CN109135927A - Flower method of extraction of essential oil - Google Patents
Flower method of extraction of essential oil Download PDFInfo
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- CN109135927A CN109135927A CN201710503908.8A CN201710503908A CN109135927A CN 109135927 A CN109135927 A CN 109135927A CN 201710503908 A CN201710503908 A CN 201710503908A CN 109135927 A CN109135927 A CN 109135927A
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- jasmine
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- 239000000341 volatile oil Substances 0.000 title claims abstract description 64
- 238000000605 extraction Methods 0.000 title claims abstract description 29
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 40
- 238000000034 method Methods 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000003208 petroleum Substances 0.000 claims abstract description 14
- 238000004090 dissolution Methods 0.000 claims abstract description 5
- 238000001914 filtration Methods 0.000 claims abstract description 5
- 239000004519 grease Substances 0.000 claims abstract description 5
- 241000207840 Jasminum Species 0.000 claims description 60
- 235000010254 Jasminum officinale Nutrition 0.000 claims description 60
- CDOSHBSSFJOMGT-UHFFFAOYSA-N linalool Chemical compound CC(C)=CCCC(C)(O)C=C CDOSHBSSFJOMGT-UHFFFAOYSA-N 0.000 claims description 26
- 239000001490 (3R)-3,7-dimethylocta-1,6-dien-3-ol Substances 0.000 claims description 13
- CDOSHBSSFJOMGT-JTQLQIEISA-N (R)-linalool Natural products CC(C)=CCC[C@@](C)(O)C=C CDOSHBSSFJOMGT-JTQLQIEISA-N 0.000 claims description 13
- 229930007744 linalool Natural products 0.000 claims description 13
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 10
- 239000003381 stabilizer Substances 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000011780 sodium chloride Substances 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 4
- 239000002893 slag Substances 0.000 claims description 4
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims description 2
- 235000011941 Tilia x europaea Nutrition 0.000 claims description 2
- 239000004571 lime Substances 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 5
- 230000006837 decompression Effects 0.000 abstract description 4
- 239000000706 filtrate Substances 0.000 abstract description 4
- 238000000354 decomposition reaction Methods 0.000 abstract description 3
- 239000006227 byproduct Substances 0.000 abstract description 2
- 239000003205 fragrance Substances 0.000 description 11
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 8
- 238000004821 distillation Methods 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 7
- 238000010521 absorption reaction Methods 0.000 description 6
- 125000003118 aryl group Chemical group 0.000 description 6
- 239000002304 perfume Substances 0.000 description 6
- 239000003463 adsorbent Substances 0.000 description 5
- 239000000284 extract Substances 0.000 description 5
- 239000012530 fluid Substances 0.000 description 5
- 239000004615 ingredient Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 241000196324 Embryophyta Species 0.000 description 4
- 244000022198 Mirabilis jalapa Species 0.000 description 4
- 235000009053 Mirabilis jalapa Nutrition 0.000 description 4
- 239000010656 jasmine oil Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 238000001256 steam distillation Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- GLZPCOQZEFWAFX-UHFFFAOYSA-N Geraniol Chemical compound CC(C)=CCCC(C)=CCO GLZPCOQZEFWAFX-UHFFFAOYSA-N 0.000 description 3
- 239000001569 carbon dioxide Substances 0.000 description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 230000018044 dehydration Effects 0.000 description 3
- 238000006297 dehydration reaction Methods 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000005979 thermal decomposition reaction Methods 0.000 description 3
- 244000025254 Cannabis sativa Species 0.000 description 2
- 244000207740 Lemna minor Species 0.000 description 2
- 235000006439 Lemna minor Nutrition 0.000 description 2
- GLZPCOQZEFWAFX-JXMROGBWSA-N Nerol Natural products CC(C)=CCC\C(C)=C\CO GLZPCOQZEFWAFX-JXMROGBWSA-N 0.000 description 2
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 2
- 235000001855 Portulaca oleracea Nutrition 0.000 description 2
- 230000003796 beauty Effects 0.000 description 2
- 229910002090 carbon oxide Inorganic materials 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 230000005672 electromagnetic field Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 235000013599 spices Nutrition 0.000 description 2
- UFLHIIWVXFIJGU-ARJAWSKDSA-N (Z)-hex-3-en-1-ol Chemical compound CC\C=C/CCO UFLHIIWVXFIJGU-ARJAWSKDSA-N 0.000 description 1
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 1
