TWI852600B - Production method of animal and plant extracts, and extracts - Google Patents

Abstract

The subject of this invention is to use natural plant and animal extracts from the conventional steam distillation method. Although it can bring a natural feel to beverages, it is not sufficient to give a unique aroma or a strong aroma with a trace amount of addition.

The solution of the present invention is a method for producing animal and plant extracts, which comprises the following steps (A) to (D): Step (A): Distilling the animal and plant raw materials with water vapor to obtain a distillate, Step (B): Making the pH of the distillate obtained in the aforementioned step (A) to be above 8.0, Step (C): Freezing the distillate with a pH above 8.0 obtained in the aforementioned step (B), Step (D): Thawing the distillate frozen in the aforementioned step (C).

By blending the plant and animal extracts obtained by the manufacturing method of the present invention into beverages, a unique flavor can be imparted to the beverages. In particular, by adding a trace amount of the green tea extract obtained by the manufacturing method of the present invention to green tea beverages, a tea beverage having a soft and full green odor of freshly brewed tea can be provided.

Description

Production method of animal and plant extracts, and extracts

The present invention relates to a method for producing animal and plant extracts, animal and plant extracts obtained by the aforementioned production method, and a method for producing food and beverages containing the animal and plant extracts obtained by the aforementioned production method.

Steam distillation has been known since ancient times as a method for obtaining the aroma components of natural animals and plants. In addition to being used for the collection of essential oils and the analysis of the aroma of natural products, it is also used in the production of animal and plant extracts with excellent aroma.

As a method for producing animal and plant extracts using a steam distillation method, for example, the following method is known.

For example, a method for preparing a steam-distilled coffee flavor, characterized in that in the method of steam-distilling the coffee flavor, condensed water containing the flavor is fractionated and collected, and the distillate rich in aroma components and less in acidity is used (Patent Document 1); a method for producing a tea flavor, characterized in that a distillate obtained by steam-distilling tea is brought into contact with tea leaves, and the hot distillation odor in the distillate is removed (Patent Document 2); a method for producing an extract for a favorite beverage, characterized in that a favorite beverage raw material is subjected to hot water extraction to recover the extract, and then the extract residue is steamed. A novel flavor comprising a flavor (A) obtained by steam distilling a raw material for a favorite beverage and a flavor (B) obtained by supplying the raw material for a favorite beverage to a gas-liquid countercurrent contact device, wherein the flavor (B) is contained in a range of 0.01 to 100 parts by mass per 1 part by mass of the flavor (A) (Patent Document 4); A green tea beverage packaged in a sealed container characterized by being blended with a distillate, wherein the distillate is obtained by distilling tea leaves of an evergreen tree of the Theaceae family (scientific name: Camellia sinensis (L) O. Kuntze) are picked and then frozen, and the frozen tea leaves are steam distilled to obtain a coffee extract (Patent Document 5); a method for producing a coffee extract, characterized in that the method comprises the following steps (1) to (5): (1) performing low-temperature extraction on roasted coffee beans at a temperature range of 0 to 30°C to obtain a low-temperature extract, (2) storing the low-temperature extract obtained in step (1) at a temperature range of 0 to 30°C, (3) performing steam distillation extraction on the extraction residue of (1) to obtain a steam distillation extract, and (4) mixing the low-temperature extract stored at a temperature range of 0 to 30°C in step (2) with (3) and the steam distillation extract obtained in step (3) to obtain a coffee extract (Patent Document 6); a method for preserving aroma components, comprising: applying steam distillation or gas-liquid countercurrent contact extraction to roasted and ground coffee beans to recover an aqueous solution containing aroma components of the roasted coffee beans, adding an alkaline substance to the aqueous solution containing the aroma components to adjust its pH to 6.6 to 10 to ionize carbon dioxide gas, storing the pH-adjusted aqueous solution containing aroma components in a container, and storing the container containing the aqueous solution at a temperature of -10 to -50°C (Patent Document 7).

On the other hand, in addition to natural extracts or steam distillation, specific sulfur-containing compounds are known to be useful as aroma compounds added to beverages. For example, there is a proposal to provide a tea beverage with a soft and full green odor of freshly brewed tea by adding 4-hydroxy-4-methylpentan-2-one as a flavoring compound to green tea beverages (Patent Document 8). In addition, it is known that natural green tea also contains a trace amount of 4-hydroxy-4-methylpentan-2-one (Non-Patent Document 1). [Prior Art Document] [Patent Document]

[Patent Document 1] Japanese Patent Publication No. 2-203750 [Patent Document 2] Japanese Patent Publication No. 8-116882 [Patent Document 3] Japanese Patent Publication No. 2000-135059 [Patent Document 4] Japanese Patent Publication No. 2003-33137 [Patent Document 5] Japanese Patent Publication No. 2005-160416 [Patent Document 6] Japanese Patent No. 6146915 [Patent Document 7] Japanese Patent No. 5374020 [Patent Document 8] Japanese Patent Publication No. 2000-342179 [Non-Patent Documents]

[Non-patent document 1] Influence of Manufacturing Conditions and Crop Season on the Formation of 4-Mercapto-4-methyl-2-pentanone in Japanese Green Tea (Sen-cha) (J. Agric. Food Chem. 2005, 53, 13 , 5390-5396)

[Problems to be solved by the invention]

However, although the natural plant and animal extracts produced by the conventional water steam distillation method can bring a natural feel to food and beverages, they are not sufficient in imparting a unique aroma or bringing a strong aroma with a trace amount of addition.

Although the present invention is a method for producing natural plant and animal extracts using a water vapor distillation method, it provides an extract having a fragrance that is significantly different in quality from the fragrance obtained using the conventional water vapor distillation method. [Means for Solving the Problem]

The inventors of the present invention have conducted in-depth research on green tea extracts including distillates (natural aroma recovery products) obtained from green tea raw materials by steam distillation. As a result, it was surprisingly found that when the steam distillation distillate of green tea leaves does not contain the so-called extract (aqueous extract obtained from green tea leaves or steam distillation residues of green tea leaves using a solvent such as water), and is frozen (pH 9.2 before freezing) and thawed in a state of only the distillate, the aroma quality changes significantly, and when it is added to beverages, the soft and full green aroma of brewed tea can be reproduced. Furthermore, the inventors found that the freezing-thawing operation significantly increased the amount of 4-hydroxy-4-methylpentan-2-one in the steam distillation distillate after thawing compared to that before thawing, thereby completing the present invention.

Therefore, the present invention provides the following. [1] A method for producing a green tea extract, comprising the following steps (A) to (D):

Step (A): distilling green tea to obtain a distillate. Step (B): adjusting the pH of the distillate obtained in step (A) to 8.0 or higher. Step (C): freezing the distillate obtained in step (B) with a pH of 8.0 or higher. Step (D): thawing the distillate frozen in step (C). [2] A green tea extract, which is a green tea extract to which 4-hydroxy-4-methylpentan-2-one is not added. When 4-hydroxy-4-methylpentan-2-one in the green tea extract is determined, it satisfies the following formula. ((yield (mass) of green tea extract)/(amount (mass) of green tea leaves used as an extraction raw material))×the content ratio of 4-hydroxy-4-methylpentan-2-one in the green tea extract (mass basis)=1× ^10-8 ～5× ^10-5 [3] A green tea extract is a green tea extract to which 4-hydroxy-4-methylpentan-2-one is not added. When the aroma components of the green tea extract are analyzed by GC/MS, a chromatogram is drawn based on the analysis results of GC/MS, and it satisfies the following formula. (Area value of the peak value (m/z=132) of 4-hydroxy-4-methylpentan-2-one detected)/(Area value of the peak value (total ions) of linalool detected)=1×10 ^-5 ～5×10 ^-2 [4] A packaged green tea beverage, comprising a green tea extract as described in [2] or [3]. [5] A green tea-flavored beverage, comprising a green tea extract as described in [2] or [3]. [6] A method for producing an animal or plant extract, comprising the following steps (A) to (D). Step (A): distilling the plant and animal raw materials by steam to obtain a distillate. Step (B): adjusting the pH of the distillate obtained in the above step (A) to 8.0 or above. Step (C): freezing the distillate obtained in the above step (B) with a pH of 8.0 or above. Step (D): thawing the distillate frozen in the above step (C). [7] The method for producing plant and animal extracts as described in [6], wherein in the freezing of the above step (C), the distillate is frozen until 99% or more of the whole distillate is in a frozen state. [8] The method for producing plant and animal extracts as described in [6], wherein in the freezing of the aforementioned step (C), the time required for more than 99% of the entire distillate to be frozen is more than 30 minutes. [9] The method for producing plant and animal extracts as described in [6], wherein in the aforementioned step (C), the concentration of soluble solid components other than the distillate obtained in the aforementioned step (A) in the distillate obtained in the aforementioned step (B) before freezing is less than 1.0 mass %. [10] The method for producing plant and animal extracts as described in [6], wherein the steam distillation in the aforementioned step (A) is one or more selected from atmospheric pressure steam distillation, reduced pressure steam distillation, pressurized steam distillation and rotary thin film steam distillation (SCC). [11] The method for producing plant and animal extracts as described in [6], wherein after step (D), it further comprises the following step (E). Step (E): Adding a solvent of the same type of plant and animal raw material as that used in the aforementioned step (A) to the thawing liquid obtained in the aforementioned step (D) to extract the extract. [12] A method for producing an animal or plant extract as described in [11], wherein the solvent-extracted extract of the animal or plant raw material is an extract obtained by extracting the animal or plant raw material with an aqueous solvent after and/or before obtaining a steam distillation distillate. [13] A method for producing an animal or plant raw material extract as described in [12], comprising a heat sterilization step. [14] A method for producing an animal or plant extract as described in any one of [6] to [13], wherein the animal or plant raw material is coffee or tea. [15] A method for producing a beverage, comprising the step of adding the animal or plant extract obtained by the production method as described in any one of [6] to [13] to a beverage. [16] A method for producing a flavor composition, comprising the step of adding an animal or plant extract obtained by the production method described in any one of [6] to [13] to the flavor composition. [17] A method for producing a beverage, comprising the step of adding the flavor composition obtained by the production method described in [16] to the beverage. [Effects of the Invention]

