CN108531526A - A kind of Folium Artemisiae Argyi extract and the preparation method and application thereof - Google Patents

A kind of Folium Artemisiae Argyi extract and the preparation method and application thereof Download PDF

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Publication number
CN108531526A
CN108531526A CN201810461118.2A CN201810461118A CN108531526A CN 108531526 A CN108531526 A CN 108531526A CN 201810461118 A CN201810461118 A CN 201810461118A CN 108531526 A CN108531526 A CN 108531526A
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folium artemisiae
artemisiae argyi
argyi extract
preparation
extract
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CN201810461118.2A
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CN108531526B (en
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周培
束影
蒋泽慧
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HUBEI AIAITIE HEALTH TECHNOLOGY CO.,LTD.
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Yangzhou Polytechnic Institute
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    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P19/00—Preparation of compounds containing saccharide radicals
    • C12P19/44—Preparation of O-glycosides, e.g. glucosides
    • C12P19/60—Preparation of O-glycosides, e.g. glucosides having an oxygen of the saccharide radical directly bound to a non-saccharide heterocyclic ring or a condensed ring system containing a non-saccharide heterocyclic ring, e.g. coumermycin, novobiocin
    • C12P19/62—Preparation of O-glycosides, e.g. glucosides having an oxygen of the saccharide radical directly bound to a non-saccharide heterocyclic ring or a condensed ring system containing a non-saccharide heterocyclic ring, e.g. coumermycin, novobiocin the hetero ring having eight or more ring members and only oxygen as ring hetero atoms, e.g. erythromycin, spiramycin, nystatin
    • C12P19/626—Natamycin; Pimaricin; Tennecetin
    • 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
    • A01N43/90—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P17/00—Preparation of heterocyclic carbon compounds with only O, N, S, Se or Te as ring hetero atoms
    • C12P17/18—Preparation of heterocyclic carbon compounds with only O, N, S, Se or Te as ring hetero atoms containing at least two hetero rings condensed among themselves or condensed with a common carbocyclic ring system, e.g. rifamycin
    • C12P17/188—Heterocyclic compound containing in the condensed system at least one hetero ring having nitrogen atoms and oxygen atoms as the only ring heteroatoms

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  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Wood Science & Technology (AREA)
  • Engineering & Computer Science (AREA)
  • Zoology (AREA)
  • General Health & Medical Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Bioinformatics & Cheminformatics (AREA)
  • Genetics & Genomics (AREA)
  • General Chemical & Material Sciences (AREA)
  • Biochemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Engineering & Computer Science (AREA)
  • Biotechnology (AREA)
  • Microbiology (AREA)
  • Agronomy & Crop Science (AREA)
  • Pest Control & Pesticides (AREA)
  • Plant Pathology (AREA)
  • Dentistry (AREA)
  • Environmental Sciences (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
  • Medicines Containing Plant Substances (AREA)

Abstract

The present invention relates to a kind of Folium Artemisiae Argyi extract and the preparation method and application thereof, the preparation method of the Folium Artemisiae Argyi extract includes the following steps：(1) it takes dry folium artemisiae argyi to crush, after sterilization processing, is placed in sterile fermentation tank, glucose then is added and yeast powder after mixing seals fermentation tank, at 20 25 DEG C, spontaneous fermentation 20 25 days, obtains fermentate；(2) the fermentate acetone soak for obtaining step (1), filtering, after filtrate concentration, through macroporous resin adsorption, the ethanol solution for being 60 70% with volume fraction elutes, and collects 56 times of column volume eluents, then through activated carbon decolorizing, concentration, dry the Folium Artemisiae Argyi extract.

