Method for producing animal and plant extract

Abstract

The present invention provides a method for producing an animal and plant extract, which comprises the following steps (A)-(D): step (A): a step for obtaining a distillate by subjecting an animal and plant raw material to steam distillation; step (B): a step for adjusting the pH of the distillate obtained in step (A) to 8.0 or more; step (C): a step for freezing the distillate having a pH of 8.0 or more obtained in step (B); step (D): a step for thawing the distillate that has been frozen in step (C). According to the present invention, the animal and plant extract obtained by the production method is added to the food and beverage, such that the food and beverage can be endowed with a unique fragrance. In particular, by adding a small amount of the green tea extract obtained by the production method of the present invention to a green tea beverage, it is possible to provide a tea beverage having a soft and strong green fragrance that freshly brewed tea has.

Description

[0001] This application is a divisional application of the application filed on June 21, 2023, with application number "202310738908.1" and invention title "Method for Manufacturing Animal and Plant Extracts". Technical Field

[0002] This invention relates to a method for manufacturing plant and animal extracts, plant and animal extracts obtained by the manufacturing method, and a method for manufacturing food and beverages containing plant and animal extracts obtained by the manufacturing method. Background Technology

[0003] Steam distillation has been known since ancient times as a method for obtaining aromatic components from natural plants and animals. In addition to its use in the collection of essential oils and the analysis of the aroma of natural substances, it is also applied to the manufacturing of plant and animal extracts with excellent aromas.

[0004] Methods for preparing plant and animal extracts using steam distillation are known, for example, as follows.

[0005] For example: a method for preparing a steam-distilled coffee flavor, characterized in that, in the method of steam distilling the coffee flavor, condensate containing the flavor is collected by fractionation, and the fraction rich in aroma components and low in acidity is utilized (Patent Document 1); a method for manufacturing tea flavor, characterized in that the distillate obtained by steam distilling tea is contacted with tea leaves to remove the heat distillation odor from the distillate (Patent Document 2); a method for manufacturing an extract for a beverage, characterized in that after extracting the beverage raw material with warm water and recovering the extract, the extraction residue is steam-extracted and the distillate is recovered, and the extract and distillate are mixed (Patent Document 3); a novel flavor containing flavor (A) obtained by steam distilling a beverage raw material and flavor (B) obtained by feeding the beverage raw material to a gas-liquid convection contact device, and each 1 part by mass of flavor (A) contains 0.01 to 100 parts by mass of flavor (B). (Patent Document 4); Green tea beverage in a sealed container, characterized by the presence of a distillate, wherein the distillate is obtained by freezing fresh leaves of tea (scientific name: Camellia sinensis (L) O. Kuntze), an evergreen tree of the Theaceae family, and then steam distilling the frozen tea leaves (Patent Document 5); A method for manufacturing coffee extract, characterized by manufacturing through the following steps (1) to (5): (1) a step of extracting roasted coffee beans at a low temperature within a temperature range of 0 to 30°C to obtain a low-temperature extract, (2) a step of storing the low-temperature extract obtained in step (1) at a temperature range of 0 to 30°C, (3) a step of steam distilling the extraction residue from step (1) to obtain a steam distilled extract, (4) A process of mixing the low-temperature extract preserved in the temperature range of 0~30°C through step (2) with the steam distillation extract obtained in step (3) to obtain coffee extract (Patent Document 6); a method for preserving aroma components, which includes a process of applying steam distillation or gas-liquid convection extraction to roasted and crushed coffee beans to recover an aqueous solution containing aroma components of roasted coffee beans, adding an alkaline substance to the aqueous solution containing the aroma components to adjust its pH to 6.6~10, ionizing carbon dioxide gas, storing the pH-adjusted aqueous solution containing aroma components in a container, and freezing the container containing the aqueous solution at a temperature of -10~-50°C (Patent Document 7).

[0006] On the other hand, besides natural extracts or steam distillation, certain sulfur-containing compounds are known to be useful as flavoring compounds added to food and beverages. For example, a method has been proposed to provide a tea beverage with the mild and rich greenscent of freshly brewed tea by adding 4-mercapto-4-methylpentan-2-one as a flavoring compound (Patent Document 8). It should be noted that trace amounts of 4-mercapto-4-methylpentan-2-one are also known to be present in natural green tea (Non-Patent Document 1).

[0007] Existing technical documents Patent documents Patent Document 1: Japanese Patent Application Publication No. 2-203750, Patent Document 2: Japanese Patent Application Publication No. 8-116882, Patent Document 3: Japanese Patent Application Publication No. 2000-135059, Patent Document 4: Japanese Patent Application Publication No. 2003-33137, Patent Document 5: Japanese Patent Application Publication No. 2005-160416, Patent Document 6: Japanese Patent No. 6146915, Patent document 7: Japanese Patent No. 5374020, Patent document 8: Japanese Patent Application Publication No. 2000-342179.

[0008] Non-patent literature 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, 5, 1, 5390-5396). Summary of the Invention

[0009] The problem that the invention aims to solve However, while the aforementioned natural plant and animal extracts obtained through steam distillation can bring a natural feel to food and beverages, they are not sufficient in imparting unique aromas or creating strong aromas with trace amounts.

[0010] Although this invention utilizes a method for preparing natural plant and animal extracts by steam distillation, it provides extracts with a type of aroma that is significantly different in quality from those obtained by conventional steam distillation methods.

[0011] Methods for solving problems The inventors conducted in-depth research on green tea extracts containing distillate (natural aroma recovery product) obtained from green tea raw materials through steam distillation. Surprisingly, they discovered that when the steam distillation distillate of green tea leaves, without the so-called extract portion (an aqueous extract from green tea leaves or steam distillation residue using water or other solvents), was frozen in its distillate-only state (pH 9.2 before freezing), the aroma quality changed significantly upon thawing. When added to beverages, it reproduced the mellow and rich green aroma characteristic of freshly brewed green tea. Furthermore, it was found that through the aforementioned freeze-thaw operation, the 4-mercapto-4-methylpentan-2-one content in the thawed steam distillation distillate significantly increased compared to before freezing, thus completing this invention.

[0012] Therefore, the present invention provides the following content.

[0013] [1] A method for manufacturing green tea extract, comprising the following steps (A) to (D): Process (A): The process of steam distilling green tea to obtain the distillate; Step (B): A step to make the pH of the distillate obtained in step (A) 8.0 or higher; Step (C): The step of freezing the distillate with a pH of 8.0 or higher obtained in step (B); Step (D): The step of thawing the frozen distillate from step (C).

[0014] [2] Green tea extract, which is green tea extract without the addition of 4-mercapto-4-methylpentan-2-one, satisfies the following formula when determining the 4-mercapto-4-methylpentan-2-one in the green tea extract: ((yield (mass) of green tea extract) / (amount (mass) of green tea leaves used as raw material for extraction)) The percentage of 4-mercapto-4-methylpentan-2-one in green tea extract (based on mass) = 1 × 10 -8 ~5×10 -5 .

[0015] [3] Green tea extract, which is green tea extract without the addition of 4-mercapto-4-methylpentan-2-one, satisfies the following formula when the aroma components of the green tea extract are analyzed by GC / MS and the chromatogram is plotted based on the GC / MS analysis results: (Area of ​​the detected peak of 4-mercapto-4-methylpentan-2-one (m / z=132)) / (Area of ​​the detected peak of linalool (total ions)) = 1 × 10 -5 ~5×10 -2 .

[0016] [4] A container for a green tea beverage containing a green tea extract as described in [2] or [3].

[0017] [5] Green tea flavored food and beverage containing green tea extract as described in [2] or [3].

[0018] [6] A method for manufacturing plant and animal extracts, comprising the following steps (A) to (D): Process (A): The process of steam distilling animal and plant raw materials to obtain distillate; Step (B): A step to make the pH of the distillate obtained in step (A) 8.0 or higher; Step (C): The step of freezing the distillate with a pH of 8.0 or higher obtained in step (B); Step (D): The step of thawing the frozen distillate from step (C).

[0019] [7] According to the method for manufacturing plant and animal extracts described in [6], in the freezing process of step (C), the distillate is frozen until more than 99% of the total distillate is in a frozen state.

[0020] [8] According to the method for manufacturing plant and animal extracts described in [6], in the freezing process of step (C), the time required for more than 99% of the total distillate to be frozen is more than 30 minutes.

