JPWO2018139068A1 - Tobacco raw material manufacturing method and tobacco raw material - Google Patents

Abstract

Tobacco raw materials containing a small amount of specific polycyclic aromatic hydrocarbons and low-molecular carboxylic acids and containing a large amount of specific flavor components and a method for producing the same are provided. A step of drying leaf tobacco before bone removal after harvesting until the water content becomes 10 to 25% by weight, and a step of smoke-treating the dried leaf tobacco before bone removal at 400 to 500 ° C. Then, following the step of smoke treatment, the solution is solved by a production method including a step of storing the smoked leaf tobacco before deboning under a semi-sealed condition.

Description

  The present invention relates to a method for producing a tobacco raw material and a tobacco raw material.

Attempts have been made to improve the flavor of raw tobacco leaves. For example, in Non-Patent Document 1, a cigarette chopstick or wood smoke is passed through to give a unique scent, and at that time, the rice husk is slowly heated, burned slowly and scalded, and smoked. Are listed.
Further, DFC (Dark Fire Cured) is known as a tobacco material that has undergone smoke treatment. The general manufacturing method includes a step of performing smoke treatment with smoke generated by burning wood or the like at a heating / combustion temperature of about 600 to 900 ° C., and then, on a fresh tobacco leaf that has not undergone a drying treatment, It is known to include a fermentation process and a process of storing it through a aging process.
DFC is used as a raw material for snuff, pipes, chewing tobacco, and the like.
Patent Document 1 describes a tobacco product using an extract of fire-cured tobacco, and the content of benzo [a] pyrene contained in normal fire-dried tobacco is described in the document, It is described to be about 150 to about 800 ng / g.
On the other hand, in Patent Document 2, an alcohol such as ethyl alcohol is added to smoked dried leaf tobacco, and thereafter, the organic acid added by smoked processing is stored by storing the alcohol-added leaf tobacco. It is described that an esterification reaction is caused with an alcohol added in step 1 to form an ester compound.

Special table 2013-542744 gazette International Publication No. 2014/203341

Tobacco Research Center, Cigarette Encyclopedia, Japan, Yamaai Shoin, March 31, 2009, first edition, page 327

Non-Patent Document 1 only describes a normal smoking means as a method for imparting a unique scent to a tobacco raw material such as cigarette chopping.
In addition, in the invention described in Patent Document 2, smoked processing is performed on dry leaf tobacco by providing the organic acid contained in the smoke to dry leaf tobacco, thereby providing the substrate in the subsequent esterification reaction to dry leaf tobacco. Therefore, the object of the invention is to increase the ester compound in the tobacco raw material.
On the other hand, in the present invention, the adhesion of benzo [a] pyrene to leaf tobacco, which may occur when performing a conventional smoke treatment that has been conventionally performed, is suppressed, the content of low-molecular carboxylic acid is reduced, It is an object to provide a tobacco raw material with a specific flavor component increased and a method for producing the same.

  As a result of intensive studies by the present inventors, the leaf tobacco before harvesting after harvesting is dried until the water content becomes 10 to 25% by weight, and the dried leaf tobacco before bone removal is subjected to a product temperature of 400 to 400%. A step of smoking treatment with smoke obtained by thermally decomposing a smoke generating material in a range of 500 ° C., and a step of storing the smoked and processed leaf tobacco under semi-sealed conditions following the step of smoking. The present invention has been found to provide a tobacco raw material that contains a small amount of benzo [a] pyrene and low-molecular carboxylic acid and contains a lot of specific flavor components.

That is, the embodiment of the present invention is as follows.
[1] A step of drying leaf tobacco before bone removal after harvesting until the water content becomes 10 to 25% by weight, and a dried leaf tobacco before bone removal in a range where the product temperature is 400 to 500 ° C. A process for smoking a smoke-producing material with pyrolyzed smoke, and a process for storing the smoked smoking-treated leaf tobacco under a semi-sealed condition following the smoking process. Production method.
[2] The method for producing a tobacco raw material according to [1], wherein when the leaf tobacco after harvesting is dried, the leaf tobacco is dried until the water content becomes 15 to 25% by weight.
[3] The method for producing a tobacco raw material according to [1] or [2], wherein the storing step is performed at room temperature, and the period is 3 months or more and less than 24 months.
[4] The method for producing a tobacco raw material according to any one of [1] to [3], wherein the tobacco raw material obtained by the production method has the following configuration.
(1) The content of benzo [a] pyrene is 100 ng / g or less based on the dry weight of the tobacco material (2) The content of acetic acid is 20 mg / g or less based on the dry weight of the tobacco material (3 ) The content of guaiacol is 5 to 5000 μg / g based on the dry weight of the tobacco raw material (4) The content of 2,6-dimethoxyphenol is 10 to 10,000 μg / g based on the dry weight of the tobacco raw material [ 5] The tobacco raw material which is comprised from the leaf tobacco which has the structure of the following (1)-(4) and into which the lamina and the inside bone are not separation-processed.
(1) The content of benzo [a] pyrene is 100 ng / g or less based on the dry weight of the tobacco material (2) The content of acetic acid is 20 mg / g or less based on the dry weight of the tobacco material (3 ) The content of guaiacol is 5 to 5000 μg / g based on the dry weight of the tobacco raw material (4) The content of 2,6-dimethoxyphenol is 10 to 10,000 μg / g based on the dry weight of the tobacco raw material [ 6] A tobacco product comprising the tobacco raw material described in [5].
[7] The tobacco product according to [6], which is a cigarette or a heated flavor inhaler.