- 235000017491 Bambusa tulda Nutrition 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000723346 Cinnamomum camphora Species 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 239000005792 Geraniol Substances 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 241000207834 Oleaceae Species 0.000 description 1
- 244000082204 Phyllostachys viridis Species 0.000 description 1
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 1
- 241001274961 Rubus repens Species 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000011425 bamboo Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- -1 cis- 3- hexene ester Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229960004756 ethanol Drugs 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000895 extractive distillation Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000004508 fractional distillation Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 229940113087 geraniol Drugs 0.000 description 1
- UFLHIIWVXFIJGU-UHFFFAOYSA-N hex-3-en-1-ol Natural products CCC=CCCO UFLHIIWVXFIJGU-UHFFFAOYSA-N 0.000 description 1
- 238000002169 hydrotherapy Methods 0.000 description 1
- MTNDZQHUAFNZQY-UHFFFAOYSA-N imidazoline Chemical class C1CN=CN1 MTNDZQHUAFNZQY-UHFFFAOYSA-N 0.000 description 1
- 125000002636 imidazolinyl group Chemical group 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000000874 microwave-assisted extraction Methods 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000013557 residual solvent Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 239000012178 vegetable wax Substances 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 230000003313 weakening effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/025—Recovery by solvent extraction
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/027—Recovery of volatiles by distillation or stripping
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Fats And Perfumes (AREA)
Abstract
The present invention provides a kind of flower method of extraction of essential oil, method includes the following steps: picking fresh flower, are put into micro-wave oven and dry to weightlessness 50~80%, then store, distill after flower is mixed with water, collect distillate;It is extracted with petroleum ether, the petroleum ether is concentrated under reduced pressure to give grease, ether dissolution is then added, is filtered with micropore filtering film, filtrate decompression is concentrated up to flower essential oil.This method simple process, extraction of essential oil rate is high, and decomposition by-products are few.
Description
Technical field
The invention belongs to extraction process technology fields, and in particular to a kind of flower method of extraction of essential oil, more particularly to it is a kind of
Extraction method for jasmine flower essential oil.
Background technique
The essential oil extracted from natural plants flowers is the important component of natural essence, in daily life and industry
There is important role in production.Essential oil is mainly used for food and drink, medicine, cosmetic industry, raw in particular with the people
The flat raising of running water, beauty culture are also increasing to the demand of essential oil, and current most popular hydrotherapy SPA, marrow is just
It is natural plant essence oil.
Earliest application is since natural perfume material to fragrance in history.Natural perfume material includes original untreated straight
The animals and plants scooped out send out fragrant position, further include the day for extracting or refining processing by physical method and have not been changed its original ingredient
Right fragrance." fragrance " that fragrant flower is come out in the Nature is to a kind of beauty of people, pleasant feeling.
Since the 1990s, global perfume industry realizes the trade monopoly of height, in addition closing in world commerce
The continuous weakening of tax limitation promotes the internationalization tendency of trans-corporation.Big spices and essence company of the world ten accounts for entirely at present
70% or more of perfume industry sales value.For China's starting than later, the research of this this respect is also fewer.
Jasmine is Oleaceae plants, is evergreen shrubs, is a kind of fine perfumery plant.Leaf, flower, the root of Mirabilis jalapa have
Medical value.Jasmine also has strong fragrance, not available for even more many flowers.Jasmine essential oil it is main effectively at
Dividing is volatile oil, mainly there is linalool, the cis- 3- hexene ester of acetic acid, nerol, cis- 3- hexenol and geraniol.
Single-lobe Jasmine is one kind that fragrance is the strongest in Jasmine.The single-lobe jasmonic bud open hour are early, Fu Huayi
As it is open at dusk 6~7, every hundred are spent weight, and volt spends 22~25 grams or so, debate that jasmine is light, and single-lobe jasmine fragrance is strong than double,
Fresh taste, considerably beyond bivalve Jasmine.
