CN108219945A - A kind of fresh flower crystal oil and more odor types flower crystal's oil - Google Patents
A kind of fresh flower crystal oil and more odor types flower crystal's oil Download PDFInfo
- Publication number
- CN108219945A CN108219945A CN201810210971.7A CN201810210971A CN108219945A CN 108219945 A CN108219945 A CN 108219945A CN 201810210971 A CN201810210971 A CN 201810210971A CN 108219945 A CN108219945 A CN 108219945A
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- Prior art keywords
- oil
- crystal
- fresh flower
- peony
- column
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- UYLTVQNKRAHSFG-UHFFFAOYSA-N 4,4-dibromobutoxybenzene Chemical compound BrC(Br)CCCOc1ccccc1 UYLTVQNKRAHSFG-UHFFFAOYSA-N 0.000 description 1
- 229910015900 BF3 Inorganic materials 0.000 description 1
- 241000193830 Bacillus <bacterium> Species 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 241000167854 Bourreria succulenta Species 0.000 description 1
- 108010059892 Cellulase Proteins 0.000 description 1
- JOZKFWLRHCDGJA-LLVKDONJSA-N Citronellyl acetate Natural products CC(=O)OCC[C@H](C)CCC=C(C)C JOZKFWLRHCDGJA-LLVKDONJSA-N 0.000 description 1
- 241000207199 Citrus Species 0.000 description 1
- 235000005979 Citrus limon Nutrition 0.000 description 1
- 244000131522 Citrus pyriformis Species 0.000 description 1
- 206010011224 Cough Diseases 0.000 description 1
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 1
- 241000255925 Diptera Species 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 241000628997 Flos Species 0.000 description 1
- 239000008868 Flower Essence Substances 0.000 description 1
- 240000005819 Magnolia denudata Species 0.000 description 1
- 235000016094 Magnolia denudata Nutrition 0.000 description 1
- 241000218394 Magnolia liliiflora Species 0.000 description 1
- 244000262613 Michelia alba Species 0.000 description 1
- 235000003415 Michelia alba Nutrition 0.000 description 1
- 241001093501 Rutaceae Species 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 244000228451 Stevia rebaudiana Species 0.000 description 1
- 235000006092 Stevia rebaudiana Nutrition 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- VYBREYKSZAROCT-UHFFFAOYSA-N alpha-myrcene Natural products CC(=C)CCCC(=C)C=C VYBREYKSZAROCT-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 230000003035 anti-peroxidant effect Effects 0.000 description 1
- 230000003260 anti-sepsis Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 229940106157 cellulase Drugs 0.000 description 1
- 235000019693 cherries Nutrition 0.000 description 1
- 235000020971 citrus fruits Nutrition 0.000 description 1
- 238000004440 column chromatography Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000004332 deodorization Methods 0.000 description 1
- 230000001877 deodorizing effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229940088598 enzyme Drugs 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 235000013355 food flavoring agent Nutrition 0.000 description 1
- 239000005452 food preservative Substances 0.000 description 1
- 235000019249 food preservative Nutrition 0.000 description 1
- 235000013376 functional food Nutrition 0.000 description 1
- 150000002240 furans Chemical class 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 235000009569 green tea Nutrition 0.000 description 1
- JHEPBQHNVNUAFL-UHFFFAOYSA-N hex-1-en-1-ol Chemical class CCCCC=CO JHEPBQHNVNUAFL-UHFFFAOYSA-N 0.000 description 1
- UFLHIIWVXFIJGU-UHFFFAOYSA-N hex-3-en-1-ol Chemical class CCC=CCCO UFLHIIWVXFIJGU-UHFFFAOYSA-N 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 210000004072 lung Anatomy 0.000 description 1
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 1
- DEDOPGXGGQYYMW-UHFFFAOYSA-N molinate Chemical compound CCSC(=O)N1CCCCCC1 DEDOPGXGGQYYMW-UHFFFAOYSA-N 0.000 description 1
- JXTPJDDICSTXJX-UHFFFAOYSA-N n-Triacontane Natural products CCCCCCCCCCCCCCCCCCCCCCCCCCCCCC JXTPJDDICSTXJX-UHFFFAOYSA-N 0.000 description 1
- 239000012044 organic layer Substances 0.000 description 1
- 229920002866 paraformaldehyde Polymers 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 239000011297 pine tar Substances 0.000 description 1
- 229940068124 pine tar Drugs 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 235000015497 potassium bicarbonate Nutrition 0.000 description 1
- 229910000028 potassium bicarbonate Inorganic materials 0.000 description 1
- 239000011736 potassium bicarbonate Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000012552 review Methods 0.000 description 1
- 229930007790 rose oxide Natural products 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 239000012047 saturated solution Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 210000000697 sensory organ Anatomy 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 238000004230 steam cracking Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 238000000194 supercritical-fluid extraction Methods 0.000 description 1
- 238000004809 thin layer chromatography Methods 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
- 230000003519 ventilatory effect Effects 0.000 description 1
- 239000003039 volatile agent Substances 0.000 description 1
- 230000002087 whitening 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
- C11B9/0003—Compounds of unspecified constitution defined by the chemical reaction for their preparation
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Fats And Perfumes (AREA)
Abstract
The present invention relates to a kind of fresh flower crystal oil and more odor types flower crystal's oil.Fresh flower crystal's oil is to mix fresh flower aqua aromatica and column arene derivatives, then adds in organic solvent and is extracted, separation organic phase, remove the organic solvent in organic phase to get；The column arene derivatives are at least one of full trimethylammonium propyl column [6] aromatic hydrocarbons of hydrobromic acid, full trimethylammoniumethyl column [6] aromatic hydrocarbons, full trimethylammonium butyl column [6] aromatic hydrocarbons.The fresh flower crystal oil of the present invention, column arene derivatives are applied in the extraction process of fresh flower aqua aromatica, efficiency of the column arene derivatives in addition to extraction process can be improved, the soluble fine ingredient in fresh flower aqua aromatica can also be promoted to be transferred to organic phase, improve the extraction rate of transform of such functional component, thus can be effectively to solve the problems, such as that the soluble fines such as terpene alcohol, aromatic alcohol ingredient can not be carried out enrichment transfer in a manner of traditional liquid-liquid extraction.
Description
Technical field
The invention belongs to plants essential oils and essence and flavoring agent field, and in particular to a kind of fresh flower crystal oil and more odor types flower crystal
Oil.
Background technology
Essential oil (Essential oil) be from fragrant plant with the methods of steam distillation extract gained oily liquids,
Not only there is preferable organoleptic quality, it is more that there is antibacterial anti-inflammatory, cough-relieving apophlegmatic, antipyretic-antalgic etc., it is widely used in fragrance
The fields such as essence, pharmacy and aromatotherapy.It is emphasized that for most fragrant plants, only distilled with water,
Steam distillation, water-steam distillation or cracking process extraction products therefrom could be referred to as essential oil, and (Rutaceae is citrous
Except fruit or pericarp, essential oils are produced using cold-press method) (Rubiolo P, Sgorbini B, Liberto E, et
al.Essential oils and volatiles:sample preparation and analysis.A review[J]
.Flavour and Fragrance Journal,2010,25(5):282-290)。
By taking peony essential oil as an example, occurs the extracting method of a variety of peony essential oils at present.
The patent application of Publication No. CN104277915A discloses a kind of method that peony essential oil is extracted from peony,
It is that fresh flower is dry and adds in cellulase processing, then be obtained by extraction under high pressure with petroleum ether；Publication No.
The patent application of CN104789359A disclose it is a kind of from peony extract essential oil method, use petroleum ether and ethyl alcohol into
Row grading extraction, then it is concentrated and prepare.Such method is mostly extracted using organic solvent, and products therefrom actually should be medicinal extract
(Concrete) rather than proper essential oil.In the medicinal extract of gained, often containing a large amount of alkane, alkene constituents, this
A little ingredients are to the contribution very little of fragrance or fragrance, also without bioactivity.