By blending the plant and animal extracts of the present invention into food and beverages, a unique aroma can be imparted to the food and beverages. In particular, the green tea extract of the present invention has a strong green tea aroma with a slight fruity taste when it is smelled directly, but by adding a small amount of it to green tea beverages, green tea foods, etc., tea beverages and tea foods with a soft and full green aroma of freshly brewed tea can be provided.

[Form used to implement the invention]

(Animal and plant raw materials) The animal and plant raw materials that can be used in the present invention can be any raw materials as long as they can be distilled by steam. For example, animal raw materials include livestock meat (muscle, fat, viscera, etc. of cattle, pigs, chickens, sheep, horses, etc.), fish and shellfish (marine fish, freshwater fish, white fish, red fish, squid, octopus, shellfish, shrimp, crab, etc.), and these heated processed products. In addition, as for plant raw materials, for example, tea (green tea, matcha, tencha, black tea, oolong tea, post-fermented tea, barley tea, brown rice tea, herbal tea, etc.), roasted coffee beans, herbs/spices (lavender, perilla, jasmine, parsley, sage, oregano, bergamot, hops, lemon balm, chamomile, rosemary, thyme, mint, parsley, black pepper, white pepper, cumin, chili, Sichuan pepper, etc.), fruits (apples, strawberries, grapes, mandarin oranges, oranges, lemons, pineapples, kiwis, etc.), vegetables (cabbage, cabbage, radish, onions, tomatoes, etc.), nuts (white sesame, black sesame, walnuts, chestnuts, cashews, macadamia nuts, peanuts, etc.). Among these, coffee and tea are particularly preferred.

The aforementioned animal and plant raw materials can be used in a raw state, but can also be used by heat treatment such as baking or roasting to enhance or improve the aroma.

The aforementioned animal and plant raw materials may also be pulverized as needed to a particle size of about 0.1 mm to 10 mm, preferably about 1 mm to 5 mm, to improve the aroma recovery rate by distillation.

(Step (A): a step of steam distilling animal and plant raw materials to obtain a distillate) Steam distillation is a phenomenon in which when steam is blown into the raw materials, when the sum of the vapor pressure (partial pressure) of the volatile substances contained in the raw materials and the vapor pressure (partial pressure) of the steam added from the outside becomes equal to or higher than the surrounding pressure (atmospheric pressure in the case of normal pressure steam distillation), the volatile components are distilled and distilled out together with the steam. By cooling the volatile components distilled out together with the steam, an aqueous solution containing the volatile components (generally so-called aroma components) can be obtained as a distillate.

As for the water vapor distillation method, for example, normal pressure water vapor distillation method, pressurized water vapor distillation method, reduced pressure water vapor distillation method, etc. can be adopted. Also, the following methods can be adopted: a method of filling a column with animal and plant raw materials and blowing steam directly into the column; a method of filling a column with animal and plant raw materials, wetting the animal and plant raw materials with a small amount of water and blowing steam into the column; a method of mixing the animal and plant raw materials with water to form a suspension, and blowing water vapor into a kettle filled with the suspension; water vapor distillation using an SCC (also called "Spinning Cone Column", "gas-liquid countercurrent contact distillation") device, etc.

For example, in the method of water vapor distillation using a column, water vapor can be blown into the bottom of the water vapor distillation kettle into which the raw materials have been fed, and the distillation vapor can be cooled by a cooler connected to the distillation side of the upper part, so that the distillate containing the aroma can be collected as a condensate. If necessary, a condensation trap using a refrigerant (dry ice-ethanol, dry ice-acetone, liquid nitrogen, etc.) can be connected to the front end of the aroma collection device to reliably collect aroma components with lower boiling points. In addition, during the water vapor distillation, if the distillation is carried out in the presence of an inert gas such as nitrogen and/or an antioxidant such as vitamin C, the deterioration of the raw materials and/or aroma components due to heating can be effectively prevented. In water vapor distillation, a large amount of aroma will be excreted in the early stage of distillation, and then the aroma will gradually decrease. When to end the distillation can be determined by referring to the results of several times and considering the economics. The amount of distillate collected is 0.1 to 10 parts by mass, preferably 0.2 to 5 parts by mass, and more preferably 0.5 to 2 parts by mass relative to 1 part by mass of the raw material, and a distillate with a Bx of about 0 to 5° can be obtained.

In the method using the SCC device, for example, a method can be adopted in which a raw material pulverized material (about 1 to 3 mm) is mixed with water to make a slurry, and a method of distilling the slurry using a device described in Japanese Patent Gazette No. 7-22646 can be used. If the means of recovering aroma using this device is specifically described, an example can be given: on a rotating cone of a gas-liquid countercurrent contact extraction device having a structure in which a rotating cone and a fixed cone are alternately combined, a liquid or paste-like raw material for a favorite drink is made to flow down from the top while steam is made to rise from the bottom, thereby recovering the aroma components originally present in the raw material. As for the operating conditions of this gas-liquid countercurrent contact extraction device, they can be arbitrarily selected according to the processing capacity of the device, the type and concentration of the raw material, the intensity of the aroma, etc. The ratio of the raw material to water in the raw material slurry can be any ratio as long as the raw material is in an amount that allows the raw material to be fluid, but an example is about 5 to 30 times the amount of water per 1 part by mass of the raw material.

The amount of the distillate collected is 0.1 to 10 parts by mass, preferably 0.2 to 5 parts by mass, and more preferably 0.5 to 2 parts by mass, relative to 1 part by mass of the animal or plant raw material, and a distillate with a Bx of about 0 to 5° can be obtained.

(Step (B): a step of making the pH of the distillate obtained in the aforementioned step (A) to be 8.0 or higher) Next, the pH of the distillate obtained in the aforementioned step (A) is made to be 8.0 or higher. Thereby, the reactivity of each component contained in the distillate in the subsequent freezing and thawing steps is improved.

The pH of the distillate is not particularly limited as long as it is 8.0 or higher, but the lower limit thereof may be 8.0, 8.2, 8.4, 8.6, 8.8, 9.0, 9.2, 9.4, 9.6, 9.8, 10.0, etc., and the upper limit thereof may be 14.0, 13.5, 13.0, 12.5, 12.0, etc. The pH range of the distillate is usually 8.0 to 14.0, preferably 8.4 to 13.0, more preferably 8.8 to 12.0, and even more preferably 9.2 to 11.0.

The pH of the distillate can be adjusted by an edible alkaline substance, but when the pH of the distillate obtained in the aforementioned step (A) is already above 8.0, there is no need to adjust it by adding an alkaline substance. Therefore, step (B) also includes the case where the pH of the distillate obtained in the aforementioned step (A) is confirmed to be above 8.0 and nothing is added. As for edible alkaline substances, sodium bicarbonate, sodium hydroxide, potassium hydroxide, etc. can be exemplified. For example, in the case of using sodium bicarbonate, the amount of sodium bicarbonate added to the aforementioned distillate can be 0.001 mass parts to 0.05 mass parts, preferably 0.002 mass parts to 0.01 mass parts, relative to 1 mass part of the distillate.

Furthermore, for example, in the case where the plant or animal raw material is coffee, carbon dioxide generated during roasting may be contained in the raw material. In such a raw material, the carbon dioxide is distilled out by water vapor distillation and contained in the distillate, and as a result, hydrogen carbonate ions and hydrogen ions exist in the distillate, and the pH may be lowered due to the hydrogen ions. In such a case, the distillate may be treated by degassing or nitrogen bubbling to discharge the carbon dioxide in the distillate in the form of carbonic acid gas, and then the pH may be adjusted directly or as needed to a pH of 8.0 or above.