  ADVANTAGE OF THE INVENTION According to this invention, the tobacco raw material with little content of a benzo [a] pyrene and low molecular carboxylic acid and many specific flavor components and its manufacturing method are provided.

It is the schematic which shows the general manufacturing process of a tobacco product. It is a figure which shows the relationship between the product temperature of a smoke generation material, and content of the benzo [a] pyrene contained in the leaf tobacco after a smoked process. It is a figure which shows the relationship between the product temperature of a smoke generation material, and content of the guaiacol contained in the leaf tobacco after a smoked process. It is a figure which shows the relationship between the product temperature of a soot production | generation material, and content of 2, 6- dimethoxyphenol contained in the leaf tobacco after smoked processing. It is the schematic of the apparatus used in order to measure the adhesion efficiency to the leaf tobacco of a specific flavor component. It is a figure which shows the relationship between the moisture content of the leaf tobacco before smoked processing, and the adhesion efficiency of a guaiacol. It is a figure which shows the relationship between the moisture content of the leaf tobacco before smoked processing, and the adhesion efficiency of 2, 6- dimethoxyphenol. It is a figure which shows a time-dependent change of content of propionic acid in the leaf tobacco in the storage under a semi-sealed condition or a sealed condition. It is a figure which shows the time-dependent change of content of the acetic acid in the leaf tobacco in the storage under a semi-sealed condition or a sealed condition. It is a figure which shows a time-dependent change of content of propionic acid in the leaf tobacco during storage in a semi-sealed condition (acceleration test). It is a figure which shows the time-dependent change of content of the acetic acid in the leaf tobacco during storage in a semi-sealed condition (acceleration test).

  Hereinafter, the present invention will be described in detail with reference to embodiments, examples, etc., but the present invention is not limited to the following embodiments, examples, etc. Can be changed and implemented.

FIG. 1 shows a normal manufacturing process of a smoking article such as a cigarette.
In this manufacturing process, the harvested tobacco is stored in a warehouse through a process called curing.
This curing is a process performed at an early stage on harvested leaf tobacco, and usually includes processes such as drying and humidity conditioning, and may activate the functions of various enzymes contained in leaf tobacco. is there.
Curing is performed mainly for the following purposes.
(1) Enhancing the action of the enzyme and promoting the change in leaf color. (2) Dry the mesophyll and fix the leaf color. (3) Drain the water from the middle bone and dry the entire leaf.
After this curing, leaf tobacco is transported to a raw material factory after being stored in a warehouse for a certain period. In addition, when curing is performed, the deboning or separation operation of the leaf tobacco is not performed, and the processing such as the deboning is performed in the raw material factory.

The production method according to the embodiment of the present invention is performed in place of the above-described curing process, and the tobacco raw material obtained through the production method according to the embodiment of the present invention is usually stored in a warehouse. After that, it is transported to the raw material factory.
On the other hand, the manufacturing method described in Patent Document 2 is performed on a tobacco raw material that has been processed in the raw material factory shown in FIG. This is because when the tobacco raw material obtained by the production method described in Patent Document 2 is subjected to a treatment usually performed in the raw material factory shown in FIG. 1, the ester compound contained in the tobacco raw material is heated by re-drying or the like. It is because it will volatilize by performing the process accompanied by. This is supported by the fact that the leaf tobacco processed by the manufacturing method described in Patent Document 2 is a “cigarette cut” that is assumed to have been processed at the raw material factory in FIG.
From this, the manufacturing method described in Patent Document 2 and the manufacturing method according to the embodiment of the present invention are completely different from each other.
In the present specification, “leaf tobacco” refers to the one before or during the processing of the steps included in the production method of the present invention, and “tobacco raw material” is processed. Point to.

<Drying process of leaf tobacco before harvesting after harvesting>
The leaf tobacco before harvesting, which is used for the tobacco raw material according to the embodiment of the present invention, is the one before discoloration such as yellowing after “harvest” shown in FIG. 1, and Leaf tobacco before the “curing” process is performed, and is before deboning.
The leaf tobacco used in the production method according to the embodiment of the present invention and the tobacco raw material described below is not particularly limited, and belongs to the genus Nicotiana, Nicotiana tabacum Burley species, yellow species, Orient species, native species, Nicotiana rustica Can be mentioned.
As for leaf tobacco after harvesting, it is particularly preferable to use the leaf tobacco immediately after harvesting, and it is preferable to perform the drying treatment described later on such leaf tobacco immediately after harvesting.
The water content of leaf tobacco (raw leaves) after harvesting is usually high and has a water content of 80 to 90% by weight with respect to the total amount of leaf tobacco.
Such leaf tobacco is dried until the water content becomes 10 to 25% by weight.
The lower limit of the water content of the leaf tobacco obtained through the drying treatment is more preferably 12% by weight, and particularly preferably 15% by weight. When the range of the water content of the leaf tobacco is 15 to 25% by weight, the effect of increasing the content (attachment amount) of the specific flavor component imparted by soot is particularly excellent. Moreover, 20 weight% can also be mentioned as an upper limit of the moisture content of leaf tobacco.
Specific flavor components include guaiacol and 2,6-dimethoxyphenol.

