JPH066028B2 - Extraction method of flavor components - Google Patents

Description

TECHNICAL FIELD The present invention relates to a method for extracting a flavor component from a palatable beverage material using a fluid in a supercritical state or in the vicinity thereof.

(Prior Art) An extraction method using a fluid in a supercritical state is capable of easily separating components that are difficult to be separated by an ordinary extraction method, and slightly changing the temperature or pressure of the extraction fluid after extraction. It has many advantages such as the ability to separate the components extracted by, and the low energy cost, and is widely practiced.

JP-A-47-28172 describes a method for extracting a volatile aroma component from water-humidified tea or coffee with liquid or gaseous carbon dioxide, but does not describe extraction in a supercritical state. Neither is there any mention of extraction in the presence of organic solvents. Japanese Patent Publication No. 59-10775 describes a method for extracting caffeine from black tea moistened with water using carbon dioxide in a supercritical state, but does not describe extraction in the presence of an organic solvent. Japanese Patent Publication No. 54-10539 describes extraction of organic substances with a supercritical gas.
1-333185 describes extraction of aroma components from coarsely crushed roasted coffee with carbon dioxide in a supercritical state, and Japanese Examined Patent Publication No.45-8624 discloses that coffee, tea, etc. can be extracted using a solvent in a supercritical state. A method for extracting volatile aroma components is described, but none of them describes extraction in the presence of an organic solvent.

These prior art methods have the above-mentioned characteristics as compared with the conventional methods that do not use the supercritical state, but they are still insufficient in terms of extraction efficiency.

(Problems to be Solved by the Invention) The present invention relates to a method for extracting a flavor component in a palatable beverage material using a fluid in a supercritical state or a state in the vicinity thereof,
It provides a method that can be extracted significantly more efficiently than prior art methods.

(Means for Solving Problems) The above problem is in a method of extracting a flavor component (flavor) in a palatable beverage material by bringing a fluid in a supercritical state or a nearby state into contact with a palatability beverage material. The method is characterized in that the contact is carried out in the presence of an organic solvent which is non-toxic and can dissolve the flavor component.

The extraction method of the present invention can be carried out in much the same manner as the prior art methods using supercritical fluids. FIG. 1 shows a schematic flow sheet. In this figure, the extractant,
For example, carbon dioxide is transferred to its storage tank 1 or liquefaction tank 2,
Here, it is cooled and liquefied. The liquefied extractant is temporarily stored in the intermediate tank 3 as needed, pressurized to a pressure higher than the critical pressure by the pump 4, and adjusted to a temperature higher than the critical temperature by the heat exchanger 5. The extractant fluid thus brought into the supercritical state is supplied to the extraction tank 6. Extraction tank 6
In order to extract, materials such as roasted coffee and black tea are charged together with an organic solvent such as an aqueous ethanol solution. In the presence of this organic solvent, the material and the fluid in the critical state are brought into contact with each other to perform extraction. An extract mainly composed of an oil component (oil) and a flavor component (flavor), and an organic solvent (these are collectively called a crude extract)
The extractant fluid containing is sent from the extraction tank 6 to the pressure control valve 7, and the pressure is reduced. Due to this pressure decrease, the extract and the organic solvent (crude extract) in the separation tank 8
Becomes liquid and separates. The extractant is ground in the liquefaction tank 2 and reused. On the other hand, the extract and the organic solvent are used in the extract tank 9
Which is used as a product, or after which the extract (product) and the organic solvent are separated (not shown in the figure), the organic solvent is purified if necessary, and then reused in the extraction tank 6. It

The method of this invention is used to extract its flavor components from palatable beverage ingredients. Examples of the palatable beverages include black tea, coffee, green tea, oolong tea, houjicha, barley tea, scented tea, and puer tea. As the extraction material of these beverages, for example, leaf tea and roasted coffee can be used for tea and coffee. These are preferably used in the form of small pieces, small particles or powder in order to increase the contact area with the extraction fluid and enhance the extraction efficiency. Both dry and wet materials can be used in the present invention.