(Step (C): A step of freezing the distillate with a pH of 8.0 or above obtained in the aforementioned step (B)) In the present invention, the distillate with a pH of 8.0 or above obtained in the aforementioned step (B) is frozen. The freezing is performed until the aforementioned distillate is almost entirely frozen, usually until more than 99%, preferably more than 99.5%, more preferably more than 99.8%, and further preferably more than 99.9% of the entire distillate is frozen. In addition, the freezing is preferably a freezing method in which the freezing state is gradually performed from the part in contact with the refrigerant to the part not in contact with the refrigerant. It is believed that by adopting such a freezing method, water (ice) that does not contain volatile components as an impurity will crystallize, and the volatile compounds will be concentrated in the unfrozen part, and the effect of the present invention will be achieved through the chemical reaction generated in the high-concentration part of the matrix before the concentrated reaction.

Such phenomenon in the present invention is not bound by any theory, but it is speculated that it is caused by the reaction of volatile sulfur-containing compounds such as hydrogen sulfide, methyl mercaptan, ethyl mercaptan and other volatile components in the distillate under alkaline conditions.

Examples of the freezing method for causing such a phenomenon include a method of filling a container with a predetermined amount of the distillate and freezing the container unit, and a method of continuously freezing the container unit.

When freezing is performed in container units, the time condition becomes an important factor. As the time until the distillate is almost completely frozen, it takes more than 30 minutes, preferably more than 1 hour, more preferably more than 2 hours, and further preferably more than 5 hours. When freezing is completed in a short time, it will be difficult to concentrate the volatile compounds in the unfrozen part. There is no particular limitation on the amount of the distillate filled into the container, but it is assumed to be about 30g (filled in an ounce bottle) to 200kg (filled in a drum), and the freezing temperature suitable for the container size can be appropriately selected.

The freezing temperature also depends on the amount of the distillate to be filled into the container, but if it is lower than 0°C, it will freeze. For example, it is usually -5°C or lower, preferably -10°C or lower, more preferably -15°C or lower, and further preferably -20°C or lower. On the other hand, if the freezing temperature is too low, whether it is the whole or part, under the condition of freezing a large amount in an instant, there is a possibility that the reaction cannot be fully carried out. Therefore, it can be exemplified as: generally -100°C or higher, preferably -80°C or higher, more preferably -60°C or higher, further preferably -45°C or higher, and particularly preferably -30°C or higher.

On the other hand, when the distillate is continuously frozen while flowing, it is preferred that the cooling process be continued until 99% or more of the entire distillate is frozen while the cooled portion undergoes partial pure crystallization of ice. Under such conditions, the purpose of the present invention can be achieved regardless of the time.

Furthermore, in the freezing step (C), in order to achieve the purpose of the present invention, it is preferred that the distillate before freezing does not contain the solvent-extracted extract of the animal or plant raw material, or other soluble (mainly water-soluble) solid components other than the components of the distillate. Furthermore, if it contains solutes, it is preferred that the amount is as small as possible. As mentioned above, the phenomenon of aroma change in the present invention is presumed to be generated by the reaction of hydrogen sulfide, methyl mercaptan, ethyl mercaptan and other volatile sulfur-containing compounds in the distillate with other volatile components under alkaline conditions in the concentrated portion after freezing and concentration. However, if the distillate contains solvent-extracted extracts of the animal and plant raw materials or other soluble (water-soluble) solid components, the concentration of hydrogen sulfide, methyl mercaptan, ethyl mercaptan and other volatile sulfur-containing compounds in the distillate will not be sufficiently increased due to these, and the chemical reaction is difficult to proceed. In addition, the solvent-extracted extracts of the animal and plant raw materials will also hinder the aforementioned chemical reaction.

The solvent-extracted extract of the animal or plant raw material or other soluble (water-soluble) solid components in the distillate is usually 1.0% or less, preferably 0.5% or less, more preferably 0.2% or less, and further preferably 0.1% or less.

Furthermore, the temperature and time from when the distillate is almost completely frozen to when the next thawing step (D) is performed do not need to be long if the conditions are such that the distillate is almost completely frozen and the chemical reaction proceeds sufficiently. Furthermore, there is no particular limitation, but the storage temperature can be exemplified as follows: generally 0°C to -100°C, preferably -5°C to -80°C, more preferably -10°C to -60°C, further preferably -15°C to -45°C, and most preferably -20°C to -30°C. The storage time is exemplified as follows: after almost all of the distillate is frozen, it is generally 30 minutes to 168 hours, preferably 1 hour to 100 hours, and more preferably 2 hours to 48 hours.

(Step (D): Thawing the distillate frozen in the above step (C)) The distillate frozen in the above step (C) is then thawed. The thawing method is not particularly limited, and any of thawing in a refrigerator (e.g., about 5°C to 10°C), room temperature thawing (e.g., 15°C to 30°C), and heating thawing (e.g., 40°C to 100°C) can be performed. The thawing time is affected by the size of the container and the thawing temperature, but can be exemplified as follows: generally 1 minute to 1 week, preferably 5 minutes to 48 hours, more preferably 10 minutes to 3 days, further preferably 15 minutes to 24 hours, and most preferably 30 minutes to 12 hours. Thawing can also be done by completely thawing the entire solution in the container, but if you consider that the pure ice crystals are concentrated in the center, you can also collect part of the solution while part of the entire solution is thawed.

In this way, the thawed liquid obtained through the above steps (A) to (D) has a unique aroma that is significantly different from the distillate before freezing. For example, when the animal or plant raw material is green tea, the distillate before freezing has a fresh and soft green tea aroma accompanied by seaweed aroma and seashore aroma (foam aroma), while the distillate after thawing, when smelled directly, will feel a strong green aroma that reminds people of the heat of grass and a sweet aroma like fruit. However, when the thawed distillate is diluted to about 100 to 100,000 times, it becomes a kind of aroma that makes people feel the soft and full green aroma of freshly brewed green tea, accompanied by a slight fruity aroma.

(Step (E): Adding the solvent-extracted extract of the animal or plant raw material to the thawed liquid obtained in the aforementioned step (D)) In the present invention, the aforementioned thawed liquid can also be directly used as a blending raw material for the purpose of imparting flavor to beverages. However, if after the aforementioned steps (A) to (D), adding the solvent-extracted extract of the animal or plant raw material or other soluble (water-soluble) solid components to the aforementioned thawed distillate does not affect the aroma characteristics of the thawed distillate. On the contrary, by adding such, the stability of the subsequent product of the present invention will be improved, so it is preferred.

The preferred ingredients for addition are generally aqueous solvent extracts of the animal or plant raw materials. The solvent extracts of the animal or plant raw materials can be obtained as follows.

The animal and plant raw materials after and/or before steam distillation are then extracted using an aqueous solvent such as water, aqueous ethanol, glycerol, or glycerol aqueous solution. The preferred solvent is water. Enzyme treatment may also be performed during and/or after the extraction. That is, the enzyme treatment may be performed simultaneously with the extraction or may be performed once the extraction is performed. Furthermore, these methods may also be combined.

Specifically, a method for producing an extract in which the residue after steam distillation using a column is subjected to water extraction and then enzyme treatment can be obtained, for example, by the following method: 1 to 100 parts by weight of water are added to each part by weight of the animal and plant raw materials after steam distillation, and extraction is carried out at room temperature to about 100°C for about 2 minutes to about 5 hours depending on the use temperature under static or stirring conditions. After cooling, solid-liquid separation is carried out by a known method such as centrifugation, pressing, filtering, etc. to remove insoluble matter. Alternatively, for example, the slag raw material can be obtained by filling a column made of a suitable material such as glass or stainless steel, and flowing hot water at room temperature to about 100°C from the top or bottom of the column using a metering pump, etc., to perform column extraction. The column extraction can be performed by connecting a plurality of columns in series as needed.

Furthermore, in the case of recovering aroma by gas-liquid countercurrent contact extraction, since the residue has become a slurry containing an extract, the extract can be obtained by separating the solid components in the residue into solid-liquid by a known method such as centrifugation, pressing, filtering, etc. to remove insoluble matter.

The method of collecting the extract before the enzyme treatment as described above can also be adopted, but in the present invention, the enzyme treatment can also be carried out in a state containing the animal and plant raw materials after steam distillation. Since the enzyme treatment is carried out in a state containing the animal and plant raw materials after steam distillation, the soluble solid components are increased by enzyme decomposition, and it is also possible to increase the yield of the soluble solid components of the entire extract from the animal and plant raw materials.

The enzymes used can be those corresponding to the animal or plant raw materials. For example, if the animal or plant raw materials are animal raw materials, proteases, lipases, etc. can be exemplified, and if they are plant raw materials, cellulases, pectinases, hemicellulases, amylases, tanninases, proteases, lipases, etc. can be exemplified. In addition, if the raw material is coffee, polymannanase can be exemplified, and if it is tea, tanninase can be exemplified as preferred enzymes.

The enzyme-treated solution is heated to inactivate the enzyme, and when it contains a slurry, solid-liquid separation and filtration are performed to obtain an extract.