In addition, about the moisture content in leaf tobacco, it calculates | requires with the following method.
In accordance with a method for analyzing moisture in food (heat drying method), the sample is heated at 100 ° C. for 1 hour under normal pressure, allowed to cool in a desiccator for 40 minutes, and moisture is determined from the weight difference before and after heating. The specific procedure is as follows.
(1) Measure the empty weight of the sample container stored in the desiccator.
(2) Weigh the required amount of tobacco and place it in the sample container and cover it.
(3) Open the lid of the sample container, arrange in a rotary dryer, and heat at 100 ° C. for 1 hour.
(4) After 1 hour, the lid of the sample container is closed and taken out and allowed to cool in a desiccator.
(5) After 40 minutes, the weight of the sample container is measured. The moisture is obtained from the following formula.

Mw: Moisture (%)
W1: Sample before drying and sample container weight (g)
W2: Sample after drying and sample container weight (g)
W0: Sample container weight (g)

The method for the drying treatment is not particularly limited, and examples thereof include the following methods.
Leave the cigarettes in a dry room where air is convection naturally and there is no gap in the air so that drying unevenness does not occur. Although it depends on the degree of production at about 0 ° C., a method of natural drying at about 25 to 35 ° C. is preferable.
Another example is a method of drying for about 5 days at a temperature of about 30 to 70 ° C. and a relative humidity of about 20 to 100% in an apparatus such as a circulating bulk dryer capable of controlling temperature and humidity.
Moreover, you may use both said methods together.
As another method, a method of drying for several hours by an apparatus having a drying temperature in the apparatus cabinet of about 100 ° C. can be mentioned.

<Smoked process>
In the step of smoking the tobacco, the smoke generating material is heated so that the smoke producing material such as wood has a temperature of 400 to 500 ° C. in order to generate smoke.
Unlike the DFC manufacturing method described above, a specific polycyclic aromatic compound with a large amount of adhering to leaf tobacco in DFC by heating in a range where the product temperature of the smoke generating material is 400 to 500 ° C. The adhesion amount of hydrocarbons such as benzo [a] pyrene can be reduced. On the other hand, by heating the smoke generating material so as to have a product temperature of 400 ° C. or higher, decomposition of a substance such as lignin contained in the smoke generating material is promoted, and a specific flavor component, specifically A sufficient amount of guaiacol and 2,6-dimethoxyphenol can be attached to leaf tobacco.
Wood can be used as the soot generation material, and the type thereof is not particularly limited, and examples thereof include white oak, cherry blossom, walnut, apple, beach beech, oak and hickory.
The time for the smoke treatment can be appropriately adjusted, for example, between about 10 minutes and 6 months.
Any of the smoking processes can be performed using a known smoking apparatus or a heating device. In the smoke treatment, there can be exemplified an aspect in which leaf tobacco is stacked and an aspect in which leaf tobacco is continuously dried or trunk-dried.

In the production method according to the embodiment of the present invention, after the above smoke treatment step, until the storing step described below, in order to modify the properties of the substance provided by the leaf tobacco or smoke treatment, There is no need to perform any treatment or addition of any substance, and such treatment or addition of substances is usually not performed.
For example, the DFC manufacturing method described above includes a fermentation process and an aging process before the storing process after the smoke treatment, but in the present invention, such a fermentation process and an aging process are included. Not included.
Moreover, the manufacturing method of this invention does not include the process of adding alcohol in order to produce | generate an ester compound at a later process as described in patent document 2, for example.
Therefore, in the manufacturing method according to the embodiment of the present invention, after the smoke processing process of leaf tobacco, the storing process described below is included following the smoke processing process.

<Process to store>
The step of storing the smoked and processed bone tobacco before deboning is performed under semi-sealed conditions so that low molecular carboxylic acids such as acetic acid are volatilized during storage.
Semi-sealed conditions include, for example, a mode in which smoked leaf tobacco is placed in an air permeable packaging material such as a plastic bag and the inlet of the packaging material is folded to prevent air inflow and out to some extent. it can.
When storing leaf tobacco under semi-sealed conditions, put smoked leaf tobacco into the packaging material as above and fold the entrance to make a packaging material with semi-sealed leaf tobacco. The aspect which puts a packaging material in storage containers, such as corrugated cardboard, can be mentioned.
During storage, a large number of leaf tobaccos may be stored at a time by preparing a plurality of packaging materials containing leaf tobacco and stacking and storing them in a storage container.
In the present invention, since the low molecular carboxylic acid such as acetic acid that can cause irritation is volatilized during storage by performing the storing step under semi-sealed conditions, the low molecular carboxylic acid in the obtained tobacco raw material The content can be reduced.
The storage period is not particularly limited as long as the low molecular carboxylic acid such as acetic acid is sufficiently reduced, but is preferably 3 months or more. On the other hand, the upper limit of the storage period is preferably about 24 months in consideration of the period until the produced tobacco raw material is shipped to the raw material factory.
The temperature at the time of storage is preferably a temperature at which volatilization of the low-molecular carboxylic acid occurs sufficiently.
Specific temperature can include room temperature. As a specific temperature range, a range of 5 to 60 ° C. can be exemplified, and an embodiment of appropriately setting in a range of 10 to 55 ° C. can also be exemplified.