Description

A kind of Folium Artemisiae Argyi extract and the preparation method and application thereof
Technical field
The invention belongs to the fields of extracting, and in particular to a kind of Folium Artemisiae Argyi extract and the preparation method and application thereof.
Background technology
Folium artemisiae argyi is composite family (Compositae) artemisia herbaceos perennial Chinese mugwort (Artemisia argyi Levl.et Vant. dried leaf), compound isolated from folium artemisiae argyi is more than 100 kinds at present, including terpene, flavones, Phenylpropanoid Glycosides, The chemical compositions such as aromatic acid (aldehyde), steroidal and aliphatic acid.Show extensive bioactivity, such as analgesia, anti-inflammatory, anti-freezing, anti- Tumour etc.；Wherein volatile argyi leaf oil also has certain except mite effect.However there has been no about Folium Artemisiae Argyi extract or active ingredient Object reports the killing of agricultural pests (such as aphid, mythimna separata).The present invention provide a kind of folium artemisiae argyi extractive from fermentative and its activity at Divide to the application in terms of agricultural insect pests control.
Invention content
The present invention provides a kind of Folium Artemisiae Argyi extract, it is characterised in that the preparation method of the Folium Artemisiae Argyi extract includes following step Suddenly：
(1) take dry folium artemisiae argyi to crush, after sterilization processing, be placed in sterile fermentation tank, then be added glucose and Yeast powder after mixing seals fermentation tank, and at 20-25 DEG C, spontaneous fermentation 20-25 days, obtains fermentate；
(2) the fermentate acetone soak for obtaining step (1), filtering after filtrate concentration, through macroporous resin adsorption, are used Volume fraction be 60-70% ethanol solution elute, collect 5-6 times of column volume eluent, then through activated carbon decolorizing, concentration, do It is dry to obtain the Folium Artemisiae Argyi extract.
The dosage of glucose is the 10%-15% of folium artemisiae argyi quality in step (1), and the dosage of yeast powder is folium artemisiae argyi quality 3%-5%；
The dosage of acetone is that every kilogram of folium artemisiae argyi uses 8-10L acetone in step (2)；The acetone soak time, preferred 20-24 was small When；The one kind of the model of the macroreticular resin in AB-8, D101.
Another embodiment of the present invention provides the preparation method of above-mentioned Folium Artemisiae Argyi extract, it is characterised in that including walking as follows Suddenly：
(1) take dry folium artemisiae argyi to crush, after sterilization processing, be placed in sterile fermentation tank, then be added glucose and Yeast powder after mixing seals fermentation tank, and at 20-25 DEG C, spontaneous fermentation 20-25 days, obtains fermentate；
(2) the fermentate acetone soak for obtaining step (1), filtering after filtrate concentration, through macroporous resin adsorption, are used Volume fraction be 60-70% ethanol solution elute, collect 5-6 times of column volume eluent, then through activated carbon decolorizing, concentration, do It is dry to obtain the Folium Artemisiae Argyi extract.
The dosage of glucose is the 10%-15% of folium artemisiae argyi quality in step (1), and the dosage of yeast powder is folium artemisiae argyi quality 3%-5%；
The dosage of acetone is that every kilogram of folium artemisiae argyi uses 8-10L acetone in step (2)；The acetone soak time, preferred 20-24 was small When；The one kind of the model of the macroreticular resin in AB-8, D101.
Another embodiment of the present invention provides application of the above-mentioned Folium Artemisiae Argyi extract in preventing agricultural pests.The agricultural The preferred aphid of pest, mythimna separata.
Another embodiment of the present invention provides application of the above-mentioned Folium Artemisiae Argyi extract in preparing insecticide.The insecticide It is preferred that killing aphid, mythimna separata.
Another embodiment of the present invention provides a kind of insecticide, it is characterised in that the insecticide is extracted with above-mentioned folium artemisiae argyi Object is as active constituent.The insecticide preferably kills aphid, mythimna separata.
Another embodiment of the present invention provides the compound or its salt of Formulas I structure, it is characterised in that the Formulas I structure is such as Under：
Another embodiment of the present invention provides the preparation method of the compound of above-mentioned Formulas I structure, it is characterised in that including Following steps：
Above-mentioned Folium Artemisiae Argyi extract obtains the compound of Formulas I structure through normal-phase silica gel column chromatography.
The normal-phase silica gel column chromatography, the preferred 200-300 mesh of mesh number of silica gel, eluant, eluent preferred volume ratio are 1:10-12 Ethyl acetate/petroleum ether mixed solvent.
The preparation method of the Folium Artemisiae Argyi extract includes the following steps：
(1) take dry folium artemisiae argyi to crush, after sterilization processing, be placed in sterile fermentation tank, then be added glucose and Yeast powder after mixing seals fermentation tank, and at 20-25 DEG C, spontaneous fermentation 20-25 days, obtains fermentate；
