CN108659957A - The method that jujube extracts essential oil - Google Patents
The method that jujube extracts essential oil Download PDFInfo
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- CN108659957A CN108659957A CN201810633318.1A CN201810633318A CN108659957A CN 108659957 A CN108659957 A CN 108659957A CN 201810633318 A CN201810633318 A CN 201810633318A CN 108659957 A CN108659957 A CN 108659957A
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- jujube
- essential oil
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- liquid nitrogen
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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
- C11B9/025—Recovery by solvent extraction
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/027—Recovery of volatiles by distillation or stripping
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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 methods that jujube extracts essential oil comprising step：(1) jujube is immersed in liquid nitrogen, it is cooling, obtain super cold jujube；(2) the super cold jujube is subjected to liquid nitrogen frozen pulverization process, obtains super cold jujube powder；(3) the super cold jujube powder is subjected to frozen dried, obtains super cold extra dry red wine date powder end；(4) by the super cold extra dry red wine date powder end, Soxhlet extraction is carried out, jujube essential oil solution is obtained；(5) the jujube essential oil solution is evaporated in vacuo, obtains jujube essential oil.The present invention has extraction of essential oil rate high, and the dense advantage of characteristic perfume can make full use of the jujube core, fructus corni and jujube meat of jujube, greatly improve the recovery rate of essential oil under the premise of not reducing jujube essential oil quality.
Description
Technical field
The present invention relates to plants essential oils to extract field, a kind of method for extracting essential oil more particularly, to jujube.
Background technology
Jujube contains the necessary multivitamin of the human bodies such as abundant vitamin A, B, C and 18 kinds of amino acid, minerals,
Wherein the content of vitamin C (ascorbic acid) be up to unexpectedly grape, 70~80 times of apple.But the storage capacity of jujube less than
20% or so of total output, refrigeration ability is 7% or so, and fresh fruit rotting rate up to 20%~25%, grind by the deep process technology of jujube
Studying carefully becomes red dates industry urgent problem.The main direction of development that essential oil is current is extracted from jujube.
Jujube essential oil is a kind of with, with volatile substance, it is a kind of with very high medicine under special odor, room temperature
With the precious liquid of value and health properties, there is making oxygen content enhancing in blood, nourishes systemic cell.It is a kind of drug effect
The tonic of mitigation.Jujube essential oil has antibechic, wind dispelling, prevents angiocardiopathy, improves the effects that immunity, stomach invigorating.
Currently, jujube essential oil, extraction mainly has steam distillation, supercritical CO2Extraction, microwave extraction method etc..This
The recovery rate of several method is all relatively low, and the jujube core more to beneficiating ingredient in jujube and fructus corni extraction are not enough.In addition, existing
Method largely need high-temperature process, easily cause the loss of fragrance and flavor.It is desirable to a kind of not reducing essential oil quality,
And it can fully extract the essential oil of entire jujube and the method that recovery rate is high.
Invention content
The object of the present invention is to provide a kind of methods that jujube extracts essential oil, can not reduce the premise of jujube essential oil quality
Under, the jujube core, fructus corni and jujube meat of jujube are made full use of, the recovery rate of essential oil is greatly improved.
To achieve the goals above, the present invention provides a kind of method of jujube extraction essential oil comprising step：It (1) will be red
Jujube immerses in liquid nitrogen, cooling, obtains super cold jujube；(2) the super cold jujube is subjected to liquid nitrogen frozen pulverization process, obtained super cold
Jujube powder；(3) the super cold jujube powder is subjected to frozen dried, obtains super cold extra dry red wine date powder end；It (4) will be described super cold dry
Jujube powder carries out Soxhlet extraction, obtains jujube essential oil solution；(5) the jujube essential oil solution is evaporated in vacuo, obtains jujube essence
Oil.
Optionally, the jujube is the jujube of fresh jujube or naturally dry.