The aforementioned water-soluble solvent extract or enzyme-treated solution may then be concentrated as needed. As for the concentration method, for example, the water-soluble solvent extract or enzyme-treated extract may be concentrated by using appropriate concentration means such as reduced pressure concentration, reverse osmosis membrane (RO membrane) concentration, and freeze concentration to obtain a concentrate of the water-soluble solvent extract or enzyme-treated extract. The concentration of the concentrate is preferably within the following range, generally Bx3° to 50°, preferably 10° to 40°.

The solvent-extracted extract of the animal and plant raw materials (water-soluble solvent extract or enzyme treatment solution, or a concentrated solution thereof) can be mixed with the thawed distillate in the step (D). The mixing ratio is not particularly limited, but the amount of the solvent-extracted extract of the animal and plant raw materials relative to the thawed distillate varies depending on the raw materials used, etc., and is not particularly limited. For example, the solvent-extracted extract of the animal and plant raw materials can be set within the following range per 1 mass part of the distillate, usually 0.005 to 100 mass parts, preferably 0.01 to 50 mass parts, more preferably 0.1 to 20 mass parts, and further preferably 0.5 to 10 mass parts.

(Heat sterilization) The plant and animal extracts of the present invention can be heat sterilized at any stage of the aforementioned steps to produce a microbially stable extract. The heat sterilization stage can be performed at any stage unless it hinders the purpose of the present invention by chemical reaction by freezing. As for the preferred aspects, it can be listed as: the middle stage and the final stage of the step of preparing the solvent extraction extract of the plant and animal raw materials; and after the solvent extraction extract of the plant and animal raw materials is mixed with the thawed distillate of the aforementioned step (D).

Heat sterilization can be carried out in either batch or plate mode. In the case of batch mode, the temperature is usually 80°C to 110°C, preferably 85°C to 105°C, and more preferably 90°C to 100°C, and the time can be exemplified as: usually 30 seconds to 60 minutes, preferably 1 minute to 30 minutes, and more preferably 2 minutes to 15 minutes. In the plate mode, the temperature is usually 80°C to 140°C, preferably 85°C to 135°C, and more preferably 90°C to 130°C, and the time can be exemplified as: usually 10 seconds to 5 minutes, preferably 20 seconds to 3 minutes, and more preferably 30 seconds to 2 minutes.

The plant and animal extracts of the present invention obtained in this way can be filled into a container after cooling, or can be filled into a container while hot, cooled, and further frozen for storage. In addition, the aroma changes less due to freezing at this stage. The reasons for this are inferred to be: the chemical reaction in the aforementioned steps (A) to (D) is fully carried out; the solvent extraction extract of the plant and animal raw materials added in step (E) hinders the aforementioned chemical reaction; the concentration of the matrix participating in the reaction is diluted by the solvent extraction extract of the plant and animal raw materials; the pH decreases, etc.

(Specific example of animal and plant raw materials: green tea) If we list the preferred specific examples of the animal and plant raw materials in the present invention, we can cite tea, among which green tea and Ichibancha can be particularly cited. When Ichibancha is subjected to steam distillation in step (A), the pH of the distillate obtained is generally around 9 even without pH adjustment. It is presumed that this is because there are more alkaline volatile components. The aroma of the steam distillate obtained in this way has a soft aroma accompanied by the aroma of the seashore.

If the distillate of the first tea obtained in this way is frozen and then thawed under the conditions detailed in the above step (C), the aroma changes significantly and becomes a tea aroma with a strong green aroma accompanied by a slight fruity feeling. After analyzing the components of the aroma, it has been found that a large amount of sulfur-containing compounds mainly composed of 4-hydroxy-4-methylpentan-2-one are contained as a characteristic component. On the other hand, the distillate before freezing contains only a very small amount of 4-hydroxy-4-methylpentan-2-one. According to non-patent document 1, the maximum amount of 4-hydroxy-4-methylpentan-2-one in tea leaves is 0.14 ppb. However, it has been found that even if 4-hydroxy-4-methylpentan-2-one is not added externally to the green tea extract obtained by the method for producing animal and plant extracts of the present invention, a large amount of 4-hydroxy-4-methylpentan-2-one is produced by subjecting the distillate of steam distillation of green tea, especially first-grade tea, to the aforementioned steps (A) to (D), and the amount thereof increases to several thousand to tens of thousands times that of the distillate before freezing. Therefore, in the case of using green tea as a raw material, the product of the present invention using green tea as a raw material can be specified by setting the range of the ratio of the content of the index compound to 4-hydroxy-4-methylpentan-2-one using a compound generally contained in green tea and having little change in the freezing-thawing step of the present invention as an index. As for the above-mentioned index compound suitable for such setting, linalool, indole, cis-3-hexenol, hexanol, linalool oxide, isobutyraldehyde, geraniol, hexanol, octanol, benzyl alcohol, trans-2-nonenol, β-ionone, etc. can be exemplified. Among them, linalool can be preferably exemplified.

(Aroma analysis) Aroma analysis can be performed using appropriate GC columns and devices, GC/MS devices, and appropriate SPME, etc.

Quantitation can be performed by plotting a chromatogram from the GC/MS analysis results, using the area values of the detected peaks, or using an absolute calibration curve, standard addition method, or internal standard method.

(4-Hydroxy-4-methylpentan-2-one) The amount of 4-hydroxy-4-methylpentan-2-one in the product of the present invention using green tea as a raw material by the method of the present invention is within the following range when the ion chromatogram extracted at m/z=132 is plotted from the analysis results of GC/MS and the area of the detected peak is used in the standard addition method.

The ratio (mass basis) of ((yield (mass) of green tea extract)/(amount (mass) of green tea leaves used as extraction raw material))×the content ratio of 4-hydroxy-4-methylpentan-2-one in the green tea extract is usually 1×10 ^-8 or more, preferably 5×10 ^-8 or more, more preferably 2×10 ^-7 or more, and further preferably 5×10 ^-7 or more. In addition, the upper limit does not need to be particularly limited, but it can generally be set to 5×10 ^-5 or less, 3×10 ^-5 or less, 2×10 ^-5 or less, 1×10 ^-5 or less, 5×10 ^-4 or less, 4×10 ^-4 or less. The range of the upper limit and the lower limit can be arbitrarily combined, but the range of 1×10 ^-8 to 5×10 ^-5 can be exemplified.

In addition, the amount of 4-hydroxy-4-methylpentan-2-one in the animal and plant extract (green tea extract) of the present invention using green tea as a raw material varies depending on the yield of the present invention from the raw material tea leaves, but when quantified by the same analytical method as above, it is within the following range.

The ratio (mass basis) of ((yield (mass) of green tea extract)/(amount (mass) of green tea leaves used as extraction raw material))×the content ratio of 4-hydroxy-4-methylpentan-2-one in the green tea extract is usually 1×10 ^-8 or more, preferably 5×10 ^-8 or more, more preferably 2×10 ^-7 or more, and further preferably 5×10 ^-7 or more. In addition, the upper limit does not need to be particularly limited, but it can generally be set to 5×10 ^-5 or less, 3×10 ^-5 or less, 2×10 ^-5 or less, 1×10 ^-5 or less, 5×10 ^-4 or less, 4×10 ^-4 or less. The range of the upper limit and the lower limit can be arbitrarily combined, and an example thereof is 1×10 ^-8 to 5×10 ^-5 .

In addition, the content of 4-hydroxy-4-methylpentan-2-one in the product of the present invention using green tea as a raw material as an animal or plant raw material can also be measured by using linalool, a volatile compound generally contained in green tea. In this case, an ion chromatogram extracted with m/z=132 (4-hydroxy-4-methylpentan-2-one) and total ions (linalool) is plotted from the analysis results of GC/MS, and the area of the detected peak is used as (area value of the peak value (m/z=132) of 4-hydroxy-4-methylpentan-2-one detected)/(area value of the peak value (total ions) of linalool detected), which can usually be set to 1×10 ^-5 or more, 2×10 ^-5 or more, 5×10 ^-5 or more, 1×10 ^-4 or more, etc. The upper limit does not need to be particularly limited, but can generally be set to 5×10 ^-2 or less, 3×10 ^-2 or less, 2×10 ^-2 or less, 1×10 ^-2 or less, 5×10 ^-3 or less, 3×10 ^-3 or less, etc. The upper limit and the lower limit range can be arbitrarily combined, and an example thereof is 1×10 ^-5 to 5×10 ^-2 .

(Fragrance composition) The plant and animal extracts of the present invention (hereinafter referred to as the plant and animal extracts of the present invention) obtained in this way can also be added to food and beverages to impart a unique flavor, and can also be used as a material for a fragrance composition (hereinafter referred to as the fragrance composition of the present invention). The fragrance composition of the present invention in one embodiment of the present invention contains a specified amount of the plant and animal extracts of the present invention, and can be mixed with various food and beverages for the purpose of imparting flavor. According to the flavor composition of the present case, for example, the flavor composition can be given a natural, juicy, moist, rich, mature, ripe, gorgeous, fresh, fragrant, bitter, spicy, mellow, or rich flavor, and the flavor of various beverages mixed with the flavor composition of the present case can be improved.