The patent application of Publication No. CN103305344A discloses a kind of side that peony essential oil is extracted from fresh peony flower
Method is to be extracted after obtaining medicinal extract using supercritical carbon dioxide, then be refining to obtain with molecularly distilled；Publication No.
The patent application of CN106190587A discloses a kind of extracting method of peony essential oil, is using supercritical carbon dioxide and specific
Agent is carried to extract.Such method polyphyly is using the post-processing approach such as means of supercritical extraction and binding molecule distillation, products therefrom
Actually " absolute oil " (Absolute oil).Its feature is, often containing more terpenes constituents, terpenes constituents be easy to oxidation,
Hydrolysis is the arch-criminal for causing to go bad between essential oil class product shelf life.
Conventional fragrant plants essential oil is the distillate for collecting distillation process, oil phase is then demultiplex out to obtain the final product；It such as can be in
State's pharmacopeia determination of volatile oil method collects the oil reservoir in extractor, you can the volatile oil of corresponding fragrant plant is made.
Fresh flower aqua aromatica, also known as hydrosol, be part derived essential oil is soluble in the aqueous phase and is formed in distillation process saturation or
Near saturated solution has excellent organoleptic quality and higher value medical health care.
Publication No. is that the patent application of CN105820880A discloses a kind of preparation method of fresh peony flower water, is to utilize
Subcritical abstraction device to fresh peony flower stoste carry out liquid-liquid extraction, while obtain the tree peony flower concrete containing derived essential oil and
Fresh peony flower water, the raffinate after the practical extraction for organic solvents such as butane, propane of the fresh peony flower water.Publication No.
The patent application of CN104087424A discloses a kind of step extraction, the method for detaching fresh peony flower essential oil, aqueous solution, lipid,
It is to extract the organic solvents such as fresh peony flower methyl ether, butane, propane, and after negative pressure concentrates, collect condensate liquid is raffinate
For peony aqueous solution.Peony aqueous solution prepared by such method is raffinate of the fresh flower after extraction, due to major part
Derived essential oil has been extracted totally, the only remaining derived essential oil not being extracted on a small quantity in raffinate, and has dissolvent residual, this kind
The quality of fresh peony flower water is limited, and utility value is little.
Notification number is that the patent of CN103142431B discloses a kind of tree peony hydrolat (i.e. aqua aromatica), is by tree peony piebald
After marinated, water is added to distill, collects the petal extracting solution of distillate, as tree peony, then with the root skin extracting solution of tree peony according to
Certain volume ratio mixes.
The bulky of fresh flower aqua aromatica, storage and transportation is inconvenient, is easy to corruption, simultaneously because the limitation of solubility, contained essential oil
Constituent concentration is very low (usually less than 500ppm), and such as without enrichment concentration, added value is relatively low, and application scenario also can be by
To larger limitation.
The conventional method for preparing crystal's oil by the enriched concentration of fresh flower aqua aromatica is to extract fresh flower aqua aromatica organic solvent
After taking, extract liquor recycling organic solvent obtains crystal's oil product, and the patent application if publication No. is CN104224633A is i.e. open
Prepare the Rose Absolute using peony and tasselled flowers as raw material in this way.The defects of this method, which is to use, to be had
Soluble fine ingredient (such as terpene alcohol, aromatic alcohol, ether, phenols oxygenatedchemicals) can not effectively be transferred to organic by solvent extraction
Xiang Zhong, it is final so as to which this kind of soluble fine ingredient being affected to organoleptic quality and bioactivity be caused to cannot be introduced into
In crystal's oil product, lead to that main odor type component damages are serious, and the quality of crystal's oil product is also a greater impact.
Invention content
The purpose of the present invention is to provide a kind of fresh flower crystal oil, so as to solve the enrichment concentration side of existing fresh flower aqua aromatica
The effectively enrichment of the soluble fines such as terpene alcohol, aromatic alcohol ingredient can not be concentrated into the problems in crystal's oil by method.The present invention also provides
More odor types flower crystal's oil based on above-mentioned fresh flower crystal oil.
To achieve the above object, the technical solution adopted in the present invention is：
A kind of fresh flower crystal oil, is prepared by method comprising the following steps：Fresh flower aqua aromatica and column aromatic hydrocarbons are derived
Object mix, then add in organic solvent extracted, separation organic phase, remove organic phase in organic solvent to get；The column
Arene derivatives are full trimethylammonium propyl column [6] aromatic hydrocarbons of hydrobromic acid, full trimethylammoniumethyl column [6] aromatic hydrocarbons, full trimethylammonium butyl column
[6] at least one of aromatic hydrocarbons.
The fresh flower crystal oil of the present invention, column arene derivatives is applied in the extraction process of fresh flower aqua aromatica, column virtue
Efficiency of the hydrocarbon derivative in addition to that can improve extraction process can also promote the soluble fine ingredient in fresh flower aqua aromatica to shift
To organic phase, the extraction rate of transform of such functional component is improved, thus can be effectively to solve in a manner of traditional liquid-liquid extraction to terpene
The soluble fines such as alcohol, aromatic alcohol ingredient can not carry out the problem of enrichment transfer.Extraction experiment proves, relative to conventional liquid-
Liquid extracts mode, and this method can significantly improve crystal's oil yield, the purpose of General Promotion crystal's oil quality.
The structural formula of full trimethylammonium propyl column [6] aromatic hydrocarbons of hydrobromic acid is：
Full trimethylammonium propyl column [6] aromatic hydrocarbons of hydrobromic acid is prepared as the prior art, and following steps specifically can be used：
1) 8.0g is taken to be placed in there-necked flask dibromo propoxy benzene, 1.0g paraformaldehydes, 200mL dichloromethane, in room temperature
2.5mL boron trifluoride ether is added with stirring, reacts 3h in a nitrogen atmosphere, 45mL saturated potassium hydrogen carbonates is added in and reaction is quenched,
Continue to stir 30min.Organic layer is poured out, the potassium bicarbonate solution of use quality a concentration of 5% is washed to neutrality, with deionized water
It washes 3 times, is dried over anhydrous sodium sulfate, filters, gained filtrate obtains solids through being concentrated under reduced pressure, being dried in vacuo.By solids into
Row column chromatography for separation fills column with the silica gel of 200-300 mesh, and using petroleum ether, dichloromethane, (volume ratio is 5：(2-3)) it is molten to elute
Agent, thin-layer chromatography detect and merge identical fraction, recycling design, and flaxen perbromo- propoxyl group column [6] aromatic hydrocarbons powder is made.
2) 2.8g perbromo- propoxyl group column [6] aromatic hydrocarbons, 100mL ethyl alcohol is taken to be placed in three-necked flask, room temperature stirs under nitrogen atmosphere
10min is mixed, adds in 20mL trimethylamines, oil bath heating is stirred at reflux 15h under nitrogen atmosphere to 80 DEG C.Reaction solution is poured out, decompression is dense
Contracting, vacuum drying, obtain off-white powder, add 15 times of amount deionized water dissolvings, filterings, collect filtrate, add in ethanol in proper amount, decompression
Remove solvent, vacuum drying.Obtained solid object adds 20 times of calorimetric ethyl alcohol dissolvings, and refrigerated overnight filters to obtain off-white powder, vacuum
Drying is to get full trimethylammonium propyl column [6] aromatic hydrocarbons of hydrobromic acid.
