CN110269071A - A kind of mosquito repellent composition and preparation method thereof - Google Patents
A kind of mosquito repellent composition and preparation method thereof Download PDFInfo
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- CN110269071A CN110269071A CN201910700126.2A CN201910700126A CN110269071A CN 110269071 A CN110269071 A CN 110269071A CN 201910700126 A CN201910700126 A CN 201910700126A CN 110269071 A CN110269071 A CN 110269071A
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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
- A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
- A01N37/02—Saturated carboxylic acids or thio analogues thereof; Derivatives 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
- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
- A01N65/40—Liliopsida [monocotyledons]
- A01N65/44—Poaceae or Gramineae [Grass family], e.g. bamboo, lemon grass or citronella grass
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Abstract
The invention belongs to biomedicine fields, and in particular to a kind of mosquito repellent composition and preparation method thereof.A kind of mosquito repellent composition, the raw material including following parts by weight: 80~160 parts of wild mint extract, 60~160 parts of Caraway essential oil, 60~120 parts of oil of Cymbopogon winterianus, 30~80 parts of rose pelargonium essential oil, 30~80 parts of mentha piperita oil, 50~100 parts of calamus essential oil, 20~60 parts of Lavender, 40~120 parts of d-8- acetoxycarvotanacetone.The mosquito repellent composition can extend d-8- acetoxycarvotanacetone to the mosquito repellent repellent guard time of user.The composition can be applied in the production and research and development of related mosquito repellent product.
Description
Technical field
The invention belongs to biomedicine fields, and in particular to a kind of mosquito repellent composition and preparation method thereof.
Background technique
Biting for mosquito brings the propagation of all a variety of viruses and disease, causes pole to people's lives and health
Big harm.Mosquito repelling drug refers to the chemicals for being applied on skin or clothing and preventing bite by mosquitos and harassing and wrecking.Repellent
Drug itself has Volatilized smell without insecticidal action, dare not approach after smelling insect, and current existing repellent drug is to keep away
Mosquito ester, dihydropyrone, octylene glycol, Metadelphene etc..China scientific research personnel is in the research of natural plants repellent ingredient, it was found that a variety of
Natural materials with repellent activity, such as d-8- acetoxycarvotanacetone.D-8- acetoxycarvotanacetone
It is a kind of active constituent extracted from the Lamiaceae plants such as wild mint (MenthahaplocalyxBriq.), d-8- second
The other dihydro Eucarvone of acyloxy has the effect of mosquito repellent.The small toxicity of d-8- acetoxycarvotanacetone, side effect
Small, manufactured frost, emulsion have preferable repellent action to 9 kinds of mosquitoes such as Anopheles sinensis, Culex quinquefasciatus and aedes vexans.d-8-
Acetoxycarvotanacetone can also be prepared using chemically synthesized method.But the other dihydro Pueraria lobota thread of d-8- acetoxyl group
The stability of ketone is general, and after being applied on skin or clothing, d-8- acetoxycarvotanacetone volatilizees quickly, and
And gradually oxidation by air is decomposed, and causes the compound limited to the mosquito repellent repellent guard time of user.If by d-8- acetyl
The case where other dihydro Eucarvone of oxygroup is directly smeared on the skin, is absorbed by the skin there is also the compound, d-8- acetoxyl group
Other dihydro Eucarvone is further depleted.In these cases, need to increase the dosage of d-8- acetoxycarvotanacetone
Or smeared repeatedly within shorter time interval and use d-8- acetoxycarvotanacetone, it can be only achieved and keep away mosquito mosquito repellent
Purpose.Drawbacks described above limits the extensive use of the compound, and repellent drug currently on the market is still with Metadelphene etc.
It is main.
Summary of the invention
The purpose of the present invention is to provide a kind of mosquito repellent composition, which can extend d-8- acetoxyl group other two
Mosquito repellent repellent guard time of the hydrogen Eucarvone to user.
In order to solve the above technical problems, technical solution of the present invention is as follows: a kind of mosquito repellent composition, including following parts by weight
Raw material: 80~160 parts of wild mint extract, 60~160 parts of Caraway essential oil, 60~120 parts of oil of Cymbopogon winterianus, Pelargonium roseum essence
Oily 30~80 parts, 30~80 parts of mentha piperita oil, 50~100 parts of calamus essential oil, 20~60 parts of Lavender, d-8- acetyl oxygen
40~120 parts of the other dihydro Eucarvone of base.
When by adopting the above technical scheme, the mosquito repellent composition of the raw material preparation of the above parts by weight, wild mint extract, Pueraria lobota thread
Sub- essential oil, oil of Cymbopogon winterianus, rose pelargonium essential oil, mentha piperita oil, calamus essential oil, Lavender and d-8- acetoxyl group are other
Dihydro Eucarvone generates synergistic effect, when extending mosquito repellent repellent protection of the d-8- acetoxycarvotanacetone to user
Between.
The utility model has the advantages that
(1) lemongrass (Cymbopogoncitratus), Pelargonium roseum (Pelargonium graveolensL'
Herit.), American mint (Mentha X piperita L), calamus (Acoruscalamus L.) and lavender
(Lavandulaangustifolia Mill.) all has certain Volatilized smell, and essential oil obtained is extracted from above-mentioned raw materials,
The repelling effect of enhancing d-8- acetoxycarvotanacetone can be cooperateed with.
