CN107287035A - A kind of preparation method for dropping the essential oil that smells good - Google Patents
A kind of preparation method for dropping the essential oil that smells good Download PDFInfo
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- CN107287035A CN107287035A CN201710675374.7A CN201710675374A CN107287035A CN 107287035 A CN107287035 A CN 107287035A CN 201710675374 A CN201710675374 A CN 201710675374A CN 107287035 A CN107287035 A CN 107287035A
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- Prior art keywords
- essential oil
- drop
- good
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- smells good
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Classifications
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- 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
-
- 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
- C11B9/022—Refining
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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)
- Extraction Or Liquid Replacement (AREA)
Abstract
A kind of preparation method for dropping the essential oil that smells good, including：The drop wood powder that smells good is passed through into supercritical CO2Drop is obtained by extraction to smell good medicinal extract；The drop medicinal extract that smells good is obtained drop through micro-filtration purifying and smelt good essential oil.The present invention uses supercritical CO2Abstraction technique is extracted to the drop essential oil that smells good, and is added without any organic solvent in extraction process, and the drop of the preparation essential oil that smells good is more pure, then by different aperture filter membranes, realizes the separation of different molecular quantity of material, reaches the purpose for purifying essential oil；This technology method mild condition, extraction efficiency is high, to heat-sensitive materials without any destruction.
Description
Technical field
The present invention relates to biological technical field, in particular to a kind of preparation method for dropping the essential oil that smells good.
Background technology
Drop smells good, also known as:Tanarius major, Thickleaf Croton Root.Pulse family wingceltis belongs to rattan perfume, is a kind of Guangdong of perennial bejuco two
Secretion grease repairs the spices that wound is tied after yellow wingceltis and oblique leaf yellow wingceltis are injured, and its rattan Song Dynasty is named lucky yncaria stem with hooks also name Wu Liteng, U.S.
Long Teng, what Hainan multitude's language was exhaled claims its house steward rattan for Teng Zong passes, Miao ethnic group.
Drop, which smells good, typically takes more than 50 years ability Edgeworthia chrysanthas, drops the place that the grease smelt good is concentrated mainly on injury, typically
All it is easy to concentrate grease in the crotch position of rattan, injured infection part, wound wound location, and the abundant fragrance of grease is strong clearly.It is main
The chemical composition is wanted to be：Bud hemiterpene, chromocor compound (derivative of chromone).It is consistent with whitewood agalloch eaglewood that the main component that smells good drops.Drop
Smell good containing abundant flavone compound, with multiple biological activities, can ease pain, stop blooding, antibacterial, anti-inflammatory.《Compendium of Materia Medica》：
" pungent-warm and non-toxic, children treat injured, metal-inflicted wound with its bad odor that exorcises evil spirits, stop blooding analgesic therapy, detumescence and promoting granulation.”.Modern pharmacological research shows,
Drop smells good with the bioactivity such as antitumor, antibacterial and cytotoxicity.
The elite that smells good drops in its essential oil, and the drop the reported at present extraction of essential oil that smells good mainly has steam distillation, surpasses
Critical extraction combines dissolving extraction method；Time-consuming for steam distillation, destroys big to heat-sensitive materials, solvent extraction can cause molten
Agent is remained, and solvent is often poisonous, and essential oil quality is low.
In view of this, it is special to propose the present invention.
The content of the invention
It is an object of the invention to provide a kind of preparation method for dropping the essential oil that smells good, this method combination supercritical CO2Extraction
Technology and micro-filtration purification technique, to solve the above problems.
In order to realize the above-mentioned purpose of the present invention, spy uses following technical scheme：
A kind of preparation method for dropping the essential oil that smells good, including：
The drop wood powder that smells good is passed through into supercritical CO2Drop is obtained by extraction to smell good medicinal extract；The drop medicinal extract that smells good is pure through micro-filtration
Change and obtain drop and smell good essential oil.
Overcritical is supercritical fluid, is a kind of not only on-gaseous but also the states of matter of non-liquid between gas-liquid, this thing
Matter can only could exist in its temperature and pressure postcritical.Supercritical fluid has the double grading of gas and liquid,
Its viscosity is similar to gas, but diffusion coefficient is more much bigger than liquid.The density of supercritical fluid is close to liquid, viscosity and diffusion
Coefficient is close to gas, and its solvability is suitable with liquid flux, and with excellent mass-transfer performance.
Supercritical fluid of the present invention is CO2, its critical-temperature is 31.265 DEG C, and critical pressure is 7.18MPa,
Critical condition easily reaches.In the supercritical state, CO2Change of the density of fluid to temperature and pressure is very sensitive, and its is molten
Solution ability is proportional within the specific limits to pressure, therefore can make extract by changing the temperature and pressure of system
Solubility changes, and separates it, so as to reach the purpose of separation and Extraction.