The concentration of the plant and animal extracts in the fragrance composition of the present invention can be arbitrarily determined according to the object of the fragrance composition. As an example of such concentration, the following range can be cited, that is, 0.1ppt to 10%, preferably 1ppb to 1%, and more preferably 0.1ppm to 0.1%, relative to the total mass of the fragrance composition of the present invention.

In addition, the flavor composition of the present invention may further contain other arbitrary compounds or components in addition to the animal and plant extracts of the present invention. Examples of such compounds or components include various types of flavor compounds or flavor compositions, oil-soluble pigments, vitamins, functional substances, fish extracts, livestock extracts, plant extracts, yeast extracts, animal and plant proteins, animal and plant protein decomposition products, starch, dextrin, sugars, amino acids, nucleic acids, organic acids, solvents, and the like. For example, natural essential oils, natural flavors, synthetic flavors, etc. listed in "Japan Patent Office Gazette, Collection of Commonly Known and Customary Techniques (Fragrances) Part II Food Flavors, published on January 14, 2001", "Survey on the Actual Use of Food Flavor Compounds in Japan" (Health Science Research Report for 2001, Japan Flavor Industry Association, published in March 2003), and "Synthetic Flavors: Chemical and Product Knowledge" (new supplement published on December 20, 2016, compiled by the Synthetic Flavors Editing Committee, Chemical Industry Daily) can be cited.

Specific examples of synthetic flavor compounds include, in terms of hydrocarbon compounds, monoterpenes such as α-pinene, β-pinene, γ-terpinene, myrcene, camphene, and limonene, sesquiterpenes such as valencene, cedrene, caryophyllene, and longifolene, and 1,3,5-undecatriene.

As alcohol compounds, there can be mentioned saturated alcohols such as butanol, pentanol, 3-octanol, hexanol, etc., unsaturated alcohols such as (Z)-3-hexen-1-ol, isopentanol, 2,6-nonadienol, etc., terpene alcohols such as linalool, geraniol, citronellol, tetrahydrogeranyl, mycochloroenol, nerolidol, cedrol, α-abietinol, terpinen-4-ol, borneol, etc., and aromatic alcohols such as benzyl alcohol, phenylethyl alcohol, cinnamyl alcohol, etc.

As the aldehyde compound, there can be mentioned saturated aldehydes such as acetaldehyde, hexanol, octanal, decanal, hydroxycitronellal, etc., unsaturated aldehydes such as (E)-2-hexenal, 2,4-octanedial, etc., terpene aldehydes such as citronellal, citral, myrthenal, perilla aldehyde, etc., and aromatic aldehydes such as benzaldehyde, cinnamaldehyde, vanillin, ethyl vanillin, helianthus annuus, p-tolualdehyde, etc.

Examples of ketone compounds include saturated and unsaturated ketones such as 2-heptanone, 2-undecanone, 1-octen-3-one, 3-hydroxy-2-butanone, and 6-methyl-5-hepten-2-one (methylheptenone), diketones and hydroxyketones such as butanedione, 2,3-pentanedione, maltol, ethyl maltol, cycloene, and 2,5-dimethyl-4-hydroxy-3(2H)-furanone, terpene ketones such as carvone, menthone, and nokatone, ketones derived from terpene decomposition products such as α-ionone, β-ionone, and β-damascenone, and aromatic ketones such as raspberry ketone.

As for the furan or ether compounds, furfuryl alcohol, furfural, oxidized rose, oxidized linalool, menthofuran, spirulinatone, p-allyl anisole, eugenol, 1,8-cineole, etc. can be listed.

As the ester compound, there can be mentioned aliphatic esters such as ethyl acetate, isoamyl acetate, octyl acetate, ethyl butyrate, ethyl isobutyrate, isoamyl butyrate, ethyl 2-methylbutyrate, ethyl isovalerate, 2-methylbutyl isobutyrate, ethyl caproate, allyl caproate, ethyl heptanoate, ethyl caprylate, isoamyl isovalerate, ethyl nonanoate, etc.; terpene alcohol esters such as linalyl acetate, geranyl acetate, lavender acetate, terpinyl acetate, neryl acetate, etc.; and aromatic esters such as benzyl acetate, methyl salicylate, methyl cinnamate, cinnamyl propionate, ethyl benzoate, cinnamyl isovalerate, ethyl 3-methyl-2-phenylglycidate, etc.

Examples of the lactone compounds include saturated lactones such as γ-decanolactone, γ-dodecanolactone, δ-decanolactone, and δ-dodecanolactone, and unsaturated lactones such as 7-decene-4-lactone and 2-decene-5-lactone.

As the acid compound, there can be mentioned saturated/unsaturated fatty acids such as acetic acid, butyric acid, isovaleric acid, caproic acid, caprylic acid, stearic acid, oleic acid, linoleic acid, linolenic acid and the like.

As nitrogen-containing compounds, indole, 3-methylindole, pyridine, alkyl-substituted pyridine, , methyl amine benzoate, trimethylpyridine wait.

As for the sulfur-containing compounds, methyl mercaptan, dimethyl sulfide, dimethyl disulfide, allyl isothiocyanate, 3-methyl-2-butene-1-thiol, 3-methyl-2-butanethiol, 3-methyl-1-butanethiol, 2-methyl-1-butanethiol, 3-butylhexanol, 4-butyl-4-methyl-2-pentanone, 3-butylhexyl acetate, p-menthyl-8-thiol-3-one and furfurylthiol can be listed.

As for natural essential oils, there are sweet orange, bitter orange, petitgrain, lemon, bergamot, tangerine, orange blossom, peppermint, green mint, lavender, chamomile, rosemary, eucalyptus, sage, basil, rose, hyacinth, lilac, geranium, jasmine, ylang-ylang (perfume tree), anise, clove, ginger, nutmeg, cardamom, cedar, cypress, vetiver, patchouli, labdanum, etc.

As for various plant and animal extracts, there can be listed extracts of herbs or spices, extracts of coffee, green tea, black tea, or oolong tea, or milk or processed milk products and various enzyme decomposition products thereof such as lipase or protease, etc.

The fragrance composition of the present invention can be prepared by mixing the animal and plant extracts of the present invention with a suitable solvent or dispersion medium by a known method.

As for the form of the fragrance composition of the present invention, it is preferably a solution, an emulsified preparation, a powder preparation, or other solid preparations (solid fats, etc.) obtained by dissolving the animal and plant extracts or other ingredients in a water-soluble or oil-soluble solvent.

As for the water-soluble solvent, ethanol, methanol, acetone, tetrahydrofuran, acetonitrile, 2-propanol, methyl ethyl ketone, glycerol, propylene glycol, dipropylene glycol, etc. can be exemplified. Among these, ethanol or glycerol is particularly preferred from the viewpoint of use in food and beverages. As for the oil-soluble solvent, vegetable oils, animal oils, refined oils (for example, processed oils such as medium-chain fatty acid triglycerides, or short-chain fatty acid triglycerides such as triacetin and tripropionin can be listed.), various essential oils, triethyl citrate, etc. can be exemplified.

In order to prepare an emulsified preparation, the plant or animal extract or the flavor composition of the present invention may be emulsified with a water-soluble solvent and an emulsifier. There is no particular limitation on the emulsification method of the plant and animal extracts or the flavor composition of the present invention. An emulsified liquid with excellent stability can be obtained by using various emulsifiers used in beverages and the like, such as monoglycerides of fatty acids, diglycerides of fatty acids, triglycerides of fatty acids, propylene glycol fatty acid esters, sucrose fatty acid esters, polyglycerol fatty acid esters, lecithin, denatured starch, sorbitan fatty acid esters, saponin extracts, gum arabic, astragalus gum, guar gum, karaya gum, xanthan gum, pectin, alginic acid and its salts, carrageenan, gelatin, casein saponin, or sodium caseinate, and performing emulsification treatment using a homogenizer, a gel mill, a rotary disc homogenizer, a high-pressure homogenizer, or the like. The amount of such emulsifiers used is not strictly limited and can be varied within a wide range depending on the type of emulsifier used. Generally, the amount is in the range of about 0.01 to about 100 parts by mass, preferably about 0.1 to about 50 parts by mass, relative to 1 part by mass of the plant or animal extract in the present invention. In addition, in order to stabilize the emulsion, the emulsion may contain, in addition to water, one or a mixture of two or more polyols such as glycerol, propylene glycol, sorbitol, maltitol, sucrose, glucose, trehalose, sugar solution, reduced syrup, etc.

Furthermore, the emulsion thus obtained can be dried to form a powder preparation if desired. When powdering, a sugar such as gum arabic, trehalose, dextrin, sugar, lactose, glucose, syrup, reduced syrup, etc. can be appropriately blended as needed. The amount of these used can be appropriately selected according to the desired properties of the powder preparation.

The plant and animal extracts or the flavor compositions of the present invention obtained in this way can be blended into beverages in an effective amount to improve, for example, the naturalness, juiceiness, moisture, richness, maturity, perfection, splendor, freshness, aroma, bitterness, spiciness, richness, or richness of the beverages.

