CN111084197A - Preparation process of ginkgol soluble agent - Google Patents

Preparation process of ginkgol soluble agent Download PDF

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Publication number
CN111084197A
CN111084197A CN201911392778.0A CN201911392778A CN111084197A CN 111084197 A CN111084197 A CN 111084197A CN 201911392778 A CN201911392778 A CN 201911392778A CN 111084197 A CN111084197 A CN 111084197A
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Prior art keywords
solution
ethanol
ginkgol
aqueous solution
paste
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Chinese (zh)
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肖建中
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Jiangsu Tenglong Biological Pharmaceutical Co Ltd
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Jiangsu Tenglong Biological Pharmaceutical Co Ltd
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Priority to CN201911392778.0A priority Critical patent/CN111084197A/en
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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
    • A01N65/06Coniferophyta [gymnosperms], e.g. cypress
    • 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
    • A01N25/00Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/02Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
    • 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

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  • 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)
  • Toxicology (AREA)
  • Medicines Containing Plant Substances (AREA)

Abstract

The invention discloses a process for preparing ginkgol soluble solution, which comprises (1) removing impurities from raw material ginkgo leaves or ginkgo testa, drying, crushing, adding acetone-water mixed solution for extraction, and concentrating the extracting solution to obtain concentrated solution; adding purified water into the concentrated solution for dilution, then performing cold precipitation and filtering to obtain clear filtrate; loading the clear filtrate on macroporous adsorbent resin, washing with water, pre-washing with ethanol, eluting with ethanol, collecting ethanol eluate, and concentrating to obtain ethanol-free paste; adding ethanol or methanol into the paste, heating, leaching, discharging the extractive solution, filtering, concentrating the filtrate, discharging, adding deionized water, exuding the aqueous solution, cooling to room temperature, layering the paste and the aqueous solution, and discarding the aqueous solution to obtain the mother medicinal material; (2) stirring and mixing the dispersing agent, the solubilizer, the emulsifier, the auxiliary agent, the organic solvent and the mother liquor, and standing to obtain a ginkgol soluble solution; the preparation process is simple and feasible, and the prepared soluble ginkgol solution has good insecticidal effect, low cost, low toxicity and environmental protection.

