960000643 adenine Drugs 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- XADJWCRESPGUTB-UHFFFAOYSA-N apigenin Natural products C1=CC(O)=CC=C1C1=CC(=O)C2=CC(O)=C(O)C=C2O1 XADJWCRESPGUTB-UHFFFAOYSA-N 0.000 description 1
- KZNIFHPLKGYRTM-UHFFFAOYSA-N apigenin Chemical compound C1=CC(O)=CC=C1C1=CC(=O)C2=C(O)C=C(O)C=C2O1 KZNIFHPLKGYRTM-UHFFFAOYSA-N 0.000 description 1
- 235000008714 apigenin Nutrition 0.000 description 1
- 229940117893 apigenin Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000010495 camellia oil Substances 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003795 chemical substances by application 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
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction 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
- 239000006185 dispersion Substances 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 230000035553 feeding performance Effects 0.000 description 1
- 229930003935 flavonoid Natural products 0.000 description 1
- 150000002215 flavonoids Chemical class 0.000 description 1
- 235000017173 flavonoids Nutrition 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 229930182470 glycoside Natural products 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 230000000266 injurious effect Effects 0.000 description 1
- 230000000749 insecticidal effect Effects 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
- 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
- IQPNAANSBPBGFQ-UHFFFAOYSA-N luteolin Chemical compound C=1C(O)=CC(O)=C(C(C=2)=O)C=1OC=2C1=CC=C(O)C(O)=C1 IQPNAANSBPBGFQ-UHFFFAOYSA-N 0.000 description 1
- LRDGATPGVJTWLJ-UHFFFAOYSA-N luteolin Natural products OC1=CC(O)=CC(C=2OC3=CC(O)=CC(O)=C3C(=O)C=2)=C1 LRDGATPGVJTWLJ-UHFFFAOYSA-N 0.000 description 1
- 235000009498 luteolin Nutrition 0.000 description 1
- 239000000463 material 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
- 230000001766 physiological effect Effects 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
- REFJWTPEDVJJIY-UHFFFAOYSA-N quercetin Natural products C=1C(O)=CC(O)=C(C(C=2O)=O)C=1OC=2C1=CC=C(O)C(O)=C1 REFJWTPEDVJJIY-UHFFFAOYSA-N 0.000 description 1
- 235000005875 quercetin Nutrition 0.000 description 1
- 229960001285 quercetin Drugs 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000004044 response 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
- 238000010998 test method Methods 0.000 description 1
- 238000009736 wetting Methods 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)
- Environmental Sciences (AREA)
- Plant Pathology (AREA)
- Dentistry (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Agronomy & Crop Science (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 tea saponin-containing pesticide, which is prepared from the following components in percentage by weight: 1.5-2.0% of tea saponin, 0.8-1.2% of a safflower extract, 1.0-1.3% of a surfactant and the balance of a solvent; and provides a preparation method thereof. The active ingredients of the pesticide are extracted from the camellia oleifera seed cake and the carthamus tinctorius, so that the pesticide is a botanical pesticide, has small environmental pollution and is environment-friendly; compared with chemical insecticides, the preparation method is simple, and the generation of a large amount of refractory and toxic chemical substances in chemical synthesis is avoided; the pesticide of the invention is easy to biodegrade, greatly reduces the residual quantity of pesticide on plants, and avoids the harm to human health caused by the action of biological enrichment through a food chain; the combined use of the tea saponin and the safflower extract obviously enhances the killing capability of the tea-tip moth, has antifeedant and contact killing effects on the tea-tip moth, and has a 72-hour killing rate of over 65 percent.
Description
Technical Field
The invention belongs to the technical field of pesticides, and particularly relates to a tea saponin-containing pesticide and a preparation method thereof.
Background
The chemical pesticide is a toxic chemical agent, and can kill the diseases and insect pests of crops and trees with a small amount of chemical pesticide or has important influence on the physiological activity of the diseases and insect pests. The chemical pesticide has the advantages of low use cost, quick response, multiple varieties and wide prevention and control objects. The disadvantages are that the environment is polluted, the residual pesticide is accumulated in food under the concentration action of a food chain, and the food is enriched in vivo after being eaten by people, thereby threatening the health and life of human beings and easily causing serious diseases such as cancer and the like; pests are susceptible to drug resistance.
