CN109135927A - Flower method of extraction of essential oil - Google Patents

Flower method of extraction of essential oil Download PDF

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Publication number
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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flower
jasmine
essential oil
extraction
water
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CN201710503908.8A
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CN109135927B (en
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不公告发明人
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Shanghai Li Mo Brand Management Co Ltd
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Shanghai Li Mo Brand Management Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B9/00Essential oils; Perfumes
    • C11B9/02Recovery or refining of essential oils from raw materials
    • C11B9/025Recovery by solvent extraction
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B9/00Essential oils; Perfumes
    • C11B9/02Recovery or refining of essential oils from raw materials
    • C11B9/027Recovery of volatiles by distillation or stripping

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  • 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

Flower method of extraction of essential oil
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 %.
CN201710503908.8A 2017-06-27 2017-06-27 Flower essential oil extraction method Expired - Fee Related CN109135927B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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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CN105950293A (en) * 2016-05-28 2016-09-21 黄宇松 Extraction method of jasmine essential oil

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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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