CN115769825A

CN115769825A - Preparation method of high-content ginkgolic acid plant source pesticide

Info

Publication number: CN115769825A
Application number: CN202111085089.2A
Authority: CN
Inventors: 石启田
Original assignee: Individual
Current assignee: Individual
Priority date: 2021-09-08
Filing date: 2021-09-08
Publication date: 2023-03-10

Abstract

The invention relates to the field of preparation of plant-derived pesticides, and particularly relates to a preparation method of a high-content ginkgolic acid plant-derived pesticide. 1. The original drug is prepared by taking ginkgo episperm as a raw material and carrying out extraction, filtration, concentration, filtration, adsorption, elution and concentration. 2. The preparation method comprises respectively heating raw materials and surfactant, and mixing the raw materials and surfactant in proportion and order.

Description

Preparation method of high-content ginkgolic acid plant source pesticide

The invention relates to the field of preparation of plant-derived pesticides, and particularly relates to a preparation method of a high-content ginkgolic acid plant-derived pesticide.

The plant-derived pesticide refers to a pesticide (active ingredient extracted from a special artificial culture or wild plant) whose active ingredient is derived from a plant body. Mainly refers to a pesticide processed by secondary metabolites in plants, such as lignin, flavone, alkaloid and terpene. These substances are the result of the co-evolution of the plant's own defense function and adaptation to the evolution of pests. The multiple secondary metabolites have the activities of antifeedant, poison, anesthesia, growth and development inhibition and normal behavior interference on insects, have a resisting effect on multiple pathogenic bacteria, and are a natural biological pesticide. At present, about 30 active ingredients of the plant-derived pesticides in an effective registration state at home and abroad are available, and the total number of products is about 300. For example, 50% pyrethrum is registered by the Australian pyrethrum company and 0.6% Celite cream is registered by the Jiukang Biotechnology Limited liability company. The preparation method of soluble solution of ginkgo biloba extract containing 23% of ginkgolic acid registered by Xuzhou Jindi agricultural chemical company Limited comprises the following steps: 1. preparing a mother medicine: sun drying testa Ginkgo, pulverizing, extracting, filtering, concentrating, and purifying. 2. Preparation of the preparation: heating the mother medicine, humectant and surfactant respectively, sequentially adding the humectant and surfactant into the mother medicine, and stirring.

At present, the problem of food safety is a great concern of people, and the use of biopesticides for preventing and treating crop diseases and insect pests is one of important measures for producing green organic agricultural products. Although there are many registered production of plant-derived pesticides, the use of plant-derived pesticides still accounts for a small proportion in controlling pests. The first reason is that agricultural resources are consumed for producing the plant-derived pesticide, and land, manpower and material resources are required for producing the agricultural resources, so that the production cost of the plant-derived pesticide is increased, and the commodity price is high. For example, the production of neem requires the first planting of the neem. The second reason is that many plant-derived pesticides have low content of active ingredients, so that the pesticide effect is poor.

The invention aims to overcome two defects of the current plant source pesticide production, and the plant source pesticide with high content of ginkgolic acid is produced by utilizing the ginkgo testa, so that the plant source pesticide with low production cost, high content of effective components, high efficiency and broad spectrum is created.

The invention is realized in such a way

1. Preparation of technical material

(1) The extraction is carried out by drying the ginkgo episperm, removing impurities, crushing, adding into 80% ethanol or methanol over 95% 6 times, heating to 80 ℃, keeping temperature for 3h, stirring once for 15-20 min. The extract is discharged.

(2) Filtering with 800-1000 mesh filter, and filtering the extractive solution.

(3) Concentrating the filtrate to 50% ethanol, and recovering ethanol.

(4) Filtering with 800-1000 mesh filter.

(5) Adsorbing the filtrate with macroporous adsorbent resin such as D101. And discarding the adsorbed liquid, and recovering ethanol from the adsorbed liquid.

(6) The resin is washed by deionized water until colorless. Then the resin is washed by 10% ethanol solution until the resin is colorless, and the washing solution is discarded. Finally, eluting with 90% ethanol, and collecting the eluent.