(2) oil of Cymbopogon winterianus, rose pelargonium essential oil, mentha piperita oil, calamus essential oil and Lavender have slow controlled release
The evaporation rate of d-8- acetoxycarvotanacetone is maintained certain level by the effect of agent, avoids d-8- acetyl oxygen
The too fast loss of the other dihydro Eucarvone of base extends this composition to the mosquito repellent repellent guard time of user.
(3) Caraway essential oil helps to alleviate stress and fatigue, can moisturize the skin, and Pueraria lobota thread is added in the present compositions
Sub- essential oil can play certain health-care efficacy while mosquito repellent.
(4) Caraway essential oil and d-8- acetoxycarvotanacetone are used in combination, d-8- acetoxyl group can be increased
Mosquito repellent repellent guard time of the other dihydro Eucarvone to user.Although inventor is not the study found that Caraway essential oil itself has
There is mosquito repellent repellent, but Caraway essential oil there is the protection of highly significant to make d-8- acetoxycarvotanacetone
With, and the rate of release of d-8- acetoxycarvotanacetone can be controlled, to extend d-8- acetoxyl group other two
Mosquito repellent repellent guard time of the hydrogen Eucarvone to user.Caraway essential oil is added in the present compositions, can increase whole
The mosquito repelling effect of a composition, has achieved the effect that unexpected.
(5) present composition is significant to bite by mosquitos repellent effect, and has effects that long-acting mosquito-driving, when average repellent
Between up to 14h or more the calculation method of repellent time (average see experimental example 1).
Further, a kind of mosquito repellent composition, the raw material including following parts by weight: 160 parts of wild mint extract, Caraway essence
Oily 160 parts, 120 parts of oil of Cymbopogon winterianus, 80 parts of rose pelargonium essential oil, 80 parts of mentha piperita oil, 100 parts of calamus essential oil, lavender
60 parts of essential oil, 120 parts of d-8- acetoxycarvotanacetone.
By adopting the above technical scheme, the mosquito repellent composition of said ratio has preferable mosquito repellent repellent effect, is a kind of excellent
The proportion mode of change.
Further, Caraway essential oil extracts acquisition by the following method:
Step (1): pre-processing the fruit of Caraway, obtains Caraway powder；
Step (2): 50% ethyl alcohol is added in the Caraway powder obtained in step (1), obtains extraction system；Ultrasonic treatment institute
After stating extraction system, liquid phase is filtered to take, obtains Caraway crude extract；
Step (3): diatomite is added in Caraway crude extract, stands after mixing, filters to take diatomite；In diatom
95% ethyl alcohol is added in soil, stands after mixing evenly, liquid phase is taken after filtering, obtains the fat-soluble crude extract of Caraway；
Step (4): air-distillation processing is carried out to the fat-soluble crude extract of Caraway in step (3), collects coarse-fine oil；Slightly
Essential oil obtains Caraway essential oil after removing moisture content.
By adopting the above technical scheme, ultrasound assisted extraction is first used, Caraway crude extract is obtained, reuses kieselguhr adsorption
Liposoluble constituent in Caraway crude extract reuses 95% ethyl alcohol and elutes to diatomite, by liposoluble substance from diatom
It is washed out in soil, is handled using air-distillation and obtain Caraway essential oil.Thus the Caraway essential oil that method obtains has preferable
Biological effect, Caraway essential oil and d-8- acetoxycarvotanacetone are used in combination, and it is other can to increase d-8- acetoxyl group
Dihydro Eucarvone is to the mosquito repellent repellent guard time of user, thus when the repellent action for significantly extending the present composition continues
Between.
The Caraway essential oil that comparison is obtained by the method for supercritical carbon dioxide extracting, the Caraway essential oil that this law obtains
The extension of repellent time acts on more preferably.Inventor analyzes this law and extracts the ingredient of the Caraway essential oil obtained and traditional super face
The ingredient for the Caraway essential oil that the method for boundary's carbon dioxide abstraction obtains, it is found that two kinds of essential oils have different on ingredient.This
The main component that method extracts the Caraway essential oil obtained is limonene, carvol, 1- methyl -5- methylene -8- (1- methyl second
Base) -1,6- cyclodecadiene and apiol.Inventor analyzes the Pueraria lobota obtained using the method for supercritical carbon dioxide extracting in turn
Sub- essential oil in detail, main component are carvol and limonene.The Caraway essential oil that different extracting methods obtains is deposited on ingredient
In certain gap, two kinds of Caraway essential oils are in the effect of mosquito repellent repellent time for extending d-8- acetoxycarvotanacetone
There is also differences.
In addition, the main function of diatomite in the prior art is the substances such as adsorbing contaminant, pigment, then diatomite is lost
Abandon, but in the present solution, using the both effectiveness ingredient of kieselguhr adsorption (i.e. liposoluble constituent) rather than impurity, then utilize height
Effect ingredient in diatomite is eluted out by the ethyl alcohol of purity again, has haved the function that purify and be enriched with functional component.At this
In technical solution, ingredient has preferable synergistic effect to d-8- acetoxycarvotanacetone the effect of kieselguhr adsorption.