The structure of full trimethylammoniumethyl column [6] aromatic hydrocarbons of hydrobromic acid：
It synthesizes the synthesis similar to full trimethylammonium propyl column [6] aromatic hydrocarbons of hydrobromic acid, only by the raw material " 8.0g in step 1)
To dibromo propoxy benzene " " 7.5g is to dibromo ethoxybenzene " is changed to, by " 2.8g perbromo- propoxyl group columns [6] virtue in step 2)
Hydrocarbon " is changed to " 2.4g perbromo- ethoxy pilum [6] aromatic hydrocarbons ".
The structure of full trimethylammonium butyl column [6] aromatic hydrocarbons of hydrobromic acid：
It synthesizes the synthesis for being similar to its synthesis similar to full trimethylammonium propyl column [6] aromatic hydrocarbons of hydrobromic acid, only by step 1)
In raw material " 8.0g is to dibromo propoxy benzene " be changed to " 8.6g is to dibromo butyl phenyl ether ", by " the 2.8g perbromo-s in step 2)
Propoxyl group column [6] aromatic hydrocarbons " is changed to " 3.4g perbromo- butoxy column [6] aromatic hydrocarbons ".
More introduce of this kind of column arene derivatives may refer to journal article：Ma Y,Yang J,Li J,et al.A
cationic water-soluble pillar[6]arene:synthesis,host–guest properties,and
self-assembly with amphiphilic guests in water[J].RSC Advances,2013,3(46):
23953-23956.
The quality of the column arene derivatives is the 1-3% of fresh flower fragrance water quality.Under the additive amount, you can to fresh flower
Soluble fine ingredient in aqua aromatica carries out effective extraction transfer, and not only dosage is few, but also can ensure obtained fresh
The quality of flower crystal's oil.For full trimethylammonium propyl column [6] aromatic hydrocarbons of hydrobromic acid to add in 2% amount of aqua aromatica, compared to not making
With column aromatic hydrocarbons, extraction yield can be improved to 2-5 times, and organic solvent consumption can be reduced to 1/3-1/6.
Organic solvent does not have particular/special requirement used in extraction process, can realize the requirement of extraction.From organic molten
The safety of agent and economy are set out, it is preferred that the mixed solvent that the organic solvent is dichloromethane, ethyl acetate forms.
It is further preferred that the volume ratio of dichloromethane, ethyl acetate is (10-20)：1.
From raising extraction efficiency aspect, the volume ratio of organic solvent and fresh flower aqua aromatica is 1：(10-20).Extraction
After 2-3 times, combining extraction liquid, then through being dehydrated, removing organic solvent, you can obtain fresh flower crystal oil.Anhydrous sulphur may be selected in dehydration
Sour sodium, addition can be the 2-5%, dewatering time 30-90min of aqua aromatica quality.Conventional vacuum distillation mode can be used
Remove organic solvent, control vacuum degree be 0.060-0.095MPa, 35-45 DEG C of heating temperature.
Fresh flower aqua aromatica raw material can be utilized and existing fresh flower aqua aromatica or be prepared according to the prior art, such as can be according to
The method of patent involved by background of invention part prepares fresh flower aqua aromatica (hydrosol).
To further improve the quality of fresh flower aqua aromatica, so as to improve the quality of crystal's oil, the present invention additionally provides one kind
The preparation scheme of fresh flower aqua aromatica.Preferably, the fresh flower aqua aromatica is made by method comprising the following steps：Using complex salt
Solution impregnates fresh flower, and water distillation collects distillate to obtain the final product；The mass percentage of the composite compaction technique forms：NaCl 8-
12%, Na2SO4·10H2O or MgSO4·7H2O 2-6%, KAl (SO4)2·12H2O or NaAl (SO4)2·12H2O 1-3%,
Solvent is water.
The fresh flower aqua aromatica prepared using the preferred embodiment carries out immersion treatment, with biography using composite compaction technique to fresh flower
System pickling treatment is compared, and can be remarkably promoted soluble fine ingredient and is precipitated inside Petal to the circular water phase body of surrounding
System promotes mass transfer of the such components in distillation process, with extraction rate is fast, extraction content is high, soluble fine ingredient kind
The characteristics of class is more.Experiments have shown that compared to comparable sodium NaCl solution is used to pickle, soaking time can foreshorten to 0.5 by 3-5d-
2hr, soluble fine content can be improved to 3-5 times.
The quality of the composite compaction technique is 1-2 times of fresh flower quality.The time of the immersion is 0.5-2h.Preferably,
When water distills, quantity of distillate hourly is 0.3-0.5 times of fresh flower quality, distillation time 0.5-2h.Joined using above-mentioned distillation
Number under the premise of higher extracted rate, can obtain the fresh flower aqua aromatica of excellent combination property.
Said extracted method is applicable to the extraction of different phytovolatilization oil content fresh flowers, such as rose, tree peony, Chinese rose, cherry
Flower, sweet osmanthus, yulan, cloves etc..
Preferably, the fresh flower is at least one of peony, rose, Chinese rose, oriental cherry, sweet osmanthus.It is further preferred that
The kind of the peony is at least one in Corallium Japonicum Kishinouye platform, WULONGPENGSHANG, Bai Xueta, beautiful ball, Hu Hong, phoenix pellet powder, the red basket of phoenix
Kind.
For the fresh flower kind of low volatile oil content, such as rose, Chinese rose, oriental cherry, tree peony, distillate is only containing a small amount of oil
The oil phases such as drop, liquid film, content can be neglected relative to water phase, can be carried out according to actual conditions or without a point oil behaviour
Make, so as to obtain corresponding fresh flower aqua aromatica.
Higher is contained for the fresh flower kind of high volatile oil content, such as cloves, Flos micheliae Albae, purple yu-lan (Magnolia liliflora), sweet osmanthus, distillate
The oil reservoir of content, the oil reservoir contain a large amount of terpenes, alkane, alkene etc. to organoleptic quality and bioactivity contribution it is smaller it is miscellaneous into
Point, after standing, removing oil phase processing, it can obtain quality more preferably fresh flower aqua aromatica.
Using above-mentioned fresh flower aqua aromatica, relatively existing hydrosol product, the content higher of soluble fine ingredient, thus
Value in terms of organoleptic quality and health care is more prominent.
The fresh flower crystal oil prepared using the fresh flower aqua aromatica of the preferred embodiment, chemistry spectrum are significantly better than common fresh flower essence
Oil, fresh flower crystal's oil almost all are made of oxygenatedchemicals, particularly the sense organs such as aromatic alcohol, monoterpene alcohols, C6 alcohols
Quality height and the significant ingredient of bioactivity, these ingredients are enriched with dense as the soluble fine ingredient in fresh flower aqua aromatica
Contracting.And common ethereal oil of flower, the oil reservoir that distillate is isolated mainly is derived from, wherein to organoleptic quality and bioactivity without contribution
Alkane and alkene constituents occupy main component, and there were significant differences for quality and added value nature.
By taking peony as an example, using peony crystal oil made from the above method, stability and storge quality are significantly better than
Traditional peony essential oil.It is mainly reflected in, without terpenes constituents.The easy oxydrolysis of terpenes constituents, is to cause
The arch-criminal that essential oil quality reduces.Common peony essential oil contains a large amount of terpenes constituents, if without de- terpene processing, Storage period
Between easily occur oxydrolysis reaction, quality is caused to reduce.And the present invention obtain peony crystal oil, without terpenes into
Point, without de- terpene, stability is good, can store for a long time.
Further, the peony of different cultivars is selected, is prepared using the method for above-mentioned fresh flower crystal oil, it can be corresponding
Different types of crystal's oil is obtained, the main component of these crystals oil is different, can provide different odor types and bioactivity.Such as
The variety selection Corallium Japonicum Kishinouye platform of peony can accordingly obtain Corallium Japonicum Kishinouye platform tree peony crystal oil；The peony of other kinds and corresponding water
The name of essential oil is similar.