Optionally, jujube is immersed into the time cooling in liquid nitrogen for 10~30min
Optionally, the process of the liquid nitrogen frozen pulverization process is：The super cold jujube by liquid nitrogen frozen pulverizer material
Pulverizing chamber is put into storehouse, and the temperature for adjusting pulverizing chamber is -190~-100 DEG C, is crushed 0.5~2 hour, is sieved, and is collected.
Optionally, the process of the frozen dried is：After freeze drying box is cooled to -50~-20 DEG C, by the super cold jujube
Powder is fitted into glass dish, is positioned in freeze drying box；It is evacuated to 0.7~1MPa of vacuum degree, is kept for 5~10 hours；It is heated to
40~50 DEG C, and kept for 5~8 hours；Restore to normal pressure, taking-up obtains super cold extra dry red wine date powder end.
Optionally, the process of the Soxhlet extraction is：The super cold extra dry red wine date powder end is placed in cylindrical filtration paper cylinder, altogether
It is same to be put into the extraction tube of Soxhlet extractor；Be put into ethyl alcohol in the extraction flask of the Soxhlet extractor, ethyl alcohol with it is described super cold
Extra dry red wine date powder end mass ratio is 1:1~15；The Soxhlet extractor is opened, extraction time is 3~5 hours.
Optionally, the extraction tube of the Soxhlet extractor receives one kind in microwave irradiation and ul-trasonic irradiation or combination.
Optionally, the process of the vacuum distillation is：The jujube essential oil solution is placed in beaker, it is dry to be positioned over vacuum
In the babinet of dry case；The gas cylinder of inert gas is connected to the air intake valve of the vacuum drying chamber by pipeline, opens the gas
The valve of bottle adjusts the output valve of decompression table, and it is 0.1~0.2MPa to keep output pressure；Vacuum pump is opened, vacuum is extracted, is adjusted
Air intake valve is saved, 0.4~0.75Mpa of vacuum degree is kept；The temperature of the vacuum drying chamber is set as 55~75 DEG C, described in holding
Jujube essential oil solution is in slight boiling condition；After distillation, vacuum pump is closed, waits for that the babinet of vacuum drying chamber naturally cools to room
Wen Hou restores pressure in babinet and closes gas cylinder valve to normal pressure, takes out beaker, closed preservation obtains jujube essential oil.
Optionally, the inert gas is one kind in argon gas and nitrogen.
The present invention by carrying out liquid nitrogen frozen in advance to jujube, then carries out liquid nitrogen frozen crushing, obtains small ultra-fine of granularity
Jujube powder, in this process, including broken wall occurs for the higher fructus corni of essential oil content and jujube core, the cell of entire jujube, in this way
It is just more favorable for during subsequent extracted, essential oil substance is diffused into solvent, greatly improves extraction of essential oil rate.It is molten to jujube essential oil
Liquid carries out heating, vacuum distillation, can reduce vapo(u)rizing temperature, and reduce contact of the air with solution, avoid jujube to a certain extent
The Oxidative inactivation of active ingredient in essential oil, to keep the medical value of jujube essential oil.
Other features and advantages of the present invention will be described in detail in subsequent specific embodiment part.
Description of the drawings
Exemplary embodiment of the invention is described in more detail in conjunction with the accompanying drawings, it is of the invention above-mentioned and its
Its purpose, feature and advantage will be apparent, wherein in exemplary embodiment of the invention, identical reference label
Typically represent same parts.
Fig. 1 shows the flow chart of the method for jujube extraction essential oil according to the present invention.
Fig. 2 shows the equipment drawings of vacuum distillation.
Specific implementation mode
The preferred embodiment of the present invention is more fully described below with reference to accompanying drawings.Although showing the present invention in attached drawing
Preferred embodiment, however, it is to be appreciated that may be realized in various forms the present invention without the embodiment party that should be illustrated here
Formula is limited.