Further, in step (2), the mass ratio of Caraway powder and 50% ethyl alcohol is 1:30, ultrasonic power 150W.
By adopting the above technical scheme, effect ingredient in Caraway can sufficiently be extracted, can get higher extraction of essential oil
Rate.
Further, in step (3), the amount ratio of diatomite and Caraway crude extract is 15g:100ml.
By adopting the above technical scheme, diatomite can sufficiently adsorb the liposoluble constituent in Caraway crude extract.
Further, in step (4), the moisture content in coarse-fine oil is removed using anhydrous sodium sulfate, obtains Caraway essential oil.
By adopting the above technical scheme, anhydrous sodium sulfate is the conventional reagent removed water from essential oil in the prior art, at low cost
And it easily obtains.
Further, the wild mint extract is prepared by the following method: carrying out overcritical dioxy to fresh wild mint
Change carbon extraction, obtains the coarse-fine oil of wild mint；Then oil coarse-fine to wild mint carries out molecular distillation, obtains wild mint extract.
By adopting the above technical scheme, it can be isolated and purified from wild mint oil with the method for molecular distillation, from each fraction
It can choose the wild mint extract for providing mosquito repelling effect.
Further, a kind of preparation method of mosquito repellent composition, comprising the following steps: by wild mint extract, Caraway essence
Oil, oil of Cymbopogon winterianus, rose pelargonium essential oil, mentha piperita oil, calamus essential oil, Lavender and the other dihydro of d-8- acetoxyl group
Eucarvone mixes in proportion, obtains mixture；Then mixture is distributed in crude vegetal, obtains mosquito repellent composition；The day
Right vegetable oil is olive oil or Sweet Almond Oil.
By adopting the above technical scheme, the advantages of available liposoluble product (mosquito repellent composition is liposoluble product), liposoluble product:
(1) liposoluble product has effects that moisturize the skin, and especially winter, two season of spring uses the liposoluble product, can prevent chapped skin；
(2) skin water loss can also be prevented in addition to it can bite with mosquito repellent using the liposoluble product in summer, two season of autumn, and
There is protective action to ultraviolet irradiation.
Further, a kind of preparation method of mosquito repellent composition, comprising the following steps: by wild mint extract, Caraway essence
Oil, oil of Cymbopogon winterianus, rose pelargonium essential oil, mentha piperita oil, calamus essential oil, Lavender and the other dihydro of d-8- acetoxyl group
Eucarvone mixes in proportion, obtains mixture；Then mixture, solubilizer are added to the water, obtain mosquito repellent combination after mixing
Object；The solubilizer is SP-115C, SP-115A or SP-410.
By adopting the above technical scheme, it can get water-soluble product (mosquito repellent composition be water-soluble product), the advantages of water-soluble product:
(1) its bioavilability is higher compared with fat-soluble product；(2) water-soluble product is increased using SP-115C, SP-115A and SP-410 etc.
Solvent can avoid using solvent (such as ethyl alcohol), reduce stimulation of the organic solvent to human skin, while making the perfume (or spice) of product again
Gas and quality are purer, and functional effect is more preferably；(3) water-soluble product has preferable skin-moisturizing, skin, non-greasy, smooth fine and smooth, suction
Receive many advantages, such as quick.
Further, a kind of preparation method of mosquito repellent composition, comprising the following steps: by wild mint extract, Caraway essence
Oil, oil of Cymbopogon winterianus, rose pelargonium essential oil, mentha piperita oil, calamus essential oil, Lavender and the other dihydro of d-8- acetoxyl group
Eucarvone mixes in proportion, obtains mixture；Then mixture and surfactant are added to the water, mosquito repellent combination is obtained after emulsification
Object；The surfactant is sorbester p18 or Tween 80.
By adopting the above technical scheme, the advantages of available emulsion products (mosquito repellent composition is emulsion products), emulsion products:
Emulsifying product is the emulsified body of Water-In-Oil or oil-in-water, and in use, which has slow releasing function to functional component, and
And the lotion property of emulsion is stablized, and saves and carries all more convenient.
Specific embodiment
It is further described below by specific embodiment:
Embodiment 1: liposoluble product of the preparation containing the present composition
Key instrument and equipment: II analytic type supercritical extract system of SFE- (global analytical and testing instrument Co., Ltd)；
VKL70-5-WRS-T type molecular distillation (German Rui Da Co., Ltd)；Wild mint, Caraway, lavender, lemongrass, Pelargonium
Certain herbaceous plants with big flowers, American mint and calamus are purchased from peasant household.
1.d-8- acetoxycarvotanacetone is prepared using semisynthesis, and d- Eucarvone adds through sodium bisulfite
At obtaining the other dihydro Eucarvone of d-8- hydroxyl, then obtain d-8- acetoxycarvotanacetone through acetylation.This method is existing
There is the known method in technology, d-8- acetoxycarvotanacetone of the purity 99% or more can get by this method.
