WO2022024307A1 - 香味成分の抽出方法及び加工済たばこ葉の構成要素の製造方法 - Google Patents
香味成分の抽出方法及び加工済たばこ葉の構成要素の製造方法 Download PDFInfo
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- WO2022024307A1 WO2022024307A1 PCT/JP2020/029275 JP2020029275W WO2022024307A1 WO 2022024307 A1 WO2022024307 A1 WO 2022024307A1 JP 2020029275 W JP2020029275 W JP 2020029275W WO 2022024307 A1 WO2022024307 A1 WO 2022024307A1
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/24—Treatment of tobacco products or tobacco substitutes by extraction; Tobacco extracts
- A24B15/241—Extraction of specific substances
- A24B15/243—Nicotine
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/24—Treatment of tobacco products or tobacco substitutes by extraction; Tobacco extracts
Definitions
- the present invention relates to a method for extracting flavor components and a method for producing components of processed tobacco leaves.
- a flavor component for example, an alkaloid containing a nicotine component
- the extracted flavor component is supported on a component of processed tobacco leaves.
- Patent Document 1 and Patent Document 2 describe a step A of heating an alkaline-treated tobacco raw material and a solvent for collecting released components released into the gas phase in the step A until a specific timing at room temperature.
- a technique relating to an extraction method of a flavor component for extracting a flavor component from a tobacco raw material which comprises a step B of obtaining a collection solution by contacting with.
- Patent Document 1 and Patent Document 2 relate to a method for producing a component of a luxury product (processed tobacco leaf), which comprises a step C of adding the collected solution to the component in addition to the steps A and B. The technology is disclosed.
- the steps A and B for extracting the flavor component from the tobacco raw material require a certain amount of extraction processing time or more in order to recover a certain amount of the flavor component from the tobacco raw material.
- 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 shortening the extraction processing time from the viewpoint of efficiency in producing the components of the processed tobacco leaves.
- Patent Document 1 and Patent Document 2 tobacco-specific nitrosamine (hereinafter, simply referred to as simply) which is a component having an undesired effect on flavor and the like when the extraction processing time in the step A and the step B exceeds a certain level. It is disclosed that the amount of "TSNA” (also referred to as "TSNA”) released from the tobacco raw material tends to increase. Therefore, it is expected that the TSNA concentration in the collection solution can be kept at a lower level by shortening the extraction processing time.
- TSNA also referred to as "TSNA”
- the time required to extract a certain amount of flavor components from the tobacco raw material or the processed tobacco leaves can be shortened as compared with the conventional method, and the TSNA concentration in the collection solution in which the flavor components are collected can be further increased. It is an object of the present invention to provide a method for extracting a flavor component that can be maintained at a low level, and a method for producing a component of processed tobacco leaves including the extraction method.
- the initial water content of the alkaline-treated tobacco raw material or processed tobacco leaf in the step of heating the alkaline-treated tobacco raw material or processed tobacco leaf to extract the flavor component is consistently water-treated, and the water content of the alkaline-treated tobacco raw material or processed tobacco leaf is not more than the specified amount.
- the present invention is as follows.
- a method for extracting flavor components from tobacco raw materials or processed tobacco leaves Step A of heating tobacco raw materials or processed tobacco leaves that have been treated with alkali using alkali, A step B of bringing the released component released into the gas phase into contact with the collecting solvent in the step A is provided.
- the initial water content of the alkali-treated tobacco raw material or processed tobacco leaves is equal to or higher than the minimum water content capable of dissolving all of the alkali.
- the alkali-treated tobacco raw material or processed tobacco leaves being heated are hydrated and treated. Consistently, the water content of the alkali-treated tobacco raw material or processed tobacco leaf is 35% by weight or less with respect to the total weight of the tobacco raw material or the processed tobacco leaf.
- the initial water content of the alkali-treated tobacco raw material or the processed tobacco leaf is more than 20% by weight with respect to the total weight of the tobacco raw material or the processed tobacco leaf.
- the method for extracting a flavor component according to. [3] The method for extracting a flavor component according to [1] or [2], wherein the pH of the alkaline-treated tobacco raw material is 9.5 or higher.
- the water treatment is performed [1]. ] To [3]. The method for extracting a flavor component.
- step A when the water content of the alkali-treated tobacco raw material or the processed tobacco leaf becomes 20% by weight or less for the first time with respect to the total weight of the tobacco raw material or the processed tobacco leaf.
- step B the temperature of the collecting solvent is 5 ° C. or higher and 35 ° C. or lower.
- a method for manufacturing a component of processed tobacco leaves is 5 ° C. or higher and 35 ° C. or lower.
- Step A of heating tobacco raw materials or processed tobacco leaves that have been treated with alkali using alkali In step B, the release component released into the gas phase in step A is brought into contact with the collection solvent to obtain a collection solution. A step C of adding the collected solution to the component is provided.
- the initial water content of the alkali-treated tobacco raw material or processed tobacco leaves is equal to or higher than the minimum water content capable of dissolving all of the alkali.
- the alkali-treated tobacco raw material or processed tobacco leaves being heated are hydrated and treated.
- a production method characterized in that the water 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.
- the time required to extract a certain amount of flavor components from tobacco raw materials or processed tobacco leaves can be shortened as compared with the conventional method, and the TSNA concentration in the collection solution in which the flavor components are collected can be reduced. It is possible to provide a method for extracting a flavor component that can be maintained at a lower level, and a method for producing a component of processed tobacco leaves.
- 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 application example of a flavor component.
- FIG. 4 is a flow chart showing an extraction method according to an embodiment of the present invention.
- FIG. 5 is a graph showing the transition of the recovery rate of the flavor component (here, nicotine) with respect to the heat treatment time of the tobacco raw material.
- FIG. 6 is a graph showing the transition of the recovery amount of TSNA with respect to the heat treatment time of the tobacco raw material.
- FIG. 7 is a graph showing the transition of the product temperature of the tobacco raw material with respect to the heat treatment time of the tobacco raw material.
- FIG. 8 is a graph showing the transition of the water content of the tobacco raw material with respect to the heat treatment time of the tobacco raw material.
- tobacco raw material refers to tobacco leaves that have not been harvested and subjected to aging treatment, or tobacco leaves that have undergone aging treatment, and have not been processed into various forms used in tobacco products. It is a general term for those of raw and dried leaves before being aged, and examples thereof include crushed products of these, ripened lamina and its crushed material, and aged middle bone and its crushed material. Further, in the present specification, “processed tobacco leaf” is a general term for processed tobacco raw materials into various forms used in tobacco products, and exemplifies tobacco chopping, tobacco sheets, tobacco granules, and the like. Can be done. 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 "component" of the processed tobacco leaf is a concept including the tobacco raw material and the other materials.
- the method for extracting the flavor component according to the embodiment of the present invention is a method for extracting the flavor component from the tobacco raw material or the processed tobacco leaf.
- the extraction method includes a step A of heating the tobacco raw material or processed tobacco leaves treated with alkali using alkali, and a step B of bringing the released component released into the gas phase in the step A into contact with a collecting solvent. , Equipped with.
- the initial water content of the alkali-treated tobacco raw material or the processed tobacco leaf is equal to or more than the minimum water content capable of dissolving all the alkali, and the alkali-treated tobacco raw material or the processed tobacco material being heated.