In the production method of the present invention, additives such as essential oils and extract fragrances can be added in any amount in any step except between the step of smoke treatment and the step of storing.
Moreover, you may include the process of adjusting the water | moisture content of the obtained tobacco raw material after the process of storing. By passing through such a process, the moisture content of the tobacco material can be adjusted to 10 to 20% by weight, preferably 10 to 15% by weight, based on the total amount of the tobacco material.
As described above, the manufacturing method according to the embodiment of the present invention is performed before the processing at the tobacco raw material factory shown in FIG. And the tobacco raw material obtained with the manufacturing method of this invention is normally transported to a tobacco raw material factory through storage in a warehouse (refer FIG. 1). The storage in the warehouse at that time is usually about 10 to 180 days.
According to the method for producing a tobacco raw material described above, a tobacco raw material having the same component content as the <tobacco raw material> described below can be obtained.

<Tobacco ingredients>
The tobacco raw material concerning embodiment of this invention can be manufactured by the manufacturing method of the tobacco raw material of this invention demonstrated above, for example.
About the leaf tobacco which comprises the tobacco raw material concerning embodiment of this invention, it is a thing before performing the deboning in the raw material factory shown in FIG. 1, and the lamina and the middle bone are not separation-processed (it is not stressed) ) Consists of leaf tobacco.
Moreover, about the kind of leaf tobacco which comprises the tobacco raw material concerning embodiment of this invention, it may be the same kind as what is used with said manufacturing method.
The tobacco raw material concerning embodiment of this invention has the structure of the following (1)-(4).
(1) The content of benzo [a] pyrene is 100 ng / g or less based on the dry weight of the tobacco raw material.
(2) The acetic acid content is 20 mg / g or less based on the dry weight of the tobacco raw material.
(3) The content of guaiacol is 5 to 5000 μg / g based on the dry weight of the tobacco raw material.
(4) The content of 2,6-dimethoxyphenol is 10 to 10,000 μg / g based on the dry weight of the tobacco raw material.

Further, in the tobacco raw material according to the embodiment of the present invention, the content of benzo [a] pyrene is more preferably 50 ng / g or less on a dry weight basis, and particularly preferably the detection limit or less. When the content of benzo [a] pyrene is within such a range, the added amount of harmful substances contained in the smoke is small.
The content of benzo [a] pyrene in the tobacco raw material according to the embodiment of the present invention adjusts the product temperature of the smoke generating material when performing the smoke treatment when producing the tobacco raw material by the above-described manufacturing method. You can adjust it. For example, when wood is used as the smoke generating material to be subjected to the smoke treatment described above, the content of the specific polycyclic aromatic hydrocarbon is adjusted to the above range by adjusting the product temperature to be in the range of 400 to 500 ° C. Can fit inside.

Furthermore, in the tobacco raw material according to the embodiment of the present invention, the content of acetic acid is preferably 20 mg / g or less, particularly preferably 15 mg / g or less, on a dry weight basis.
When the content of acetic acid is in such a range, the tobacco material is less irritating to the user. On the other hand, the tobacco raw material of the present invention may contain 10 μg / g or more of acetic acid.
Further, in the tobacco raw material according to the embodiment of the present invention, the content of propionic acid is preferably 1 mg / g or less, particularly preferably 0.5 mg / g or less, on a dry weight basis. On the other hand, the tobacco raw material of the present invention can include an embodiment in which 10 μg / g or more of propionic acid is contained.

  The content of acetic acid and propionic acid in the tobacco raw material according to the embodiment of the present invention can be adjusted by adjusting the temperature and time of storage when the tobacco raw material is produced by the above-described production method. For example, if the storage time is lengthened, the amount of the low molecular carboxylic acid to be volatilized increases, so that the content of the low molecular carboxylic acid in the tobacco raw material can be further reduced.

  Although the tobacco raw material concerning embodiment of this invention can be manufactured by the manufacturing method concerning embodiment of this invention demonstrated above, in the manufacturing method concerning embodiment of this invention, it describes in patent document 2 It does not include a step of adding an alcohol for producing an ester compound. Therefore, the tobacco raw material according to the embodiment of the present invention does not substantially contain the ester compound described in Patent Document 2, such as ethyl acetate and ethyl valerate. “Substantially free” means below the detection limit.

Moreover, in the tobacco raw material concerning embodiment of this invention, it is more preferable that content of a guaiacol is 5-5000 microgram / g on a dry weight basis, and it is especially preferable that it is 100-1500 microgram / g.
Furthermore, in the tobacco raw material according to the embodiment of the present invention, the content of 2,6-dimethoxyphenol is more preferably 10 to 10,000 μg / g, and particularly preferably 500 to 2000 μg / g, based on the dry weight. .
Guaiacol and 2,6-dimethoxyphenol are components unique to soot and give the user a smoky, scent, taste, and savory taste that impacts the perception from the oral cavity to the nasal cavity It is an ingredient.
The content of guaiacol and 2,6-dimethoxyphenol in the tobacco raw material according to the embodiment of the present invention can be adjusted by adjusting the time required for the smoke treatment when producing the tobacco raw material by the above-described manufacturing method. For example, when it is desired to add more of these components, the time for the smoke treatment is increased.