[0021] [9] According to the method for manufacturing plant and animal extracts as described in [6], in step (C), the concentration of soluble solids other than the distillate obtained in step (A) in the pre-freezing distillate obtained in step (B) is less than 1.0% by mass.

[0022]

[10] According to the method for manufacturing plant and animal extracts described in [6], the steam distillation in step (A) is selected from one or more of atmospheric steam distillation, vacuum steam distillation, pressurized steam distillation and rotary thin-film steam distillation (SCC).

[0023]

[11] The method for manufacturing plant and animal extracts according to [6] further includes the following step (E) after step (D): Step (E): A step of adding a solvent-extracted portion of plant or animal material of the same kind as the raw material used in step (A) to the thawing solution obtained in step (D).

[0024]

[12] According to the method for manufacturing plant and animal extracts described in

[11] , the solvent extraction extract portion of the plant and animal raw materials is the extract portion obtained by extracting the plant and animal raw materials with an aqueous solvent after and / or before obtaining the steam distillation distillate.

[0025]

[13] The method for manufacturing plant and animal extracts according to

[12] includes a heating sterilization step.

[0026]

[14] The method for manufacturing plant and animal extracts according to any one of [6] to

[13] , wherein the plant and animal raw materials are coffee or tea.

[0027]

[15] A method for manufacturing food and beverage, comprising the step of adding plant or animal extracts obtained by any one of the manufacturing methods according to [6] to

[13] to the food and beverage.

[0028]

[16] A method for manufacturing a spice composition, comprising the step of adding plant or animal extracts obtained by any one of the manufacturing methods according to [6] to

[13] into the spice composition.

[0029]

[17] A method for manufacturing a food or beverage, comprising the step of adding a flavoring composition obtained by the manufacturing method according to

[16] to the food or beverage.

[0030] The effects of the invention By incorporating the plant and animal extracts of this invention into food and beverages, unique aromas can be imparted to them. In particular, the green tea extract of this invention has a strong, fresh aroma reminiscent of tea with a hint of fruit when smelled directly. By adding trace amounts of it to green tea beverages, green tea foods, etc., tea beverages and tea foods can be provided with the mellow and rich fresh aroma characteristic of freshly brewed tea. Detailed Implementation

[0031] (Plant and animal ingredients) The animal and plant materials that can be used in this invention are any materials that can be steam distilled. For example, animal materials include meat (muscle, fat, and offal of cattle, pigs, chickens, sheep, horses, etc.), fish and shellfish (marine fish, freshwater fish, white-fleshed fish, red-fleshed fish, squid, octopus, shellfish, shrimp, crab, etc.) and their cooked products. In addition, plant-based ingredients include, for example, teas (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, coriander, black pepper, white pepper, cumin, chili, Sichuan pepper, etc.), fruits (apples, strawberries, grapes, tangerines, oranges, lemons, pineapples, kiwis, etc.), vegetables (cabbage, cabbage, radishes, onions, tomatoes, etc.), and nuts (white sesame seeds, black sesame seeds, walnuts, chestnuts, cashews, macadamia nuts, peanuts, etc.). Among these, coffee and tea are particularly preferred.

[0032] The plant and animal raw materials can be used fresh or through heating treatments such as baking or roasting to enhance or improve their aroma.

[0033] The plant and animal raw materials can be pulverized as needed to achieve a particle size of about 0.1 mm to 10 mm, preferably about 1 mm to 5 mm, in order to improve the aroma recovery rate through distillation.

[0034] (Process (A): The process of steam distilling animal and plant raw materials to obtain distillate) Steam distillation is a phenomenon in which volatile components are distilled off along with steam when steam is blown into the feedstock. When the sum of the vapor pressure (partial pressure) of the volatile substances contained in the feedstock and the vapor pressure (partial pressure) of the steam added from the outside becomes equal to or greater than the surrounding pressure (atmospheric pressure in normal steam distillation), the volatile components are distilled off along with the steam. By cooling the volatile components distilled off with the steam, an aqueous solution containing volatile components (generally known as aroma components) can be obtained as the distillate.

[0035] Steam distillation methods include, for example, atmospheric steam distillation, pressurized steam distillation, and reduced-pressure steam distillation. Other methods include directly blowing steam into a column containing plant or animal materials, wetting the plant or animal materials with a small amount of water before blowing steam into the column, mixing plant or animal materials with water to form a suspension and blowing steam into a vessel filled with the suspension, and steam distillation using an SCC (also known as a "Spinning Cone Column" or "Gas-Liquid Convection Distillation") apparatus.

[0036] For example, in a column-based steam distillation method, steam is blown into the bottom of the steam distillation vessel containing the raw material, and the distillate vapor is cooled by a cooler connected to the upper distillation side, thereby capturing the aroma-containing distillate as condensate. If necessary, by connecting a cold trap using a refrigerant (dry ice-ethanol, dry ice-acetone, liquid nitrogen, etc.) to the front end of this aroma capturing device, aroma components with lower boiling points can also be reliably captured. Furthermore, during steam distillation, if distillation is carried out in the presence of inert gases such as nitrogen and / or antioxidants such as vitamin C, the deterioration of the raw material and / or aroma components due to heating can be effectively prevented. In steam distillation, a large amount of aroma is distilled out initially, and then the amount of aroma gradually decreases. The decision of when to end the distillation is based on the results of several distillations and considerations such as economic efficiency. The amount of distillate collected is 0.1 to 10 parts by mass relative to 1 part by mass of raw material, preferably about 0.2 to 5 parts by mass, and more preferably about 0.5 to 2 parts by mass, to obtain distillate with a Bx of about 0 to 5°.

[0037] In methods using the SCC apparatus, for example, a slurry can be prepared by mixing pulverized raw material (approximately 1-3 mm) with water, and then distilling it using an apparatus as described in Japanese Patent Publication No. 7-22646. Specifically, a method for recovering aroma using this apparatus can be illustrated by using a gas-liquid convection extraction apparatus with an alternating structure of rotating and fixed cones. Liquid or paste-like raw material for a beverage is allowed to flow down from the top while vapor rises from the bottom, thus recovering the aroma components originally present in the raw material. The operating conditions of this gas-liquid convection extraction apparatus can be arbitrarily selected based on the apparatus's processing capacity, the type and concentration of the raw material, and the intensity of the aroma. The ratio of raw material to water in the raw material slurry can be any ratio, as long as the amount of raw material is in a fluid state; an example is approximately 5 to 30 times the amount of water relative to 1 part by mass of the raw material.

[0038] The amount of distillate collected is 0.1 to 10 parts by mass relative to 1 part by mass of animal or plant raw material, preferably about 0.2 to 5 parts by mass, and more preferably about 0.5 to 2 parts by mass, to obtain distillate with a Bx of about 0 to 5°.

[0039] (Step (B): Step to make the pH of the distillate obtained in step (A) 8.0 or higher) Next, the pH of the distillate obtained in step (A) is set to 8.0 or higher. As a result, the reactivity of the components contained in the distillate in subsequent freezing and thawing steps is increased.

[0040] The pH of the distillate is not particularly limited as long as it is 8.0 or higher. Examples of lower limits include 8.0, 8.2, 8.4, 8.6, 8.8, 9.0, 9.2, 9.4, 9.6, 9.8, and 10.0. Similarly, the upper limit is not particularly limited, but examples include 14.0, 13.5, 13.0, 12.5, and 12.0. Furthermore, the pH range of these distillates is typically 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.

[0041] The pH of the distillate can be adjusted using an edible alkaline substance, but since the distillate obtained in step (A) already has a pH of 8.0 or higher, there is no need to adjust it by adding an alkaline substance. Therefore, step (B) also includes confirming that the pH of the distillate obtained in step (A) is 8.0 or higher without adding anything. Examples of edible alkaline substances include sodium bicarbonate, sodium hydroxide, and potassium hydroxide. For example, when using sodium bicarbonate, the amount of sodium bicarbonate added to the distillate can be 0.001 to 0.05 parts by mass relative to 1 part by mass of the distillate, preferably 0.002 to 0.01 parts by mass.

[0042] Additionally, for example, in the case of coffee made from plant or animal ingredients, carbon dioxide produced during roasting is sometimes contained in the raw material. In such raw materials, this carbon dioxide is distilled off by steam distillation and remains in the distillate. As a result, bicarbonate ions and hydrogen ions are present in the distillate, and the pH may sometimes be lowered due to the hydrogen ions. In such cases, the carbon dioxide in the distillate can be expelled as carbon dioxide gas by degassing or nitrogen bubbling, and then the pH can be adjusted to 8.0 or higher, either as is or as needed.

