CN110226598A - A kind of tea tree pest repellant of Extracts from Plant Recourses - Google Patents

A kind of tea tree pest repellant of Extracts from Plant Recourses Download PDF

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Publication number
CN110226598A
CN110226598A CN201910618832.2A CN201910618832A CN110226598A CN 110226598 A CN110226598 A CN 110226598A CN 201910618832 A CN201910618832 A CN 201910618832A CN 110226598 A CN110226598 A CN 110226598A
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eutectic
mass ratio
extract
niacinamide
saccharin
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刘登威
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Fuding Creative Century Tea Industry Co Ltd
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Fuding Creative Century Tea Industry Co Ltd
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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
    • A01N25/00—Biocides, 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
    • A01N25/02—Biocides, 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
    • 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
    • A01N31/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic oxygen or sulfur compounds
    • A01N31/08—Oxygen or sulfur directly attached to an aromatic ring system
    • 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
    • A01N37/18—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 the group —CO—N<, e.g. carboxylic acid amides or imides; Thio analogues thereof
    • 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
    • A01N43/02—Biocides, 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
    • A01N43/04—Biocides, 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
    • A01N43/14—Biocides, 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
    • A01N43/16—Biocides, 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

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  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Dentistry (AREA)
  • Plant Pathology (AREA)
  • Engineering & Computer Science (AREA)
  • Pest Control & Pesticides (AREA)
  • Agronomy & Crop Science (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Environmental Sciences (AREA)
  • Toxicology (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

This application discloses a kind of tea tree pest repellants of Extracts from Plant Recourses, based on molal weight, the tea tree pest repellant includes 1 part of carvacrol, 0.90~1.10 part of capsaicine, 0.45~0.55 part of Gastrodin and 0.30~0.37 part of naringenin, conducive to plant source expelling parasite, efficient, less toxic, degradable, noresidue and without drug resistance.

Description

A kind of tea tree pest repellant of Extracts from Plant Recourses
Technical field
The present invention relates to a kind of tea tree pest repellants of Extracts from Plant Recourses.
Background technique
Tealeaves originates from China, is one of the beverage most generally drunk in the world, and consumption figure is only second to water, is higher than coffee Coffee, beer, grape wine and soda.In general, tea polyphenols, tea polysaccharide, caffeine, protein, amino are contained in tealeaves A variety of nutrition such as acid, vitamin, minerals and pharmaceutical component, this is the material base of tealeaves biological action, by drinking tea The antioxidant activities object such as the nutrients such as minerals, vitamin, amino acid not only can be directly supplemented, but also tea polyphenols can be taken in Matter generates comprehensive physiological regulatory action to body.
The plantation of tealeaves at present is mainly based on various regions on the south China main product the Changjiang river, due to topography, gas in planting process It waits, the influence of soil, has various pests and occur, therefore inevitably to carry out chemical pesticide sprinkling deinsectization, this Disagreed with the theory of non-polluted planting, be easy residual noxious material, to drink the human body after tealeaves cause it is inestimable Injury.
There is the pest repellant for developing a Extracts from Plant Recourses certain production application to be worth.
Summary of the invention
The object of the present invention is to provide a kind of tea tree pest repellants of Extracts from Plant Recourses, are conducive to plant source expelling parasite, efficient, low Malicious, degradable, noresidue and without drug resistance.
Above-mentioned technical purpose of the invention has the technical scheme that
A kind of tea tree pest repellant of Extracts from Plant Recourses, based on molal weight, including 1 part of carvacrol, capsaicine 0.90~1.10 Part, 0.45~0.55 part of Gastrodin and 0.30~0.37 part of naringenin.
Preferably, the form of the carvacrol of selection is the eutectic of carvacrol and fumaric acid, and the form of the capsaicine of selection is The eutectic of capsaicine and succinic acid, the form of the Gastrodin of selection are the eutectic of Gastrodin and niacinamide, the naringenin of selection Form is the eutectic of naringenin and saccharin；
Based on molal weight, the tea tree pest repellant includes being total to for 1 part of eutectic, capsaicine and the succinic acid of carvacrol and fumaric acid The eutectic 0.30 of 0.45~0.55 part of the eutectic and naringenin and saccharin of 0.90~1.10 part brilliant, Gastrodin and niacinamide~ 0.37 part.
Preferably, it is radiated using Cu-K α, the X-ray powder diffraction that the eutectic of the carvacrol and fumaric acid is indicated with 2 θ Figure following position have characteristic peak: 3.5 ± 0.2 °, 4.3 ± 0.2 °, 6.2 ± 0.2 °, 8.9 ± 0.2 °, 15.4 ± 0.2 ° and 20.1±0.2°；
It is radiated using Cu-K α, the X-ray powder diffraction figure that the eutectic of the capsaicine and succinic acid is indicated with 2 θ is with bottom Set with characteristic peak: 5.1 ± 0.2 °, 7.1 ± 0.2 °, 10.3 ± 0.2 °, 13.2 ± 0.2 °, 17.2 ± 0.2 ° and 22.8 ± 0.2°；
It is radiated using Cu-K α, the X-ray powder diffraction figure that the eutectic of the Gastrodin and niacinamide is indicated with 2 θ is with bottom Set with characteristic peak: 3.3 ± 0.2 °, 3.9 ± 0.2 °, 4.4 ± 0.2 °, 6.9 ± 0.2 °, 10.9 ± 0.2 °, 19.2 ± 0.2 °, 25.5 ± 0.2 °, 29.2 ± 0.2 ° and 33.2 ± 0.2 °；
It is radiated using Cu-K α, the X-ray powder diffraction figure that the eutectic of the naringenin and saccharin is indicated with 2 θ is in following position With characteristic peak: 7.2 ± 0.2 °, 8.2 ± 0.2 °, 10.2 ± 0.2 °, 11.2 ± 0.2 °, 15.5 ± 0.2 °, 17.5 ± 0.2 °, 18.3 ± 0.2 °, 19.7 ± 0.2 °, 23.2 ± 0.2 ° and 25.1 ± 0.2 °.
Preferably, it is radiated using Cu-K α, the X-ray powder diffraction that the eutectic of the carvacrol and fumaric acid is indicated with 2 θ Figure has characteristic peak and its relative intensity in following position:
2 θ of the angle of diffraction Relative intensity I%
3.5±0.2° 1.2
4.3±0.2° 4.5
6.2±0.2° 15.2
8.9±0.2° 45.6
15.4±0.2° 100.0
20.1±0.2° 5.1；
It is radiated using Cu-K α, the X-ray powder diffraction figure that the eutectic of the capsaicine and succinic acid is indicated with 2 θ is with bottom It sets with characteristic peak and its relative intensity:
2 θ of the angle of diffraction Relative intensity I%
5.1±0.2° 22.1
7.1±0.2° 3.2
10.3±0.2° 4.5
13.2±0.2° 8.0
17.2±0.2° 46.4
22.8±0.2° 100.0；
It is radiated using Cu-K α, the X-ray powder diffraction figure that the eutectic of the Gastrodin and niacinamide is indicated with 2 θ is with bottom It sets with characteristic peak and its relative intensity:
It is radiated using Cu-K α, the X-ray powder diffraction figure that the eutectic of the naringenin and saccharin is indicated with 2 θ is in following position With characteristic peak and its relative intensity:
2 θ of the angle of diffraction Relative intensity I%
7.2±0.2° 6.2
8.2±0.2° 7.3
10.2±0.2° 4.2
11.2±0.2° 25.3
15.5±0.2° 100.0
17.5±0.2° 17.9
18.3±0.2° 8.1
19.7±0.2° 22.4
23.2±0.2° 9.1
25.1±0.2° 4.2。
Preferably, the eutectic of the carvacrol and fumaric acid the preparation method comprises the following steps: respectively prepare carvacrol ethanol solution and richness The ethanol solution of horse acid, under agitation adds to the ethanol solution of fumaric acid in the ethanol solution of carvacrol, 48~52 It is stirred to react 3~5hr at DEG C, filters to take solid, drying；The mole dosage of carvacrol and fumaric acid ratio is 1:0.95~1.05； In the ethanol solution of carvacrol, the mass ratio of carvacrol and ethyl alcohol is 1:0.8~1.2；In the ethanol solution of fumaric acid, fumaric acid Mass ratio with ethyl alcohol is 1:1.8~2.5；
The eutectic of the capsaicine and succinic acid the preparation method comprises the following steps: preparing the aqueous isopropanol and succinic acid of capsaicine respectively Isopropanol suspension under agitation adds to the isopropanol suspension of succinic acid in the aqueous isopropanol of capsaicine, 54 It is stirred to react 7~9hr at~56 DEG C, filters to take solid, drying；The mole dosage of capsaicine and succinic acid ratio be 1:0.95~ 1.00；In the aqueous isopropanol of capsaicine, the mass ratio of capsaicine and isopropanol is 1:0.8~1.2；The isopropanol of succinic acid is mixed In suspension, the mass ratio of succinic acid and isopropanol is 1:2.8~3.2；