In particular, when the aforementioned animal or plant raw material is green tea, a tea beverage or tea food having a soft and full green aroma of freshly brewed tea can be provided by adding a trace amount of the green tea extract of the present invention or a flavoring composition of the green tea extract of the present invention to green tea beverages or green tea foods.

(Beverages) There are no particular limitations on the beverages that can be blended with the animal or plant extracts or the flavoring composition of the present invention, but as examples, beverages with one or more of the following flavors can be listed: various citrus flavors such as lemon, orange, grapefruit, lime, tangerine, mandarin orange, lime, sour orange, hassakukan, iyokan, grapefruit, Taiwanese lemon, kumquat, etc.; strawberry, blueberry, raspberry, apple, cherry, plum, apricot, peach, pineapple, banana, melon, mango, papaya, Various fruit flavors such as kiwi, pear, grape, muscat, Kyoho grape, etc.; milk flavors such as milk, yogurt, cream, etc.; vanilla flavor; various tea flavors such as green tea, black tea, oolong tea, herbal tea, etc.; coffee flavor; cola flavor; cocoa bean flavor; cocoa flavor; various mint flavors such as green mint and peppermint; cinnamon, chamomile, cardamom, celery, fennel, cloves, pepper, coriander, prickly ash, basil, ginger, star anise, thyme, Various spices or herbal flavors such as chili, nutmeg, basil, marjoram, rosemary, laurel, garlic, mustard, etc.; various nut flavors such as almonds, cashews, walnuts, etc.; various alcoholic flavors such as wine, brandy, whiskey, rum, gin, liqueur, sake, soju, beer, etc.; vegetable flavors such as onion, celery, carrot, tomato, cucumber, etc.; various meat flavors such as chicken, duck, pork, beef, mutton, horse meat, etc.; tuna, etc. Red fish, white fish such as mackerel, sea bream, salmon, and horse mackerel, freshwater fish such as sweetfish, trout, and carp, shellfish such as conch, clams, clams, and cockles, various crustaceans such as shrimps and crabs, various seaweeds such as kelp sprouts and kombu, and various fish and shellfish or seaweed flavors; various grain flavors such as rice, barley, wheat, and malt; various fat flavors of meat fats such as butter, chicken fat, and lard, or various fish oils, etc.

More specific examples of food and beverages include: senbei, arare, rice krispie candy, mochi, steamed buns, uiro, bean fillings, yokan, mizuyokan, agar jelly, jelly, honey cake, sugar balls, biscuits, crackers, potato chips, cookies, pies, puddings, butter cream, custard cream, and so on. Snacks such as chocolate, chocolate, chocolate, chocolate chips, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, chocolate cakes, pickles, such as tara pickle), thinly sliced radish pickle (senmai pickle), shallot, miso pickle, takuan pickle, and seasoning bases (vegetarian) for these pickles; mackerel, sardines, saury, salmon, tuna, bonito, whale, Fish such as mackerel, sand eel, and sweetfish; squids such as surumi, long-lance squid, cuttlefish, and frog squid; octopuses such as octopus and short-clawed octopus; shrimps such as prawns, botan shrimps, Japanese lobsters, and black tiger shrimps; cod crabs, snow crabs, Fish and shellfish such as swimming crabs and hairy crabs, clams, clams, scallops, oysters, and mussels; processed food such as canned food, fish stew, tsukudani, meat paste, fish paste products (chikuwa, kamaboko, fried fish cake (揚げ蒲鉾), crab meat sticks (カニ足蒲鉾)), fried food, tempura, etc.; livestock meat such as chicken, pork, beef, mutton, and horse meat; curry, Western-style stew (シチュー), beef stew, Japanese-style beef stew (ハヤシライス) sauce, tomato meat sauce (ミートソース), mapo beans Tofu, hamburger meat, dumplings, rice pot seasonings, soups (corn soup, tomato soup, clear meat soup, etc.), meatballs, stewed meat (kakuni), canned meat, etc. processed drinks using livestock meat; small bottled salt (table salt), seasoning salt, soy sauce, powdered soy sauce, miso, miso powder, moromi, fermented seasoning (hishio), Japanese pancake (furikake), tea rice seasonings, margarine, mayonnaise, salad dressing (dressing), vinegar, three-ingredient vinegar (three cups of vinegar), powdered sukiyaki vinegar, Chinese food seasoning bases, tempura dipping sauce (Tentsuyu), noodle dipping sauce (Mentsuyu) (kelp stock or bonito stock, etc.), sauces (medium-thick sauces, tomato sauce, etc.), tomato sauce, barbecue sauce, curry sauce (Karelu), Western-style stew seasoning bases, soup seasoning bases, stock seasoning bases (kelp stock or bonito stock, etc.), compound seasonings, mirin-style seasoning (Shinmirin), fried chicken powder, takoyaki powder, etc., seasonings such as mixed powders, seasonings containing these seasonings Animal or plant-based soup-flavored drinks; dairy products such as cheese, yogurt, and butter; various yeasts such as brewer's yeast and bread yeast, and various microbial fermentation products such as lactic acid bacteria; stewed vegetables, Chikuzen-ni, oden, hot pots, and other stewed foods; ingredients and side dishes for takeout lunch boxes; fruit juice drinks and soft drinks containing fruit juice such as apples, grapes, and citrus fruits (grapefruit, orange, lemon, etc.), fruit pulp drinks, and fruit drinks containing fruit pulp; tomatoes, green peppers, celery, melons, bitter melons, carrots, Vegetables such as potatoes, asparagus, bracken, and fern, and vegetable-containing beverages such as vegetable drinks and vegetable soups containing these vegetables; specialty beverages such as coffee, cocoa, green tea, black tea, oolong tea, sodas, cola drinks, carbonated beverages (citrus-flavored and other flavored sodas), lactic acid bacteria beverages; beverages containing herbal or herbal medicines; cola drinks, fruit juice drinks, milk drinks, beer-flavored drinks including non-alcoholic beer and so-called "third beer", sports drinks, honey drinks, vitamin supplement drinks , mineral supplement drinks, nutritional drinks, nourishing drinks, lactic acid bacteria drinks and other functional drinks; various alcoholic flavored drinks (beer flavor, plum wine flavor, carbonated shochu flavor, etc.) and other non-alcoholic hobby drinks; wine, shochu (shochu), awamori, sake, beer, carbonated shochu, cocktail drinks, sparkling wine, fruit wine, medicinal wine, so-called "third beer" and other brewed wine (sparkling) or liqueur (sparkling), etc., or alcoholic beverages containing these.

The amount of the animal or plant extract or the flavor composition of the present invention added to the food or beverage can be arbitrarily determined according to the flavor of the food or beverage or the degree of the desired effect.

As an example of the concentration of the added amount, if it is a beverage, the following range can be listed, that is, relative to the total mass of the beverage, the concentration of the animal or plant extract or the flavor composition of the present invention is 0.001ppt~0.1%, preferably 1ppt~100ppm, and more preferably 1ppb~100ppm. More specifically, the lower limit is set to any one of 0.001ppt, 0.01ppt, 0.1ppt, 1ppt, 10ppt, 100ppt, 1ppb, 10ppb, 100ppb, 1ppm, 10ppm, and 100ppm, and the upper limit is set to any one of 0.1%, 100ppm, 10ppm, 1ppm, 100ppb, 10ppb, 1ppb, 100ppt, 10ppt, 1ppt, 0.1ppt, and 0.01ppt, and any combination of these lower limit values and upper limit values can be listed, but is not limited to them. As an example of a preferred concentration, it can be selected from the following range according to the flavor characteristics of the beverage, that is, the concentration of the animal or plant extract or the flavor composition of the present invention is 100ppt~100ppb, 100ppt~1ppm, 1ppb~100ppb, 1ppb~1ppm, 10ppb~1ppm, 10ppb~100ppb, 100ppb~10ppm, 1ppm~100ppm, but is not limited to these.

The present invention is described in more detail below through examples, but the essence of the present invention lies in the technical ideas disclosed above and is not limited by the examples. [Examples]

(Example 1) 600g of Ichibancha (Yabukita variety, lightly steamed) produced in Shizuoka Prefecture was filled into a 3L column, and an aqueous solution of 1.2g of sodium L-ascorbate dissolved in 180g of soft water was evenly sprinkled from the top of the column to moisten the tea leaves. After replacing the inside of the column with nitrogen, water vapor mixed with nitrogen was blown into the bottom of the column, and the water vapor containing volatile components of tea obtained from the top of the column was condensed by a cooling tube (tap water cooling, about 20°C) for about 20 minutes to obtain 300g of distillate containing volatile components of tea (50% for tea leaves). The pH of the obtained distillate was 9.2.