The tea top moth, lepidoptera, poinsettidae, hosts comprise tea, tea-oil tree and camellia, and the larvae mainly eat the young shoots at the top of the tea tree to damage the young shoots, so that the young shoots die and the yield of the tea is influenced. The existing medicines for preventing and controlling the tea leaf roller moth mainly comprise 40 percent of dimethoate, 80 percent of dichlorvos emulsion 1500 times liquid, 2.5 percent of tianwangxing emulsifiable 3000 times liquid and 50 percent of minium powder 1500 times liquid, and the medicines generally have the defects of the chemical insecticide described above.
Disclosure of Invention
The first purpose of the present invention is to overcome the above drawbacks and to provide a tea saponin-containing pesticide, the active ingredient of which is a plant extract, which has the advantages of low environmental pollution and easy degradation.
The second object of the present invention is to provide a process for preparing the above-mentioned insecticide.
A third object of the present invention is to provide the use of the above-mentioned pesticide.
The purpose of the invention is realized by the following technical scheme:
the pesticide containing the tea saponin is prepared from the following components in percentage by weight: 1.5-2.0% of tea saponin, 0.8-1.2% of a safflower extract, 1.0-1.3% of a surfactant and the balance of a solvent.
Preferably, the pesticide is prepared from the following components in percentage by weight: 1.8% of tea saponin, 1.0% of a safflower extract, 1.1% of a surfactant and the balance of a solvent.
Further, the surfactant comprises C8-C10 fatty alcohol polyoxyethylene ether.
Further, the solvent is an aqueous solution containing 8-10 wt% of esters.
The preparation method of the pesticide containing tea saponin specifically comprises the following steps:
(1) preparation of tea saponin
Crushing the camellia seed cake, performing secondary reflux extraction on camellia seed cake powder by using an ethanol water solution, performing reduced pressure concentration on an extracting solution to prepare an extract, adding purified water into the extract for dissolving, then extracting by using a mixed solvent of diethyl ether and ethyl acetate, collecting an organic solvent layer solution, adding anhydrous magnesium sulfate into the obtained organic solvent layer solution, stirring uniformly, standing, filtering, and performing reduced pressure concentration and drying on the obtained filtrate to obtain tea saponin;
(2) preparation method of Carthami flos extract
Drying aerial parts of the carthamus tinctorius, crushing, carrying out secondary reflux extraction on the carthamus tinctorius powder by using an ethanol water solution, carrying out reduced pressure concentration on an extracting solution to prepare an extract, adding purified water into the extract to dissolve the extract, then extracting the extract by using ethyl acetate, collecting an ethyl acetate layer, adding anhydrous magnesium sulfate into the ethyl acetate layer, stirring the mixture uniformly, standing the mixture, filtering, and carrying out reduced pressure concentration and drying on obtained filtrate to obtain a carthamus tinctorius extract;
(3) preparation of insecticides
And (3) sequentially adding the tea saponin obtained in the step (1) and the safflower extract obtained in the step (2) into a solvent, uniformly mixing, then adding a surfactant, and fully and uniformly mixing to obtain the pesticide.
Further, in the step (1), the volume fraction of ethanol in the ethanol aqueous solution is 50-70%;
the volume of the ethanol aqueous solution is 8-10 times of the weight of the camellia seed cake powder during the first extraction, the extraction time is 4-6 hours, the volume of the ethanol aqueous solution is 6-8 times of the weight of the camellia seed cake powder during the second extraction, and the extraction time is 2-3 hours;
the reduced pressure concentration is carried out at-0.07 to-0.08 Mpa.
Further, in the step (1), the consumption of the purified water is 8-10 times of the weight of the extract;
the volume ratio of the ethyl ether to the ethyl acetate in the mixed solvent is 1: 3-4;
extracting for 3-4 times by using the mixed solvent, wherein the dosage of the mixed solvent is 3-4 times of the weight of the extract during extraction;
the standing time is 20-24 h.