Specifically, the main component of Corallium Japonicum Kishinouye platform tree peony crystal oil is：1,3,5- trimethoxy-benzenes 66.5%, benzyl carbinol
27.6%th, citronellol 1.8% etc.；
The main component of WULONGPENGSHANG tree peony crystal's oil is：Benzyl carbinol 63.6%, linalool oxide (furan type) 9.8%,
Cis- 3- hexenols 7.4%, geraniol 6.6%, linalool 3.0%, nerol 2.0%, hexanol 1.8%, benzyl alcohol 1.2%, nonyl
Aldehyde 1.1% etc.；
The main component of Bai Xueta tree peonies crystal's oil is：Citronellol 46.7%, geraniol 13.6%, cis- 3- hexenols
9.4%th, 1,3,5- trimethoxy-benzenes 7.5%, hexanol 7.3%, geranic acid 7.0%, linalool 2.8%, linalool oxide (furans
Type) 2.0%, cis-rose oxide 1.2%, alpha-terpineol 1.3% etc.；
The main component of beautiful ball tree peony crystal oil is：Cis- 3- hexenols 21.5%, benzyl carbinol 16.3%, 1,4- diformazans
Oxygroup benzene 17.4%, hexanol 8.7%, linalool 8.3%, geraniol 8.0%, linalool oxide (furan type) 3.5%, 1- benzene second
Alcohol 3.3%, 4,7- dimethyl benzofurans 2.4%, nerol 2.1%, alpha-terpineol 1.9%, benzyl alcohol 1.0% etc.；
The main component of Hu red peony crystal's oil is：1,3,5- trimethoxy-benzenes 21.9%, geraniol 20.4%, nerol
15.0%th, linalool oxide (furan type) 10.3%, cis- 3- hexenols 8.5%, hexanol 3.9%, geranic acid 3.5%, α-pine tar
Alcohol 2.7%, furtural 2.4%, 6- methyl -5- heptene -2- alcohol 1.0%, enanthaldehyde 1.0% etc.；
The main component of phoenix pellet pink peony crystal's oil is：Benzyl alcohol 18.8%, 5- hydroxyl -2- decylenic acid delta-lactones
14.7%th, 1,4- dimethoxy benzenes 9.5%, furfural 8.4%, benzaldehyde 6.8%, linalool 5.9%, alpha-terpineol 4.3%, orange
Flower alcohol 4.0%, geraniol 3.7%, 1,2- dimethoxy benzenes 3.0%, linalool oxide (furan type) 2.8%, to terpane -1-
Alcohol 2.6%, geranyl acetone 2.3%, 1,2,4- trimethoxy-benzenes 2.0%, Ergol 1.8% etc.；
The main component of the red blue tree peony crystal's oil of phoenix is：Linalool oxide (furan type) 21.6%, cinnamyl alcohol 19.7%, 1,
3,5- trimethoxy-benzenes 18.5%, geraniol 12.4%, linalool 9.8%, nerol 9.0% etc..
Ingredient contained by crystal's oil of these types, including listed main component (single component content >=1.0%) and
Unlisted micro constitutent (<1.0%) it is, that larger oxygenatedchemicals is contributed to organoleptic quality and bioactivity, without alkane
Hydrocarbon, alkene etc. are to the ingredient of organoleptic quality and bioactivity without contribution, also without the terpenes for having negative effect to essential oil stability
Constituents, thus with splendid quality and value.
In addition, above-mentioned different types of peony crystal oil assigns flower crystal's oil with soft, strong fragrant with more preferably chemistry spectrum
Natural tree peony fragrance breath, while have certain anti-corrosive fresh-keeping, antibacterial, mite killing, mosquito repellent, local analgesia, improve lung
Ventilatory function and reduction airway resistance, the calmness and pressure that minds at rest, the function of removing free radical, inhibit melanin generation, because
And available for fields such as food additives, superior cosmetics, aromatotherapies.
The odor type and bioactivity of the main component of above-mentioned crystal oil are briefly described below.
In aromatic alcohol substance, benzyl carbinol has Rose Essentielle breath, while has antibacterial and antisepsis.Benzyl alcohol has
There is sweet fruit aroma, can also be used as preservative, the fixastive of essence, external application then has local analgesia effect；Cinnamyl alcohol has
The fragrant and sweet gas of similar hyacinthine cream, fragrance is quiet and tastefully laid out mild lasting, can be used as fixastive, while have the works such as sterilization, fresh-keeping, deodorization
With.
In monoterpene alcohols ingredient, citronellol has quiet and tastefully laid out rose fragrance, can inhibit golden yellow grape and typhoid bacillus etc.
Pathogenic bacteria；Geraniol have rose fragrance, have antibacterial and mosquito repellent effect, while can improve pulmonary ventilation function with
Airway resistance is reduced, accelerates the recovery from illness of chronic bronchitis；Nerol has the fragrant and sweet breath of approximate fresh rose, while slightly has
Citrus and lemon breath；Linalool has the Radix Aucklandiae of dense sweet tea, and the green fragrance for having green tea ceases, and has the works such as antibacterial, mite killing, calmness
With；Linalool oxide (furan type) has strong Radix Aucklandiae and the fragrance of a flower.
In methoxybenzene constituents, the glycol of 1,3,5- trimethoxy-benzene and Isosorbide-5-Nitrae-dimethoxy benzene with fermentation after-ripening tea
Agalloch eaglewood, while there is calmness and the pressure that minds at rest.
In C6 alcohol compounds, cis- 3- hexenols have strong fresh leafiness fragrance, can assign essential oil and naturally feel；Hexanol
Fragrant breath with similar fruit.
In aldehydes ingredient, furfural has the function of anti peroxidation of lipid and removes free radical, and benzaldehyde, which has, inhibits junket ammonia
Sour enzyme activity blocks melanin generation and the effect of skin whitening.
On the basis of above-mentioned fresh flower crystal oil, at least two fresh flower crystal's oil are mixed, can obtain more odor type flowers
Crystal's oil.
Specifically, it is male to be selected from Corallium Japonicum Kishinouye platform tree peony, WULONGPENGSHANG tree peony, Bai Xueta tree peonies, beautiful ball tree peony, Hu Hong for fresh flower
The red blue tree peony of pellet, phoenix pellet pink peony, phoenix, it is male accordingly to obtain Corallium Japonicum Kishinouye platform tree peony crystal oil, WULONGPENGSHANG tree peony crystal oil, Bai Xueta
The red blue tree peony crystal oil of red crystal's oil, beautiful ball tree peony crystal oil, Hu red peony crystal oil, phoenix pellet pink peony crystal oil, phoenix, will
At least two kinds of crystal's oil mixing therein are to get more odor types flower crystal's oil.
After crystal's oil of different cultivars is mixed, vibrating 5-15min at room temperature makes it reconcile uniformly to get more odor types flower water
Essential oil, it is not corrupt that long-term preservation can be achieved in this more fragrant water essential oils under sealing, cold storage environment.
The present invention only provides 6 kinds of natural peony crystal oil with special odor type, respectively soft floral type, pure and fresh flower
Leaf odor type, glycol jasmine tea odor type, green sweet tea flowers and fruits odor type, balance tree peony odor type I and balance tree peony odor type II.Other odor types and biology
Crystal's oil of living features can be allocated according to actual demand.
By WULONGPENGSHANG tree peony crystal oil and Bai Xueta tree peony crystals oil in mass ratio (1-25)：5 mixing, obtain soft flower
Odor type peony crystal oil.
By the red blue tree peony crystal oil of Corallium Japonicum Kishinouye platform tree peony crystal oil and phoenix in mass ratio (1-8)：2 mixing, obtain glycol jasmine tea
Odor type peony crystal oil.
By beautiful ball tree peony crystal oil and Hu red peony crystal oil in mass ratio (2-6)：1 mixing, it is fragrant to obtain pure and fresh floral leaf
Type peony crystal oil.