CN104887604A discloses a kind of Extraction method for jasmine flower essential oil, includes the following steps: the absorption of (1) essential oil:
With humid air stream by Jasmine under room temperature, then the humid air with jasmine essential oil is cooled to 0~10 DEG C, removes part water
Part;The condensed water for removing part moisture content adsorbs essential oil with adsorbent;(2) desorption of essential oil: extracted with supercritical carbon dioxide fluid
The active carbon for taking above-mentioned absorption jasmine essential oil obtains jasmine essential oil, and condensed water solubilizer recycles fragrance, air-introduced machine discharge
Gas also recycles fragrance.
CN104120037A discloses a kind of extracting method of jasmine essential oil, is made to being extracted with petroleum ether or pentane
Jasmine flower concrete, by ethyl alcohol dissolve freezing removing vegetable wax impurity, be distilled to recover etoh solvent, washing dealcoholysis thick jasmine is made
Thick refined jasmine oil is further separated off residual solvent with supercritical CO 2 by jasmine essential oil, and the pure jasmine anthosin of fragrance is made
Oil.
CN103740466A discloses a kind of Extraction method for jasmine flower essential oil, includes the following steps: the absorption of (1) essential oil:
New fresh jasmine is put on the flower stand of closed colored room, a point multilayer is placed, and humid air stream is passed through jasmine with air-introduced machine under room temperature
Then flower is placed the humid air with jasmine essential oil in cryogenic condensation room, the humid air with jasmine essential oil is made to cool down
To 0~10 DEG C, condensed water is discharged;The humid air for removing part moisture content, is adsorbed with adsorbent;(2) desorption of essential oil: overcritical two
Carbon oxide fluid extracts the adsorbent of above-mentioned absorption jasmine essential oil, obtains jasmine essential oil.
CN106318630A discloses a kind of Extraction method for jasmine flower essential oil, after including the following steps: that (1) cleans Jasmine
It is dried to the jasmine flower piece that moisture is no more than 10%, it is spare to be crushed to 40 mesh;(2) using LED light irradiation Jasmine grain: specifically adopting
With the light application time of 15-25min, intensity of illumination 15-20lx, the colour temperature of illumination is 5500-6000K;(3) weight is added is
Its 3 times dehydrated alcohol, stands 1h at 20 degrees celsius, obtains mixed solution;(4) mixing after step (3) processing is molten
Liquid is placed in Microwave Extraction Apparatus, under the conditions of the microwave power of 400w, carries out microwave treatment 10min;(5) vapor is then carried out
It extracts, and the crude product being collected into is refrigerated into 2h in 5 degrees Celsius of refrigerator, finally carry out centrifugally operated, water-oil separating again.
CN105482895A discloses a kind of extracting method of jasmine petal essential oil, male using supercritical carbon dioxide extracting
Red essential oil includes the following steps: that (1) morning 9-11 point is acquired without the undamaged of dewdrop, the branches and leaves with unopened petal,
It selects large bamboo or wicker basket dress to take the branches and leaves of picking, is transported to Hua Ku, single layer is spread out;(2) blade is cut off, the petiole and petal of 2-3cm long are stayed;
(3) Hua Ku keeps ventilation, and sprays fog, keeps relative humidity between 80-90%, and temperature is between 32-34 DEG C, culture flower
Bud is open;(4) after petal expansion, drying is sent into extractor, and extraction conditions is extractor: 34 DEG C of temperature, pressure
20MPa, separator: 35-38 DEG C of temperature, pressure 16MPa;Essential oil is isolated in the separator.
CN1202228A discloses one kind and is suitable for the pure natural New method for extracting jasmine oil of large-scale industry method production,
This method is at room temperature, without any solvent treatment process, to blow over the new fresh jasmine that layering is placed with humid air,
It takes the aroma ingredients that Jasmine distributes out of, and is trapped with special adsorbent, until Jasmine spits perfume (or spice) and finishes, then with overcritical two
Essential oil in carbon oxide fluid extraction and recovery adsorbent.