The extractant used in the supercritical state or in the vicinity thereof may be one that has a relatively low critical temperature and does not substantially change the flavor component when it comes into contact with the flavor component in the critical state. Examples of the extractant include carbon dioxide (critical temperature 31.6 ° C .; critical pressure 74.3 atm), ethylene (9.2 ° C .; 49.7 atm), ethane (3
2.2 ° C; 48.2 atm), propylene (91.8 ° C;
45.6 atm), propane (96.6 ° C .; 41.9 atm) and the like. Of these, carbon dioxide is most preferable because it has a relatively low critical temperature and is not toxic to the human body.

These extractants are used in a supercritical state or a state in the vicinity thereof (critical state or subcritical state). The supercritical state means, for example, a state in which carbon dioxide has a temperature higher than 31.6 ° C. and higher than 74.3 atm,
The state in the vicinity of the supercritical state means, for example, a state in which the pressure is higher than the critical pressure and the temperature is approximately 25 ° C to 31.6 ° C. Even in such a state, the same extraction effect as in the supercritical state can be obtained.

To obtain high extraction efficiency of flavor components, 30% by volume
It is preferable to allow an aqueous ethanol solution having a water content of 70% to 70% by volume (water content of 30%) to exist in the extraction tank.
In order to make ethanol having such a concentration exist in the extraction tank, when a dry material is used as the extraction material, ethanol having the above concentration range may be used. When a wet material is used as the extraction material, it is preferable to use an alcohol aqueous solution having a slightly high concentration in consideration of its water content.

The amount of the organic solvent used depends on the type of extraction material, the type of extraction agent, etc., but is generally about 10 to 100 parts by weight, and preferably about 10 to 30 parts by weight per 100 parts by weight of the extraction material.
Parts by weight.

As a method of introducing the organic solvent into the extraction tank, for example, a method of separately putting the organic solvent and the extraction material into the extraction tank, a method of uniformly mixing the organic solvent and the extraction material in advance, and putting them into the extraction tank at once, extraction It is possible to use a method in which the extractant introduced into the tank is continuously injected and mixed at a constant rate.

The extractant extracted from the extraction tank is still in a supercritical state, or
It is in the vicinity thereof and is accompanied by an extract mainly composed of an oil component (oil) and a flavor component, and an organic solvent. This is an extract and an organic solvent (crude extract),
In order to separate the extractant from the extractant, a method commonly used for supercritical extraction, for example, a method of decreasing the pressure, a method of changing the temperature or the like can be used. When lowering the pressure, a pressure control valve is used, for example, the pressure is lowered below the critical pressure. The depressurized extractant is introduced into the separation tank, where the liquid crude extract and the gaseous extractant are separated, and the extractant is transported to the liquefaction tank for reuse.

The crude extract separated from the extractant is used as it is, or the organic solvent is removed and used as an extract. This extract, which is mainly composed of an oil component (oil) and a flavor component (flavor), usually does not need to be separated.
For example, when ethanol is used as the organic solvent, ethanol has no toxicity, so it is convenient to use it in the state of a crude extract without removing it. For example, a crude extract extracted from black tea is mixed with instant black tea, and then ethanol is evaporated and removed in a state where the flavor components are adsorbed to obtain instant black tea in which the flavor components are enriched.

(Effect of the Invention) In the method of the present invention, which is characterized by allowing an organic solvent to exist when performing extraction using a fluid in a supercritical state or a state in the vicinity thereof, compared with the supercritical extraction method of the prior art. The extraction speed of flavor and oil components is fast, and complete extraction can be performed within a short period of time. Moreover, various components including low and medium boiling point volatile components can be extracted, and high quality flavor components can be obtained. can get.

(Examples) Next, the present invention will be described in more detail with reference to Examples.

Example 1. (Reference Example) 20 g of 99.9% by volume (water content 0.1%) of ethanol was added to 100 g of Ceylon leaf tea, and the extractor for supercritical gas was filled with this. 40 ℃, 30
Extraction was carried out by passing carbon dioxide in a supercritical state of 0 atm at a rate of 50 to 60 g / min. As a control, extraction was performed under the same conditions as above, in the case of adding the same amount of water instead of the above ethanol and in the case of not adding it. For each test, the oil component contained in the black tea leaves was measured before and after extraction, and the amount of the extracted oil component was determined from the difference.
The results are shown in Table 1 below.

As shown in the above results, the addition of ethanol extracted about 3 times as much oil component as the conventional method with or without addition of water.