Description

Preparation process of ginkgol soluble agent
Technical Field
The invention relates to a preparation process, in particular to a preparation process of a ginkgol soluble agent.
Background
The ginkgol is a plant-derived pesticide-ginkgol soluble solution prepared from components such as ginkgol separated and extracted from ginkgo leaves and ginkgo testa. The botanical pesticide has the functions of broad-spectrum prevention and control of crop diseases and insect pests, has the characteristics of broad spectrum, low toxicity, high efficiency, good safety and the like, has better prevention and control effects on apple rot, tomato gray mold, vegetable early blight and the like, and has the insecticidal efficacy. The product is a green pesticide and has great popularization value. The ginkgol is a botanical pesticide bactericide, is particularly suitable for pest control in greenhouse planting, green food planting and the like, and highlights the concept of green environmental protection, so that the ginkgol has a very wide market space under the trend that the country increasingly attaches importance to environmental protection, particularly agricultural production safety and environmental protection, and meanwhile, enterprises can be promoted to establish new environment-friendly images.
Disclosure of Invention
The invention aims to solve the technical problem that the preparation process of the ginkgol soluble solution is simple and feasible, and the prepared ginkgol soluble solution has good insecticidal effect, low cost, low toxicity and environmental protection.
The technical scheme for solving the technical problems is as follows:
a preparation process of a ginkgol soluble agent specifically comprises the following steps:
(1) preparation of mother medicine
Removing impurities from folium Ginkgo or testa Ginkgo, drying, pulverizing, extracting with 50-60% acetone water mixed solution for 2-3 times, and concentrating the extractive solution to obtain concentrated solution;
adding purified water into the concentrated solution to dilute to 30-40 deg.C, then cold precipitating at 4-9 deg.C for 10-12h, and filtering to obtain clear filtrate;
loading the clear filtrate on macroporous adsorbent resin, washing with water, pre-washing with 14% ethanol, eluting with 50-60% ethanol, collecting ethanol eluate, and concentrating to obtain ethanol-free paste;
taking the paste, adding 85-90% ethanol or 92-96% methanol, heating to 75-79 deg.C, leaching, discharging the extractive solution, filtering, concentrating the filtrate until the ethanol content is 7-8%, discharging, adding equivalent volume of deionized water, heating to 91-95 deg.C, maintaining for 1-2 hr, exuding the aqueous solution, cooling to room temperature, completely layering the paste and the aqueous solution, and discarding the aqueous solution to obtain the final product;
(2) preparation of a soluble solution
Stirring and mixing the diffusant, the solubilizer, the emulsifier, the auxiliary agent, the organic solvent and the mother liquor at the stirring speed of 30-50r/min for 10-20min to ensure that the diffusant, the solubilizer, the emulsifier, the auxiliary agent, the organic solvent and the mother liquor are mixed uniformly in a working time, and standing to obtain the ginkgol soluble solution.
The invention further defines the technical scheme as follows:
in the preparation process of the ginkgol soluble solution, the concentration in the step (1) is carried out to ensure that the content of acetone is 1-4%.
In the preparation process of the ginkgol soluble solution, the amount of 85-90% ethanol or 92-96% methanol added is 8-10 times of that of the paste.
In the preparation process of the ginkgol soluble agent, when the raw material is ginkgo episperm, the specific operation is as follows: removing rotten and rotten seeds from the peeled mature ginkgo fruits, vacuum drying at 50-80 deg.C for 24-48h, pulverizing, and sieving with 60-80 mesh sieve.
In the preparation process of the ginkgol soluble solution, the diffusant, the solubilizer, the emulsifier, the auxiliary agent, the organic solvent and the mother liquor in the step (2) are respectively as follows by mass percent:
mother medicine: 70-80 parts of a dispersing agent: 20-25 parts of a solubilizer: 20-30 parts of an emulsifier: 10-12 parts of an auxiliary agent: 3-7 parts of organic solvent: 10-15 parts.
In the preparation process of the ginkgol soluble agent, the emulsifier is Tween 80 or calcium dodecyl benzene sulfonate aqueous solution.
In the preparation process of the ginkgol soluble solution, the organic solvent is one or more of dimethyl sulfoxide, N-dimethylformamide, acetone and ethanol.
In the preparation process of the ginkgol soluble solution, the auxiliary agent is a wetting agent and a dispersing agent which are mixed in equal proportion, wherein:
the wetting agent is sodium dodecyl sulfate; the dispersant is sodium lignosulfonate.
In the preparation process of the ginkgol soluble agent, the solubilizer is fatty alcohol-polyoxyethylene ether.
The invention has the beneficial effects that:
the preparation of the mother medicine of the invention uses ethanol with a concentration of more than 80 percent or methanol with a concentration of more than 90 percent to extract the ginkgol and other extracts by an extraction method. Removing impurities by water extraction method, and purifying ginkgol as mother medicine. The preparation method comprises adding dispersing agent and solubilizer into the parent drug, stirring and heating to mix well to obtain the soluble ginkgol solution. The reaction condition is mild, and no three wastes are discharged.
The invention has rich raw material resources and changes waste into valuable. A plurality of gingko production bases exist in China, 30 ten thousand tons of gingko leaves and 4000 ten thousand kilograms of abandoned gingko seed coats are produced every year, and the method ensures that the rich agricultural resources are utilized, changes waste into valuable and does not need to consume other plant resources; the extraction rate of the ginkgol extract is high, 25-30%, and the content of the ginkgol in the extract is over 85%. The cost for producing the botanical pesticide is reduced due to the fact that only existing resources are utilized, waste is changed into valuable, the extraction rate of the ginkgol is high, and the like.
The plant pesticide-ginkgol soluble agent has the function of broad-spectrum prevention and control of crop diseases and insect pests, and can be used for broad-spectrum disinsection and broad-spectrum inhibition and killing of fungus diseases.
Meanwhile, the invention reasonably utilizes the special insecticidal and bactericidal action of ginkgolic acids in the testa to lay a foundation for developing ginkgolic acids into biological pesticides; the developed pesticide replaces the traditional synthetic pesticide, and the natural pesticide is natural, low in toxicity, environment-friendly and pollution-free, so that the ecological system is better protected.
Detailed Description
Example 1
The embodiment provides a preparation process of a ginkgol soluble agent, which specifically comprises the following steps:
(1) preparation of mother medicine
Removing impurities from folium Ginkgo or testa Ginkgo, drying, pulverizing, extracting with 50% acetone water mixed solution for 2 times, and concentrating the extractive solution to obtain concentrated solution;
adding purified water into the concentrated solution to dilute the solution to 30 ℃, then performing cold precipitation at 4 ℃ for 10 hours, and filtering to obtain clear filtrate;
passing the clear filtrate through macroporous adsorbent resin, washing with water, pre-washing with 14% ethanol, eluting with 50% ethanol, collecting ethanol eluate, and concentrating to obtain ethanol-free paste;
taking the paste, adding 85% ethanol or 92% methanol, heating to 75 deg.C, leaching, discharging the extractive solution, filtering, concentrating the filtrate until the alcohol content is 7% and discharging, adding equivalent volume of deionized water, heating to 91 deg.C, maintaining for 1 hr, exuding the aqueous solution, cooling to room temperature until the paste and the aqueous solution are completely layered, and discarding the aqueous solution to obtain the final product;
(2) preparation of a soluble solution
Stirring and mixing the diffusant, the solubilizer, the emulsifier, the auxiliary agent, the organic solvent and the mother liquor at the stirring speed of 30r/min for 10min to fully and uniformly mix the components with overtime, and standing to obtain the ginkgol soluble solution.
In this example, step (1) concentration resulted in an acetone content of 1%.
In this example, 85% ethanol or 92% methanol was added in an amount 8 times that of the paste.
In this embodiment, when the raw material is ginkgo episperm, the specific operations are as follows: removing rotten and rotten seeds from the peeled mature ginkgo fruits, then vacuum-drying at 50 ℃ for 24h, crushing and sieving by a 60-mesh sieve.
In this embodiment, the dispersing agent, the solubilizer, the emulsifier, the auxiliary agent, the organic solvent, and the mother liquor in step (2) are, by mass:
mother medicine: 70 parts of dispersing agent: 20 parts, solubilizer: 20 parts of an emulsifier: 10 parts of an auxiliary agent: 3 parts, organic solvent: 10 parts.
In this example, the emulsifier is Tween 80; the organic solvent is dimethyl sulfoxide.
In this example, the adjuvant is a wetting agent and a dispersing agent mixed in equal proportions, wherein:
the wetting agent is sodium dodecyl sulfate; the dispersant is sodium lignosulfonate.
In this embodiment, the solubilizer is fatty alcohol-polyoxyethylene ether.
Example 2
The embodiment provides a preparation process of a ginkgol soluble agent, which specifically comprises the following steps:
(1) preparation of mother medicine
Removing impurities from folium Ginkgo or testa Ginkgo, drying, pulverizing, extracting with 60% acetone water mixed solution for 3 times, and concentrating the extractive solution to obtain concentrated solution;
adding purified water into the concentrated solution to dilute the solution to 40 ℃, then performing cold precipitation at 9 ℃ for 12 hours, and filtering to obtain clear filtrate;