Half of each distillate (150 g) was divided into 300 ml brown bottles, and after replacing the top space with nitrogen, one of them was stored in a refrigerator (5°C) (comparative product 1), and the other was stored in a freezer (-20°C). The one stored in the freezer was frozen from about 30 minutes after storage in the freezer, and was almost completely frozen in about 3 hours. Each was stored in the above state for about 20 hours from the start of storage, and then placed at room temperature (23°C). The frozen product was completely thawed in about 2 hours, and a frozen-thawed product (present invention product 1: pH 9.2) was obtained.

Each of the two was diluted to 0.1% with water and subjected to sensory evaluation. The summary of the aroma of each is as follows.

Comparative product 1 (refrigerated product): Fresh and gentle green tea aroma accompanied by seaweed aroma and seashore aroma Inventive product 1 (frozen-thawed product): Strong green tea aroma accompanied by tropical fruity feeling The aroma of each sample was analyzed by the following method.

1 g of each sample solution (comparative product 1, present invention product 1) was added directly or 1 ppb, 10 ppb, 100 ppb or 1000 ppb of a standard of 4-hydroxy-4-methylpentan-2-one was added to each sample for analysis. Analysis conditions ・Equipment Gas chromatography equipment: 7890B GC System, Agilent Technologies MSD equipment: 5977B MSD, Agilent Technologies ・Column InertCap WAX 0.25mmφ×30m (film thickness 0.25μm) GL Sciences ・SPME fiber 50/30μm DVB/CAR/PDMS StableFlex/SS (2cm) Merck (Supelco: registered trademark) ・Sample amount: 1g ・Vial capacity: 20ml ・Sample equilibration conditions: Stirring at 60℃ for 30 minutes ・SPME extraction conditions: Standing at 60℃ for 30 minutes ・Inlet temperature: 250℃ ・Temperature conditions: After maintaining at 40℃ for 8 minutes, increase to 180℃ at 4℃/min, then increase to 230℃ at 3℃/min, and maintain at 230℃ for 10 minutes ・Carrier gas: He (constant pressure) ・Injection method: splitless ・Flow rate: 1.2ml/min In addition, the GC/MS analysis results are drawn as chromatograms, the peak of 4-hydroxy-4-methylpentan-2-one uses m/z=132, the peak of linalool uses total ions, and the respective area values are used for quantification.

(Analysis results) GC/MS confirmed that the frozen-thawed product contained a large amount of 4-hydroxy-4-methylpentan-2-one.

The content of 4-hydroxy-4-methylpentan-2-one in the above sample obtained by the standard addition method is as follows.

Comparative product 1: 0.25 ppb Inventive product 1: 495.9 ppb In addition, the peak area value of 4-hydroxyl-4-methylpentan-2-one of the inventive product 1 (without the addition of 4-hydroxyl-4-methylpentan-2-one as a standard substance) was 9.9×10 ⁴ , and the area value of linalool was 3.9×10 ⁸ . The peak area value of 4-hydroxyl-4-methylpentan-2-one of the comparative product 1 was 49.9, and the area value of linalool was 3.9×10 ⁸ .

From the above results, it was confirmed that the inventive product 1 contained (produced) about 2,000 times more 4-pentyl-4-methylpentan-2-one than the comparative product 1.

In addition, since 300 g of the present invention product 1 was obtained from 600 g of green tea leaves as a raw material, ((yield (mass) of green tea extract)/(amount (mass) of green tea leaves used as an extraction raw material))×the content ratio of 4-hydroxy-4-methylpentan-2-one in the green tea extract (mass basis) was 2.5×10 ^-7 .

In contrast, in Comparative Product 1, ((yield (mass) of green tea extract)/(amount (mass) of green tea leaves used as an extraction raw material))×the content ratio of 4-hydroxy-4-methylpentan-2-one in the green tea extract (mass basis) was 1.75×10 ^-10 .

In addition, the (area value of the peak value (m/z=132) of 4-hydroxy-4-methylpentan-2-one detected)/(area value of the peak value (total ions) of linalool detected) of the present invention product 1 was 2.5×10 ^-4 .

In contrast, in Comparative Product 1, (area value of the peak value (m/z=132) of 4-hydroxy-4-methylpentan-2-one detected)/(area value of the peak value (total ions) of linalool detected) was 1.25×10 ^-7 .

(Example 2) First, the present product 1 and comparative product 1 were obtained by the same operation as in Example 1. Then, 4800 g of 40°C warm water (0.05% aqueous solution of sodium ascorbate) was introduced from the top of the column at a flow rate of 60 ml/min, and 3000 g of Bx3° extract was extracted from the bottom of the column. The extracted extract was cooled to 20°C and centrifuged at 3000 rpm for 10 minutes to remove the precipitate, thereby obtaining a water extract (reference product 1, Bx3.0°, pH5.6).

150 g of each of the present invention product 1 and reference product 1 were mixed, sterilized at 90°C for 10 minutes, cooled to 20°C, and filled to obtain a green tea extract (present invention product 2) (Bx1.6°, pH6.7). 150 g of each of the comparative product 1 and reference product 1 were mixed, sterilized at 90°C for 10 minutes, cooled to 20°C, and filled to obtain a green tea extract (comparative product 2) (Bx1.6°, pH6.7).

The above analytical method was also used to measure the content of 4-hydroxy-4-methylpentan-2-one in Comparative Product 2 and Inventive Product 2. The results are as follows. Comparative Product 2: 0.11 ppb Inventive Product 2: 245.9 ppb As shown above, the contents of 4-hydroxy-4-methylpentan-2-one that are approximately the same as the calculated amounts of 4-hydroxy-4-methylpentan-2-one believed to be derived from Comparative Product 1 and Inventive Product 1 were confirmed in Comparative Product 2 and Inventive Product 2, respectively, indicating that the content of 4-hydroxy-4-methylpentan-2-one is not easily affected by adding a water extract of green tea to the distillate or by heat sterilization.

In addition, for Comparative Product 2 and Inventive Product 2, the above-mentioned analytical method was also used to measure (the area value of the peak value (m/z=132) of 4-hydroxy-4-methylpentan-2-one detected)/(the area value of the peak value (total ions) of linalool detected). The results are shown below.

(Area value of the peak value (m/z=132) of 4-hydroxy-4-methylpentan-2-one detected)/(Area value of the peak value (total ions) of linalool detected) of comparative product 2 = 5.5× ^10-8 (Area value of the peak value (m/z=132) of 4-hydroxy-4-methylpentan-2-one detected)/(Area value of the peak value (total ions) of linalool detected) of inventive product 2 = 1.1× ^10-4

As shown above, in Comparative Product 2 and Inventive Product 2, values approximately equal to those in (area value of the peak value (m/z=132) detected for 4-hydroxyl-4-methylpentan-2-one)/(area value of the peak value (total ions) detected for linalool) believed to be derived from Comparative Product 1 and Inventive Product 1 were respectively confirmed, indicating that the content of linalool or 4-hydroxyl-4-methylpentan-2-one is not easily affected by adding a water extract of green tea to the distillate or heat sterilization.

(Comparative Example 1) Prepare 300g of Comparative Product 2 (pH 6.7) again, divide into 2 portions of 150g each, and adjust one of them to pH 9.5 using a 1% potassium hydroxide aqueous solution. Place each in a 300ml brown bottle, replace the top space with nitrogen, and store in a freezer (-20℃). The freezer is frozen from about 30 minutes after being stored in the freezer, and is almost completely frozen in about 3 hours. Each is stored in the above state for about 20 hours from the start of storage, and then placed at room temperature (23℃). The frozen product is completely thawed in about 2 hours. The samples frozen and thawed at pH 6.7 were used as comparator 3, and the samples frozen and thawed at pH 9.5 were used as comparator 4.

Comparative Samples 3 and 4 were analyzed for 4-hydroxy-4-methylpentan-2-one and linalool in the same manner as described above. The results are shown in Table 1.

[Table 1] pH before freezing MMP concentration (ppb) ((yield (mass) of green tea extract)/(amount (mass) of green tea leaves used as extraction raw material)) × content ratio of 4-hydroxy-4-methylpentan-2-one in green tea extract (mass basis) Peak area ratio (MMP/linalool) Comparison product 3 5.7 0.16 1.6× ^10-10 1.3×10 ^-7 Comparison 4 9.5 0.18 1.8× ^10-10 1.4×10 ^-7 MMP: 4-hydroxy-4-methylpentan-2-one

In the state containing the water extract of green tea, even when freeze-thawing was performed, no increase of 4-hydroxy-4-methylpentan-2-one was observed at either pH 6.7 or pH 9.5.

(Example 3) 1000g of Kyushu-produced Ichibancha (Abuki variety, medium steamed) was filled into a 3L column and the same operation as in Example 1 was performed. An aqueous solution of 2.0g of sodium L-ascorbate dissolved in 300g of soft water was evenly sprinkled from the top of the column to moisten the tea leaves. After the inside of the column was replaced with nitrogen, water vapor mixed with nitrogen was blown into the bottom of the column, and the water vapor containing volatile components of tea obtained from the top of the column was condensed by a cooling tube (tap water cooling, about 20°C) for about 20 minutes to obtain 500g of distillate containing volatile components of tea (50% for tea leaves). The pH of the obtained distillate was 7.6.