- the finished tobacco leaves are hydrated and the water content of the alkali-treated tobacco raw material 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 water content" of the alkaline-treated tobacco raw material or processed tobacco leaf is the water content of the alkaline-treated tobacco raw material or processed tobacco leaf after the alkaline treatment and before the heat treatment. It can be expressed by weight% with respect to the total weight of the tobacco raw material or the processed tobacco leaf.
- the total weight of the tobacco raw material or the processed tobacco leaf which is the basis for calculating the water content, means the dry weight of each. The same applies to the following.
- the initial water content of the alkali-treated tobacco raw material or processed tobacco leaf is the whole of the tobacco raw material or the processed tobacco leaf. It is 39% ⁇ 2% with respect to the weight.
- One of the reasons why the water content is initially set in this way in the conventional method for extracting flavor components is that after the tobacco raw material or processed tobacco leaves are charged into the extraction device and subjected to alkaline treatment, the heating operation is started. This is because the flavor component could be obtained at a desired recovery rate without performing any additional operation until the end.
- the time from the start to the end of the heating operation that is, the time required to obtain the flavor component with a desired recovery rate is about 180 minutes, and the processed tobacco is processed. It took a relatively long time in the process of manufacturing leaf components. Further, it has been generally known that the longer the time of heating at a high temperature, the greater the amount of TSNA released from the tobacco raw material or the processed tobacco leaves. Also in the extraction method, it has been reported that the longer the heat treatment time is obtained in order to obtain the flavor component having a desired recovery rate, the higher the recovery amount of TSNA is.
- the present inventor has studied in the method for extracting a flavor component to shorten the time required to obtain a flavor component having a desired recovery rate and suppress the recovery amount of TSNA.
- the above conditions that is, the step.
- the initial water content of the alkali-treated tobacco raw material or processed tobacco leaves is equal to or higher than the minimum water content capable of dissolving all of the alkali, and the alkali-treated tobacco raw material or processed tobacco being heated is used.
- the leaves are hydrated and the water content of the alkaline-treated tobacco raw material or processed tobacco leaves is 35% by weight or less based on the total weight of the tobacco raw materials or processed tobacco leaves. I found.
- the reason why the time required to obtain the flavor component with the desired recovery rate can be shortened is considered as follows.
- the alkali-treated tobacco raw material or processed tobacco leaf according to the embodiment of the present invention is initially set to have a lower water content than before, and even if water treatment is applied during the heat treatment, the above-mentioned
- the water content of the alkaline-treated tobacco raw material or the processed tobacco leaves is controlled to 35% by weight or less, which is lower than the initial water content in the conventional method. Therefore, the product temperature of the alkali-treated tobacco raw material or processed tobacco leaf rises rapidly, and the flavor component is released from the tobacco raw material or processed tobacco leaf at a timing earlier than that of the conventional method. ..
- the reason why the amount of TSNA recovered can be suppressed is considered as follows.
- the alkaline-treated tobacco raw material or processed tobacco leaves according to the embodiment of the present invention are subjected to water treatment during the heat treatment, so that the product temperature is temporarily lowered. As a result, it is possible to shorten the time for the product temperature of the tobacco raw material or the processed tobacco leaf to be in a high temperature state.
- the initial water content of the alkali-treated tobacco raw material or the processed tobacco leaf is preferably more than 20% by weight with respect to the total weight of the tobacco raw material or the processed tobacco leaf.
- the initial water content of the alkali-treated tobacco raw material or processed tobacco leaves is more preferably 25% by weight or more, further preferably 30% by weight or more. Further, the initial water content of the alkali-treated tobacco raw material or processed tobacco leaves is preferably 35% by weight or less.
- the initial water content of the alkali-treated tobacco raw material or processed tobacco leaf released from the tobacco raw material or processed tobacco leaf at an early timing is 20 weight with respect to the total weight of the tobacco raw material or processed tobacco leaf. When it is less than%, the alkali added to the tobacco raw material or the processed tobacco leaves may not be completely dissolved and may precipitate.
- the initial water content of the alkaline-treated tobacco raw material or the processed tobacco leaf can be adjusted by the concentration of the alkaline aqueous solution added to the tobacco raw material or the processed tobacco leaf in the alkaline treatment described later.
- the pH of the alkali-treated tobacco raw material or processed tobacco leaves is preferably 9.5 or higher.
- the flavor component can be efficiently released from the tobacco raw material or the processed tobacco leaf, and the recovery rate of the flavor component is increased.
- the pH is less than 9.5, the recovery rate of the flavor component from the tobacco raw material or the processed tobacco leaf may decrease.
- the upper limit of the pH of the alkali-treated tobacco raw material or the processed tobacco leaf is not particularly limited, but is usually 12 or less, preferably 11 or less, from the viewpoint of the treatment time required to raise the pH.
- the pH of the alkaline-treated tobacco raw material or the processed tobacco leaf can be adjusted by the type of alkali added to the tobacco raw material or the processed tobacco leaf in the alkaline treatment described later and the concentration of the alkaline aqueous solution.
- the alkali used for the alkali treatment is not particularly limited as long as the pH of the tobacco raw material or the processed tobacco leaves can be within the above numerical range, but is preferably a substance that can be used as a food additive, for example, carbonate. Potassium, sodium carbonate, or a mixture thereof can be preferably used. Potassium carbonate and sodium carbonate are preferable because they have good solubility in water and can easily adjust an alkaline aqueous solution for spraying on a tobacco raw material or processed tobacco leaves.
- the water treatment is preferably performed when the product temperature of the alkali-treated tobacco raw material or processed tobacco leaves reaches a temperature range of 100 ° C. or higher and 150 ° C. or lower.
- the temperature range is more preferably 100 ° C. or higher and 130 ° C. or lower, and further preferably 100 ° C. or higher and 110 ° C. or lower.
- the water content of the alkaline-treated tobacco raw material or the processed tobacco leaf is 20% by weight or less for the first time with respect to the total weight of the tobacco raw material or the processed tobacco leaf. It is preferable to apply it when it becomes.
- the water treatment at such a timing, it is possible to suppress the amount of TSNA released while maintaining the efficient release of the flavor component from the alkaline-treated tobacco raw material or the processed tobacco leaves. can.
- the temperature of the collecting solvent is preferably 5 ° C. or higher and 35 ° C. or lower, and more preferably 10 ° C. or higher and 20 ° C. or lower.
- the temperature of the collecting solvent is within such a temperature range, it is possible to prevent the collecting solvent from coagulating and to prevent the flavor component from volatilizing from the collecting solution, so that the flavor component can be efficiently produced. Can be recovered.
- the method for producing a component of a processed tobacco leaf according to an embodiment of the present invention is a method for extracting a flavor component from the tobacco raw material or the processed tobacco leaf, to which the method for extracting a flavor component is applied. It is a manufacturing method. That is, the method for producing the constituent elements of the processed tobacco leaf according to the embodiment of the present invention is the step A of heating the tobacco raw material or the processed tobacco leaf treated with alkali using an alkali, and the gas phase in the step A.
- the present invention comprises the step B of contacting the release component released therein with a collection solvent to obtain a collection solution, and the step C of adding the collection solution to the components of the processed tobacco leaf.