passing the clear filtrate through macroporous adsorbent resin, washing with water, pre-washing with 14% ethanol, eluting with 60% ethanol, collecting ethanol eluate, and concentrating to obtain ethanol-free paste;
taking the paste, adding 90% ethanol or 96% methanol, heating to 79 deg.C, leaching, discharging the extractive solution, filtering, concentrating the filtrate until the alcohol content is 8%, discharging, adding equivalent volume of deionized water, heating to 95 deg.C, maintaining for 2 hr, exuding the aqueous solution, cooling to room temperature until the paste and the aqueous solution are completely layered, and discarding the aqueous solution to obtain the final product;
(2) preparation of a soluble solution
Stirring and mixing the diffusant, the solubilizer, the emulsifier, the auxiliary agent, the organic solvent and the mother liquor at the stirring speed of 50r/min for 20min to fully and uniformly mix the components with overtime, and standing to obtain the ginkgol soluble solution.
In this example, step (1) concentration resulted in an acetone content of 4%.
In this example, 90% ethanol or 96% methanol was added in an amount 10 times that of the paste.
In this embodiment, when the raw material is ginkgo episperm, the specific operations are as follows: removing rotten and rotten seeds from the peeled mature ginkgo fruits, vacuum drying at 50-80 deg.C for 24-48h, pulverizing, and sieving with 60-80 mesh sieve.
In this embodiment, the dispersing agent, the solubilizer, the emulsifier, the auxiliary agent, the organic solvent, and the mother liquor in step (2) are, by mass:
mother medicine: 80 parts, dispersing agent: 25 parts, solubilizer: 30 parts, emulsifier: 12 parts of auxiliary agent: 7 parts, organic solvent: 15 parts.
In this example, the emulsifier is an aqueous solution of calcium dodecylbenzenesulfonate; the organic solvent is N, N-dimethylformamide.
In this example, the adjuvant is a wetting agent and a dispersing agent mixed in equal proportions, wherein:
the wetting agent is sodium dodecyl sulfate; the dispersant is sodium lignosulfonate.
In this embodiment, the solubilizer is fatty alcohol-polyoxyethylene ether.
Example 3
The embodiment provides a preparation process of a ginkgol soluble agent, which specifically comprises the following steps:
(1) preparation of mother medicine
Removing impurities from folium Ginkgo or testa Ginkgo, drying, pulverizing, extracting with 55% acetone water mixed solution for 2 times, and concentrating the extractive solution to obtain concentrated solution;
adding purified water into the concentrated solution to dilute the solution to 35 ℃, then performing cold precipitation at 7 ℃ for 11 hours, and filtering to obtain clear filtrate;
passing the clear filtrate through macroporous adsorbent resin, washing with water, pre-washing with 14% ethanol, eluting with 55% ethanol, collecting ethanol eluate, and concentrating to obtain ethanol-free paste;
taking the paste, adding 88% ethanol or 94% methanol, heating to 78 deg.C, leaching, discharging the extractive solution, filtering, concentrating the filtrate until the alcohol content is 7% and discharging, adding equivalent volume of deionized water, heating to 92 deg.C, maintaining for 1 hr, exuding the aqueous solution, cooling to room temperature until the paste and the aqueous solution are completely layered, and discarding the aqueous solution to obtain the mother medicine;
(2) preparation of a soluble solution
Stirring and mixing the diffusant, the solubilizer, the emulsifier, the auxiliary agent, the organic solvent and the mother liquor at the stirring speed of 40r/min for 15min to fully and uniformly mix the components with overtime, and standing to obtain the ginkgol soluble solution.
In this example, step (1) concentration resulted in an acetone content of 1-4%.
In this example, 88% ethanol or 94% methanol was added in an amount 9 times that of the paste.
In this embodiment, when the raw material is ginkgo episperm, the specific operations are as follows: removing the deteriorated and rotten outer seeds of the mature ginkgo fruits, then carrying out vacuum drying for 38h at the temperature of 60 ℃, and crushing and screening by a sieve of 70 meshes.
In this embodiment, the dispersing agent, the solubilizer, the emulsifier, the auxiliary agent, the organic solvent, and the mother liquor in step (2) are, by mass:
mother medicine: 75 parts of dispersing agent: 22 parts, solubilizer: 25 parts of an emulsifier: 11 parts of an auxiliary agent: 5 parts, organic solvent: 13 parts.
In this example, the emulsifier is Tween 80; the organic solvent is acetone.
In this example, the adjuvant is a wetting agent and a dispersing agent mixed in equal proportions, wherein:
the wetting agent is sodium dodecyl sulfate; the dispersant is sodium lignosulfonate.
In this embodiment, the solubilizer is fatty alcohol-polyoxyethylene ether.
In addition to the above embodiments, the present invention may have other embodiments. All technical solutions formed by adopting equivalent substitutions or equivalent transformations fall within the protection scope of the claims of the present invention.