The eutectic of the Gastrodin and niacinamide the preparation method comprises the following steps: respectively prepare Gastrodin aqueous suspension and niacinamide water Solution under agitation adds to the aqueous solution of niacinamide in the aqueous suspension of Gastrodin, is stirred to react 1 at 38~41 DEG C ~3hr filters to take filtrate, filtrate freeze-drying；The mole dosage of Gastrodin and niacinamide ratio is 1:0.95~1.00；The water of Gastrodin In suspension, the mass ratio of Gastrodin and water is 1:0.5~0.7；In the aqueous solution of niacinamide, the mass ratio of niacinamide and water is 1:1.4~1.6；
The eutectic of the naringenin and saccharin the preparation method comprises the following steps: respectively prepare naringenin aqueous suspension and saccharin it is water-soluble Liquid under agitation adds to the aqueous solution of saccharin in the aqueous suspension of naringenin, it is stirred to react 5 at 54~56 DEG C~ 7hr filters to take filtrate, filtrate freeze-drying；The mole dosage of naringenin and saccharin ratio is 1:0.95~1.00；The water of naringenin is suspended In liquid, the mass ratio of naringenin and water is 1:0.9~1.1；In the aqueous solution of saccharin, the mass ratio of saccharin and water be 1:1.8~ 2.1。
Preferably, the eutectic of the carvacrol and fumaric acid the preparation method comprises the following steps: dry origanum oil crushes, ethyl alcohol is added, returns Stream 3~5hr of reaction, filters to take filtrate concentration, as wild marjoram oil extract；The ethanol solution for preparing fumaric acid, in stirring condition It is lower to add to the ethanol solution of fumaric acid in wild marjoram oil extract, be stirred to react 3~5hr at 48~52 DEG C, filter to take solid, Drying；When preparing wild marjoram oil extract, the mass ratio of origanum oil and ethyl alcohol is 1:4.5~5.5, and filtrate is concentrated into the 1/ of original volume 4~1/3；In wild marjoram oil extract and fumaric acid reaction system, the mass ratio of origanum oil and fumaric acid is 150:110~122；Ox Into oil extract, the mass ratio of carvacrol and ethyl alcohol is 1:0.8~1.2；In the ethanol solution of fumaric acid, fumaric acid and ethyl alcohol Mass ratio be 1:1.8~2.5；
The eutectic of the capsaicine and succinic acid the preparation method comprises the following steps: xerophagia Capsicum crushing, ethyl acetate, back flow reaction is added 7~9hr filters to take filtrate, and filtrate is lyophilized into powder, as pepper extract；The aqueous isopropanol of pepper extract is prepared respectively With the isopropanol suspension of succinic acid, the isopropanol suspension of succinic acid is added to the isopropyl of pepper extract under agitation In alcoholic solution, it is stirred to react 7~9hr at 54~56 DEG C, filters to take solid, drying；When preparing pepper extract, capsicum and second The mass ratio of acetoacetic ester is 1:3.2~3.6；In pepper extract and succinic acid reaction system, pepper extract and succinic acid Mass ratio is 305:112~118；In the aqueous isopropanol of pepper extract, the mass ratio of pepper extract and isopropanol is 1: 0.8~1.2；In the isopropanol suspension of succinic acid, the mass ratio of succinic acid and isopropanol is 1:2.8~3.2；
The eutectic of the Gastrodin and niacinamide the preparation method comprises the following steps: dry day snippings block crushes, acetonitrile and ethyl acetate is added, returns Stream 2~4hr of reaction, filters to take filtrate, filtrate is lyophilized into powder, as Rhizoma Gastrodiae extract；The water for preparing Rhizoma Gastrodiae extract respectively is mixed The aqueous solution of suspension and niacinamide under agitation adds to the aqueous solution of niacinamide in the aqueous suspension of Rhizoma Gastrodiae extract, It is stirred to react 1~3hr at 38~41 DEG C, filters to take filtrate, filtrate freeze-drying；When preparing Rhizoma Gastrodiae extract, day snippings block, acetonitrile Mass ratio with ethyl acetate is 1:1.2~1.5:1.0~1.2；In Rhizoma Gastrodiae extract and niacinamide reaction system, Rhizoma Gastrodiae is extracted The mass ratio of object and niacinamide is 286:116~122；In the aqueous suspension of gastrodin, gastrodin and water Mass ratio is 1:0.5~0.7；In the aqueous solution of niacinamide, the mass ratio of niacinamide and water is 1:1.4~1.6；
The eutectic of the naringenin and saccharin the preparation method comprises the following steps: Anacardiaceae plant stalk tree fruit dry nucleocapsid crush, add acetic acid Ethyl ester and water, 4~6hr of back flow reaction, take ethyl acetate phase, are lyophilized into powder, as dry nucleocapsid extract；Dry nucleocapsid is prepared respectively The aqueous solution of saccharin is added to the water of dry nucleocapsid extract by the aqueous suspension of extract and the aqueous solution of saccharin under agitation In suspension, it is stirred to react 5~7hr at 54~56 DEG C, filters to take filtrate, filtrate freeze-drying；When preparing dry nucleocapsid extract, paint The mass ratio that tree section plant obstructs the dry nucleocapsid powder for setting fruit, ethyl acetate and water is 1:1.9~2.1:1.9~2.1；Dry nucleocapsid mentions It takes in object and saccharin reaction system, the mole dosage ratio of dry nucleocapsid extract and saccharin is 272:174~183；Dry nucleocapsid extracts In the aqueous suspension of object, the mass ratio of dry nucleocapsid extract and water is 1:0.9~1.1；In the aqueous solution of saccharin, saccharin and water Mass ratio is 1:1.8~2.1.
Preferably, based on molal weight, the tea tree pest repellant includes 1 part of eutectic, the capsaicine of carvacrol and fumaric acid With 0.33 part of eutectic of 1.00 parts of the eutectic of succinic acid, 0.50 part of the eutectic and naringenin of Gastrodin and niacinamide and saccharin.
The technology of the present invention effect major embodiment is in the following areas:
1, by the combination of carvacrol, capsaicine, Gastrodin and naringenin, anthelminthic effect is greatly improved, hence it is evident that better than existing There is technology；Using plant source insect-repelling method, conducive to plant source expelling parasite, efficient, less toxic, degradable, noresidue and without drug resistance；
2, select carvacrol and the eutectic of fumaric acid, the eutectic of capsaicine and succinic acid, Gastrodin and niacinamide eutectic and The combination of the eutectic of naringenin and saccharin, greatly improves water solubility, is conducive to obtained aqueous solution preparation；Utilize the property, this Shen Pest repellant please after the application, easily by soil absorption, enters inside plants by root system of plant, plays the purpose of long-acting insect expelling, This is to disperse insoluble pest repellant by emulsifier to be unable to reach；And since its water solubility is good, when use, can be by simple Flushing can remove, and residual is negligible.
Detailed description of the invention
Fig. 1 is the X-ray powder diffraction figure of the eutectic of carvacrol and fumaric acid；
Fig. 2 is the X-ray powder diffraction figure of capsaicine and succinic acid；
Fig. 3 is the X-ray powder diffraction figure of Gastrodin and niacinamide；
Fig. 4 is the X-ray powder diffraction figure of naringenin and saccharin.
Specific embodiment
Embodiment 1: a kind of eutectic of carvacrol and fumaric acid, preparation method are as follows: the ethyl alcohol for preparing carvacrol respectively is molten The ethanol solution of liquid and fumaric acid under agitation adds to the ethanol solution of fumaric acid in the ethanol solution of carvacrol, It is stirred to react 4hr at 50 DEG C, filters to take solid, drying.
The mole dosage of carvacrol and fumaric acid ratio is 1:1.00；In the ethanol solution of carvacrol, carvacrol and ethyl alcohol Mass ratio is 1:1.0；In the ethanol solution of fumaric acid, the mass ratio of fumaric acid and ethyl alcohol is 1:2.0.
Nuclear-magnetism test verifying carvacrol and fumaric acid form eutectic.
The purity that HPLC tests the eutectic of the carvacrol and fumaric acid is 99.2%.
X-ray powder diffraction test is as shown in Figure 1.The X-ray powder that the eutectic of carvacrol and fumaric acid is indicated with 2 θ Diffraction pattern has characteristic peak and its relative intensity in following position:
2 θ of the angle of diffraction Relative intensity I%
3.5±0.2° 1.2
4.3±0.2° 4.5
6.2±0.2° 15.2
8.9±0.2° 45.6
15.4±0.2° 100.0
20.1±0.2° 5.1。
Embodiment 2: a kind of eutectic of carvacrol and fumaric acid, preparation method are as follows: respectively prepare carvacrol ethanol solution and The ethanol solution of fumaric acid under agitation adds to the ethanol solution of fumaric acid in the ethanol solution of carvacrol, at 48 DEG C Under be stirred to react 5hr, filter to take solid, drying.
The mole dosage of carvacrol and fumaric acid ratio is 1:0.95；In the ethanol solution of carvacrol, carvacrol and ethyl alcohol Mass ratio is 1:0.8；In the ethanol solution of fumaric acid, the mass ratio of fumaric acid and ethyl alcohol is 1:1.8.
The purity that HPLC tests the eutectic of the carvacrol and fumaric acid is 97.8%.
X-ray powder diffraction test is same as Example 1.
Embodiment 3: a kind of eutectic of carvacrol and fumaric acid, preparation method are as follows: the ethyl alcohol for preparing carvacrol respectively is molten The ethanol solution of liquid and fumaric acid under agitation adds to the ethanol solution of fumaric acid in the ethanol solution of carvacrol, It is stirred to react 3hr at 52 DEG C, filters to take solid, drying.
The mole dosage of carvacrol and fumaric acid ratio is 1:1.05；In the ethanol solution of carvacrol, carvacrol and ethyl alcohol Mass ratio is 1:1.2；In the ethanol solution of fumaric acid, the mass ratio of fumaric acid and ethyl alcohol is 1:2.5.