2. the preparation of wild mint extract
Wild mint herb is crushed, is placed in extraction kettle, extraction of essential oil is carried out, using supercritical carbon dioxide extracting
Method, each Parameter Conditions are as follows: extracting pressure 30MPa, 50 DEG C of extraction temperature, extraction time 2h.After extraction process is completed, by dioxy
Change carbon flow body and be passed through the separation that separator carries out purpose ingredient, the flow of CO 2 fluid is 7kg/h, and separator pressure is
8MPa, temperature are 40 DEG C, and separation process continues 2h, and after separation process terminates, 4 DEG C of standing 2h take oil after water-oil separation
Phase obtains the coarse-fine oil of wild mint.Then passing through molecular distillation, half fraction, obtains the limpid oiliness active matter of wild mint before taking,
As wild mint extract.
3. the preparation of Caraway essential oil
The fruit of Caraway is crushed, Caraway powder is obtained, Caraway powder is then put into flask and is added extracting solution, is obtained
Extraction system.Wherein, 30g extracting solution is added in every 1g Caraway powder, extracting solution is 50% ethyl alcohol.It is ultrasonically treated said extracted body
System, ultrasonic power 150W, ultrasonic treatment number are that twice, each 30min is spaced 5min between ultrasonic treatment twice.Whole
In a ultrasonication, 80 DEG C of waters bath with thermostatic control of flask are filtered to take liquid phase, obtain Caraway crude extract after completing ultrasonic treatment.
Diatomite is added in Caraway crude extract, diatomite is used to adsorb the liposoluble constituent in Caraway crude extract, diatomite
Additional amount is that 15g diatomite is added in every 100ml Caraway crude extract, stands 2h after mixing evenly, filters to take diatomite.It is inhaling
95% ethyl alcohol is added in diatomite with liposoluble constituent, 95% ethyl alcohol of 20ml is added in every 1g diatomite, quiet after mixing evenly
2h is set, takes liquid phase after filtering, obtains the fat-soluble crude extract of Caraway.The fat-soluble crude extract of Caraway is put into distilling flask, into
Row air-distillation processing stops distillation when in the fraction of outflow without oil droplet, and the coarse-fine oil distillated is collected using collector, uses
Anhydrous sodium sulfate is carried out dehydrating coarse-fine oil, obtains Caraway essential oil, and Caraway essential oil is light yellow transparent liquid.Gas phase
Chromatograph-mas spectrometer identifies that the main component of Caraway essential oil is limonene to chemical component in Caraway essential oil
(25.41%) and carvol (20.81%), 1- methyl -5- methylene -8- (1- Methylethyl) -1,6- cyclodecadiene
(21.30%) and apiol (17.23%).
4. the preparation of other essential oils
Lavender: the pollen of lavender is broken, it is placed in extraction kettle, extraction of essential oil is carried out, using overcritical two
Carbonoxide extraction, each Parameter Conditions are as follows: extracting pressure 20MPa, 30 DEG C of extraction temperature, extraction time 1.5h, carbon dioxide stream
Amount is 15kg/h.After extraction process is completed, CO 2 fluid is passed through the separation that separator carries out purpose ingredient, titanium dioxide
The flow of carbon flow body is 8kg/h, and separator pressure 8MPa, temperature is 30 DEG C, and separation process continues 1h, and separation process terminates it
Afterwards, 4 DEG C of standing 2h take oily phase, obtain Lavender after water-oil separation.
Oil of Cymbopogon winterianus: lemongrass herb being crushed, is placed in extraction kettle, extraction of essential oil is carried out, using overcritical titanium dioxide
Carbon extraction, each Parameter Conditions are as follows: extracting pressure 30MPa, 35 DEG C of extraction temperature, extraction time 1.5h, carbon dioxide flow is
15kg/h.After extraction process is completed, CO 2 fluid is passed through the separation that separator carries out purpose ingredient, carbon dioxide stream
The flow of body is 7kg/h, and separator pressure 8MPa, temperature is 30 DEG C, and separation process continues 1h, after separation process terminates, 4
DEG C stand 2h take oily phase after water-oil separation, obtain oil of Cymbopogon winterianus.
Rose pelargonium essential oil: the blade of Pelargonium roseum being crushed, is placed in extraction kettle, is carried out extraction of essential oil, is adopted
With supercritical carbon dioxide extraction method, each Parameter Conditions are as follows: extracting pressure 15MPa, 40 DEG C of extraction temperature, extraction time 2h, two
Oxidation carbon flow is 15kg/h.After extraction process is completed, CO 2 fluid is passed through point that separator carries out purpose ingredient
From the flow of CO 2 fluid is 7kg/h, and separator pressure 4MPa, temperature is 40 DEG C, and separation process continues 2h, separation
After process terminates, 4 DEG C of standing 2h take oily phase, obtain rose pelargonium essential oil after water-oil separation.
American mint essential oil: American mint blade being crushed, is placed in extraction kettle, carries out extraction of essential oil, is faced using super
Boundary's carbon dioxide extraction method, each Parameter Conditions are as follows: extracting pressure 25MPa, 40 DEG C of extraction temperature, extraction time 1.5h, titanium dioxide
Carbon flow is 15kg/h.Extraction process complete after, by CO 2 fluid be passed through separator carry out purpose ingredient separation, two
The flow of carbon oxide fluid is 9kg/h, and separator pressure 8MPa, temperature is 40 DEG C, and separation process continues 1h, separation process knot
After beam, 4 DEG C of standing 2h take oily phase after water-oil separation, obtain American mint essential oil.