" the progress leaf autumn duckweed of jasmine essential oil extractive technique ", leaf autumn duckweed etc., " tropical crops journal ", 2014,35
(2): 406-412 analyzes Jasmine and releases fragrant mechanism and fragrance component, illustrate the common Water distillation extractor of current refined jasmine oil,
The principle and its advantage and disadvantage of the extracting methods such as solvent extraction method, absorption method, supercritical carbon dioxide fluid extraction release perfume according to Jasmine
Special habit is proposed using advanced technology subcritical fluid extraction method as a kind of environmental protection, efficient refined jasmine oil extracting method.
Above-mentioned document and it is other jasmine essential oil extraction efficiency is low in the prior art, and during the extraction process due to
Solvent action, heat effect etc. are easy to happen the degradation of volatile ingredient.This field need a kind of high extraction efficiency, simple process and
The flower method of extraction of essential oil that aromatic substance decomposes in extraction process can be effectively reduced.
Summary of the invention
In order to solve the above problems simultaneously, the present inventor is by further investigation and many experiments, to flower, especially jasmine
Flower fragrance ingredient is studied, and following technical scheme is proposed, and makes it possible to obtain flower essential oil with high recovery rate.
In one aspect of the invention, a kind of flower method of extraction of essential oil is provided, method includes the following steps: (1) is adopted
Pluck fresh flower, be put into micro-wave oven dry to weightlessness 50~80%, be then stored in refrigerator, storage temperature be -5 DEG C~-
10℃;(2) flower is shredded, is mixed according to flower with the ratio of water 1: 3~1: 5, is then distilled, be collected into from condenser cold
Lime set outflow starts timing, every the flower slag of taking-up in 1~2 hour, while being reentered into fresh flower, after continuous still 5-10 times, collects
Distillate;(3) petroleum ether that the 1/3-1/5 of distillate volume is incorporated as into distillate is extracted, and the extraction behaviour is repeated
Make 2-5 times, merges petroleum ether;(4) petroleum ether is concentrated under reduced pressure to give grease, ether dissolution is then added, use micropore
Filter membrane filtering, filtrate decompression is concentrated up to flower essential oil.
Preferably, the storage time in refrigerator is 10-60 days.
Preferably, the flower is the flower of Jasmine.It is highly preferred that the Jasmine is single-lobe jasmine.
In existing flower extraction of essential oil, often extraction of essential oil can not can be carried out after flower picking, be usually to adopt
Pluck rear room temperature storage.However, aromatic substance is easy in the case where flower is rich in moisture in flower in room temperature storing process
Recurring structure variation, can slowly be changed into non-aromatic Studies of The Aromatic Substances.Therefore, present invention selection is dried using micro-wave oven to weightlessness 50
~80%, preferably 70%.Microwave heating is different from traditional heating method, is not required to heat transfer process, it can make heating object
Material itself becomes calandria, even therefore the poor material of heat conductivity, heating temperature can also be reached in a very short period of time
Degree.For flower heating, hydrone is polarized in microwave electromagnetic field, has dipole characteristics, and with electromagnetic field
Frequency is constantly changing polar orientation, and molecule makees vibration at high speed, generates frictional heat, so that flower is heated up from inner deep, and each
Place's temperature is consistent, this characteristic of microwave heating can make flower be rapidly heated, and reach the critical point temperature of wherein inactive enzyme, add
The migration of fast flower constitution water, to keep essential oil loss minimum, and essential oil will not change colour because of heating.After quick dehydration
Flower carries out low-temperature storage again, can store for a long time and essential oil hardly occurs to reduce or deterioration, storage period may be up to 1
Year is even longer.If directly carrying out low-temperature storage without the quick dehydration of microwave, about 40% or more can be lost after 1 year
Essential oil.
Preferably, the single-lobe jasmine is the single-lobe jasmine of fresh flower half-open position.
For the present invention, in step (2), the water is the water containing NaCl.Preferably, the concentration of NaCl is 5-20
Weight %.
