Tobacco component concentrate and its manufacturing method, and flavored product and its manufacturing method

The interfacial progressive freeze concentration method addresses the challenges of energy-intensive solvent removal and thermal denaturation in tobacco extract concentration, enabling low-cost, high-concentration tobacco component concentrates with retained flavor.

JP7777543B2Active Publication Date: 2025-11-28JAPAN TOBACCO INC
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Patent Information

Application Number
JP2022571082
Authority / Receiving Office
JP · JP
Patent Type
Patents
Current Assignee / Owner
Priority Date
2020-12-21
Filing Date
2021-10-13
Publication Date
2025-11-28
Estimated Expiration
2041-10-13

AI Technical Summary

Technical Problem

Existing methods for concentrating tobacco extracts face challenges such as energy-intensive solvent removal, thermal denaturation of flavor components, microbial contamination, and high equipment costs, making it difficult to produce a high-concentration tobacco component concentrate while retaining flavor.

Method used

A method using interfacial progressive freeze concentration, which involves cooling the solution to selectively solidify and remove the solvent, allowing for high-concentration tobacco component concentrates to be produced at low temperatures, preventing flavor loss and microbial contamination, and reducing energy consumption.

Benefits of technology

The method enables low-cost production of high-concentration tobacco component concentrates with retained flavor components, reducing energy costs and preventing microbial growth, while maintaining flavor integrity.

✦ Generated by Eureka AI based on patent content.

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Abstract

Provided is a method for manufacturing an inexpensive tobacco-component-concentrated liquid, the method making it possible to concentrate a flavor component to a high degree of concentration while adequately retaining the flavor component. This method for manufacturing a tobacco-component-concentrated liquid includes a step for concentrating a tobacco-component-containing liquid through a progressive freeze concentration method.
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Description

[Technical Field]

[0001] The present invention relates to a tobacco component concentrate and a method for producing the same, and a flavored product and a method for producing the same. [Background technology]

[0002] Extraction of tobacco components from tobacco raw materials is carried out for the purpose of improving the flavor of the tobacco raw material and reducing the content of other components in the tobacco raw material.

[0003] For example, Patent Document 1 discloses a method for obtaining tobacco raw materials with a good flavor by further extracting the residue of a leaf tobacco material with a low-polarity solvent using a high-polarity solvent, and then adding the extract extracted with the low-polarity solvent back to the residue. Patent Document 2 discloses a method for preparing a tobacco product with a reduced amount of phenolic compounds by extracting a tobacco material with a solvent to provide an extract and the residue, treating the extract with a phenol oxidase to reduce the amount of phenolic compounds, and then combining the extract with the residue. Patent Document 3 discloses a method for mixing a fraction obtained by steam distilling leaf tobacco as an essential oil with other materials. Patent Document 4 discloses a method for preparing a distillate by vacuum distilling a tobacco raw material. [Prior art documents] [Patent documents]

[0004] [Patent Document 1] International Publication No. 2015 / 029977 [Patent Document 2] Special Publication No. 2002-520005 [Patent Document 3] Special Publication No. 60-045909 [Patent Document 4] Chinese Patent Application Publication No. 104757703 Summary of the Invention [Problem to be solved by the invention]

[0005] The extract, fraction, or distillate obtained by the above method contains an extraction solvent such as water. Therefore, if the extract is added directly to a tobacco product, the extraction solvent must be removed by vaporization. However, this removal process requires energy costs. Therefore, it is possible to concentrate the extract before adding it to the tobacco product. By carrying out this concentration process, not only can the removal process be eliminated, but the volume of the extract can be reduced, thereby reducing transportation and storage costs. Furthermore, when the extraction solvent is water, the concentration process reduces the amount of water, thereby inhibiting the growth of microorganisms in the liquid and improving shelf life.

[0006] Commonly used methods for concentrating solutions include, for example, evaporation, membrane, and freeze-drying. Evaporation is a method in which the solvent in a solution is vaporized and removed by heating the solution. This method can be performed using simple equipment, which reduces equipment costs. However, when used to concentrate an extract containing tobacco components, heating can cause components useful for imparting flavor (hereinafter referred to as flavor components) in the tobacco components to volatilize and dissipate or to deteriorate. Furthermore, removing the solvent requires a large amount of energy.

[0007] Membrane concentration is a method of separating a solvent from a solution by applying pressure to the solution using a reverse osmosis (RO) membrane or similar. This method can be carried out at room temperature, which prevents thermal denaturation of the components in the solution and reduces energy consumption because no phase change occurs during the concentration and separation process. However, it is difficult to concentrate at high concentrations, and there is a risk of microbial contamination because the concentration operation is carried out at room temperature. Furthermore, cleaning and replacing the membrane requires time and money.

[0008] Freeze-drying is a method for removing a solvent by sublimating it from a frozen raw material. This method is also often used to concentrate liquids. In this method, the solvent in the raw material remains solid throughout the entire drying period, preventing it from moving in liquid form within the raw material. Furthermore, drying is performed at low temperatures, which can prevent thermal denaturation and chemical changes in the material. However, this method has many technical challenges to overcome and is expensive in terms of energy consumption and capital investment, so it is currently only practically applied to certain foods, such as fruits.

[0009] The present invention aims to provide a method for producing a low-cost tobacco component concentrate that can be concentrated to a high concentration while sufficiently retaining flavor components, a tobacco component concentrate obtained by said method, and a method for producing a flavor product that includes the method for producing said tobacco component concentrate, and a flavor product obtained by said method. [Means for solving the problem]

[0010] The present invention includes the following embodiments.

[0011] [1] A method for producing a tobacco component concentrate, comprising a step of concentrating a liquid containing tobacco components by an interfacial progressive freeze concentration method.

[0012] [2] Before the step of concentrating the liquid containing the tobacco component by the interfacial progressive freeze concentration method, The method according to [1], further comprising a step of extracting tobacco components in the tobacco raw material with a solvent to produce a liquid containing the tobacco components.

[0013] [3] The method according to [2], wherein the solvent comprises water.

