CN109609273A - The preparation method of coffee essential oil - Google Patents
The preparation method of coffee essential oil Download PDFInfo
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- CN109609273A CN109609273A CN201811520138.9A CN201811520138A CN109609273A CN 109609273 A CN109609273 A CN 109609273A CN 201811520138 A CN201811520138 A CN 201811520138A CN 109609273 A CN109609273 A CN 109609273A
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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
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- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
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- Organic Chemistry (AREA)
- Tea And Coffee (AREA)
- Fats And Perfumes (AREA)
Abstract
The present invention relates to food Primary processing technology field more particularly to the preparation methods of coffee essential oil.In coffee essential oil preparation method provided by the invention, ground coffee carries out supercritical CO2Using pressurization Dynamic Separation after extraction, this method can save the time compared with the existing technology, and simple process, strong operability；Recovery rate is significantly increased, and active constituent content is high.
Description
Technical field
The present invention relates to food Primary processing technology field more particularly to the preparation methods of coffee essential oil.
Background technique
Coffee is one of big beverage in the world three, is widely distributed in the torrid zone and subtropical zone within 25 ° of north and south latitude, at present
There is a countries and regions plantation coffee more than 80.Coffee is mainly planted in the ground such as Yunnan, Hainan in China, is that its important torrid zone is special
Color agricultural product.It bakes in coffee containing about 10% essential oil, containing a large amount of coffee aromatic odor component itself, and has preferable
Health-care effect, therefore coffee essential oil can be applied to food, cosmetics and medicine etc..
Plants essential oil, which extracts, at present mostly uses greatly steam distillation, organic solvent extraction, supercritical CO2Extraction
The shortcomings that there are recovery rates is lower, time-consuming Deng, steam distillation, essential oil difficult collection；Organic solvent extractionprocess exists time-consuming, no
It easily cleans, disadvantage at high cost and poor safety, often impurity is more in essential oil, and use scope is narrow.And existing super face
Boundary CO2Extraction is that have the shortcomings that time-consuming, recovery rate is low.
Supercritical CO2Extraction is to utilize its high osmosis and high dissolution using the carbon dioxide under supercriticality as solvent
Ability extracts the process of separating mixture, and the carbon dioxide under supercriticality, density significantly increases, cause to solute
The increase of solubility declines the density of solvent often through reduction pressure in lock out operation, its is caused to dissolve physical capacity
Decline, extract can be made to separate with solvent.But conventional Supercritical CO2The parameter of extraction is not suitable for the extraction of coffee essential oil, makes
At extraction efficiency wretched insufficiency, therefore, the supercritical CO of coffee essential oil is further studied2Extraction method is still the hot spot of this field.
Summary of the invention
In view of this, this method obtains the technical problem to be solved in the present invention is that providing the preparation method of coffee essential oil
Volatile flavor components content is more in essential oil, and recovery rate is high；And the time can be saved, and simple process, strong operability.
Coffee essential oil preparation method provided by the invention, comprising:
Ground coffee is subjected to supercritical CO2Essential oil is collected after extraction,
Extraction conditions are as follows: 25MPa~35Mpa, 50 DEG C~70 DEG C extract 30min~60min；
Collect the condition of essential oil are as follows: 35MPa~40Mpa collects 8min~15min.
Extracting process provided by the invention is in supercritical CO2It is carried out in extraction equipment, in setup parameter, temperature has two
A, one is temperature inside extraction kettle, i.e. extraction temperature, and extraction temperature is 50 DEG C~70 DEG C in the present invention program, another
A is the temperature of the cabinet where extraction kettle, i.e. the temperature of kettle temperature case, and spin manifold temperature is higher than the temperature inside extraction kettle, is set as
80 DEG C~100 DEG C.
Fresh coffee beans are subjected to baking processing using baking device, ground coffee face is measured using Agtron caramelization analyzer
Color, in the present invention, the color difference of the ground coffee is 55~70；The coffee bean surface chromatic aberration for preparing the ground coffee is 45~65.
Require to roast beans surface smooth, corrugationless phenomenon simultaneously.In some embodiments, baking and banking up with earth coffee bean surface chromatic aberration is 55, and coffee is ground
Ground coffee color difference is 60 after mill；In other embodiments, baking and banking up with earth coffee bean surface chromatic aberration is 45, ground coffee color difference after Coffee Grinding
It is 55；In other embodiments, baking and banking up with earth coffee bean surface chromatic aberration is 65, and ground coffee color difference is 70 after Coffee Grinding.