In the tobacco raw material according to the embodiment of the present invention, the content ratio of 2,6-dimethoxyphenol and guaiacol (hereinafter also referred to as 2,6-DMP / G ratio) is preferably 1-20. 2 to 15 is more preferable, and 2 to 10 is particularly preferable.
When the 2,6-DMP / G ratio is in the above range, it is possible to give the user with a good balance of the smokyness, the scent and taste peculiar to the tobacco material, and the perception from the oral cavity to the nasal cavity.
This 2,6-DMP / G ratio can be adjusted, for example, by changing (smoked conditions (wood chip type, thermal decomposition temperature, etc.) and storage conditions (temperature, degree of contact with air, period, etc.). it can.
For example, when the product temperature of the smoke generating material in the process of smoking is increased, the temperature is lowered, and when the temperature is increased among the storage conditions, the 2,6-DMP / G ratio is increased. As for the storage conditions, the 2,6-DMP / G ratio increases when the degree of contact with air is increased. Moreover, when the storage period is lengthened, the 2,6-DMP / G ratio is increased.
In the conventional DFC, since the drying process is not performed before the smoking process, the water content of the leaf tobacco is considerably higher than that of the leaf tobacco of the present invention, and the amount of 2,6-dimethoxyphenol attached to the leaf tobacco is reduced. Moreover, in the conventional DFC, the product temperature of the smoke generating material during the smoke treatment is higher than that of the present invention, and this tends to reduce 2,6-DMP / G. Therefore, in the conventional DFC, the 2,6-DMP / G ratio is estimated to be smaller than 1, which is the lower limit value of the above range.

In the tobacco raw material according to the embodiment of the present invention, the content ratio of 2,6-dimethoxyphenol to phenol (also referred to as 2,6-DMP / P ratio) is preferably 1 to 100, More preferably, it is 70, and it is especially preferable that it is 20-50.
When the 2,6-DMP / P ratio is in such a range, the smoky feeling is more emphasized.
For example, the 2,6-DMP / P ratio decreases as the product temperature of the smoke generating material in the process of smoking is increased, and decreases as the storage period is extended among the storage conditions. Moreover, if the temperature at the time of storage is made high, it will become low.
In the conventional DFC, since the drying process is not performed before the smoking process, the water content of the leaf tobacco is considerably higher than that of the leaf tobacco of the present invention, and the amount of 2,6-dimethoxyphenol attached to the leaf tobacco is reduced. Therefore, in the conventional DFC, the 2,6-DMP / P ratio is estimated to be smaller than 1, which is the lower limit value of the above range.

Furthermore, in the tobacco raw material according to the embodiment of the present invention, the ratio of the content of guaiacol and phenol (also referred to as G / P ratio) is preferably 0.5 to 12.0, and preferably 0.5 to 6.0. Is more preferable, and 2.0 to 5.0 is particularly preferable.
When the G / P ratio is in such a range, a smoky feeling is emphasized.
For example, the G / P ratio decreases as the product temperature of the smoke generating material in the process of smoking is increased, and the G / P ratio decreases as the temperature increases in the storage conditions.

  The moisture content in the tobacco raw material concerning embodiment of this invention can mention the aspect which is 10-20 weight%, and it is preferable that it is 10-15 weight%.

The content of polycyclic aromatic hydrocarbons (benzo [a] pyrene) in tobacco raw materials can be determined by the following method.
Accurately weigh 0.5 g of dried tobacco into a glass screw vial (20 ml capacity), add 200 μl of internal standard substance (deuterium of each polycyclic aromatic hydrocarbon), and add 10 ml of cyclohexane as an extraction solvent. Cover and extract with shaking at 190 rpm for 30 minutes at room temperature. The supernatant is filtered through a 0.45 μm membrane filter, concentrated to 1 ml, purified and concentrated with an SPE solid phase extraction column (SPE: Si 2 g / 12 cc, Na ₂ SO ₄ ), and dispensed into a GC vial. The sample is analyzed by GCMS with an autosampler, and the amount of each target component in the sample is quantified by an internal standard method.
The following conditions can be used for GC / MS conditions.
<GC / MS analysis conditions>
Apparatus: Gas chromatograph analyzer (5975N) manufactured by Agilent
Inlet conditions: inlet temperature -300 ° C, injection method-pulsed splitless, injection volume-1 μL
Analytical column: DB-17ms 30 m × 0.25 mm × 0.25 μm manufactured by Agilent
Column flow rate: 1.2 mL / min. (He)
Temperature rising conditions: 60 ° C. (1 min.) − 15 ° C./min.−150° C. (0.5 min.) − 5 ° C./min. -320 ° C (18.5 min.) Run time (60 min.)
MS conditions: ion source -300 ° C, quadrupole -180 ° C, SIM mode

The content of low-molecular carboxylic acids such as acetic acid in tobacco raw materials and the content of flavor components (guaiacol, 2,6-dimethoxyphenol, phenol) in tobacco raw materials can be determined by the following methods.
Accurately weigh 0.5 g of the dried and ground tobacco material into a glass screw vial (20 ml capacity), and add 0.05 μg of quinoline as an internal standard substance. Add 10 ml of methanol as an extraction solvent, cap and extract with shaking at 200 rpm for 60 minutes at room temperature. The supernatant is filtered through a 0.45 μm membrane filter, transferred to a GC vial, and analyzed by GC / MS with an autosampler. The ratio of the analysis target component of the obtained GC chromatogram and the peak area of quinoline is obtained, and the amount of the analysis target component contained in each sample is quantified.
The following conditions can be used for GC / MS conditions.
Apparatus: Gas chromatograph analyzer manufactured by Agilent (6890N), mass detector manufactured by Agilent (5973N)
Injection volume: 1 μl (injected in pulsed splitless mode)
Column: HP-INNOWAX (30 m × 0.25 mm (film thickness 0.25 μm)) manufactured by Agilent
Oven: 40 ° C. → 260 ° C. (5 ° C./min)
Mass detector: TIC mode (mass number 29-550)