[0014] [4] Before the step of concentrating the liquid containing the tobacco component by the interfacial progressive freeze concentration method, The method according to any one of [1] to [3], further comprising a step of filtering the liquid containing the tobacco components to remove solid matter.

[0015] [5] A method according to any one of [1] to [4], wherein, when the tobacco component concentrate is subjected to headspace analysis, in a chromatogram obtained by gas chromatography with a mass spectrometer (GC / MS), the ratio of the total area of ​​the peaks of a group of compounds with an RI of 2000 or less to the total area of ​​all peaks is 70% or more.

[0016] [6] A tobacco component concentrate produced by a method according to any one of [1] to [5].

[0017] [7] A step of producing a tobacco component concentrate by the method according to any one of [1] to [5]; a step of applying the tobacco component concentrate to a substrate and drying the substrate to produce a tobacco component-containing substrate; producing a flavored product comprising the tobacco-containing substrate; A method for producing a flavored product, comprising:

[0018] [8] A flavor product produced by the method described in [7].

[0019] [9] The flavor product according to [8], which is a combustion-type flavor inhaler or a non-combustion-heating-type flavor inhaler. [Effects of the Invention]

[0020] According to the present invention, it is possible to provide a low-cost method for producing a tobacco component concentrate that can be concentrated to a high concentration while sufficiently retaining flavor components, a tobacco component concentrate obtained by said method, and a method for producing a flavor product that includes the method for producing the tobacco component concentrate, and a flavor product obtained by said method. [Brief explanation of the drawings]

[0021] [Figure 1] FIG. 1 is a cross-sectional view showing an example of a freeze concentration apparatus that can be used in the interface progressive freeze concentration method of the present embodiment. [Figure 2] 1 is a cross-sectional view showing an example of a combustion-type flavor inhaler according to an embodiment of the present invention. [Figure 3]1A and 1B are schematic diagrams showing an example of a non-combustion heating type flavor inhalation system according to the present embodiment, illustrating (a) a state before a non-combustion heating type flavor inhalation tool is inserted into a heating device, and (b) a state after the non-combustion heating type flavor inhalation tool is inserted into the heating device and heated. [Figure 4] 1 shows chromatograms obtained by component analysis of the tobacco component concentrates of Example 1 and Comparative Example 1. [Figure 5] 5 is a graph showing the total peak area in each RI range of the chromatogram of FIG. 4. DETAILED DESCRIPTION OF THE INVENTION

[0022] [Manufacturing method of tobacco component concentrate] The method for producing a tobacco component concentrate according to this embodiment includes a step of concentrating a liquid containing tobacco components by a progressive interface freeze concentration method (hereinafter also referred to as a concentration step). The "freeze concentration method" is a method of increasing the concentration of a solution by cooling the solution to selectively solidify the solvent in the solution and physically separating and removing the solidified solvent. Note that the aforementioned "freeze drying method" freezes the entire solution, and then sublimes and removes only the solvent, and therefore differs from the "freeze concentration method" which selectively solidifies and removes only the solvent in the solution by cooling. In the method according to this embodiment, a liquid containing tobacco components is concentrated by a progressive interface freeze concentration method, which is one of the freeze concentration methods. The "progressive interface freeze concentration method" is a method of concentrating a solution by cooling to form a single large crystal of a solvent solid.

[0023] In the method according to the present embodiment, the concentration operation is performed at a low temperature, thereby preventing the flavor components contained in the liquid containing tobacco components from volatilizing and dissipating or from deteriorating. In other words, this method allows concentration while adequately preserving the flavor components. Furthermore, concentration at a low temperature also prevents microbial contamination. Furthermore, selective solidification of the solvent alone, followed by separation and removal of the solidified solvent, allows for a sufficiently high concentration of the concentrated liquid. Furthermore, compared to, for example, evaporation concentration methods, the latent heat required for phase change is approximately 1 / 7, thereby saving energy and reducing running costs. The method according to the present embodiment concentrates the liquid containing tobacco components using a progressive interfacial freeze concentration method, which is a freeze concentration method in particular. Therefore, it is less expensive than other freeze concentration methods such as suspension crystallization, and is capable of concentrating even highly viscous liquids.

[0024] The method according to this embodiment is not particularly limited as long as it includes the concentration step, but preferably further includes a step of extracting tobacco components from the tobacco raw material with a solvent to produce a liquid containing the tobacco components (hereinafter also referred to as a tobacco component extract production step) before the concentration step. It is also preferable that the method further includes a step of filtering the liquid containing the tobacco components to remove solids (hereinafter also referred to as a filtration step) before the concentration step. When the method includes both the tobacco component extract production step and the filtration step, the filtration step can be carried out after the tobacco component extract production step and before the concentration step. The method can also include other steps in addition to these steps. Each step will be described below, but the method according to this embodiment is not limited to embodiments related to each of these steps.

[0025] (Tobacco component extract manufacturing process) The method according to the present embodiment preferably further comprises, prior to the concentration step, a step of extracting tobacco components from the tobacco raw material with a solvent to produce a liquid containing the tobacco components. That is, the liquid containing the tobacco components is preferably a tobacco component extract obtained by extracting tobacco components from the tobacco raw material with a solvent. This step makes it possible to easily produce a liquid containing tobacco components (tobacco component extract).

[0026] A variety of tobacco varieties can be used as the tobacco raw material. Examples include flue-cured tobacco, burley tobacco, oriental tobacco, native tobacco, other Nicotiana tabacum varieties, and Nicotiana rustica varieties. These varieties can be used alone or in blends to achieve the desired flavor. Details of the tobacco varieties are disclosed in "Encyclopedia of Tobacco," Tobacco Research Center, March 31, 2009.

[0027] The form of the tobacco raw material is preferably a form suitable for extracting tobacco components, and can be, for example, tobacco pulverization, etc. Regarding the size of the tobacco raw material, for example, when the form of the tobacco raw material is tobacco pulverization, the average particle size can be 10 μm or less.