Claims (9)

1. A preparation process of a ginkgol soluble agent is characterized by comprising the following steps:
(1) preparation of mother medicine
Removing impurities from folium Ginkgo or testa Ginkgo, drying, pulverizing, extracting with 50-60% acetone water mixed solution for 2-3 times, and concentrating the extractive solution to obtain concentrated solution;
adding purified water into the concentrated solution to dilute to 30-40 deg.C, then cold precipitating at 4-9 deg.C for 10-12h, and filtering to obtain clear filtrate;
loading the clear filtrate on macroporous adsorbent resin, washing with water, pre-washing with 14% ethanol, eluting with 50-60% ethanol, collecting ethanol eluate, and concentrating to obtain ethanol-free paste;
taking the paste, adding 85-90% ethanol or 92-96% methanol, heating to 75-79 deg.C, leaching, discharging the extractive solution, filtering, concentrating the filtrate until the ethanol content is 7-8%, discharging, adding equivalent volume of deionized water, heating to 91-95 deg.C, maintaining for 1-2 hr, exuding the aqueous solution, cooling to room temperature, completely layering the paste and the aqueous solution, and discarding the aqueous solution to obtain the final product;
(2) preparation of a soluble solution
Stirring and mixing the diffusant, the solubilizer, the emulsifier, the auxiliary agent, the organic solvent and the mother liquor at the stirring speed of 30-50r/min for 10-20min to ensure that the diffusant, the solubilizer, the emulsifier, the auxiliary agent, the organic solvent and the mother liquor are mixed uniformly in a working time, and standing to obtain the ginkgol soluble solution.
2. The process of claim 1, wherein the aqueous solution of ginkgols is prepared by: the concentration in step (1) is carried out to ensure that the content of acetone is 1-4%.
3. The process of claim 1, wherein the aqueous solution of ginkgols is prepared by: the amount of 85-90% ethanol or 92-96% methanol added is 8-10 times of the paste.
4. The process of claim 1, wherein the aqueous solution of ginkgols is prepared by: when the raw material is ginkgo episperm, the specific operation is as follows: removing rotten and rotten seeds from the peeled mature ginkgo fruits, vacuum drying at 50-80 deg.C for 24-48h, pulverizing, and sieving with 60-80 mesh sieve.
5. The process of claim 1, wherein the aqueous solution of ginkgols is prepared by: in the step (2), the dispersing agent, the solubilizer, the emulsifier, the auxiliary agent, the organic solvent and the mother liquor are respectively as follows by mass percent:
mother medicine: 70-80 parts of a dispersing agent: 20-25 parts of a solubilizer: 20-30 parts of an emulsifier: 10-12 parts of an auxiliary agent: 3-7 parts of organic solvent: 10-15 parts.
6. The process of claim 5, wherein the reaction mixture comprises: the emulsifier is Tween 80 or calcium dodecyl benzene sulfonate water solution.
7. The process of claim 5, wherein the reaction mixture comprises: the organic solvent is one or more of dimethyl sulfoxide, N-dimethylformamide, acetone and ethanol.
8. The process of claim 5, wherein the reaction mixture comprises: the auxiliary agent is a wetting agent and a dispersing agent which are mixed in equal proportion, wherein:
the wetting agent is sodium dodecyl sulfate; the dispersant is sodium lignosulphonate.
9. The process of claim 5, wherein the reaction mixture comprises: the solubilizer is fatty alcohol-polyoxyethylene ether.
CN201911392778.0A 2019-12-30 2019-12-30 Preparation process of ginkgol soluble agent Pending CN111084197A (en)

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CN113826646A (en) * 2021-08-15 2021-12-24 江苏小禾生物技术研究院有限公司 Ginkgolic acid solution and preparation method thereof

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Application publication date: 20200501