(2) the fermentate acetone soak for obtaining step (1), filtering after filtrate concentration, through macroporous resin adsorption, are used Volume fraction be 60-70% ethanol solution elute, collect 5-6 times of column volume eluent, then through activated carbon decolorizing, concentration, do It is dry to obtain the Folium Artemisiae Argyi extract.
The dosage of glucose is the 10%-15% of folium artemisiae argyi quality in step (1), and the dosage of yeast powder is folium artemisiae argyi quality 3%-5%；
The dosage of acetone is that every kilogram of folium artemisiae argyi uses 8-10L acetone in step (2)；The acetone soak time, preferred 20-24 was small When；The one kind of the model of the macroreticular resin in AB-8, D101.
Another embodiment of the present invention provides compound or its salt the answering in preventing agricultural pests of above-mentioned Formulas I structure With.The preferred aphid of the agricultural pests, mythimna separata.
Another embodiment of the present invention provides compound or its salt the answering in preparing insecticide of above-mentioned Formulas I structure With.The insecticide preferably kills aphid, mythimna separata.
Another embodiment of the present invention provides a kind of insecticide, it is characterised in that the insecticide is with above-mentioned Formulas I structure Compound or its salt as active constituent.The insecticide preferably kills aphid, mythimna separata.
Specific implementation mode
For the ease of a further understanding of the present invention, examples provided below has done more detailed description to it.But It is that these embodiments are only not supposed to be a limitation to the present invention or implementation principle for being better understood from invention, reality of the invention The mode of applying is not limited to the following contents.
Embodiment 1
(1) it takes dry folium artemisiae argyi (1.0kg) to crush, after sterilization processing, is placed in sterile fermentation tank, Portugal is then added Grape sugar (100g) and yeast powder (30g) after mixing seal fermentation tank, and at 20-25 DEG C, spontaneous fermentation 20 days, obtains Fermentate；
(2) fermentate for obtaining step (1) is impregnated 24 hours with acetone (8L), filtering, after filtrate concentration, through AB-8 types Macroporous resin adsorption, the ethanol solution for being 60% with volume fraction elute, and collect 6 times of column volume eluents, then de- through activated carbon Color, concentration, dry the Folium Artemisiae Argyi extract (hereinafter referred to as product A).
Embodiment 2
(1) it takes dry folium artemisiae argyi (1.0kg) to crush, after sterilization processing, is placed in sterile fermentation tank, Portugal is then added Grape sugar (150g) and yeast powder (50g) after mixing seal fermentation tank, and at 20-25 DEG C, spontaneous fermentation 25 days, obtains Fermentate；
(2) fermentate for obtaining step (1) is impregnated 20 hours with acetone (10L), filtering, after filtrate concentration, through D101 Type macroporous resin adsorption, the ethanol solution for being 70% with volume fraction elute, and collect 5 times of column volume eluents, then through activated carbon Decoloration, concentration, dry the Folium Artemisiae Argyi extract (hereinafter referred to as product B).
Embodiment 3
(1) it takes dry folium artemisiae argyi (1.0kg) to crush, is impregnated 24 hours with acetone (8L), filtering, after filtrate concentration, through AB- 8 type macroporous resin adsorptions, the ethanol solution for being 60% with volume fraction elute, and collect 6 times of column volume eluents, then through activated carbon Decoloration, concentration, dry products C (products C does not find compound of formula I through TLC detections).
Embodiment 4
Take product A (1.0g) through normal-phase silica gel column chromatography, the mesh number 200-300 mesh of silica gel, eluant, eluent is ethyl acetate/stone Oily ether=1/10-1/12 obtains the compound (382mg) of Formulas I structure, HPLC purity 98.0%.
Show that Formulas I has the following structure through MS, one-dimensional, two-dimentional NMR data：Formulas I is only listed below ESIMS and1H,13C NMR datas.Structural identification data：ESIMS m/z 154.09[M+H]+；1H,13C NMR datas are seen below Table.
Table 11H,13C NMR datas (CDCl3, 600/150MHz)
Embodiment 5
Take product B (1.0g) through normal-phase silica gel column chromatography, the mesh number 200-300 mesh of silica gel, eluant, eluent is ethyl acetate/stone Oily ether=1/10-1/12, obtains the compound (398mg) of Formulas I structure, HPLC purity 97.5%,1H,13C NMR datas and embodiment 4 is consistent.
Embodiment 6
According to described in Chinese invention patent application publication No. CN101875653A embodiments 14 to aphid and mythimna separata Insecticidal activity test method, test formula Compound I, product A, product B, products C are under the concentration of 300 μ g/mL to aphid The insecticidal activity of worm and mythimna separata, as a result see the table below.
Tester Aphid (death rate %) Mythimna separata (death rate %)
Compound of formula I 100 100
Product A 52 61
Product B 56 62
Products C 0 8

