JP7342277B2 - Method for extracting flavor components and manufacturing method for components of processed tobacco leaves - Google Patents

Description

The present invention relates to a method for extracting flavor components and a method for producing components of processed tobacco leaves.

Conventionally, a technique has been proposed in which flavor components (for example, alkaloids containing nicotine components) are extracted from tobacco raw materials and the extracted flavor components are supported on components of processed tobacco leaves.

For example, Patent Documents 1 and 2 describe a process A in which tobacco raw materials subjected to alkali treatment are heated, and a collection solvent at room temperature that collects the released components released into the gas phase in the process A until a specific timing. A technique related to a flavor component extraction method for extracting flavor components from tobacco raw materials is disclosed, which includes a step B of contacting the tobacco raw material with the tobacco raw material to obtain a collection solution. Further, Patent Document 1 and Patent Document 2 relate to a method for manufacturing a component of a luxury item (processed tobacco leaf), which includes a step C of adding the collection solution to the component in addition to the steps A and B. The technology has been disclosed.

International Publication No. 2015/129679 International Publication No. 2015/129680

In the techniques disclosed in Patent Document 1 and Patent Document 2, Step A and Step B of extracting flavor components from tobacco raw materials require an extraction processing time of a certain amount or more in order to recover a certain amount of flavor components from tobacco raw materials. I need. For example, the extraction processing time required for the nicotine concentration in the tobacco raw material to reach 0.4% by weight is 180 minutes. Therefore, there is room for improvement in terms of reducing the extraction processing time from the viewpoint of efficiency in producing components of processed tobacco leaves.

Further, Patent Document 1 and Patent Document 2 disclose that when the extraction processing time in Step A and Step B exceeds a certain level, tobacco-specific nitrosamines (hereinafter simply referred to as It is disclosed that the amount of TSNA released from tobacco raw materials tends to increase. Therefore, it is expected that by shortening the extraction processing time, the TSNA concentration in the collection solution can be kept at a lower level.

Therefore, in the present invention, the time required to extract a certain amount of flavor components from tobacco raw materials or processed tobacco leaves can be reduced compared to conventional methods, and the TSNA concentration in the collection solution that collects flavor components can be further reduced. It is an object of the present invention to provide a method for extracting flavor components that can be kept at a low level, and a method for producing components of processed tobacco leaves that include said extraction method.

As a result of intensive studies by the present inventors, the initial moisture content of the alkali-treated tobacco raw material or processed tobacco leaf is is above a specific amount, and the alkali-treated tobacco raw material or processed tobacco leaf is subjected to hydration treatment during heating, and the water content of the alkali-treated tobacco raw material or processed tobacco leaf is consistently below the specified amount. The inventors have discovered that the above problems can be solved by doing the following, and have arrived at the present invention.

That is, the present invention is as follows.
[1] A method for extracting flavor components from tobacco raw materials or processed tobacco leaves, comprising:
Step A of heating the alkali-treated tobacco raw material or processed tobacco leaves using an alkali;
A step B of bringing the released component released into the gas phase in the step A into contact with a collection solvent,
In the step A,
The initial moisture content of the alkali-treated tobacco raw material or processed tobacco leaf is at least the minimum moisture content that can dissolve all of the alkali,
The alkali-treated tobacco raw material or processed tobacco leaf being heated is subjected to a hydration treatment,
Consistently, the moisture content of the alkali-treated tobacco raw material or processed tobacco leaf is 35% by weight or less based on the total weight of the tobacco raw material or the processed tobacco leaf,
Method for extracting flavor components.
[2] In the step A, the initial moisture content of the alkali-treated tobacco raw material or processed tobacco leaf is more than 20% by weight based on the total weight of the tobacco raw material or processed tobacco leaf, [ 1].The method for extracting flavor components described in [1].
[3] The method for extracting flavor components according to [1] or [2], wherein the alkali-treated tobacco raw material has a pH of 9.5 or higher.
[4] In the step A, the hydrolysis treatment is performed when the temperature of the alkali-treated tobacco raw material or processed tobacco leaf reaches a temperature range of 100°C or more and 150°C or less, [1 ] to [3]. The method for extracting flavor components.
[5] In step A, when the moisture content of the alkali-treated tobacco raw material or processed tobacco leaf becomes 20% by weight or less based on the total weight of the tobacco raw material or processed tobacco leaf for the first time. The method for extracting flavor components according to [1] to [4], wherein the above-mentioned hydrolysis treatment is performed.
[6] The method for extracting flavor components according to [1] to [5], wherein the alkali is potassium carbonate or sodium carbonate.
[7] The method for extracting flavor components according to [1] to [6], wherein in the step B, the temperature of the collection solvent is 5° C. or higher and 35° C. or lower.
[8] A method for producing components of processed tobacco leaves, comprising:
Step A of heating the alkali-treated tobacco raw material or processed tobacco leaves using an alkali;
Step B of contacting the released component released into the gas phase in the step A with a collection solvent to obtain a collection solution;
step C of adding the collection solution to the component,
In the step A,
The initial moisture content of the alkali-treated tobacco raw material or processed tobacco leaf is at least the minimum moisture content that can dissolve all of the alkali,
The alkali-treated tobacco raw material or processed tobacco leaf being heated is subjected to a hydration treatment,
A manufacturing method characterized in that the moisture content of the alkali-treated tobacco raw material or processed tobacco leaf is consistently 35% by weight or less based on the total weight of the tobacco raw material or processed tobacco leaf.

According to the present invention, the time required to extract a certain amount of flavor components from tobacco raw materials or processed tobacco leaves can be reduced compared to conventional methods, and the TSNA concentration in the collection solution in which flavor components are collected can be reduced. A method for extracting flavor components and producing components of processed tobacco leaves that can be maintained at lower levels can be provided.