Microfiltration membranes, are that a kind of permission macromolecular and soluble solid etc. pass through, but can retain suspension, and macromolecule glue
The mwco membrane of the materials such as body.
The present invention is purified using micro-filtration membrane separation technique to dropping the extract that smells good, and this method can pass through different filters
Membrane aperture, realizes the separation of different molecular quantity of material；Membrane separation technique mild condition, to heat-sensitive materials without any destruction.
It is preferred that, drop as described above smells good the preparation method of essential oil, and the smell good particle diameter of wood powder of the drop is 30~60 mesh；
More preferably 40~50 mesh.
Granule size can influence extraction recovery.Reduce sample granularity, the contact area of solid and solvent can be increased, improve
Rate of extraction.But if undersized, sieve aperture can be blocked, the blocking that extractor exports filter screen is in turn resulted in.
It is preferred that, the preparation method as described above for dropping the essential oil that smells good, the supercritical CO2Pressure during extraction is
25MPa~50MPa；More preferably 30MPa~45MPa, can also select 35MPa~40MPa.
Extracting pressure is supercritical CO2One of most important parameter of fluid extraction process.In the timing of extraction temperature one, work as pressure
Power increases, and the density of fluid will increase, and its solvent strength also strengthens, thus the solvability of solvent just strengthens, extraction efficiency
Also just corresponding raising.For example, CO2At 37 DEG C, when pressure rises to 10MPa by 8MPa, nearly 1 times of its density increase, significantly
Improve CO2Dissolve the ability of material.
It is preferred that, the preparation method as described above for dropping the essential oil that smells good, the supercritical CO2Temperature during extraction is 30 DEG C
~70 DEG C；
It is furthermore preferred that the supercritical CO2Temperature during extraction is 40 DEG C~60 DEG C, can also select 50 DEG C.
It is preferred that, the preparation method as described above for dropping the essential oil that smells good, the supercritical CO2The extraction time of extraction is
120min~250min；
It is furthermore preferred that the supercritical CO2The extraction time of extraction is 140min~230min；Or 170min~
200min；180min~190min can also be selected.
Supercritical CO2Change of the density of fluid to temperature and pressure is very sensitive, and its solvability is in certain pressure intensity model
Relation proportional to its density in enclosing, changes the solubility of material by the regulation and control to temperature and pressure.Particularly critical
Near state, supercritical CO2Fluid has a high compressibility, and the minor variations of temperature and pressure frequently can lead to the molten of solute
The mutation of several orders of magnitude occurs for Xie Du.Most preferably, supercritical CO of the present invention2The extraction conditions of extraction is 27.5MPa
~32.5MPa, 35 DEG C~36 DEG C extraction 170min~190min.
It is preferred that, the preparation method as described above for dropping the essential oil that smells good, the filter sizes of the micro-filtration are 0.2 μm~1.0 μ
M, more preferably 0.4 μm~0.8 μm, or 0.45 μm~0.6 μm, or 0.5 μm.
The raw material of the filter sizes of micro-filtration and institute's Purification by filtration is closely related.
It is preferred that, the preparation method as described above for dropping the essential oil that smells good, the pressure of the micro-filtration is 0.2MPa~0.5MPa；
More preferably 0.3MPa~0.4MPa.
It is preferred that, the preparation method as described above for dropping the essential oil that smells good, the temperature of the micro-filtration is 20 DEG C~40 DEG C；It is more excellent
Elect 25 DEG C~35 DEG C, or 30 DEG C as.
The smell good drop for preparing of preparation method of essential oil of drop as described above smells good essential oil.
Compared with prior art, beneficial effects of the present invention are：
1), the present invention uses supercritical CO2Abstraction technique is extracted to dropping the essential oil that smells good, and is added without in extraction process
Any organic solvent, the drop of the preparation essential oil that smells good is more pure.
2), the method that the present invention is provided can realize the separation of different molecular quantity of material by different filter sizes；Film
Isolation technics mild condition, to heat-sensitive materials without any destruction.
Brief description of the drawings
, below will be to specific in order to illustrate more clearly of the specific embodiment of the invention or technical scheme of the prior art
The accompanying drawing used required in embodiment or description of the prior art is briefly described, it should be apparent that, in describing below
Accompanying drawing is some embodiments of the present invention, for those of ordinary skill in the art, before creative work is not paid
Put, other accompanying drawings can also be obtained according to these accompanying drawings.