By phoenix pellet pink peony crystal oil, the red blue tree peony crystal oil of phoenix, Hu red peony crystal oil in mass ratio (5-6)：(3-
4)：1 mixing obtains green sweet tea flowers and fruits odor type peony crystal oil.
By WULONGPENGSHANG tree peony crystal oil, Corallium Japonicum Kishinouye platform tree peony crystal oil, beautiful ball tree peony crystal oil, the red blue tree peony crystal of phoenix
Oil is in mass ratio (1-3)：(2-4)：(2-4)：(1-3) is mixed, and is balanced tree peony odor type I crystals oil.
Bai Xueta tree peonies crystal oil, Corallium Japonicum Kishinouye platform tree peony crystal oil, Hu red peony crystal oil, phoenix pellet pink peony crystal's oil are pressed
Mass ratio (2-4)：(1-4)：(1-3)：(1-4) is mixed, and is balanced tree peony odor type II crystals oil.
The above-mentioned natural peony crystal oil of more odor types, chemistry spectrum, stability and storge quality are significantly better than common male
Red essential oil, application range are significantly widened, and have higher added value, available for food additives, superior cosmetics, champignon
In the numerous areas such as treatment.
The present invention also provides a kind of fresh flower aqua aromatica or fresh flower crystal's oil extract complex salt and composite compaction techniques.
The complex salt is made of the component of following parts by weight：8-12 parts of NaCl, Na2SO4·10H2O or MgSO4·7H2O
2-6 parts, KAl (SO4)2·12H2O or NaAl (SO4)2·12H21-3 parts of O.
The composite compaction technique is dissolved in water, you can be prepared molten for fresh flower aqua aromatica or crystal's oil extract complex salt
Liquid.The mass percentage of the composite compaction technique forms：NaCl 8-12%, Na2SO4·10H2O or MgSO4·7H2O 2-
6%, KAl (SO4)2·12H2O or NaAl (SO4)2·12H2O 1-3%, solvent are water.
The mechanism of action of the composite compaction technique is that soluble fine ingredient is promoted to be precipitated inside Petal to ring around
Around aqueous phase system, promote mass transfer of the such components in distillation process.The composite compaction technique can improve water-soluble essence in fresh flower
The extraction of oil component so as to improve the content of the constituents in fresh flower crystal's oil, improves the quality and valency of crystal's oil product
Value.
On the extraction exemplary basis for providing peony in the present invention, the fresh flowers such as rose, Chinese rose, oriental cherry, sweet osmanthus can be carried out
Similar distillation extraction process prepares fresh flower hydrosol or fresh flower aqua aromatica, can further be carried out by the exemplary method of the present invention
Concentration is enriched with, prepares corresponding crystal's oil product.
Description of the drawings
Fig. 1 is the exemplary fragrance component content figure of the different flavor crystal oil of embodiment 8-10；
Fig. 2 is the comparison diagram using crystal's oil yield obtained by complex salt pretreatment and sodium chloride pretreatment distillation flower water；
Fig. 3 is that comparative example 2 and the method for embodiment 1 prepare the extraction yield of crystal's oil and the comparison of organic solvent consumption
Figure, wherein (a) is extraction yield, (b) is organic solvent consumption；
Fig. 4 is the beautiful ball tree peony crystal oil of embodiment 2 and the beautiful ball peony essential oil exemplary fragrance ingredient of comparative example 3
Content balance figure.
Specific embodiment
Embodiments of the present invention are described further with reference to specific embodiment.
Embodiment 1
The present embodiment selects fresh flower kind as Bai Xueta tree peonies, corresponding to prepare Bai Xueta tree peonies aqua aromatica and Bai Xueta tree peonies
Crystal's oil.
Bai Xueta tree peonies aqua aromatica is prepared using following steps：Bai Xueta fresh peony flowers are taken, add in 1.5 mass times
Composite compaction technique, soaking at room temperature 1.5h, water distillation distillate the 0.4 times/h that speed is fresh flower quality, distill 2h, collect distillate,
It filters up to Bai Xueta tree peony aqua aromaticas.The mass content of composite compaction technique forms：NaCl 10%, Na2SO4·10H2O
3%, KAl (SO4)2·12H2O 2%, solvent are water.
Bai Xueta tree peony crystal oil is prepared using following steps：Quality is added in into Bai Xueta tree peony aqua aromaticas as virtue
Full trimethylammonium propyl column [6] aromatic hydrocarbons of hydrobromic acid of perfume quality 2%, is stirred to dissolve, and volume is pressed with dichloromethane, ethyl acetate
Than 15:1 composition mixed solvent extracted, each dosage be Bai Xueta tree peony fragrance water volumes 1/10, coextraction 2 times,
Combining extraction liquid adds in quality and is dehydrated 50min, filtering, filtrate for 5% anhydrous sodium sulfate of Bai Xueta tree peony fragrance water qualities
Through be concentrated under reduced pressure (vacuum degree 0.090MPa, 35 DEG C of heating temperature) to mixed solvent recycling finish to get.
Gained Bai Xueta peonies crystal oil, is detected, main component is through GC-MS：Citronellol 46.7%, geraniol
13.6%th, cis- 3- hexenols 9.4%, 1,3,5- trimethoxy-benzenes 7.5%, hexanol 7.3%, geranic acid 7.0%, linalool
2.8%th, linalool oxide (furan type) 2.0%, cis-rose oxide 1.2%, alpha-terpineol 1.3%, 1- benzyl carbinols 0.6%, anti-
Formula rose oxide 0.3%, citronellyl acetate 0.3%.The all oxygenatedchemicals of its ingredient, particularly aromatic alcohol, monoterpene alcohol, methoxy
The excellent ingredient significant with bioactivity of the organoleptic qualities such as base benzene, C6 alcohol；Without to organoleptic quality and bioactivity without contribution
Alkane and alkene；Without terpenes constituents, stability is good, can store for a long time.
The unique chemical composition of gained Bai Xueta peonies crystal oil, assigns its quiet and tastefully laid out fragrance of a flower and fresh and sweet leaf is fragrant, together
When there is antibacterial, mosquito repellent, promote the fully recovering of chronic bronchitis, the calm and pressure that minds at rest.Therefore it is available
In the multiple fields such as superior cosmetics and champignon therapy.
Embodiment 2
The present embodiment prepares beautiful ball tree peony aqua aromatica and beautiful ball tree peony crystal oil.
Beautiful ball tree peony aqua aromatica is prepared using following steps：Beautiful ball fresh peony flower is taken, adds in answering for 2 mass times
Salting liquid, soaking at room temperature 0.5h are closed, water distillation distillates the 0.4 times/h that speed is fresh flower quality, distills 1h, collects distillate, mistake
It filters up to beautiful ball tree peony aqua aromatica.The mass content of composite compaction technique forms：NaCl 12%, Na2SO4·10H2O 5%,
KAl(SO4)2·12H2O 3%, solvent are water.
Beautiful ball tree peony crystal oil is prepared using following steps：Quality is added in into beautiful ball tree peony aqua aromatica as virtue
Full trimethylammonium propyl column [6] aromatic hydrocarbons of hydrobromic acid of perfume quality 1%, is stirred to dissolve, and volume is pressed with dichloromethane, ethyl acetate
Than 20:1 composition mixed solvent extracted, each dosage be beautiful ball tree peony fragrance water volume 1/20, coextraction 3 times,
Combining extraction liquid adds in quality and is dehydrated 90min, filtering, filtrate for 2% anhydrous sodium sulfate of beautiful ball tree peony fragrance water quality
Through be concentrated under reduced pressure (vacuum degree 0.080MPa, 40 DEG C of heating temperature) to mixed solvent recycling finish to get.