FIG. 1 is a diagram showing an example of an extraction device according to an embodiment of the present invention. FIG. 2 is a diagram showing an example of an extraction device according to an embodiment of the present invention. FIG. 3 is a diagram for explaining an example of application of flavor components. FIG. 4 is a flow diagram showing an extraction method according to an embodiment of the present invention. FIG. 5 is a graph showing changes in the recovery rate of flavor components (here, nicotine) with respect to the heat treatment time of tobacco raw materials. FIG. 6 is a graph showing the change in the amount of TSNA recovered with respect to the heat treatment time of tobacco raw materials. FIG. 7 is a graph showing changes in temperature of tobacco raw materials with respect to heat treatment time of tobacco raw materials. FIG. 8 is a graph showing the transition of the moisture content of tobacco raw materials with respect to the heat treatment time of tobacco raw materials.

Embodiments of the present invention will be described in detail below, but these descriptions are only examples (representative examples) of the embodiments of the present invention, and the present invention is not limited to these contents unless the gist thereof is exceeded.
In this specification, when "~" is used to express a numerical value or physical property value before and after it, it is used to include the values before and after it. Furthermore, it should be noted that the drawings are schematic and the ratio of each dimension may differ from the actual one.

As used herein, "tobacco raw material" refers to tobacco leaves that have been harvested and have not undergone ripening treatment, or tobacco leaves that have undergone ripening treatment, and that have not yet been processed into various forms used in tobacco products. It is a general term for things, and examples include fresh leaves and dried leaves before ripening, crushed products thereof, ripened lamina and crushed products thereof, aged backbones and crushed products thereof, etc.
In addition, in this specification, "processed tobacco leaves" is a general term for products processed from the above-mentioned tobacco raw materials into various forms used in tobacco products, and includes shredded tobacco, tobacco sheets, tobacco granules, etc. I can do it. Such processed tobacco leaves may be composed only of the tobacco raw material, or may be composed of the tobacco raw material and other materials. Therefore, the "components" of processed tobacco leaves include the tobacco raw materials and other materials.

A method for extracting flavor components according to an embodiment of the present invention is a method for extracting flavor components from tobacco raw materials or processed tobacco leaves. The extraction method includes a step A of heating alkali-treated tobacco raw materials or processed tobacco leaves using an alkali, and a step B of bringing the released components released into the gas phase in the step A into contact with a collection solvent. , is provided.

In step A, the initial moisture content of the alkali-treated tobacco raw material or processed tobacco leaf is at least the minimum moisture content that can dissolve all of the alkali, and the alkali-treated tobacco raw material or processed tobacco leaf is heated. Hydrogenation treatment is applied to finished tobacco leaves, and the moisture content of the alkali-treated tobacco raw materials or processed tobacco leaves is 35% by weight or less based on the total weight of the tobacco raw materials or processed tobacco leaves. be.
The "initial moisture content" of the alkali-treated tobacco raw material or processed tobacco leaf refers to the moisture content of the alkali-treated tobacco raw material or processed tobacco leaf after the alkali treatment and before heat treatment. It can be expressed in weight % based on the total weight of the tobacco raw material or the processed tobacco leaf. Here, the total weight of the tobacco raw material or the processed tobacco leaf, which is the basis for calculating the moisture content, means the dry weight of each. The same applies below.

In the conventional flavor component extraction methods disclosed in Patent Document 1 and Patent Document 2 mentioned above, the initial moisture content of the alkali-treated tobacco raw material or processed tobacco leaf is the total amount of the tobacco raw material or the processed tobacco leaf. It is 39%±2% of the weight. One of the reasons why the moisture content was initially set in this way in the conventional extraction method of flavor components is that after the tobacco raw material or processed tobacco leaves are loaded into the extractor and subjected to alkali treatment, the heating operation is started. This is because the flavor components could be obtained at the desired recovery rate without any additional operations.
However, in such conventional flavor component extraction methods, the time from the start to the end of the heating operation, that is, the time required to obtain the desired recovery rate of flavor components, is approximately 180 minutes, and It took up a relatively long time in the process of manufacturing leaf components.
In addition, it was generally known that the longer the time for heating at high temperatures, the greater the amount of TSNA released from tobacco raw materials or processed tobacco leaves. In the extraction method, it has been reported that the longer the heat treatment time is to obtain the desired recovery rate of flavor components, the more the amount of TSNA recovered increases.

The present inventor investigated ways to shorten the time required to obtain a flavor component with a desired recovery rate and to suppress the amount of TSNA recovered in a flavor component extraction method, and found that the above conditions, that is, the step In A, the initial moisture content of the alkali-treated tobacco raw material or processed tobacco leaf is at least the minimum moisture content that can completely dissolve the alkali, and the alkali-treated tobacco raw material or processed tobacco leaf is heated. The moisture content of the tobacco raw material or processed tobacco leaf that has been subjected to hydrolysis treatment and that has been consistently treated with alkali is 35% by weight or less based on the total weight of the tobacco raw material or processed tobacco leaf. , was found.
By performing the step A under the above conditions, the time required to obtain a flavor component with a desired recovery rate can be shortened, and the amount of TSNA recovered can be suppressed, compared to conventional methods.

The reason why the time required to obtain flavor components with a desired recovery rate can be shortened is thought to be as follows. In the alkali-treated tobacco raw material or processed tobacco leaf according to the embodiment of the present invention, the initial moisture content is set lower than that of the conventional one, and even if hydration treatment is performed during heat treatment, the above-mentioned The moisture content of the alkali-treated tobacco raw material or processed tobacco leaf is controlled to 35% by weight or less, which is lower than the initial moisture content in conventional methods. Therefore, the temperature of the alkali-treated tobacco raw material or processed tobacco leaf rises quickly, and flavor components are released from the tobacco raw material or processed tobacco leaf at an earlier timing than in conventional methods. .
Furthermore, the reason why the amount of TSNA recovered can be suppressed is thought to be as follows. The alkali-treated tobacco raw material or processed tobacco leaf according to the embodiment of the present invention is subjected to a hydrolysis treatment during the heat treatment, so that its temperature temporarily decreases. This is because, as a result, the time during which the temperature of the tobacco raw material or the processed tobacco leaf reaches a high temperature can be shortened.