[0028] The solvent used for extraction is not particularly limited, and examples thereof include water, ethanol, chloroform, ethyl acetate, etc. These solvents may be used alone or in combination of two or more. Among these, water is preferred as the solvent from the viewpoint of easy control of freeze concentration.

[0029] From the viewpoint of efficient extraction, the mass ratio of the tobacco material to the total mass of the solvent and tobacco material during extraction is preferably 5 to 20 mass%, and more preferably 8 to 15 mass%. The extraction temperature depends on the extraction solvent, but can be, for example, 20 to 60°C. The extraction time depends on the extraction solvent and extraction temperature, but can be, for example, 1 to 3 hours. Extraction can be carried out, for example, by introducing the tobacco material and extraction solvent into an extraction device and stirring them.

[0030] In addition, the "liquid containing tobacco components" in the method according to this embodiment is not limited to the tobacco component extract, but may also be, for example, a fraction obtained by distilling tobacco raw materials, a compressed liquid of tobacco raw materials, etc.

[0031] (filtration process) The method according to the present embodiment preferably further includes a step of filtering the liquid containing tobacco components to remove solids prior to the concentration step. By performing the filtration step, solids contained in the liquid containing tobacco components, such as proteins and suspended solids, can be removed. This can prevent flavor components from being incorporated into the solidified solvent during the cooling process in the subsequent concentration step, thereby further improving the concentration of flavor components in the concentrated liquid.

[0032] Filtration of a liquid containing tobacco components can be carried out using a filter medium such as a filter cloth or membrane filter. The mesh size of the filter medium is not particularly limited, but when the main purpose is to remove fine tobacco powder and other suspended matter, it can be, for example, 0.1 μm to 800 μm. When the main purpose is to remove protein, the mesh size of the filter medium can be, for example, 2 nm to 100 nm. Filtration can also be carried out using two or more filter mediums with different mesh sizes.

[0033] (concentration process) The method according to the present embodiment includes a step of concentrating a liquid containing tobacco components using the progressive interface freeze concentration method. A common freeze concentration method is the suspension crystallization method. The suspension crystallization method concentrates a solution by cooling to form numerous fine crystals of a solvent-solidified product. However, this method requires high equipment costs, is limited in its application to large-scale continuous production, and has a long residence time. Therefore, the method according to the present embodiment concentrates a liquid containing tobacco components using the progressive interface freeze concentration method, which is one of the freeze concentration methods. The progressive interface freeze concentration method concentrates a solution by cooling to form a single large crystal of a solvent-solidified product. This method requires simple and versatile equipment and can reduce costs. Furthermore, while the viscosity of the solution to be concentrated using the suspension crystallization method is limited to approximately 200 cP, the progressive interface freeze concentration method can sufficiently concentrate even solutions with viscosities of 200 cP or more.

[0034] FIG. 1 shows an example of a freeze concentration apparatus that can be used in the progressive interface freeze concentration method of this embodiment. The freeze concentration apparatus 1 shown in FIG. 1 is provided with an agitator blade 4 inside, and a refrigerant 2 circulates around the periphery. A liquid 3 containing tobacco components is introduced into the freeze concentration apparatus 1, and the refrigerant 2 is set to a predetermined temperature while stirring with the agitator blade 4, thereby cooling the liquid 3 containing tobacco components to a predetermined temperature. After a predetermined time has passed since the start of cooling, a layer of solidified solvent 5 is formed on the inner surface of the freeze concentration apparatus 1, allowing the liquid 3 containing tobacco components to be concentrated. In the freeze concentration apparatus 1, cooling the liquid 3 containing tobacco components while stirring it can suppress the inflow of flavor components into the solidified solvent 5. Furthermore, by controlling the temperature of the refrigerant 2 and thereby controlling the temperature of the liquid 3 containing tobacco components to a predetermined temperature, freeze concentration can be performed in a short period of time. The freeze concentration apparatus that can be used in this embodiment is not limited to the batch-type freeze concentration apparatus 1 shown in FIG. 1 , but may also be, for example, a flow-through type freeze concentration apparatus.

[0035] The set temperature of the refrigerant 2 depends on the type of solvent contained in the tobacco component-containing liquid 3, but if the solvent is water, for example, it is preferably −15 to 0° C., and more preferably −10.0 to −3.0° C. At this set temperature, the temperature of the tobacco component-containing liquid 3 will be within the range of −3.0 to 0° C. By keeping the temperature within this range, it is possible to further suppress the inflow of flavor components into the solidified solvent 5 (ice), and also to complete the concentration operation in a short time.

[0036] The stirring speed of the stirring blades 4 is preferably 70 to 250 rpm, and more preferably 100 to 180 rpm. When the stirring speed is within the above range, the inflow of flavor components into the solidified solvent 5 can be further suppressed.

[0037] When freeze concentration is performed using a batch-type freeze concentration apparatus such as that shown in FIG. 1, the freeze concentration operation may be performed multiple times. For example, a liquid 3 containing tobacco components is introduced into the freeze concentration apparatus 1 shown in FIG. 1, cooled, and after a predetermined time has passed, the concentrated liquid 3 containing tobacco components is removed and the solidified solvent 5 formed on the inner surface of the freeze concentration apparatus 1 is recovered. The concentrated liquid 3 containing tobacco components is then introduced back into the freeze concentration apparatus 1, cooled, and the concentration operation is performed again. This operation may be repeated two or more times, or even three or more times. Repeating this operation can sufficiently increase the concentration ratio ((mass of liquid containing tobacco components after concentration / mass of liquid containing tobacco components before concentration) * 100). The concentration ratio in this concentration step can be appropriately set according to the desired purpose, but can be, for example, 5 to 20%, and preferably 7 to 15%.