It is further preferred that the extraction stabilizer (or distillation stabilizer) in the water also containing 0.1-0.5 weight %.It steams
The temperature for evaporating extraction may result in essential oil and decomposed occur.Distillation of the invention is preferably steam distillation.Studies have shown that
It is the simplest with steam distillation operation in various distillation modes, it can not only reduce essential oil and fractionate out temperature, and can prevent
It decomposes or rotten.But there is also disadvantages for steam distillation, can cause thermographic compound in essential oil since operation temperature is higher
Thermal decomposition and facile hydrolysis ingredient hydrolysis.Based on described problem, the measure taken at present is directed to improve distillation equipment, example
Such as using the steaming of pressurization string, continuous still, multiple fractional distillation column distillation and the quick steam distillation form of worm-gear type.These modes flower
Take larger, needs biggish investment.For this purpose, the present invention joined stabilizer in distillation process, can subtract to a certain extent
The thermal decomposition of few essential oil.The stabilizer is preferably imidazoline stabilizer.It is highly preferred that the extraction stabilizer is lower formula (I)
Shown in imidazolinium compounds:
When the compound is added, should can associate with some derived essential oils in distillation process, so as to subtract
It is few to be thermally decomposed, when being extracted with organic solvent, and solution association can occur.
Primary Study proves, what the addition of formula (I) compound can make essential oil is reduced 30% or more by thermal decomposition.Especially
The decomposition of linalool can be reduced, this can clearly be seen that from the infrared spectrogram of Fig. 1 of the invention.
In another aspect of this invention, the jasmine essential oil obtained according to preceding method is additionally provided.Preferably, Jasmine
Free alcohol content is 30-70 weight % in essential oil.Preferably, linalool content is greater than 4.0 weight % in jasmine essential oil.
Detailed description of the invention
Fig. 1 is the infrared spectrogram for the jasmine essential oil that 2 method according to embodiments of the present invention obtains;
Fig. 2 is the infrared spectrogram for the jasmine essential oil that 2 method of comparative example obtains according to the present invention.
Specific embodiment
Below with reference to following embodiment and comparative example, the present invention is described in further detail, but embodiment party of the invention
Formula is without being limited thereto.
Embodiment 1
It chooses fresh Mirabilis jalapa (deriving from hundred Li Xin grass cultivation Co., Ltd of Jining), is put into micro-wave oven and dries to weightlessness
75%, it is then stored in refrigerator, storage temperature is -10 DEG C, and storage time is 30 days, flower is shredded, according to colored and water 1: 4
Ratio mixing, then distilled, be collected into condensate liquid outflow since condenser and start timing, every the colored slag of taking-up in 1 hour, together
When be reentered into fresh flower, after continuous still 6 times, collect distillate;1/5 petroleum of distillate volume is incorporated as into distillate
Ether is extracted, and is repeated described extracting operation 3 times, is merged petroleum ether;The petroleum ether is concentrated under reduced pressure to give grease, then
Ether dissolution is added, is filtered with micropore filtering film, filtrate decompression is concentrated up to jasmine essential oil, its infrared light is measured and sets a song to music
Line, while linalool content is measured with GC-MC, linalool content is 4.6wt.%.
Embodiment 2
It chooses fresh Mirabilis jalapa (deriving from hundred Li Xin grass cultivation Co., Ltd of Jining), is put into micro-wave oven and dries to weightlessness
75%, it is then stored in refrigerator, storage temperature is -10 DEG C, and storage time is 30 days, flower is shredded, according to colored and water 1: 4
Ratio mixing, the water be the formula (I) containing 10 weight %NaCl and 0.2 weight % shown in extract stabilizer (derive from lark
Prestige Reagent Company), then to be distilled, the timing since condenser is collected into condensate liquid outflow spends slag every taking-up in 1 hour,
While it being reentered into fresh flower, after continuous still 6 times, collect distillate;1/5 stone of distillate volume is incorporated as into distillate
Oily ether is extracted, and is repeated described extracting operation 3 times, is merged petroleum ether;The petroleum ether is concentrated under reduced pressure to give grease, so
After ether dissolution is added, filtered with micropore filtering film, filtrate decompression be concentrated up to jasmine essential oil, its infrared light is measured and sets a song to music
Line (see Fig. 1), while linalool content is measured with GC-MC, linalool content is 5.3wt.%.