- the initial water content of the alkali-treated tobacco raw material or the processed tobacco leaf is equal to or more than the minimum water content capable of dissolving all the alkali, and the alkali-treated tobacco raw material or the processed tobacco material being heated.
- the finished tobacco leaves are hydrated and the water content of the alkali-treated tobacco raw material or processed tobacco leaves is 35% by weight or less based on the total weight of the tobacco raw materials or the processed tobacco leaves. Is.
- FIG. 1 and 2 are views showing an example of an extraction device according to an embodiment of the present invention.
- the alkali treatment device 10 has a container 11 and a sprayer 12.
- the container 11 stores the tobacco raw material (or processed tobacco leaf) 50.
- the container 11 is composed of, for example, a member having heat resistance and pressure resistance (for example, SUS; Steel Used Stainless).
- the container 11 preferably constitutes a closed space.
- the "closed space” is a state in which solid foreign matter is prevented from being mixed in during normal handling (transportation, storage, etc.). As a result, the volatilization of the flavor component contained in the tobacco raw material (or processed tobacco leaf) 50 to the outside of the container 11 is suppressed.
- the sprayer 12 performs alkaline treatment by applying the alkaline aqueous solution to the tobacco raw material (or processed tobacco leaf) 50.
- the initial content of the flavor component (here, the nicotine component) contained in the tobacco raw material (or processed tobacco leaf) 50 is 100% by weight of the total weight of the tobacco raw material (or processed tobacco leaf) 50 in a dry state. In some cases, it is preferably 2.0% by weight or more, and more preferably 4.0% by weight or more.
- Examples of the tobacco raw material (or processed tobacco leaf) 50 include unripened tobacco leaves of the genus Nicotiana such as Nicotiana tabacum and Nicotiana rustica, or aged tobacco leaves thereof. Aged tobacco leaves processed into various forms used in tobacco products can be used. As the Nicotiana tabacum, for example, varieties such as Burley and Yellow can be used. As the tobacco raw material (or processed tobacco leaf) 50, various types of unripened tobacco leaves other than Burley and yellow species, aged ones, and various aged tobacco leaves used in tobacco products. Those processed into a form may be used.
- the tobacco raw material (or processed tobacco leaf) 50 is preferably composed of a tobacco raw material or a processed tobacco leaf chop or a powder or granular material, and more preferably composed of a powder or granular material.
- the particle size of the chopped or powder or granular material is usually 0.5 mm or more and 10 mm or less, and preferably 0.5 mm or more and 5 mm or less. When the particle size is smaller than 0.5 mm, sticking to the wall surface of the container 11 often occurs, which is not preferable from the viewpoint of extraction efficiency.
- the particle size is 10 mm or less, the surface area of the chopped or powder or granular material is large, so that the extraction efficiency is good, and when the particle size is 5 mm or less, the surface area of the chopped or powder or granular material is larger, so that the extraction is performed. The efficiency becomes even better.
- “chopping” is obtained by finely chopping a tobacco raw material or processed tobacco leaves.
- the “granular material” is obtained by coarsely crushing a tobacco raw material or processed tobacco leaves.
- the collection device 20 includes a container 21, an introduction pipe 22, a discharge portion 23, and a take-out pipe 24.
- the container 21 contains the collecting solvent 70.
- the container 21 is made of, for example, glass.
- the container 21 preferably constitutes a closed space.
- the "closed space” is a state in which solid foreign matter is prevented from being mixed in during normal handling (transportation, storage, etc.).
- the collecting solvent 70 for example, glycerin, water or ethanol can be used. Among these collecting solvents 70, it is preferable to use water from the viewpoint of ease of handling and cost reduction.
- any acid such as malic acid or citric acid may be added to the collection solvent 70.
- a component or substance such as an aqueous citric acid solution may be added to the collection solvent 70. That is, the collecting solvent 70 may be composed of a plurality of types of components or substances.
- the initial pH of the collection 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 release 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.
- the release component 61 contains at least a nicotine component which is an index 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 release portion 23 has a plurality of openings 23A.
- the release component 61 guided by the introduction pipe 22 is released into the collection solvent 70 as a foamy release component 62 from the plurality of openings 23A.
- the lead-out pipe 24 guides the residual component 63 that was not captured by the collection solvent 70 to the outside of the container 21.
- 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 collecting solvent 70 may rise 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 have Raschig ring in order to increase the contact area of the release component 62 with respect to the collection solvent 70.
- FIG. 3 is a diagram for explaining an application example of a flavor component.
- the flavor component is applied to processed tobacco leaves and the like.
- the flavor suction tool 100 has a holder 110, a carbon heat source 120, a processed tobacco leaf 130, and a filter 140.
- the holder 110 is, for example, a paper tube having a cylindrical shape.
- the carbon heat source 120 generates heat for heating the processed tobacco leaves 130.
- the processed tobacco leaf 130 is a substance that generates a flavor, and is an example of a flavor source base material to which an alkaloid containing a nicotine component is added.
- the filter 140 suppresses the introduction of contaminants to the mouthpiece side.
- the flavor suction tool 100 has been described as an application example of the flavor component, but the embodiment is not limited to this.
- the flavor component may be applied to other flavor suction tools.
- the tobacco sheet filled in the tobacco rod can be mentioned, and as another example, the tobacco granules filled in the tobacco cartridge can be mentioned.
- the flavor component may be applied to, for example, an aerosol source (so-called E-ligid) of an electronic cigarette.
- the flavor component may be applied to a flavor source base material such as gum, tablets, films, and candy.
- FIG. 4 is a flow chart showing a method for extracting the flavor component.
- step S10 the alkali is applied to the tobacco raw material (or processed tobacco leaf) 50 by using the above-mentioned alkali treatment device 10.
- the alkali as described above, potassium carbonate, sodium carbonate, a mixture thereof and the like can be exemplified.
- the tobacco raw material (or processed tobacco leaf) 50 is treated with an alkaline solution by adding the alkaline aqueous solution.
- the initial content of the flavor component (here, the nicotine component) contained in the tobacco raw material (or processed tobacco leaf) 50 is 100% by weight of the total weight of the tobacco raw material (or processed tobacco leaf) 50 in a dry state. In some cases, it is preferably 2.0% by weight or more, and more preferably 4.0% by weight or more.
- the pH of the tobacco raw material (or processed tobacco leaf) 50 after the alkali treatment is preferably 9.5 or higher.
- the pH is 9.5 or higher, the flavor component can be efficiently released from the tobacco raw material (or processed tobacco leaf) 50, and the recovery rate of the flavor component is increased.
- the pH is less than 9.5, the recovery rate of the flavor component from the tobacco raw material (or processed tobacco leaf) 50 is lowered.
- the upper limit of the pH of the alkali-treated tobacco raw material (or processed tobacco leaf) 50 is not particularly limited, but as described above, it is usually 12 or less from the viewpoint of the treatment time required to raise the pH. , 11 or less is preferable.
- the water content of the tobacco raw material (or processed tobacco leaf) 50 after the alkali treatment is preferably more than 20% by weight, preferably 25% by weight or more, based on the total weight of the tobacco raw material or the processed tobacco leaf. More preferably, it is more preferably 30% by weight or more.
- the rate at which the product temperature of the alkali-treated tobacco raw material or the processed tobacco leaf to be heat-treated rises becomes faster, and the flavor component becomes higher than that of the conventional method. Is also released from the tobacco raw material or processed tobacco leaves at an early timing.
