CN110973164A - Ginkgolic acid soluble solution and preparation method thereof - Google Patents
Ginkgolic acid soluble solution and preparation method thereof Download PDFInfo
- Publication number
- CN110973164A CN110973164A CN201811193998.6A CN201811193998A CN110973164A CN 110973164 A CN110973164 A CN 110973164A CN 201811193998 A CN201811193998 A CN 201811193998A CN 110973164 A CN110973164 A CN 110973164A
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- Prior art keywords
- acid
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- mother
- mother medicine
- ginkgolic acid
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- 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
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- 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
- A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
- A01N37/36—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a singly bound oxygen or sulfur atom attached to the same carbon skeleton, this oxygen or sulfur atom not being a member of a carboxylic group or of a thio analogue, or of a derivative thereof, e.g. hydroxy-carboxylic acids
- A01N37/38—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a singly bound oxygen or sulfur atom attached to the same carbon skeleton, this oxygen or sulfur atom not being a member of a carboxylic group or of a thio analogue, or of a derivative thereof, e.g. hydroxy-carboxylic acids having at least one oxygen or sulfur atom attached to an aromatic ring system
- A01N37/40—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a singly bound oxygen or sulfur atom attached to the same carbon skeleton, this oxygen or sulfur atom not being a member of a carboxylic group or of a thio analogue, or of a derivative thereof, e.g. hydroxy-carboxylic acids having at least one oxygen or sulfur atom attached to an aromatic ring system having at least one carboxylic group or a thio analogue, or a derivative thereof, and one oxygen or sulfur atom attached to the same aromatic ring system
Abstract
The preparation method of the ginkgolic acid soluble solution comprises the following steps: extracting ginkgolic acid substances in the ginkgo episperm with 80% ethanol or methanol as solvent, removing impurities by water extraction method, and purifying the extract, wherein the extract contains about 31% ginkgolic acid as the mother medicine containing effective components. The preparation method of the preparation comprises the following steps: with G18And OSHeating and mixing the mother medicine and the solubilizer as solubilizer to prepare the preparation containing about 23% of ginkgolic acid serving as an effective component. 2. The botanical pesticide prepared by the method is both an insecticide and a bactericide, has no toxic or side effect on human and livestock, and has no influence on the environment.
Description
The invention relates to an extract which is separated and extracted from ginkgo episperm and takes ginkgolic acid as a main component, a botanical pesticide prepared by taking the extract as a raw material and a preparation method thereof, belonging to the technical field of preparation of botanical pesticides.
The plant-derived pesticide refers to a pesticide whose active ingredient is derived from a plant (active ingredient extracted from a plant cultivated by a special artificial plant or a wild plant). Mainly refers to a pesticide prepared by processing secondary metabolites in plants, such as lignin, flavone, alkaloid, terpene and the like. These substances are the result of the plant's own defense functions and co-evolution with pest adaptation. The multiple secondary metabolites have the activities of antifeedant, poison and poison, anesthesia, growth and development inhibition and normal behavior interference on insects, have an inhibition effect on multiple pathogenic bacteria, and are a natural biological pesticide. At present, about 30 plant-derived pesticides exist in effective registration state in China, and the total number of products is about 300. For example: 50% of pyrethrum mother drug, 70% of pyrethrum original drug, 0.6% of azadirachtin emulsifiable concentrate, 5% of matrine aqua, 2.5% of rotenone and the like.
At present, the food safety problem is a very concern of people, green safe food is urgently needed in the whole society, and the biological pesticide for preventing and treating crop diseases and insect pests is one of measures for solving the food safety problem. At present, although a plurality of plant-derived pesticides are produced in registration, the plant-derived pesticides still account for a small proportion to prevent and treat agricultural diseases and insect pests. The reason for this is that the plant raw pesticide has a low production amount and a higher price than chemical pesticides. The deep reason is that plant resources are consumed for producing the botanical pesticide, and the plant resources use land, manpower and financial resources, so that the production cost of the botanical pesticide is higher, and the commodity value of the botanical pesticide is higher. For example, azadirachtin is extracted from fruit and leaves of Azadirachta indica, and culture of Azadirachta indica requires land and manpower, and the neem can not bear fruit after 5-6 years of growth. The ginkgo episperm is the meat part outside the sclerotin and hard shell of the ginkgo seed kernel, and accounts for about two thirds of the ginkgo. In the harvesting season of ginkgo, a large amount of ginkgo episperm is discarded. The ginkgolic acid is an active ingredient extracted from ginkgo episperm, and the ginkgolic acid soluble agent is a plant-derived pesticide prepared by using ginkgolic acid as an active ingredient.