The distillate was divided into 4 300ml brown bottles at 100g each and stored as follows. Comparative product 5: After replacing the top space with nitrogen, store in a freezer (-20℃) Comparative product 6: After replacing the top space with nitrogen, store in a freezer (5℃) Comparative product 7: Use ascorbic acid powder to adjust to pH 6.5, replace the top space with nitrogen, and store in a freezer (-20℃) Inventive product 3: Use 0.1% potassium hydroxide aqueous solution, adjust to pH 9.5, replace the top space with nitrogen, and store in a freezer (-20℃)

The samples stored in the freezer were frozen about 30 minutes after being stored in the freezer, and were almost completely frozen in about 3 hours. Each was stored in the above state for about 20 hours from the start of storage, and then left at room temperature (23°C). The frozen products were completely thawed in about 2 hours, and frozen-thawed products (Comparative Products 6, Comparative Products 7, and Invention Product 3) were obtained.

The present invention product 3 and comparative products 5 to 7 were analyzed for 4-hydroxy-4-methylpentan-2-one and linalool in the same manner as above. The results are shown in Table 2.

[Table 2] pH before freezing MMP concentration (ppb) ((yield (mass) of green tea extract)/(amount (mass) of green tea leaves used as extraction raw material)) × content ratio of 4-hydroxy-4-methylpentan-2-one in green tea extract (mass basis) Peak area ratio (MMP/linalool) Product 3 of the present invention 9.5 442 1:2.2×10 ^-7 3.7× ^10-4 Comparison product 5 7.6 9.2 1:4.6×10 ^-9 7.7×10 ^-6 Comparison product 6 7.6 (Keep refrigerated) 0.22 1:1.1×10 ^-10 8.0×10 ^-7 Comparison product 7 6.5 0.28 1:1.4× ^10-10 1.0×10 ^-6 MMP: 4-hydroxy-4-methylpentan-2-one

As shown in Table 2, even when freezing and thawing were performed at pH 7.6 (Comparative Product 5), an increase in 4-hydroxyl-4-methylpentan-2-one was observed compared to the unfrozen product, but even when freezing and thawing were performed at pH 6.5, 4-hydroxyl-4-methylpentan-2-one hardly increased (Comparative Product 7). On the other hand, when freezing was performed at pH 9.5, 4-hydroxyl-4-methylpentan-2-one increased by more than 40 times compared to the case of freezing at pH 7.6.

(Example 4) 1 kg of green tea (Ichibancha, deep steamed) produced in Shizuoka Prefecture was added to 20 kg of ion exchange water heated to 80°C, and the mixture was slowly stirred for 5 minutes. The tea leaves were separated using a 40-mesh metal mesh, and the separated solution was cooled to 20°C to obtain 14 kg of extract. 7.0 g (500 ppm) of sodium ascorbate was added, and the extract was filtered using No. 2 filter paper (manufactured by ADVANTEC: particle size retention 5 μ) to obtain a stock solution for green tea beverage (analysis values of the stock solution for green tea beverage; Bx: 2.22°, pH: 6.4, tannin content (ferric tartrate method): 0.44%, amino acid content: 0.071%). The solution was divided and diluted 10 times (mass ratio) with ion exchange water, and the dilution solution was prepared by adding the inventive product 2 or the comparative product 2 at the concentrations listed in Table 2, respectively. After heat sterilization at 137°C for 30 seconds, the solution was cooled to 88°C, filled into 500 ml PET bottles, kept for 2 minutes, and then cooled to room temperature (25°C) to prepare PET bottled green tea drinks. Each green tea drink was evaluated by 10 panelists using tea extract without additives as a control group. The evaluation criteria were set at 5 points for no additives, and the freshness of the foam, green fragrance, fullness, sweetness, fruitiness, and seaweed aroma were rated as very good: 10 points, good: 8 points, slightly good: 6 points, slightly bad: 4 points, bad: 2 points, and very bad: 0 points. The results are shown in Table 3.

[Table 3] Add Concentration Fresh foam feeling Green fragrance Sweetness Fullness Fruity Seaweed aroma No Additive 5 5 5 5 5 5 This invention 2 1ppm 8.2 8.3 7.7 7.8 6.4 5.5 10ppm 8.4 8.5 8.2 8 7 5.8 100ppm 8.5 8.8 8.3 8 7.2 6.1 Comparison product 2 1ppm 5 5 5 5 5 5 10ppm 5.6 5.3 5.4 5.2 5.3 5.4 100ppm 6.8 5.8 5.8 5.8 6 6.8

As shown in Table 3, the present invention product 2 significantly increases the freshness of green tea with a slight fruity taste, green aroma, sweetness, and fullness with only a trace amount of 1ppm to 10ppm added to green tea beverages (equivalent to 0.00025ppb to 0.0025ppb of 4-hydroxy-4-methylpentan-2-one). On the other hand, the results of comparative product 2 are: at an addition amount of 1ppm, there is almost no change from no addition, at an addition amount of about 10ppm, a slight effect is observed, and at an addition amount of about 100ppm, the effect becomes clear. Therefore, the present invention product (present invention product 2) exerts its effect even at a concentration far lower than that of the previous aroma extract (comparative product 2), and it can be said that it has unique flavor characteristics and is also advantageous in terms of cost.

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Claims (17)

A method for producing a green tea extract comprises the following steps (A) to (D): Step (A): distilling green tea to obtain a distillate; Step (B): adjusting the pH of the distillate obtained in step (A) to above 8.0; Step (C): freezing the distillate obtained in step (B) with a pH of above 8.0; Step (D): thawing the distillate frozen in step (C). A green tea extract is a green tea extract without added 4-hydroxy-4-methylpentan-2-one obtained by the method for producing a green tea extract as claimed in claim 1, wherein when the 4-hydroxy-4-methylpentan-2-one in the green tea extract is measured, it satisfies the following formula: ((yield (mass) of green tea extract)/(amount (mass) of green tea leaves used as an extraction raw material)))×content ratio of 4-hydroxy-4-methylpentan-2-one in the green tea extract (mass basis)=1× ^10-8 ~5× ^10-5 . A green tea extract is a green tea extract obtained by the method for producing a green tea extract as claimed in claim 1 without adding 4-hydroxy-4-methylpentan-2-one. When the aroma components of the green tea extract are analyzed by GC/MS, a chromatogram is drawn based on the analysis results of GC/MS, which satisfies the following formula: (area value of the peak value (m/z=132) of 4-hydroxy-4-methylpentan-2-one detected)/(area value of the peak value (total ions) of linalool detected)=1×10 ^-5 ~5×10 ^-2 . A containerized green tea beverage containing the green tea extract as claimed in claim 2 or 3. A green tea flavored beverage containing the green tea extract as described in claim 2 or 3. A method for producing animal and plant extracts, comprising the following steps (A) to (D): Step (A): distilling animal and plant raw materials with water vapor to obtain a distillate, Step (B): making the pH of the distillate obtained in step (A) above 8.0, Step (C): freezing the distillate with a pH above 8.0 obtained in step (B), Step (D): thawing the distillate frozen in step (C). The method for producing plant and animal extracts as claimed in claim 6, wherein in the freezing of step (C), the freezing is performed until more than 99% of the entire distillate is in a frozen state. The method for producing plant and animal extracts as claimed in claim 6, wherein in the freezing of step (C), the time required for more than 99% of the entire distillate to be frozen is more than 30 minutes. The method for producing plant and animal extracts as claimed in claim 6, wherein in step (C), the concentration of soluble solid components other than the distillate obtained in step (A) in the distillate obtained in step (B) before freezing is less than 1.0 mass %. The method for producing plant and animal extracts as claimed in claim 6, wherein the steam distillation in step (A) is one or more selected from atmospheric pressure steam distillation, reduced pressure steam distillation, pressurized steam distillation and rotary film steam distillation (SCC). The method for producing plant and animal extracts as claimed in claim 6 further comprises the following step (E) after step (D): step (E): adding a solvent of the same type of plant and animal raw materials as that used in step (A) to the thawing solution obtained in step (D) to extract the extract. For example, the method for producing animal and plant extracts as claimed in claim 11, wherein the solvent-extracted extract of the animal and plant raw materials is the extract obtained by extracting the animal and plant raw materials with an aqueous solvent after and/or before obtaining the steam distillation distillate. The manufacturing method of animal and plant raw material extracts as claimed in claim 12 includes a heat sterilization step. A method for producing plant and animal extracts as claimed in any one of claims 6 to 13, wherein the plant and animal raw materials are coffee or tea. A method for producing a food product, comprising the step of adding an animal or plant extract obtained by the production method of any one of claims 6 to 13 to the food product. A method for producing a flavor composition, comprising the step of adding an animal or plant extract obtained by the production method of any one of claims 6 to 13 to the flavor composition. A method for manufacturing a beverage, comprising the step of adding a flavoring composition obtained by the manufacturing method of claim 16 to the beverage.