Comparative example 1
The difference of the comparative example and embodiment 1, which is only that, does not carry out the processing of microwave weightlessness to fresh Mirabilis jalapa, uses simultaneously
GC-MC measures linalool content, and linalool content is 2.3wt.%.
Comparative example 2
The difference of the comparative example and embodiment 2 is only that in water used in extractive distillation to be added without shown in formula (I) and extract surely
Determine agent, measures the infrared spectrum curve (see Fig. 2) of the jasmine essential oil of acquisition, while measuring linalool content, fragrant camphor tree with GC-MC
Alcohol content is 2.9wt.%.
By above-described embodiment and comparative example clearly it can be seen from when using extracting method of the invention, aromatic substance
In representational linalool content it is significantly higher, show that it is more stable during the extraction process, this mainly has benefited from microwave
Quick dehydration improves its storage stability and extracts stability, and the addition for extracting stabilizer further improves its stabilization
Property.From infrared common, it is added without shown in formula (I) when extracting stabilizer, as seen from Figure 2, in 3000cm-1Observe bright in place
Aobvious absorption peak, is analyzed through MS, is aromatic substance, particularly the peak that linalool decomposition by-products generate.
This written description discloses the present invention, including optimal mode using example, and also enables those skilled in the art
The manufacture and use present invention.It is of the invention can patentable scope be defined by the claims, and may include this field skill
Other examples that art personnel expect.If this other examples have not different from the structural elements of the literal language of claims
Element, or if this other examples include the equivalent structure element with the literal language of claims without substantial differences,
Then this other examples are intended within the scope of claims.In the case where not will cause inconsistent degree, by reference to
It will be incorporated herein in place of all references referred to herein.
Claims (10)
1. flower method of extraction of essential oil, method includes the following steps:
(1) fresh flower is picked, is put into micro-wave oven and dries to weightlessness 50~80%, be then stored in refrigerator, storage temperature
It is -5 DEG C~-10 DEG C;
(2) flower is shredded, is mixed according to flower with the ratio of water 1: 3~1: 5, is then distilled, be collected into from condenser cold
Lime set outflow starts timing, every the flower slag of taking-up in 1~2 hour, while being reentered into fresh flower, after continuous still 5-10 times, collects
Distillate;
(3) petroleum ether that the 1/3-1/5 of distillate volume is incorporated as into distillate is extracted, and the extracting operation 2- is repeated
5 times, merge petroleum ether;
(4) petroleum ether is concentrated under reduced pressure to give grease, ether dissolution is then added, filtered with micropore filtering film, will filtered
Liquid is concentrated under reduced pressure up to flower essential oil.
2. according to the method described in claim 1, wherein the flower is the flower of Jasmine.
3. according to the method described in claim 2, wherein the Jasmine is single-lobe jasmine.
4. according to the method described in claim 3, wherein the single-lobe jasmine is the single-lobe jasmine of fresh flower half-open position.
5. method according to any of the preceding claims, wherein the water is to contain NaCl's in step (2)
Water.
6. according to the method described in claim 5, wherein the concentration of NaCl is 20 weight %.
Extraction stabilizer 7. method according to claim 5 or 6, in the water also containing 0.1-0.5 weight %.
8. the jasmine essential oil that method according to any of the preceding claims obtains.
9. jasmine essential oil according to claim 8, wherein free alcohol content is 30-70 weight %.
10. jasmine essential oil according to claim 9, wherein linalool content is greater than 4.0 weight %.
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CN105950293A (en) * | 2016-05-28 | 2016-09-21 | 黄宇松 | Extraction method of jasmine essential oil |
CN104513707B (en) * | 2014-12-16 | 2017-07-28 | 四川农业大学 | A kind of extracting method of chrysanthemum essential oil and the essential oil of extraction |
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CN104513707B (en) * | 2014-12-16 | 2017-07-28 | 四川农业大学 | A kind of extracting method of chrysanthemum essential oil and the essential oil of extraction |
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CN110903908A (en) * | 2019-12-13 | 2020-03-24 | 河北省农林科学院遗传生理研究所(河北省农林科学院农产品质量安全研究中心) | Preparation method of natural pear essence |
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