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CN107484778B - 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 PDF

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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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extract
extraction
filtrate
camellia seed
ethyl acetate
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CN107484778A (en
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荣佳黎
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Ruyuan Yao Autonomous County Weijin Pharmaceutical Co ltd
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Sanjiang Daoxiangshan Tea Oil Ecological Development Co ltd
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N65/00Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/02Biocides, 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
    • A01N43/04Biocides, 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
    • A01N43/14Biocides, 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
    • A01N43/16Biocides, 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
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N65/00Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
    • A01N65/08Magnoliopsida [dicotyledons]
    • A01N65/20Fabaceae or Leguminosae [Pea or Legume family], e.g. pea, lentil, soybean, clover, acacia, honey locust, derris or millettia

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  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
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  • 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

本发明公开了一种含有茶皂素的杀虫剂,所述杀虫剂由如下重量百分比的组分制成:茶皂素1.5~2.0%、红花菜提取物0.8~1.2%、表面活性剂1.0~1.3%,余量为溶剂;并提供了其制备方法。本发明杀虫剂的有效成分从油茶籽饼和红花菜提取得到,是一种植物源杀虫剂,对环境污染小,环境友好;与化学杀虫剂相比制备方法简单,避免了化学合成中大量难降解、有毒化学物质的产生;本发明的杀虫剂易生物降解,大大减少了农药在植物上的残留量,避免生物富集作用通过食物链对人体健康造成的危害;茶皂素和红花菜提取物联合使用后对茶梢蛾的杀灭能力明显增强,对茶梢蛾产生拒食和触杀作用,72h杀灭率可达65%以上。The invention discloses an insecticide containing tea saponin. The insecticide is prepared from the following components by weight percentage: 1.5-2.0% of tea saponin, 0.8-1.2% of broccoli extract, surface active 1.0-1.3% of the solvent, the balance being solvent; and a preparation method thereof is provided. The active ingredient of the pesticide of the invention is extracted from camellia seed cake and safflower, and is a botanical pesticide, which has little environmental pollution and is environmentally friendly; A large number of refractory and toxic chemical substances are produced in the synthesis; the insecticide of the present invention is easy to biodegrade, greatly reduces the residual amount of the pesticide on the plant, and avoids the harm to human health caused by the biological enrichment through the food chain; tea saponin After being used in combination with the safflower extract, the killing ability of the tea shoot moth is obviously enhanced, and the anti-feeding and contact killing effects are produced on the tea shoot moth, and the killing rate can reach more than 65% in 72 hours.

Description

Insecticide containing tea saponin and preparation method thereof
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
Figure BDA0001428885040000111
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)