[0043] (Step (C): The step of freezing the distillate with a pH of 8.0 or higher obtained in step (B)) In this invention, the distillate with a pH of 8.0 or higher obtained in step (B) is frozen. This freezing is carried out until almost all of the distillate is frozen, typically until at least 99%, preferably at least 99.5%, more preferably at least 99.8%, and even more preferably at least 99.9% of the total distillate is frozen. Furthermore, this freezing is preferably carried out by gradually freezing the portion in contact with the refrigerant towards the portion not in contact with the refrigerant. It is believed that by employing such a freezing method, crystallization of water (ice) without volatile components as impurities occurs, concentration of volatile compounds occurs in the unfrozen portion, and the effects of this invention are achieved through a chemical reaction occurring in the high-concentration portion of the matrix before the concentrated reaction.

[0044] Such phenomena in this invention are not bound by any theory, but it is speculated that they are produced by the reaction of volatile sulfur-containing compounds such as hydrogen sulfide, methanethiol, and ethanethiol in the distillate under alkaline conditions with other volatile components.

[0045] Examples of freezing methods for producing such a phenomenon include a method of freezing a container by filling it with a predetermined amount of the distillate, and a method of freezing continuously.

[0046] When freezing is performed on a container-by-container basis, time becomes a crucial factor. The time required for freezing until almost all the distillate is frozen should be at least 30 minutes, preferably at least 1 hour, more preferably at least 2 hours, and even more preferably at least 5 hours. If freezing is completed too quickly, the concentration of volatile compounds in the unfrozen portion becomes difficult. The amount of distillate filled into the container is not particularly limited, but is assumed to be approximately 30g (filled in an ounce flask) to 200kg (filled in a drum), as long as a freezing temperature suitable for the size of these containers is appropriately selected.

[0047] Such freezing temperature also depends on the amount of distillate filled into the container, but freezing will occur if the temperature is below 0°C. Examples include typically below -5°C, preferably below -10°C, more preferably below -15°C, and even more preferably below -20°C. On the other hand, if partial freeze-concentration as described above is considered, the reaction may not proceed sufficiently if the freezing temperature is too low, whether it is the whole or a part, under conditions of freezing a large amount in an instant. Therefore, examples include approximately -100°C or higher, preferably above -80°C, more preferably -60°C, even more preferably above -45°C, and particularly preferably above -30°C.

[0048] On the other hand, when the distillate is continuously frozen while flowing, it is preferable to carry out the process under conditions where pure crystallization of ice occurs in the cooled portion, and the process continues until at least 99% of the final distillate is frozen. Under such conditions, the object of the present invention can be achieved without being limited by time.

[0049] Furthermore, in the freezing process described in (C), to achieve the objectives of this invention, it is preferable that the distillate before freezing does not contain solutes other than those from the distillate, such as solvent-extracted portions of the plant or animal raw materials or other soluble (mainly water-soluble) solids. Additionally, if solutes are present, it is preferable that they are present in as small a quantity as possible. As described above, the aroma change phenomenon in this invention is presumably caused by the reaction of volatile sulfur-containing compounds such as hydrogen sulfide, methanethiol, and ethanethiol with other volatile components in the distillate under alkaline conditions during the concentrated portion after freezing and concentration. However, if the distillate contains solvent-extracted portions of the plant or animal raw materials or other soluble (water-soluble) solids, the concentration of volatile sulfur-containing compounds such as hydrogen sulfide, methanethiol, and ethanethiol, or other volatile components, will not increase sufficiently, making the chemical reaction difficult to proceed. Furthermore, the solvent-extracted portions of the plant or animal raw materials also hinder the chemical reaction.

[0050] The solvent extract portion or other soluble (water-soluble) solid portion of the plant or animal raw material in the distillate is typically less than 1.0%, preferably less than 0.5%, more preferably less than 0.2%, and even more preferably less than 0.1%.

[0051] Furthermore, the temperature and time from when almost all the distillate is frozen until the subsequent thawing step (D) are performed do not need to be long, as long as the conditions are met that almost all the distillate is kept frozen and the chemical reaction is fully carried out. While not particularly limited, examples of storage temperatures include 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. As for storage time, examples include generally 30 minutes to 168 hours after almost all the distillate is frozen, preferably 1 hour to 100 hours, and more preferably 2 hours to 48 hours.

[0052] (Step (D): The step of thawing the frozen distillate from step (C)) The frozen distillate from step (C) is then thawed. The thawing method is not particularly limited and can be any of the following: thawing in a cold storage facility (e.g., around 5°C to 10°C), thawing at room temperature (e.g., 15°C to 30°C), or thawing by heating (e.g., 40°C to 100°C). While the thawing time is affected by the container size and the thawing temperature, examples show a general range of 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. Although thawing can completely thaw the entire solution in the container, if the pure ice crystals are concentrated in the center, a portion of the solution can be collected while a part of the whole is thawed.

[0053] Thus, the thawed liquid obtained through processes (A) to (D) possesses a unique aroma significantly different from the distillate before freezing. For example, when the raw material is green tea, the distillate before freezing has a fresh and mellow green tea aroma with hints of seaweed and rocky shore. In contrast, the thawed distillate, when smelled directly, has a strong grassy aroma reminiscent of warm grass and a sweet, fruity scent. However, when the thawed distillate is diluted approximately 100 to 100,000 times, it becomes a mellow and rich aroma reminiscent of freshly brewed green tea, with a slight fruity note.

[0054] (Step (E): The step of adding the solvent extract of the plant or animal material to the thawing solution obtained in step (D)) In this invention, the thawed liquid can also be used directly as a compounding ingredient for imparting flavor to food and beverages. However, if the solvent extract portion of the animal or plant raw material or other soluble (water-soluble) solid portion is added to the thawed distillate after the process (A) to (D), it does not affect the aroma characteristics of the thawed distillate. On the contrary, adding them improves the stability of the product of this invention, which is therefore preferred.

[0055] The preferred ingredient used for addition is generally an aqueous solvent extract of the plant or animal material. This solvent extract can be obtained as follows.

[0056] The plant and animal materials, after and / or before steam distillation, are then extracted with aqueous solvents such as water, aqueous ethanol, glycerol, or aqueous glycerol solution. Water is the preferred solvent. Enzyme treatment may also be performed during and / or after extraction. That is, enzyme treatment can be carried out simultaneously with extraction or after extraction. Furthermore, these methods can be combined.

[0057] Specifically, a method for preparing an extract is described where the residue from column steam distillation is first subjected to water extraction followed by enzyme treatment. For example, it can be obtained by adding 1 to 100 parts by weight of water to each part by weight of the aforementioned steam-distilled plant or animal material. Extraction is carried out for approximately 2 minutes to approximately 5 hours at room temperature to approximately 100°C, depending on the operating temperature, under static or stirring conditions. After cooling, insoluble matter is removed by solid-liquid separation using known methods such as centrifugation, pressing, or filtration. Alternatively, it can be obtained, for example, by filling the residue material into a column of suitable material such as glass or stainless steel, and using a metering pump to flow hot water at room temperature to approximately 100°C from the top or bottom of the column for column extraction. Such column extraction can be performed by connecting multiple columns in series as desired.

[0058] In addition, when aroma is recovered by gas-liquid convection contact extraction, since the residue has become a slurry containing the extract, the solid part of the residue can be separated into solid and liquid components by known methods such as centrifugation, pressing, and filtration to remove insoluble matter and obtain the extract.

[0059] The method described above, which involves collecting the extract before enzyme treatment, can also be used. However, in this invention, enzyme treatment can also be performed while the animal and plant materials are still containing the steam-distilled raw materials. By performing enzyme treatment while the animal and plant materials are still containing the steam-distilled raw materials, the soluble solids portion increases due to enzymatic hydrolysis, thereby improving the yield of the soluble solids portion of the extract derived from the animal and plant materials.

[0060] The enzymes used can be those corresponding to the animal or plant raw materials. For example, if the raw material is animal, proteases and lipases can be used; if the raw material is plant, cellulase, pectinase, hemicellulase, amylase, tanninase, protease, and lipase can be used. In addition, mannanase can be specifically mentioned when the raw material is coffee, and tanninase can be specifically mentioned as a preferred enzyme when the raw material is tea.

[0061] Enzyme treatment solution can be deactivated by heating or other means, and then solid-liquid separation and filtration can be performed in the presence of slurry to obtain extract.