<Tobacco products>
The tobacco raw material according to the embodiment of the present invention is the one before the bone removal, and the lamina and the middle bone remain as they are.
Therefore, when the tobacco raw material according to the embodiment of the present invention is used for the manufacture of the tobacco product exemplified below, the raw material factory shown in FIG. Available. That is, the manufacturing method of said tobacco raw material can mention the aspect which includes the process of deboning and isolation | separation after the process of storing the leaf tobacco before smoke removal processed under semi-sealing conditions.
The raw material shipped from the raw material factory shown in FIG. 1 may be mixed with an ordinary tobacco raw material, for example, at an arbitrary ratio in the manufacturing factory, and a cigarette may be produced using the mixed raw material.
Moreover, you may arrange | position the tobacco raw material concerning embodiment of this invention in the filter part of a well-known cigarette, for example, mixing with a normal tobacco engraving in arbitrary ratios. As an arrangement of the filter portion, for example, an arrangement in the cavity or an arrangement in which the filter portion is dispersed in the filter fiber can be used.
The tobacco raw material concerning embodiment of this invention can also be used for a heating type flavor suction device or a non-heating type flavor suction device.
When the tobacco raw material concerning embodiment of this invention is applied to a cigarette or a heating-type flavor suction device, a user can enjoy the flavor resulting from said specific flavor component.

The “heated flavor inhaler” is an aspirator that heats a tobacco material without burning it, and allows the user to taste the flavor of the heated tobacco material by suction, for example, heating the tobacco material with the combustion heat of a carbon heat source Carbon heat source aspirator (see for example WO 2006/073065); an electrically heated aspirator with an aspirator and a heating device for electrically heating the aspirator (for example see WO 2010/110226); or containing tobacco material And a liquid atomizing type aspirator that atomizes a liquid aerosol source by heating (see, for example, WO2015 / 046385).
Among these, the electric heating type flavor inhaler includes a mouthpiece, a container in which a composition containing a tobacco raw material and a main body including an electronic heater, a temperature controller for adjusting the temperature of the electronic heater, and the like. Including. As a specific configuration, the one described in JP 2014-524313 A can be used. A pod can be mentioned as a container in which a composition containing a tobacco raw material is stored, for example. The tobacco raw material according to the embodiment of the present invention is mixed in an arbitrary ratio with, for example, a normal tobacco cut and stored in the above container. Also good. The material of the container in which the tobacco raw material concerning the embodiment of this invention is accommodated is not restrict | limited, A metal with high heat conductivity, such as aluminum, can be mentioned.
When the tobacco raw material according to the embodiment of the present invention is applied to the above-described heating type flavor inhaler, for example, the tobacco raw material according to the embodiment of the present invention is mixed with, for example, a normal tobacco engraver at an arbitrary ratio. It is accommodated in said container as a composition containing what mixed, polyhydric alcohols, such as glycerol and / or propylene glycol, a thickener, and other components, such as a fragrance | flavor as needed.
As a composition applied to a heating type flavor inhaler, an embodiment including a tobacco raw material according to an embodiment of the present invention, a polyhydric alcohol, and a thickener can be preferably exemplified.
There is no restriction | limiting in particular also about the magnitude | size of each leaf tobacco contained in a tobacco raw material, The magnitude | size used for a normal electric heating type flavor suction device can be employ | adopted.
About 10 to 40% of the weight ratio of the tobacco raw material according to the embodiment of the present invention in the composition filled in the container can be mentioned.
In a liquid atomization type aspirator that atomizes a liquid aerosol source containing a tobacco raw material by heating, as an example of a raw material for producing a liquid flavor source incorporated in a liquid container, the embodiment of the present invention is used. Such tobacco raw materials may be used.

When the tobacco raw material according to the embodiment of the present invention is an oral tobacco product, for example, snus can be cited as an example. In this case, the tobacco raw material produced by the above-described manufacturing method is filled with, for example, a normal tobacco engraved in an arbitrary ratio into a packaging material using a raw material such as a nonwoven fabric by a known method. It is obtained by. For example, the amount of tobacco material is adjusted and filled, and sealed by means such as heat sealing to obtain snus.
The packaging material can be used without any particular limitation, but a cellulose-based nonwoven fabric is preferably used.
For example, when the gum is used as the oral tobacco product, it is obtained by mixing the tobacco raw material obtained using the production method according to the embodiment of the present invention with a known gum base and a known method. Chewing tobacco, snuff, and compressed tobacco can also be obtained using a known method, except that the tobacco raw material obtained using the production method according to the embodiment of the present invention is used. Moreover, an edible film can also be obtained using a known material or method, except that the tobacco raw material obtained using the production method according to the embodiment of the present invention is used.