Fig. 1 is that the essential oil GC-MS collection of illustrative plates that smells good drops in oblique leaf yellow wingceltis prepared by the embodiment of the present invention 4；
Fig. 2 is that the essential oil GC-MS collection of illustrative plates that smells good drops in Lignum Dalbergiae benthamii prepared by the embodiment of the present invention 5.
Embodiment
Unless otherwise defined, all technologies for using of the present invention and scientific terminology have with belonging to disclosed embodiment
The identical implication that the those of ordinary skill in field is generally understood that.Although similar or equivalent with method of the present invention and material
Method and material can be used in the practice or test of present embodiment, but hereafter still describe suitable method and material.
All publications, patent application, patent and other bibliography that the present invention is referred to are incorporated into this by quoting full content
Wen Zhong.In the case of a conflict, this specification (including definition) will play dominating role.In addition, material, method and embodiment are only
It is merely illustrative, and is not intended to limitation.Other feature and advantage of embodiment will be from following detailed description of book and right
It is required that in become obvious.
In order to promote to understand implementations described herein this purpose, some embodiments will be referred to, and will use
Language-specific describes these embodiments.Term as used herein is only used for describing embodiment purpose, without purport
In limitation the scope of the present disclosure.
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the present invention.It is unreceipted specific in embodiment
Condition person, the condition advised according to normal condition or manufacturer is carried out.Agents useful for same or the unreceipted production firm person of instrument, be
The conventional products that can be obtained by commercially available purchase.
Embodiment 1
Present embodiments provide the preparation method that the essential oil that smells good drops in a kind of oblique leaf yellow wingceltis.
1. oblique leaf wingceltis is dropped into the wood powder that smells good is broken to 30 mesh；
2. above-mentioned powder is added into supercritical CO2In extraction kettle；
3. the pressure for adjusting supercritical extract is 35MPa, extraction temperature is 31.265 DEG C, extracts 250min；
4. above-mentioned extraction medicinal extract is collected, it is placed in ultrafiltration apparatus and carries out ultrafiltration；
5. above-mentioned micro-filtration pressure is 0.5MPa, filter sizes are 0.22 micron, and temperature is 40 DEG C.
6. the essential oil product that smells good must be dropped by collecting above-mentioned micro-filtration material.
Embodiment 2
Present embodiments provide the preparation method that the essential oil that smells good drops in a kind of oblique leaf yellow wingceltis.
1. oblique leaf wingceltis is dropped into the wood powder that smells good is broken to 60 mesh；
2. above-mentioned powder is added into supercritical CO2In extraction kettle；
3. the pressure for adjusting supercritical extract is 30MPa, extraction temperature is 50 DEG C, extracts 120min；
4. above-mentioned extraction medicinal extract is collected, it is placed in ultrafiltration apparatus and carries out ultrafiltration；
5. above-mentioned micro-filtration pressure is 0.2MPa, filter sizes are 0.5 micron, and temperature is 20 DEG C.
6. the essential oil product that smells good must be dropped by collecting above-mentioned micro-filtration material.
Embodiment 3
Present embodiments provide the preparation method that the essential oil that smells good drops in a kind of Lignum Dalbergiae benthamii.
1. oblique leaf wingceltis is dropped into the wood powder that smells good is broken to 40 mesh；
2. above-mentioned powder is added into supercritical CO2In extraction kettle；
3. the pressure for adjusting supercritical extract is 40MPa, extraction temperature is 35.5 DEG C, extracts 180min；
4. above-mentioned extraction medicinal extract is collected, it is placed in ultrafiltration apparatus and carries out ultrafiltration；
5. above-mentioned micro-filtration pressure is 0.4MPa, filter sizes are 0.45 micron, and temperature is 30 DEG C.
6. the essential oil product that smells good must be dropped by collecting above-mentioned micro-filtration material.
Embodiment 4
Present embodiments provide the preparation method that the essential oil that smells good drops in a kind of oblique leaf yellow wingceltis.
1. oblique leaf wingceltis is dropped into the wood powder that smells good is broken to 50 mesh；
2. above-mentioned powder is added into supercritical CO2In extraction kettle；
3. the pressure for adjusting supercritical extract is 35MPa, extraction temperature is 35.5 DEG C, extracts 180min；
4. above-mentioned extraction medicinal extract is collected, it is placed in ultrafiltration apparatus and carries out ultrafiltration；
5. above-mentioned micro-filtration pressure is 0.5MPa, filter sizes are 0.45 micron, and temperature is 25 DEG C.
6. the essential oil product that smells good must be dropped by collecting above-mentioned micro-filtration material.