Calamus essential oil: calamus herb being crushed, is placed in extraction kettle, extraction of essential oil is carried out, using overcritical titanium dioxide
Carbon extraction, each Parameter Conditions are as follows: extracting pressure 30MPa, 30 DEG C of extraction temperature, extraction time 2h, carbon dioxide flow is
15kg/h.After extraction process is completed, CO 2 fluid is passed through the separation that separator carries out purpose ingredient, carbon dioxide stream
The flow of body is 7kg/h, and separator pressure 8MPa, temperature is 30 DEG C, and separation process continues 2h, after separation process terminates, 4
DEG C stand 2h take oily phase after water-oil separation, obtain calamus essential oil.
5. the preparation of liposoluble product
By wild mint extract, Caraway essential oil, oil of Cymbopogon winterianus, rose pelargonium essential oil, mentha piperita oil, calamus essence
Oil, Lavender and d-8- acetoxycarvotanacetone are according to mass ratio 160:160:120:80:80:100:60:120
Mixing, obtains mixture A, and olive oil then is added in mixture A, obtains mosquito repellent composition after mixing, is named as liposoluble product
A.Wherein, 80ml olive oil is added in every 10g mixture A, olive oil can be substituted with crude vegetals such as Sweet Almond Oil etc..
By wild mint extract, Caraway essential oil, oil of Cymbopogon winterianus, rose pelargonium essential oil, mentha piperita oil, calamus essence
Oil, Lavender and d-8- acetoxycarvotanacetone are mixed according to mass ratio 80:60:60:30:30:50:20:40,
Mixture B is obtained, olive oil then is added in mixture B, mosquito repellent composition is obtained after mixing, is named as liposoluble product B.Its
In, 80ml olive oil is added in every 10g mixture B, olive oil can be substituted with crude vegetals such as Sweet Almond Oil etc..
By wild mint extract, Caraway essential oil, oil of Cymbopogon winterianus, rose pelargonium essential oil, mentha piperita oil, calamus essence
Oil, Lavender and d-8- acetoxycarvotanacetone are mixed according to mass ratio 120:120:100:50:50:70:40:60
It closes, obtains mixture C, olive oil then is added in mixture C, obtain mosquito repellent composition after mixing, be named as liposoluble products C.
Wherein, 80ml olive oil is added in every 10g mixture C, olive oil can be substituted with crude vegetals such as Sweet Almond Oil etc..
Embodiment 2: water-soluble product of the preparation containing the present composition
In the present embodiment, each raw material 1-4 that the preparation method is the same as that of Example 1, difference be manufactured in the present embodiment be
Final water-soluble products, concrete operation method are as follows:
By wild mint extract, Caraway essential oil, oil of Cymbopogon winterianus, rose pelargonium essential oil, mentha piperita oil, calamus essence
Oil, Lavender and d-8- acetoxycarvotanacetone are according to mass ratio 160:160:120:80:80:100:60:120
Mixing, obtains mixture A, then mixture A is added in solubilizer SP-115C, is stirred evenly, deionized water is added, and mixes
Mosquito repellent composition is obtained after closing uniformly, is named as water-soluble product A.Wherein, in every 10g mixture A be added 50ml deionized water and
30mlSP-115C.
By wild mint extract, Caraway essential oil, oil of Cymbopogon winterianus, rose pelargonium essential oil, mentha piperita oil, calamus essence
Oil, Lavender and d-8- acetoxycarvotanacetone are mixed according to mass ratio 80:60:60:30:30:50:20:40,
Mixture B is obtained, then mixture B is added in solubilizer SP-115A, is stirred evenly, adds deionized water, mixing is equal
Mosquito repellent composition is obtained after even, is named as water-soluble product B.Wherein, 50ml deionized water and 30ml are added in every 10g mixture B
SP-115A.
By wild mint extract, Caraway essential oil, oil of Cymbopogon winterianus, rose pelargonium essential oil, mentha piperita oil, calamus essence
Oil, Lavender and d-8- acetoxycarvotanacetone are mixed according to mass ratio 120:120:100:50:50:70:40:60
It closes, obtains mixture C, then mixture C is added in solubilizer SP-410, is stirred evenly, add deionized water, mix
Mosquito repellent composition is obtained after uniformly, is named as water-soluble products C.Wherein, 50ml deionized water and 30ml are added in every 10g mixture C
SP-410.
Embodiment 3: emulsion products of the preparation containing the present composition
In the present embodiment, each raw material 1-4 that the preparation method is the same as that of Example 1, difference be manufactured in the present embodiment be
Final emulsion products, the present embodiment use emulsifying technology, form emulsion with surfactant emulsifies such as sorbester p18 or Tween 80s
Series of products, concrete operation method are as follows:
By wild mint extract, Caraway essential oil, oil of Cymbopogon winterianus, rose pelargonium essential oil, mentha piperita oil, calamus essence
Oil, Lavender and d-8- acetoxycarvotanacetone are according to mass ratio 160:160:120:80:80:100:60:120
Mixing, obtains mixture A, is then add to deionized water mixture A, and sorbester p18 is added in water, in 88 DEG C of temperature
Under, mosquito repellent composition is obtained after strong stirring emulsification, is named as emulsion products A.Wherein, in every 10g mixture A be added 50ml go from
Sub- water and 30ml sorbester p18.