Referring to Fig.1, the method for jujube extraction essential oil according to the present invention includes step：(1) jujube is immersed in liquid nitrogen, it is cold
But, super cold jujube is obtained；(2) the super cold jujube is subjected to liquid nitrogen frozen pulverization process, obtains super cold jujube powder；(3) will
The super cold jujube powder carries out frozen dried, obtains super cold extra dry red wine date powder end；(4) it by the super cold extra dry red wine date powder end, carries out
Soxhlet extraction obtains jujube essential oil solution；(5) the jujube essential oil solution is evaporated in vacuo, obtains jujube essential oil.
In the method that jujube according to the present invention extracts essential oil, the jujube is the red of fresh jujube or naturally dry
Jujube.
In the method that jujube according to the present invention extracts essential oil, by jujube immerse the time cooling in liquid nitrogen be 10~
30min
In the method that jujube according to the present invention extracts essential oil, the process of the liquid nitrogen frozen pulverization process is：It is described
Super cold jujube puts into pulverizing chamber by the feed bin of liquid nitrogen frozen pulverizer, and the temperature for adjusting pulverizing chamber is -190~-100 DEG C, powder
It broken 0.5~2 hour, is sieved, collects.
In the method that jujube according to the present invention extracts essential oil, the process of the frozen dried is：Freeze drying box is cooled down
After to -50~-20 DEG C, the super cold jujube powder is fitted into glass dish, is positioned in freeze drying box；It is evacuated to vacuum degree
0.7~1MPa is kept for 5~10 hours；40~50 DEG C are heated to, and is kept for 5~8 hours；Restore to normal pressure, taking-up obtains super cold
Extra dry red wine date powder end.
In the method that jujube according to the present invention extracts essential oil, the process of the Soxhlet extraction is：It will be described super cold dry
Jujube powder is placed in cylindrical filtration paper cylinder, is put into the extraction tube of Soxhlet extractor jointly；In carrying for the Soxhlet extractor
It takes and is put into ethyl alcohol in bottle, ethyl alcohol is 1 with the super cold extra dry red wine date powder end mass ratio:1~15；The Soxhlet extractor is opened, is carried
It is 3~5 hours to take the time.
In the method that jujube according to the present invention extracts essential oil, the extraction tube of the Soxhlet extractor receives microwave spoke
According to in ul-trasonic irradiation one kind or combination.
In the method that jujube according to the present invention extracts essential oil, with reference to Fig. 2, the process of the vacuum distillation is：By institute
It states jujube essential oil solution to be placed in beaker, be positioned in the babinet of vacuum drying chamber；The gas cylinder of inert gas is connected by pipeline
The air intake valve for leading to the vacuum drying chamber, opens the valve of the gas cylinder, adjusts the output valve of decompression table, keeps output pressure
For 0.1~0.2MPa；Vacuum pump is opened, vacuum is extracted, adjusts air intake valve, keeps 0.4~0.75Mpa of vacuum degree；Setting institute
The temperature for stating vacuum drying chamber is 55~75 DEG C, and the jujube essential oil solution is kept to be in slight boiling condition；After distillation, close
Vacuum pump restores pressure in babinet and closes gas cylinder valve to normal pressure after the babinet cooled to room temperature of vacuum drying chamber,
Beaker is taken out, closed preservation obtains jujube essential oil.
In the method that jujube according to the present invention extracts essential oil, the inert gas is one kind in argon gas and nitrogen.
Hereinafter, the method for extracting essential oil to the jujube of the present invention in conjunction with specific embodiments illustrates.
Embodiment 1
(1) liquid nitrogen cools down：Fresh jujube is immersed in liquid nitrogen, cooling time, 10min, obtained super cold jujube.
(2) liquid nitrogen frozen crushes：Super cold jujube is put into pulverizing chamber by the feed bin of liquid nitrogen frozen pulverizer, adjusts and crushes
The temperature of room is -100 DEG C, is crushed 0.5 hour, is sieved, and collects, obtains super cold jujube powder.