[0062] The extract or enzyme-treated solution of the water-soluble solvent can be further concentrated as needed. Concentration methods may include, for example, vacuum concentration, reverse osmosis (RO) membrane concentration, or freeze concentration, to obtain a concentrate of the water-soluble solvent extract or enzyme-treated extract. The concentration of the concentrate is generally suitable in the range of 3° to 50°, preferably 10° to 40°.

[0063] The solvent-extracted fraction of the plant and animal raw materials (extracts in water-soluble solvents or enzyme-treated solutions, or their concentrates) can be mixed with the thawed distillate from step (D). The mixing ratio is not particularly limited, and the amount of the solvent-extracted fraction of the plant and animal raw materials relative to the thawed distillate varies depending on the raw materials used and is not particularly limited. However, for example, the amount of the solvent-extracted fraction of the plant and animal raw materials per 1 part by mass of the distillate can be typically in the range of 0.005 to 100 parts by mass, preferably 0.01 to 50 parts by mass, more preferably 0.1 to 20 parts by mass, and even more preferably 0.5 to 10 parts by mass.

[0064] (Heat sterilization) The plant and animal extracts of the present invention can be made into microbially stable extracts by heat sterilization at any stage of the process. The heat sterilization stage can be carried out at any stage as long as it does not impede the chemical reaction caused by freezing, which is the objective of the present invention. Preferably, examples include intermediate and final stages of the process for preparing the solvent-extracted portion of the plant and animal raw materials, and after mixing the solvent-extracted portion of the plant and animal raw materials with the thawed distillate from step (D).

[0065] Heat sterilization can be performed in either batch or plate manner. In batch sterilization, the temperature can be typically 80°C to 110°C, preferably 85°C to 105°C, and more preferably 90°C to 100°C. The time can be typically 30 seconds to 60 minutes, preferably 1 minute to 30 minutes, and more preferably 2 minutes to 15 minutes. In plate sterilization, the temperature can be typically 80°C to 140°C, preferably 85°C to 135°C, and more preferably 90°C to 130°C. The time can be typically 10 seconds to 5 minutes, preferably 20 seconds to 3 minutes, and more preferably 30 seconds to 2 minutes.

[0066] The plant and animal extracts obtained in this way can be filled into containers after cooling or filled into containers while hot and then cooled for freezing preservation. Furthermore, the aroma changes during this freezing stage are minimal. This is presumably because the chemical reactions in steps (A) to (D) are fully carried out, the solvent-extracted plant and animal materials added in step (E) partially hinder the chemical reactions, the concentration of the matrix involved in the reaction is partially diluted by the solvent-extracted plant and animal materials, and the pH decreases.

[0067] (A specific example of plant and animal raw materials – green tea) If suitable specific examples of the plant and animal raw materials described in this invention are listed, tea can be cited as an example, particularly green tea, and especially new tea. When new tea is subjected to steam distillation in step (A), the pH of the resulting distillate is mostly around 9, even without pH adjustment. This is presumably due to the high content of alkaline volatile components. The steam distillate thus obtained has a gentle aroma with a hint of rocky, angular fragrance.

[0068] If the distillate of the newly obtained tea is frozen and then thawed under the conditions detailed in step (C), the aroma undergoes a significant change, becoming a strong, green tea aroma with a hint of fruitiness. Analysis of the aroma components revealed that it contains a large amount of sulfur-containing compounds, primarily 4-mercapto-4-methylpentan-2-one, as a characteristic component. On the other hand, the distillate before freezing contains only trace amounts of 4-mercapto-4-methylpentan-2-one. According to Non-Patent Literature 1, the highest concentration of 4-mercapto-4-methylpentan-2-one in tea is reported to be 0.14 ppb. However, it has been determined that even without the external addition of 4-mercapto-4-methylpentan-2-one, the green tea extract obtained by the method for producing plant and animal extracts of the present invention generates a large amount of 4-mercapto-4-methylpentan-2-one by subjecting the steam distillation distillate of green tea, especially new tea, to the processes described in (A) to (D). The amount of 4-mercapto-4-methylpentan-2-one can be increased by thousands to tens of thousands of times compared to the distillate before freezing. Therefore, when using green tea as the raw material, by using compounds that are generally present in green tea and that change little during the freezing-thawing process of the present invention as indicators, and by setting a range for the ratio of the content of these indicator compounds to 4-mercapto-4-methylpentan-2-one, the product of the present invention made from green tea can be specifically determined. Examples of suitable index compounds for such a design include linalool, indole, cis-3-hexenol, hexanal, linalool oxide, isobutyraldehyde, geraniol, hexanol, octanol, benzyl alcohol, trans-2-nonenal, and β-ionone. Linalool is a preferred example among these.

[0069] (Aroma Analysis) Aroma analysis can be performed using appropriate GC columns and apparatus, GC / MS apparatus, and appropriate SPME, etc.

[0070] Quantification can be performed by plotting chromatograms from GC / MS analysis results, using the area values ​​of the detected peaks, or by using the absolute standard curve method, standard addition method, or internal standard method.

[0071] (4-Mercapto-4-methylpentan-2-one) The amount of 4-mercapto-4-methylpentan-2-one of the present invention, obtained by means of green tea as raw material, is within the following range when the ion chromatogram of the extracted product is plotted at m / z = 132 by GC / MS analysis, using the area of ​​the detected peak, and determined by the standard addition method.

[0072] The percentage of 4-mercapto-4-methylpentan-2-one in the green tea extract (based on mass) is typically 1 × 10⁻⁶. This is calculated as ((yield (mass) of green tea extract) / (amount (mass) of green tea leaves used as extraction raw material)) × the percentage of 4-mercapto-4-methylpentan-2-one in the green tea extract. -8 The preferred value is 5×10. -8 The above is preferred, specifically 2×10 -7 The above is further optimized to be 5×10 -7 That's all. Additionally, as an upper limit, there's no specific requirement; it's typically around 5 × 10. -5 The following can be set to 3×10 -5 Below, 2×10 -5 Below, 1×10 -5 Below, 5×10 -4 Below, 4×10 -4 The following are examples. The upper and lower limits can be combined arbitrarily; for instance, a range of 1×102 can be exemplified. -8 ~5×10 -5 The range.

[0073] Furthermore, the amount of 4-mercapto-4-methylpentane-2-one in the plant extract (green tea extract) of the present invention, which is made from green tea as a raw material, varies depending on the yield of the present invention from the raw tea leaves, but is within the following range when quantified by the same analytical method as described above.

[0074] The percentage of 4-mercapto-4-methylpentan-2-one in the green tea extract (based on mass) is typically 1 × 10⁻⁶. This is calculated as ((yield (mass) of green tea extract) / (amount (mass) of green tea leaves used as extraction raw material)) × the percentage of 4-mercapto-4-methylpentan-2-one in the green tea extract. -8 The preferred value is 5×10. -8 The above is preferred, specifically 2×10 -7 The above is further optimized to be 5×10 -7 That's all. Additionally, as an upper limit, there's no specific requirement; it's typically around 5 × 10. -5 The following can be set to 3×10 -5 Below, 2×10 -5 Below, 1×10 -5 Below, 5×10 -4 Below, 4×10 -4 The following are examples. The upper and lower limits can be combined arbitrarily; for instance, a range of 1×102 can be exemplified.-8 ~5×10 -5 The range.

[0075] Furthermore, the content of 4-mercapto-4-methylpentan-2-one in the present invention, which uses green tea as a raw material, can also be indicated by linalool, a volatile compound commonly found in green tea. Based on the GC / MS analysis results under these conditions, an ion chromatogram is plotted with m / z = 132 (4-mercapto-4-methylpentan-2-one) and total ions (linalool). The area of ​​the detected peaks is used, calculated as (area of ​​the detected 4-mercapto-4-methylpentan-2-one peak (m / z = 132)) / (area of ​​the detected linalool peak (total ions)). This is typically set to 1 × 10⁻⁶. -5 Above, 2×10 -5 Above, 5×10 -5 Above, 1×10 -4 The above, etc. Additionally, as an upper limit, no special limitation is needed; it is typically around 5 × 10. -2 The following can be set to 3×10 -2 Below, 2×10 -2 Below, 1×10 -2 Below, 5×10 -3 Below, 3×10 -3 The following are examples. The upper and lower limits can be combined arbitrarily; for instance, a range of 1×102 can be exemplified. -5 ~5×10 -2 The range.