In step A, the initial moisture content of the alkali-treated tobacco raw material or processed tobacco leaf is preferably more than 20% by weight based on the total weight of the tobacco raw material or processed tobacco leaf.
The initial moisture content of the alkali-treated tobacco raw material or processed tobacco leaf is more preferably 25% by weight or more, and even more preferably 30% by weight or more. Further, the initial moisture content of the alkali-treated tobacco raw material or processed tobacco leaf is preferably 35% by weight or less. When the initial moisture content is within such a numerical range, the temperature of the alkali-treated tobacco raw material or processed tobacco leaf to be heat-treated increases faster, and the flavor components are more concentrated than in the conventional method. The initial moisture content of the alkali-treated tobacco raw material or processed tobacco leaf is released from the tobacco raw material or processed tobacco leaf at an early timing. % or less, the alkali added to the tobacco raw material or processed tobacco leaves may not be completely dissolved and may precipitate.
The initial moisture content of the alkali-treated tobacco raw material or processed tobacco leaf can be adjusted by adjusting the concentration of the alkaline aqueous solution added to the tobacco raw material or processed tobacco leaf in the alkali treatment described below.

The pH of the alkali-treated tobacco raw material or processed tobacco leaf is preferably 9.5 or higher. When the pH is 9.5 or higher, flavor components can be efficiently released from tobacco raw materials or processed tobacco leaves, and the recovery rate of flavor components increases. On the other hand, if the pH is less than 9.5, the recovery rate of flavor components from tobacco raw materials or processed tobacco leaves may decrease.
The upper limit of the pH of the alkali-treated tobacco raw material or processed tobacco leaf is not particularly limited, but from the viewpoint of the treatment time required to increase the pH, it is usually 12 or less, preferably 11 or less.
The pH of the alkali-treated tobacco raw material or processed tobacco leaf can be adjusted by the type of alkali and the concentration of the aqueous alkali solution added to the tobacco raw material or processed tobacco leaf in the alkali treatment described below.

The alkali used in the alkali treatment is not particularly limited as long as it can bring the pH of tobacco raw materials or processed tobacco leaves within the above numerical range, but it is preferably a substance that can be used as a food additive, such as carbonic acid. Potassium, sodium carbonate, or a mixture thereof can be suitably used. Potassium carbonate and sodium carbonate are preferable since they have good solubility in water and can easily prepare an alkaline aqueous solution for spraying on tobacco raw materials or processed tobacco leaves.

In the step A, the hydrolysis treatment is preferably performed when the temperature of the alkali-treated tobacco raw material or processed tobacco leaf reaches a temperature range of 100°C or more and 150°C or less. The temperature range is more preferably 100°C or more and 130°C or less, and even more preferably 100°C or more and 110°C or less. By performing the hydrolysis treatment within such a temperature range, the amount of TSNA released can be suppressed while maintaining efficient release of flavor components from the alkali-treated tobacco raw material or processed tobacco leaves. be able to.

In addition, in the step A, the water addition treatment is such that the water content of the alkali-treated tobacco raw material or processed tobacco leaf is 20% by weight or less based on the total weight of the tobacco raw material or processed tobacco leaf for the first time. It is preferable to apply it when it becomes necessary. By performing the hydrolysis treatment at such a timing, it is possible to suppress the amount of TSNA released while maintaining efficient release of flavor components from the alkali-treated tobacco raw material or processed tobacco leaves. can.

In the step B, the temperature of the collection solvent is preferably 5°C or more and 35°C or less, more preferably 10°C or more and 20°C or less. By setting the temperature of the collection solvent within such a temperature range, it is possible to prevent the collection solvent from coagulating and to suppress volatilization of the flavor components from the collection solution, so that the flavor components can be efficiently absorbed. It can be recovered.

The method for producing components of processed tobacco leaves according to an embodiment of the present invention includes applying the flavor component extraction method of extracting flavor components from the tobacco raw material or processed tobacco leaves. This is the manufacturing method. That is, the method for producing components of processed tobacco leaves according to an embodiment of the present invention includes the step A of heating the tobacco raw material or processed tobacco leaf treated with an alkali using an alkali; said step B of contacting the emitted components released into a collection solvent with a collection solvent to obtain a collection solution; and step C of adding said collection solution to said constituents of the processed tobacco leaf. In step A, the initial moisture content of the alkali-treated tobacco raw material or processed tobacco leaf is at least the minimum moisture content that can dissolve all of the alkali, and the alkali-treated tobacco raw material or processed tobacco leaf is heated. Hydrogenation treatment is applied to finished tobacco leaves, and the moisture content of the tobacco raw materials or processed tobacco leaves that have been consistently treated with alkali is 35% by weight or less based on the total weight of the tobacco raw materials or the processed tobacco leaves. It is.
By applying a flavor component extraction method that extracts flavor components from the tobacco raw material or processed tobacco leaf to the method for manufacturing the components of the processed tobacco leaf, the manufacturing time for the components of the processed tobacco leaf is shortened. At the same time, the amount of TSNA that may be contained in the constituent elements can be suppressed.

(Extraction device)
An extraction device according to an embodiment of the present invention will be described below. 1 and 2 are diagrams showing an example of an extraction device according to an embodiment of the present invention.

First, an example of the alkali treatment apparatus 10 will be described with reference to FIG. 1. The alkali treatment apparatus 10 includes a container 11 and a sprayer 12.

The container 11 contains tobacco raw material (or processed tobacco leaves) 50. The container 11 is made of, for example, a member having heat resistance and pressure resistance (for example, SUS; Steel Used Stainless). Preferably, the container 11 constitutes a closed space. A "closed space" is a state that prevents solid foreign matter from entering during normal handling (transportation, storage, etc.). This suppresses the volatilization of flavor components contained in the tobacco raw material (or processed tobacco leaves) 50 to the outside of the container 11.

The atomizer 12 applies the alkaline aqueous solution to the tobacco raw material (or processed tobacco leaf) 50 to perform alkali treatment.