The main component of the beautiful ball tree peony crystal oil of gained is：Cis- 3- hexenols 21.5%, benzyl carbinol 16.3%, 1,4-
Dimethoxy benzene 17.4%, hexanol 8.7%, linalool 8.3%, geraniol 8.0%, linalool oxide (furan type) 3.5%, 1-
Benzyl carbinol 3.3%, 4,7- dimethyl benzofurans 2.4%, nerol 2.1%, alpha-terpineol 1.9%, benzyl alcohol 1.0% etc..
Beautiful ball peony crystal oil has the agalloch eaglewood of fragrant, the soft glycol of pure and fresh leaf, while has Antimicrobial preservative, calmness
With the pressure that minds at rest, mite killing, the effect for improving pulmonary ventilation function and reduction airway resistance.Therefore available for food flavor, medicine
It applies some make up and the multiple fields such as aromatotherapy.
Embodiment 3
The present embodiment prepares Corallium Japonicum Kishinouye platform tree peony aqua aromatica and Corallium Japonicum Kishinouye platform tree peony crystal oil.
The preparation of Corallium Japonicum Kishinouye platform tree peony aqua aromatica can refer to embodiment 1, differ only in：The mass content group of composite compaction technique
Become：NaCl 8%, Na2SO4·10H2O 2%, KAl (SO4)2·12H2O 1%, solvent are water；The addition of composite compaction technique
Measure 1 times for fresh flower quality.
The preparation of Corallium Japonicum Kishinouye platform tree peony crystal's oil can refer to embodiment 1, differ only in：The full trimethylammonium propyl column of hydrobromic acid
[6] the addition quality of aromatic hydrocarbons is the 3% of fragrant water quality；Extractant is by dichloromethane, ethyl acetate by volume 10:1 composition,
The volumetric usage extracted every time is the 1/15 of fragrant water volume, coextraction 2 times.
The main component of gained Corallium Japonicum Kishinouye platform tree peony crystal's oil is：1,3,5- trimethoxy-benzenes 66.5%, benzyl carbinol 27.6%,
Citronellol 1.8% etc..
Embodiment 4
The method of the present embodiment reference implementation example 1 prepares WULONGPENGSHANG tree peony aqua aromatica and WULONGPENGSHANG tree peony crystal oil.
The preparation of WULONGPENGSHANG tree peony aqua aromatica can refer to embodiment 1, differ only in：Used composite compaction technique and
Mass content forms：NaCl 9%, MgSO4·7H2O 3%, NaAl (SO4)2·12H2O 1%.
The preparation of WULONGPENGSHANG tree peony crystal's oil can refer to embodiment 1, differ only in：The column aromatic hydrocarbons used is hydrobromic acid
Full trimethylammoniumethyl column [6] aromatic hydrocarbons adds in 2% of quality for fragrant water quality.
The main component of gained WULONGPENGSHANG crystal's oil is：Benzyl carbinol 63.6%, linalool oxide (furan type) 9.8%,
Cis- 3- hexenols 7.4%, geraniol 6.6%, linalool 3.0%, nerol 2.0%, hexanol 1.8%, benzyl alcohol 1.2%, nonyl
Aldehyde 1.1% etc..
Embodiment 5
The method of the present embodiment reference implementation example 2 prepares Hu red peony aqua aromatica and Hu red peony crystal oil.
The preparation of Hu red peony aqua aromatica can refer to embodiment 2, differ only in：Used composite compaction technique and quality
Content groups become：NaCl 11%, MgSO4·10H2O 3%, KAl (SO4)2·12H2O 2%.
The preparation of Hu red peony crystal's oil can refer to embodiment 2, differ only in：The column aromatic hydrocarbons used is hydrobromic acid complete three
First ammonium butyl column [6] aromatic hydrocarbons adds in 3% of quality for fragrant water quality.
The main component of gained Hu red peony crystal's oil is：1,3,5- trimethoxy-benzenes 21.9%, geraniol 20.4%, orange
Flower alcohol 15.0%, linalool oxide (furan type) 10.3%, cis- 3- hexenols 8.5%, hexanol 3.9%, geranic acid 3.5%, α-
Terpinol 2.7%, furtural 2.4%, 6- methyl -5- heptene -2- alcohol 1.0%, enanthaldehyde 1.0% etc..
Embodiment 6
The method of the present embodiment reference implementation example 1 prepares phoenix pellet pink peony aqua aromatica and phoenix pellet pink peony crystal oil.
The preparation of phoenix pellet pink peony aqua aromatica can refer to embodiment 1, differ only in：Used composite compaction technique and matter
Amount content groups become：NaCl 10%, NaSO4·10H2O 2%, NaAl (SO4)2·12H2O 3%.
The preparation of phoenix pellet pink peony crystal's oil can refer to embodiment 1, differ only in：The column aromatic hydrocarbons used is complete for hydrobromic acid
Trimethylammoniumethyl column [6] aromatic hydrocarbons adds in 2% of quality for fragrant water quality.
The main component of gained phoenix pellet pink peony crystal's oil is：Benzyl alcohol 18.8%, 5- hydroxyl -2- decylenic acid delta-lactones
14.7%th, 1,4- dimethoxy benzenes 9.5%, furfural 8.4%, benzaldehyde 6.8%, linalool 5.9%, alpha-terpineol 4.3%, orange
Flower alcohol 4.0%, geraniol 3.7%, 1,2- dimethoxy benzenes 3.0%, linalool oxide (furan type) 2.8%, to terpane -1-
Alcohol 2.6%, geranyl acetone 2.3%, 1,2,4- trimethoxy-benzenes 2.0%, Ergol 1.8% etc..
Embodiment 7
The method of the present embodiment reference implementation example 1 prepares the red blue tree peony aqua aromatica of phoenix and the red blue tree peony crystal oil of phoenix.Feng Dan
The preparation of blue tree peony aqua aromatica can refer to embodiment 1, differ only in：Used composite compaction technique and mass content composition
For：NaCl 12%, NaSO4·10H2O 2%, NaAl (SO4)2·12H2O 2%.
The preparation of the red blue tree peony crystal's oil of phoenix can refer to embodiment 1, differ only in：The column aromatic hydrocarbons used is complete for hydrobromic acid
Trimethylammonium butyl column [6] aromatic hydrocarbons adds in 3% of quality for fragrant water quality.
The main component of the red blue tree peony crystal's oil of gained phoenix is：Linalool oxide (furan type) 21.6%, cinnamyl alcohol
19.7%th, 1,3,5- trimethoxy-benzenes 18.5%, geraniol 12.4%, linalool 9.8%, nerol 9.0% etc..
Embodiment 8
The present embodiment prepares the natural peony crystal oil of soft floral type, by the WULONGPENGSHANG water of 5 mass parts embodiments 4
Essential oil and the combination of the Bai Xueta tree peony crystals oil of 3 mass parts embodiments 1, two kinds of crystal's oil are mixed, shaken at room temperature 5min makes tune
Uniformly to get the natural peony crystal oil of soft floral type, closed, refrigeration.
The natural peony crystal oil of the soft floral type of gained, exemplary fragrance ingredient is as shown in Figure 1, be specially：Benzyl carbinol
40.8%th, citronellol 18.6%, geraniol 10.7%, linalool oxide (furan type) 8.5%, suitable 3 hexenols 5.3%, 1,3,
5- trimethoxy-benzenes 4.7%, hexanol 3.0%.Wherein, floral type ingredient (benzyl carbinol, citronellol+geraniol+nerol+virtue camphor tree
Alcohol+linalool oxide+terpinol) 76.0% is accounted for, assign its soft and quiet and tastefully laid out fragrance of a flower.