[0038] In particular, in the method according to the present embodiment, flavor components are sufficiently retained in the tobacco component concentrate even after the concentration step. Specifically, when headspace analysis of the tobacco component concentrate obtained by the method according to the present embodiment is performed, in a chromatogram obtained by gas chromatography with a mass spectrometer (GC / MS), the ratio of the total area of ​​peaks of compounds with an RI of 2000 or less (the ratio of compounds with 20 or less carbon atoms) to the total area of ​​all peaks is preferably 70% or more, more preferably 80% or more, even more preferably 90% or more, and particularly preferably 95% or more. The upper limit of this ratio range is not particularly limited, but can be, for example, 99.9% or less. Furthermore, in the chromatogram, the ratio of the total area of ​​peaks of compounds with an RI of 1000 to 2000 (the ratio of compounds with 10 to 20 carbon atoms) is preferably 55% or more, more preferably 65% ​​or more, and even more preferably 70% or more. The upper limit of this ratio range is not particularly limited, but can be, for example, 90% or less. In the chromatogram, the ratio of the total area of ​​the peaks of compounds with an RI of 1000 or less (the ratio of compounds with 10 or less carbon atoms) is preferably 20% or more, more preferably 25% or more. The upper limit of this ratio range is not particularly limited, but can be, for example, 50% or less. The analytical conditions for gas chromatography with a mass spectrometer (GC / MS) are as follows:

[0039] <Analysis conditions> Gas chromatography with mass spectrometry (GC / MS) Instrument: Agilent Technologies 7890B / 5977B GC / MSD ·GC conditions Column: HP-5MS UI (Agilent Technologies) Inner diameter 0.25mm x length 30m, film thickness 0.25μm Injection volume: 1μl Injection mode: Split (10:1) Inlet temperature: 270℃ Septum purge flow rate: 5 ml / min Carrier gas: Helium (He) Column flow rate: 1 ml / min (constant flow mode) Oven temperature: 40°C (3 min) - 4°C / min - 280°C (20 min) Transfer line temperature: 280℃ MS conditions Solvent waiting time: 4 minutes Ionization method: Electron impact ionization (EI), 70 eV Ion source temperature: 230℃ Quadrupole temperature: 150℃ Measurement mode: Scan MS scan range: m / z 26-450 Threshold: 50 Sampling rate: 2

[0040] The peaks of the compound group with an RI of 2000 or less in the chromatogram mainly correspond to flavor components, and by having the ratio fall within the above range, the flavor components are contained in sufficient amounts in the tobacco component concentrate. RI stands for retention index, and is calculated specifically by the method described below.

[0041] [Tobacco ingredient concentrate] The tobacco component concentrate according to the present embodiment is produced by the tobacco component concentrate production method according to the present embodiment. Because the tobacco component concentrate is produced by the method according to the present embodiment, it can have a high content of flavor components and a low solvent concentration (high concentration rate).

[0042] For example, when the tobacco raw material is flue-cured tobacco, with regard to the content of flavor components, as described above, in a chromatogram obtained by analysis using the above-mentioned analytical method, the ratio of the total area of ​​peaks of compounds with an RI of 1000 or less (the ratio of the total area of ​​peaks of compounds with 10 or less carbon atoms) to the total area of ​​all peaks is preferably 20% or more, and in this case, the tobacco component concentrate contains a large amount of compounds such as 6-methyl-5-hepten-2-one. Furthermore, the ratio of the total area of ​​peaks of compounds with an RI of 2000 or less (the ratio of the total area of ​​peaks of compounds with 20 or less carbon atoms) is preferably 70% or more. A high content of compounds with an RI of 2000 or less (compounds with 20 or less carbon atoms) results in a good amount and balance of flavor components.

[0043] Furthermore, with regard to the solvent concentration, for example, when the solvent is water, the water content in the tobacco component concentrate is preferably 20 to 90 mass %, more preferably 40 to 80 mass %, as measured by Karl Fischer titration.

[0044] [Method of manufacturing flavored products] The method for producing a flavor product according to this embodiment includes the steps of producing a tobacco component concentrate using the method according to this embodiment (hereinafter referred to as the tobacco component concentrate production step), applying the tobacco component concentrate to a substrate and drying it to produce a tobacco component-containing substrate (hereinafter referred to as the tobacco component-containing substrate production step), and producing a flavor product comprising the tobacco component-containing substrate (hereinafter referred to as the flavor product production step). In the method according to this embodiment, a tobacco component concentrate is produced using the method according to this embodiment, and a flavor product is produced using the tobacco component concentrate, making it possible to produce a flavor product containing a predetermined amount of flavor components at low cost. The method according to this embodiment is not particularly limited as long as it includes the tobacco component concentrate production step, the tobacco component-containing substrate production step, and the flavor product production step, and may further include other steps besides these steps.

[0045] (Tobacco ingredient-containing base material manufacturing process) The method according to this embodiment includes a step of applying the tobacco component concentrate produced by the method according to this embodiment to a substrate and drying the substrate to produce a tobacco component-containing substrate. The substrate is not particularly limited, but examples include the residue and pulp remaining after extracting tobacco components from tobacco raw materials with a solvent in the tobacco component extract production process. The tobacco component concentrate can be applied to the substrate by, for example, coating. The drying conditions after applying the tobacco component concentrate to the substrate are not particularly limited. For example, in the case of hot air drying, drying can be performed at 35 to 100°C until the final moisture content reaches the desired value. Moisture can also be removed using far infrared rays, mid-infrared rays, or near infrared rays. Drying using infrared rays can suppress evaporation and denaturation due to heat compared to hot air drying, thereby preserving the tobacco components more effectively. Furthermore, drying using infrared rays has the advantage of selectively vaporizing components.

[0046] When the flavor product is a non-combustion heating type flavor inhaler, an aerosol-generating substrate that generates aerosol smoke upon heating may be further applied to the substrate. The type of aerosol-generating substrate is not particularly limited, and extracts from various natural products and / or their constituent components may be selected depending on the application. Specific examples of the aerosol-generating substrate include, but are not limited to, polyhydric alcohols such as glycerin, propylene glycol, sorbitol, xylitol, and erythritol, triacetin, 1,3-butanediol, and mixtures thereof. In addition to the tobacco component concentrate and the aerosol-generating substrate, a flavoring or the like may also be applied to the substrate.