1.一种含有脱脂油茶籽提取物的杀虫剂,其特征在于,所述杀虫剂由如下重量百分比的组分制成:脱脂油茶籽提取物1 .5~2 .0%、红花菜提取物0 .8~1 .2%、表面活性剂1.0~1 .3%,余量为溶剂;1. An insecticide containing a defatted camellia seed extract, characterized in that the insecticide is made from the following components by weight: 1.5-2.0% of the defatted camellia seed extract, safflower Vegetable extract 0.8-1.2%, surfactant 1.0-1.3%, and the balance is solvent; 所述脱脂油茶籽提取物的提取方法为:将榨油脱脂后的油茶籽饼粉碎,放入回流提取设备中,加入乙醇水溶液,对油茶籽饼粉加热回流提取,过滤收集滤液,向滤渣中再加入乙醇水溶液,加热回流提取,过滤收集滤液,滤液合并得油茶籽提取液;提取液加热浓缩制成浸膏,向浸膏中加入纯净水溶解,然后用乙醚和乙酸乙酯混合溶剂萃取;收集有机溶剂层溶液,合并,向有机溶剂层溶液中加入无水硫酸镁,搅拌均匀后静置,过滤,收集滤液,滤液减压浓缩、干燥成固体状,得脱脂油茶籽提取物;The extraction method of the defatted camellia seed extract is as follows: pulverizing the camellia seed cake after oil pressing and degreasing, putting it into a reflux extraction device, adding an aqueous ethanol solution, heating the camellia seed cake powder under reflux for extraction, filtering and collecting the filtrate, and adding the filtrate to the filter residue. Then add ethanol aqueous solution, heat under reflux for extraction, filter and collect the filtrate, and combine the filtrates to obtain the Camellia oleifera seed extract; the extract is heated and concentrated to make an extract, and pure water is added to the extract to dissolve, and then extracted with a mixed solvent of ether and ethyl acetate; The organic solvent layer solution is collected, combined, anhydrous magnesium sulfate is added to the organic solvent layer solution, stirred evenly, left to stand, filtered, the filtrate is collected, the filtrate is concentrated under reduced pressure, and dried to form a solid to obtain a defatted Camellia oleifera seed extract; 所述红花菜提取物的提取方法为:将红花菜地上部分晾干,粉碎,放入回流提取设备中,加入乙醇水溶液,对红花菜粉加热回流提取,过滤收集滤液,向滤渣中再加入乙醇水溶液,加热回流提取,过滤收集滤液,滤液合并得红花菜提取液;提取液加热浓缩制成浸膏,向浸膏中加入纯净水溶解,然后用乙酸乙酯萃取;收集乙酸乙酯层,合并,加入无水硫酸镁,搅拌均匀后静置,过滤,收集滤液,滤液减压浓缩、干燥成固体状,得红花菜提取物。The extraction method of the safflower extract is as follows: drying the aerial part of safflower, pulverizing it, putting it into a reflux extraction device, adding an aqueous ethanol solution, heating and refluxing the safflower powder, filtering and collecting the filtrate, and adding it to the filter residue. Then add ethanol aqueous solution, heat under reflux for extraction, filter and collect the filtrate, and combine the filtrates to obtain a broccoli extract; the extract is heated and concentrated to make an extract, pure water is added to the extract to dissolve, and then extracted with ethyl acetate; the ethyl acetate is collected The ester layers were combined, and anhydrous magnesium sulfate was added, stirred evenly, and then allowed to stand, filtered, and the filtrate was collected. The filtrate was concentrated under reduced pressure and dried to form a solid to obtain a broccoli extract. 2.根据权利要求1所述的含有脱脂油茶籽提取物的杀虫剂,其特征在于,所述杀虫剂由如下重量百分比的组分制成:脱脂油茶籽提取物1 .8%、红花菜提取物1 .0%、表面活性剂1 .1%,余量为溶剂。2. The insecticide containing degreasing oil camellia seed extract according to claim 1, wherein the insecticide is made from the following components by weight: 1.8% defatted oil tea seed extract, red oil 1.0% of cauliflower extract, 1.1% of surfactant, and the balance of solvent. 3.根据权利要求1或2所述的含有脱脂油茶籽提取物的杀虫剂,其特征在于,所述表面活性剂包括C8-C10脂肪醇聚氧乙烯醚。3. The insecticide containing defatted camellia seed extract according to claim 1 or 2, wherein the surfactant comprises C8-C10 fatty alcohol polyoxyethylene ether. 4.根据权利要求1或2所述的含有脱脂油茶籽提取物的杀虫剂,其特征在于,所述溶剂为含酯类8~10wt%的水溶液。4 . The insecticide containing defatted camellia seed extract according to claim 1 or 2 , wherein the solvent is an aqueous solution containing 8-10 wt % of esters. 5 . 5.权利要求1-4任一项所述的含有脱脂油茶籽提取物的杀虫剂的制备方法,其特征在于,具体包括如下步骤:5. the preparation method of the pesticide containing the degreasing oil camellia seed extract described in any one of claim 1-4, is characterized in that, specifically comprises the steps: (1)脱脂油茶籽提取物的制备(1) Preparation of Defatted Camellia Seed Extract 将榨油脱脂后的油茶籽饼粉碎,放入回流提取设备中,加入乙醇水溶液,对油茶籽饼粉加热回流提取,过滤收集滤液,向滤渣中再加入乙醇水溶液,加热回流提取,过滤收集滤液,滤液合并得油茶籽提取液;提取液加热浓缩制成浸膏,向浸膏中加入纯净水溶解,然后用乙醚和乙酸乙酯混合溶剂萃取;收集有机溶剂层溶液,合并,向有机溶剂层溶液中加入无水硫酸镁,搅拌均匀后静置,过滤,收集滤液,滤液减压浓缩、干燥成固体状,得脱脂油茶籽提取物;Pulverize the camellia oleifera seed cake after oil pressing and degreasing, put it into the reflux extraction equipment, add ethanol aqueous solution, heat and reflux the camellia oleifera seed cake powder, filter and collect the filtrate, add the ethanol aqueous solution to the filter residue, heat under reflux for extraction, and filter and collect the filtrate. , the filtrate was combined to obtain the Camellia oleifera seed