[0076] (Fragrance composition) The plant and animal extracts obtained in this way (hereinafter sometimes referred to as the plant and animal extracts of this invention) can also be added to food and beverages to impart a unique flavor, and can also be used as raw materials for flavoring compositions (hereinafter sometimes referred to as flavoring compositions of this invention). One embodiment of the present invention relates to a flavoring composition containing a predetermined amount of the plant and animal extracts of this invention, intended to impart flavor, and suitable for incorporation into various food and beverages. According to the flavoring composition of this invention, for example, a natural, juicy, moist, full-bodied, mature, luxurious, fresh, aromatic, bitter, spicy, mellow, or full-bodied flavor can be imparted to the flavoring composition, thereby improving the flavor of various food and beverages incorporating the flavoring composition of this invention.

[0077] The concentration of the plant and animal extracts in the fragrance composition can be arbitrarily determined according to the compounding ingredients of the fragrance composition. As an example of such concentration, a range of 0.1 ppt to 10%, preferably 1 ppb to 1%, and more preferably 0.1 ppm to 0.1% relative to the total mass of the fragrance composition can be listed.

[0078] In addition to the plant and animal extracts described herein, the flavoring composition may further contain any other arbitrary compounds or ingredients. Examples of such compounds or ingredients include various types of flavoring compounds or flavoring compositions, oil-soluble pigments, vitamins, functional substances, fish extracts, meat extracts, plant extracts, yeast extracts, plant and animal proteins, plant and animal protein decomposition products, starch, dextrin, sugars, amino acids, nucleic acids, organic acids, solvents, etc. For example, examples include natural essential oils, natural flavorings, and synthetic flavorings as recorded in "Japan Patent Office Gazette, Commonly Used Techniques (Flavors) Part II Food Flavorings, issued January 14, 2012", "Survey on the Use of Food Flavoring Compounds in Japan" (Heisei 12 Annual Health and Welfare Scientific Research Report, Japan Flavor Industry Association, issued March 2013), and "Synthetic Flavoring Chemistry and Commercial Knowledge" (supplemented and reissued December 20, 2016, edited by the Synthetic Flavoring Editorial Committee, Chemical Industry Daily).

[0079] Specific examples of synthetic fragrance compounds include, as hydrocarbon compounds, monoterpenes such as α-pinene, β-pinene, γ-terpinene, myrcene, limonene, etc.; sesquiterpenes such as valencene, cedrene, caryophyllene, longleafene, etc.; and 1,3,5-undecanetriene, etc.

[0080] As alcohol compounds, examples include saturated alcohols such as butanol, pentanol, 3-octanol, and hexanol; unsaturated alcohols such as (Z)-3-hexen-1-ol, isopentenol, and 2,6-nonadienol; terpenols such as linalool, geraniol, citronellol, tetrahydromyrceneol, farnesol, nerolidol, cedrol, α-terpineol, terpinen-4-ol, and borneol; and aromatic alcohols such as benzyl alcohol, phenethyl alcohol, and cinnamyl alcohol.

[0081] Aldehydes include saturated aldehydes such as acetaldehyde, hexanal, octanal, decanal, and hydroxycitronellol; unsaturated aldehydes such as (E)-2-hexenal and 2,4-octadienal; terpenoid aldehydes such as citronellol, citral, myrtol, and perillaldehyde; and aromatic aldehydes such as benzaldehyde, cinnamaldehyde, vanillin, ethyl vanillin, piperaldehyde, and p-methylbenzaldehyde.

[0082] As ketone compounds, examples include saturated and unsaturated ketones such as 2-heptanone, 2-undecanone, 1-octen-3-one, acetoin, and 6-methyl-5-hepten-2-one (methylheptenone); diketones and hydroxy ketones such as diacetone, 2,3-pentanedione, maltol, ethyl maltol, methylcyclopentenolone, and 2,5-dimethyl-4-hydroxy-3(2H)-furanone; terpene ketones such as carvone, menthone, and nocaketone; ketones derived from terpene decomposition products such as α-ionone, β-ionone, and β-damastenone; and aromatic ketones such as raspberry ketone.

[0083] Examples of furan or ether compounds include furfuryl alcohol, furfural, rose oxide, linalool oxide, menthol, theaspirane, artemisinin, eugenol, and 1,8-cineole.

[0084] Examples of ester compounds include aliphatic esters such as ethyl acetate, isoamyl acetate, octyl acetate, ethyl butyrate, isobutyrate, isoamyl butyrate, 2-methylbutyrate, isovalerate, 2-methylbutyrate, ethyl hexanoate, allyl hexanoate, ethyl heptaate, ethyl octanoate, isovalerate, and ethyl nonanoate; terpene alcohol esters such as linalyl acetate, geranyl acetate, lavender acetate, terpineol acetate, and nerol acetate; and aromatic esters such as benzyl acetate, methyl salicylate, methyl cinnamate, cinnamonyl propionate, ethyl benzoate, cinnamonyl isovalerate, and ethyl 3-methyl-2-phenylglycidyl acid.

[0085] As lactone compounds, examples include saturated lactones such as γ-decyl lactone, γ-dodecyl lactone, δ-decyl lactone, and δ-dodecyl lactone, and unsaturated lactones such as 7-decene-4-lactone and 2-decene-5-lactone.

[0086] As acid compounds, examples include saturated / unsaturated fatty acids such as acetic acid, butyric acid, isovaleric acid, hexanoic acid, caprylic acid, stearic acid, oleic acid, linoleic acid, and linolenic acid.

[0087] Examples of nitrogen-containing compounds include indole, skatole, pyridine, alkyl-substituted pyrazines, methyl anthranilate, and trimethylpyrazine.

[0088] Examples of sulfur-containing compounds include methanethiol, dimethyl sulfide, dimethyl disulfide, allyl isothiocyanate, 3-methyl-2-buten-1-thiol, 3-methyl-2-butanethiol, 3-methyl-1-butanethiol, 2-methyl-1-butanethiol, 3-mercaptohexanol, 4-mercapto-4-methyl-2-pentanone, 3-mercaptohexyl acetate, p-menth-8-thiol-3-one, and furfuryl thiol.

[0089] As natural essential oils, examples include sweet orange, bitter orange, petitgrain, lemon, bergamot, mandarin, orange blossom, peppermint, spearmint, lavender, chamomile, rosemary, eucalyptus, sage, basil, rose, hyacinth, lilac, geranium, jasmine, ylang-ylang, fennel, clove, ginger, nutmeg, cardamom, cedar, cypress, vetiver, patchouli, and rockrose.

[0090] Examples of various plant and animal extracts include extracts of herbs or spices, extracts of coffee, green tea, black tea or oolong tea, or milk or dairy products and their various enzymatic breakdown products such as lipases or proteases.

[0091] The fragrance composition of this case can be prepared by combining the plant and animal extracts of this case with a suitable solvent or dispersion medium using known methods.

[0092] The preferred form of the fragrance composition in this case is a solution, emulsion, powder, or other solid preparation (such as solid lipids) formed by dissolving the plant or animal extracts or other ingredients in a water-soluble or oil-soluble solvent.

[0093] Examples of water-soluble solvents include ethanol, methanol, acetone, tetrahydrofuran, acetonitrile, 2-propanol, methyl ethyl ketone, glycerol, propylene glycol, and dipropylene glycol. From the viewpoint of use in food and beverages, ethanol or glycerol is particularly preferred. Examples of oil-soluble solvents include vegetable oils, animal oils, purified oils (e.g., processed oils such as medium-chain triglycerides, or short-chain triglycerides such as triacetylglycerol and tripropionate), various essential oils, and triethyl citrate.

[0094] Furthermore, to prepare an emulsified formulation, the plant and animal extracts or the flavoring composition of this invention can be emulsified together with a water-soluble solvent and an emulsifier. There are no particular limitations on the emulsification method for the plant and animal extracts or the flavoring composition of this invention. Various types of emulsifiers conventionally used in food and beverages, such as monoglycerides, diglycerides, triglycerides, propylene glycol fatty acid esters, sucrose fatty acid esters, polyglycerol fatty acid esters, lecithin, processed starch, sorbitol fatty acid esters, quillaia extract, gum arabic, tragacanth gum, guar gum, guilarin gum, xanthan gum, pectin, alginic acid and its salts, carrageenan, gelatin, casein saponins, or sodium caseinate, can be used for emulsification using a homogenizer, colloid mill, rotary disc homogenizer, or high-pressure homogenizer to obtain an emulsion with excellent stability. There are no strict limitations on the amount of these emulsifiers used, and they can vary widely depending on the type of emulsifier used. However, it is generally appropriate to use approximately 0.01 to approximately 100 parts by weight, preferably approximately 0.1 to approximately 50 parts by weight, relative to 1 part by weight of the plant or animal extracts of this invention. In addition, to stabilize the emulsion, in addition to water, one or more polyols such as glycerol, propylene glycol, sorbitol, maltitol, sucrose, glucose, trehalose, sugar solution, and reducing sugar syrup may be added to the emulsion.