[0047] (Flavor producing product manufacturing process) The method according to this embodiment includes a step of producing a flavor product comprising the tobacco component-containing substrate produced by the method. The flavor product may be, for example, a combustion-type flavor inhaler or a non-combustion-heating flavor inhaler, as described below. The tobacco component-containing substrate may be contained in, for example, a tobacco-containing segment of the device. The flavor product may be produced by a known method.

[0048] [Flavour-generating articles] The flavor product according to the present embodiment is manufactured by the method for manufacturing a flavor product according to the present embodiment. Since the flavor product is manufactured by the method for manufacturing a flavor product according to the present embodiment, it can contain a desired amount of flavor components and is low-cost. Examples of the flavor product include a combustion-type flavor inhaler and a non-combustion-heating-type flavor inhaler.

[0049] (Combustion-type flavor inhaler) An example of a combustion-type flavor inhalation device according to this embodiment is shown in FIG. 2. As shown in FIG. 2, the combustion-type flavor inhalation device 6 includes a tobacco-containing segment 7 and a filter segment 8 disposed adjacent to the tobacco-containing segment 7. The tobacco-containing segment 7 includes a tobacco filler 9 containing a tobacco component-containing substrate to which the tobacco component concentrate according to this embodiment has been applied, and cigarette paper 10 wrapped around the tobacco filler 9. The filter segment 8 is not particularly limited as long as it functions as a general filter, and can be, for example, a tow (also simply referred to as "tow") made of synthetic fiber or a cylindrically shaped material such as paper. The tobacco-containing segment 7 and the filter segment 8 are connected by a tipping paper member 11 wrapped around the tobacco-containing segment 7 and the filter segment 8. The tipping paper member 11 may have a ventilation hole in part of its outer periphery. The number of ventilation holes may be one or more, for example, 10 to 40. When the number of ventilation holes is more than one, the ventilation holes may be arranged, for example, in a circular line around the outer periphery of the tipping paper member 11. The plurality of ventilation holes can be arranged at substantially regular intervals. By providing the ventilation holes, air is drawn into the filter segment 8 through the ventilation holes during inhalation. By diluting the mainstream smoke with outside air through the ventilation holes, a product with a desired tar value can be designed.

[0050] The user can enjoy the flavor of tobacco by lighting the tip of the tobacco-containing segment 7 and drawing on the mouth end of the filter segment 8. The number of filter segments 8 is not limited to one, and multiple filter segments with different functions may be connected together.

[0051] (Non-combustion heating type flavor inhaler) The non-combustion and heating type flavor inhalation device according to this embodiment may include, for example, a tobacco-containing segment, a cylindrical cooling segment having perforations on its circumference, a center-hole segment, and a filter segment. The non-combustion and heating type flavor inhalation device according to this embodiment may include other segments in addition to the tobacco-containing segment, cooling segment, center-hole segment, and filter segment.

[0052] The axial length of the non-combustion and heating type flavor inhalation device according to this embodiment is not particularly limited, but is preferably 40 mm to 90 mm, more preferably 50 mm to 75 mm, and even more preferably 50 mm to 60 mm. The circumferential length of the non-combustion and heating type flavor inhalation device is preferably 16 mm to 25 mm, more preferably 20 mm to 24 mm, and even more preferably 21 mm to 23 mm. For example, the tobacco-containing segment may be 20 mm long, the cooling segment 20 mm long, the center hole segment 8 mm long, and the filter segment 7 mm long. The length of the filter segment may be selected within a range of 4 mm to 10 mm. The airflow resistance of the filter segment is selected to be 15 mmH2O / segment or more and 60 mmH2O / segment or less per segment. These individual segment lengths may be appropriately adjusted depending on manufacturing suitability, required quality, and the like. Furthermore, even if a center hole segment is not used and only a filter segment is disposed downstream of the cooling segment, it can still function as a non-combustion heating type flavor inhaler.

[0053] <Tobacco-containing segment> The tobacco-containing segment may include a tobacco filler containing a tobacco component-containing substrate to which the tobacco component concentrate according to this embodiment has been applied, and cigarette paper wrapped around the tobacco filler. The method for filling the tobacco filler into the cigarette paper (hereinafter also referred to as a wrapper) is not particularly limited; for example, the tobacco filler may be wrapped in the wrapper, or the tobacco filler may be filled into a tubular wrapper. When the tobacco component-containing substrate has a longitudinal direction, such as a rectangular shape, the tobacco component-containing substrates may be filled so that the longitudinal direction is in an unspecified direction within the wrapper, or may be aligned so that the longitudinal direction is in the axial direction of the tobacco-containing segment or perpendicular to the axial direction. When the tobacco-containing segment is heated, the tobacco components (flavor components), aerosol-generating substrate, and water contained in the tobacco filler vaporize, and are transferred to the mouthpiece segment by inhalation.

[0054] <Cooling segment> The cooling segment may be formed of a cylindrical member, for example, a cardboard tube formed into a cylindrical shape.

[0055] The total surface area of ​​the cooling segment is 300 mm 2 / mm or more, 1000mm 2 / mm or less. This surface area is the surface area per length (mm) of the cooling segment in the airflow direction. The total surface area of ​​the cooling segment is 400 mm 2 / mm or more is preferable, and 450mm 2 / mm or more is more preferable, while 600mm 2 / mm or less is preferable, and 550mm 2 / mm or less is more preferable.

[0056] It is desirable for the cooling segment to have a large total surface area due to its internal structure. Thus, in a preferred embodiment, the cooling segment may be formed by a thin sheet of material that is wrinkled to form channels, and then pleated, gathered, and folded. The more folds or pleats within a given volume of the element, the greater the total surface area of ​​the cooling segment.

[0057] In some embodiments, the thickness of the cooling segment material may be 5 μm or more and 500 μm or less, such as 10 μm or more and 250 μm or less.