Further, in the step (2), the volume fraction of ethanol in the ethanol aqueous solution is 50-70%;
the volume of the ethanol aqueous solution is 8-10 times of the weight of the red flower vegetable powder in the first extraction, the extraction time is 3-5 hours, the volume of the ethanol aqueous solution is 6-8 times of the weight of the camellia seed cake powder in the second extraction, and the extraction time is 2-3 hours;
the reduced pressure concentration is carried out at-0.07 to-0.08 Mpa.
Further, in the step (2), the consumption of the purified water is 8-10 times of the weight of the extract;
extracting for 3-4 times, wherein the dosage of the ethyl acetate is 3-4 times of the weight of the extract during extraction;
the standing time is 20-24 h.
The pesticide containing tea saponin is used for preventing and treating tea top moth.
Tea saponin, also known as tea saponin, is a botanical insecticide extracted from seeds of Theaceae plants, such as tea seed cakes and tea cakes obtained after oil extraction from tea seeds, the active ingredients belong to pentacyclic triterpenoid compounds, the tea saponin is bitter, spicy, easy to dissolve in organic solvents such as water, alcohols and the like, and has contact killing and antifeedant effects on pests. Tea saponin is also a natural non-ionic surfactant, and has good functions of emulsification, dispersion, foaming, wetting and the like.
The safflower belongs to leguminosae, and is a safflower seed, which contains various flavonoid components: quercetin glycoside, apigenin, isorhamnetin, luteolin, robinin, kaempferol, and additionally contains trigonelline, choline, adenine, etc., and the simple extract of Carthamus tinctorius has weak insecticidal ability.
Fatty alcohol polyoxyethylene ether (AEO), belonging to nonionic surfactant, is ether formed by condensation of polyethylene glycol and fatty alcohol.
The invention takes ethanol water solution as solution to respectively carry out reflux extraction on the camellia oleifera seed cake and the safflower carthamus to prepare the crude products of the tea saponin and the safflower carthamus extract, the crude products of the tea saponin and the safflower carthamus extract are taken as the effective components of the pesticide, and the killing capability of the tea saponin and the safflower carthamus extract on the injurious insect, namely the tea tip moth, is obviously enhanced after the tea saponin and the safflower carthamus extract are jointly used.
The invention has the following beneficial effects:
(1) the active ingredients of the pesticide are extracted from the camellia oleifera seed cake and the carthamus tinctorius, so that the pesticide is a botanical pesticide, has small environmental pollution and is environment-friendly;
(2) compared with chemical insecticides, the preparation method is simple, and the generation of a large amount of refractory and toxic chemical substances in chemical synthesis is avoided;
(3) the pesticide of the invention is easy to biodegrade, greatly reduces the residual quantity of pesticide on plants, and avoids the harm to human health caused by the action of biological enrichment through a food chain;
(4) the combined use of the tea saponin and the safflower extract obviously enhances the killing capability of the tea-tip moth, has antifeedant and contact killing effects on the tea-tip moth, and has a 72-hour killing rate of over 65 percent.
Detailed Description
The following description of the preferred embodiments of the present invention is provided for the purpose of illustration and description, and is in no way intended to limit the invention.
The raw materials in the embodiment of the invention are all commercially available products.
Example 1
A preparation method of the pesticide comprises the following steps:
(1) crushing oil-tea camellia seed cakes after oil pressing and degreasing, weighing 200g of oil-tea camellia seed cake powder, putting the oil-tea camellia seed cake powder into a reflux extraction device, adding 1800g of 60 vt% ethanol aqueous solution, heating and refluxing the oil-tea camellia seed cake powder for 5 hours, filtering and collecting filtrate, adding 1400g of 60 vt% ethanol aqueous solution into filter residues, heating and refluxing for 3 hours, filtering and collecting filtrate, and mixing the filtrate to obtain an oil-tea camellia seed extracting solution. Heating and concentrating the extracting solution under the condition of-0.07 to-0.08 Mpa to prepare an extract, adding 10 times of purified water to the extract for dissolving, then extracting for 4 times by using a mixed solvent of ethyl ether and ethyl acetate with the volume ratio of 1:4, wherein the using amount of the mixed solvent is 3 times of the weight of the extract each time. Collecting organic solvent layer solution, mixing, adding anhydrous magnesium sulfate into the organic solvent layer solution, stirring, standing for 24h, filtering, collecting filtrate, concentrating the filtrate under reduced pressure of-0.07 to-0.08 Mpa, and drying to obtain solid tea saponin.