- the alkali added to the tobacco raw material is dissolved. It may not be cut and precipitate.
- the water content of the tobacco raw material (or processed tobacco leaf) 50 after the alkali treatment is the initial water content of the alkali-treated tobacco raw material (or processed tobacco leaf) 50 in the heat treatment of step 20S.
- step S20 the alkaline-treated tobacco raw material (or processed tobacco leaf) 50 is heated.
- the tobacco raw material (or processed tobacco leaf) 50 may be heated together with the container 11 in a state where the tobacco raw material (or processed tobacco leaf) 50 is contained in the container 11 of the alkali treatment device 10. can.
- the introduction pipe 22 of the collection device 20 is attached to the container 11.
- 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.
- the heating temperature of the tobacco raw material (or processed tobacco leaf) 50 is 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.
- the heating temperature of the tobacco raw material 50 is 150 ° C. or lower, the timing at which TSNA is released from the tobacco raw material (or processed tobacco leaf) 50 can be delayed.
- step S20 the tobacco raw material (or processed tobacco leaf) 50 being heat-treated is subjected to water treatment.
- the tobacco raw material (or processed tobacco leaf) 50 being heat-treated is subjected to the water treatment, the product temperature thereof is temporarily lowered, and the amount of TSNA recovered can be suppressed.
- the water content of the tobacco raw material (or processed tobacco leaf) 50 after the heat treatment is 35% by weight or less with respect to the total weight of the tobacco raw material. Therefore, the amount of water added is adjusted so that the water content of the tobacco raw material (or processed tobacco leaf) 50 is 35% by weight or less with respect to the total weight of the tobacco raw material or processed tobacco leaf.
- the number of times of water treatment on the tobacco raw material (or processed tobacco leaf) 50 during the heat treatment is not particularly limited as long as the above upper limit of the water content is not exceeded, and may be once or twice or more. Further, the tobacco raw material (or processed tobacco leaf) 50 may be continuously hydrotreated. The number of times of the water treatment is preferably one. The reason is that the less the number of water treatments is, the less labor is required. Further, since the temperature of the tobacco raw material or the processed tobacco leaf during the heat treatment is lowered every time the water treatment is performed, it is preferable that the number of water treatments is small from the viewpoint of the extraction efficiency of the flavor component.
- the timing of adding water to the tobacco raw material (or processed tobacco leaf) 50 being heat-treated is within the temperature range in which the product temperature of the tobacco raw material (or processed tobacco leaf) 50 is 100 ° C. or higher and 150 ° C. or lower. It is preferably when it is reached.
- the temperature range is more preferably 100 ° C. or higher and 130 ° C. or lower, and further preferably 100 ° C. or higher and 110 ° C. or lower.
- the timing of adding water to the tobacco raw material (or processed tobacco leaf) 50 being heat-treated is such that the water content of the alkali-treated tobacco raw material or processed tobacco leaf is the tobacco raw material or processed tobacco. It is preferable to apply it when it becomes 20% by weight or less with respect to the total weight of the leaves for the first time.
- the water treatment at such a timing, it is possible to suppress the amount of TSNA released while maintaining the efficient release of the flavor component from the alkaline-treated tobacco raw material or the processed tobacco leaves. can.
- step S20 it is preferable to perform aeration treatment on the tobacco raw material (or processed tobacco leaf) 50.
- the amount of the flavor component contained in the release component 61 released into the gas phase from the alkali-treated tobacco raw material (or processed tobacco leaf) 50 can be increased.
- saturated water vapor at 80 ° C. is brought into contact with the tobacco raw material (or processed tobacco leaf) 50.
- the aeration time in the aeration treatment cannot be unconditionally specified because it depends on the device for processing the tobacco raw material (or processed tobacco leaf) 50 and the amount of the tobacco raw material (or processed tobacco leaf) 50, but for example, tobacco.
- the aeration time is 90 minutes or less.
- the total aeration amount in the aeration treatment cannot be unequivocally specified because it depends on the device for processing the tobacco raw material (or processed tobacco leaf) 50 and the amount of the tobacco raw material (or processed tobacco leaf) 50, but for example.
- the tobacco raw material (or processed tobacco leaf) 50 is 500 g
- the total aeration amount is about 3 L / g.
- the aeration flow rate cannot be unconditionally specified because it depends on the apparatus for processing the tobacco raw material (or processed tobacco leaf) 50 and the amount of the tobacco raw material (or processed tobacco leaf) 50, but for example, aeration.
- the flow rate is about 15 L / min.
- the air used in the aeration treatment does not have to be saturated steam.
- the moisture content of the air used in the aeration treatment does not require humidification of the tobacco raw material (or processed tobacco leaf) 50, for example, the tobacco raw material (or processed tobacco leaf) to which the heat treatment and the aeration treatment are applied.
- the amount of water contained in 50 may be adjusted to be within the range of 35% by weight or less.
- the gas used in the aeration treatment is not limited to air, and may be an inert gas such as nitrogen or argon.
- step S30 the release component released into the gas phase in step S20 is brought into contact with the collection solvent 70 by using the collection device 20 described above.
- step S20 and step S30 are described as separate processes in FIG. 4, but it should be noted that step S20 and step S30 are processes performed in parallel. It should be noted that parallel means that the period in which step S30 is performed overlaps with the period in which step S20 is performed, and it is not necessary for steps S20 and S30 to start and end at the same time.
- the pressure in the container 11 of the alkali treatment device 10 is equal to or lower than the normal pressure.
- the upper limit of the pressure in the container 11 of the alkali treatment device 10 is +0.1 MPa or less in gauge pressure.
- the inside of the container 11 of the alkali treatment device 10 may have a reduced pressure atmosphere.
- the collecting solvent 70 for example, glycerin, water, or ethanol can be used, as described above.
- the temperature of the collecting solvent 70 is preferably 5 ° C. or higher and 35 ° C. or lower, and more preferably 10 ° C. or higher and 20 ° C. or lower.
- the temperature of the collecting solvent is within such a temperature range, it is possible to prevent the collecting solvent from coagulating and to prevent the flavor component from volatilizing from the collecting solution, so that the flavor component can be efficiently produced. Can be recovered.
- step S40 in order to increase the concentration of the flavor component contained in the collection solution, the collection solvent 70 (that is, the collection solution) that has captured the flavor component is subjected to a vacuum concentration treatment, a heat concentration treatment, or salting out. Processing is applied.
- the vacuum concentration treatment is performed in a closed space, there is little air contact, and the collection solvent 70 does not need to be heated to a high temperature, so there is little concern about component changes. Therefore, the use of vacuum concentration increases the types of collection solvents available.
- salting out treatment it is possible to increase the concentration of the flavor component as compared with the vacuum concentration treatment, but the yield of the flavor component is poor because the flavor component is separated into each of the liquid solvent phase and the aqueous phase. Further, since it is assumed that the coexistence of a hydrophobic substance (MCT or the like) is indispensable, salting out may not occur depending on the ratio of the collecting solvent, water and the flavor component.
- MCT hydrophobic substance
- step S50 the collection solution containing the flavor component is added to the constituent components of the processed tobacco leaves. That is, in step S50, the flavor component captured by the collection solvent 70 is supported on the flavor source base material (component of the processed tobacco leaf).