(3) it is lyophilized：After freeze drying box is cooled to -50 DEG C, super cold jujube powder is fitted into glass dish, freeze drying box is positioned over
In；It is evacuated to vacuum degree 0.7MPa, is kept for 5 hours；40 DEG C are heated to, and is kept for 5 hours；Restore to normal pressure, taking-up obtains
Super cold extra dry red wine date powder end.
(4) Soxhlet extraction：Super cold extra dry red wine date powder end is placed in cylindrical filtration paper cylinder, is put into carrying for Soxhlet extractor jointly
It takes in pipe, wherein extraction tube receives microwave irradiation；Ethyl alcohol, ethyl alcohol and super cold extra dry red wine jujube are put into the extraction flask of Soxhlet extractor
Powder quality ratio is 1:1；Soxhlet extractor is opened, extraction time is 3 hours, obtains jujube essential oil solution.
(5) it is evaporated in vacuo：Jujube essential oil solution is placed in beaker, is positioned in the babinet of vacuum drying chamber；By argon gas
Gas cylinder the air intake valve of the vacuum drying chamber is connected to by pipeline, open the valve of gas cylinder, adjust the delivery valve of decompression table
Door, it is 0.1MPa to keep output pressure；Vacuum pump is opened, vacuum is extracted, adjusts air intake valve, keeps vacuum degree 0.4Mpa；Setting
The temperature of vacuum drying chamber is 55 DEG C, and jujube essential oil solution is kept to be in slight boiling condition；After distillation, vacuum pump is closed, is waited for
After the babinet cooled to room temperature of vacuum drying chamber, restores pressure in babinet and closes gas cylinder valve to normal pressure, take out beaker,
Closed preservation obtains jujube essential oil.
Embodiment 2
(1) liquid nitrogen cools down：The jujube of naturally dry is immersed in liquid nitrogen, cooling time, 30min, obtained super cold jujube.
(2) liquid nitrogen frozen crushes：Super cold jujube is put into pulverizing chamber by the feed bin of liquid nitrogen frozen pulverizer, adjusts and crushes
The temperature of room is -190 DEG C, is crushed 2 hours, is sieved, and collects, obtains super cold jujube powder.
(3) it is lyophilized：After freeze drying box is cooled to -20 DEG C, super cold jujube powder is fitted into glass dish, freeze drying box is positioned over
In；It is evacuated to vacuum degree 1MPa, is kept for 10 hours；50 DEG C are heated to, and is kept for 8 hours；Restore to normal pressure, taking-up is surpassed
Cold extra dry red wine date powder end.
(4) Soxhlet extraction：Super cold extra dry red wine date powder end is placed in cylindrical filtration paper cylinder, is put into carrying for Soxhlet extractor jointly
It takes in pipe, wherein extraction tube receives microwave irradiation；Ethyl alcohol, ethyl alcohol and super cold extra dry red wine jujube are put into the extraction flask of Soxhlet extractor
Powder quality ratio is 1:15；Soxhlet extractor is opened, extraction time is 5 hours, obtains jujube essential oil solution.
(5) it is evaporated in vacuo：Jujube essential oil solution is placed in beaker, is positioned in the babinet of vacuum drying chamber；By nitrogen
Gas cylinder the air intake valve of the vacuum drying chamber is connected to by pipeline, open the valve of gas cylinder, adjust the delivery valve of decompression table
Door, it is 0.2MPa to keep output pressure；Vacuum pump is opened, vacuum is extracted, adjusts air intake valve, keeps vacuum degree 0.75Mpa；Setting
The temperature of vacuum drying chamber is 75 DEG C, and jujube essential oil solution is kept to be in slight boiling condition；After distillation, vacuum pump is closed, is waited for
After the babinet cooled to room temperature of vacuum drying chamber, restores pressure in babinet and closes gas cylinder valve to normal pressure, take out beaker,
Closed preservation obtains jujube essential oil.
Embodiment 3
(1) liquid nitrogen cools down：Fresh jujube is immersed in liquid nitrogen, cooling time, 20min, obtained super cold jujube.