The purity that HPLC tests the eutectic of the carvacrol and fumaric acid is 98.1%.
X-ray powder diffraction test is same as Example 1.
Comparative example 1: a kind of reaction of carvacrol and fumaric acid, operating method are as follows: prepare the second of carvacrol respectively The ethyl acetate solution of fumaric acid is added to carvacrol under agitation by the ethyl acetate solution of acetate solution and fumaric acid Ethyl acetate solution in, be stirred to react 4hr at 50 DEG C, filter to take solid, drying.
The mole dosage of carvacrol and fumaric acid ratio is 1:1.00；In the ethyl acetate solution of carvacrol, carvacrol and second The mass ratio of alcohol is 1:1.0；In the ethyl acetate solution of fumaric acid, the mass ratio of fumaric acid and ethyl acetate is 1:2.0.
Nuclear-magnetism test verifying carvacrol and the not formed eutectic of fumaric acid.
Comparative example 2: a kind of reaction of carvacrol and fumaric acid, operating method are as follows: prepare the second of carvacrol respectively The ethanol solution of fumaric acid is added to the ethanol solution of carvacrol by the ethanol solution of alcoholic solution and fumaric acid under agitation It is interior, it is stirred to react 4hr at 40 DEG C, filters to take solid, drying.
The mole dosage of carvacrol and fumaric acid ratio is 1:1.00；In the ethanol solution of carvacrol, carvacrol and ethyl alcohol Mass ratio is 1:1.0；In the ethanol solution of fumaric acid, the mass ratio of fumaric acid and ethyl alcohol is 1:2.0.
Nuclear-magnetism test verifying carvacrol and the not formed eutectic of fumaric acid.
Embodiment 4: a kind of eutectic of carvacrol and fumaric acid, preparation method are as follows: dry origanum oil crushes, and ethyl alcohol is added, Back flow reaction 4hr filters to take filtrate concentration, as wild marjoram oil extract；The ethanol solution of fumaric acid is prepared, under agitation The ethanol solution of fumaric acid is added in wild marjoram oil extract, is stirred to react 4hr at 50 DEG C, filters to take solid, drying.
When preparing wild marjoram oil extract, the mass ratio of origanum oil and ethyl alcohol is 1:5.0, and filtrate is concentrated into the 1/4 of original volume； In wild marjoram oil extract and fumaric acid reaction system, the mass ratio of origanum oil and fumaric acid is 150:115；Wild marjoram oil extract In, the mass ratio of carvacrol and ethyl alcohol is 1:1.0；In the ethanol solution of fumaric acid, the mass ratio of fumaric acid and ethyl alcohol is 1: 2.0。
The purity that HPLC tests the eutectic of the carvacrol and fumaric acid is 97.5%.
X-ray powder diffraction test is same as Example 1.
Embodiment 5: a kind of eutectic of carvacrol and fumaric acid, preparation method are as follows: dry origanum oil crushes, and ethyl alcohol is added, Back flow reaction 3hr filters to take filtrate concentration, as wild marjoram oil extract；The ethanol solution of fumaric acid is prepared, under agitation The ethanol solution of fumaric acid is added in wild marjoram oil extract, is stirred to react 5hr at 48 DEG C, filters to take solid, drying.
When preparing wild marjoram oil extract, the mass ratio of origanum oil and ethyl alcohol is 1:4.5, and filtrate is concentrated into the 1/4 of original volume； In wild marjoram oil extract and fumaric acid reaction system, the mass ratio of origanum oil and fumaric acid is 150:110；Wild marjoram oil extract In, the mass ratio of carvacrol and ethyl alcohol is 1:0.8；In the ethanol solution of fumaric acid, the mass ratio of fumaric acid and ethyl alcohol is 1: 1.8。
The purity that HPLC tests the eutectic of the carvacrol and fumaric acid is 95.9%.
X-ray powder diffraction test is same as Example 1.
Embodiment 6: a kind of eutectic of carvacrol and fumaric acid, preparation method are as follows: dry origanum oil crushes, and ethyl alcohol is added, Back flow reaction 5hr filters to take filtrate concentration, as wild marjoram oil extract；The ethanol solution of fumaric acid is prepared, under agitation The ethanol solution of fumaric acid is added in wild marjoram oil extract, is stirred to react 3hr at 52 DEG C, filters to take solid, drying.
When preparing wild marjoram oil extract, the mass ratio of origanum oil and ethyl alcohol is 1:5.5, and filtrate is concentrated into the 1/3 of original volume； In wild marjoram oil extract and fumaric acid reaction system, the mass ratio of origanum oil and fumaric acid is 150:122；Wild marjoram oil extract In, the mass ratio of carvacrol and ethyl alcohol is 1:1.2；In the ethanol solution of fumaric acid, the mass ratio of fumaric acid and ethyl alcohol is 1: 2.5。
The purity that HPLC tests the eutectic of the carvacrol and fumaric acid is 95.6%.
X-ray powder diffraction test is same as Example 1.
Comparative example 3: a kind of reaction of carvacrol and fumaric acid, operating method are as follows: dry origanum oil crushes, and second is added Acetoacetic ester, back flow reaction 4hr filter to take filtrate and are lyophilized into powder, as wild marjoram oil extract；Respectively prepare wild marjoram oil extract and The ethanol solution of fumaric acid under agitation adds to the ethanol solution of fumaric acid in the ethanol solution of wild marjoram oil extract, It is stirred to react 4hr at 50 DEG C, filters to take solid, drying.
When preparing wild marjoram oil extract, the mass ratio of origanum oil and ethyl acetate is 1:5.0；Wild marjoram oil extract and Fu Ma In sour reaction system, the mass ratio of origanum oil and fumaric acid is 150:115；In wild marjoram oil extract, the matter of carvacrol and ethyl alcohol Amount is than being 1:1.0；In the ethanol solution of fumaric acid, the mass ratio of fumaric acid and ethyl alcohol is 1:2.0.
Nuclear-magnetism test verifying carvacrol and the not formed eutectic of fumaric acid.
Comparative example 4: a kind of reaction of carvacrol and fumaric acid, operating method are as follows: dry origanum oil crushes, and second is added Alcohol, back flow reaction 4hr filter to take filtrate concentration, as wild marjoram oil extract；The aqueous solution for preparing fumaric acid, in stirring condition It is lower to add to the aqueous solution of fumaric acid in wild marjoram oil extract, it is stirred to react 4hr at 50 DEG C, filtrate is filtered to take, is lyophilized into powder.
When preparing wild marjoram oil extract, the mass ratio of origanum oil and ethyl alcohol is 1:5.0, and filtrate is concentrated into the 1/4 of original volume； In wild marjoram oil extract and fumaric acid reaction system, the mass ratio of origanum oil and fumaric acid is 150:115；Wild marjoram oil extract In, the mass ratio of carvacrol and ethyl alcohol is 1:1.0；In the aqueous solution of fumaric acid, the mass ratio of fumaric acid and water is 1:2.0.
Nuclear-magnetism test verifying carvacrol and the not formed eutectic of fumaric acid.
Embodiment 7: a kind of eutectic of capsaicine and succinic acid, preparation method are as follows: prepare the isopropanol of capsaicine respectively The isopropanol suspension of succinic acid is added to the isopropyl of capsaicine by the isopropanol suspension of solution and succinic acid under agitation In alcoholic solution, it is stirred to react 8hr at 55 DEG C, filters to take solid, drying.
The mole dosage of capsaicine and succinic acid ratio is 1:0.98；In the aqueous isopropanol of capsaicine, capsaicine and isopropyl The mass ratio of alcohol is 1:1.0；In the isopropanol suspension of succinic acid, the mass ratio of succinic acid and isopropanol is 1:3.0.
Nuclear-magnetism test verifying capsaicine and succinic acid form eutectic.
The purity that HPLC tests the eutectic of the capsaicine and succinic acid is 98.7%.
X-ray powder diffraction test is as shown in Figure 2.The X-ray powder that the eutectic of capsaicine and succinic acid is indicated with 2 θ Diffraction pattern has characteristic peak and its relative intensity in following position:
2 θ of the angle of diffraction Relative intensity I%
5.1±0.2° 22.1
7.1±0.2° 3.2
10.3±0.2° 4.5
13.2±0.2° 8.0
17.2±0.2° 46.4
22.8±0.2° 100.0。
Embodiment 8: a kind of eutectic of capsaicine and succinic acid, preparation method are as follows: prepare the aqueous isopropanol of capsaicine respectively With the isopropanol suspension of succinic acid, the isopropanol that the isopropanol suspension of succinic acid is added to capsaicine under agitation is molten In liquid, it is stirred to react 9hr at 54 DEG C, filters to take solid, drying.
The mole dosage of capsaicine and succinic acid ratio is 1:0.95；In the aqueous isopropanol of capsaicine, capsaicine and isopropyl The mass ratio of alcohol is 1:0.8；In the isopropanol suspension of succinic acid, the mass ratio of succinic acid and isopropanol is 1:2.8.
The purity that HPLC tests the eutectic of the capsaicine and succinic acid is 96.0%.
X-ray powder diffraction test is same as Example 7.
Embodiment 9: a kind of eutectic of capsaicine and succinic acid, preparation method are as follows: prepare the isopropanol of capsaicine respectively The isopropanol suspension of succinic acid is added to the isopropyl of capsaicine by the isopropanol suspension of solution and succinic acid under agitation In alcoholic solution, it is stirred to react 9hr at 56 DEG C, filters to take solid, drying.