- a collection solvent that is, a collection solution
- a collection solvent that is, a collection solution
- components ammonium ions, TSNA, etc.
- the collection solution added to the extraction residue may be neutralized.
- the extraction residue containing the flavor component may be neutralized after the collection solution is added to the extraction residue.
- the amount of the flavor component (here, the nicotine component) contained in the tobacco raw material or the processed tobacco leaf after the collection solution is reapplied to the extraction residue is the tobacco raw material before the flavor component is released.
- the amount is less than or equal to the amount of flavor component (here, nicotine component) contained in the processed tobacco leaves.
- the tobacco raw material (or processed tobacco leaf) 50 (extraction residue) after releasing the flavor component in step S20 may be washed with a washing solvent before the above-mentioned reconstitution treatment is performed.
- a washing solvent an aqueous solvent can be mentioned, and specific examples thereof may be pure water or ultrapure water, and city water can be mentioned. As a result, substances that have an undesired effect on the flavor and the like remaining in the extraction residue are removed.
- components (ammonium ions, TSNA, etc.) that have an undesired effect on the flavor and the like can be further removed, and the tobacco raw material or processed tobacco material in which the loss of the fragrance component is suppressed can be further removed. Tobacco leaves can be produced.
- the pH of the alkaline-treated tobacco raw material or processed tobacco leaves can be measured with a pH meter (for example, IQ240 manufactured by IQ Scientific Instruments Inc.), for example, the alkaline-treated tobacco raw material or processed tobacco leaves 2 to. 10 times the weight of distilled water was added to 10 g, and the mixture of water and tobacco raw material or processed tobacco leaves was shaken at 200 rpm for 10 minutes and allowed to stand for 5 minutes at room temperature (for example, 22 ° C.), and then the obtained extraction was obtained. Measure the pH of the solution with a pH meter.
- a pH meter for example, IQ240 manufactured by IQ Scientific Instruments Inc.
- the collected solution is left in a closed container until it reaches room temperature in a laboratory controlled at room temperature of 22 ° C. to adjust the temperature.
- the lid is opened and the glass electrode of the pH meter (for example, METTLER TORDO Co., Ltd .: Seven Easy S20) is immersed in the collection solution to start the measurement.
- the pH meter is calibrated in advance with a pH meter calibration solution having a pH of 4.01, 6.87, or 9.21.
- the point at which the output fluctuation from the sensor stabilizes within 0.1 mV within 5 seconds is defined as the pH of the collected solution.
- the amount of nicotine contained in the tobacco raw material or the processed tobacco leaves is determined by a method according to the German standardization organization DIN 10373. That is, 250 mg of a tobacco raw material or a processed tobacco leaf is collected, 7.5 mL of an 11% sodium hydroxide aqueous solution and 10 mL of hexane are added, and the mixture is shaken and extracted 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 tobacco raw material or processed tobacco leaves.
- GC / MS gas chromatograph mass spectrometer
- asuring method of water content in tobacco raw material or processed tobacco leaves 250 mg of tobacco raw material or processed tobacco leaves are collected, 10 mL of ethanol is added, and shaking extraction is performed for 60 minutes. After extraction, the extract is filtered through a 0.45 ⁇ m 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.
- GC / TCD gas chromatograph
- the weight of the tobacco raw material or the processed tobacco leaf in the dry state is calculated by subtracting the above-mentioned water content from the total weight of the tobacco raw material or the processed tobacco leaf.
- the amount of nicotine contained in the collection solution is determined by a method according to the German standardization mechanism DIN 10373, similarly to the measurement of the amount of nicotine contained in the tobacco raw material or processed tobacco leaves described above. That is, 250 mg of the collected solution is collected, 7.5 mL of an 11% sodium hydroxide aqueous solution and 10 mL of hexane are added, and the mixture is shaken for 60 minutes for extraction. 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.
- GC / MS gas chromatograph mass spectrometer
- the recovery rate of nicotine can be expressed as a percentage of the amount of nicotine contained in the collection solution with respect to the content of nicotine contained in the tobacco raw material or processed tobacco leaves before alkali treatment and heat treatment.
- GC analysis conditions The conditions of the GC analysis used for measuring the nicotine component and the water content contained in the tobacco raw material or the processed tobacco leaves are as shown in the table below.
- Tobacco raw materials were prepared by coarsely crushing the aged Tobacco lamina of Burley seeds so that the particle size was 0.5 mm or more and 10 mm or less.
- the flavor component here, the nicotine component
- the weight of nicotine contained in the tobacco raw material was the total weight of the tobacco raw material. It was 2.0% by weight.
- Heat treatment and collection treatment By introducing jacket steam to the outer periphery of the container of the locking dryer, heat treatment of the alkali-treated tobacco raw material was started.
- the components released from the tobacco raw material by heating were collected in the collection solvent via the introduction pipe.
- the amount of nicotine and the amount of TSNA contained in the collection solvent (that is, the collection solution) in which the components released from the tobacco raw material were collected were measured at regular intervals by the methods described above.
- the time course of the nicotine recovery amount and the TSNA recovery amount calculated from the results are shown in FIGS. 5 and 6.
- the temperature was appropriately adjusted by adjusting the temperature and the inflow amount of the jacket steam so that the product temperature of the alkaline-treated tobacco raw material did not exceed 120 ° C.
- the product temperature of the alkaline-treated tobacco raw material was measured at regular time intervals using a thermocouple installed inside the container of the locking dryer. The measurement result is shown in FIG.
- the water content of the alkaline-treated tobacco raw material was measured at regular time intervals by the method described above. The measurement result is shown in FIG.
- the container of the locking dryer was rotated and rocked so that the alkali-treated tobacco raw material in the container was uniformly heated.
- a cooling operation was appropriately performed using a chiller in order to maintain the temperature of the collection solvent, that is, water, at 15 ° C ⁇ 5 ° C.
- the recovery rate of nicotine exceeds 60% when the treatment time has passed 90 minutes.
- the recovery rate of nicotine finally exceeds 60% when the treatment time has passed 160 minutes. Therefore, in the present invention, the flavor component is released from the tobacco raw material at an earlier timing than the conventional method.
- the integrated value of the TSNA recovery amount up to the treatment time of 90 minutes is 8735.09 ng
- the TSNA recovery amount up to the treatment time of 160 minutes is Since the integrated value is 36608.27 ng
- the recovery amount of TSNA can be further suppressed in the example in the treatment time for recovering the same degree of nicotine.
- the processing time exceeds 160 minutes
- the amount of TSNA recovered tends to increase further. Therefore, the amount of TSNA recovered can be suppressed by shortening the processing time.