The object of the invention is thus achieved.
The preparation method of the ginkgolic acid soluble solution mother medicine comprises the following steps: sun drying the ginkgo biloba testa, removing impurities, pulverizing, adding 80% ethanol or 90% methanol at a ratio of 1: 6-8, heating to 80 deg.C, keeping the temperature for 3h, discharging the solution, filtering, concentrating the filtrate until the alcohol content is about 10%, adding deionized water with the same volume, heating to 80 deg.C-90 deg.C, stirring, standing for layering, and filtering to obtain brown black paste extract, i.e. the mother medicine. The content of the ginkgolic acid is 31 percent according to the detection of an HLPC method. The ginkgolic acid is tridecane phenolic acid and pentadecene phenolic acid.
The preparation method of the ginkgolic acid soluble agent preparation comprises the following steps: polyol ethylene oxide Polymer (trade name G)18) Alkyl phenol sulfosuccinate sodium salt (trade name O)S) Heating the above materials to 80 deg.C, and slowly pouring G18 into the above materials at a ratio of G18: 4.5: 100 under stirringStirring for 5 minutes at the temperature of 80 ℃; then according to OSMixing with the mother medicine at a ratio of 31.5: 100, and slowly adding OSPouring into the mother medicine while stirring, stirring thoroughly, and keeping at 80 deg.C for 10 min. G18、OSIn the preparation process, the solubilizer can be selected from other nonionic surfactants which have solubilization effect on the parent drug, do not influence the drug effect and do not influence the environment.
The preparation contains 23% of ginkgolic acid determined by HLPC, and the ginkgolic acid is tridecane phenolic acid and pentadecenylphenolic acid.
The parent drugs and preparations contain pentadecylphenylphenolic acid, heptadecenylphenolic acid and heptadecadienylphenylphenolic acid in addition to tridecylphenylic acid and pentadecenylphenolic acid.
The ginkgolic acid soluble solution is both an insecticide and a bactericide. The pesticide has a control rate of more than 80 percent on pests such as aphids, cabbage caterpillar thrips and the like; the control effect on cucumber downy mildew, strawberry gray mold, rice sheath blight, rice blast, tomato leaf blight and the like is more than 90%. The botanical pesticide prepared by the method has no toxic or side effect on human and livestock, has no residue, and belongs to low-toxicity pesticide. No pollution to environment.
Compared with the prior plant source pesticide production technology, the invention has the following advantages:
1. the raw material for producing the ginkgolic acid soluble solution is ginkgo episperm, according to 2016 statistics, 1400T ginkgo episperm produced in Jiangsu Houttuynian, 2500T exocperm produced in Taixing and 1300T exocperm produced in Tan tanchen, which are the yields of ginkgo episperm produced in three ginkgo production areas, and the episperms are discarded as waste. It can be seen that the raw materials for producing the pesticide are sufficient. The production of the pesticide changes the ginkgo testa into valuable. However, the raw materials for producing other plant-derived pesticides are not so many, and the plant-derived pesticides also need to be reproduced, such as matrine, azadirachtin and the like.
2. The content of the active component, namely ginkgolic acid, in the ginkgo episperm is high, about 28 percent, so that the extraction rate is high, and the production cost is reduced.
3. The pesticide has low toxicity, broad spectrum and high efficiency. Is not only an insecticide, but also a bactericide.
Claims (2)
1. Preparation method of ginkgolic acid soluble solution
(1) The preparation method of the mother medicine comprises the following steps: sun drying the ginkgo biloba testa, removing impurities, crushing, adding 80% ethanol or 90% methanol according to the proportion of 1: 6-8, heating to 80 ℃, keeping for 3-4h, discharging, filtering, concentrating the filtrate to a concentrated solution containing about 10% ethanol, adding equivalent volume of deionized water into the concentrated solution, heating to 80-90 ℃, stirring uniformly, standing until the solution is layered, filtering, and obtaining the brown black pasty mother medicine.