The initial content of the flavor component (here, nicotine component) contained in the tobacco raw material (or processed tobacco leaf) 50 is such that the total weight of the tobacco raw material (or processed tobacco leaf) 50 is 100% by weight in the dry state. In some cases, it is preferably 2.0% by weight or more, more preferably 4.0% by weight or more.

The tobacco raw material (or processed tobacco leaf) 50 may be, for example, unripened tobacco leaves of the Nicotiana genus such as Nicotiana tabacum or Nicotiana rustica, or aged tobacco leaves thereof; It is possible to use aged tobacco leaves processed into various forms used in tobacco products. As Nicotiana tabacum, varieties such as burley variety or yellow variety can be used, for example. The tobacco raw material (or processed tobacco leaf) 50 may include unripened tobacco leaves of types other than burley and yellow varieties, aged tobacco leaves, or aged tobacco leaves of various types used in tobacco products. You may use what has been processed into a shape.

The tobacco raw material (or processed tobacco leaf) 50 is preferably composed of shredded or powdered tobacco raw materials or processed tobacco leaves, and more preferably composed of powdered or granulated material. In such a case, the particle size of the chopped or powdered material is usually 0.5 mm or more and 10 mm or less, preferably 0.5 mm or more and 5 mm or less. If the particle size is smaller than 0.5 mm, it is unfavorable from the viewpoint of extraction efficiency because it often sticks to the wall of the container 11. In addition, when the particle size is 10 mm or less, the surface area of the chopped or powdered material becomes large, resulting in good extraction efficiency, and when the particle size is 5 mm or less, the surface area of the chopped or powdered material becomes larger, resulting in better extraction. Efficiency becomes even better. In this specification, "shredded" refers to something obtained by finely chopping tobacco raw materials or processed tobacco leaves. Moreover, "powder" is obtained by coarsely crushing tobacco raw materials or processed tobacco leaves.

Second, an example of the collection device 20 will be described with reference to FIG. 2. The collection device 20 has a container 21 , an inlet pipe 22 , a discharge section 23 , and an outlet pipe 24 .

Container 21 accommodates collection solvent 70 . The container 21 is made of glass, for example. Preferably, the container 21 constitutes a closed space. A "closed space" is a state that prevents solid foreign matter from entering during normal handling (transportation, storage, etc.).

As the collection solvent 70, for example, glycerin, water, or ethanol can be used. Among these collection solvents 70, it is preferable to use water from the viewpoint of ease of handling and cost reduction. In order to prevent the flavor components captured by the collection solvent 70 from revolatilizing, any acid such as malic acid or citric acid may be added to the collection solvent 70. In order to increase the capture efficiency of flavor components, a component or substance such as an aqueous citric acid solution may be added to the capture solvent 70. That is, the collection solvent 70 may be composed of multiple types of components or substances. In order to increase the capture efficiency of flavor components, the initial pH of the capture solvent 70 is preferably lower than the pH of the tobacco raw material (or processed tobacco leaf) 50 after the alkali treatment.

The introduction pipe 22 guides the released component 61 released into the gas phase from the tobacco raw material (or processed tobacco leaf) 50 by heating the tobacco raw material (or processed tobacco leaf) 50 to the collection solvent 70 . Release component 61 includes at least a nicotine component, which is indicative of a flavor component.

The discharge portion 23 is provided at the tip of the introduction pipe 22 and is immersed in the collection solvent 70 . The discharge portion 23 has a plurality of openings 23A. The released component 61 guided by the introduction pipe 22 is released into the collection solvent 70 as a foamy released component 62 from the plurality of openings 23A.

The outlet pipe 24 guides the remaining components 63 that have not been captured by the capturing solvent 70 to the outside of the container 21 .

Here, since the released component 62 is a component released into the gas phase by heating the tobacco raw material (or processed tobacco leaf) 50, the temperature of the collection solvent 70 may increase due to the released component 62. . Therefore, the collection device 20 may have a function of cooling the collection solvent 70 in order to maintain the temperature of the collection solvent 70 at room temperature.

The collection device 20 may include a Raschig ring to increase the contact area of the emitted component 62 to the collection solvent 70.

(Application example)
Below, examples of application of flavor components extracted from tobacco raw material (or processed tobacco leaves) 50 will be described. FIG. 3 is a diagram for explaining an example of application of flavor components. For example, flavor components are applied to processed tobacco leaves and the like.

As shown in FIG. 3, the flavor suction device 100 includes a holder 110, a carbon heat source 120, processed tobacco leaves 130, and a filter 140.

The holder 110 is, for example, a paper tube having a cylindrical shape. Carbon heat source 120 generates heat for heating processed tobacco leaves 130. Processed tobacco leaf 130 is a substance that generates flavor, and is an example of a flavor source base material to which an alkaloid containing a nicotine component is added. The filter 140 prevents contaminants from being introduced to the mouthpiece side.

Although the flavor suction tool 100 has been described here as an application example of flavor components, the embodiment is not limited thereto.
Flavor components may also be applied to other flavor suction devices. For example, a tobacco rod is filled by wrapping processed tobacco leaves with wrapping paper on the inside, and processed tobacco leaves are filled into a flow path of a container having an air inlet and an air outlet. It is applied to the tobacco filler of so-called non-combustible heated tobacco products, which generate flavor by heating the tobacco cartridge directly or indirectly using a non-combustion heat source such as an electric heater. Good too. Here, an example of the tobacco filler is a tobacco sheet filled in the tobacco rod, and another example is tobacco granules filled in the tobacco cartridge.
In addition, flavor components may be applied, for example, to the aerosol source of electronic cigarettes (so-called E-liguid). Further, the flavor component may be applied to a flavor source base material such as a gum, tablet, film, or candy.

(Extraction method)
Below, a method for extracting flavor components according to an embodiment of the present invention will be described. FIG. 4 is a flow diagram showing a method for extracting the flavor components.

As shown in FIG. 4, in step S10, alkali is applied to the tobacco raw material (or processed tobacco leaf) 50 using the alkali treatment device 10 described above. Examples of the alkali include potassium carbonate, sodium carbonate, and mixtures thereof, as described above.