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Abstract
Description
[1] たばこ原料又は加工済たばこ葉から香味成分を抽出する香味成分の抽出方法であって、
アルカリを用いてアルカリ処理されたたばこ原料又は加工済たばこ葉を加熱する工程Aと、
前記工程Aで気相中に放出される放出成分を捕集溶媒に接触させる工程Bと、を備え、
前記工程Aにおいて、
前記アルカリ処理されたたばこ原料又は加工済たばこ葉の当初水分量は、前記アルカリを全て溶解し得る最小の水分量以上であり、
加熱中の前記アルカリ処理されたたばこ原料又は加工済たばこ葉に加水処理が施され、
一貫して前記アルカリ処理されたたばこ原料又は加工済たばこ葉の水分量が、該たばこ原料又は該加工済たばこ葉の全重量に対して、35重量%以下であることを特徴とする、
香味成分の抽出方法。
[2] 前記工程Aにおいて、前記アルカリ処理されたたばこ原料又は加工済たばこ葉の当初水分量は、該たばこ原料又は該加工済たばこ葉の全重量に対して、20重量%超である、[1]に記載の香味成分の抽出方法。
[3] 前記アルカリ処理されたたばこ原料のpHが9.5以上である、[1]又は[2]に記載の香味成分の抽出方法。
[4] 前記工程Aにおいて、前記アルカリ処理されたたばこ原料又は加工済たばこ葉の品温が100℃以上、150℃以下の温度範囲に達した際に、前記加水処理が施される、[1]~[3]に記載の香味成分の抽出方法。
[5] 前記工程Aにおいて、前記アルカリ処理されたたばこ原料又は加工済たばこ葉の水分量が、該たばこ原料又は該加工済たばこ葉の全重量に対して、初めて20重量%以下となった際に、前記加水処理が施される、[1]~[4]に記載の香味成分の抽出方法。
[6] 前記アルカリが、炭酸カリウム又は炭酸ナトリウムである、[1]~[5]に記載の香味成分の抽出方法。
[7] 前記工程Bにおいて、前記捕集溶媒の温度が、5℃以上、35℃以下である、[1]~[6]に記載の香味成分の抽出方法。
[8] 加工済たばこ葉の構成要素の製造方法であって、
アルカリを用いてアルカリ処理されたたばこ原料又は加工済たばこ葉を加熱する工程Aと、
前記工程Aで気相中に放出される放出成分を捕集溶媒に接触させて、捕集溶液を得る工程Bと、
前記捕集溶液を前記構成要素に添加する工程Cと、を備え、
前記工程Aにおいて、
前記アルカリ処理されたたばこ原料又は加工済たばこ葉の当初水分量は、前記アルカリを全て溶解し得る最小の水分量以上であり、
加熱中の前記アルカリ処理されたたばこ原料又は加工済たばこ葉に加水処理が施され、
一貫して前記アルカリ処理されたたばこ原料又は加工済たばこ葉の水分量が、該たばこ原料又は該加工済たばこ葉の全重量に対して、35重量%以下であることを特徴とする製造方法。
本明細書において、「~」を用いてその前後に数値又は物性値を挟んで表現する場合、その前後の値を含むものとして用いることとする。また、図面は模式的なものであり、各寸法の比率などは現実のものとは異なることに留意すべきである。
また、本明細書において、「加工済たばこ葉」とは、前記たばこ原料をたばこ製品で利用される種々の形態に加工したものの総称であり、たばこ刻やたばこシート、たばこ顆粒などを例示することができる。このような加工済たばこ葉は、前記たばこ原料のみから構成されることもあり、また、前記たばこ原料及びその他の材料から構成されることもある。そのため、加工済たばこ葉の「構成要素」とは、前記たばこ原料及び前記その他の材料を含む概念である。
なお、前記アルカリ処理されたたばこ原料又は加工済たばこ葉の「当初水分量」とは、アルカリ処理された後、加熱処理される前の、アルカリ処理されたたばこ原料又は加工済たばこ葉の水分量であり、該たばこ原料又は該加工済たばこ葉の全重量に対する重量%により表すことができる。ここで、水分量の算出基準となるたばこ原料又は該加工済たばこ葉の全重量とは、それぞれの乾燥重量のことを意味する。以下でも同様である。
しかしながら、このような従来の香味成分の抽出方法では、前記加熱操作を始めてから終わるまでの時間、すなわち、所望の回収率の香味成分を得るまでに要する時間が180分程度であり、加工済たばこ葉の構成要素を製造する工程の中でも比較的長い時間を占めていた。
また、一般的に、高温で加熱される時間が長くなる程、たばこ原料又は加工済たばこ葉からのTSNAの放出量が増加することが知られていたが、上述したような従来の香味成分の抽出方法においても、所望の回収率の香味成分を得るために加熱処理の時間を長くする程、TSNAの回収量が上昇することが報告されていた。
前記工程Aを上記のような条件とすることで、従来の方法に比べて、所望の回収率の香味成分を得るまでに要する時間を短縮できるとともに、TSNAの回収量を抑制できる。
また、TSNAの回収量を抑制できる理由は、次のように考えられている。本発明の実施形態に係る前記アルカリ処理されたたばこ原料又は加工済たばこ葉は、加熱処理中に加水処理を受けることからその品温が一時的に下がる。その結果、前記たばこ原料又は加工済たばこ葉の品温が高温状態となる時間を短縮できるためである。
前記アルカリ処理されたたばこ原料又は加工済たばこ葉の当初水分量は、25重量%以上であることがより好ましく、30重量%以上であることがさらに好ましい。また、前記アルカリ処理されたたばこ原料又は加工済たばこ葉の当初水分量は、35重量%以下であることが好ましい。前記当初水分量がこのような数値範囲内にあることで、加熱処理される前記アルカリ処理されたたばこ原料又は加工済たばこ葉の品温が上昇する速度が速くなり、香味成分が従来の方法よりも早いタイミングで該たばこ原料又は加工済たばこ葉から放出される
前記アルカリ処理されたたばこ原料又は加工済たばこ葉の当初水分量が、たばこ原料又は加工済たばこ葉の全重量に対して、20重量%以下である場合、たばこ原料又は加工済たばこ葉に付与されたアルカリが溶解しきらず析出してしまうことがある。
前記アルカリ処理されたたばこ原料又は加工済たばこ葉の当初水分量は、後述するアルカリ処理においてたばこ原料又は加工済たばこ葉に添加する、アルカリ水溶液の濃度によって調整することができる。
前記アルカリ処理されたたばこ原料又は加工済たばこ葉のpHの上限は特に制限されないが、pHを上昇させるために要する処理時間の観点から、通常12以下であり、11以下であることが好ましい。
前記アルカリ処理されたたばこ原料又は加工済たばこ葉のpHは、後述するアルカリ処理においてたばこ原料又は加工済たばこ葉に添加する、アルカリの種類やアルカリ水溶液の濃度によって調整することができる。
前記加工済たばこ葉の構成要素の製造方法に、前記たばこ原料又は加工済たばこ葉から香味成分を抽出する香味成分の抽出方法を適用することにより、加工済たばこ葉の構成要素の製造時間を短縮できるとともに、前記構成要素に含まれ得るTSNA量を抑制できる。
以下において、本発明の実施形態に係る抽出装置について説明する。図1及び図2は、本発明の実施形態に係る抽出装置の一例を示す図である。
以下において、たばこ原料(又は加工済たばこ葉)50から抽出された香味成分の適用例について説明する。図3は、香味成分の適用例を説明するための図である。例えば、香味成分は、加工済たばこ葉等に付与される。