Claims (9)

1. a kind of Folium Artemisiae Argyi extract, it is characterised in that the preparation method of the Folium Artemisiae Argyi extract includes the following steps：
(1) it takes dry folium artemisiae argyi to crush, after sterilization processing, is placed in sterile fermentation tank, glucose and yeast is then added Powder after mixing seals fermentation tank, and at 20-25 DEG C, spontaneous fermentation 20-25 days, obtains fermentate；
(2) the fermentate acetone soak for obtaining step (1), filtering, through macroporous resin adsorption, use volume after filtrate concentration The ethanol solution that score is 60-70% elutes, and collects 5-6 times of column volume eluent, then through activated carbon decolorizing, concentration, dry The Folium Artemisiae Argyi extract.
2. Folium Artemisiae Argyi extract described in claim 1, it is characterised in that the dosage of glucose is folium artemisiae argyi quality in step (1) 10%-15%, the dosage of yeast powder are the 3%-5% of folium artemisiae argyi quality.
3. claim 1-2 any one of them Folium Artemisiae Argyi extracts, it is characterised in that the dosage of acetone is every kilogram in step (2) Folium artemisiae argyi uses 8-10L acetone；The acetone soak time is 20-24 hours preferred；The model of the macroreticular resin is in AB-8, D101 One kind.
4. application of the claim 1-3 any one of them Folium Artemisiae Argyi extract in preventing agricultural pests.
5. the application described in claim 4, it is characterised in that the preferred aphid of the agricultural pests, mythimna separata.
6. application of the claim 1-3 any one of them Folium Artemisiae Argyi extracts in preparing insecticide.
7. a kind of insecticide, it is characterised in that the insecticide using claim 1-3 any one of them Folium Artemisiae Argyi extract as Active constituent.
8. claim 6-7 any one of them insecticides, it is characterised in that the insecticide preferably kills aphid, mythimna separata.
9. the preparation method of claim 1-3 any one of them Folium Artemisiae Argyi extracts.
CN201810461118.2A 2018-05-14 2018-05-14 Folium artemisiae argyi extract and preparation method and application thereof Active CN108531526B (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102727550A (en) * 2012-07-10 2012-10-17 河北联合大学 Antifungal artemisia argyi rhizome leavening and preparation technology thereof
CN104152514A (en) * 2014-07-24 2014-11-19 北京翰若生物科技有限公司 Origin fermentation method and origin fermentation product prepared by same
KR20160079269A (en) * 2014-12-26 2016-07-06 가톨릭대학교 산학협력단 Anti-inflammatory pharmaceutical composition and health functional food containing artemisia fermentation extract
CN108690047A (en) * 2018-05-14 2018-10-23 扬州工业职业技术学院 A kind of heterocyclic compound and its application as insecticide

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102727550A (en) * 2012-07-10 2012-10-17 河北联合大学 Antifungal artemisia argyi rhizome leavening and preparation technology thereof
CN104152514A (en) * 2014-07-24 2014-11-19 北京翰若生物科技有限公司 Origin fermentation method and origin fermentation product prepared by same
KR20160079269A (en) * 2014-12-26 2016-07-06 가톨릭대학교 산학협력단 Anti-inflammatory pharmaceutical composition and health functional food containing artemisia fermentation extract
CN108690047A (en) * 2018-05-14 2018-10-23 扬州工业职业技术学院 A kind of heterocyclic compound and its application as insecticide

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
WEN-JUAN ZHANG 等: ""Bioactivity of Essential Oil of Artemisia argyi Lévl. et Van. and Its Main Compounds Against Lasioderma serricorne"", 《JOURNAL OF OLEO SCIENCE》 *
孙娅 等: ""菊花近缘种属植物抗蚜性机制研究"", 《南京农业大学学报》 *
李真真 等: ""艾叶的化学成分及药理作用研究进展"", 《国际药学研究杂志》 *
白静 等: ""艾叶水提物及其发酵物体内外抗阴道毛滴虫作用"", 《中成药》 *

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