(2) Drying aerial parts of the carthamus tinctorius, crushing, weighing 200g of carthamus tinctorius powder, putting into a reflux extraction device, adding 1800g of 60 vt% ethanol water solution, heating and refluxing the carthamus tinctorius powder for 4 hours, filtering and collecting filtrate, adding 1400g of 60 vt% ethanol water solution into filter residue, heating and refluxing for 3 hours, filtering and collecting filtrate, and combining the filtrate to obtain a carthamus tinctorius extract. Heating and concentrating the extracting solution under the condition of-0.07 to-0.08 Mpa to prepare an extract, adding purified water with the weight being 10 times that of the extract to dissolve the extract, and then extracting the extract by using ethyl acetate for 4 times, wherein the using amount of the ethyl acetate for each time is 3 times of the weight of the extract. Collecting ethyl acetate layers, mixing, adding anhydrous magnesium sulfate, stirring, standing for 24h, filtering, collecting filtrate, concentrating the filtrate under reduced pressure of-0.07 to-0.08 Mpa, and drying to obtain solid.
(3) Weighing 1.8g of the obtained tea saponin and 1.0g of the safflower extract, sequentially adding 96.1g of aqueous solution containing 10 wt% of ethyl acetate, uniformly mixing, then adding 1.1g C8-C10 fatty alcohol polyoxyethylene ether, and fully and uniformly mixing to obtain the pesticide.
Example 2
A preparation method of the pesticide comprises the following steps:
(1) crushing oil-tea camellia seed cakes after oil pressing and degreasing, weighing 200g of oil-tea camellia seed cake powder, putting the oil-tea camellia seed cake powder into a reflux extraction device, adding 1600g of 70 vt% ethanol aqueous solution, heating and refluxing the oil-tea camellia seed cake powder for 6 hours, filtering and collecting filtrate, adding 1600g of 50 vt% ethanol aqueous solution into filter residues, heating and refluxing for 2 hours, filtering and collecting the filtrate, and mixing the filtrate to obtain an oil-tea camellia seed extracting solution. Heating and concentrating the extracting solution under the condition of-0.07 to-0.08 Mpa to prepare an extract, adding 10 times of purified water to the extract for dissolving, then extracting for 3 times by using a mixed solvent of ethyl ether and ethyl acetate with the volume ratio of 1:3, wherein the using amount of the mixed solvent is 4 times of the weight of the extract each time. Collecting organic solvent layer solution, mixing, adding anhydrous magnesium sulfate into the organic solvent layer solution, stirring, standing for 24h, filtering, collecting filtrate, concentrating the filtrate under reduced pressure of-0.07 to-0.08 Mpa, and drying to obtain solid tea saponin.
(2) Drying aerial parts of the carthamus tinctorius, crushing, weighing 200g of carthamus tinctorius powder, putting into a reflux extraction device, adding 1600g of 70 vt% ethanol water solution, heating and refluxing the carthamus tinctorius powder for 5 hours, filtering and collecting filtrate, adding 1600g of 50 vt% ethanol water solution into filter residue, heating and refluxing for 2 hours, filtering and collecting the filtrate, and combining the filtrate to obtain a carthamus tinctorius extract. Heating and concentrating the extracting solution under the condition of-0.07 to-0.08 Mpa to prepare an extract, adding purified water with the weight being 10 times of that of the extract to dissolve the extract, and then extracting the extract for 3 times by using ethyl acetate, wherein the using amount of the ethyl acetate is 4 times of the weight of the extract each time. Collecting ethyl acetate layers, mixing, adding anhydrous magnesium sulfate, stirring, standing for 24h, filtering, collecting filtrate, concentrating the filtrate under reduced pressure of-0.07 to-0.08 Mpa, and drying to obtain solid.
(3) Weighing 1.8g of the obtained tea saponin and 1.0g of the safflower extract, sequentially adding 96.1g of aqueous solution containing 10 wt% of ethyl acetate, uniformly mixing, then adding 1.1g C8-C10 fatty alcohol polyoxyethylene ether, and fully and uniformly mixing to obtain the pesticide.