The tobacco raw material (or processed tobacco leaf) 50 is subjected to alkali treatment by adding the aqueous alkali solution.
The initial content of the flavor component (here, nicotine component) contained in the tobacco raw material (or processed tobacco leaf) 50 is such that the total weight of the tobacco raw material (or processed tobacco leaf) 50 is 100% by weight in the dry state. In some cases, it is preferably 2.0% by weight or more, more preferably 4.0% by weight or more.

As mentioned above, the pH of the tobacco raw material (or processed tobacco leaf) 50 after the alkali treatment is preferably 9.5 or higher. When the pH is 9.5 or higher, flavor components can be efficiently released from the tobacco raw material (or processed tobacco leaves) 50, and the recovery rate of flavor components increases. On the other hand, if the pH is less than 9.5, the recovery rate of flavor components from the tobacco raw material (or processed tobacco leaves) 50 decreases. Further, the upper limit of the pH of the alkali-treated tobacco raw material (or processed tobacco leaf) 50 is not particularly limited, but as mentioned above, from the viewpoint of the processing time required to increase the pH, it is usually 12 or less. , 11 or less.

The moisture content of the tobacco raw material (or processed tobacco leaf) 50 after the alkali treatment is preferably more than 20% by weight, and 25% by weight or more, based on the total weight of the tobacco raw material or processed tobacco leaf. It is more preferable that the amount is 30% by weight or more. When the initial moisture content is within such a numerical range, the temperature of the alkali-treated tobacco raw material or processed tobacco leaf to be heat-treated increases faster, and the flavor components are more concentrated than in the conventional method. It is also released from the tobacco raw material or processed tobacco leaves at an early timing. When the initial moisture content of the alkali-treated tobacco raw material or processed tobacco leaf is 20% by weight or less based on the total weight of the tobacco raw material or processed tobacco leaf, the alkali added to the tobacco raw material is dissolved. It may precipitate without being removed.
The moisture content of the tobacco raw material (or processed tobacco leaf) 50 after the alkali treatment is the initial moisture content of the alkali-treated tobacco raw material (or processed tobacco leaf) 50 in the heat treatment in step 20S.

In step S20, the tobacco raw material (or processed tobacco leaf) 50 that has been subjected to alkali treatment is heated. For example, in the heat treatment, the tobacco raw material (or processed tobacco leaf) 50 may be heated together with the container 11 while the tobacco raw material (or processed tobacco leaf) 50 is housed in the container 11 of the alkali treatment device 10. can. In such a case, the introduction pipe 22 of the collection device 20 is of course attached to the container 11.

Here, the heating temperature of the tobacco raw material (or processed tobacco leaf) 50 is in the range of 80°C or higher and 150°C or lower. By heating the tobacco raw material (or processed tobacco leaf) 50 at a heating temperature of 80° C. or higher, the timing at which sufficient flavor components are released from the tobacco raw material (or processed tobacco leaf) 50 can be accelerated. On the other hand, by heating the tobacco raw material 50 at a temperature of 150° C. or lower, the timing at which TSNA is released from the tobacco raw material (or processed tobacco leaf) 50 can be delayed.

In step S20, the tobacco raw material (or processed tobacco leaf) 50 undergoing heat treatment is subjected to a hydration treatment. When the tobacco raw material (or processed tobacco leaf) 50 undergoing heat treatment is subjected to the hydrolysis treatment, its temperature is temporarily lowered, and the amount of TSNA recovered can be suppressed.
The moisture content of the heat-treated tobacco raw material (or processed tobacco leaf) 50 is 35% by weight or less based on the total weight of the tobacco raw material. Therefore, the amount of water added is adjusted so that the moisture content of the tobacco raw material (or processed tobacco leaf) 50 is 35% by weight or less based on the total weight of the tobacco raw material or processed tobacco leaf.

The number of times the tobacco raw material (or processed tobacco leaf) 50 is subjected to the hydrolysis treatment during the heat treatment is not particularly limited as long as the above-mentioned upper limit of the moisture content is not exceeded, and may be once, twice or more. Further, the tobacco raw material (or processed tobacco leaf) 50 may be continuously subjected to hydrohydration treatment.
The number of times of the hydrolysis treatment is preferably one. The reason for this is that the fewer times the water addition treatment is performed, the less time and effort it takes. Furthermore, since the temperature of the tobacco raw material or processed tobacco leaf during heat treatment decreases each time the hydrolysis treatment is performed, it is preferable that the number of hydrolysis treatments is small from the viewpoint of extraction efficiency of flavor components.

The timing to perform the hydrolysis treatment on the tobacco raw material (or processed tobacco leaf) 50 during heat treatment is such that the temperature of the tobacco raw material (or processed tobacco leaf) 50 is within a temperature range of 100°C or higher and 150°C or lower. It is preferable that the time is reached. The temperature range is more preferably 100°C or more and 130°C or less, and even more preferably 100°C or more and 110°C or less. By performing the hydrolysis treatment within such a temperature range, the amount of TSNA released can be suppressed while maintaining efficient release of flavor components from the alkali-treated tobacco raw material or processed tobacco leaves. be able to.
Furthermore, the timing of performing the hydration treatment on the tobacco raw material (or processed tobacco leaf) 50 during heat treatment is such that the moisture content of the tobacco raw material or processed tobacco leaf subjected to the alkali treatment is It is preferable that the treatment is applied when the total weight of the leaves reaches 20% by weight or less. By performing the hydrolysis treatment at such a timing, it is possible to suppress the amount of TSNA released while maintaining efficient release of flavor components from the alkali-treated tobacco raw material or processed tobacco leaves. can.