By wild mint extract, Caraway essential oil, oil of Cymbopogon winterianus, rose pelargonium essential oil, mentha piperita oil, calamus essence
Oil, Lavender and d-8- acetoxycarvotanacetone are mixed according to mass ratio 80:60:60:30:30:50:20:40,
Mixture B, then mixture B is add to deionized water, and Tween 80 is added in water, 88 DEG C at a temperature of, by force
Mosquito repellent composition is obtained after power stirring and emulsifying, is named as emulsion products B.Wherein, 50ml deionized water is added in every 10g mixture B
With 30ml Tween 80.
By wild mint extract, Caraway essential oil, oil of Cymbopogon winterianus, rose pelargonium essential oil, mentha piperita oil, calamus essence
Oil, Lavender and d-8- acetoxycarvotanacetone are mixed according to mass ratio 120:120:100:50:50:70:40:60
Close, obtain mixture C, be then add to deionized water mixture C, and sorbester p18 is added in water, 88 DEG C at a temperature of,
Mosquito repellent composition is obtained after strong stirring emulsification, is named as emulsion products C.Wherein, 50ml deionization is added in every 10g mixture C
Water and 30ml sorbester p18.
Comparative example 1: prior art preparation Caraway essential oil is used
Caraway essential oil is prepared with the following method: the fruit of Caraway being crushed, obtains Caraway powder, and by Caraway powder
It is placed in extraction kettle, the condition extracted using supercritical carbon dioxide extraction method are as follows: extracting pressure 35MPa, extraction temperature
46 DEG C, extraction time 2h, carbon dioxide flow 18kg/h.After said extracted process is completed, CO 2 fluid is passed through
Separator carries out the separation of purpose ingredient, and the flow of CO 2 fluid is 9kg/h, separator pressure 8MPa, temperature 50
DEG C, separation process continues 1h, and after separation process terminates, 4 DEG C of standing 2h take oily phase, as Caraway after water-oil separation
Essential oil.Chemical component is identified in the Caraway essential oil prepared using gas chromatograph-mass spectrometer (GC-MS) to this comparative example, Pueraria lobota thread
The main component of sub- essential oil is carvol (55.62%) and limonene (21.35%).
Experimental example 1: the research of influence of the Caraway essential oil to d-8- acetoxycarvotanacetone mosquito repellent repellent effect
This experiment is referring to " GB/T 13917.9-2009 agriculture chemical registration hygienic insecticide indoor pharmacodynamic test and evaluation the 9th
Part: repellant " it carries out.
1. experimental group designs
Group 1.1 is prepared by the following method for agent of having a try: preparation d-8- acetoxycarvotanacetone solution, Example
D-8- acetoxycarvotanacetone in 1 is added in olive oil, obtains d-8- acetoxycarvotanacetone solution, so that
The mass fraction of d-8- acetoxycarvotanacetone is 20 weight %.Take the Caraway essential oil and d-8- second in comparative example 1
Acyloxy other dihydro Eucarvone solution mixing, must organize 1 for agent of having a try.Wherein, Caraway essential oil and d-8- acetoxyl group other two
The mass ratio of hydrogen Eucarvone solution is 1:1.
Group 1.2 is prepared by the following method for agent of having a try: preparation d-8- acetoxycarvotanacetone solution, Example
D-8- acetoxycarvotanacetone in 1 is added in olive oil, obtains d-8- acetoxycarvotanacetone solution, so that
The mass fraction of d-8- acetoxycarvotanacetone is 20 weight %.Caraway essential oil and d-8- second in Example 1
Acyloxy other dihydro Eucarvone solution mixing, must organize 2 for agent of having a try.Wherein, Caraway essential oil and d-8- acetoxyl group other two
The mass ratio of hydrogen Eucarvone solution is 1:1.
Group 1.3 is prepared by the following method for agent of having a try: the d-8- acetoxycarvotanacetone in Example 1, and
D-8- acetoxycarvotanacetone solution is prepared for solvent using olive oil, wherein d-8- acetoxycarvotanacetone
Mass fraction be 10 weight %.
Group 1.4 is for the Caraway essential oil that agent of having a try is in embodiment 1.
Group 1.5 is for the Caraway essential oil that agent of having a try is in comparative example 1.
Group 1.6 is olive oil for agent of having a try.
2. test method
The adult of aedes albopictus is placed in mosquito cage (80cm × 40cm × 40cm), the mosquito kind of aedes albopictus is purchased from Yunnan Province
Epidemic disease study on prevention institute.500 female aedes albopictus are put into each mosquito cage.Experiment carries out at room temperature, humidity
It is 70%.Subject protrudes into hand in the mosquito cage equipped with 500 female aedes albopictus, if stopping falling in the lineae ablicantes of subject on hand
The quantity of yellow-fever mosquito is greater than 35, illustrates that the preparation of mosquito cage is qualified, can be used to carry out the repellent experiment of next step.