The production method according to the embodiment of the present invention has been a problem with tobacco raw materials that have undergone conventional smoke processing such as DFC, for example, polycyclic aroma contained in smoke produced at a temperature at which incomplete combustion is likely to occur. While the problem of aromatic hydrocarbons adhering to leaf tobacco and the problem of generating substances that give irritating sensations such as acetic acid have been solved, tobacco raw materials with increased components that have the characteristic flavor of smoke Can be provided.
Moreover, you may use the tobacco raw material manufactured by the method of this invention as a part of tobacco raw material in tobacco products. The tobacco raw material obtained by this invention can be used in arbitrary ratios, when using it as a part of tobacco raw material in tobacco products.

  Examples The present invention will be described more specifically with reference to examples. However, the present invention is not limited to the description of the following examples unless it exceeds the gist.

<Experimental example 1>
Drying of leaf tobacco Leaf tobacco immediately after harvesting was dried or trunk-dried, and then naturally dried in a drying room where direct sunlight was not permeable in the range of 25 ° C. to 35 ° C. for about one month.
About the moisture content of the leaf tobacco after drying, it prepared so that it might become 5 to 50 weight% about each sample.

A compact smoker (manufactured by Snow Peak Co., Ltd.) was used for the smoked and smoked tobacco apparatus. About 20 g of wood chips were put on the bottom surface, and about 10 g of the leaf tobacco before deboning, which had been dried as described above, was stacked on top and covered. It installed so that the bottom face part of a smoke-making apparatus might earth | ground on the heating apparatus which can control temperature (Azwan company make, hot plate CHR-250DN). Next, the preset temperature of the heating device was set to 500 ° C., and the wood chips were pyrolyzed. The thermal decomposition time of the wood chip was 10 minutes, and white oak, walnut, hickory, oak or walnut was used as the smoke generating material.
The product temperature of the smoke generating material was adjusted to be about 300 ° C to 600 ° C.

The raw material after smoked processing was put into a plastic bag with a storage processing chuck of leaf tobacco (produced by Nippon Shokubai Co., Ltd.) and lamizip AL-E (produced by Nippon Shokubai Co., Ltd.). The upper part of the plastic bag with the zipper was closed to a slight degree to make it a semi-sealed system. On the other hand, the upper part of Lam Zip AL-E was heat-sealed to make a completely sealed system. These bags were stored in a temperature-controlled room at a temperature of 22 ° C. and a humidity of 62%. The storage period was up to 4 months.

<Differences in content of benzo [a] pyrene, guaiacol, and 2,6-dimethoxyphenol based on differences in the temperature of smoked leaves of tobacco>
With respect to the leaf tobacco (moisture content: 13% by weight) subjected to the drying treatment described in Experimental Example 1, the product temperature of the smoke generating material is 300 ° C, 400 ° C, 450 ° C, 500 ° C, or 600 ° C. About what was smoked so that it might become, content of benzo [a] pyrene, a guaiacol, and 2, 6- dimethoxyphenol was measured, respectively. For reference, the content of the raw material of untreated leaf tobacco and the content of conventional DFC (smoked by hanging tobacco leaves as they are without separating the central bone and lamina) It was measured.
(1) Benzo [a] pyrene The measurement results of benzo [a] pyrene are shown in FIG.
As is apparent from FIG. 2, the content of benzo [a] pyrene was low at 300 to 500 ° C., but the content of benzo [a] pyrene increased dramatically at 600 ° C. This indicates that leaf tobacco obtained by smoking at a temperature exceeding 600 ° C. like conventional DFC contains benzo [a] pyrene at a high content.
FIG. 2 also shows the content of benzo [a] pyrene contained in the original material for comparison.
Table 1 below summarizes the content of benzo [a] pyrene shown in FIG.

(2) Guaiacol Fig. 3 shows the measurement results of guaiacol.
As apparent from FIG. 3, it was found that a large amount of guaiacol was contained in the leaf tobacco when the product temperature of the smoke generating material was 400 to 500 ° C., and the most guaiacol was contained at 450 ° C. FIG. 3 also shows the content of guaiacol contained in the original raw material and the content of guaiacol contained in the conventional DFC for comparison. As shown in FIG. 3, guaiacol is hardly contained in the original raw material. This is because guaiacol is produced by thermal decomposition of lignin and is imparted to leaf tobacco by smoke processing.

(3) 2,6-Dimethoxyphenol The measurement results of 2,6-dimethoxyphenol are shown in FIG.
As apparent from FIG. 4, it was found that a large amount of 2,6-dimethoxyphenol is contained in leaf tobacco when the product temperature of the smoke generating material is 400 to 500 ° C. FIG. 4 also shows the content of 2,6-dimethoxyphenol contained in the original raw material and the content of 2,6-dimethoxyphenol contained in the conventional DFC for comparison.
As shown in FIG. 4, 2,6-dimethoxyphenol is hardly contained in the original raw material. This is because 2,6-dimethoxyphenol is produced by thermal decomposition of lignin and is imparted to leaf tobacco by smoke treatment.
The contents of guaiacol and 2,6-dimethoxyphenol are summarized in Table 2 below.

