RU2587075C1 - Aroma-bearing cigarette ingredients and cigarette containing same - Google Patents

Abstract

FIELD: tobacco industry.

SUBSTANCE: invention relates to cigarette aroma carrying component and to cigarette containing it. Aroma carrying cigarette component is obtained by application of aromatic composition in the state of sol onto surface of cigarette component, aromatic composition includes flavouring agent, water and polysaccharide, selected from group consisting of carrageenan, gellan gum and combination of gellan gum and tamarind gum; then cooling of containing aromatic composition cigarette component till the temperature from 0 to 40°C to cause jellying of aromatic composition; and then drying of containing aromatic composition component cigarette during heating.

EFFECT: technical result is creation of aroma carrying component of cigarette, which has high stability of aroma and which enables to obtain uniform distribution of flavouring agent in cigarette during its introduction into cigarette.

7 cl, 9 dwg, 3 tbl, 10 ex

Description

Technical field

The present invention relates to a flavor component of a cigarette and to a cigarette containing it.

State of the art

If a volatile aromatic component, such as menthol, is added to the ground tobacco in a solution state, the aromatic component is dispersed during long-term storage and the flavoring effect is short-lived. The solution to this problem is discussed in various posts.

Patent Publications 1 to 3 represent an example in which the aromatic component is placed in shredded tobacco, which is the burning site, or in cigarette paper that wraps shredded tobacco.

Patent Document 1 describes that a cigarette paper wrapping a tobacco filler is coated with an aromatic material in which the aromatic component is embedded in a three-dimensional network of glucan molecules. The cigarette according to Patent Document 1 has a good aroma conservation ability because the aromatic component is fixed and held in a state of incorporation of glucan molecules into a three-dimensional network. However, the aromatic component is present in glucan molecules in a relatively small amount (20 wt.% Or less). Accordingly, in the case of an aromatic component such as menthol, which needs to be added in a relatively large amount, the amount of mixed aromatic material added to the cigarette increases.

Patent Document 2 describes that a “stabilized aromatic substance that remains stable up to 180 ° C” is made by mixing a liquid flavor and a carrageenan sol; introducing the mixture in drops into an ionic solution (a solution containing potassium ions) to produce a granular gel; and drying the gel in air. However, when using the method according to patent document 2, it takes a long time and large equipment to produce a large amount of material, because the granular gel is dried in air.

Patent Document 3 describes that a sheet containing an aromatic component that covers a polysaccharide gel is made by drying a suspension containing an aromatic component such as menthol and a polysaccharide; the leaf is ground and the ground particles are added to the ground tobacco. The scent sheet according to Patent Document 3 has a high flavor content because a polysaccharide gel is applied to the scent component, and thus, evaporation of the scent component is difficult.

State of the art publications

Patent documents

Patent Document 1: Published Application JP (KOKAI) 9-28366 (1998).

Patent Document 2: Published PCT Application JP 11-509566 (2000).

Patent Document 3: International Publication WO 2009/142159.

SUMMARY OF THE INVENTION

Technical problem

The inventors of the present invention have found that when crushed particles of a flavoring sheet having a high flavoring content are added to a cigarette as a tobacco filler in a small amount (for example, when contained in a mixture of 2% by weight) according to Patent Document 3, sometimes in a cigarette rod uneven distribution of flavoring occurs.

In order to eliminate this defect, the present invention provides an aroma-bearing component of a cigarette that has high flavor stability and which allows to obtain a uniform distribution of flavor in the cigarette when it is introduced into the cigarette.

Solution

The present inventors have found that by applying a suspension containing a specific polysaccharide and flavor to a component of a cigarette, such as a tobacco filler or cigarette paper, high flavor stability can be obtained, the flavor can be evenly distributed in the cigarette, and the variability of the flavoring content of the cigarettes can be suppressed. . As a result of this, the present inventors have completed the present invention.

According to a first aspect of the present invention, there is provided an aromatic component of a cigarette obtained by: applying an aromatic composition in a sol state on the surface of a component of a cigarette, the aromatic composition comprising a flavoring agent, water and a polysaccharide selected from the group consisting of carrageenan, gellan gum and a combination of gellan gum and tamarind gums; then cooling the cigarette component containing the aroma composition to a temperature of 0 to 40 ° C. to cause the aroma composition to gel; and then drying by heating the aromatic composition-containing component of the cigarette.

According to a preferred embodiment, the drying by heating is carried out in such a way that the surface temperature of the aromatic composition is maintained in the range from 70 to 100 ° C.

According to a specific embodiment, the component of the cigarette is a tobacco filler or cigarette paper. According to a more specific embodiment, the tobacco filler is ground tobacco or leaf tobacco.

According to a second aspect of the present invention, there is provided a cigarette comprising an aroma-bearing component of a cigarette of the invention.

The technical result of the invention

The aroma-bearing component of a cigarette according to the invention has a high flavor retention capacity after aging, and its advantage is that the aroma can be uniformly introduced into the cigarette (more precisely, at the place where the aroma-bearing component of the cigarette is introduced) when it is introduced into the cigarette. In other words, when a cigarette is manufactured using the aroma-bearing component of the cigarette of the invention, the uneven distribution of flavor in the cigarette rod can be suppressed. As a result of this, a cigarette made using the flavored component of the cigarette of the invention can continuously and stably release the flavor during the entire smoking period, and for this reason, smokers can feel the same aroma and taste during smoking throughout the entire smoking time.

In addition, the flavoring component of the cigarette of the invention also has the advantage that it becomes possible to suppress the variability of the flavoring content of cigarettes in the manufacture of a plurality of cigarettes using this component because the flavoring is uniformly distributed in the cigarette.

Brief Description of the Drawings

FIG. 1 is a graph illustrating the ability to maintain menthol flavor after aging in shredded tobacco, on the surface of which a menthol-containing composition is applied.

FIG. 2 is a graph illustrating the ability to maintain menthol flavor after aging in the case of a cigarette containing ground tobacco on the surface of which a menthol-containing composition is applied.

FIG. 3 is a graph illustrating the ability to maintain menthol flavor after aging in the case of leaf tobacco, on the surface of which a menthol-containing composition is applied.

FIG. 4 is a graph illustrating the ability to maintain the menthol flavor after aging in the case of a cigarette containing leaf tobacco, on the surface of which a menthol-containing composition is applied.