香味成分は、その他の香味吸引具に適用されてもよい。例えば、加工済たばこ葉が内側となるように巻紙で巻装されることで充填されるたばこロッドや、加工済たばこ葉が空気の流入口と流出口とを備える収容体の流路に充填されるたばこカートリッジを、電気ヒーター等の燃焼を用いない熱源を利用することで直接的に又は間接的に加熱することで香味を発生させる、いわゆる非燃焼加熱式たばこ製品のたばこ充填物に適用されてもよい。ここで、前記たばこ充填物の一例としては、前記たばこロッドに充填されているたばこシートを挙げることができ、他の例としては、前記たばこカートリッジに充填されているたばこ顆粒を挙げることができる。
その他にも、香味成分は、例えば、電子シガレットのエアロゾル源(いわゆるE-liguid)に適用されてもよい。また、香味成分は、ガム、タブレット、フィルム、飴等の香味源基材に付与されてもよい。
以下において、本発明の実施形態に係る香味成分の抽出方法について説明する。図4は、前記香味成分の抽出方法を示すフロー図である。
たばこ原料(又は加工済たばこ葉)50に含まれる香味成分(ここでは、ニコチン成分)の初期含有量は、乾燥状態において、たばこ原料(又は加工済たばこ葉)50の総重量が100重量%である場合に、2.0重量%以上であることが好ましく、4.0重量%以上であることがより好ましい。
なお、前記アルカリ処理後のたばこ原料(又は加工済たばこ葉)50の水分量は、ステップ20Sの加熱処理におけるアルカリ処理されたたばこ原料(又は加工済たばこ葉)50の当初水分量である。
加熱処理後のたばこ原料(又は加工済たばこ葉)50の水分量は、該たばこ原料の全重量に対して、35重量%以下である。そのため、加水量は、たばこ原料(又は加工済たばこ葉)50の水分量が、該たばこ原料又は加工済たばこ葉の全重量に対して、35重量%以下となるように調整される。
前記加水処理の回数は、1回であることが好ましい。その理由としては、加水処理の回数が極力少ないほど、作業の手間が少なく済むからである。また、加水処理を行う度に加熱処理中のたばこ原料又は加工済たばこ葉の温度が下がることから、香味成分の抽出効率の観点からも加水処理の回数が少ないことが好ましいためである。
また、加熱処理中のたばこ原料(又は加工済たばこ葉)50に対し、加水処理を施すタイミングは、前記アルカリ処理されたたばこ原料又は加工済たばこ葉の水分量が、該たばこ原料又は加工済たばこ葉の全重量に対して、初めて20重量%以下となった際に施されることが好ましい。前記加水処理がこのようなタイミングで施されることにより、前記アルカリ処理されたたばこ原料又は加工済たばこ葉からの香味成分の効率的な放出を維持しつつ、TSNAの放出量を抑制することができる。
本発明を上述した実施形態によって説明したが、この開示の一部をなす論述及び図面は、この発明を限定するものであると理解すべきではない。この開示から当業者には様々な代替実施形態、実施例及び運用技術が明らかとなろう。
(たばこ原料又は加工済たばこ葉のpHの測定方法)
アルカリ処理後のたばこ原料又は加工済たばこ葉のpHは、pHメーター(例えば、IQ Scientific InstrumentsInc.製のIQ240)で測定することができ、例えば、アルカリ処理後のたばこ原料又は加工済たばこ葉2~10gに重量比で10倍の蒸留水を加え、室温(例えば22℃)で水とたばこ原料又は加工済たばこ葉との混合物を200rpmで10分間振盪し5分間静置した後、得られた抽出液のpHをpHメーターで測定する。
捕集溶液を22℃の室温でコントロールされた実験室内で、室温になるまで密閉容器内で放置して温度調和する。調和後、ふたを開けて、pHメーター(例えば、METTLER TOLEDO社製:セブンイージーS20)のガラス電極を捕集溶液に浸して測定を開始する。pHメーターは、あらかじめpH4.01、6.87、9.21のpHメーター校正液にて校正する。センサーからの出力変動が5秒間で0.1mV以内に安定した点を、その捕集溶液のpHとする。
たばこ原料又は加工済たばこ葉に含まれるニコチン量は、ドイツ標準化機構DIN 10373に準ずる方法で行う。すなわち、たばこ原料又は加工済たばこ葉を250mg採取し、11%水酸化ナトリウム水溶液7.5mLとヘキサン10mLを加え、60分間振とう抽出する。抽出後、上澄みであるヘキサン相をガスクロマトグラフ質量分析計(GC/MS)に供し、たばこ原料又は加工済たばこ葉に含まれるニコチン重量を定量する。
たばこ原料又は加工済たばこ葉を250mg採取し、エタノール10mLを加え、60分間振とう抽出を行う。抽出後、抽出液を0.45μmのメンブレンフィルタでろ過し、熱伝導度検出器を備えたガスクロマトグラフ(GC/TCD)に供し、たばこ原料又は加工済たばこ葉に含まれる水分量を定量する。
捕集溶液に含まれるニコチン量は、上述したたばこ原料又は加工済たばこ葉に含まれるニコチン量の測定と同様にドイツ標準化機構DIN 10373に準ずる方法で行う。すなわち、捕集溶液を250mg採取し、11%水酸化ナトリウム水溶液7.5mLとヘキサン10mLを加え、60分間振とう抽出する。抽出後、上澄みであるヘキサン相をガスクロマトグラフ質量分析計(GC/MS)に供し、捕集溶液に含まれるニコチン重量を定量する。
捕集溶液を0.5mL採取し、0.1Mの酢酸アンモニウム水溶液9.5mLを添加することで希釈し、高速液体クロマトグラフ質量分析計(LC-MS/MS)にて分析し、捕集溶液に含まれるTSNA重量を定量する。
たばこ原料又は加工済たばこ葉に含まれるニコチン成分及び水分量の測定で用いるGC分析の条件は、以下の表に示す通りである。
(たばこ原料の準備)
熟成させたバーレー種のたばこラミナを、粒度が0.5mm以上、10mm以下となるように粗砕することで、たばこ原料を準備した。
得られたたばこ原料に含まれる香味成分(ここでは、ニコチン成分)の測定を、上述したドイツ標準化機構DIN 10373に準ずる方法で行ったところ、たばこ原料に含まれるニコチン重量は、たばこ原料の総重量に対して、2.0重量%であった。
得られたたばこ原料500gを、噴霧器を備える容器(容器回転揺動型粉体真空乾燥機ロッキングドライヤ、愛知電気株式会社製、容量10L)に投入した後、炭酸カリウム90gを水180gに溶解させて得た炭酸カリウム水溶液270gを、噴霧器を介して噴霧速度55g/minでたばこ原料に噴霧した。炭酸カリウム水溶液を噴霧する際に、容器を回転・揺動させることで炭酸カリウム水溶液をたばこ原料になじませた。アルカリ処理後のたばこ原料のpHの測定を上述した方法で行ったところ、該pHは、9.6であった。また、アルカリ処理後のたばこ原料の水分量の測定を上述した方法で行ったところ、該水分量は、該たばこ原料の総重量に対して、30重量%であった。
アルカリ処理されたたばこ原料が入った前記ロッキングドライヤの容器内を減圧することで真空状態とした後、前記ロッキングドライヤの容器内に圧縮空気(約20℃、約60%-RH)を導入した。さらに、前記ロッキングドライヤの容器と、捕集溶媒が入った容器とを導入パイプで連結し、前記圧縮空気を流速15L/minで流入させることで、前記ロッキングドライヤの容器から捕集溶媒が入った容器への空気流れを発現させた。前記捕集溶媒には水を用いた。