(2) The preparation method of the preparation comprises the following steps: polyol ethylene oxide Polymer (trade name G)18) Alkyl phenol sulfosuccinate sodium salt (trade name O)S) Heating the mother medicines to 80 deg.C respectively according to G18The ratio of the mother medicine to the mother medicine is 4.5: 100, G is firstly mixed18Slowly pouring into the mother medicine while stirring, and stirring at 80 deg.C for 5 min; then according to OSMixing the mother medicine in the ratio of 31.5 to 100, and mixing with waterSSlowly adding into the above raw materials, stirring, and holding at 80 deg.C for 10 min. G18、OSIn the preparation process, the solubilizer can be used, and other nonionic surfactants which have solubilization effect on the parent drug, do not influence the drug effect and do not influence the environment can be selected as the solubilizer for preparing the pesticide.
2. The HLPC method is used for detecting the active ingredients of the parent drug prepared by the method for preparing the ginkgolic acid soluble solution, namely tridecyl phenolic acid and pentadecenyl phenolic acid, wherein the content of the tridecyl phenolic acid and the pentadecenyl phenolic acid is about 31 percent; the preparation contains tridecyl benzene phenolic acid as effective component, and pentadecenyl benzene phenolic acid with content of about 23% detected by HLPC method. The effective components of the mother medicine and the preparation contain pentadecylphenylphenolic acid, heptadecenylphenolic acid and heptadecadienylphenylphenolic acid besides tridecylphenylphenolic acid and pentadecenylphenolic acid.
The ginkgolic acid soluble solution is not only an insecticide, but also a bactericide. The pesticide has a control rate of more than 80% on pests such as aphids, cabbage caterpillars, thrips and the like, and has a control rate of more than 90% on agricultural fungal diseases such as cucumber downy mildew, strawberry gray mold, tomato leaf blight, rice sheath blight and the like.
The pesticide prepared by the method has no toxic and side effects on human and livestock, is safe, has no residue, and has no pollution to environment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811193998.6A CN110973164A (en) | 2018-10-03 | 2018-10-03 | Ginkgolic acid soluble solution and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811193998.6A CN110973164A (en) | 2018-10-03 | 2018-10-03 | Ginkgolic acid soluble solution and preparation method thereof |
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| Publication Number | Publication Date |
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| CN110973164A true CN110973164A (en) | 2020-04-10 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201811193998.6A Withdrawn CN110973164A (en) | 2018-10-03 | 2018-10-03 | Ginkgolic acid soluble solution and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113170793A (en) * | 2021-04-28 | 2021-07-27 | 临沂市农业科学院 | Ningnanmycin and ginkgolic acid composite bactericide and preparation method thereof |
| 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 |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1382379A (en) * | 2001-10-13 | 2002-12-04 | 石启田 | Biologic agricultural chemical prepared from liposoluble extract of gingko testa and its preparing process |
| KR101332742B1 (en) * | 2012-06-12 | 2013-11-25 | 순천향대학교 산학협력단 | Mushroom fly repellent using plant extract and method of the same |
| CN103749550A (en) * | 2014-01-15 | 2014-04-30 | 东南大学 | Comprehensive utilization method of ginkgo biloba testa |
| CN106305795A (en) * | 2015-07-07 | 2017-01-11 | 石启田 | Ginkgol soluble concentrate and preparation method thereof |
| CN108041040A (en) * | 2017-12-19 | 2018-05-18 | 平昌县西兴小学 | A kind of insecticide prepared by gingko episperm active ingredient and preparation method thereof |
-
2018
- 2018-10-03 CN CN201811193998.6A patent/CN110973164A/en not_active Withdrawn
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1382379A (en) * | 2001-10-13 | 2002-12-04 | 石启田 | Biologic agricultural chemical prepared from liposoluble extract of gingko testa and its preparing process |
| KR101332742B1 (en) * | 2012-06-12 | 2013-11-25 | 순천향대학교 산학협력단 | Mushroom fly repellent using plant extract and method of the same |
| CN103749550A (en) * | 2014-01-15 | 2014-04-30 | 东南大学 | Comprehensive utilization method of ginkgo biloba testa |
| CN106305795A (en) * | 2015-07-07 | 2017-01-11 | 石启田 | Ginkgol soluble concentrate and preparation method thereof |
| CN108041040A (en) * | 2017-12-19 | 2018-05-18 | 平昌县西兴小学 | A kind of insecticide prepared by gingko episperm active ingredient and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113170793A (en) * | 2021-04-28 | 2021-07-27 | 临沂市农业科学院 | Ningnanmycin and ginkgolic acid composite bactericide and preparation method thereof |
| 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: 20200410 |
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