[0095] Furthermore, the resulting emulsion can be dried to form a powder if needed. During pulverization, sugars such as gum arabic, trehalose, dextrin, sucrose, lactose, glucose, syrup, and reducing syrup can be added as needed. The amount used can be appropriately selected based on the desired properties of the powder formulation.

[0096] The plant and animal extracts or flavoring compositions obtained in this way, when added in effective amounts to food and beverages, can improve the natural, juicy, moist, full-bodied, mature, luxurious, fresh, aromatic, bitter, spicy, mellow, or full-bodied flavors of food and beverages.

[0097] In particular, when the plant or animal raw material is green tea, the green tea extract of this invention or a flavoring composition containing the green tea extract of this invention can be added in small amounts to green tea beverages, green tea foods, etc., to provide tea beverages or tea foods with the mild and rich aroma of freshly brewed tea.

[0098] (Food and Beverages) There are no particular limitations on the food and beverages that can be combined with the plant and animal extracts or flavoring compositions of this application. Examples include food and beverages having one or more of the following flavors: lemon, orange, grapefruit, lime, Chinese tangerine, mandarin orange, sour orange, hachisaku mandarin orange, iyokan, pomelo, flat lemon, kumquat, and other citrus flavors; strawberry, blueberry, raspberry, apple, cherry, plum, apricot, peach, pineapple, banana, melon, mango, papaya, kiwi, pear, grape, muscat grape, Kyoho grape, and other fruit flavors; milk, yogurt, butter, and other dairy flavors; vanilla flavor; green tea, black tea, oolong tea, herbal tea, and other tea flavors; coffee flavor; cola flavor; cocoa bean flavor; cocoa flavor; green mint, peppermint, and other mint flavors; cinnamon, chamomile, cardamom, caraway, cumin, clove, pepper, coriander, Sichuan pepper, perilla, ginger, and other flavors. Flavors of various spices or herbs such as anise, thyme, chili, nutmeg, basil, marjoram, rosemary, bay leaf, garlic, and mustard; flavors of various nuts such as almonds, cashews, and walnuts; flavors of various alcoholic beverages such as wine, brandy, whiskey, rum, gin, liqueur, sake, shochu, and beer; flavors of vegetables such as onions, celery, carrots, tomatoes, and cucumbers; flavors of various meats such as chicken, duck, pork, beef, lamb, and horse meat. Flavors of various types of livestock meat; red-fleshed fish such as tuna; white-fleshed fish such as mackerel, sea bream, salmon, and horse mackerel; freshwater fish such as sweetfish, trout, and carp; shellfish such as snails, clams, oysters, and mussels; various crustaceans such as shrimp and crab; and various seaweed such as wakame and kelp; flavors of various grains such as rice, barley, wheat, and malt; and flavors of various oils such as beef tallow, chicken fat, lard, and the fats of various types of livestock meat or fish.

[0099] More specific examples of food and beverages include: rice crackers, millet cakes, rice candy, rice cakes, steamed buns, rice flour cakes, fillings, yokan (sweet bean jelly), soft yokan, agar jelly, jelly, castella cake, sugar balls, biscuits, crisps, potato chips, cookies, pies, puddings, buttercream, and custard. Cream, puffs, waffles, sponge cakes, donuts, chocolate, chewing gum, caramel, candy, peanut butter and other sauces; bread, udon noodles, ramen, Chinese noodles, sushi, mixed rice, fried rice, spicy pilaf, dumpling wrappers, shumai wrappers, Japanese mixed omelet, takoyaki and other bread, noodle and rice dishes; rice bran pickles, dried plums, fukujin pickles, rice koji pickled daikon radish pickles, thinly sliced ​​turnip pickles, scallions, miso pickles, rice bran pickled radish pickles and the seasonings for these pickles; mackerel, sardines, saury, salmon, tuna, bonito, whale, halibut, sand eel, sweetfish and other fish, squid, longfin squid, etc. Squid such as the spotted squid and firefly squid; octopus such as the true octopus and short octopus; shrimp such as prawns, peony shrimp, Ise lobster, and black tiger shrimp; crabs such as king crab, snow crab, swimming crab, and hairy crab; and shellfish such as clams, hard clams, scallops, oysters, and mussels; processed foods and beverages of fish and shellfish such as canned fish, stewed fish, salted seafood, minced meat, seafood stews (chikuwa fish rolls, fish cakes, fried fish cakes, crab sticks, etc.), fried foods, and tempura; meats such as chicken, pork, beef, mutton, and horse meat; seasonings for curry, stews, stewed beef, Japanese beef risotto sauce, tomato meat sauce, mapo tofu, hamburger patties, dumplings, and consommé; and soups (corn soup, tomato soup, consommé). Processed foods and beverages using meat, such as soup, meatballs, roasted pork chunks, and canned meat; table salt, seasoning salt, soy sauce, soy sauce powder, miso, miso powder, fermented rice wine, salted meat sauce, rice bowl powder, ochazuke seasoning, margarine, mayonnaise, sauces, vinegar, three-cup vinegar, sushi vinegar powder, Chinese food seasonings, tempura dipping sauce, noodle dipping sauce (kelp broth or bonito broth, etc.), sauces (medium-thick sauce, tomato sauce, etc.), ketchup, barbecue sauce, and curry sauce. Seasonings for stews, soups, and broths (such as kelp broth or bonito broth), compound seasonings, new-style cooking wines, and mixed powders such as fried chicken powder / takoyaki powder; animal- or plant-based flavored foods and beverages containing these seasonings; dairy products such as cheese, yogurt, and butter; various yeasts such as brewer's yeast and baker's yeast, and various microbial fermented products such as lactic acid bacteria; stews such as vegetable stews, Chikuzen-ni, Oden, and hot pot; ingredients and side dishes for takeout meals; fruit juices or refreshing drinks containing fruit juices, fruit pulp drinks, or fruit drinks containing fruit pieces from fruits such as apples, grapes, and citrus fruits (grapefruit, oranges, lemons, etc.).Vegetables such as tomatoes, green peppers, celery, melons, bitter melons, carrots, potatoes, asparagus, bracken, and osmanthus, or vegetable-based beverages and soups containing these vegetables; beverages containing coffee, cocoa, green tea, black tea, oolong tea, soft drinks, cola drinks, carbonated drinks (citrus-flavored and other flavored soft drinks), lactic acid bacteria drinks, etc.; beverages containing raw herbs or medicinal materials; cola drinks, fruit juice drinks, dairy drinks, beer-flavored drinks containing non-alcoholic beer or so-called "third-category beer," and sports drinks. Functional beverages such as beverages containing ingredients, honey, vitamins, minerals, nutrients, nourishing drinks, and lactic acid bacteria; non-alcoholic beverages such as alcoholic drinks with various alcoholic flavors (beer-flavored, plum-flavored, carbonated shochu-flavored, etc.); and alcoholic beverages containing wine, shochu, awamori, sake, beer, carbonated shochu, cocktails, sparkling wine, fruit wine, medicinal wine, and so-called "third-category beer," etc.

[0100] The amount of plant and animal extracts or flavoring compositions added to the food and beverage can be arbitrarily determined based on the flavor of the food and beverage or the degree of desired effect.

[0101] As an example of the concentration of this addition amount, if it is a food or beverage, the concentration of the plant or animal extract or flavoring composition of this invention relative to the total mass of the food or beverage can be listed in the range of 0.001 ppt to 0.1%, preferably 1 ppt to 100 ppm, and more preferably 1 ppb to 100 ppm. More specifically, setting the lower limit to any one of 0.001 ppt, 0.01 ppt, 0.1 ppt, 1 ppt, 10 ppt, 100 ppt, 1 ppb, 10 ppb, 100 ppb, 1 ppm, 10 ppm, and 100 ppm, and setting the upper limit to any one of 0.1%, 100 ppm, 10 ppm, 1 ppm, 100 ppb, 10 ppb, 1 ppb, 100 ppt, 10 ppt, 1 ppt, 0.1 ppt, and 0.01 ppt, can be listed within any combination of these lower and upper limits, but is not limited to them. As an example of a preferred concentration, the concentration of the plant and animal extracts or flavoring composition of this invention relative to the total mass of the food or beverage may be selected from, but is not limited to, 100 ppt to 100 ppb, 100 ppt to 1 ppm, 1 ppb to 100 ppb, 1 ppb to 1 ppm, 10 ppb to 1 ppm, 10 ppb to 100 ppb, 100 ppb to 10 ppm, or 1 ppm to 100 ppm, depending on the flavor characteristics of the food or beverage.