前記ロッキングドライヤの容器外周にジャケット蒸気を導入することで、アルカリ処理されたたばこ原料の加熱処理を開始した。加熱によりたばこ原料から放出された成分を、導入パイプを介して捕集溶媒に捕集した。
たばこ原料から放出された成分を捕集した捕集溶媒(すなわち、捕集溶液)に含まれるニコチン量とTSNA量を、一定時間毎に、それぞれ上述した方法で行った。その結果から算出したニコチン回収量及びTSNA回収量の経時変化を図5及び図6に示す。
また、前記ロッキングドライヤの容器内部に設置した熱電対により、アルカリ処理されたたばこ原料の品温を一定時間毎に測定した。この測定結果を図7に示す。
さらに、アルカリ処理されたたばこ原料の水分量を、上述した方法により、一定時間毎に測定した。この測定結果を図8に示す。
なお、上記加熱処理の間、前記ロッキングドライヤの容器を回転・揺動させることで、容器内のアルカリ処理されたたばこ原料が均一に加熱されるようにした
上記加熱処理中のアルカリ処理されたたばこ原料の品温が、初めて105℃となったときに、該たばこ原料に対する加水処理を行った。この加水処理は、前記ロッキングドライヤが備える噴霧器を介して、水220gを噴霧速度55g/minで噴霧することで行われた。
加水処理直前のアルカリ処理されたたばこ原料の水分量は、該たばこ原料の総重量に対して、20重量%であった。
また、加水処理直後の、アルカリ処理されたたばこ原料の水分量は、該たばこ原料の総重量に対して、35重量%であった。
なお、加水処理の間、前記ロッキングドライヤの容器を回転・揺動させることで、容器内のアルカリ処理されたたばこ原料が均一に加水されるようにした。
一方で、上述した準備及び処理の内、(アルカリ処理)において、「炭酸カリウム90gを水180gに溶解させて得た炭酸カリウム水溶液270gを、噴霧器を介して噴霧速度55g/minでたばこ原料に噴霧」する工程を、「炭酸カリウム90gを水400gに溶解させて得た炭酸カリウム水溶液490gを、噴霧器を介して噴霧速度55g/minでたばこ原料に噴霧」する工程に変更し、(加水処理)を行わなかった実験例を比較例とする。
また、比較例においては、処理時間が160分を過ぎると、TSNAの回収量がより増大する傾向にある。したがって、処理時間を短縮することでTSNAの回収量を抑制できる。
Claims (8)
- たばこ原料又は加工済たばこ葉から香味成分を抽出する香味成分の抽出方法であって、
アルカリを用いてアルカリ処理されたたばこ原料又は加工済たばこ葉を加熱する工程Aと、
前記工程Aで気相中に放出される放出成分を捕集溶媒に接触させる工程Bと、を備え、
前記工程Aにおいて、
前記アルカリ処理されたたばこ原料又は加工済たばこ葉の当初水分量は、前記アルカリを全て溶解し得る最小の水分量以上であり、
加熱中の前記アルカリ処理されたたばこ原料又は加工済たばこ葉に加水処理が施され、
一貫して前記アルカリ処理されたたばこ原料又は加工済たばこ葉の水分量が、該たばこ原料又は該加工済たばこ葉の全重量に対して、35重量%以下であることを特徴とする、
香味成分の抽出方法。 - 前記工程Aにおいて、前記アルカリ処理されたたばこ原料又は加工済たばこ葉の当初水分量は、該たばこ原料又は該加工済たばこ葉の全重量に対して、20重量%超である、請求項1に記載の香味成分の抽出方法。
- 前記アルカリ処理されたたばこ原料又は加工済たばこ葉のpHが9.5以上である、請求項1又は2に記載の香味成分の抽出方法。
- 前記工程Aにおいて、前記アルカリ処理されたたばこ原料又は加工済たばこ葉の品温が初めて100℃以上、150℃以下の温度範囲に達した際に、前記加水処理が施される、請求項1~3のいずれか1項に記載の香味成分の抽出方法。
- 前記工程Aにおいて、前記アルカリ処理されたたばこ原料又は加工済たばこ葉の水分量が、該たばこ原料又は該加工済たばこ葉の全重量に対して、初めて20重量%以下となった際に、前記加水処理が施される、請求項1~4のいずれか1項に記載の香味成分の抽出方法。
- 前記アルカリが、炭酸カリウム又は炭酸ナトリウムである、請求項1~5のいずれか1項に記載の香味成分の抽出方法。
- 前記工程Bにおいて、前記捕集溶媒の温度が、5℃以上、35℃以下である、請求項1~6のいずれか1項に記載の香味成分の抽出方法。
- 加工済たばこ葉の構成要素の製造方法であって、
アルカリを用いてアルカリ処理されたたばこ原料又は加工済たばこ葉を加熱する工程Aと、
前記工程Aで気相中に放出される放出成分を捕集溶媒に接触させて、捕集溶液を得る工程Bと、
前記捕集溶液を前記構成要素に添加する工程Cと、を備え、
前記工程Aにおいて、
前記アルカリ処理されたたばこ原料又は加工済たばこ葉の当初水分量は、前記アルカリを全て溶解し得る最小の水分量以上であり、
加熱中の前記アルカリ処理されたたばこ原料又は加工済たばこ葉に加水処理が施され、
一貫して前記アルカリ処理されたたばこ原料又は加工済たばこ葉の水分量が、該たばこ原料又は該加工済たばこ葉の全重量に対して、35重量%以下であることを特徴とする製造方法。
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JP2006180715A (ja) * | 2004-12-24 | 2006-07-13 | Japan Tobacco Inc | タバコ固有のニトロソアミンを低減するためのタバコ抽出液の処理方法、再生タバコ材の製造方法および再生タバコ材 |
JP2014501104A (ja) * | 2010-12-17 | 2014-01-20 | アール・ジエイ・レイノルズ・タバコ・カンパニー | タバコ由来シロップ組成物 |
WO2015129680A1 (ja) | 2014-02-26 | 2015-09-03 | 日本たばこ産業株式会社 | 香喫味成分の抽出方法及び嗜好品の構成要素の製造方法 |
WO2015129679A1 (ja) | 2014-02-26 | 2015-09-03 | 日本たばこ産業株式会社 | 香喫味成分の抽出方法及び嗜好品の構成要素の製造方法 |
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JP2006180715A (ja) * | 2004-12-24 | 2006-07-13 | Japan Tobacco Inc | タバコ固有のニトロソアミンを低減するためのタバコ抽出液の処理方法、再生タバコ材の製造方法および再生タバコ材 |
JP2014501104A (ja) * | 2010-12-17 | 2014-01-20 | アール・ジエイ・レイノルズ・タバコ・カンパニー | タバコ由来シロップ組成物 |
WO2015129680A1 (ja) | 2014-02-26 | 2015-09-03 | 日本たばこ産業株式会社 | 香喫味成分の抽出方法及び嗜好品の構成要素の製造方法 |
WO2015129679A1 (ja) | 2014-02-26 | 2015-09-03 | 日本たばこ産業株式会社 | 香喫味成分の抽出方法及び嗜好品の構成要素の製造方法 |
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