The coffee bean grinding that will be baked and banked up with earth is crushed coffee bean using pulverizer, in the present invention, the granularity of the ground coffee
For 20 mesh~40 mesh.In some embodiments, the granularity of the ground coffee is 30 mesh, 20 mesh, 40 mesh.
Supercritical CO2The process of extraction is by extracting and separating made of two processes combine.The extraction is in extraction kettle
Middle progress, does not add entrainer, and ground coffee is put into extraction kettle, in the supercritical state, CO2As supercritical fluid and coffee
Powder contact is extracted in turn it selectively the ingredient of polarity size, boiling point height and molecular size range.Existing skill
In art, the separating step usually makes supercritical fluid become common gases by the method for decompression, heating, and extracted substance is then
It is completely or almost completely precipitated, to achieve the purpose that separation.Since in extraction process, pressure is significantly larger than big in extraction kettle
Air pressure, therefore, extraction time, which terminates to open, collects valve, will make CO2It is rapidly gone out out of extraction kettle, while taking CO out of2In fluid
Extracting substance, but due to rapid pressure drop in kettle, intracellular CO2Fluid gasifies rapidly, prevents in cell essential oil from fine
It is precipitated.Studies have shown that the mode of decompression separation is difficult to realize the high efficiency extraction of coffee essential oil, so the application is using pressurization dynamic
Isolated method is separated and is collected to coffee essential oil.Namely continue charged air induction after this extraction kettle valve opening,
Holding and adherence pressure, to make coffee essential oil with CO2Fluid is precipitated from rigidifying cell wall, then with CO2Fluid takes extraction out of
Kettle.In the present invention, dynamic rate of pressurization is 2~5Mpa/min after extraction.
In some embodiments, the extraction conditions are as follows: 28Mpa, 62 DEG C extract 45min；The condition for collecting essential oil
Are as follows: 38Mpa collects 12min.
In some embodiments, the extraction conditions are as follows: 35Mpa, 50 DEG C extract 30min；The condition for collecting essential oil
Are as follows: 35Mpa collects 15min.
In some embodiments, the extraction conditions are as follows: 25Mpa, 70 DEG C extract 60min；The condition for collecting essential oil
Are as follows: 40Mpa collects 8min.
The method for the pressurization Dynamic Separation that the present invention uses specifically includes: to the end of ground coffee extraction time, by extraction kettle
Pressure is slowly increased to 35MPa~40Mpa, opens simultaneously collection valve and starts to collect coffee essential oil, makes to enter extraction kettle CO2It is more than
Discharge CO2, coffee essential oil is made to follow CO2Rigid cell wall structure is discharged in fluid, then with CO2Extraction kettle is discharged in fluid, collects knot
Beam sealing is spare.
Extracting method of the invention is determined by the design feature of baking coffee, has specific aim.Baking ground coffee is
Closely knit, porous honeycomb structure.Coffee bean during roasting cell wall due to high temperature action occur glass transition become rigid
Property structural form, therefore general extraction methods extraction effect is bad, and supercritical CO2Extraction can make CO due to pressure2Stream
Body is penetrated into well in the cell wall rigid structure of coffee；Conventional overcritical separation phase is static decompression process, experiment card
Bright static decompression coffee extraction of essential oil rate is relatively low, and uses pressurization Dynamic Separation method, enable coffee essential oil preferably with
With CO2Fluid is discharged in the rigid structure of coffee, greatly improves the recovery rate of coffee essential oil.
In the present invention, the rate of the boosting is 2~5Mpa/min.Collect essential oil when collection port temperature be 90 DEG C~
130℃。
In the present invention, during the collection, CO2Rate into extraction kettle is 10~14L/min；CO2Release extraction
The initial rate of kettle is 8~10L/min, and pressurization dynamic collection terminates, and stops pressurization, and static state decompression is collected, and pressure is gradually reduced
Until CO2Release is complete.
Coffee essential oil made from preparation method of the present invention.