[0058] The aerosol cooling element has a specific surface area of ​​10 mm 2 / mg or more, 100mm 2 In one embodiment, the specific surface area of ​​the constituent material is about 35 mm 2 The specific surface area can be calculated as 1 / mg. The specific surface area can be determined by considering a material with a known width and thickness. For example, the material can be polylactic acid with an average thickness of 50 μm and a variation of ±2 μm. If the material also has a known width, for example, between 200 mm and 250 mm, the specific surface area and density can be calculated.

[0059] The tubular member and the mouthpiece lining paper, which will be described later, are provided with perforations that penetrate both. The presence of the perforations allows outside air to be introduced into the cooling segment during inhalation. As a result, the vaporized aerosol components generated by heating the tobacco-containing segment come into contact with the outside air, their temperature drops, and they liquefy, forming an aerosol. The diameter (distance across) of the perforations is not particularly limited, but may be, for example, 0.5 mm or more and 1.5 mm or less. The number of perforations is not particularly limited, and may be one or two or more. For example, multiple perforations may be provided around the circumference of the cooling segment.

[0060] The amount of outside air introduced through the perforations is preferably 85% by volume or less, more preferably 80% by volume or less, of the total volume of gas inhaled by the user. By keeping the ratio of the amount of outside air at 85% by volume or less, it is possible to sufficiently suppress the reduction in flavor due to dilution by the outside air. This is also called the ventilation ratio. From the viewpoint of cooling performance, the lower limit of the ventilation ratio range is preferably 55% by volume or more, more preferably 60% by volume or more.

[0061] Preferably, the cooling segment offers little resistance to air passing through the tobacco-containing segment. Preferably, the cooling segment does not substantially affect the resistance to draw of the non-combustion heating flavor inhalation device. Resistance to draw (RTD) is the pressure required to force air through the entire length of the object under a test of 17.5 ml / sec flow rate at 22°C and 101 kPa (760 Torr). RTD is typically expressed in mmH2O and is measured in accordance with ISO 6565:2011. Therefore, it is preferable that the pressure drop from the upstream end of the cooling segment to the downstream end of the cooling segment is small. To achieve this, it is preferable that the longitudinal porosity is greater than 50% and the airflow path through the cooling segment is relatively unrestricted. The longitudinal porosity of the cooling segment can be determined by the ratio of the cross-sectional area of ​​the material forming the cooling segment to the internal cross-sectional area of ​​the cooling segment.

[0062] In some embodiments, the generated aerosol may experience a temperature drop of 10° C. or more as it passes through the cooling segment and is drawn by the user. In another embodiment, the temperature drop may be 15° C. or more, and in yet another embodiment, 20° C. or more.

[0063] The cooling segment may be constructed from a sheet material selected from the group consisting of metal foil, polymer sheet, and substantially non-perforated paper or cardboard. In one embodiment, the cooling segment may comprise a sheet material selected from the group consisting of polyethylene, polypropylene, polyvinyl chloride, polyethylene terephthalate, polylactic acid, cellulose acetate, and aluminum foil. The construction material of the cooling segment may be made from a biodegradable material, such as non-perforated paper, or a biodegradable polymer such as polylactic acid, or a starch-based copolymer.

[0064] Preferably, the airflow through the cooling segments does not substantially deviate between adjacent segments. In other words, the airflow through the cooling segments preferably follows the longitudinal segments without substantial radial deviation. In some embodiments, the cooling segments are formed from a material that has low porosity or is substantially pore-free, except for the longitudinally extending channels. The material used to define or form the longitudinally extending channels, e.g., a creped or gathered sheet, has low porosity or is substantially pore-free.

[0065] As noted above, the cooling segment may comprise a sheet of suitable construction material that is wrinkled, pleated, gathered, or folded. The cross-sectional profile of such an element may exhibit randomly oriented channels. The cooling segment may be formed by other means. For example, the cooling segment may be formed from a bundle of longitudinally extending tubes. The cooling segment may be formed by extrusion, molding, lamination, injection, or chopping of suitable material.

[0066] The cooling segment can be formed, for example, by wrapping a pleated, gathered, or folded sheet material with a wrapping paper. In some embodiments, the cooling segment can include a sheet of crinkled material gathered into a rod shape and bound by a wrapper, e.g., a filter paper wrapping paper.

[0067] The cooling segment may be formed in a rod shape with an axial length of, for example, 7 mm to 28 mm, For example, the axial length of the cooling segment may be 18 mm.

[0068] In some embodiments, the cooling segment may have a substantially circular axial cross-sectional shape and a diameter of at least 5 mm and not more than 10 mm, for example, the diameter of the cooling segment may be about 7 mm.

[0069] <Center hole segment> The center hole segment is composed of a filling layer having one or more hollow portions and an inner plug wrapper (inner wrapping paper) covering the filling layer. For example, the center hole segment is composed of a second filling layer having a hollow portion and a second inner plug wrapper covering the second filling layer. The center hole segment functions to increase the strength of the mouthpiece segment. The second filling layer can be, for example, a rod with an inner diameter of 1.0 mm or more and 5.0 mm or less, which is densely packed with cellulose acetate fibers and hardened by adding a plasticizer containing triacetin in an amount of 6% by mass or more and 20% by mass or less relative to the mass of the cellulose acetate. Because the second filling layer has a high fiber packing density, during inhalation, air and aerosol flow only through the hollow portions and hardly flow within the second filling layer. Because the second filling layer inside the center hole segment is a fiber-packed layer, the feel from the outside during use is less likely to cause discomfort to the user. Note that the center hole segment may not have a second inner plug wrapper and its shape may be maintained by thermoforming.

[0070] <filter segment> The configuration of the filter segment is not particularly limited, and may be composed of one or more packed layers. The packed layer may be wrapped with one or more wrapper sheets. The airflow resistance per filter segment can be appropriately changed depending on the amount and material of the filler packed in the filter segment. For example, when the filler is cellulose acetate fiber, the airflow resistance can be increased by increasing the amount of cellulose acetate fiber packed in the filter segment. When the filler is cellulose acetate fiber, the packing density of the cellulose acetate fiber is 0.13 to 0.18 g / cm. 3 The airflow resistance is a value measured using an airflow resistance measuring device (trade name: SODIMAX, manufactured by SODIM).