(7) Concentrating the eluate, and recovering ethanol to obtain crude drug.

2. Preparation of the formulations

Heating the crude drug and surfactant to 80 deg.C, respectively, and adding lipophilic surfactant with low HLB value, such as polyalcohol ethylene oxide polymer, into the crude drug at a ratio of crude drug to surfactant = 20: 1. Stirring for 5-10 min. Adding hydrophilic surfactant with high HLB value such as alkylphenol ether sulfosuccinate sodium salt at a ratio of raw material to surfactant = 20: 7, stirring, and stirring for 5-10 min.

Compared with the prior botanical pesticide, the invention has the following advantages:

1. the plant source pesticide prepared by the invention has high content of active ingredients, and has high pesticide effect due to the high content of the active ingredients.

2. The required raw materials are abundant, and the waste is utilized, so the production cost is low.

3. The pesticide developed by the invention has the functions of efficiently and broadly preventing and treating crop diseases and insect pests, and can kill insects and pathogenic fungi.

Examples

1000 kg of dry ginkgo testa is used as a raw material to prepare the botanical pesticide with high content of ginkgolic acid.

1. Preparation of technical material

(1) The extraction method comprises the steps of removing impurities from 1000 kg of dry ginkgo biloba sarcotesta, crushing, putting into an extraction tank, adding 7500 kg of 80% ethanol into the extraction tank, heating to 80 ℃, stirring once every 15-20 minutes, keeping the temperature for 3h, and discharging the extracting solution.

(2) Filtering with 800 mesh filter.

(3) Concentrating, placing the filtrate into a concentrating tank, heating the concentrated solution to 50% ethanol, and recovering ethanol.

(4) Filtering with 800 mesh filter.

(5) After the D101 macroporous resin column is pretreated by adsorption, the filtered concentrated filtrate flows through the adsorption column at a proper flow rate, and effluent is discarded. Treating the effluent liquid and recovering the ethanol.

(6) Eluting with deionized water until colorless, and eluting with 10% ethanol until colorless. And discarding the cleaning solution. And finally eluting the resin column by using 90% ethanol, and collecting eluent.

(7) Concentrating, concentrating the eluate in a concentrating tank, heating, concentrating, and recovering ethanol. 167 kg of thin paste raw medicine is obtained.

2. Preparation of the formulations

Respectively heating the original drug and the surfactant to 80 ℃, adding 8.4 kg of polyol ethylene oxide polymer into the original drug while stirring, continuously stirring for 10 minutes, then adding 59 kg of alkylphenol ether sulfosuccinate sodium salt while stirring, continuously stirring for 10 minutes, discharging and filling.

Claims

1. The extraction method comprises drying the testa Ginkgo, removing impurities, pulverizing, adding 6 times of 80% ethanol or methanol over 95%, heating to 80 deg.C, maintaining for 3 hr, stirring for 15-20 min, and stirring.

2. Filtering with 800-1000 mesh filter.

3. Concentrating the filtrate to 50% ethanol.

4. Filtering with 800-1000 mesh filter.

5. Adsorbing with macroporous resin such as D101, discarding the adsorbed liquid, and recovering ethanol from the adsorbed liquid.

6. The resin is washed by deionized water until the resin is colorless, then by 10 percent ethanol until the resin is colorless, and the washing liquid is discarded. Finally, eluting the ginkgolic acid by using 90% ethanol, and collecting the eluent.

7. Concentrating the eluent, and recovering ethanol to obtain the crude drug.

8. Separately heating the raw drug and surfactant to 80 deg.C, adding lipophilic surfactant with low HLB value, such as polyalcohol ethylene oxide polymer, etc., into the raw drug at a ratio of raw drug to surfactant = 20: 1, stirring, and stirring for 5-10 min. Further adding hydrophilic surfactant with high HLB value, such as alkylphenol ether sulfosuccinate sodium salt, at a ratio of raw material to surfactant = 20: 7, stirring, and stirring for 5-10 min.