Being uniformly applied on the skin of 5 × 5cm of the back of the hand in every group of experimental group for agent of having a try, hand rest part tightly hides
Lid.Every kind of applying amount for agent of having a try is as shown in table 1 in group 1.1- group 1.6.After coating 4h, subject protrudes into hand in mosquito cage,
Hand stops 3min in mosquito cage, and every 2h is once tested later.As long as the hand of subject is primary by bite by mosquitos, this is decided that
The repellent effect failure for agent of having a try of experimental group.Before each test, mosquito aggressiveness test need to be carried out, to guarantee to test
As a result reliability.In test process, records data and calculate effective percentage: the effective percentage (%) of experimental group each time point=not
The quantity for the subject bitten/subject's sum × 100%；Total effective guarantor of average repellent time (h)=each experimental group
Protect the time/subject's sum.Some subject at 14 hours, bitten by this time point, that has the subject for agent of having a try
Effect guard time is denoted as 12 hours；Some subject at 4 hours, bitten by this time point, that is for having a try agent to the subject's
Effective protecting time is denoted as 0 hour.In addition, not continuing test inspection to the repellent situation behind 20 hours for agent of having a try
It surveys, what subject was not bitten also after 20 hours, the effective protecting time of the subject is denoted as 20 hours for having a try agent.Often
Total effective protecting time of a experimental group refers to that every group of confession has a try agent to the summation of the repellent guard time of each subject.It is real
Test that the results are shown in Table 1:
Table 1: 1 repellent experimental result of experimental example (N/A indicates the test for not carrying out the time point)
As shown in table 1, from a group experimental result for 1.1- group 1.6: Caraway essential oil as negative control olive oil,
Do not have repelling effect, but Caraway essential oil so enters into d-8- acetoxycarvotanacetone, has and significantly prolongs
The effect of long repellent time；In addition, the extracting mode of Caraway essential oil can influence the effect of Caraway essential oil, prepared by embodiment 1
Caraway essential oil repellent time prolongation effect than Caraway essential oil prepared by comparative example 1 repellent time prolongation effect more
It is good.
Experimental example 2: the research of influence of the Caraway essential oil to mosquito repellent composition mosquito repellent repellent effect
The method of this experimental example is substantially with experimental example 2, referring again to " GB/T 13917.9-2009 agriculture chemical registration health
The 9th part of insecticide indoor pharmacodynamic test and evaluation: repellant " it carries out, main research Caraway essential oil is (real to mosquito repellent composition
Apply 1-3 preparation) influence of mosquito repellent repellent effect, experimental group is as follows:
Group 2.1 is for the liposoluble product A that agent of having a try is in embodiment 1.
Group 2.2 is for the water-soluble product A that agent of having a try is in embodiment 2.
Group 2.3 is for the emulsion products A that agent of having a try is in embodiment 3.
Group 2.4 is the liposoluble product A without Caraway derived essential oil for agent of having a try, and is named as liposoluble product A '.Liposoluble produces
The preparation method of product A ' is substantially with the preparation method of liposoluble product A, the difference lies in that being added without Pueraria lobota when mixing each raw material
Sub- derived essential oil in detail.
Group 2.5 is the water-soluble product A without Caraway derived essential oil for agent of having a try, and is named as water-soluble product A '.Water-soluble production
The preparation method of product A ' is substantially with the preparation method of water-soluble product A, the difference lies in that being added without Pueraria lobota when mixing each raw material
Sub- derived essential oil in detail.
Group 2.6 is the emulsion products A without Caraway derived essential oil for agent of having a try, and is named as emulsion products A '.Emulsion produces
The preparation method of product A ' is substantially with the preparation method of emulsion products A, the difference lies in that being added without Pueraria lobota when mixing each raw material
Sub- derived essential oil in detail.
Group 2.7 is olive oil for agent of having a try.
Group 2.8 is the Caraway essential oil prepared in embodiment 1 for agent of having a try.
Experimental result is as shown in table 2, by group experimental result of 2.1- group 2.8 it is found that Caraway essential oil increases liposoluble production
The repellent time of product A, water-soluble product A and emulsion products A.The activity of the not no mosquito repellent of Caraway essential oil itself, still, Pueraria lobota thread
Sub- essential oil be added to containing in combined object liposoluble product of the invention, water-soluble product and emulsion products, can increase repellent effect
The duration of fruit can extend 4 hours or so repellent time, reach unexpected technical effect.
Table 2: 1 repellent experimental result of experimental example (N/A indicates the test for not carrying out the time point)
Experimental example 3: the validity experiment of the mosquito repellent combination of embodiment 1-3 preparation
The method of this experimental example is substantially with experimental example 2, referring again to " GB/T 13917.9-2009 agriculture chemical registration health
The 9th part of insecticide indoor pharmacodynamic test and evaluation: repellant " it carries out, the mosquito repellent combination average of testing example 1-3 preparation drives
The time is kept away, the results are shown in Table 3, and the mosquito repellent combination product of embodiment 1-3 preparation all has the longer repellent time, can satisfy
Use demand.