FIG. 5 is a graph illustrating the ability to maintain menthol flavor after aging in the case of cigarette paper, on the surface of which a menthol-containing composition is applied.

FIG. 6 is a graph illustrating the ability to maintain menthol flavor after aging in the case of a cigarette containing cigarette paper on the surface of which a menthol-containing composition is applied.

FIG. 7A is a graph illustrating a change in viscosity after a decrease in temperature of a carrageenan-containing liquid.

FIG. 7B is a graph illustrating a change in viscosity after an increase in temperature of a carrageenan-containing liquid.

FIG. 8A is a graph illustrating a change in viscosity after a decrease in temperature of a gellan gum-containing liquid.

FIG. 8B is a graph illustrating a change in viscosity after an increase in temperature of a gellan gum-containing liquid.

FIG. 9A is a graph illustrating a change in viscosity after a decrease in temperature of a liquid containing gellan gum and tamarind gum.

FIG. 9B is a graph illustrating a change in viscosity after an increase in temperature of a liquid containing gellan gum and tamarind gum.

Description of Embodiments

The present invention is explained below. The following explanations are intended to describe the present invention in detail and are not intended to limit the present invention.

The flavor component of a cigarette according to the invention is obtained by:

applying the aromatic composition in a sol state to the surface of the cigarette component, the aromatic composition comprising a flavoring agent, water and a polysaccharide selected from the group consisting of carrageenan, gellan gum and a combination of gellan gum and tamarind gum; then

cooling the cigarette component containing the aromatic composition to a temperature of from 0 to 40 ° C. to cause gelation of the aromatic composition; and then

drying by heating the aroma-containing component of the cigarette.

The flavoring used according to the invention is not limited, provided that it is a flavoring used in smoking articles. You can use any type of flavor. Examples of flavoring are mainly menthol; tobacco leaf extract; natural plant flavors (e.g. cinnamon, sage, aromatic herbs, chamomile, kudzu (hairy pueraria), sweet hydrangea leaf, cloves, lavender, cardamom, cloves, nutmeg, bergamot, geranium, honey essence, rose oil, lemon, orange , Chinese cinnamon bark, cumin, jasmine, ginger, coriander, vanilla extract, curly mint, peppermint, acacia, coffee, celery, croton tree, sandalwood, cocoa, ylang-ylang, fennel, anise, licorice, carob, extract prunes and peach extract); saccharides (e.g. glucose, fructose, isomerized saccharide and caramel); cocoa (e.g., powder and extract); esters (e.g. isoamyl acetate, linalyl acetate, isoamyl propionate and linalyl butyrate); ketones (e.g., menton, ionon, damascenone and ethyl maltol); alcohols (e.g. geraniol, linalool, anethole and eugenol); aldehydes (e.g. vanillin, benzaldehyde and anisic aldehyde); lactones (e.g., γ-undecalactone and γ-nonalactone); flavors of animal origin (e.g., musk, ambergris, cibetin and beaver musk); and hydrocarbons (e.g., limonene and pinene). A flavoring agent that is readily dispersible in a solvent by adding an emulsifier such as a hydrophobic flavoring agent and an oil soluble flavoring agent may be preferably used. Such a flavor can be used individually or in combination.

The present invention is further explained by way of example in which menthol is used as a flavoring agent.

1. Menthol Composition

According to one embodiment of the present invention, an aroma-bearing component of a cigarette is made by applying an aromatic composition containing menthol and a polysaccharide selected from the group consisting of carrageenan, gellan gum and a combination of gellan gum and tamarind gum (hereinafter referred to as "menthol-containing composition") to the cigarette component. The flavor component of a cigarette according to the invention is preferably obtained by applying an aromatic composition to the surface of a component of a cigarette.

The menthol-containing composition used according to the invention is in a state of suspension having flowability at a heating temperature (for example, from 60 to 90 ° C.) before it is dried.

The menthol-containing composition (suspension) may have the following composition: for example, from 200 to 500 g of polysaccharide, from 1000 to 2500 g of menthol and from 80 to 200 ml of a solution containing from 2 to 10 weight. % emulsifier, per 10 liters of water. The menthol-containing composition (suspension) has a water content of typically 70 to 95 weight. % and preferably from 80 to 90 weight. % In a menthol-containing composition, the ratio (weight ratio) of polysaccharide and menthol may be from 1: 1 to 1:10.

According to the invention, the polysaccharide has the property that it fixes micelles of a flavoring agent, such as menthol, covering the flavoring and causing gelation of the aqueous polysaccharide solution upon cooling. As a polysaccharide having this property, a polysaccharide selected from the group consisting of carrageenan, gellan gum and a combination of gellan gum and tamarind gum can be used. According to the invention, when carrageenan is used as a polysaccharide, another polysaccharide such as gellan gum or tamarind gum can be introduced into the menthol-containing composition in a smaller amount than the amount of carrageenan. Similarly, when gellan gum is used as a polysaccharide, another polysaccharide, such as carrageenan, can be introduced into the menthol-containing composition in a smaller amount than the amount of gellan gum.

According to the invention, 1-menthol can be used as menthol.

According to the invention, an emulsifier of natural origin, such as lecithin, in particular Sun Lecithin A-1 from Taiyo Kagaku Co., Ltd., can be used as an emulsifier.

According to the invention, a menthol-containing composition (suspension) can be prepared by a method which comprises: step (i) mixing the polysaccharide with water and heating the mixture to produce an aqueous polysaccharide solution; and step (ii) adding menthol and an emulsifier to the aqueous solution, mixing and emulsifying the mixture.

Step (i) can be carried out, in particular, by adding the polysaccharide to the water in small portions during the mixing process, and as a result, the polysaccharide is dissolved. The heating temperature at this stage may be from 60 to 90 ° C, and preferably from 75 to 85 ° C. Step (ii) can be carried out by a known emulsification method using a homogenizer, because the menthol-containing composition (suspension) has a viscosity of about 10,000 mPa · s or less (sol state) at the aforementioned heating temperature, whereby emulsification is not slowed down.

2. Application of a menthol-containing composition to a cigarette component

According to the invention, a menthol-containing composition is applied to a component of a cigarette, preferably to the surface of a component of a cigarette.