extract; the extract was heated and concentrated to make an extract, pure water was added to the extract to dissolve, and then extracted with a mixed solvent of ether and ethyl acetate; the organic solvent layer solution was collected, combined, and added to the organic solvent layer. Add anhydrous magnesium sulfate to the solution, stir evenly, let stand, filter, collect the filtrate, concentrate the filtrate under reduced pressure, and dry it into a solid state to obtain a defatted Camellia oleifera seed extract; (2)红花菜提取物的制备(2) Preparation of cauliflower extract 红花菜地上部分晾干,粉碎,用乙醇水溶液对红花菜粉进行二次回流提取,提取液减压浓缩制成浸膏,向所述浸膏中加入纯净水溶解,然后用乙酸乙酯萃取,收集乙酸乙酯层,向乙酸乙酯层加入无水硫酸镁,搅拌均匀后静置,过滤,得到的滤液减压浓缩、干燥,得红花菜提取物;The aerial part of the saffron is dried and pulverized, and the safflower powder is extracted by secondary reflux with an aqueous ethanol solution. The extract is concentrated under reduced pressure to prepare an extract, and pure water is added to the extract to dissolve, and then ethyl acetate is used. Extraction, collecting the ethyl acetate layer, adding anhydrous magnesium sulfate to the ethyl acetate layer, stirring evenly, standing, and filtering, the obtained filtrate is concentrated under reduced pressure and dried to obtain a broccoli extract; (3)杀虫剂的制备(3) Preparation of pesticides 取步骤(1)得到的脱脂油茶籽提取物和步骤(2)得到的红花菜提取物,依次加入溶剂中,混合均匀,然后加入表面活性剂,充分混合均匀,即得杀虫剂。The defatted camellia seed extract obtained in step (1) and the saffron cauliflower extract obtained in step (2) are taken, sequentially added to a solvent, mixed uniformly, and then a surfactant is added and fully mixed to obtain an insecticide. 6.根据权利要求5所述的含有脱脂油茶籽提取物的杀虫剂的制备方法,其特征在于,所述步骤(1)中,所述乙醇水溶液中乙醇体积分数50~70%;6. The preparation method of the pesticide containing defatted camellia seed extract according to claim 5, characterized in that, in the step (1), the ethanol volume fraction in the ethanol aqueous solution is 50-70%; 第一次提取时乙醇水溶液体积为油茶籽饼粉重量的8~10倍,提取时间为4~6h,第二次提取时乙醇水溶液体积为油茶籽饼粉重量的6~8倍,提取时间为2~3h;During the first extraction, the volume of the aqueous ethanol solution is 8 to 10 times the weight of the camellia seed cake, and the extraction time is 4 to 6 hours. During the second extraction, the volume of the aqueous ethanol solution is 6 to 8 times the weight of the camellia seed cake, and the extraction time is 2~3h; 所述减压浓缩在-0 .07~-0 .08Mpa下进行。The concentration under reduced pressure is carried out under -0.07~-0.08Mpa. 7.根据权利要求5所述的含有脱脂油茶籽提取物的杀虫剂的制备方法,其特征在于,所述步骤(1)中,纯净水的用量为浸膏重量的8~10倍;7. the preparation method of the pesticide containing the degreasing camellia seed extract according to claim 5, is characterized in that, in described step (1), the consumption of pure water is 8~10 times of extract weight; 所述混合溶剂中乙醚和乙酸乙酯的体积比为1:3~4;The volume ratio of ether and ethyl acetate in the mixed solvent is 1:3-4; 混合溶剂萃取3-4次,萃取时混合溶剂的用量为浸膏重量的3~4倍;The mixed solvent is extracted 3-4 times, and the amount of the mixed solvent during extraction is 3 to 4 times the weight of the extract; 所述静置时间为20~24h。The standing time is 20-24h. 8.根据权利要求5所述的含有脱脂油茶籽提取物的杀虫剂的制备方法,其特征在于,所述步骤(2)中,所述乙醇水溶液中乙醇体积分数50~70%;8 . The preparation method of the pesticide containing defatted camellia seed extract according to claim 5 , wherein, in the step (2), the ethanol volume fraction in the ethanol aqueous solution is 50-70%; 8 . 第一次提取时乙醇水溶液体积为红花菜粉重量的8~10倍,提取时间为3~5h,第二次提取时乙醇水溶液体积为油茶籽饼粉重量的6~8倍,提取时间为2~3h;During the first extraction, the volume of the aqueous ethanol solution is 8 to 10 times the weight of the safflower powder, and the extraction time is 3 to 5 hours. During the second extraction, the volume of the aqueous ethanol solution is 6 to 8 times the weight of the camellia oleifera seed cake, and the extraction time is 2~3h; 所述减压浓缩在-0 .07~-0 .08Mpa下进行。The concentration under reduced pressure is carried out under -0.07~-0.08Mpa. 9.根据权利要求5所述的含有脱脂油茶籽提取物的杀虫剂的制备方法,其特征在于,所述步骤(2) 中,纯净水的用量为浸膏重量的8~10倍;9. The preparation method of the insecticide containing the defatted camellia seed extract according to claim 5, characterized in that, in the step (2), the consumption of purified water is 8 to 10 times the weight of the extract; 萃取进行3~4次,萃取时乙酸乙酯的用量为浸膏重量的3~4倍;The extraction is carried out 3 to 4 times, and the consumption of ethyl acetate is 3 to 4 times the weight of the extract during extraction; 所述静置时间为20~24h。The standing time is 20-24h. 10.权利要求1-4任一项所述的含有脱脂油茶籽提取物的杀虫剂用于防治茶梢蛾。10. The insecticide containing the defatted camellia seed extract according to any one of claims 1 to 4 is used for the control of Camellia sinensis.
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