The mole dosage of capsaicine and succinic acid ratio is 1:1.00；In the aqueous isopropanol of capsaicine, capsaicine and isopropyl The mass ratio of alcohol is 1:1.2；In the isopropanol suspension of succinic acid, the mass ratio of succinic acid and isopropanol is 1:3.2.
The purity that HPLC tests the eutectic of the capsaicine and succinic acid is 95.7%.
X-ray powder diffraction test is same as Example 7.
Comparative example 5: a kind of reaction of capsaicine and succinic acid, operating method are as follows: prepare the second of capsaicine respectively The ethyl alcohol suspension of alcoholic solution and succinic acid, the ethyl alcohol that the ethyl alcohol suspension of succinic acid is added to capsaicine under agitation are molten In liquid, it is stirred to react 8hr at 55 DEG C, filters to take solid, drying.
The mole dosage of capsaicine and succinic acid ratio is 1:0.98；In the ethanol solution of capsaicine, capsaicine and ethyl alcohol Mass ratio is 1:1.0；In the ethyl alcohol suspension of succinic acid, the mass ratio of succinic acid and ethyl alcohol is 1:3.0.
Nuclear-magnetism test verifying capsaicine and the not formed eutectic of succinic acid.
Comparative example 6: a kind of reaction of capsaicine and succinic acid, operating method are as follows: prepare the different of capsaicine respectively The isopropanol suspension of succinic acid is added to capsaicine under agitation by the isopropanol suspension of propanol solution and succinic acid In aqueous isopropanol, it is stirred to react 8hr at 50 DEG C, filters to take solid, drying.
The mole dosage of capsaicine and succinic acid ratio is 1:0.92；In the aqueous isopropanol of capsaicine, capsaicine and isopropyl The mass ratio of alcohol is 1:1.0；In the isopropanol suspension of succinic acid, the mass ratio of succinic acid and isopropanol is 1:3.0.
Nuclear-magnetism test verifying capsaicine and the not formed eutectic of succinic acid.
Embodiment 10: a kind of eutectic of capsaicine and succinic acid, preparation method are as follows: second is added in xerophagia Capsicum crushing Acetoacetic ester, back flow reaction 8hr filter to take filtrate, and filtrate is lyophilized into powder, as pepper extract；Pepper extract is prepared respectively Aqueous isopropanol and succinic acid isopropanol suspension, the isopropanol suspension of succinic acid is added into capsicum under agitation In the aqueous isopropanol of extract, it is stirred to react 8hr at 55 DEG C, filters to take solid, drying.
When preparing pepper extract, the mass ratio of capsicum and ethyl acetate is 1:3.3；Pepper extract and succinic acid reaction In system, the mass ratio of pepper extract and succinic acid is 305:115；In the aqueous isopropanol of pepper extract, capsicum is extracted The mass ratio of object and isopropanol is 1:1.0；In the isopropanol suspension of succinic acid, the mass ratio of succinic acid and isopropanol is 1: 3.0。
It is 97.9% that HPLC, which tests the capsaicine and the purity of succinic acid,.
X-ray powder diffraction test is same as Example 7.
Embodiment 11: a kind of eutectic of capsaicine and succinic acid, preparation method are as follows: second is added in xerophagia Capsicum crushing Acetoacetic ester, back flow reaction 7hr filter to take filtrate, and filtrate is lyophilized into powder, as pepper extract；Pepper extract is prepared respectively Aqueous isopropanol and succinic acid isopropanol suspension, the isopropanol suspension of succinic acid is added into capsicum under agitation In the aqueous isopropanol of extract, it is stirred to react 9hr at 54 DEG C, filters to take solid, drying.
When preparing pepper extract, the mass ratio of capsicum and ethyl acetate is 1:3.2；Pepper extract and succinic acid reaction In system, the mass ratio of pepper extract and succinic acid is 305:112；In the aqueous isopropanol of pepper extract, capsicum is extracted The mass ratio of object and isopropanol is 1:0.8；In the isopropanol suspension of succinic acid, the mass ratio of succinic acid and isopropanol is 1: 2.8。
The purity that HPLC tests the eutectic of the capsaicine and succinic acid is 95.3%.
X-ray powder diffraction test is same as Example 7.
Embodiment 12: a kind of eutectic of capsaicine and succinic acid, preparation method are as follows: second is added in xerophagia Capsicum crushing Acetoacetic ester, back flow reaction 9hr filter to take filtrate, and filtrate is lyophilized into powder, as pepper extract；Pepper extract is prepared respectively Aqueous isopropanol and succinic acid isopropanol suspension, the isopropanol suspension of succinic acid is added into capsicum under agitation In the aqueous isopropanol of extract, it is stirred to react 7hr at 56 DEG C, filters to take solid, drying.
When preparing pepper extract, the mass ratio of capsicum and ethyl acetate is 1:3.6；Pepper extract and succinic acid reaction In system, the mass ratio of pepper extract and succinic acid is 305:118；In the aqueous isopropanol of pepper extract, capsicum is extracted The mass ratio of object and isopropanol is 1:1.2；In the isopropanol suspension of succinic acid, the mass ratio of succinic acid and isopropanol is 1: 3.2。
The purity that HPLC tests the eutectic of the capsaicine and succinic acid is 95.6%.
X-ray powder diffraction test is same as Example 7.
Comparative example 7: a kind of reaction of capsaicine and succinic acid, operating method are as follows: xerophagia Capsicum crushing is added Isopropanol, back flow reaction 8hr filter to take filtrate, and filtrate is lyophilized into powder, as pepper extract；Pepper extract is prepared respectively Aqueous isopropanol and succinic acid isopropanol suspension, the isopropanol suspension of succinic acid is added into capsicum under agitation In the aqueous isopropanol of extract, it is stirred to react 8hr at 55 DEG C, filters to take solid, drying.
When preparing pepper extract, the mass ratio of capsicum and isopropanol is 1:3.3；Pepper extract and succinic acid reactant In system, the mass ratio of pepper extract and succinic acid is 305:115；In the aqueous isopropanol of pepper extract, pepper extract Mass ratio with isopropanol is 1:1.0；In the isopropanol suspension of succinic acid, the mass ratio of succinic acid and isopropanol is 1:3.0.
Nuclear-magnetism test verifying capsaicine and the not formed eutectic of succinic acid.
Comparative example 8: a kind of reaction of capsaicine and succinic acid, operating method are as follows: xerophagia Capsicum crushing is added Ethyl acetate, back flow reaction 8hr filter to take filtrate, and filtrate is lyophilized into powder, as pepper extract；Capsicum is prepared respectively to extract The ethyl acetate solution of object and the ethyl acetate suspension of succinic acid, under agitation by the ethyl acetate suspension of succinic acid It adds in the ethyl acetate solution of pepper extract, is stirred to react 8hr at 55 DEG C, filter to take filtrate, be lyophilized into powder.
When preparing pepper extract, the mass ratio of capsicum and ethyl acetate is 1:3.3；Pepper extract and succinic acid reaction In system, the mass ratio of pepper extract and succinic acid is 305:115；In the ethyl acetate solution of pepper extract, capsicum is mentioned Taking the mass ratio of object and ethyl acetate is 1:1.0；In the ethyl acetate suspension of succinic acid, the quality of succinic acid and ethyl acetate Than for 1:3.0.
Nuclear-magnetism test verifying capsaicine and the not formed eutectic of succinic acid.
Embodiment 13: a kind of eutectic of Gastrodin and niacinamide, preparation method are as follows: the water for preparing Gastrodin respectively is suspended The aqueous solution of liquid and niacinamide under agitation adds to the aqueous solution of niacinamide in the aqueous suspension of Gastrodin, at 40 DEG C Under be stirred to react 2hr, filter to take filtrate, filtrate freeze-drying.
The mole dosage of Gastrodin and niacinamide ratio is 1:0.98；In the aqueous suspension of Gastrodin, the matter of Gastrodin and water Amount is than being 1:0.6；In the aqueous solution of niacinamide, the mass ratio of niacinamide and water is 1:1.5.
Nuclear-magnetism test verifying Gastrodin and niacinamide form eutectic.
The purity that HPLC tests the eutectic of the Gastrodin and niacinamide is 99.0%.
X-ray powder diffraction test is as shown in Figure 3.The X-ray powder that the eutectic of Gastrodin and niacinamide is indicated with 2 θ Diffraction pattern has characteristic peak and its relative intensity in following position:
2 θ of the angle of diffraction Relative intensity I%
3.3±0.2° 2.6
3.9±0.2° 4.5
4.4±0.2° 3.9
6.9±0.2° 100.0
10.9±0.2° 22.2
19.2±0.2° 33.8
25.5±0.2° 7.3
29.2±0.2° 4.2
33.2±0.2° 6.2。
Embodiment 14: a kind of eutectic of Gastrodin and niacinamide, preparation method are as follows: respectively prepare Gastrodin aqueous suspension and The aqueous solution of niacinamide under agitation adds to the aqueous solution of niacinamide in the aqueous suspension of Gastrodin, stirs at 38 DEG C Reaction 3hr is mixed, filtrate, filtrate freeze-drying are filtered to take.
The mole dosage of Gastrodin and niacinamide ratio is 1:0.95；In the aqueous suspension of Gastrodin, the matter of Gastrodin and water Amount is than being 1:0.5；In the aqueous solution of niacinamide, the mass ratio of niacinamide and water is 1:1.4.
The purity that HPLC tests the eutectic of the Gastrodin and niacinamide is 97.5%.
X-ray powder diffraction test is identical as embodiment 13.