In particular, according to the invention, the component of the cigarette is a component that occupies a position in which there is no contact with the mouth or oral cavity of the smoker when this component is placed in the cigarette. In other words, a component of a cigarette is a component in a position in which a flavor, such as menthol, can be released along with smoke inhaled by the smoker during combustion during smoking, when this component is placed in the cigarette.

More specifically, the cigarette component is a tobacco filler or cigarette paper. Even more specifically, the tobacco filler is ground tobacco or leaf tobacco.

The method of applying the menthol-containing composition to the cigarette component is not limited in a particular way, provided that the menthol-containing composition (suspension) can be uniformly applied to the cigarette component. The menthol-containing composition (suspension) may be introduced or applied to the surface of the cigarette component, the menthol-containing composition (suspension) may be sprayed onto the surface of the cigarette component, or the cigarette component may be immersed in the menthol-containing composition (suspension).

When the menthol-containing composition (suspension) is in a sol state at a temperature of about 60 to 90 ° C, is applied to the crushed tobacco, the menthol-containing composition (suspension) can be applied directly to the surface of the crushed tobacco using a transfer pump, or the composition can be sprayed onto chopped tobacco using a spray tip. Alternatively, the ground tobacco may be immersed in a menthol-containing composition (suspension) so that the menthol-containing composition (suspension) covers the ground tobacco.

When the menthol-containing composition (suspension) is in a sol state at a temperature of about 60 to 90 ° C, and is applied to the tobacco sheet, the menthol-containing composition (suspension) can be applied by extrusion to the surface of the tobacco sheet using a slot feeder, or the composition can be coated leaf tobacco surface using a film applicator. Alternatively, spraying or dipping may be carried out in the same manner as is used to apply to ground tobacco.

When the menthol-containing composition (suspension) is in a sol state at a temperature of about 60 to 90 ° C, is applied to cigarette paper, the menthol-containing composition (suspension) can be applied by extrusion using a slot feeder, or by coating using a coating device films as described above. Alternatively, spraying or dipping may be carried out in the same manner as is used to apply to ground tobacco. In the case of ground tobacco, the menthol-containing composition (suspension) can be applied in an amount of 5 to 40 parts by weight and preferably 15 to 25 parts by weight per 100 parts by weight of the ground tobacco. In the case of leaf tobacco, the menthol-containing composition (suspension) can be applied in an amount of 50 to 400 parts by weight and preferably 100 to 200 parts by weight per 100 parts by weight of sheet tobacco. In the case of cigarette paper, the menthol-containing composition (suspension) can be applied in an amount of 10 to 70 parts by weight, preferably 30 to 50 parts by weight, per 100 parts by weight of cigarette paper.

Before drying the component of the cigarette on which the menthol-containing composition (suspension) has been applied, it is preferable to cool the component of the cigarette once so that the suspension acquires a temperature that provides sufficient gelation of the suspension (40 ° C or less) and prevents the emulsion from breaking due to freezing (0 ° C or more). In particular, it is preferable that the component of the cigarette be cooled once so that the suspension acquires a temperature of 0 to 40 ° C, preferably 0 to 30 ° C, and more preferably 15 to 25 ° C. Here, the menthol-containing composition (suspension), before it is cooled, has a temperature of 60 to 90 ° C, and preferably 75 to 85 ° C, and is in a sol state. Such pre-cooling can be carried out by blowing air or introducing cold air (for example, at 10 ° C), which produces a local cooler (for example, Suiden SS-25DD-1), on the component of the cigarette on which the menthol-containing composition (suspension) was applied , for 2 to 3 minutes. Alternatively, pre-cooling can be carried out by introducing the component of the cigarette onto which the menthol-containing composition (suspension) has been applied into contact with the tube through which the cooling medium (for example, at 10 ° C), produced by a cold or warm water generator, such as a cooler, for example, the PCU-1600R from Apiste Corporation, for 1 to 2 minutes. Alternatively, pre-cooling can be carried out by keeping the component of the cigarette onto which the menthol-containing composition (suspension) applied, at room temperature.

When the aqueous polysaccharide solution used according to the invention is cooled, which causes gelation, the resulting gel has the ability to maintain a gel state without easily returning to the sol state, even if the temperature then rises and reaches the gelation temperature (see examples described below). Using the property described above, the menthol-containing composition (suspension) is pre-cooled before it is dried. As a result, the polysaccharide that is present in the menthol-containing composition (which has been pre-cooled but not dried) is difficult to sol, even if the temperature rises during drying, and it becomes especially difficult to vaporize the menthol coated with the polysaccharide. Thus, according to the invention, due to pre-cooling, it is possible to influence heat on the menthol-containing composition in a subsequent drying step, and for this reason, a short drying time can be provided.

The component of the cigarette on which the menthol-containing composition has been applied can be dried by heating, by performing a drying process by heating of any type, such as drying with hot air or drying with heat of infrared radiation.

The menthol-containing composition that has been applied to the cigarette component can be dried so that the temperature of the sample is kept at 100 ° C or lower, preferably from 70 to 100 ° C, during the entire drying step. To maintain the temperature of the sample at 100 ° C or lower, a drying temperature of 100 ° C to 130 ° C is preferably used. In order to maintain the temperature of the sample in the range of 70 to 100 ° C, a drying temperature of 100 ° C to 130 ° C is preferably used. Here, “sample temperature” means the surface temperature of the menthol-containing composition in the drying step, and “drying temperature” means the temperature in the drying oven. The temperature in the drying oven is equal to the temperature of the hot air in the case of drying with hot air.

Preferably, drying includes drying at a drying temperature of 100 ° C or more, and preferably from 100 ° C to 130 ° C, for a quarter or most of the total drying time. Drying can be carried out for 20 minutes or less from the full drying time until the water content in the flavored component of the cigarette is less than 10%. Preferably, drying at a drying temperature of 100 ° C or more is carried out in an initial drying step, and then drying is carried out at a drying temperature that is equal to or less than the initial drying temperature, preferably 70 ° C or more and less than 100 ° C.