The natural peony crystal oil of the soft floral type of gained, all oxygenatedchemicals of ingredient are especially enriched in fragrance
Alcohol, monoterpene alcohol, C6 alcohol etc.；Without alkane and alkene etc. to ingredient of the organoleptic quality without contribution；Without terpenes constituents, Storage period
Between oxydrolysis reaction will not occur, stability is good；There is certain anti-corrosive fresh-keeping simultaneously, inhibit golden yellow grape and typhoid fever bar
The pathogenic bacterias such as bacterium, mosquito repellent, improve pulmonary ventilation function and reduce airway resistance the effects that, available for food preservative,
The multiple fields such as superior cosmetics and champignon therapy.
Embodiment 9
The present embodiment prepares the natural peony crystal oil of green sweet tea flowers and fruits odor type, takes the phoenix pellet pink peony of 6 mass parts embodiments 6
Crystal's oil, the red blue tree peony crystal oil of phoenix of 3 mass parts embodiments 7, the Hu red peony crystal of 1 mass parts embodiment 5 are oily, at room temperature
Mixing, oscillation 10min make reconciliation uniformly to get the natural peony crystal oil of green sweet tea flowers and fruits odor type, closed, refrigeration.
The natural peony crystal oil of gained blueness sweet tea flowers and fruits odor type, is detected, main component is as shown in Figure 1, specific through GC-MS
For：Benzyl alcohol 13.8%, 5- hydroxyl -2- decylenic acids delta-lactone 12.8%, cinnamyl alcohol 9.9%, 1,3,5- trimethoxy-benzenes
9.7%th, 1,4- dimethoxy benzenes 6.7%, nerol 6.2%, geraniol 5.5%, furfural 4.9%, benzaldehyde 4.1%, fragrant camphor tree
Alcohol 4.0%, alpha-terpineol 3.6%.Wherein, Fruity type ingredient (benzyl alcohol+cinnamyl alcohol+hexanol+delta-lactone) and floral type ingredient
(citronellol+geraniol+nerol+linalool+linalool oxide+terpinol) accounts for 36.5% and 20.3% respectively, assigns its blueness
The flowers and fruits of sweet tea elegance are fragrant, and fragrance is mildly lasting.
The natural peony crystal oil of gained blueness sweet tea flowers and fruits odor type, all oxygenatedchemicals of ingredient are especially enriched in virtue
Aromatic, delta-lactone, methoxybenzene, monoterpene alcohol, aldehydes etc., without alkane and alkene etc. to ingredient of the organoleptic quality without contribution.Together
When with certain anti-corrosive fresh-keeping, local analgesia, calmness and the pressure that minds at rest, remove free radical, inhibit melanin generation
Effect.Available for multiple fields such as food fine perfumery essence, aromatherapy and superior cosmetics.In addition, without terpenes
Ingredient, is susceptible to oxydrolysis reaction, and storge quality is good.
Embodiment 10
The present embodiment prepares the natural peony crystal oil of balance tree peony odor type I, takes the WULONGPENGSHANG of 2 mass parts embodiments 4
Crystal's oil, the Corallium Japonicum Kishinouye platform crystal oil of 3 mass parts embodiments 3, the beautiful ball crystal oil of 3 mass parts embodiments 2,2 mass parts are implemented
The red blue tree peony crystal oil of the phoenix of example 7, mixes, it is uniformly naturally male to get balance tree peony odor type I that oscillation 15min makes reconciliation at room temperature
Pellet flower crystal's oil, closed, refrigeration.
The natural peony crystal oil of gained balance tree peony odor type I, is detected, main component is as shown in Figure 1, specific through GC-MS
For：Benzyl carbinol 21.7%, 1,3,5- trimethoxy-benzenes 21.5%, cis- 3- hexenols 9.6%, cinnamyl alcohol 8.6%, hexanol
6.7%th, geraniol 6.2%, 1,4- dimethoxy benzenes 4.9%, linalool 3.4%, linalool oxide (furan type) 3.3%, orange
Flower alcohol 3.0%.
The natural peony crystal oil of gained balance tree peony odor type I, all kinds of fragrance component balanced proportions assign its soft elegance
Natural fresh peony flower fragrance.Wherein, floral type ingredient (benzyl carbinol, citronellol+geraniol+nerol+linalool+oxidation virtue
Camphor tree alcohol+terpinol) account for 37.6%, Fruity type ingredient (benzyl alcohol+cinnamyl alcohol+hexanol+delta-lactone) 15.3%, glycol jasmine tea odor type
Ingredient (1,3,5- trimethoxy-benzene+Isosorbide-5-Nitrae-dimethoxy benzene) accounts for 26.4%, and pure and fresh leaf odor type ingredient (cis- 3- hexenols) accounts for
9.6%.
The natural peony crystal oil of gained balance tree peony odor type I, all oxygenatedchemicals of ingredient.Gained balance is male
The natural peony crystal oil of red odor type I, without alkane and alkene etc. to ingredient of the organoleptic quality without contribution, without terpenes into
Point, oxidation, hydrolysis are not susceptible to during storage, stability is good.There is certain Antimicrobial preservative, fresh-keeping deodorizing, drive simultaneously
Mosquito effect is kept away, also have the function of to improve pulmonary ventilation function and reduces airway resistance, calmness and the pressure that minds at rest.It can conduct
Advanced natural tree peony fragrance in functional food and superior cosmetics, also available for aromatherapy.
Embodiment 11
The present embodiment prepares the natural peony crystal oil of balance tree peony odor type II, by Bai Xueta tree peonies crystal oil, Corallium Japonicum Kishinouye platform
Tree peony crystal oil, Hu red peony crystal oil, phoenix pellet pink peony crystal oil in mass ratio 4:4:1:1 composition.Specific preparation method can
Reference implementation example 10, wherein Contents of Main Components can be converted to obtain by the ingredient of crystal's oil of corresponding embodiment.
Embodiment 12
The present embodiment prepares the natural peony crystal oil of pure and fresh floral leaf odor type, by beautiful ball tree peony crystal oil, Hu red peony
Crystal's oil in mass ratio 3:1 composition.Specific preparation method can refer to embodiment 10, and wherein Contents of Main Components can be by accordingly implementing
The ingredient of crystal's oil of example converts to obtain.
Embodiment 13
The present embodiment prepares the natural peony crystal oil of glycol jasmine tea odor type, by Corallium Japonicum Kishinouye platform crystal oil, the red blue crystal's oil of phoenix
In mass ratio 1:1 composition.Specific preparation method can refer to embodiment 10, and wherein Contents of Main Components can be by the water of corresponding embodiment
The ingredient of essential oil converts to obtain.
Comparative example 1
Comparative example 1 selects mass concentration to pickle Bai Xueta fresh peony flower 3d for 15% NaCl solution, then referring to implementation
The method of example 1 prepares Bai Xueta tree peonies aqua aromatica and crystal's oil.
Gained Bai Xueta peonies crystal oil, is detected, main component is through GC-MS：Citronellol 37.3%, geraniol
10.8%th, nonadecane 10.0%, heptadecane 6.3%, germacrene D 5.6%, cis- 3- hexenols 5.4%, 1,3,5- front threes
Oxygroup benzene 4.6%, 1,3,5- trimethoxy-benzenes 4.0%, hexanol 3.9%, geranic acid 3.7%, pentadecane 3.2%, limonene
1.5%th, cis-rose oxide 1.3%, linalool 0.9%, alpha-terpineol 0.8%, pohytol 0.7%.
From embodiment 1 with and comparative example 1 crystal's oil component can be seen that use quality a concentration of 15% NaCl it is molten
Liquid, gained are spent containing some unworthy ingredients in crystal's oil, such as alkane (nonadecane, heptadecane, pentadecane) and terpenes (big root
Myrcene D, limonene) etc..And the composite compaction technique dialogue snow tower tree peony of embodiment 1 is used to extract, it on the one hand can be rich
The type of significant oxygenatedchemicals is influenced in Fu Baixueta tree peonies aqua aromatica and crystal's oil on organoleptic quality and bioactivity,
On the other hand the content of alkane and the valueless ingredient of terpenes can be reduced, improves the high valuable compounds such as aromatic alcohol, monoterpene alcohol
Content, so as to improve the quality of aqua aromatica and crystal's oil product.