Table 1
| Color shape | Optical activity | Refraction index | Hold fragrance | Moisture/% | |
| The present invention | Brown color liquid | -15° | 1.54 | 4.5h | 1.3 |
| Ether is extracted | Light brown liquid | -15° | 1.52 | 3.5h | 1.7 |
Table 2
Embodiment 5
Present embodiments provide the preparation method that the essential oil that smells good drops in a kind of Lignum Dalbergiae benthamii.
1. Lignum Dalbergiae benthamii is dropped into the wood powder that smells good is broken to 50 mesh；
2. above-mentioned powder is added into supercritical CO2In extraction kettle；
3. the pressure for adjusting supercritical extract is 42MPa, extraction temperature is 35.5 DEG C, extracts 180min；
4. above-mentioned extraction medicinal extract is collected, it is placed in micro-filtration and carries out membrane filtration；
5. above-mentioned micro-filtration pressure is 0.15MPa, filter sizes are 0.22 micron, and temperature is 50 DEG C.
6. the essential oil product that smells good must be dropped by collecting above-mentioned micro-filtration material.
Table 3
| Color shape | Optical activity | Light transmittance | Hold fragrance | Moisture/% | |
| The present invention | Brown liquid | -12° | 1.52 | 5.5h | 1.4 |
| Ether is extracted | Brown liquid | -11 | 1.53 | 5.0h | 1.8 |
Table 4
Finally it should be noted that：Various embodiments above is merely illustrative of the technical solution of the present invention, rather than its limitations；To the greatest extent
The present invention is described in detail with reference to foregoing embodiments for pipe, but it will be understood by those within the art that：Its
The technical scheme described in foregoing embodiments can still be modified, or to which part or all technical characteristic
Carry out equivalent substitution；And these modifications or replacement, the essence of appropriate technical solution is departed from various embodiments of the present invention skill
The scope of art scheme.
Claims (10)
1. a kind of preparation method for dropping the essential oil that smells good, it is characterised in that including：
The drop wood powder that smells good is passed through into supercritical CO2Drop is obtained by extraction to smell good medicinal extract；The drop is smelt good into medicinal extract through micro-filtration purifying acquisition
The essential oil that smells good drops.
The preparation method of essential oil 2. drop according to claim 1 smells good, it is characterised in that the drop smells good the particle diameter of wood powder
For 30~60 mesh.
The preparation method of essential oil 3. drop according to claim 1 smells good, it is characterised in that the supercritical CO2During extraction
Pressure is 25MPa~50MPa.
The preparation method of essential oil 4. drop according to claim 3 smells good, it is characterised in that the supercritical CO2During extraction
Temperature is 30 DEG C~70 DEG C.
The preparation method of essential oil 5. drop according to claim 4 smells good, it is characterised in that the supercritical CO2The extraction of extraction
It is 120min~250min to take the time.
The preparation method of essential oil 6. drop according to claim 5 smells good, it is characterised in that the supercritical CO2The extraction of extraction
It is 27.5MPa~32.5MPa, 35 DEG C~36 DEG C extraction 170min~190min to take condition.
The preparation method of essential oil 7. drop according to claim 1 smells good, it is characterised in that the filter sizes of the micro-filtration are
0.2 μm~1.0 μm.
The preparation method of essential oil 8. drop according to claim 1 smells good, it is characterised in that the pressure of the micro-filtration is
0.2MPa~0.5MPa.
The preparation method of essential oil 9. drop according to claim 8 smells good, it is characterised in that the temperature of the micro-filtration is 20 DEG C
~40 DEG C.
The drop that the preparation method of essential oil is prepared 10. the drop described in any one of claim 1~9 smells good smells good essential oil.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109646329A (en) * | 2018-11-29 | 2019-04-19 | 中国热带农业科学院农产品加工研究所 | It is a kind of to drop the essential oil content in freckle cream and preparation method thereof that smells good |
| CN113616839A (en) * | 2021-07-28 | 2021-11-09 | 海南长永恒生物科技有限公司 | Smokeless environment-friendly line incense and manufacturing method thereof |
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| JP2013040289A (en) * | 2011-08-17 | 2013-02-28 | Central Research Institute Of Electric Power Industry | Oil and fat extraction method from oilseed plant, and manufacturing method of defatted product of oilseed plant |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109646329A (en) * | 2018-11-29 | 2019-04-19 | 中国热带农业科学院农产品加工研究所 | It is a kind of to drop the essential oil content in freckle cream and preparation method thereof that smells good |
| CN113616839A (en) * | 2021-07-28 | 2021-11-09 | 海南长永恒生物科技有限公司 | Smokeless environment-friendly line incense and manufacturing method thereof |
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