Example 3
A preparation method of the pesticide comprises the following steps:
(1) crushing oil-tea camellia seed cakes after oil pressing and degreasing, weighing 200g of oil-tea camellia seed cake powder, putting the oil-tea camellia seed cake powder into a reflux extraction device, adding 2000g of 50 vt% ethanol aqueous solution, heating and refluxing the oil-tea camellia seed cake powder for 4 hours, filtering and collecting filtrate, adding 1200g of 70 vt% ethanol aqueous solution into filter residues, heating and refluxing for 3 hours, filtering and collecting filtrate, and mixing the filtrate to obtain an oil-tea camellia seed extracting solution. Heating and concentrating the extracting solution under the condition of-0.07 to-0.08 Mpa to prepare an extract, adding 8 times of purified water to the extract for dissolving, then extracting for 4 times by using a mixed solvent of ethyl ether and ethyl acetate with the volume ratio of 1:4, wherein the using amount of the mixed solvent is 3 times of the weight of the extract each time. Collecting organic solvent layer solution, mixing, adding anhydrous magnesium sulfate into the organic solvent layer solution, stirring, standing for 20h, filtering, collecting filtrate, concentrating the filtrate under reduced pressure of-0.07 to-0.08 Mpa, and drying to obtain solid tea saponin.
(2) Drying aerial parts of the carthamus tinctorius, crushing, weighing 200g of carthamus tinctorius powder, putting into a reflux extraction device, adding 2000g of 50 vt% ethanol water solution, heating and refluxing the carthamus tinctorius powder for 3 hours, filtering and collecting filtrate, adding 1200g of 70 vt% ethanol water solution into filter residue, heating and refluxing for 3 hours, filtering and collecting the filtrate, and combining the filtrate to obtain a carthamus tinctorius extract. Heating and concentrating the extracting solution under the condition of-0.07 to-0.08 Mpa to prepare an extract, adding purified water with the weight 8 times of that of the extract to dissolve the extract, and then extracting the extract for 4 times by using ethyl acetate, wherein the using amount of the ethyl acetate is 3 times of the weight of the extract each time. Collecting ethyl acetate layers, mixing, adding anhydrous magnesium sulfate, stirring, standing for 20h, filtering, collecting filtrate, concentrating the filtrate under reduced pressure of-0.07 to-0.08 Mpa, and drying to obtain solid.
(3) Weighing 1.8g of the obtained tea saponin and 1.0g of the safflower extract, sequentially adding 96.1g of an aqueous solution containing 8 wt% of ethyl acetate, uniformly mixing, then adding 1.1g C8-C10 fatty alcohol-polyoxyethylene ether, and fully and uniformly mixing to obtain the pesticide.
Example 4
The insecticide of this example was prepared in substantially the same manner as in example 1, except that in step (3) of this example, the amount of tea saponin was 2.0g, the amount of the extract of safflower was 0.8g, the amount of C8-C10 fatty alcohol polyoxyethylene ether was 1.0g, and the amount of the aqueous solution containing 10 wt% ethyl acetate was 96.2 g.
Example 5
The insecticide of this example was prepared in substantially the same manner as in example 1, except that in step (3) of this example, the amount of tea saponin was 1.5g, the amount of the extract of safflower was 1.2g, the amount of C8-C10 fatty alcohol polyoxyethylene ether was 1.3g, and the amount of the aqueous solution containing 10 wt% ethyl acetate was 96.0 g.
Comparative example 1
The present comparative example differs from example 1 in that: this comparative example does not include step (2) of example 1; in step (3), this comparative example did not contain the safflower extract, and the amount of the aqueous solution containing 10 wt% ethyl acetate was 97.1 g.
Comparative example 2
The present comparative example differs from example 1 in that: this comparative example does not include step (2) of example 1; in step (3), this comparative example did not contain the safflower extract, the amount of tea saponin was 2.5g, and the amount of the aqueous solution containing 10 wt% ethyl acetate was 96.4 g.