It in the coffee essential oil that preparation method of the present invention obtains, is detected through GC-MS, inspection arrives 56 kinds of aromatic substance altogether.
Since coffee essential oil produced by the present invention contains coffee aromatic odor itself, which be can be applied to
Food, cosmetics and medicine etc..
Include the food of coffee essential oil, drug and/or cosmetics made from preparation method of the present invention.
In the preparation method of coffee essential oil provided by the invention, ground coffee carries out supercritical CO2It is dynamic using pressurization after extraction
State separation, at least has the advantages that compared with prior art
(1) time is saved, and simple process, strong operability, conventional supercritical fluid CO2Extraction time is longer, pressurization dynamic
Extraction time is shorter, stablizes when pressure reaches setting and pressure, can carry out dynamic extraction separation coffee essential oil, extraction time can
It substantially reduces；
(2) recovery rate is high, and this method is based on supercritical CO2On the basis of depressurizing static extracting, static extracting is depressurized
Critical CO2Coffee cell wall rigid structure is discharged with gas form in fluid, and coffee essential oil discharge rate is low, causes coffee extraction of essential oil
Rate is lower；And being pressurized Dynamic Extraction is that slowly pressurization makes essential oil with CO in separation2The honeycomb structure of fluid discharge rigidity, significantly
Increase recovery rate.
(3) active constituent content is high, and the total separation of this method obtains 56 kinds of aromatic substances, and depressurizes static extracting and obtain 21
Kind aromatic substance, it is seen that for the essential oil that decompression static extracting obtains, the method for the present invention can obtain more fragrance
Substance, and harvesting effective component total amount is 2.8 times for depressurizing static separation method.
Detailed description of the invention
Fig. 1 shows the scanning electron microscope image for baking coffee.
Specific embodiment
The present invention provides the preparation method of coffee essential oil, those skilled in the art can use for reference present disclosure, suitably change
Into realization of process parameters.In particular, it should be pointed out that all similar substitutions and modifications are aobvious for a person skilled in the art
And be clear to, they are considered as being included in the present invention.Method and application of the invention is carried out by preferred embodiment
Description, related personnel can obviously not depart from the content of present invention, are being modified in spirit and scope to methods herein and application
Or appropriate changes and combinations, carry out implementation and application the technology of the present invention.
The test material that the present invention uses is all common commercially available product, can all be bought in market.
The present invention is tested using the prosperous coffee that is produced from Hainan, but method of the present invention is not limited to prosperous coffee
Coffee, the coffee of other kinds are all suitable for method provided by the invention.
Below with reference to embodiment, the present invention is further explained:
Embodiment 1
1, it bakes and banks up with earth: fresh coffee beans is subjected to baking processing using baking device, measured using Agtron caramelization analyzer
Ground coffee color, baking and banking up with earth coffee bean surface chromatic aberration is 55, and ground coffee color difference is 60 after Coffee Grinding, while requiring to roast beans surface
It is smooth, corrugationless phenomenon.
2, be milled: the coffee bean grinding that will be baked and banked up with earth is crushed coffee bean using pulverizer, and grinding particle size is 30 mesh.
3, extract: ground coffee is put into extraction kettle, and set extraction conditions: 62 DEG C of extraction temperature, 28MPa, kettle temperature are pressed in extraction
Box temperature degree is 90 DEG C, extraction time 45min.
4, it is pressurized Dynamic Separation: to the end of ground coffee extraction time, extraction kettle pressure being slowly increased to 38MPa, simultaneously
It opens collection valve to start to collect coffee essential oil, makes to enter extraction kettle CO2Slightly more than discharge CO2, accelerate to promote essential oil separation, pressurization
Acquisition time is 12min, and pressurization time to stopping pressurizeing, collect by static state decompression, and pressure is gradually reduced until CO2Release is complete,
Recovery rate reaches 4.2071%, and it is spare to collect end sealing.
Embodiment 2
The technical solution adopted in the present invention is specifically implemented according to the following steps:
1, it bakes and banks up with earth: fresh coffee beans is subjected to baking processing using baking device, measured using Agtron caramelization analyzer
Ground coffee color, baking and banking up with earth coffee bean surface chromatic aberration is 45, and ground coffee color difference is 58 after Coffee Grinding, while requiring to roast beans surface
It is smooth, corrugationless phenomenon.