[0071] The circumferential length of the filter segment is not particularly limited, but is preferably 16 to 25 mm, more preferably 20 to 24 mm, and even more preferably 21 to 23 mm. The axial length of the filter segment can be selected from 4 to 10 mm, and is selected so that the airflow resistance is 15 to 60 mmH2O / seg. The axial length of the filter segment is preferably 5 to 9 mm, more preferably 6 to 8 mm. The cross-sectional shape of the filter segment is not particularly limited, but may be, for example, circular, elliptical, polygonal, etc. In addition, a flavor-containing breakable capsule, flavor beads, or flavor may be directly added to the filter segment.

[0072] The center hole segment and the filter segment can be connected by an outer plug wrapper (outer wrapping paper). The outer plug wrapper can be, for example, a cylindrical piece of paper. The tobacco-containing segment, the cooling segment, and the connected center hole segment and filter segment can also be connected by a mouthpiece lining paper. These connections can be made, for example, by applying glue such as vinyl acetate glue to the inner surface of the mouthpiece lining paper, and then wrapping the three segments. These segments may also be connected in multiple layers using multiple lining papers.

[0073] (Non-combustion heating type flavor inhalation system) The non-combustion heating type flavor inhalation system according to this embodiment may include the non-combustion heating type flavor inhalation implement according to this embodiment and a heating device that heats the tobacco-containing segment of the non-combustion heating type flavor inhalation implement. The non-combustion heating type flavor inhalation system according to this embodiment may have other configurations in addition to the non-combustion heating type flavor inhalation implement according to this embodiment and the heating device.

[0074] An example of a non-combustion heating type flavor inhalation system according to this embodiment is shown in Figure 3. The non-combustion heating type flavor inhalation system shown in Figure 3 includes a non-combustion heating type flavor inhalation device 12 according to this embodiment and a heating device 13 that heats the tobacco-containing segment of the non-combustion heating type flavor inhalation device 12 from the outside.

[0075] FIG. 3(a) shows the non-combustion heat-type flavor inhalation device 12 in a state before it is inserted into the heating device 13, and FIG. 3(b) shows the non-combustion heat-type flavor inhalation device 12 inserted into the heating device 13 and being heated. The heating device 13 shown in FIG. 3 comprises a body 14, a heater 15, a metal tube 16, a battery unit 17, and a control unit 18. The body 14 has a cylindrical recess 19, and the heater 15 and metal tube 16 are disposed on the inner side of the recess 19 at a position corresponding to the tobacco-containing segment of the non-combustion heat-type flavor inhalation device 12 to be inserted into the recess 19. The heater 15 may be an electric resistance heater, and is heated by being supplied with power from the battery unit 17 in response to instructions from the control unit 18, which controls the temperature. The heat generated by the heater 15 is transferred to the tobacco-containing segment of the non-combustion heat-type flavor inhalation device 12 via the metal tube 16, which has high thermal conductivity.

[0076] 3(b) is a schematic illustration, and therefore there is a gap between the outer periphery of the non-combustion heating type flavor inhalation device 12 and the inner periphery of the metal tube 16, but in reality, for the purpose of efficient heat transfer, it is preferable that there is no gap between the outer periphery of the non-combustion heating type flavor inhalation device 12 and the inner periphery of the metal tube 16. Note that although the heating device 13 heats the tobacco-containing segment of the non-combustion heating type flavor inhalation device 12 from the outside, it may also heat from the inside.

[0077] The heating temperature by the heating device is not particularly limited, but is preferably 400° C. or less, more preferably 150° C. or more and 400° C. or less, and even more preferably 200° C. or more and 350° C. or less. The heating temperature refers to the temperature of the heater of the heating device. [Example]

[0078] The present embodiment will be described in detail below with reference to examples, but the present embodiment is not limited to these examples. Analysis of the components of the tobacco component concentrate was carried out by the following method.

[0079] [Component analysis of tobacco concentrate] Headspace analysis was performed on the tobacco component concentrates obtained in each Example and Comparative Example. First, 5 mL of the tobacco component concentrate was heated at 60°C for 1 hour to adsorb volatile components onto an adsorbent. The adsorbent used was Monotrap RCC 18 (product name) manufactured by GL Sciences. 300 μL of a 1:1 (volume ratio) hexane:acetone mixed solvent was added to the adsorbent for extraction. The resulting extract was analyzed by a gas chromatograph equipped with a mass spectrometer (GC / MS). The gas chromatograph used was a 7890B manufactured by Agilent, with a 5977B MSD (product name) detector and an HP-5 ms UI (30 m × 250 μm × 0.25 μm) column. Helium gas was used as the carrier gas, and the flow rate was 1.0 mL per minute. The temperature was increased from 40°C to 280°C at a rate of 4°C per minute and maintained at 280°C for 20 minutes.

[0080] The retention index (RI) of the chromatogram obtained by the above analysis was calculated by the following method. The retention index (RI) was calculated by the linear method using an n-alkane mixture ranging from n-hexane (C6, RI: 600) to n-pentatricontane (C35, RI: 3500). Note that the n-alkane mixture used to calculate the retention index (RI) is not limited to this. RI: 0 to 1000 corresponds to a group of compounds having 10 or less carbon atoms, RI: 1000 to 1500 corresponds to a group of compounds having 10 to 15 carbon atoms, RI: 1500 to 2000 corresponds to a group of compounds having 15 to 20 carbon atoms, and RI: 2000 to 2500 corresponds to a group of compounds having 20 to 25 carbon atoms.

[0081] [Example 1] (Tobacco component extract manufacturing process) Tobacco leaves (flue-cured) and water were mixed in a mass ratio of tobacco leaves:water=1:10, and the mixture was stirred at 50° C. for 2 hours to obtain a tobacco component extract.

[0082] (filtration process) The tobacco component extract was filtered using a filter cloth (a nylon gyoza piping bag, mesh size: 0.45 mm) to remove fine particles from the tobacco component extract.