The drying temperature is set so that the temperature of the sample is maintained at 100 ° C or lower at any time during the entire drying step, and the drying temperature can be kept constant throughout the drying step, or it can be changed during the drying step. When the drying temperature changes, the drying is preferably carried out by initial drying at a high drying temperature of 100 ° C or more, and subsequent final drying at a low drying temperature of less than 100 ° C. As used herein, “initial drying” means drying using a high temperature of 100 ° C. or more in a first drying step, and “final drying” means drying carried out after an initial drying using a low temperature of less than 100 ° C. When the initial drying at high temperature is carried out in combination with the final drying at low temperature, the temperature of the sample does not become excessively high, and the temperature of the sample is kept at 100 ° C or lower at any time throughout the drying step, and the drying time can preferably be shortened.

More preferably, the drying can be carried out by initial drying at a drying temperature of 100 ° C or more, for a quarter or most of the total drying time; thereafter, final drying is carried out at a drying temperature of less than 100 ° C. for a quarter or most of the total drying time. Drying can be carried out for 20 minutes or less than the entire drying time until the water content in the flavored component of the cigarette reaches a predetermined value (in particular, until the water content is about 12 wt.% Or less in the case of the flavored component of the cigarette obtained by applying the menthol composition to crushed tobacco, and until the water content is about 10 wt.% or less in the case of the flavored component of whitefish a diet obtained by applying a menthol-containing composition to tobacco leaf or cigarette paper).

As described above, when the initial drying at high temperature is carried out in combination with the final drying at low temperature, the aroma-bearing component of the cigarette according to the invention has a particularly high menthol content after manufacture, and the menthol content can remain at a particularly high level even after aging.

When hot air drying is carried out, initial drying can be carried out, for example, at a hot air temperature of 100 ° C or more and 130 ° C or less, for 4 to 6 minutes, and final drying can be carried out, for example, at hot temperature air of 70 ° C or more and less than 100 ° C for 4 to 6 minutes. The air velocity can be set, for example, in the range from 3 to 20 m / s. The total drying time is 20 minutes or less, and preferably from 10 to 18 minutes.

Conditions (temperature, time and air flow rate) at the initial drying and final drying stages can be set appropriately, for example, at the intervals presented above.

The drying temperature in the initial drying step may be kept constant, or it may be changed so that the temperature then drops to a level of 100 ° C to 130 ° C. The drying temperature in the final drying step may also be kept constant, or it may be changed so that the temperature then decreases to a level of from 70 ° C to less than 100 ° C. For example, the drying oven used in the examples described below has three drying chambers, and the sample is fed sequentially to the first, second, and third chambers via a conveyor belt. Thus, the first and second chambers can be used for initial drying at the same or different temperatures of 100 ° C or more, and the third chamber can be used for final drying at temperatures of less than 100 ° C. Alternatively, the first chamber can be used for initial drying at temperatures of 100 ° C or more, and the second and third chambers can be used for final drying at the same or different temperatures of less than 100 ° C.

Drying is preferably carried out until the water content of the flavored component of the cigarette reaches a predetermined value (in particular, until the water content reaches about 12 wt.% Or less in the case of the flavored component of the cigarette obtained by applying the menthol-containing composition to chopped tobacco, and until the water content becomes equal to about 10 wt.% or less in the case of a flavored component of a cigarette obtained by n incurring composition comprising menthol sheet tobacco or cigarette paper). The water content in the present description means the value obtained by the measurement method described in the examples below.

3. Cigarette

The present invention provides a cigarette comprising an aroma-bearing component of a cigarette of the invention. The cigarette of the invention has the same construction as a conventional cigarette, except that the flavoring component of the cigarette of the invention is used instead of the component of a conventional cigarette. According to a specific embodiment of the present invention, the cigarette contains ground tobacco on which the aromatic composition of the invention is applied, leaf tobacco on which the aromatic composition of the invention is applied, or cigarette paper on which the aromatic composition of the invention is applied. The cigarette of the invention may comprise a combination of the flavored components of the cigarette of the invention. For example, a cigarette may contain ground tobacco coated with the aromatic composition of the invention in combination with leaf tobacco coated with the aromatic composition of the invention. Alternatively, the cigarette may comprise ground tobacco coated with the aromatic composition of the invention in combination with cigarette paper coated with the aromatic composition of the invention.

The ground tobacco on which the aromatic composition of the invention is applied may be present in a cigarette at a content of 20 to 100 weight. % of the total weight of the tobacco filler when the tobacco filler contained in one cigarette is defined as 100 weight. % Leaf tobacco coated with the aromatic composition of the invention may be present in a cigarette at a content of 10 to 40 weight. % of the total weight of the tobacco filler when the tobacco filler contained in one cigarette is defined as 100 weight. %

Examples

The present invention is explained through the examples below.

1. The manufacture of containing menthol compositions (suspensions) 1-3

The composition of the menthol-containing composition (suspension) 1 (carrageenan was used as the polysaccharide)

Water 10 l.

Carrageenan (CS-530 / San-Ei Gen F. F. I., Inc.) 500 g

Lecithin (Sun Lecithin A-1 / Taiyo Kagaku Co., Ltd.) 200 ml (5% aqueous solution).

Menthol (Takasago International Corporation) 2500

The composition of the menthol-containing composition (suspension) 2 (gellan gum was used as the polysaccharide)

Water 10 l.

Gellan Gum (KELCOGEL / San-Ei Gen F. F. I., Inc.) 300 g.

Lecithin (Sun Lecithin A-1 / Taiyo Kagaku Co., Ltd.) 120 ml (5% aqueous solution).

Menthol (Takasago International Corporation) 1500

The composition of the menthol-containing composition (suspension) 3 (gellan gum and tamarind gum were used as the polysaccharide)

Water 10 l.

Gellan Gum (KELCOGEL / San-Ei Gen F. F. I., Inc.) 150 g.

Tamarind gum (VIS TOP D-2032 / San-Ei Gen F. F. I., Inc.) 150 g.

Lecithin (Sun Lecithin A-1 / Taiyo Kagaku Co., Ltd.) 120 ml (5% aqueous solution).

Menthol (Takasago International Corporation) 1500

Menthol containing compositions (suspensions) 1-3, having the above compositions, were prepared as follows: water (10 L) was kept at 80 ° C, and polysaccharide (carrageenan (500 g) in the case of menthol containing composition 1, gellan gum (300 g ) in the case of menthol-containing composition 2, or gellan gum (150 g) and tamarind gum (150 g) in the case of menthol-containing composition 3) was dissolved in water, adding in small portions so that no lumps formed (the required time was approximately 20 minutes), and the mixture was stirred using zuya mixer model PRIMIX T. K. AUTO MIXER 40, equipped with a rotor for stirring the solution at 2000 r / min. After this, menthol was added (2500 g in the case of menthol-containing composition 1 and 1500 g in cases of menthol-containing compositions 2 and 3).