<Relationship between water content of tobacco leaf before smoked processing and adhesion efficiency of guaiacol and 2,6-dimethoxyphenol>
In order to confirm the relationship between the moisture content of the leaf tobacco after the drying treatment in Experiment Example 1 (before the smoked treatment) and the adhesion efficiency of Guiacol and 2,6-dimethoxyphenol by the smoked treatment to Experiment 1 A test was conducted using the apparatus shown in FIG. 5 instead of the smoke treatment described.
In the apparatus of FIG. 5, the leaf tobacco 3 that has undergone the drying treatment of the first embodiment is disposed in the middle of the cylindrical tube, and the filter 4 is disposed downstream of the leaf tobacco. The smoked product material 1 is heated using a hot plate 2 and smoked, and the amounts of guaiacol and 2,6-dimethoxyphenol attached to the leaf tobacco 3 and guaiacol and 2,6-dimethoxyphenol attached to the filter 4 are determined. Each was measured.
The adhesion efficiency was calculated by the following formula.
Adhesion efficiency (%) = Amount of guaiacol or 2,6-dimethoxyphenol adhering to leaf tobacco / (Amount of guaiacol or 2,6-dimethoxyphenol adhering to leaf tobacco + Amount of guaiacol or 2,6-dimethoxyphenol adhering to filter) × 100
For each of guaiacol and 2,6-dimethoxyphenol, the water content after the drying treatment (before the smoked treatment) is plotted on the horizontal axis, and the adhesion efficiency is plotted on the vertical axis as FIGS.

Regarding the results of adhesion efficiency, the adhesion efficiency of guaiacol and 2,6-dimethoxyphenol was high when the water content of the leaf tobacco after drying treatment (before smoked treatment) was about 15 to 25% by weight. In addition, when the water content of the leaf tobacco after the drying treatment exceeds 30% by weight, fermentation by the action of microorganisms contained in the leaf tobacco progresses, and the balance of the components of the leaf tobacco may be lost, which is not preferable.

<Change over time in content of acetic acid and propionic acid in leaf tobacco during storage under semi-sealed condition or sealed condition>
The smoked tobacco obtained in Experimental Example 1 is stored in a semi-closed system or a closed system, and when the storage period is 0 month, 1 month, 2 months, 3 months, 4 months, The contents of acetic acid and propionic acid were measured. The temperature during storage was 22 ° C. and 66% RH. Moreover, the water content of the leaf tobacco at the time of storage was 15% by weight.
The result of propionic acid is shown in FIG. 8, and the result of acetic acid is shown in FIG.
From the results of FIGS. 8 and 9, as the elapsed time increases, especially when the storage period is 4 months, the contents stored in the semi-enclosed system have higher contents of propionic acid and acetic acid than those stored in the closed system. It was low.

<Time-dependent changes in the contents of propionic acid and acetic acid in leaf tobacco during storage in a semi-sealed condition (acceleration test)>
Storage in a semi-sealed system of leaf tobacco after smoked processing obtained in Example 1 was performed by an accelerated test (40 ° C., 60% RH). It is estimated that 4 months in this accelerated test corresponds to about 24 months of the test at 22 ° C. The result of propionic acid is shown in FIG. 10, and the result of acetic acid is shown in FIG.
From the results of FIGS. 10 and 11, it was found that when the storage period in the semi-enclosed system was made longer, the contents of propionic acid and acetic acid in the stored leaf tobacco decreased.

  According to the production method of the present invention, it is possible to provide a tobacco raw material having a low content of low-molecular carboxylic acids such as benzo [a] pyrene and acetic acid or propionic acid and containing a large amount of specific flavor components. it can.

Claims (7)

  A step of drying leaf tobacco before bone removal after harvesting until the moisture content becomes 10 to 25% by weight, and generation of smoke in the range of 400 to 500 ° C in the temperature of dried leaf tobacco before bone removal A method for producing a tobacco raw material, comprising a step of smoking treatment with smoke obtained by thermally decomposing a material, and a step of storing the smoked and processed leaf tobacco under semi-sealed conditions following the step of smoking treatment.   The method for producing a tobacco raw material according to claim 1, wherein when the leaf tobacco after harvesting is dried, the leaf tobacco is dried until the water content becomes 15 to 20% by weight.   The manufacturing method of the tobacco raw material of Claim 1 or 2 whose said process to store is performed at room temperature, and the period is 3 months or more and less than 24 months. The manufacturing method of the tobacco raw material as described in any one of Claims 1-3 with which the tobacco raw material obtained by the said manufacturing method has the structure of the following (1)-(4).
(1) The content of benzo [a] pyrene is 100 ng / g or less based on the dry weight of the tobacco material (2) The content of acetic acid is 20 mg / g or less based on the dry weight of the tobacco material (3 ) The content of guaiacol is 5 to 5000 μg / g based on the dry weight of the tobacco material. (4) The content of 2,6-dimethoxyphenol is 10 to 10,000 μg / g based on the dry weight of the tobacco material. The tobacco raw material which is comprised from the leaf tobacco which has the structure of the following (1)-(4) and from which the lamina and the inside bone are not separation-processed.
(1) The content of benzo [a] pyrene is 100 ng / g or less based on the dry weight of the tobacco material (2) The content of acetic acid is 20 mg / g or less based on the dry weight of the tobacco material (3 ) The content of guaiacol is 5 to 5000 μg / g based on the dry weight of the tobacco material. (4) The content of 2,6-dimethoxyphenol is 10 to 10,000 μg / g based on the dry weight of the tobacco material.   A tobacco product comprising the tobacco raw material according to claim 5.   The tobacco product according to claim 6, which is a cigarette or a heated flavor inhaler.