Further, in step S20, it is preferable that the tobacco raw material (or processed tobacco leaf) 50 is subjected to aeration treatment. Thereby, the amount of flavor components contained in the released components 61 released into the gas phase from the alkali-treated tobacco raw material (or processed tobacco leaves) 50 can be increased. In the aeration treatment, for example, the tobacco raw material (or processed tobacco leaf) 50 is brought into contact with saturated steam at 80°C. The aeration time in the aeration process varies depending on the equipment that processes the tobacco raw material (or processed tobacco leaf) 50 and the amount of the tobacco raw material (or processed tobacco leaf) 50, so it cannot be specified unconditionally. When the raw material (or processed tobacco leaf) 50 is 500 g, the aeration time is within 90 minutes. The total amount of aeration in the aeration process also varies depending on the equipment that processes the tobacco raw material (or processed tobacco leaf) 50 and the amount of the tobacco raw material (or processed tobacco leaf) 50, so it cannot be specified unconditionally, but for example, When the tobacco raw material (or processed tobacco leaf) 50 is 500 g, the total aeration amount is about 3 L/g. In addition, the aeration flow rate also varies depending on the equipment that processes the tobacco raw material (or processed tobacco leaves) 50 and the amount of the tobacco raw materials (or processed tobacco leaves) 50, so it cannot be specified unconditionally. The flow rate is about 15 L/min.

The air used in the aeration process does not have to be saturated steam. The moisture content of the air used in the aeration treatment can be determined without particularly requiring humidification of the tobacco raw material (or processed tobacco leaf) 50, for example, the tobacco raw material (or processed tobacco leaf) to which heat treatment and aeration treatment have been applied. The amount of water contained in 50 may be adjusted to fall within a range of 35% by weight or less. The gas used in the aeration process is not limited to air, and may be an inert gas such as nitrogen or argon.

In step S30, the above-mentioned collection device 20 is used to bring the released component released into the gas phase in step S20 into contact with the collection solvent 70. Note that for convenience of explanation, step S20 and step S30 are shown as separate processes in FIG. 4, but it should be noted that step S20 and step S30 are processes that are performed in parallel. Parallel means that the period in which step S30 is performed overlaps with the period in which step S20 is performed, and it should be noted that step S20 and step S30 do not need to start and end at the same time.

Here, in step S20 and step S30, the pressure inside the container 11 of the alkali treatment apparatus 10 is below normal pressure. Specifically, the upper limit of the pressure inside the container 11 of the alkali treatment apparatus 10 is +0.1 MPa or less in gauge pressure. Further, the inside of the container 11 of the alkali treatment apparatus 10 may be in a reduced pressure atmosphere.

Here, as the collection solvent 70, as described above, for example, glycerin, water, or ethanol can be used. As mentioned above, the temperature of the collection solvent 70 is preferably 5°C or more and 35°C or less, more preferably 10°C or more and 20°C or less. By setting the temperature of the collection solvent within such a temperature range, it is possible to prevent the collection solvent from coagulating and to suppress volatilization of the flavor components from the collection solution, so that the flavor components can be efficiently absorbed. It can be recovered.

In step S40, in order to increase the concentration of the flavor components contained in the capture solution, the capture solvent 70 that has captured the flavor components (i.e., the capture solution) is subjected to vacuum concentration treatment, heat concentration treatment, or salting out. Processing is performed.

Here, since the vacuum concentration process is performed in a closed space, there is little air contact and there is no need to heat the collection solvent 70 to a high temperature, so there is little concern about changes in components. Therefore, the use of vacuum concentration increases the variety of available collection solvents.

Although there is a concern that the heating concentration process may cause denaturation of the liquid such as oxidation of flavor components, it may have the effect of enhancing flavor. However, compared to vacuum concentration, the types of usable collection solvents are reduced. For example, there is a possibility that a collection solvent having an ester structure such as MCT (Medium Chain Triglyceride) cannot be used.

Salting-out treatment can increase the concentration of flavor components compared to vacuum concentration treatment, but since flavor components are separated into the liquid solvent phase and the aqueous phase, the yield of flavor components is poor. Furthermore, since it is assumed that the coexistence of a hydrophobic substance (such as MCT) is essential, salting out may not occur depending on the ratio of the collection solvent, water, and flavor component.

In step S50, a collection solution containing flavor components is added to the processed tobacco leaf components. That is, in step S50, the flavor component captured by the capture solvent 70 is supported on the flavor source base material (component of processed tobacco leaves).

[Other embodiments]
Although the present invention has been described by the embodiments described above, the statements and drawings that form part of this disclosure should not be understood as limiting the present invention. Various alternative embodiments, implementations, and operational techniques will be apparent to those skilled in the art from this disclosure.

For example, with respect to the tobacco raw material (or processed tobacco leaf) 50 (extraction residue) after releasing the flavor component in step S20, the flavor component released from the tobacco raw material (or processed tobacco leaf) 50 in step S30 is A collection solvent (ie, collection solution) that comes to contain the flavor components of the tobacco raw material (or processed tobacco leaf) 50 upon contact may be added (returning treatment). By carrying out such a refolding process, it is possible to further remove components (ammonium ions, TSNA, etc.) that have an undesirable effect on flavor, etc., and produce tobacco raw materials or processed tobacco leaves with suppressed loss of flavor components. can be manufactured. In the hanging back process, the capture solution added to the extraction residue may be neutralized. In the reloading process, the extraction residue containing flavor components may be neutralized after the collection solution is added to the extraction residue. In addition, in the re-spraying process, the amount of flavor components (herein, nicotine component) contained in the tobacco raw material or processed tobacco leaves after the extraction residue is re-spun with the collection solution is the amount of flavor components (here, nicotine component) contained in the tobacco raw material before releasing the flavor components. Or, it should be noted that the amount of flavor components (here, nicotine component) contained in processed tobacco leaves is lower than that contained in processed tobacco leaves.

Furthermore, before performing the above-described hanging back process, the tobacco raw material (or processed tobacco leaf) 50 (extraction residue) after releasing the flavor components in step S20 may be washed with a washing solvent. Examples of the cleaning solvent include aqueous solvents, and specific examples thereof include pure water, ultrapure water, and city water. This removes substances remaining in the extraction residue that have an undesirable effect on flavor and the like. Therefore, when performing the above-mentioned recombination process, it is possible to further remove components that have an undesirable effect on flavor (ammonium ions, TSNA, etc.), and to suppress the loss of flavor components from tobacco raw materials or processed tobacco products. Tobacco leaves can be produced.