In addition, oily using the distillation time and crystal of complex salt pretreatment and the pretreatment of traditional sodium chloride of the present invention
The correspondence figure of rate, as shown in Figure 2.
As seen from Figure 2, it is pre-processed using complex salt, distillation 45min is close to balance yield, and uses sodium chloride
Pretreatment then takes 150min and is just close to balance yield.It, can using complex salt pretreatment compared with sodium chloride is used to pre-process
Flower crystal's oil is balanced yield to improve to 4.6 times.
Pass through the chemistry spectrum of the crystal of comparative example 1 and embodiment 1 oil and the comparing result of yield, it can be seen that the present invention
Used composite compaction technique shortens the immersion salting period of fresh flower, optimizes mass transport process, improves the yield of crystal's oil,
Improve the quality of aqua aromatica and crystal's oil.
Comparative example 2
The method of 2 reference implementation example 1 of comparative example prepares Bai Xueta tree peony aqua aromaticas, is then added without the full trimethylammonium of hydrobromic acid
Propyl column [6] aromatic hydrocarbons, but directly extracted using the mixed solvent of embodiment 1, the mixed solvent that extraction adds in every time
Volume is same as Example 1, coextraction 6 times, combining extraction liquid, after filtered, removing solvent, prepares Bai Xueta crystals oil.
Fig. 3 is to prepare the extraction efficiency of crystal's oil and organic solvent consumption by the method for comparative example 2 and embodiment 1
Comparison diagram.As can be seen that when not using column [6] aromatic hydrocarbons, the extraction yield that continuous extraction is 6 times is only 35.0%；When using hydrobromic acid
During full trimethylammonium propyl column [6] aromatic hydrocarbons, 2 extraction yields i.e. reachable 93.4% is extracted, solvent-oil ratio is reduced to 1/3 at this time.
The above result shows that it can be remarkably promoted using full trimethylammonium propyl column [6] aromatic hydrocarbons of hydrobromic acid water-soluble in perfume
The extraction rate of transform of property derived essential oil, so as to improve extraction yield, reduces the consumption of organic solvent.
Comparative example 3
Comparative example 3 selects beautiful ball fresh peony flower same as Example 2, by four general rules of version Chinese Pharmacopoeia in 2015
2204 determination of volatile oil methods (first method), steam distillation 2.5h collect gained oil reservoir in extractor, as beautiful ball tree peony essence
Oil.
The main component (single component content >=1.0%) of beautiful ball peony essential oil is：Heptadecane 12.3%, nonadecane
9.4%th, pentadecane 9.1%, 1,4- dimethoxy benzenes 8.8%, cis- 9- tetradecenes -1- alcohol 7.2%, germacrene D
6.6%th, tricosane 5.9%, 17 alkene 4.7% of (E) -8-, suitable 3- hexenols 4.2%, pentacosane 3.9%, heneicosane
3.7%th, linalool 3.4%, hexanol 3.3%, 2- methyl hexadecane 2.9%, the tetradecane 2.1%, geraniol 1.7%, 4,7- bis-
Methyl benzofuran 1.0% etc..In all the components, oxygenatedchemicals only accounts for 35.0%, and alkane and olefines account for 57.8%, terpenes
Class accounts for 7.2%.A large amount of alkane and alkene have no its organoleptic quality and bioactivity contribution, and institute in beautiful ball peony essential oil
Constituents containing terpenes easily occur oxydrolysis reaction and lead to the reduction of essential oil quality.
The typical composition comparison of the 2 beautiful ball tree peony crystal oil of gained of the beautiful ball peony essential oil of 3 gained of comparative example and embodiment
As shown in Figure 4, it can be seen that all oxygenatedchemicals of ingredient of the beautiful ball tree peony crystal oil of embodiment 2, without pair
Organoleptic quality and bioactivity alkane and alkene without contribution, without terpenes constituents, chemistry spectrum composition is significantly better than comparison
The beautiful ball peony essential oil of example 3.
In the other embodiment of the composite compaction technique of the present invention, composition can be used as " NaCl 8-12%, MgSO4·
7H2O 2-6%, KAl (SO4)2·12H2O 1-3%, solvent are water "；Or " NaCl 8-12%, Na2SO4·10H2O 2-6%,
NaAl(SO4)2·12H2O 1-3%, solvent are water "；Or " NaCl 8-12%, MgSO4·7H2O 2-6%, NaAl (SO4)2·
12H2O 1-3%, solvent is by water " composite compaction technique replace the composite compaction technique in embodiment 1, in the mechanism of action
It is identical, it can obtain and the comparable extraction effect of the composite compaction technique of embodiment 1.
In the other embodiment of the fresh flower crystal oil of the present invention, full trimethylammoniumethyl column [6] aromatic hydrocarbons, full trimethylammonium can be used
Butyl column [6] aromatic hydrocarbons to carry out the column arene derivatives in embodiment 1 equivalent replacement, the attainable technique effect of institute and reality
It is suitable to apply example 1.
Claims (10)
1. a kind of fresh flower crystal oil, which is characterized in that be prepared by method comprising the following steps：By fresh flower aqua aromatica and column
Arene derivatives mix, and then add in organic solvent and are extracted, the organic solvent in separation organic phase, removing organic phase, i.e.,
；The column arene derivatives are full trimethylammonium propyl column [6] aromatic hydrocarbons of hydrobromic acid, full trimethylammoniumethyl column [6] aromatic hydrocarbons, full front three
At least one of ammonium butyl column [6] aromatic hydrocarbons.
2. fresh flower crystal oil as described in claim 1, which is characterized in that the quality of column arene derivatives is fresh flower fragrance water quality
The 1-3% of amount.
3. fresh flower crystal oil as described in claim 1, which is characterized in that the organic solvent is dichloromethane, ethyl acetate
The mixed solvent of composition.
4. fresh flower crystal as claimed in claim 3 oil, which is characterized in that dichloromethane, ethyl acetate volume ratio be (10-
20)：1.
5. the fresh flower crystal oil as described in claim 1 or 3 or 4, which is characterized in that during extraction, organic solvent and fresh flower fragrance
The volume ratio of water is 1：(10-20).
6. fresh flower crystal as described in claim 1 oil, which is characterized in that the fresh flower is peony, rose, Chinese rose, oriental cherry,
At least one of sweet osmanthus.
7. fresh flower crystal oil as claimed in claim 6, which is characterized in that the kind of the peony is Corallium Japonicum Kishinouye platform, oolong is held in both hands
At least one of Sheng, Bai Xueta, beautiful ball, Hu Hong, phoenix pellet powder, phoenix pellet indigo plant.
8. a kind of more odor type flower crystal's oil, which is characterized in that mixed by least two fresh flower crystal oil as described in claim 1
It forms.
9. more odor type flower crystal's oil as claimed in claim 8, which is characterized in that by WULONGPENGSHANG tree peony crystal oil and Bai Xueta
Tree peony crystal oil (1-25) in mass ratio：5 mixing obtain soft floral type peony crystal oil.
10. more odor type flower crystal's oil as claimed in claim 8, which is characterized in that Corallium Japonicum Kishinouye platform tree peony crystal oil and phoenix is red blue
Tree peony crystal oil (1-8) in mass ratio：2 mixing obtain glycol jasmine tea odor type peony crystal oil.
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Denomination of invention: A type of flower water essential oil and multi fragrance flower water essential oil Granted publication date: 20210730 Pledgee: Beijing first financing Company limited by guarantee Pledgor: Wellfin (Beijing) Technology Development Co.,Ltd. Registration number: Y2024110000095 |