(2) liquid nitrogen frozen crushes：Super cold jujube is put into pulverizing chamber by the feed bin of liquid nitrogen frozen pulverizer, adjusts and crushes
The temperature of room is -150 DEG C, is crushed 1 hour, is sieved, and collects, obtains super cold jujube powder.
(3) it is lyophilized：After freeze drying box is cooled to -30 DEG C, super cold jujube powder is fitted into glass dish, freeze drying box is positioned over
In；It is evacuated to vacuum degree 0.8MPa, is kept for 8 hours；45 DEG C are heated to, and is kept for 6.5 hours；Restore to normal pressure, takes out
To super cold extra dry red wine date powder end.
(4) Soxhlet extraction：Super cold extra dry red wine date powder end is placed in cylindrical filtration paper cylinder, is put into carrying for Soxhlet extractor jointly
It takes in pipe, wherein extraction tube receives ul-trasonic irradiation；Ethyl alcohol, ethyl alcohol and super cold extra dry red wine are put into the extraction flask of Soxhlet extractor
Date powder end mass ratio is 1:8；Soxhlet extractor is opened, extraction time is 4 hours, obtains jujube essential oil solution.
(5) it is evaporated in vacuo：Jujube essential oil solution is placed in beaker, is positioned in the babinet of vacuum drying chamber；By argon gas
Gas cylinder the air intake valve of the vacuum drying chamber is connected to by pipeline, open the valve of gas cylinder, adjust the delivery valve of decompression table
Door, it is 0.15MPa to keep output pressure；Vacuum pump is opened, vacuum is extracted, adjusts air intake valve, keeps vacuum degree 0.6Mpa；Setting
The temperature of vacuum drying chamber is 65 DEG C, and jujube essential oil solution is kept to be in slight boiling condition；After distillation, vacuum pump is closed, is waited for
After the babinet cooled to room temperature of vacuum drying chamber, restores pressure in babinet and closes gas cylinder valve to normal pressure, take out beaker,
Closed preservation obtains jujube essential oil.
Comparative example 1
The step of jujube is crushed and is lyophilized without liquid nitrogen cooling, liquid nitrogen frozen, other are same as Example 3.
Comparative example 2
In addition to jujube essential oil is distilled in the natural environment, outer without being evaporated in vacuo, other are same as Example 3.
Performance test
1, the quality of jujube essential oil of weighing and the quality of jujube calculate extraction of essential oil rate
Extraction of essential oil rate=(quality of quality/jujube of jujube essential oil) × 100%
2, whether the fragrance of sensory evaluation essential oil and fragrance are strong.
Performance comparison table
| Embodiment | Extraction of essential oil rate/% | Characteristic perfume |
| Embodiment 1 | 18 | Have, it is dense |
| Embodiment 2 | 19 | Have, it is dense |
| Embodiment 3 | 20 | Have, it is dense |
| Comparative example 1 | 4 | Have, it is light |
| Comparative example 2 | 7 | Nothing |
Jujube essential oil prepared by the present invention is used it can be seen from the above embodiments that, and relative contrast's example is carried with essential oil
Take rate high, the dense advantage of characteristic perfume, under the premise of not reducing jujube essential oil quality, can make full use of jujube jujube core,
Fructus corni and jujube meat, greatly improve the recovery rate of essential oil.
Various embodiments of the present invention are described above, above description is exemplary, and non-exclusive, and
It is not limited to disclosed each embodiment.Without departing from the scope and spirit of illustrated each embodiment, for this skill
Many modifications and changes will be apparent from for the those of ordinary skill in art field.
Claims (9)
1. a kind of method of jujube extraction essential oil, which is characterized in that including step：
(1) jujube is immersed in liquid nitrogen, it is cooling, obtain super cold jujube；
(2) the super cold jujube is subjected to liquid nitrogen frozen pulverization process, obtains super cold jujube powder；
(3) the super cold jujube powder is subjected to frozen dried, obtains super cold extra dry red wine date powder end；
(4) by the super cold extra dry red wine date powder end, Soxhlet extraction is carried out, jujube essential oil solution is obtained；
(5) the jujube essential oil solution is evaporated in vacuo, obtains jujube essential oil.