[0102] The present invention will be described in more detail below through embodiments, but the essence of the present invention lies in the technical ideas disclosed above and is not limited by the embodiments. Example

[0103] (Example 1) 600g of fresh tea leaves from Shizuoka Prefecture (Yabukata variety, lightly steamed) were packed into a 3L column. 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 purging the column with nitrogen, nitrogen-mixed water vapor was blown in from the bottom. The water vapor containing the volatile components of the tea obtained from the top of the column was condensed through a cooling tube (cooled with tap water, approximately 20°C). After approximately 20 minutes, 300g (50% relative to the tea leaves) of distillate containing the volatile components of the tea was obtained. The pH of the resulting distillate was 9.2.

[0104] The distillate was dispensed in equal portions (150g each) into 300ml amber bottles. After purging the headspace with nitrogen, one bottle was stored in a refrigerator (5°C) (Comparative Product 1), and the other in a freezer (-20°C). The bottle stored in the freezer began to freeze approximately 30 minutes after being placed in the freezer and was almost completely frozen in about 3 hours. Both were stored in the aforementioned condition for approximately 20 hours from the start of storage, and then placed at room temperature (23°C). The frozen product thawed completely in about 2 hours, yielding the frozen-thawed product (Inventory Product 1: pH 9.2).

[0105] Both were diluted with water to 0.1% and then subjected to sensory evaluation. The aroma profiles of each are summarized below.

[0106] Comparative Product 1 (Refrigerated): A fresh and mellow green tea aroma with hints of seaweed and rocky cliff. Product 1 of this invention (frozen-thawed): has a strong, fresh green tea aroma with tropical fruit notes. Aroma analysis was performed on each sample using the following methods.

[0107] Analyze 1g of sample solution (comparative sample 1, present invention sample 1) either as is or by adding 1 ppb, 10 ppb, 100 ppb or 1000 ppb of 4-mercapto-4-methylpentane-2-one standard to each sample.

[0108] Analysis conditions • Device Gas chromatography apparatus: 7890B GC system, manufactured by Agilent Technologies. MSD device: 5977B MSD, manufactured by Agilent Technologies. ·column InertCap WAX 0.25 mmφ × 30 m (film thickness 0.25 μm), manufactured by GL Sciences Inc. SPME fiber 50 / 30 μm DVB / CAR / PDMS StableFlex / SS (2cm), manufactured by Merck (Supelco: registered trademark). • Sample size: 1g Small bottle capacity: 20ml • Equilibrium conditions for the sample: stirring at 60°C for 30 minutes. SPME extraction conditions: stand at 60℃ for 30 minutes. • Inlet temperature: 250℃ • Temperature conditions: Hold at 40°C for 8 minutes, then increase to 180°C at a rate of 4°C / min, followed by an increase to 230°C at a rate of 3°C / min, and hold at 230°C for 10 minutes. Carrier gas: He (constant pressure) • Injection method: No branching • Flow rate: 1.2 ml / min It should be noted that when plotting chromatograms from GC / MS analysis results, the peak of 4-mercapto-4-methylpentan-2-one was plotted using m / z = 132, and the peak of linalool was plotted using total ions. The area values ​​of each peak were used for quantification.

[0109] (Analysis Results) GC / MS confirmed the presence of a large amount of 4-mercapto-4-methylpentan-2-one in the frozen-thawed product.

[0110] In addition, the content of 4-mercapto-4-methylpentane-2-one obtained by the standard addition method in the sample is shown below.

[0111] Comparative standard 1: 0.25 ppb Product 1 of this invention: 495.9 ppb Furthermore, the peak area of ​​4-mercapto-4-methylpentan-2-one in sample 1 of this invention (the sample without the addition of 4-mercapto-4-methylpentan-2-one as a standard) is 9.9 × 10⁻⁶. 4 The area value of linalool is 3.9 × 10⁻⁶. 8 The peak area of ​​4-mercapto-4-methylpentan-2-one in Comparative Sample 1 was 49.9, while the peak area of ​​linalool was 3.9 × 10⁻⁶. 8 .

[0112] The above results confirm that the present invention sample 1 contains approximately 2,000 times more 4-mercapto-4-methylpentane-2-one compared to comparative sample 1.

[0113] Furthermore, since product 1 of the present invention is obtained by using 600g of green tea leaves as raw material to produce 300g of product 1 of the present invention, the proportion (based on mass) of 4-mercapto-4-methylpentan-2-one in the green tea extract is 2.5 × 10⁻⁶. -7 .

[0114] In contrast, in Comparative Product 1, the proportion (based on mass) of 4-mercapto-4-methylpentan-2-one in the green tea extract was 1.75 × 10⁻⁶. ((yield (mass) of green tea extract) / (amount (mass) of green tea leaves used as extraction raw material)) × 10⁻⁶ -10 .

[0115] Furthermore, the area of ​​the detected 4-mercapto-4-methylpentan-2-one peak (m / z = 132) / the area of ​​the detected linalool peak (total ions) in product 1 of the present invention is 2.5 × 10⁻⁶. -4 .

[0116] In contrast, in Comparative Standard 1, the area of ​​the peak of 4-mercapto-4-methylpentan-2-one (m / z = 132) / the area of ​​the peak of linalool (total ions) was 1.25 × 10⁻⁶. -7 .

[0117] (Example 2) First, the present invention sample 1 and comparative sample 1 were obtained by the same procedure as in Example 1. Next, 4800 g of 40°C warm water (0.05% sodium ascorbate aqueous solution) was fed into the column at a flow rate of 60 ml / min from the top, and 3000 g of extract at Bx 3° was collected from the bottom of the column. The collected extract was cooled to 20°C and centrifuged at 3000 rpm for 10 minutes to remove the precipitate, yielding the water extract (reference sample 1, Bx 3.0°, pH 5.6).

[0118] The present invention sample 1 and reference sample 1 were each mixed at 150g, sterilized at 90°C for 10 minutes, cooled to 20°C, and then filled to obtain green tea extract (present invention sample 2) (Bx 1.6°, pH 6.7). Alternatively, the comparative sample 1 and reference sample 1 were each mixed at 150g, sterilized at 90°C for 10 minutes, cooled to 20°C, and then filled to obtain green tea extract (comparative sample 2) (Bx 1.6°, pH 6.7).

[0119] The content of 4-mercapto-4-methylpentan-2-one was also determined by the aforementioned analytical method for both Comparative Product 2 and Product 2 of the present invention. The results are shown below.

[0120] Comparative sample 2: 0.11 ppb Product 2 of this invention: 245.9 ppb As described above, in Comparative Product 2 and Product 2 of the present invention, the calculated amounts of 4-mercapto-4-methylpentan-2-one, which are considered to be derived from Comparative Product 1 and Product 1 of the present invention, were confirmed to be almost the same, indicating that the content of 4-mercapto-4-methylpentan-2-one is not easily affected by the addition of water extract of green tea to the distillate or by heating for sterilization.

[0121] In addition, for Comparative Sample 2 and Sample 2 of the present invention, the area of ​​the peak of 4-mercapto-4-methylpentan-2-one (m / z = 132) / the area of ​​the peak of linalool (total ions) was also determined by the analytical method described above. The results are shown below.

[0122] The area of ​​the peak of 4-mercapto-4-methylpentan-2-one (m / z = 132) detected in Comparative Standard 2 / the area of ​​the peak of linalool (total ions) detected = 5.5 × 10⁻⁶ -8 The area of ​​the detected peak of 4-mercapto-4-methylpentan-2-one (m / z = 132) / the area of ​​the detected peak of linalool (total ions) in product 2 of this invention is 1.1 × 10⁻⁶. -4 As described above, in Comparative Sample 2 and Sample 2 of the present invention, values ​​were confirmed to be almost at the same level as those considered to be from Comparative Sample 1 and Sample 1 of the present invention (area value of the detected peak of 4-mercapto-4-methylpentan-2-one (m / z = 132) / (area value of the detected peak of linalool (total ions)). This indicates that the content of linalool or 4-mercapto-4-methylpentan-2-one is not easily affected by the addition of water extract of green tea to the distillate or by heat sterilization.