The mixer was replaced with a PRIMIX T.K. AUTO MIXER 40 model homogenizer equipped with a rotor-stator head, and the mixture was emulsified at 4000 rpm for 10 minutes. After that, lecithin was added to the emulsion (200 ml of a 5% aqueous solution in the case of menthol-containing composition 1 and 120 ml of a 5% aqueous solution in the cases of menthol-containing compositions 2 and 3), emulsification was continued for 10 minutes, and a menthol-containing composition was obtained (suspension )

The resulting menthol-containing compositions (suspensions) 1-3 were used in the experiments described below.

2. The manufacture of the flavored component of the cigarette

2-1. Making Flavored Shredded Tobacco

A menthol-containing composition (suspension) (20 parts by weight) in a sol state at approximately 60 ° C. was uniformly applied to shredded Mild Seven Super Lights brand tobacco manufactured by Japan Tobacco Inc. (100 parts by weight). In this experiment, a menthol-containing composition (suspension) was added to the milled tobacco using a Heisin Mohno-Pump 2NVL06F transfer pump manufactured by HEISHIN Ltd.

The shredded tobacco to which the menthol-containing composition (suspension) was added was cooled once by blowing cold air having a temperature of 10 ° C. using a Suiden SS-25DD-1 cold air generator until the temperature of the menthol-containing composition added to chopped tobacco did not reach a level of 20 ° C or lower (product temperature was measured with a PT-7LD device manufactured by Optex Co., Ltd.).

After that, the chilled ground tobacco was dried with hot air, passing on a conveyor belt through a drying oven (the hot air temperature was set at 110 ° C, reduced to 2.5 ° C in 2.5 minutes, reduced to 80 ° C in 5 minutes and kept at this level for 2.5 minutes) until the water content in the crushed tobacco, to which the menthol-containing composition was added, reached about 12 weight. % (see below, "Measurement of water content"). The interweaving of ground tobacco was unraveled, and the result was “flavored ground tobacco of the invention”. Ground tobacco on which menthol-containing composition 1 was applied is called the term “flavored ground tobacco 1 of the invention”. Shredded tobacco on which menthol-containing composition 2 was applied is called the term “flavored shredded tobacco 2 of the invention”, and shredded tobacco on which menthol-containing composition 3 was applied is called the term “flavored shredded tobacco of 3 according to the invention”. All types of flavored shredded tobacco 1-3 according to the invention had a water content of from 2 weight. % to 13 weight. %

On the other hand, a control sample in the case of ground tobacco was prepared by adding menthol to the ground tobacco in the usual manner. In the case of a control sample, flavor (menthol) was applied to the ground tobacco by spraying an ethanol solution containing the flavor to the ground tobacco. The flavor was applied in such a way that the ground tobacco had a menthol content of 1.0 weight. % of the total weight of the crushed tobacco.

2-2. Making Flavored Menthol Tobacco

The composition (suspension) in the sol state at approximately 60 ° C was applied uniformly, as far as possible, to leaf tobacco (reconstituted tobacco material), which was made by the paper manufacturing method. In particular, using a device for applying a film, the menthol-containing composition (suspension) was poured onto tobacco sheet to obtain a layer 0.2 mm thick, and as a result, the tobacco sheet was coated with a menthol-containing composition (suspension). Here, the menthol-containing composition (suspension) was applied in an amount of 150 parts by weight per 100 parts by weight of leaf tobacco.

The leaf tobacco that was coated with the menthol-containing composition (suspension) was cooled once by blowing cold air at 10 ° C using a Suiden SS-25DD-1 cold air generator until the temperature of the menthol-containing composition applied to the leaf tobacco , did not reach a level of 20 ° C or lower (product temperature was measured with a PT-7LD device manufactured by Optex Co., Ltd.).

After that, the chilled leaf tobacco was dried with hot air, passing on a conveyor belt through a drying oven (the hot air temperature was set at 110 ° C, reduced to 2.5 ° C in 2.5 minutes, reduced to 80 ° C in 5 minutes and kept at this level for 2.5 minutes) until the water content in the leaf tobacco to which the menthol-containing composition was added reaches about 12 weight. % (see below, "Measurement of water content"). The interlacing of the crushed tobacco was unraveled, and the result was “flavored tobacco leaf according to the invention”. The leaf tobacco on which the menthol-containing composition 1 has been applied is called the term “flavored leaf tobacco 1 of the invention”. The leaf tobacco on which the menthol-containing composition 2 has been applied is called the term “flavored leaf tobacco 2 of the invention”. The leaf tobacco on which the menthol-containing composition 3 has been applied is called the term “flavored leaf tobacco 3 of the invention”. All kinds of flavored tobacco leaf 1-3 according to the invention had a water content of 9 wt. % to 10 weight. %

On the other hand, a control sample in the case of leaf tobacco was prepared using a conventional flavoring method that is used for ground tobacco. In the case of a control sample, a flavor (menthol) was applied to the tobacco sheet by spraying an ethanol solution containing the flavoring onto the tobacco sheet. The flavor was applied in such a way that the leaf tobacco had a menthol content of 5.0 weight. % of the total weight of leaf tobacco.

2-3. Making Flavored Cigarette Paper

A menthol-containing composition (suspension) in a sol state at approximately 60 ° C. was applied as uniformly as possible onto cigarette paper having a surface density of 40 g / m ² and a thickness of 35 μm. In particular, using a device for applying a film containing a menthol composition (suspension) was poured onto cigarette paper, obtaining a layer with a thickness of 0.05 mm Here, the menthol-containing composition (suspension) was applied in an amount of 150 parts by weight per 100 parts by weight of cigarette paper.

Cigarette paper coated with a menthol-containing composition (suspension) was cooled once by blowing cold air at 10 ° C using a Suiden SS-25DD-1 cold air generator until the temperature of the menthol-containing composition applied to the cigarette paper , did not reach a level of 20 ° C or lower (product temperature was measured with a PT-7LD device manufactured by Optex Co., Ltd.).