Comparative example 3
The present comparative example differs from example 1 in that: this comparative example does not include step (1) of example 1; in step (3), this comparative example contained no tea saponin, and the amount of an aqueous solution containing 10 wt% ethyl acetate was 97.9 g.
Comparative example 4
The present comparative example differs from example 1 in that: this comparative example does not include step (1) of example 1; in step (3), this comparative example did not contain tea saponin, the amount of the safflower extract was 1.5g, and the amount of the aqueous solution containing 10 wt% ethyl acetate was 97.4 g.
Pest control test
1. Test materials
The insects are selected from tea top moths.
The insecticides were selected from the insecticides prepared in examples 1 to 5 and comparative examples 1 to 4 above.
2. Test method
30 tea leaf moths are put in each culture dish, and a proper amount of tea tree fresh leaves are put in each culture dish. The insecticide is dropped on the back of the abdomen of the tea shoot moth by a micro dropper by adopting a dropping method, each insecticide test is repeated for 3 times, and a control test is carried out at the same time.
After the medicine is taken, the activity and the eating condition of the tea top moth are observed, the death number is counted for 24h, 48h and 72h, and the corrected death rate is calculated. The results are shown in Table 1.
TABLE 1 Effect of different insecticides on the killing of Spodoptera frugiperda
As can be seen from table 1, when the tea saponin and the carthamus tinctorius extract are used alone, the tea saponin has a certain antifeedant and killing effect on the tea tip moth, the killing effect of the tea saponin is higher than that of the carthamus tinctorius extract, but the killing effect of the tea saponin and the killing effect of the carthamus tinctorius extract are both lower.
After the tea saponin and the carthamus tinctorius extract are used together, the activity of the tea top moth is obviously reduced, the feeding performance is obviously reduced, and the pest killing effect is obviously improved, wherein the killing effect of the embodiment 1 is the best, and the death rate of the pests reaches 68.89% after 72 h.
The botanical pesticide can be used in combination with chemical pesticide, or can be used for killing pests firstly and then further killing pests by using the chemical pesticide.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The pesticide containing the degreased camellia seed extract is characterized by being prepared from the following components in percentage by weight: 1.5-2.0% of defatted camellia seed extract, 0.8-1.2% of safflower extract, 1.0-1.3% of surfactant and the balance of solvent;
the extraction method of the degreased camellia seed extract comprises the following steps: crushing oil-tea camellia seed cakes after oil pressing and degreasing, putting the crushed oil-tea camellia seed cakes into a reflux extraction device, adding an ethanol water solution, heating and reflux-extracting the oil-tea camellia seed cake powder, filtering and collecting filtrate, adding the ethanol water solution into filter residues, heating and reflux-extracting, filtering and collecting the filtrate, and mixing the filtrate to obtain an oil-tea camellia seed extracting solution; heating and concentrating the extracting solution to prepare an extract, adding purified water into the extract for dissolving, and then extracting by using a mixed solvent of diethyl ether and ethyl acetate; collecting organic solvent layer solution, mixing, adding anhydrous magnesium sulfate into organic solvent layer solution, stirring, standing, filtering, collecting filtrate, concentrating the filtrate under reduced pressure, and drying to obtain defatted Camellia seed extract;
the extraction method of the safflower extract comprises the following steps: air drying aerial parts of Carthami flos, pulverizing, placing into reflux extraction equipment, adding ethanol water solution, heating and reflux extracting Carthami flos powder, filtering, collecting filtrate, adding ethanol water solution into residue, heating and reflux extracting, filtering, collecting filtrate, and mixing filtrates to obtain Carthami flos extract; heating and concentrating the extracting solution to prepare an extract, adding purified water into the extract for dissolving, and then extracting with ethyl acetate; collecting ethyl acetate layers, mixing, adding anhydrous magnesium sulfate, stirring, standing, filtering, collecting filtrate, concentrating under reduced pressure, and drying to obtain solid.
2. The defatted camellia seed extract-containing pesticide according to claim 1, wherein the pesticide is prepared from the following components in percentage by weight: 1.8% of defatted camellia seed extract, 1.0% of safflower extract, 1.1% of surfactant and the balance of solvent.