Embodiment 15: a kind of eutectic of Gastrodin and niacinamide, preparation method are as follows: the water for preparing Gastrodin respectively is suspended The aqueous solution of liquid and niacinamide under agitation adds to the aqueous solution of niacinamide in the aqueous suspension of Gastrodin, at 41 DEG C Under be stirred to react 1hr, filter to take filtrate, filtrate freeze-drying.
The mole dosage of Gastrodin and niacinamide ratio is 1:1.00；In the aqueous suspension of Gastrodin, the matter of Gastrodin and water Amount is than being 1:0.7；In the aqueous solution of niacinamide, the mass ratio of niacinamide and water is 1:1.6.
The purity that HPLC tests the eutectic of the Gastrodin and niacinamide is 96.4%.
X-ray powder diffraction test is identical as embodiment 13.
Comparative example 9: a kind of reaction of Gastrodin and niacinamide, operating method are as follows: prepare the second of Gastrodin respectively The ethanol solution of niacinamide is added to the ethanol solution of Gastrodin by the ethanol solution of alcoholic solution and niacinamide under agitation It is interior, it is stirred to react 3hr at 38 DEG C, filters to take filtrate, filtrate freeze-drying.
The mole dosage of Gastrodin and niacinamide ratio is 1:0.95；In the ethanol solution of Gastrodin, Gastrodin and ethyl alcohol Mass ratio is 1:0.5；In the ethanol solution of niacinamide, the mass ratio of niacinamide and ethyl alcohol is 1:1.4.
Nuclear-magnetism test verifying Gastrodin and the not formed eutectic of niacinamide.
Comparative example 10: a kind of reaction of Gastrodin and niacinamide, operating method are as follows: prepare the second of Gastrodin respectively The ethyl acetate solution of niacinamide is added to Gastrodin under agitation by the ethyl acetate solution of acetate solution and niacinamide Ethyl acetate solution in, be stirred to react 3hr at 38 DEG C, filter to take filtrate, filtrate freeze-drying.
The mole dosage of Gastrodin and niacinamide ratio is 1:0.95；In the ethyl acetate solution of Gastrodin, Gastrodin and second The mass ratio of acetoacetic ester is 1:0.5；In the ethyl acetate solution of niacinamide, the mass ratio of niacinamide and ethyl acetate is 1:1.4.
Nuclear-magnetism test verifying Gastrodin and the not formed eutectic of niacinamide.
Embodiment 16: a kind of eutectic of Gastrodin and niacinamide, preparation method are as follows: dry day snippings block crushes, and second is added Nitrile and ethyl acetate, back flow reaction 3hr filter to take filtrate, and filtrate is lyophilized into powder, as Rhizoma Gastrodiae extract；Rhizoma Gastrodiae is prepared respectively The aqueous suspension of extract and the aqueous solution of niacinamide, add to Rhizoma Gastrodiae extract for the aqueous solution of niacinamide under agitation In aqueous suspension, it is stirred to react 2hr at 40 DEG C, filters to take filtrate, filtrate freeze-drying.
When preparing Rhizoma Gastrodiae extract, the mass ratio of day snippings block, acetonitrile and ethyl acetate is 1:1.3:1.1；Rhizoma Gastrodiae extracts In object and niacinamide reaction system, the mass ratio of Rhizoma Gastrodiae extract and niacinamide is 286:119；The water of gastrodin is suspended In liquid, the mass ratio of gastrodin and water is 1:0.6；In the aqueous solution of niacinamide, the mass ratio of niacinamide and water is 1: 1.5。
The purity that HPLC tests the eutectic of the Gastrodin and niacinamide is 98.1%.
X-ray powder diffraction test is identical as embodiment 13.
Embodiment 17: a kind of eutectic of Gastrodin and niacinamide, preparation method are as follows: dry day snippings block crushes, and second is added Nitrile and ethyl acetate, back flow reaction 2hr filter to take filtrate, and filtrate is lyophilized into powder, as Rhizoma Gastrodiae extract；Rhizoma Gastrodiae is prepared respectively The aqueous suspension of extract and the aqueous solution of niacinamide, add to Rhizoma Gastrodiae extract for the aqueous solution of niacinamide under agitation In aqueous suspension, it is stirred to react 3hr at 38 DEG C, filters to take filtrate, filtrate freeze-drying.
When preparing Rhizoma Gastrodiae extract, the mass ratio of day snippings block, acetonitrile and ethyl acetate is 1:1.2:1.0；Rhizoma Gastrodiae extracts In object and niacinamide reaction system, the mass ratio of Rhizoma Gastrodiae extract and niacinamide is 286:116；The water of gastrodin is suspended In liquid, the mass ratio of gastrodin and water is 1:0.5；In the aqueous solution of niacinamide, the mass ratio of niacinamide and water is 1: 1.4。
The purity that HPLC tests the eutectic of the Gastrodin and niacinamide is 96.1%.
X-ray powder diffraction test is identical as embodiment 13.
Embodiment 18: a kind of eutectic of Gastrodin and niacinamide, preparation method are as follows: dry day snippings block crushes, and second is added Nitrile and ethyl acetate, back flow reaction 4hr filter to take filtrate, and filtrate is lyophilized into powder, as Rhizoma Gastrodiae extract；Rhizoma Gastrodiae is prepared respectively The aqueous suspension of extract and the aqueous solution of niacinamide, add to Rhizoma Gastrodiae extract for the aqueous solution of niacinamide under agitation In aqueous suspension, it is stirred to react 1hr at 41 DEG C, filters to take filtrate, filtrate freeze-drying.
When preparing Rhizoma Gastrodiae extract, the mass ratio of day snippings block, acetonitrile and ethyl acetate is 1:1.5:1.2；Rhizoma Gastrodiae extracts In object and niacinamide reaction system, the mass ratio of Rhizoma Gastrodiae extract and niacinamide is 286:122；The water of gastrodin is suspended In liquid, the mass ratio of gastrodin and water is 1:0.7；In the aqueous solution of niacinamide, the mass ratio of niacinamide and water is 1: 1.6。
The purity that HPLC tests the eutectic of the Gastrodin and niacinamide is 96.7%.
X-ray powder diffraction test is identical as embodiment 13.
Comparative example 11: a kind of reaction of Gastrodin and niacinamide, operating method are as follows: dry day snippings block crushes, and adds Enter acetonitrile, back flow reaction 3hr filters to take filtrate, and filtrate is lyophilized into powder, as Rhizoma Gastrodiae extract；Rhizoma Gastrodiae extract is prepared respectively Aqueous suspension and niacinamide aqueous solution, under agitation by the aqueous solution of niacinamide add to Rhizoma Gastrodiae extract water be suspended In liquid, it is stirred to react 2hr at 40 DEG C, filters to take filtrate, filtrate freeze-drying.
When preparing Rhizoma Gastrodiae extract, day snippings block, acetonitrile mass ratio be 1:1.3；Rhizoma Gastrodiae extract and niacinamide reaction In system, the mass ratio of Rhizoma Gastrodiae extract and niacinamide is 286:119；In the aqueous suspension of gastrodin, Gastrodin is mentioned Taking the mass ratio of object and water is 1:0.6；In the aqueous solution of niacinamide, the mass ratio of niacinamide and water is 1:1.5.
Nuclear-magnetism test verifying Gastrodin and the not formed eutectic of niacinamide.
Comparative example 12: a kind of reaction of Gastrodin and niacinamide, operating method are as follows: dry day snippings block crushes, and adds Enter ethyl acetate, back flow reaction 3hr filters to take filtrate, and filtrate is lyophilized into powder, as Rhizoma Gastrodiae extract；Rhizoma Gastrodiae is prepared respectively to mention The aqueous suspension of object and the aqueous solution of niacinamide are taken, the aqueous solution of niacinamide is added to the water of Rhizoma Gastrodiae extract under agitation In suspension, it is stirred to react 2hr at 40 DEG C, filters to take filtrate, filtrate freeze-drying.
When preparing Rhizoma Gastrodiae extract, the mass ratio of day snippings block and ethyl acetate is 1:1.1；Rhizoma Gastrodiae extract and niacinamide In reaction system, the mass ratio of Rhizoma Gastrodiae extract and niacinamide is 286:119；In the aqueous suspension of gastrodin, Rhizoma Gastrodiae The mass ratio of extract and water is 1:0.6；In the aqueous solution of niacinamide, the mass ratio of niacinamide and water is 1:1.5.
Nuclear-magnetism test verifying Gastrodin and the not formed eutectic of niacinamide.
Comparative example 13: a kind of reaction of Gastrodin and niacinamide, operating method are as follows: dry day snippings block crushes, and adds Enter acetonitrile and ethyl acetate, back flow reaction 3hr filters to take filtrate, and filtrate is lyophilized into powder, as Rhizoma Gastrodiae extract；It prepares respectively The ethyl alcohol suspension of Rhizoma Gastrodiae extract and the ethanol solution of niacinamide, add to day for the ethanol solution of niacinamide under agitation In the ethyl alcohol suspension of nettle extract, it is stirred to react 2hr at 40 DEG C, filters to take filtrate, filtrate freeze-drying.
When preparing Rhizoma Gastrodiae extract, the mass ratio of day snippings block, acetonitrile and ethyl acetate is 1:1.3:1.1；Rhizoma Gastrodiae extracts In object and niacinamide reaction system, the mass ratio of Rhizoma Gastrodiae extract and niacinamide is 286:119；The ethyl alcohol of gastrodin is mixed In suspension, the mass ratio of gastrodin and ethyl alcohol is 1:0.6；In the ethanol solution of niacinamide, the matter of niacinamide and ethyl alcohol Amount is than being 1:1.5.