The crude extract (containing a flavor component, an oil component and ethanol) was collected at a time of 0 to 60 minutes and 60 to 360 minutes, and each sample was analyzed by gas chromatography to determine the quality of black tea among the flavor components. Peak areas corresponding to linalool and linalool oxide, which are important indexes for determination, were measured, and linalool and linalool oxide extracted from the total value and the amount of crude extract were calculated as arbitrary units. The results are shown in Table 2 below.

As is clear from the above results, when ethanol was added, about 60% of linalool and linalool oxide extracted in 6 hours was extracted in the first hour, and the extraction rate was extremely high. On the other hand, in the case of adding water, the extraction rate was slow, and the total extraction amount after 6 hours was also small.

The crude extract obtained in this example has a strong refreshing scent of green note, and when added to instant black tea, a remarkable addition effect occurs and the scent of instant black tea is remarkably improved.

Example 2. Extraction was performed in the same manner as in Example 1. However, Kenya black tea was used as the extraction material, and (A) (reference example) ethanol of 99.9% by volume (water content 0.1%) and (B) (example) 70% by volume (water content) as the organic solvent. An aqueous solution of 30% ethanol and an aqueous solution of (C) (Example) 50% by volume (water content 50%) were used. The results are shown in Table 3 below.

The amount of extracted oily matter did not differ greatly depending on the concentration of ethanol, but the amounts of linalool and linalool oxide extracted were very large in the 50-70% by volume aqueous ethanol solution.

Example 3. (Reference Example) 20 g of 99.9% by volume (water content 0.1%) of ethanol was added to 100 g of Ceylon leaf tea, and the extractor for supercritical gas was filled with this. 60 ℃, 30
Extraction was performed by passing supercritical carbon dioxide at 0 atm for 1 hour. The amount of flavor component was analyzed for the extracted crude extract. As a control, 100 g of Ceylon leaf tea to which 150 g of ethanol was added was heated to 60 ° C. with stirring in a flask equipped with a cooling tube and extracted for 1 hour. The same analysis was performed on the crude extract. The results are shown in Table 4.

The results of the gas chromatography of the crude extract obtained by the flask extraction showed only a few peaks in the high boiling point portion and almost no peaks other than ethanol in the low and medium boiling point portions. On the other hand, in the crude extract with supercritical gas,
An extremely wide variety of peaks were found evenly in the low, middle and high boiling points, and the latter was also organoleptically superior in that it had a refreshing green note scent. Further, the concentration of linalool and linalool oxide in the crude extract obtained by the flask extraction is extremely thin, and it cannot be used as a flavor unless the crude extract is further concentrated.

Example 4. (Reference Example) 20 g of 99.9% by volume (water content 0.1%) ethanol was added to 100 g of Ceylon leaf tea, and this was filled in a supercritical gas extraction apparatus. This extractor is operated at 30 ℃, 150
Extraction was carried out by passing subcritical carbon dioxide at atmospheric pressure for 1 hour. 17 g of crude extract was obtained. 48% of the oil component in the raw black tea leaves was extracted into this crude extract.
The amount of linalool and linalool oxide was 95. (100 linalool and linalool oxide extracted with 99.9% ethanol in Example 1 were used.
As Example 5 (Reference Example) 10 g of 99.9% by volume (water content 0.1%) of ethanol was added to 100 g of Ceylon leaf tea, and this was filled in a supercritical gas extraction apparatus. This extractor is 40 ℃, 300
Extraction was performed by passing supercritical carbon dioxide at atmospheric pressure for 5 hours. 8 g of crude extract was obtained. The amount of linalool and linalool oxide was 77. (Based on linalool and linalool oxide extracted with 99.9% ethanol in Example 1 as 100) Example 6. In 100 g of ground roasted coffee, 99.9% by volume (water content 0.1%) (reference example), 50% by volume (water content 50%)
(Example) and 20 g of an aqueous ethanol solution of 5% by volume (water content 95%) (Reference Example) were added, and each was filled in an extraction device for supercritical gas. Extraction was carried out by passing carbon dioxide in a supercritical state at 40 ° C. and 30 atm. As a control, extraction was carried out under the same conditions as above, even when 20 g of water was added instead of the aqueous ethanol solution and when no water was added. The amount of oil component in the roasted coffee before and after extraction was measured, and the difference was determined as the amount of extracted oil component. Moreover, the amount of the flavor component is analyzed by gas chromatography,
Of the peaks obtained by the analysis under the same conditions, the peak areas of all flavor components except ethanol were measured, and the flavor component amount extracted from the total value and the crude extract amount was calculated as an arbitrary unit. The results are shown in Table 5 below.