Table 3: the validity experimental result of the mosquito repellent combination of embodiment 1-3 preparation
| Tested number | Applying amount (mg) | The average repellent time (h) | |
| Liposoluble product A (embodiment 1) | 20 | 50 | 15.0 |
| Liposoluble product B (embodiment 1) | 20 | 50 | 14.6 |
| Liposoluble products C (embodiment 1) | 20 | 50 | 14.2 |
| Water-soluble product A (embodiment 2) | 20 | 50 | 15.2 |
| Water-soluble product B (embodiment 2) | 20 | 50 | 14.2 |
| Water-soluble products C (embodiment 2) | 20 | 50 | 14.8 |
| Emulsion products A (embodiment 3) | 20 | 50 | 15.4 |
| Emulsion products B (embodiment 3) | 20 | 50 | 14.8 |
| Emulsion products C (embodiment 3) | 20 | 50 | 14.6 |
What has been described above is only an embodiment of the present invention, and the common sense such as well known specific structure and characteristic are not made herein in scheme
Excessive description.It, without departing from the structure of the invention, can be with it should be pointed out that for those skilled in the art
Several modifications and improvements are made, these also should be considered as protection scope of the present invention, these all will not influence what the present invention was implemented
Effect and patent practicability.The scope of protection required by this application should be based on the content of the claims, in specification
The records such as specific embodiment can be used for explaining the content of claim.
Claims (10)
1. a kind of mosquito repellent composition, which is characterized in that the raw material including following parts by weight: 80~160 parts of wild mint extract, Pueraria lobota
60~160 parts of sub- essential oil, 60~120 parts of oil of Cymbopogon winterianus, 30~80 parts of rose pelargonium essential oil, mentha piperita oil 30~80 in detail
Part, 50~100 parts of calamus essential oil, 20~60 parts of Lavender, 40~120 parts of d-8- acetoxycarvotanacetone.
2. a kind of mosquito repellent composition according to claim 1, which is characterized in that the raw material including following parts by weight: wild thin
160 parts of lotus extract, 160 parts of Caraway essential oil, 120 parts of oil of Cymbopogon winterianus, 80 parts of rose pelargonium essential oil, mentha piperita oil 80
Part, 100 parts of calamus essential oil, 60 parts of Lavender, 120 parts of d-8- acetoxycarvotanacetone.
3. a kind of mosquito repellent composition according to claim 1 or 2, which is characterized in that Caraway essential oil mentions by the following method
Take acquisition:
Step (1): pre-processing the fruit of Caraway, obtains Caraway powder；
Step (2): 50% ethyl alcohol is added in the Caraway powder obtained in step (1), obtains extraction system；It is mentioned described in ultrasonic treatment
After taking system, liquid phase is filtered to take, obtains Caraway crude extract；
Step (3): diatomite is added in Caraway crude extract, stands after mixing, filters to take diatomite；In diatomite
95% ethyl alcohol is added, stands after mixing evenly, liquid phase is taken after filtering, obtains the fat-soluble crude extract of Caraway；
Step (4): air-distillation processing is carried out to the fat-soluble crude extract of Caraway in step (3), collects coarse-fine oil；Coarse-fine oil
Caraway essential oil is obtained after removing moisture content.
4. a kind of mosquito repellent composition according to claim 3, which is characterized in that in step (2), Caraway powder and 50%
The mass ratio of ethyl alcohol is 1:30, ultrasonic power 150W.
5. a kind of mosquito repellent composition according to claim 4, which is characterized in that in step (3), diatomite and Caraway
The amount ratio of crude extract is 15g:100ml.
6. a kind of mosquito repellent composition according to claim 5, which is characterized in that in step (4), use anhydrous sodium sulfate
The moisture content in coarse-fine oil is removed, Caraway essential oil is obtained.
7. a kind of mosquito repellent composition according to claim 6, which is characterized in that the wild mint extract is by the following method
It is prepared: supercritical carbon dioxide extracting being carried out to fresh wild mint, obtains the coarse-fine oil of wild mint；Then coarse-fine to wild mint
Oil carries out molecular distillation, obtains wild mint extract.
8. a kind of preparation method of mosquito repellent composition described in any one of according to claim 1-2,4-7 claim, special
Sign is, comprising the following steps: wild mint extract, Caraway essential oil, oil of Cymbopogon winterianus, rose pelargonium essential oil, green pepper sample is thin
Lotus oil, calamus essential oil, Lavender and d-8- acetoxycarvotanacetone mix in proportion, obtain mixture；Then will
Mixture is distributed in crude vegetal, obtains mosquito repellent composition；The crude vegetal is olive oil or Sweet Almond Oil.
9. a kind of preparation method of mosquito repellent composition described in any one of according to claim 1-2,4-7 claim, special
Sign is, comprising the following steps: wild mint extract, Caraway essential oil, oil of Cymbopogon winterianus, rose pelargonium essential oil, green pepper sample is thin
Lotus oil, calamus essential oil, Lavender and d-8- acetoxycarvotanacetone mix in proportion, obtain mixture；Then will
Mixture, solubilizer are added to the water, and obtain mosquito repellent composition after mixing；The solubilizer be SP-115C, SP-115A or
SP-410 is one such.
10. a kind of preparation method of mosquito repellent composition described in any one of according to claim 1-2,4-7 claim, special
Sign is, comprising the following steps: wild mint extract, Caraway essential oil, oil of Cymbopogon winterianus, rose pelargonium essential oil, green pepper sample is thin
Lotus oil, calamus essential oil, Lavender and d-8- acetoxycarvotanacetone mix in proportion, obtain mixture；Then will
Mixture and surfactant are added to the water, and mosquito repellent composition is obtained after emulsification；The surfactant is sorbester p18 or tween
80。
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