[Measuring method]
(Method for measuring pH of tobacco raw materials or processed tobacco leaves)
The pH of tobacco raw materials or processed tobacco leaves after alkali treatment can be measured with a pH meter (for example, IQ240 manufactured by IQ Scientific Instruments Inc.). Add 10 times the weight of distilled water to 10 g, shake the mixture of water and tobacco raw material or processed tobacco leaves at room temperature (e.g. 22°C) at 200 rpm for 10 minutes, and leave it to stand for 5 minutes. Measure the pH of the solution with a pH meter.

(Method for measuring pH of collection solution)
The collection solution is temperature conditioned in a room temperature controlled laboratory at 22° C. by leaving it in a closed container until it reaches room temperature. After harmonization, the lid is opened and the glass electrode of a pH meter (for example, Seven Easy S20 manufactured by METTLER TOLEDO) is immersed in the collection solution to begin measurement. The pH meter is calibrated in advance with pH meter calibration solutions of pH 4.01, 6.87, and 9.21. The point at which the output fluctuation from the sensor stabilizes within 0.1 mV for 5 seconds is defined as the pH of the collection solution.

(Method for measuring the amount of nicotine contained in tobacco raw materials or processed tobacco leaves)
The amount of nicotine contained in tobacco raw materials or processed tobacco leaves is determined by a method according to DIN 10373 of the German Organization for Standardization. That is, 250 mg of tobacco raw material or processed tobacco leaves are collected, 7.5 mL of 11% aqueous sodium hydroxide solution and 10 mL of hexane are added, and shaken and extracted for 60 minutes. After extraction, the supernatant hexane phase is subjected to a gas chromatograph/mass spectrometer (GC/MS) to determine the weight of nicotine contained in the tobacco raw material or processed tobacco leaves.

(Method for measuring the amount of moisture contained in tobacco raw materials or processed tobacco leaves)
250 mg of tobacco raw material or processed tobacco leaves are collected, 10 mL of ethanol is added, and extraction is performed by shaking for 60 minutes. After extraction, the extract is filtered through a 0.45 μm membrane filter and subjected to a gas chromatograph (GC/TCD) equipped with a thermal conductivity detector to quantify the amount of water contained in the tobacco raw material or processed tobacco leaves.

The weight of the tobacco raw material or processed tobacco leaf in a dry state is calculated by subtracting the above-mentioned moisture content from the total weight of the tobacco raw material or processed tobacco leaf.

(Method for measuring the amount of nicotine contained in the collection solution)
The amount of nicotine contained in the collection solution is determined by a method according to DIN 10373 of the German Organization for Standardization, similar to the measurement of the amount of nicotine contained in the tobacco raw material or processed tobacco leaf described above. That is, 250 mg of the collection solution is collected, 7.5 mL of 11% aqueous sodium hydroxide solution and 10 mL of hexane are added, and the mixture is extracted by shaking for 60 minutes. After extraction, the supernatant hexane phase is subjected to a gas chromatograph/mass spectrometer (GC/MS) to quantify the weight of nicotine contained in the collection solution.

The nicotine recovery rate can be expressed as a percentage of the amount of nicotine contained in the collection solution with respect to the nicotine content contained in the tobacco raw material or processed tobacco leaf before alkali treatment and heat treatment.

(Method for measuring the amount of TSNA contained in the collection solution)
Collect 0.5 mL of the collection solution, dilute it by adding 9.5 mL of 0.1M ammonium acetate aqueous solution, analyze it with a high performance liquid chromatography mass spectrometer (LC-MS/MS), and collect the collection solution. Quantify the weight of TSNA contained in the sample.

(GC analysis conditions)
The conditions for GC analysis used to measure the nicotine component and water content contained in tobacco raw materials or processed tobacco leaves are as shown in the table below.

The present invention will be explained in more detail with reference to examples, but the present invention is not limited to the description of the following examples unless it exceeds the gist thereof.

[Experiment example]
(Preparation of tobacco raw materials)
A tobacco raw material was prepared by coarsely crushing aged Burley tobacco lamina to a particle size of 0.5 mm or more and 10 mm or less.
When the flavor component (here, nicotine component) contained in the obtained tobacco raw material was measured using a method according to the above-mentioned German Organization for Standardization DIN 10373, the weight of nicotine contained in the tobacco raw material was determined to be the total weight of the tobacco raw material. The amount was 2.0% by weight.

(alkali treatment)
After putting 500 g of the obtained tobacco raw material into a container equipped with an atomizer (container rotating rocking type powder vacuum dryer rocking dryer, manufactured by Aichi Electric Co., Ltd., capacity 10 L), 90 g of potassium carbonate was dissolved in 180 g of water. 270 g of the obtained potassium carbonate aqueous solution was sprayed onto the tobacco raw material through a sprayer at a spray rate of 55 g/min. When spraying the potassium carbonate aqueous solution, the container was rotated and rocked to blend the potassium carbonate aqueous solution into the tobacco raw material. When the pH of the tobacco raw material after the alkali treatment was measured using the method described above, the pH was 9.6. Further, when the moisture content of the tobacco raw material after the alkali treatment was measured by the method described above, the moisture content was 30% by weight based on the total weight of the tobacco raw material.

(Preparation for heat treatment and collection treatment)
After the inside of the rocking dryer container containing the alkali-treated tobacco raw material was reduced to a vacuum state, compressed air (approximately 20° C., approximately 60%-RH) was introduced into the rocking dryer container. Furthermore, by connecting the container of the rocking dryer and the container containing the collection solvent with an introduction pipe and flowing the compressed air at a flow rate of 15 L/min, the container of the rocking dryer contained the collection solvent. Developed air flow into the container. Water was used as the collection solvent.

(Heating treatment and collection treatment)
By introducing jacket steam to the outer periphery of the container of the rocking dryer, heat treatment of the alkali-treated tobacco raw material was started. Components released from the tobacco raw material upon heating were collected in a collection solvent via an introduction pipe.
The amount of nicotine and the amount of TSNA contained in the collection solvent (that is, the collection solution) that collected the components released from the tobacco raw materials were measured at regular intervals using the methods described above. Figures 5 and 6 show changes over time in the amount of nicotine recovered and the amount of TSNA recovered calculated from the results.