There was no difference in the amount of the extracted oil component between the case of adding water and the case of adding the aqueous ethanol solution, but the amount of flavor components extracted was higher when the aqueous ethanol solution was added than when water was added. Obviously there were many. Further, of the aqueous ethanol solutions used in this example, the amount of the flavor component extracted was the largest when 50% ethanol was used, and this result was in good agreement with the result of Example 2.

In addition, in the case of 50% ethanol addition (Example), water addition (Reference Example), and no addition (Reference Example), the crude extract was collected by dividing into 0 to 60 minutes and 60 to 300 minutes, and extracted. The change of the amount with time was observed. The results are shown in Table 6 below.

As is clear from this result, when the 50% by volume aqueous ethanol solution was added, not only the total amount of the flavor components extracted but also the extraction speed were obviously higher than those in the case of adding water and the case of not adding water. .

Example 7. Reference Example 10 g of 99.9% by volume (water content 0.1%) of ethanol was added to 100 g of crushed and roasted coffee, and this was filled in a supercritical gas extraction apparatus. 40 ℃, 50 in this filling device
Extraction was carried out by passing supercritical carbon dioxide at 0 atm for 6 hours. 22 g of crude extract was obtained. All of the oil components in the raw coffee have been extracted into this crude extract. The amount of flavor component was 591 (99.9% in Table 5).
The amount of flavor component extracted by adding ethanol was set to 100).

Example 8. (Example) 50 volume% (water content 5
100 g of 0% aqueous ethanol solution was added, and this was filled in a supercritical gas extraction apparatus. 40 ℃, 3
Extraction was carried out by passing supercritical carbon dioxide at 00 atm for 5 hours. 56 g of crude extract was obtained. All of the oil components in the raw coffee have been extracted into this crude extract. The amount of flavor component was 237. (In Table 5, 99.
The amount of the flavor component extracted by adding 9% ethanol was set to 100).

Example 9. (Example) 50 volume% (water content 5
30 g of 0% aqueous ethanol solution was added, and this was filled in the supercritical gas extraction apparatus. 40 ℃, 30
Extraction was performed by passing supercritical carbon dioxide at 0 atm for 1 hour. 20 g of crude extract was obtained. In this crude extract, 76% of the oil component in the raw coffee has been extracted. The amount of the flavor component was 180 (99.9% in Table 5).
The amount of flavor component extracted by adding ethanol was set to 100).

Example 10. (Example) 30% by volume (water content 7
20 g of 0%) aqueous ethanol solution was added, and this was filled in a supercritical gas extraction apparatus. 40 ℃, 30
Extraction was performed by passing supercritical carbon dioxide at 0 atm for 1 hour. 9 g of crude extract was obtained. In this crude extract, 65% of the oil component in the raw coffee has been extracted. The amount of flavor component was 118 (99.9% in Table 5)
The amount of flavor component extracted by adding ethanol was set to 100).

[Brief description of drawings]

FIG. 1 shows one of the devices used in the method of the invention.
It is an example flow sheet. In the figure, 1 is an extractant storage tank, 2 is a liquefaction tank, 3 is an intermediate tank, 4 is a pump, 5 is a heat exchanger, 6 is an extraction tank, 7 is a pressure control valve, 8 is a separation tank, and 9 is an extract tank. Show.

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Claims (2)

[Claims] 1. A method of extracting a flavor component in a palatable beverage material by bringing a fluid in a supercritical state or in the vicinity thereof into contact with a palatability beverage material, wherein the contacting is performed with an aqueous ethanol solution of 30 to 70% by volume. A method characterized by being carried out in the presence of. 2. The method according to claim 1, wherein the palatable beverage material is leaf tea, green tea, roasted coffee, oolong tea, hoji tea, barley tea, fragrant tea, or puer tea.