[0123] (Comparative Example 1) The 300g of Comparative Sample 2 (pH 6.7) was readjusted and divided into two 150g portions. One portion was prepared to pH 9.5 using a 1% potassium hydroxide aqueous solution. Each portion was placed in a 300ml amber bottle, and after nitrogen replacement of the headspace, it was stored in a freezer (-20°C). The sample stored in the freezer began to freeze approximately 30 minutes after being placed in the freezer and was almost completely frozen in approximately 3 hours. It was then stored in the described condition for approximately 20 hours from the start of storage, and then placed at room temperature (23°C). The frozen samples thawed completely in approximately 2 hours. The sample subjected to freeze-thaw at pH 6.7 was designated as Comparative Sample 3, and the sample subjected to freeze-thaw at pH 9.5 was designated as Comparative Sample 4.

[0124] Comparative samples 3 and 4 were analyzed for 4-mercapto-4-methylpentan-2-one and linalool in the same manner as described above. The results are shown in Table 1.

[0125] [Table 1] pH before freezing MMP concentration (ppb) ((yield (mass) of green tea extract) / (amount (mass) of green tea leaves used as raw material for extraction)) × the percentage of 4-mercapto-4-methylpentan-2-one in the green tea extract (based on mass) Peak area ratio (MMP / linalool) Comparative product 3 5.7 0.16 <![CDATA[1.6×10 -10 ]]> <![CDATA[1.3×10 -7 ]]> Comparative product 4 9.5 0.18 <![CDATA[1.8×10 -10 ]]> <![CDATA[1.4×10 -7 ]]> MMP: 4-Mercapto-4-methylpentan-2-one.

[0126] Even when frozen and thawed in the presence of the water extract fraction containing green tea, no increase in 4-mercapto-4-methylpentane-2-one was observed at either pH 6.7 or pH 9.5.

[0127] (Example 3) 1000g of new Kyushu tea (Yabukata variety, medium steaming) was packed into a 3L column, and the same procedure 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 purging the column with nitrogen, nitrogen-mixed water vapor was blown in from the bottom of the column. The water vapor containing the volatile components of the tea obtained from the top of the column was condensed through a cooling tube (cooled by tap water, approximately 20°C). After approximately 20 minutes, 500g (50% relative to the tea leaves) of distillate containing the volatile components of the tea was obtained. The pH of the resulting distillate was 7.6.

[0128] The distillate was dispensed into four 300 ml brown bottles, each containing 100 g of the distillate, and stored according to the following classification.

[0129] Comparative product 5: After nitrogen replacement of the headspace, it was stored in a freezer (-20°C). Comparative Product 6: After nitrogen replacement of the headspace, it was stored in a cold storage (5°C). Comparative Product 7: Prepared with ascorbic acid powder at pH 6.5, and after nitrogen replacement of the headspace, stored in a freezer (-20°C). Product 3 of this invention: prepared with a pH of 9.5 using a 0.1% potassium hydroxide aqueous solution, and after nitrogen replacement of the headspace, stored in a freezer (-20°C). Samples stored in the freezer began to freeze approximately 30 minutes after being placed in the freezer and were almost completely frozen in about 3 hours. They were then stored in the aforementioned condition for approximately 20 hours from the start of storage, and then placed at room temperature (23°C). The frozen products were completely thawed in about 2 hours, yielding frozen-thawed products (Comparative Product 6, Comparative Product 7, and Product 3 of the Invention).

[0130] These present invention samples 3, comparative samples 5 to 7 were analyzed for 4-mercapto-4-methylpentan-2-one and linalool in the same manner as described above. The results are shown in Table 2.

[0131] [Table 2] pH before freezing MMP concentration (ppb) ((yield (mass) of green tea extract) / (amount (mass) of green tea leaves used as raw material for extraction)) × the percentage of 4-mercapto-4-methylpentan-2-one in the green tea extract (based on mass) Peak area ratio (MMP / linalool) Product 3 of this invention 9.5 442 <![CDATA[1:2.2×10 -7 ]]> <![CDATA[3.7×10 -4 ]]> Comparison Item 5 7.6 9.2 <![CDATA[1:4.6×10 -9 ]]> <![CDATA[7.7×10 -6 ]]> Comparison product 6 7.6 (Refrigerate) 0.22 <![CDATA[1:1.1×10 -10 ]]> <![CDATA[8.0×10 -7 <!-- 16 -->]]> Comparison Product 7 6.5 0.28 <![CDATA[1:1.4×10 -10 ]]> <![CDATA[1.0×10 -6 ]]> MMP: 4-Mercapto-4-methylpentan-2-one.

[0132] As shown in Table 2, even when freeze-thawed at pH 7.6 (Comparative Product 5), no increase in 4-mercapto-4-methylpentan-2-one was observed compared to the unfrozen product. At pH 6.5, even with freeze-thaw, 4-mercapto-4-methylpentan-2-one showed almost no increase (Comparative Product 7). On the other hand, when frozen at pH 9.5, the result was a more than 40-fold increase in 4-mercapto-4-methylpentan-2-one compared to freezing at pH 7.6.

[0133] (Example 4) 1 kg of Shizuoka Prefecture green tea (fresh, deep-steamed) was added to 20 kg of ion-exchange water heated to 80°C. After stirring slowly for 5 minutes, the tea leaves were separated using a 40-mesh metal mesh. The separated liquid was cooled to 20°C to obtain 14 kg of extract. 7.0 g (500 ppm) of sodium ascorbate was added, and the mixture was filtered through No. 2 filter paper (manufactured by ADVANTEC: retaining a particle size of 5 μ) to obtain the green tea beverage concentrate (analytical values ​​of the green tea beverage concentrate: Bx: 2.22°, pH: 6.4, tannin content (ferric tartrate method): 0.44%, amino acid content: 0.071%). The product was dispensed and diluted 10 times (by mass) with deionized water. Solutions of either the present invention's second or comparative product's second, as described in Table 2, were then added to the diluted solution. The solutions were sterilized at 137°C for 30 seconds, cooled to 88°C, and filled into 500 ml PET plastic bottles. After holding the solution for 2 minutes, it was cooled to room temperature (25°C) to produce bottled green tea beverages. Various green tea beverages were evaluated by a panel of 10 members, using the unadded tea extract as a control. The evaluation criteria were: with the unadded product scored as 5 points, the following scores were assigned: excellent (10 points), good (8 points), slightly good (6 points), slightly poor (4 points), poor (2 points), and very poor (0 points). The results are shown in Table 3.

[0134] [Table 3]

[0135] As shown in Table 3, the present invention's Product 2, added at a trace amount of only 1 ppm to 10 ppm relative to green tea beverages (equivalent to 0.00025 ppb to 0.0025 ppb based on 4-mercapto-4-methylpentan-2-one), significantly increases the fresh brewing sensation, greenness, sweetness, and fullness, accompanied by a slight fruity taste, compared to green tea. On the other hand, Comparative Product 2 showed almost no change compared to no addition at 1 ppm, a slight effect was observed at around 10 ppm, and the effect became definite at around 100 ppm. Therefore, the present invention (Product 2) is effective even at concentrations far lower than conventional aromatic extracts (Comparative Product 2), demonstrating distinctive flavor characteristics and cost advantages.

Claims

1. Green tea extract, which is green tea extract without the addition of 4-mercapto-4-methylpentan-2-one, satisfies the following formula when determining the 4-mercapto-4-methylpentan-2-one content in the green tea extract: ((yield (mass) of green tea extract) / (amount (mass) of green tea leaves used as raw material for extraction)) × (percentage of 4-mercapto-4-methylpentan-2-one in green tea extract (based on mass)) = 1 × 10 -8 ~5×10 -5 .

2. Green tea extract, specifically green tea extract without the addition of 4-mercapto-4-methylpentan-2-one, satisfies the following formula when its aroma components are analyzed by GC / MS and a chromatogram is plotted based on the GC / MS analysis results: (Area of ​​the detected peak of 4-mercapto-4-methylpentan-2-one (m / z = 132)) / (Area of ​​the detected peak of linalool (total ions)) = 1 × 10 -5 ~5×10 -2 .

3. A container holding a green tea beverage containing the green tea extract as described in claim 1 or 2.

4. A green tea flavored food or beverage containing the green tea extract as described in claim 1 or 2.

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