After that, the cooled cigarette paper was dried with hot air, passing on a conveyor belt through a drying oven (the hot air temperature was set at 110 ° C, reduced to 2.5 ° C in 2.5 minutes, reduced to 80 ° C in 3 minutes and kept at this level for 2.5 minutes) until the water content in the cigarette paper onto which the menthol-containing composition was applied reaches about 12 weight. % (see “Measuring the water content” described below), and as a result, the “cigarette paper of the invention” was obtained.

Cigarette paper onto which menthol-containing composition 1 was applied is called the term “flavored cigarette paper 1 of the invention”. Cigarette paper onto which menthol-containing composition 2 was applied is called the term “flavored cigarette paper 2 of the invention”. Cigarette paper onto which menthol-containing composition 3 was applied is called the term “flavored cigarette paper 3 of the invention”. All types of flavored cigarette paper 1-3 according to the invention had a water content of 6 wt. % to 7 weight. %

On the other hand, a control sample in the case of cigarette paper was obtained using the conventional flavoring method used for ground tobacco. In the case of a control sample, a flavor (menthol) was applied to cigarette paper by spraying an ethanol solution containing a flavor on cigarette paper. The flavor was applied in such a way that the cigarette paper had a menthol content of 1.0 weight. % by weight of cigarette paper.

3. Measurement of water content

In order to ensure a dry state of the menthol-containing composition (suspension) applied to the cigarette component, the water content was measured as follows.

3-1. Production of a solution for measuring water content

10 ml of methanol was added to a weighed mass of 0.1 g of the manufactured aromatic component of the cigarette (fresh reagent of high purity or higher purity was introduced through a dispenser without air access to exclude the effects of water absorption in air) in an airtight container of 50 ml, which was stored in a desiccator . The resulting mixture was shaken using a SHAKER SRR-2 model shaker manufactured by AS ONE for 40 minutes by linear (reciprocating) shaking with an amplitude of 3 cm and a frequency of 200 rpm. The mixture was kept overnight, and then it was shaken again for 40 minutes under the same conditions as described above at 200 rpm. The supernatant obtained after aging (at the lowest possible air access) was poured into a vessel and used as a solution for measuring the water content.

3-2. Measurement of water content by gas chromatography with a thermal conductivity detector (GC-TCD)

The resulting water content measurement solution was investigated by the GC-TCD method as described below, and quantification was carried out using a calibration curve.

GC-TCD system: 6890 gas chromatograph manufactured by Hewlett Packard.

Column: the full HP Polapack Q column.

Carrier gas: He.

Constant flow mode: 20.0 ml / min.

Injection volume: 1.0 μl.

Intake: the inlet of a filled column with electronic pressure control (EPC) purge.

Heater temperature: 230 ° C.

Intake Gas: He.

Total flow rate: 21.1 ml / min.

Oven mode: keeping for 4.5 minutes at 160 ° C, heating at a speed of 60 ° C / min to 220 ° C, keeping for 4.0 minutes.

Detector: thermal conductivity detector (TCD).

Gas Comparison: He.

Flow rate: 20 ml / min.

Auxiliary gas: He.

Flow rate: 3.0 ml / min.

Signal transfer rate: 5 Hz.

The concentration of the solutions for the calibration curve: six points 0, 1, 3, 5, 10 and 20 mg of H ₂ O / 10 ml.

4. Measurement of menthol

The “menthol content of the flavored component of the cigarette” and the “menthol content of the smoke inhaled by the smoker” were measured by the following methods. The menthol content of the manufactured flavored component of the cigarette was measured to examine the ability to retain flavor after aging and the uniform distribution of flavor in the mixture. In addition, the menthol content of the smoke inhaled by the smoker was measured in order to examine the ability to retain aroma after aging.

4-1. The manufacture of a solution for measuring the menthol content in a cigarette component

10 ml of methanol (reagent of high purity or higher purity) in an airtight container (tube with a screw cap) with a volume of 50 ml was added to a sample weighing 0.1 g of the manufactured flavored component of the cigarette. The resulting mixture was shaken using a SHAKER SRR-2 model shaker manufactured by AS ONE for 40 minutes by linear (reciprocating) shaking with an amplitude of 3 cm and a frequency of 200 rpm. The mixture was kept overnight, and then it was shaken again for 40 minutes under the same conditions as described above at 200 rpm. The supernatant obtained after aging was diluted sufficiently to make it suitable for measurement by gas chromatography (ten-fold dilution with methanol was performed here), and was used as a solution for determining the menthol content by gas chromatography with a flame ionization detector (GC-FID).

4-2. Production of a solution for measuring menthol in inhaled smoke

An extraction solution after passing through a Cambridge filter was prepared as described below, and was used as a solution for measuring menthol content. In particular, 10 ml of methanol (reagent of high purity or higher purity) was added to a sample passed through a Cambridge filter in an airtight container (tube with screw cap) with a volume of 50 ml. The resulting mixture was shaken using a SHAKER SRR-2 model shaker manufactured by AS ONE for 40 minutes by linear (reciprocating) shaking with an amplitude of 3 cm and a frequency of 200 rpm. The supernatant obtained after aging was poured into a vessel and used as a solution to determine the menthol content by gas chromatography with a flame ionization detector (GC-FID).

4-3. Measurement of menthol by gas chromatography with flame ionization detector (GC-FID)

The resulting menthol content measurement solution was investigated by the GC-FID method as described below, and quantification was performed using a calibration curve.

GC-FID System: 6890N Gas Chromatograph manufactured by Agilent Technologies, Inc.

Column: DB-WAX 30 m × 530 μm × 1 μm (maximum temperature 220 ° C).

Carrier gas: He (helium).

Constant Pressure Mode: 5.5 psi (37.92 kPa) (50 cm / s).

Injection volume: 1.0 μl.

Intake: Non-split mode, temperature 250 ° C, pressure 5.5 psi (37.92 kPa).

Oven mode: heating from 80 ° C to 170 ° C at a speed of 10 ° C / min and holding for 6.0 minutes.

Detector: flame ionization detector (FID), temperature 250 ° C, hydrogen flow 40 ml / air flow 450 ml / min).

Signal transfer rate: 20 Hz.

The concentration of solutions for the calibration curve: eight points 0, 0.01, 0.05, 0.1, 0.3, 0.5, 0.7 and 1.0 mg of menthol / ml.