2, be milled: the coffee bean grinding that will be baked and banked up with earth is crushed coffee bean using pulverizer, and grinding particle size is 20 mesh.
3, extract: ground coffee is put into extraction kettle, and set extraction conditions: 50 DEG C of extraction temperature, 35MPa, kettle temperature are pressed in extraction
Box temperature degree is 80 DEG C, extraction time 30min.
4, it is pressurized Dynamic Separation: to the end of ground coffee extraction time, extraction kettle pressure being slowly increased to 35MPa, simultaneously
It opens collection valve to start to collect coffee essential oil, makes to enter extraction kettle CO2Slightly more than discharge CO2, accelerate to promote essential oil separation, pressurization
Acquisition time is 15min, and pressurization time to stopping pressurizeing, collect by static state decompression, and pressure is gradually reduced until CO2Release is complete,
Recovery rate reaches 4.4189%, and it is spare to collect end sealing.
Embodiment 3
The technical solution adopted in the present invention is specifically implemented according to the following steps:
1, it bakes and banks up with earth: fresh coffee beans is subjected to baking processing using baking device, measured using Agtron caramelization analyzer
Ground coffee color, baking and banking up with earth coffee bean surface chromatic aberration is 65, and ground coffee color difference is 70 after Coffee Grinding, while requiring to roast beans surface
It is smooth, corrugationless phenomenon.
2, be milled: the coffee bean grinding that will be baked and banked up with earth is crushed coffee bean using pulverizer, and grinding particle size is 40 mesh.
3, extract: ground coffee is put into extraction kettle, and set extraction conditions: 70 DEG C of extraction temperature, 25MPa, kettle temperature are pressed in extraction
Box temperature degree is 100 DEG C, extraction time 60min.
4, it is pressurized Dynamic Separation: to the end of ground coffee extraction time, extraction kettle pressure being slowly increased to 40MPa, simultaneously
It opens collection valve to start to collect coffee essential oil, makes to enter extraction kettle CO2Slightly more than discharge CO2, accelerate to promote essential oil separation, pressurization
Acquisition time is 8min, and pressurization time to stopping pressurizeing, collect by static state decompression, and pressure is gradually reduced until CO2Release completely, mentions
It takes rate to reach 4.3482%, it is spare to collect end sealing.
Comparative example 1
1, it bakes and banks up with earth: fresh coffee beans is subjected to baking processing using baking device, measured using Agtron caramelization analyzer
Ground coffee color, baking and banking up with earth coffee bean surface chromatic aberration is 55, and ground coffee color difference is 60 after Coffee Grinding, while requiring to roast beans surface
It is smooth, corrugationless phenomenon.
2, be milled: the coffee bean grinding that will be baked and banked up with earth is crushed coffee bean using pulverizer, and grinding particle size is 30 mesh.
3, extract: ground coffee is put into extraction kettle, and set extraction conditions: 62 DEG C of extraction temperature, 28MPa, kettle temperature are pressed in extraction
Box temperature degree is 90 DEG C, extraction time 150min.
4, it depressurizes static extracting: opening and collect valve, deflate, collect essential oil, discharged by 8min carbon dioxide gas, collect
Terminate, seals spare.
Comparative example 2
The technical solution adopted in the present invention is specifically implemented according to the following steps:
1, it bakes and banks up with earth: fresh coffee beans is subjected to baking processing using baking device, measured using Agtron caramelization analyzer
Ground coffee color, baking and banking up with earth coffee bean surface chromatic aberration is 45, and ground coffee color difference is 58 after Coffee Grinding, while requiring to roast beans surface
It is smooth, corrugationless phenomenon.
2, be milled: the coffee bean grinding that will be baked and banked up with earth is crushed coffee bean using pulverizer, and grinding particle size is 20 mesh.
3, extract: ground coffee is put into extraction kettle, and set extraction conditions: 50 DEG C of extraction temperature, 35MPa, kettle temperature are pressed in extraction
Box temperature degree is 80 DEG C, extraction time 90min.
4, it depressurizes static extracting: opening and collect valve, deflate；Essential oil is collected, is discharged by 10min carbon dioxide gas, is received
Collection terminates, and seals spare.