[0083] (concentration process) The tobacco component extract after the filtration step was concentrated by a progressive interface freeze concentration method using an agitation freeze concentration device (product name: PFC-M10, manufactured by Meiwa Kogyo Co., Ltd.). Specifically, 10 kg of the tobacco component extract was placed in a 12 L container and concentrated to 7.145 kg under conditions of a brine temperature of -17°C while stirring at 120 rpm, to obtain a first concentrate (concentration rate: 71.45%). At the same time, 2.855 kg of first ice was collected as the ice portion. Thereafter, 7.145 kg of the first concentrate was placed in an 8 L container and concentrated to 3.765 kg under conditions of a brine temperature of -17°C while stirring at 120 rpm, to obtain a second concentrate (concentration rate: 37.65%). At the same time, 3.38 kg of second ice was collected as the ice portion. Furthermore, 3.765 kg of the second concentrate was placed in a 6 L container and concentrated to 1.605 kg under conditions of a brine temperature of -17°C while stirring at 150 rpm, to obtain a third concentrate (tobacco component concentrate) (concentration rate 16.05%). At the same time, 2.16 kg of third ice was collected as the ice portion.

[0084] The tobacco component concentrate thus obtained was subjected to component analysis using the method described above. The chromatogram obtained by the component analysis is shown in Figure 4. The total peak area in each RI range in the chromatogram is shown in Figure 5. The percentage of the total peak area in each RI range is also shown in Table 1.

[0085] [Comparative Example 1] (Tobacco component extract manufacturing process, filtration process) A tobacco component extract was prepared in the same manner as in Example 1, and a filtration step was carried out.

[0086] (concentration process) The tobacco component extract after the filtration step was concentrated by evaporation. Specifically, 200 g of the tobacco component extract was concentrated to 32 g by heating under reduced pressure of 40 mmHg while maintaining the temperature at 40°C using a rotary evaporator (manufactured by Nippon Buchi). The evaporation temperature was 34°C. This resulted in a tobacco component concentrate (concentration rate 16%).

[0087] The tobacco component concentrate thus obtained was subjected to component analysis using the method described above. The chromatogram obtained by the component analysis is shown in Figure 4. The total peak area in each RI range in the chromatogram is shown in Figure 5. The percentage of the total peak area in each RI range is also shown in Table 1.

[0088] [Table 1]

[0089] As is clear from the chromatogram shown in FIG. 4, when Example 1 and Comparative Example 1 are compared, it is found that Example 1 has a larger number of peaks of the component group having an RI of 2000 or less (compound group having 20 or less carbon atoms) than Comparative Example 1, and the intensity of each peak is also greater.

[0090] As shown in FIG. 5 and Table 1, it was found that, particularly within the RI range of 1000 to 1500, Example 1 had approximately three times as many components within this range as Comparative Example 1. Examples of components within this RI range include phenolic compounds characterized by various tobacco-specific aromas. Furthermore, within the RI range of 1500 to 2000, it was found that Example 1 had approximately two times as many components within this range as Comparative Example 1. Examples of components within this RI range include carotenoid degradation products such as megastigmatluenone, a type of tobacco flavor component.

[0091] From the above results, it was confirmed that concentration by the freeze concentration method can sufficiently concentrate a liquid containing tobacco components, such as a tobacco component extract, while retaining more of the aroma components contained in the liquid, compared to conventional evaporation concentration methods.

[0092] [Example 2, Comparative Example 2] 5 g of the tobacco component concentrates prepared in Example 1 and Comparative Example 1 were sprayed onto 50 g of tobacco base sheet shreds to add flavor. The resulting aromatized sheet shreds were each dried at 35°C for 1 hour in open air to obtain aromatized sheet shreds. A non-combustion heat-type flavor inhaler containing the aromatized sheet shreds in a tobacco-containing segment was prepared, and the tobacco-containing segment of the device was heated externally and inhaled, and flavor evaluation was performed. The non-combustion heat-type flavor inhaler containing the aromatized sheet shreds of Example 1 (Example 2) expressed the original tobacco aroma better than the non-combustion heat-type flavor inhaler containing the aromatized sheet shreds of Comparative Example 1 (Comparative Example 2). [Explanation of symbols]

[0093] 1 Freeze concentrator 2. Refrigerant 3. Liquid containing tobacco ingredients 4 stirring blades 5 Solidified solvent 6. Combustion-type flavor inhaler 7 Tobacco-containing segment 8 filter segments 9. Tobacco filler 10 Rolling Paper 11 Tipping paper component 12 Non-combustion heating type flavor inhaler 13 Heating device 14 Body 15 Heater 16 metal tube 17 Battery unit 18 Control Unit 19 Recess

Claims

1. A step of extracting tobacco components from a tobacco raw material with a solvent containing water to produce a liquid containing the tobacco components; Concentrating the liquid containing the tobacco components by an interface progressive freeze concentration method; A method for producing a tobacco component concentrate, comprising: The water content in the tobacco component concentrate is 40 to 90% by mass, A method for producing a tobacco component concentrate, wherein, when the tobacco component concentrate is subjected to headspace analysis, the ratio of the total area of ​​the peaks of a group of compounds having an RI of 2000 or less to the total area of ​​all peaks in a chromatogram obtained by gas chromatography with a mass spectrometer (GC / MS) is 70% or more.

2. Before the step of concentrating a liquid containing tobacco components by the interfacial progressive freeze concentration method, The method of claim 1 , further comprising filtering the liquid containing the tobacco components to remove solids.

3. A step of producing a tobacco component concentrate by the method according to claim 1 or 2; a step of applying the tobacco component concentrate to a substrate and drying the substrate to produce a tobacco component-containing substrate; producing a flavored product comprising the tobacco-containing substrate; A method for producing a flavored product, comprising:

4. A method for producing a flavor product as described in claim 3, wherein the flavor product is a combustion-type flavor inhaler or a non-combustion-heating-type flavor inhaler.

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