5. Research in harsh conditions

The manufactured flavor component of the cigarette was placed at 50 ° C in a DX 600 thermostat manufactured by Yamato Scientific Co., Ltd. and held for one week, two weeks, or one month (30 days). The menthol content was measured at each point in time, as described above, and the ability to retain aroma after aging was evaluated based on the change in menthol content.

6. Cigarette making and smoking experiment

Using the aroma-bearing component of the cigarette of the invention, cigarettes were made as described below.

Cigarettes were made by the method of manufacturing cigarettes Mild Seven Super Lights (Japan Tobacco Inc.), and for each of them used manufactured flavor-bearing component of the cigarette.

In particular, cigarettes containing flavored shredded tobacco according to the invention were made using shredded tobacco brand Mild Seven Super Lights as a starting material, making flavored shredded tobacco according to the invention and using it together with various materials (cigarette paper, filter, etc. ) that make up the Mild Seven Super Lights cigarettes.

Cigarettes containing flavored tobacco sheet according to the invention were made by mixing ground tobacco (85 parts by weight) for the manufacture of Mild Seven Super Lights cigarettes and flavored tobacco sheet according to the invention (15 parts by weight) and using this mixture in a predetermined quantity for filling cigarettes together with various the materials (cigarette paper, filter, etc.) that make up Mild Seven Super Lights cigarettes.

Cigarettes containing flavored cigarette paper of the invention were made by replacing cigarette paper of Mild Seven Super Lights cigarettes with flavored cigarette paper of the invention. Cigarettes were made in such a way that osmolability was as uniform as possible.

The smoking experiment was carried out under standard smoking conditions that the ISO standard provides (puff duration was 2 seconds with intervals between puffs of 58 seconds for one minute, puff volume was 35 ml, and the length of the cigarette butt was 35 mm (at 3 mm from rim paper).

The smoke collected in the Cambridge filter was extracted as described above, and the menthol content of the smoke inhaled by the smoker was measured as described above.

7. Results (ground tobacco)

In the case of ground tobacco, using the experimental methods described above, the following results were obtained.

7-1. The ability to preserve the menthol flavor after aging (evaluation in the case of using crushed tobacco)

Using the “flavored shredded tobacco 1-3 according to the invention” and the “shredded tobacco control sample” made as described above, the ability to maintain menthol flavor in shredded tobacco after aging was evaluated. The results are shown in FIG. one.

The crushed tobacco was kept for a predetermined period (0 days, 7 days, 14 days or 30 days) under harsh conditions. The menthol content in the ground tobacco was measured by performing a GC-FID assay as described above. In FIG. 1 the results of flavored crushed tobacco 1 according to the invention, the results of flavored crushed tobacco 2 according to the invention, the results of flavored crushed tobacco 3 according to the invention and the results of the control sample, respectively, are presented as "Carrageenan", "Gellan gum", "Gellan gum + tamarind gum" and "Control sample." The menthol content (wt.%) Was calculated by the formula: {measured value of the menthol content (mg) / mass of ground tobacco (mg)} × 100.

The control sample had a menthol content of approximately 0.7 weight. %, at the time of the beginning of storage (day 0). When the control sample was kept in a thermostat at a temperature of 50 ° C, the menthol content tended to decrease significantly over time.

On the other hand, flavored shredded tobacco 1-3 according to the invention had a menthol content of 1.2 to 1.5 weight. % at the time of the beginning of storage (day 0), and showed good ability to preserve the aroma for at least one month even after aging at 50 ° C in harsh conditions.

7-2. The ability to preserve the menthol flavor after aging (evaluation in the case of a cigarette)

Using cigarettes containing “flavored ground tobacco 1-3 according to the invention” and control cigarettes containing a “control ground tobacco sample”, the ability to maintain menthol flavor in cigarettes after aging was evaluated. The results are shown in FIG. 2.

The crushed tobacco was kept for a predetermined period (0 days, 7 days, 14 days or 30 days) under severe conditions as described above, and then cigarettes were made using crushed tobacco. A smoking experiment was carried out using cigarettes. The menthol content in the smoke inhaled by the smoker was measured using a GC-FID test as described above.

In FIG. 2 the results of a cigarette containing flavored ground tobacco 1 according to the invention, the results of a cigarette containing flavored ground tobacco 2 according to the invention, the results of a cigarette containing flavored ground tobacco 3 according to the invention, and the results of a cigarette containing a control sample are respectively represented as “Carrageenan”, “Gellan gum”, “Gellan gum + tamarind gum” and “Control sample”. In FIG. 2, the menthol content in smoker's inhaled smoke [mg / cigarette] represents the measured amount of menthol (mg) per cigarette.

A cigarette containing a control sample of shredded tobacco shows a high menthol content in the smoke inhaled by the smoker when grinded tobacco aged for 0 days was used, but the amount of menthol was significantly reduced when grinded tobacco kept for 7 days was used.

On the other hand, it was observed that cigarettes containing flavored shredded tobacco 1-3 according to the invention showed good flavor retention for at least one month, even if shredded tobacco was used which was kept at 50 ° C. under severe conditions.

7-3. The uniformity of the menthol content in the mixture

In the case of 10 cigarettes containing flavored ground tobacco according to the invention, the degree of variability of the content of the flavoring mixture among cigarettes was investigated. In addition, the cigarette rod containing the flavored ground tobacco of the invention was divided into three parts, and the degree of variability of the content of the flavoring mixture among these parts was also examined. The results are presented in table 1, in which the first parameter is presented as “Variability between cigarettes”, and the second parameter is presented as “Variability in the composition of the cigarette”. “Variability in cigarette composition (CV%)” is the average of 10 cigarettes.

In the case of a control sample, a cigarette sample was made by mixing 2 weight. % milled particles of a menthol-containing sheet (international patent application WO 2009/142159) instead of the flavored milled tobacco of the invention, with milled tobacco, and making the osmolability uniform. The menthol content in the smoker's inhaled smoke of this sample of cigarette was 0.4 mg per cigarette, which was almost equal to the result obtained in the case of a cigarette using the flavored ground tobacco of the invention.