In the above heat treatment, the temperature was appropriately adjusted by adjusting the temperature and inflow amount of jacket steam so that the temperature of the alkali-treated tobacco raw material did not exceed 120°C.
Furthermore, the temperature of the alkali-treated tobacco raw material was measured at regular intervals using a thermocouple installed inside the container of the rocking dryer. The measurement results are shown in FIG.
Furthermore, the moisture content of the alkali-treated tobacco raw material was measured at regular intervals by the method described above. The measurement results are shown in FIG.
During the heat treatment, the container of the rocking dryer was rotated and rocked so that the alkali-treated tobacco raw material in the container was heated uniformly.

In addition, in the above-mentioned collection process, a cooling operation was performed as appropriate using a chiller in order to maintain the temperature of the collection solvent, that is, water, at 15°C±5°C.

(hydration treatment)
When the temperature of the alkali-treated tobacco raw material during the heat treatment reached 105° C. for the first time, the tobacco raw material was subjected to a hydrolysis treatment. This water addition treatment was carried out by spraying 220 g of water at a spray rate of 55 g/min through a sprayer included in the rocking dryer.
The moisture content of the alkali-treated tobacco raw material immediately before the hydrolysis treatment was 20% by weight based on the total weight of the tobacco raw material.
Further, the moisture content of the alkali-treated tobacco raw material immediately after the hydrolysis treatment was 35% by weight based on the total weight of the tobacco raw material.
During the hydration process, the container of the rocking dryer was rotated and rocked so that the alkali-treated tobacco raw material in the container was uniformly hydrated.

An experimental example including all the preparations and processes described above will be referred to as an example.
On the other hand, in the above-mentioned preparation and treatment (alkali treatment), ``270 g of a potassium carbonate aqueous solution obtained by dissolving 90 g of potassium carbonate in 180 g of water was sprayed onto the tobacco raw material at a spray rate of 55 g/min through a sprayer. '' was changed to the step of ``spraying 490 g of a potassium carbonate aqueous solution obtained by dissolving 90 g of potassium carbonate in 400 g of water onto tobacco raw materials at a spray rate of 55 g/min through a sprayer'', and (hydration treatment) An experimental example that was not performed will be used as a comparative example.

As shown in FIG. 5, in the example, the nicotine recovery rate exceeded 60% after 90 minutes of treatment time. On the other hand, in the comparative example, the nicotine recovery rate finally exceeds 60% after the processing time has passed for 160 minutes. Therefore, in the present invention, flavor components are released from the tobacco raw material at an earlier timing than in conventional methods.

Furthermore, as shown in Figure 6, in the example, the integrated value of the amount of TSNA recovered up to 90 minutes of processing time was 8735.09 ng, whereas in the comparative example, the amount of TSNA recovered up to 160 minutes of processing time was 8735.09 ng. Since the integrated value is 36608.27 ng, the amount of TSNA recovered can be more suppressed in the example in the processing time for recovering the same amount of nicotine.
Furthermore, in the comparative example, when the treatment time exceeds 160 minutes, the amount of TSNA recovered tends to increase. Therefore, by shortening the processing time, the amount of TSNA recovered can be suppressed.

Claims (8)

A method for extracting flavor components from tobacco raw materials or processed tobacco leaves, the method comprising:
Step A of heating the alkali-treated tobacco raw material or processed tobacco leaves using an alkali;
A step B of bringing the released component released into the gas phase in the step A into contact with a collection solvent,
In the step A,
The initial moisture content of the alkali-treated tobacco raw material or processed tobacco leaf is at least the minimum moisture content that can dissolve all of the alkali,
The alkali-treated tobacco raw material or processed tobacco leaf being heated is subjected to a hydration treatment,
Consistently, the moisture content of the alkali-treated tobacco raw material or processed tobacco leaf is 35% by weight or less based on the total weight of the tobacco raw material or the processed tobacco leaf,
Method for extracting flavor components. According to claim 1, in the step A, the initial moisture content of the alkali-treated tobacco raw material or the processed tobacco leaf is more than 20% by weight based on the total weight of the tobacco raw material or the processed tobacco leaf. Extraction method of flavor components described. The method for extracting flavor components according to claim 1 or 2, wherein the pH of the alkali-treated tobacco raw material or processed tobacco leaf is 9.5 or higher. In the step A, the hydrolysis treatment is performed when the temperature of the alkali-treated tobacco raw material or processed tobacco leaf reaches a temperature range of 100°C or more and 150°C or less for the first time. 3. The method for extracting flavor components according to any one of 3. In the step A, when the moisture content of the alkali-treated tobacco raw material or the processed tobacco leaf becomes 20% by weight or less based on the total weight of the tobacco raw material or the processed tobacco leaf for the first time, the The method for extracting flavor components according to any one of claims 1 to 4, wherein a hydrolysis treatment is performed. The method for extracting flavor components according to any one of claims 1 to 5, wherein the alkali is potassium carbonate or sodium carbonate. The method for extracting flavor components according to any one of claims 1 to 6, wherein in the step B, the temperature of the collection solvent is 5° C. or higher and 35° C. or lower. A method for producing components of processed tobacco leaves, the method comprising:
Step A of heating the alkali-treated tobacco raw material or processed tobacco leaves using an alkali;
Step B of contacting the released component released into the gas phase in the step A with a collection solvent to obtain a collection solution;
step C of adding the collection solution to the component,
In the step A,
The initial moisture content of the alkali-treated tobacco raw material or processed tobacco leaf is at least the minimum moisture content that can dissolve all of the alkali,
The alkali-treated tobacco raw material or processed tobacco leaf being heated is subjected to a hydration treatment,
A manufacturing method characterized in that the moisture content of the alkali-treated tobacco raw material or processed tobacco leaf is consistently 35% by weight or less based on the total weight of the tobacco raw material or processed tobacco leaf.

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