3. The defatted camellia seed extract as claimed in claim 1 or 2, wherein the surfactant comprises C8-C10 fatty alcohol polyoxyethylene ether.
4. The defatted camellia seed extract-containing pesticide according to claim 1 or 2, wherein the solvent is an aqueous solution containing 8 to 10 wt% of esters.
5. The method for producing a pesticide containing defatted camellia seed extract as claimed in any of claims 1 to 4, comprising the steps of:
(1) preparation of defatted Camellia seed extract
Crushing oil-tea camellia seed cakes after oil pressing and degreasing, putting the crushed oil-tea camellia seed cakes into a reflux extraction device, adding an ethanol water solution, heating and reflux-extracting the oil-tea camellia seed cake powder, filtering and collecting filtrate, adding the ethanol water solution into filter residues, heating and reflux-extracting, filtering and collecting the filtrate, and mixing the filtrate to obtain an oil-tea camellia seed extracting solution; heating and concentrating the extracting solution to prepare an extract, adding purified water into the extract for dissolving, and then extracting by using a mixed solvent of diethyl ether and ethyl acetate; collecting organic solvent layer solution, mixing, adding anhydrous magnesium sulfate into organic solvent layer solution, stirring, standing, filtering, collecting filtrate, concentrating the filtrate under reduced pressure, and drying to obtain defatted Camellia seed extract;
(2) preparation method of Carthami flos extract
Drying aerial parts of the carthamus tinctorius, crushing, carrying out secondary reflux extraction on the carthamus tinctorius powder by using an ethanol water solution, carrying out reduced pressure concentration on an extracting solution to prepare an extract, adding purified water into the extract to dissolve the extract, then extracting the extract by using ethyl acetate, collecting an ethyl acetate layer, adding anhydrous magnesium sulfate into the ethyl acetate layer, stirring the mixture uniformly, standing the mixture, filtering, and carrying out reduced pressure concentration and drying on obtained filtrate to obtain a carthamus tinctorius extract;
(3) preparation of insecticides
And (3) sequentially adding the degreased camellia seed extract obtained in the step (1) and the carthamus tinctorius extract obtained in the step (2) into a solvent, uniformly mixing, then adding a surfactant, and fully and uniformly mixing to obtain the pesticide.
6. The method for preparing a pesticide containing defatted camellia seed extract according to claim 5, wherein in the step (1), the volume fraction of ethanol in the ethanol aqueous solution is 50-70%;
the volume of the ethanol aqueous solution is 8-10 times of the weight of the camellia seed cake powder during the first extraction, the extraction time is 4-6 hours, the volume of the ethanol aqueous solution is 6-8 times of the weight of the camellia seed cake powder during the second extraction, and the extraction time is 2-3 hours;
the reduced pressure concentration is carried out at-0.07 to-0.08 Mpa.
7. The method for preparing the insecticide containing the defatted oil tea seed extract according to claim 5, wherein in the step (1), the amount of the purified water is 8-10 times of the weight of the extract;
the volume ratio of the ethyl ether to the ethyl acetate in the mixed solvent is 1: 3-4;
extracting for 3-4 times by using the mixed solvent, wherein the dosage of the mixed solvent is 3-4 times of the weight of the extract during extraction;
the standing time is 20-24 h.
8. The method for preparing a pesticide containing defatted camellia seed extract according to claim 5, wherein in the step (2), the volume fraction of ethanol in the ethanol aqueous solution is 50-70%;
the volume of the ethanol aqueous solution is 8-10 times of the weight of the red flower vegetable powder in the first extraction, the extraction time is 3-5 hours, the volume of the ethanol aqueous solution is 6-8 times of the weight of the camellia seed cake powder in the second extraction, and the extraction time is 2-3 hours;
the reduced pressure concentration is carried out at-0.07 to-0.08 Mpa.
9. The method for preparing the insecticide containing the defatted oil tea seed extract according to claim 5, wherein in the step (2), the amount of the purified water is 8-10 times of the weight of the extract;
extracting for 3-4 times, wherein the dosage of the ethyl acetate is 3-4 times of the weight of the extract during extraction;
the standing time is 20-24 h.
10. The insecticide containing defatted camellia seed extract according to any one of claims 1 to 4 for controlling spidia.
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