Comparative example 3
The technical solution adopted in the present invention is specifically implemented according to the following steps:
1, it bakes and banks up with earth: fresh coffee beans is subjected to baking processing using baking device, measured using Agtron caramelization analyzer
Ground coffee color, baking and banking up with earth coffee bean surface chromatic aberration is 65, and ground coffee color difference is 70 after Coffee Grinding, while requiring to roast beans surface
It is smooth, corrugationless phenomenon.
2, be milled: the coffee bean grinding that will be baked and banked up with earth is crushed coffee bean using pulverizer, and grinding particle size is 40 mesh.
3, extract: ground coffee is put into extraction kettle, and set extraction conditions: 70 DEG C of extraction temperature, 25MPa, kettle temperature are pressed in extraction
Box temperature degree is 100 DEG C, extraction time 120min.
4, it depressurizes static extracting: opening and collect valve, deflate；Essential oil is collected, is discharged by 5min carbon dioxide gas, is collected
Terminate, seals spare.
Compliance test result
1, each embodiment, the extraction efficiency of comparative example are counted,
Statistical result such as table 1:
1 coffee extraction of essential oil efficiency comparative's table of table
The result shows that separated using pressurization dynamic extraction method, obtain the extraction efficiency of caffeol significantly greater than with
Static extracting is depressurized, which has extremely significant difference, p < 0.01 through statistical analysis.Meanwhile using pressurization dynamic extraction energy
The enough time for substantially shortening extraction, improve extraction efficiency.In all embodiments, the recovery rate highest of embodiment 2 is reachable
4.42%.
2, the extract of each embodiment, comparative example is counted
Coffee flavor component is demarcated using 3- octanol semiquantitative method, as a result such as table 2:
2 sapidity ingredient testing result of table (unit: mg/g)
Shown in table 2, it is total that the resulting aroma substance total amount of Examples 1 to 3 is significantly higher than the resulting aroma substance of comparative example 1
Amount, p < 0.05, about 2.8 times.The testing result to comparative example 1 of coffee essential oil made from other comparative examples is similar, all with implementation
There are significant difference, p < 0.05 for example 1~3.The testing result of coffee essential oil made from other embodiments is similar to Example 2,
But all not as good as embodiment 2.
The above is only the preferred embodiment of the present invention, it is noted that those skilled in the art are come
It says, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications also should be regarded as
Protection scope of the present invention.
Claims (10)
1. ground coffee is carried out supercritical CO by the preparation method of coffee essential oil2Essential oil is collected after extraction,
Extraction conditions are as follows: 25MPa~35Mpa, 50 DEG C~70 DEG C extract 30min~60min；
Collect the condition of essential oil are as follows: 35MPa~40Mpa collects 8min~15min.
2. preparation method according to claim 1, which is characterized in that the granularity of the ground coffee is 20 mesh~40 mesh.
3. preparation method according to claim 1 or 2, which is characterized in that the color difference of the ground coffee is 55~70；Preparation
The coffee bean surface chromatic aberration of the ground coffee is 45~65.
4. preparation method according to claim 1, which is characterized in that
The extraction conditions are as follows: 28Mpa, 62 DEG C extract 45min；
The condition for collecting essential oil are as follows: 38Mpa collects 12min.
5. preparation method according to claim 1, which is characterized in that
The extraction conditions are as follows: 35Mpa, 50 DEG C extract 30min；
The condition for collecting essential oil are as follows: 35Mpa collects 15min.
6. preparation method according to claim 1, which is characterized in that
The extraction conditions are as follows: 25Mpa, 70 DEG C extract 60min；
The condition for collecting essential oil are as follows: 40Mpa collects 8min.
7. described in any item preparation methods according to claim 1~6, which is characterized in that the rate boosted after extraction be 2~
5Mpa/min。
8. described in any item preparation methods according to claim 1~6, which is characterized in that the collection valve temperature for collecting essential oil is
90 DEG C~130 DEG C.
9. coffee essential oil made from the described in any item preparation methods of claim 1~6.
10. food, drug and/or makeup comprising coffee essential oil made from the described in any item preparation methods of claim 1~6
Product.
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Cited By (1)
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| CN111387327A (en) * | 2020-03-30 | 2020-07-10 | 黑龙江八一农垦大学 | Preparation method of green coffee oil |
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