Nuclear-magnetism test verifying Gastrodin and the not formed eutectic of niacinamide.
Embodiment 19: a kind of eutectic of naringenin and saccharin, preparation method are as follows: prepare the aqueous suspension of naringenin respectively With the aqueous solution of saccharin, the aqueous solution of saccharin is added in the aqueous suspension of naringenin under agitation, is stirred at 55 DEG C 6hr is reacted, filtrate, filtrate freeze-drying are filtered to take.
The mole dosage of naringenin and saccharin ratio is 1:0.98；In the aqueous suspension of naringenin, the quality of naringenin and water Than for 1:1.0；In the aqueous solution of saccharin, the mass ratio of saccharin and water is 1:2.0.
Nuclear-magnetism test verifying naringenin and saccharin form eutectic.
The purity that HPLC tests the eutectic of the naringenin and saccharin is 98.6%.
X-ray powder diffraction test is as shown in Figure 4.The eutectic of naringenin and saccharin is spread out with the X-ray powder that 2 θ are indicated Penetrating figure has characteristic peak and its relative intensity in following position:
2 θ of the angle of diffraction Relative intensity I%
7.2±0.2° 6.2
8.2±0.2° 7.3
10.2±0.2° 4.2
11.2±0.2° 25.3
15.5±0.2° 100.0
17.5±0.2° 17.9
18.3±0.2° 8.1
19.7±0.2° 22.4
23.2±0.2° 9.1
25.1±0.2° 4.2。
Embodiment 20: a kind of eutectic of naringenin and saccharin, preparation method are as follows: prepare the aqueous suspension and sugar of naringenin respectively The aqueous solution of essence, the aqueous solution of saccharin is added in the aqueous suspension of naringenin, be stirred to react at 54 DEG C under agitation 7hr filters to take filtrate, filtrate freeze-drying.
The mole dosage of naringenin and saccharin ratio is 1:0.95；In the aqueous suspension of naringenin, the quality of naringenin and water Than for 1:0.9；In the aqueous solution of saccharin, the mass ratio of saccharin and water is 1:1.8.
The purity that HPLC tests the eutectic of the naringenin and saccharin is 96.2%.
X-ray powder diffraction test is identical as embodiment 19.
Embodiment 21: a kind of eutectic of naringenin and saccharin, preparation method are as follows: prepare the aqueous suspension of naringenin respectively With the aqueous solution of saccharin, the aqueous solution of saccharin is added in the aqueous suspension of naringenin under agitation, is stirred at 56 DEG C 5hr is reacted, filtrate, filtrate freeze-drying are filtered to take.
The mole dosage of naringenin and saccharin ratio is 1:1.00；In the aqueous suspension of naringenin, the quality of naringenin and water Than for 1:1.1；In the aqueous solution of saccharin, the mass ratio of saccharin and water is 1:2.1.
The purity that HPLC tests the eutectic of the naringenin and saccharin is 95.7%.
X-ray powder diffraction test is identical as embodiment 19.
Comparative example 14: a kind of reaction of naringenin and saccharin, operating method are as follows: prepare the ethyl alcohol of naringenin respectively The ethanol solution of solution and saccharin under agitation adds to the ethanol solution of saccharin in the ethanol solution of naringenin, 55 It is stirred to react 6hr at DEG C, filters to take filtrate, filtrate freeze-drying.
The mole dosage of naringenin and saccharin ratio is 1:0.98；In the ethanol solution of naringenin, the matter of naringenin and ethyl alcohol Amount is than being 1:1.0；In the ethanol solution of saccharin, the mass ratio of saccharin and ethyl alcohol is 1:2.0.
Nuclear-magnetism test verifying naringenin and the not formed eutectic of saccharin.
A kind of embodiment 22: eutectic of naringenin and saccharin, preparation method are as follows: the dry core of Anacardiaceae plant stalk tree fruit Shell crushes, and adds ethyl acetate and water, back flow reaction 5hr takes ethyl acetate phase, is lyophilized into powder, as dry nucleocapsid extract；Respectively The aqueous suspension of dry nucleocapsid extract and the aqueous solution of saccharin are prepared, the aqueous solution of saccharin is added into dry nucleocapsid under agitation In the aqueous suspension of extract, it is stirred to react 6hr at 55 DEG C, filters to take filtrate, filtrate freeze-drying.
When preparing dry nucleocapsid extract, Anacardiaceae plant stalk sets the mass ratio of the dry nucleocapsid powder of fruit, ethyl acetate and water For 1:2.0:2.0；In dry nucleocapsid extract and saccharin reaction system, the mole dosage ratio of dry nucleocapsid extract and saccharin is 272: 177；In the aqueous suspension of dry nucleocapsid extract, the mass ratio of dry nucleocapsid extract and water is 1:1.0；In the aqueous solution of saccharin, The mass ratio of saccharin and water is 1:2.0.
The purity that HPLC tests the eutectic of the naringenin and saccharin is 98.1%.
X-ray powder diffraction test is identical as embodiment 19.
A kind of embodiment 23: eutectic of naringenin and saccharin, preparation method are as follows: the dry core of Anacardiaceae plant stalk tree fruit Shell crushes, and adds ethyl acetate and water, back flow reaction 4hr takes ethyl acetate phase, is lyophilized into powder, as dry nucleocapsid extract；Respectively The aqueous suspension of dry nucleocapsid extract and the aqueous solution of saccharin are prepared, the aqueous solution of saccharin is added into dry nucleocapsid under agitation In the aqueous suspension of extract, it is stirred to react 7hr at 54 DEG C, filters to take filtrate, filtrate freeze-drying.
When preparing dry nucleocapsid extract, Anacardiaceae plant stalk sets the mass ratio of the dry nucleocapsid powder of fruit, ethyl acetate and water For 1:1.9:1.9；In dry nucleocapsid extract and saccharin reaction system, the mole dosage ratio of dry nucleocapsid extract and saccharin is 272: 174；In the aqueous suspension of dry nucleocapsid extract, the mass ratio of dry nucleocapsid extract and water is 1:0.9；In the aqueous solution of saccharin, The mass ratio of saccharin and water is 1:1.8.
The purity that HPLC tests the eutectic of the naringenin and saccharin is 94.9%.
X-ray powder diffraction test is identical as embodiment 19.
A kind of embodiment 24: eutectic of naringenin and saccharin, preparation method are as follows: the dry core of Anacardiaceae plant stalk tree fruit Shell crushes, and adds ethyl acetate and water, back flow reaction 6hr takes ethyl acetate phase, is lyophilized into powder, as dry nucleocapsid extract；Respectively The aqueous suspension of dry nucleocapsid extract and the aqueous solution of saccharin are prepared, the aqueous solution of saccharin is added into dry nucleocapsid under agitation In the aqueous suspension of extract, it is stirred to react 5hr at 56 DEG C, filters to take filtrate, filtrate freeze-drying.
When preparing dry nucleocapsid extract, Anacardiaceae plant stalk sets the mass ratio of the dry nucleocapsid powder of fruit, ethyl acetate and water For 1:2.1:2.1；In dry nucleocapsid extract and saccharin reaction system, the mole dosage ratio of dry nucleocapsid extract and saccharin is 272: 183；In the aqueous suspension of dry nucleocapsid extract, the mass ratio of dry nucleocapsid extract and water is 1:1.1；In the aqueous solution of saccharin, The mass ratio of saccharin and water is 1:2.1.
The purity that HPLC tests the eutectic of the naringenin and saccharin is 95.2%.
X-ray powder diffraction test is identical as embodiment 19.
Comparative example 15: a kind of reaction of naringenin and saccharin, operating method are as follows: Anacardiaceae plant stalk tree fruit Dry nucleocapsid crushes, and adds ethyl acetate, back flow reaction 5hr filters to take filtrate, is lyophilized into powder, as dry nucleocapsid extract；Match respectively The aqueous suspension of dry nucleocapsid extract and the aqueous solution of saccharin are made, the aqueous solution of saccharin is added into dry nucleocapsid under agitation and is mentioned It takes in the aqueous suspension of object, is stirred to react 6hr at 55 DEG C, filter to take filtrate, filtrate freeze-drying.
When preparing dry nucleocapsid extract, the dry nucleocapsid powder of Anacardiaceae plant stalk tree fruit, the mass ratio of ethyl acetate are 1: 2.0；In dry nucleocapsid extract and saccharin reaction system, the mole dosage ratio of dry nucleocapsid extract and saccharin is 272:177；Dry core In the aqueous suspension of shell extract, the mass ratio of dry nucleocapsid extract and water is 1:1.0；In the aqueous solution of saccharin, saccharin and water Mass ratio be 1:2.0.
Nuclear-magnetism test verifying naringenin and the not formed eutectic of saccharin.
Embodiment 25: a kind of tea tree pest repellant of Extracts from Plant Recourses, based on molal weight, including 1 part of carvacrol, capsicum 1.00 parts of element, 0.50 part of Gastrodin and 0.33 part of naringenin.
Embodiment 26: a kind of tea tree pest repellant of Extracts from Plant Recourses, based on molal weight, carvacrol and fumaric acid are total to Brilliant 1 part, 1.00 parts of the eutectic of capsaicine and succinic acid, 0.50 part of the eutectic and naringenin of Gastrodin and niacinamide and saccharin 0.33 part of eutectic.