2. the method for jujube extraction essential oil as described in claim 1, which is characterized in that the jujube is for fresh jujube or certainly
The jujube so dried.
3. the method for jujube as described in claim 1 extraction essential oil, which is characterized in that when jujube is immersed cooling in liquid nitrogen
Between be 10~30min.
4. the method for jujube extraction essential oil as described in claim 1, which is characterized in that the mistake of the liquid nitrogen frozen pulverization process
Cheng Wei：The super cold jujube puts into pulverizing chamber by the feed bin of liquid nitrogen frozen pulverizer, adjust pulverizing chamber temperature be -190~-
It 100 DEG C, crushes 0.5~2 hour, is sieved, collect.
5. the method for jujube as described in claim 1 extraction essential oil, which is characterized in that the process of the frozen dried is：It will
After freeze drying box is cooled to -50~-20 DEG C, the super cold jujube powder is fitted into glass dish, is positioned in freeze drying box；It vacuumizes
To 0.7~1MPa of vacuum degree, kept for 5~10 hours；40~50 DEG C are heated to, and is kept for 5~8 hours；Restore to normal pressure, takes out
Obtain super cold extra dry red wine date powder end.
6. the method for jujube as described in claim 1 extraction essential oil, which is characterized in that the process of the Soxhlet extraction is：It will
The super cold extra dry red wine date powder end is placed in cylindrical filtration paper cylinder, is put into the extraction tube of Soxhlet extractor jointly；In the Soxhlet
Ethyl alcohol is put into the extraction flask of extractor, ethyl alcohol is 1 with the super cold extra dry red wine date powder end mass ratio:1~15；Open the Soxhlet
Extractor, extraction time are 3~5 hours.
7. the method for jujube extraction essential oil as claimed in claim 6, which is characterized in that the extraction tube of the Soxhlet extractor,
Receive one kind in microwave irradiation and ul-trasonic irradiation or combination.
8. the method for jujube as described in claim 1 extraction essential oil, which is characterized in that the process of the vacuum distillation is：It will
The jujube essential oil solution is placed in beaker, is positioned in the babinet of vacuum drying chamber；The gas cylinder of inert gas is passed through into pipeline
It is connected to the air intake valve of the vacuum drying chamber, opens the valve of the gas cylinder, adjusts the output valve of decompression table, keeps output
Pressure is 0.1~0.2MPa；Vacuum pump is opened, vacuum is extracted, adjusts air intake valve, keeps 0.4~0.75Mpa of vacuum degree；Setting
The temperature of the vacuum drying chamber is 55~75 DEG C, and the jujube essential oil solution is kept to be in slight boiling condition；After distillation, close
Vacuum pump is closed, after the babinet cooled to room temperature of vacuum drying chamber, restores pressure in babinet and closes bottle valve to normal pressure
Door, takes out beaker, and closed preservation obtains jujube essential oil.
9. the method for jujube extraction essential oil as claimed in claim 8, which is characterized in that the inert gas is argon gas and nitrogen
In one kind.
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| CN112877138A (en) * | 2021-03-03 | 2021-06-01 | 郑州市鑫磊香料有限公司 | Red date absolute oil purification equipment and process |
| CN112877138B (en) * | 2021-03-03 | 2024-01-30 | 郑州市鑫磊香料有限公司 | Equipment and process for purifying red date absolute oil |
| CN113930288A (en) * | 2021-09-17 | 2022-01-14 | 广东石油化工学院 | Exocarpium citri grandis essential oil and application thereof in vehicle-mounted refreshing aroma |
| CN114644960A (en) * | 2022-03-23 | 2022-06-21 | 宝爵生物科技(广州)有限公司 | Plant essential oil and preparation method thereof |
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