Embodiment 27: a kind of tea tree pest repellant of Extracts from Plant Recourses, based on molal weight, carvacrol and fumaric acid are total to Brilliant 1 part, 0.90 part of the eutectic of capsaicine and succinic acid, 0.45 part of the eutectic and naringenin of Gastrodin and niacinamide and saccharin 0.30 part of eutectic.
Embodiment 28: a kind of tea tree pest repellant of Extracts from Plant Recourses, based on molal weight, carvacrol and fumaric acid are total to Brilliant 1 part, 1.10 parts of the eutectic of capsaicine and succinic acid, 0.55 part of the eutectic and naringenin of Gastrodin and niacinamide and saccharin 0.37 part of eutectic.
The solubility test of pest repellant
Solubility of the ocular estimate test sample in 25 DEG C of pure water, parallel testing 5 times, is averaged.
Test sample includes carvacrol, capsaicine, Gastrodin and naringenin and embodiment 25-28 as control；Its The sample source of the eutectic of carvacrol and fumaric acid is embodiment 1 in middle embodiment 26-28, the eutectic of capsaicine and succinic acid Sample source is embodiment 7, and the sample source of the eutectic of Gastrodin and niacinamide is
The sample source of the eutectic of embodiment 13, naringenin and saccharin is embodiment 19.
Test result is as shown in table 1.Table 1 show: in 25 DEG C of pure water, carvacrol, capsaicine, Gastrodin, naringenin with And the solubility of embodiment 25 is below 0.01mg/ml, the solubility of embodiment 26-28 is 15~20mg/ml, embodiment 26- 28 solubility is significantly improved.
Table 1
Sample Solubility (mg/ml)
Carvacrol < 0.01
Capsaicine < 0.01
Gastrodin < 0.01
Naringenin < 0.01
Embodiment 25 < 0.01
Embodiment 26 15~20
Embodiment 27 15~20
Embodiment 28 15~20
Each component in embodiment 26 is changed into source, carries out solubility test, test result is as shown in table 2.Table 2 is shown: In 25 DEG C of pure water, the sample source of the eutectic of carvacrol and fumaric acid is the sample of the eutectic of embodiment 1-6, capsaicine and succinic acid Product source is that the sample source of the eutectic of embodiment 7-12, Gastrodin and niacinamide is embodiment 13-18, naringenin and saccharin The sample source of eutectic is that the solubility of the embodiment 26 of embodiment 19-24 is 15~20mg/ml, and difference in solubility is little.
Table 2
Indoor toxicity test
Carvacrol, capsaicine, Gastrodin and naringenin and embodiment 25 are dissolved with dehydrated alcohol respectively, and a small amount of Tween 80 is added After emulsification, 40,10g/L concentration is diluted to respectively with water for examination.
Embodiment 26-28 is diluted with water to 40,5g/L concentration for examination respectively.Wherein carvacrol and richness in embodiment 26-28 The sample source of the eutectic of horse acid is embodiment 1, and the sample source of the eutectic of capsaicine and succinic acid is embodiment 7, Gastrodin It is embodiment 13 with the sample source of the eutectic of niacinamide, the sample source of the eutectic of naringenin and saccharin is embodiment 19.
Using infusion process, each 30 test worms of processing (select Euproctis pseudoconspersa Euproctispseudoconspersa Strand, also known as malicious caterpillar, yaw worm, caterpillar, euproctis pseudoconspersa, the spicy that itches etc., belong to squama, wing mesh Lymantriidae), 3 repetitions.It is same The test worm of processing is dipped in well 30s in medical fluid with small yarn cage mounted simultaneously, then takes out and is put into difference after blotting excessive moisture with filter paper Culture dish in.It is fed with fresh tea free, the raising in growth cabinet (temperature is 25 DEG C, relative humidity 80%), separately If distilled water control treatment, 3d inspection result after processing calculates the death rate.
Test result is as shown in table 3.Table 3 is shown: carvacrol, capsaicine, Gastrodin, naringenin and embodiment 25-28 There is certain cytotoxicity to Euproctis pseudoconspersa, wherein embodiment 25-28 is stronger to the cytotoxicity of Euproctis pseudoconspersa.
Table 3
Pharmacodynamic test
With reference to National Standard of the People's Republic of China GB/T17980.55-2004 (insecticide control tea tree tea geometrid, tea hair Worm), test medicine, comparison medicament and the processing of the cell of blank control arrange (plot area 24m using random district's groups2), cell Between set protection row separate.
Carvacrol, capsaicine, Gastrodin and naringenin and embodiment 25 are dissolved with dehydrated alcohol respectively, and addition is spat on a small quantity After 80 emulsification of temperature, it is diluted with water.
Embodiment 26-28 is diluted with water respectively.Wherein the sample of the eutectic of carvacrol and fumaric acid comes in embodiment 26-28 Source is embodiment 1, and the sample source of the eutectic of capsaicine and succinic acid is embodiment 7, the sample of the eutectic of Gastrodin and niacinamide Product source is embodiment 13, and the sample source of the eutectic of naringenin and saccharin is embodiment 19.
Sample applied amount is 1125g/hm2, clear water is used as blank control, 4 repetitions of every processing by spraying.Selection is in Euproctis pseudoconspersa The application of low instar larvae occurance peak, medical fluid dosage 750L/hm spraying to tea leaf front and back sides2.5 points of every cell samplings, every point Fixed 2 plants of tea tree for taking Euproctis pseudoconspersa ovum and larva investigate the larva number on 10 plants of tea trees altogether.Insect population, medicine are investigated before medicine Afterwards 1,3,7d respectively investigates 1 remaining worm amount, calculates control efficiency as follows respectively: Revision insect recluced rate=(borer population-before being administered Borer population after application)/it is administered preceding borer population × 100%；Control efficiency=(treatment region Revision insect recluced rate-blank district insect population decline Rate)/(100- blank district Revision insect recluced rate) × 100%.
Test result is as shown in table 4.Table 4 is shown: carvacrol, capsaicine, Gastrodin, naringenin and embodiment 25-28 There is certain control efficiency to Euproctis pseudoconspersa, wherein embodiment 25-28 is preferable to the control efficiency of Euproctis pseudoconspersa；Compared to embodiment 25, embodiment 26-28 is more preferable in the time delay of control efficiency.
Table 4
Certainly, above is representative instance of the invention, and in addition to this, the present invention can also have other a variety of specific embodiment parties Formula, all technical solutions formed using equivalent substitution or equivalent transformation, is all fallen within the scope of protection of present invention.

Claims (7)

1. a kind of tea tree pest repellant of Extracts from Plant Recourses, characterized in that based on molal weight, including 1 part of carvacrol, capsaicine 0.90~1.10 part, 0.45~0.55 part of Gastrodin and 0.30~0.37 part of naringenin.
2. a kind of tea tree pest repellant of Extracts from Plant Recourses according to claim 1, characterized in that the carvacrol of selection Form is the eutectic of carvacrol and fumaric acid, and the form of the capsaicine of selection is the eutectic of capsaicine and succinic acid, the day of selection The form of numb element is the eutectic of Gastrodin and niacinamide, and the form of the naringenin of selection is the eutectic of naringenin and saccharin；
Based on molal weight, the tea tree pest repellant includes being total to for 1 part of eutectic, capsaicine and the succinic acid of carvacrol and fumaric acid The eutectic 0.30 of 0.45~0.55 part of the eutectic and naringenin and saccharin of 0.90~1.10 part brilliant, Gastrodin and niacinamide~ 0.37 part.
3. a kind of tea tree pest repellant of Extracts from Plant Recourses according to claim 2, characterized in that
It is radiated using Cu-K α, the X-ray powder diffraction figure that the eutectic of the carvacrol and fumaric acid is indicated with 2 θ is with bottom It sets with characteristic peak: 3.5 ± 0.2 °, 4.3 ± 0.2 °, 6.2 ± 0.2 °, 8.9 ± 0.2 °, 15.4 ± 0.2 ° and 20.1 ± 0.2 °；
It is radiated using Cu-K α, the X-ray powder diffraction figure that the eutectic of the capsaicine and succinic acid is indicated with 2 θ is with bottom Set with characteristic peak: 5.1 ± 0.2 °, 7.1 ± 0.2 °, 10.3 ± 0.2 °, 13.2 ± 0.2 °, 17.2 ± 0.2 ° and 22.8 ± 0.2°；
It is radiated using Cu-K α, the X-ray powder diffraction figure that the eutectic of the Gastrodin and niacinamide is indicated with 2 θ is with bottom Set with characteristic peak: 3.3 ± 0.2 °, 3.9 ± 0.2 °, 4.4 ± 0.2 °, 6.9 ± 0.2 °, 10.9 ± 0.2 °, 19.2 ± 0.2 °, 25.5 ± 0.2 °, 29.2 ± 0.2 ° and 33.2 ± 0.2 °；
It is radiated using Cu-K α, the X-ray powder diffraction figure that the eutectic of the naringenin and saccharin is indicated with 2 θ is in following position With characteristic peak: 7.2 ± 0.2 °, 8.2 ± 0.2 °, 10.2 ± 0.2 °, 11.2 ± 0.2 °, 15.5 ± 0.2 °, 17.5 ± 0.2 °, 18.3 ± 0.2 °, 19.7 ± 0.2 °, 23.2 ± 0.2 ° and 25.1 ± 0.2 °.
4. a kind of tea tree pest repellant of Extracts from Plant Recourses according to claim 3, characterized in that
It is radiated using Cu-K α, the X-ray powder diffraction figure that the eutectic of the carvacrol and fumaric acid is indicated with 2 θ is with bottom It sets with characteristic peak and its relative intensity:
2 θ of the angle of diffraction Relative intensity 1% 3.5±0.2° 1.2 4.3±0.2° 4.5 6.2±0.2° 15.2 8.9±0.2° 45.6 15.4±0.2° 100.0 20.1±0.2° 5.1；
It is radiated using Cu-K α, the X-ray powder diffraction figure that the eutectic of the capsaicine and succinic acid is indicated with 2 θ is with bottom It sets with characteristic peak and its relative intensity:
2 θ of the angle of diffraction Relative intensity 1% 5.1±0.2° 22.1 7.1±0.2° 3.2 10.3±0.2° 4.5 13.2±0.2° 8.0 17.2±0.2° 46.4 22.8±0.2° 100.0；
It is radiated using Cu-K α, the X-ray powder diffraction figure that the eutectic of the Gastrodin and niacinamide is indicated with 2 θ is with bottom It sets with characteristic peak and its relative intensity；
2 θ of the angle of diffraction Relative intensity 1% 3.3±0.2° 2.6 3.9±0.2° 4.5 4.4±0.2° 3.9 6.9±0.2° 100.0 10.9±0.2° 22.2 19.2±0.2° 33.8 25.5±0.2° 7.3 29.2±0.2° 4.2 33.2±0.2° 6.2；
It is radiated using Cu-K α, the X-ray powder diffraction figure that the eutectic of the naringenin and saccharin is indicated with 2 θ is in following position With characteristic peak and its relative intensity:
2 θ of the angle of diffraction Relative intensity 1% 7.2±0.2° 6.2 8.2±0.2° 7.3 10.2±0.2° 4.2 11.2±0.2° 25.3 15.5±0.2° 100.0 17.5±0.2° 17.9 18.3±0.2° 8.1 19.7±0.2° 22.4 23.2±0.2° 9.1 25.1±0.2° 4.2。
。
5. a kind of tea tree pest repellant of Extracts from Plant Recourses according to claim 1, characterized in that
The eutectic of the carvacrol and fumaric acid the preparation method comprises the following steps: respectively prepare carvacrol ethanol solution and fumaric acid second Alcoholic solution under agitation adds to the ethanol solution of fumaric acid in the ethanol solution of carvacrol, stirs at 48~52 DEG C 3~5hr is reacted, solid, drying are filtered to take；The mole dosage of carvacrol and fumaric acid ratio is 1:0.95~1.05；Carvacrol In ethanol solution, the mass ratio of carvacrol and ethyl alcohol is 1:0.8~1.2；In the ethanol solution of fumaric acid, fumaric acid and ethyl alcohol Mass ratio is 1:1.8~2.5；
The eutectic of the capsaicine and succinic acid the preparation method comprises the following steps: preparing the aqueous isopropanol and succinic acid of capsaicine respectively Isopropanol suspension under agitation adds to the isopropanol suspension of succinic acid in the aqueous isopropanol of capsaicine, 54 It is stirred to react 7~9hr at~56 DEG C, filters to take solid, drying；The mole dosage of capsaicine and succinic acid ratio be 1:0.95~ 1.00；In the aqueous isopropanol of capsaicine, the mass ratio of capsaicine and isopropanol is 1:0.8~1.2；The isopropanol of succinic acid is mixed In suspension, the mass ratio of succinic acid and isopropanol is 1:2.8~3.2；
The eutectic of the Gastrodin and niacinamide the preparation method comprises the following steps: respectively prepare Gastrodin aqueous suspension and niacinamide water Solution under agitation adds to the aqueous solution of niacinamide in the aqueous suspension of Gastrodin, is stirred to react 1 at 38~41 DEG C ~3hr filters to take filtrate, filtrate freeze-drying；The mole dosage of Gastrodin and niacinamide ratio is 1:0.95~1.00；The water of Gastrodin In suspension, the mass ratio of Gastrodin and water is 1:0.5~0.7；In the aqueous solution of niacinamide, the mass ratio of niacinamide and water is 1:1.4~1.6；
The eutectic of the naringenin and saccharin the preparation method comprises the following steps: respectively prepare naringenin aqueous suspension and saccharin it is water-soluble Liquid under agitation adds to the aqueous solution of saccharin in the aqueous suspension of naringenin, it is stirred to react 5 at 54~56 DEG C~ 7hr filters to take filtrate, filtrate freeze-drying；The mole dosage of naringenin and saccharin ratio is 1:0.95~1.00；The water of naringenin is suspended In liquid, the mass ratio of naringenin and water is 1:0.9~1.1；In the aqueous solution of saccharin, the mass ratio of saccharin and water be 1:1.8~ 2.1。
6. a kind of tea tree pest repellant of Extracts from Plant Recourses according to claim 2, characterized in that
The eutectic of the carvacrol and fumaric acid the preparation method comprises the following steps: dry origanum oil crushes, be added ethyl alcohol, back flow reaction 3~ 5hr filters to take filtrate concentration, as wild marjoram oil extract；The ethanol solution for preparing fumaric acid, under agitation by fumaric acid Ethanol solution add in wild marjoram oil extract, be stirred to react 3~5hr at 48~52 DEG C, filter to take solid, drying；Preparation When wild marjoram oil extract, the mass ratio of origanum oil and ethyl alcohol is 1:4.5~5.5, and filtrate is concentrated into the 1/4~1/3 of original volume；Ox Into oil extract and fumaric acid reaction system, the mass ratio of origanum oil and fumaric acid is 150:110~122；Wild marjoram oil extract In object, the mass ratio of carvacrol and ethyl alcohol is 1:0.8~1.2；In the ethanol solution of fumaric acid, the mass ratio of fumaric acid and ethyl alcohol For 1:1.8~2.5；
The eutectic of the capsaicine and succinic acid the preparation method comprises the following steps: xerophagia Capsicum crushing, ethyl acetate, back flow reaction is added 7~9hr filters to take filtrate, and filtrate is lyophilized into powder, as pepper extract；The aqueous isopropanol of pepper extract is prepared respectively With the isopropanol suspension of succinic acid, the isopropanol suspension of succinic acid is added to the isopropyl of pepper extract under agitation In alcoholic solution, it is stirred to react 7~9hr at 54~56 DEG C, filters to take solid, drying；When preparing pepper extract, capsicum and second The mass ratio of acetoacetic ester is 1:3.2~3.6；In pepper extract and succinic acid reaction system, pepper extract and succinic acid Mass ratio is 305:112~118；In the aqueous isopropanol of pepper extract, the mass ratio of pepper extract and isopropanol is 1: 0.8~1.2；In the isopropanol suspension of succinic acid, the mass ratio of succinic acid and isopropanol is 1:2.8~3.2；
The eutectic of the Gastrodin and niacinamide the preparation method comprises the following steps: dry day snippings block crushes, acetonitrile and ethyl acetate is added, returns Stream 2~4hr of reaction, filters to take filtrate, filtrate is lyophilized into powder, as Rhizoma Gastrodiae extract；The water for preparing Rhizoma Gastrodiae extract respectively is mixed The aqueous solution of suspension and niacinamide under agitation adds to the aqueous solution of niacinamide in the aqueous suspension of Rhizoma Gastrodiae extract, It is stirred to react 1~3hr at 38~41 DEG C, filters to take filtrate, filtrate freeze-drying；When preparing Rhizoma Gastrodiae extract, day snippings block, acetonitrile Mass ratio with ethyl acetate is 1:1.2~1.5:1.0~1.2；In Rhizoma Gastrodiae extract and niacinamide reaction system, Rhizoma Gastrodiae is extracted The mass ratio of object and niacinamide is 286:116~122；In the aqueous suspension of gastrodin, gastrodin and water Mass ratio is 1:0.5~0.7；In the aqueous solution of niacinamide, the mass ratio of niacinamide and water is 1:1.4~1.6；
The eutectic of the naringenin and saccharin the preparation method comprises the following steps: Anacardiaceae plant stalk tree fruit dry nucleocapsid crush, add acetic acid Ethyl ester and water, 4~6hr of back flow reaction, take ethyl acetate phase, are lyophilized into powder, as dry nucleocapsid extract；Dry nucleocapsid is prepared respectively The aqueous solution of saccharin is added to the water of dry nucleocapsid extract by the aqueous suspension of extract and the aqueous solution of saccharin under agitation In suspension, it is stirred to react 5~7hr at 54~56 DEG C, filters to take filtrate, filtrate freeze-drying；When preparing dry nucleocapsid extract, paint The mass ratio that tree section plant obstructs the dry nucleocapsid powder for setting fruit, ethyl acetate and water is 1:1.9~2.1:1.9~2.1；Dry nucleocapsid mentions It takes in object and saccharin reaction system, the mole dosage ratio of dry nucleocapsid extract and saccharin is 272:174~183；Dry nucleocapsid extracts In the aqueous suspension of object, the mass ratio of dry nucleocapsid extract and water is 1:0.9~1.1；In the aqueous solution of saccharin, saccharin and water Mass ratio is 1:1.8~2.1.
7. a kind of tea tree pest repellant of Extracts from Plant Recourses according to claim 2, characterized in that based on molal weight, The tea tree pest repellant include 1.00 parts of the eutectic of 1 part of eutectic, capsaicine and the succinic acid of carvacrol and fumaric acid, Gastrodin and 0.33 part of eutectic of 0.50 part of the eutectic of niacinamide and naringenin and saccharin.
CN201910618832.2A 2019-07-10 2019-07-10 A kind of tea tree pest repellant of Extracts from Plant Recourses Pending CN110226598A (en)

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