Table 1 Shredded tobacco Variability between cigarettes [CV%] Variability in cigarette composition [CV%] Control sample (ground particles of menthol-coated sheet) 34% 54% Flavored shredded tobacco 1 according to the invention fourteen% fifteen% Flavored shredded tobacco 2 according to the invention fourteen% fourteen% Flavored shredded tobacco 3 according to the invention 13% fifteen%

In the case where the menthol-containing sheet was crushed to obtain the same shape as crushed tobacco and the resulting crushed sheet was mixed with crushed tobacco, the variability between cigarettes (CV%) was 34% and the variability in the composition of the cigarette was 54%. This variability was caused by a low content in the mixture of menthol-containing sheet, and if the content in the mixture of menthol-containing sheet was 10 weight. % or more, variability (CV%) is reduced to approximately 10%. On the other hand, when a cigarette was made using the flavored shredded tobacco of the invention, both the variability between the cigarettes and the variability in the composition of the cigarette were significantly reduced compared to the results for the control sample.

Based on these results, it was found that in the case of a cigarette containing flavored shredded tobacco according to the invention, it is possible to better suppress the variability of the menthol mixture between cigarettes and distribute menthol more evenly in the cigarette rod than in the case of a cigarette obtained by mixing the ground particles containing menthol leaf as a tobacco filler. In the case of a cigarette containing flavored ground tobacco according to the invention, accordingly, it is possible to suppress the variability of aroma and taste during smoking for each cigarette, as well as the variability of aroma and taste during smoking during the smoking time of the cigarette. In addition, according to the invention, the aroma composition is applied to a commonly used component of a cigarette, and thus, the production of cigarettes can be easily carried out at existing enterprises.

8. Results (leaf tobacco)

In the case of leaf tobacco, using the experimental methods described above, the following results were obtained.

8-1. The ability to preserve the menthol flavor after aging (evaluation in the case of leaf tobacco)

The use of “flavored tobacco sheet 1-3 according to the invention” and “control sample of tobacco leaf” made as described above, evaluated the ability of menthol flavoring in tobacco leaf after aging. The results are shown in FIG. 3.

Leaf tobacco was aged for a predetermined period (0 days, 7 days, 14 days or 30 days) under harsh conditions. The menthol content of leaf tobacco was measured by performing a GC-FID assay as described above. In FIG. 3, the results of flavored tobacco leaf 1 according to the invention, the results of flavored tobacco leaf 2 according to the invention, the results of flavored tobacco leaf 3 according to the invention and the results of the control sample, respectively, are presented as "Carrageenan", "Gellan gum", "Gellan gum + tamarind gum" and "Control sample." The menthol content (wt.%) Was calculated by the formula: {measured menthol content (mg) / leaf tobacco weight (mg)} × 100.

The control sample had a menthol content of approximately 3 weight. %, at the time of the beginning of storage (day 0). When the control sample was kept in a thermostat at a temperature of 50 ° C, the menthol content significantly decreased over time and reached almost zero level after the end of a week.

On the other hand, the flavored tobacco sheet 1-3 according to the invention had a menthol content of about 5 to 7 weight. % at the time of the beginning of storage (day 0), and showed a relatively high menthol content even after aging at 50 ° C in harsh conditions; those. good aroma retention ability was observed.

8-2. The ability to preserve the menthol flavor after aging (evaluation in the case of a cigarette)

Using cigarettes containing “flavored tobacco sheet 1-3 according to the invention” and control cigarettes containing a “control sheet tobacco sample”, the ability to maintain menthol flavor in cigarettes after aging was evaluated. The results are shown in FIG. four.

Leaf tobacco was aged for a predetermined period (0 days, 7 days, 14 days or 30 days) under stringent conditions as described above, and then cigarettes using this sheet tobacco. The menthol content in the smoke inhaled by the smoker was measured using a GC-FID test as described above.

In FIG. 4 the results of a cigarette containing flavored tobacco sheet 1 according to the invention, the results of a cigarette containing flavored tobacco sheet 2 according to the invention, the results of a cigarette containing flavored tobacco sheet 3 according to the invention, and the results of a cigarette containing a control sample, respectively, are presented as "Carrageenan", “Gellan gum”, “Gellan gum + tamarind gum” and “Control sample”. In FIG. 4, the menthol content in smoker's inhaled smoke [mg / cigarette] represents the measured amount of menthol (mg) per cigarette.

A cigarette containing a control sample of leaf tobacco exhibits a menthol content in the smoke inhaled by the smoker, which is the same as in the case of a cigarette containing flavored leaf tobacco according to the invention, when leaf tobacco aged for 0 days was used, but the amount of menthol was almost zero when used tobacco leaf aged for 7 days.

On the other hand, samples of cigarettes containing flavored tobacco sheet 1-3 showed a relatively large amount of menthol in the smoke inhaled by the smoker, and good aroma retention ability was observed even if tobacco leaf which was kept at 50 ° C. under severe conditions was used.

8-3. The uniformity of the menthol content in the mixture

In the case of 10 cigarettes containing flavored tobacco leaf according to the invention, investigated the degree of variability of the content in the mixture of flavoring among cigarettes. In addition, the cigarette rod containing the flavored tobacco sheet of the invention was divided into three parts, and the degree of variability of the content of the flavoring mixture among these parts was also examined. The results are presented in table 2, in which the first parameter is presented as “Variability between cigarettes”, and the second parameter is presented as “Variability in the composition of the cigarette”. “Variability in cigarette composition (CV%)” is the average of 10 cigarettes.

In the case of a control sample, a cigarette sample was made by mixing 2 weight. % milled particles of a menthol-containing sheet (international patent application WO 2009/142159) with milled tobacco, and making the osmolability uniform, in the same way as when using flavored milled tobacco, as described above.

table 2 Leaf tobacco Variability between cigarettes [CV%] Variability in cigarette composition [CV%] Control sample (ground particles of menthol-coated sheet) 34% 54% Flavored tobacco leaf 1 according to the invention fifteen% fifteen% Flavored tobacco leaf 2 according to the invention fifteen% 16% Flavored tobacco sheet 3 according to the invention fourteen% 16%

In the case where the menthol-containing sheet was crushed to obtain the same shape as crushed tobacco and the resulting crushed sheet (2 wt.%) Was mixed with crushed tobacco, the variability between cigarettes (CV%) was 34%, and the variability in the composition of the cigarette accounted for 54%. On the other hand, when a cigarette was made using flavored tobacco sheet according to the invention (the content in the mixture was 15% by weight relative to the total), both the variability between the cigarettes and the variability in the composition of the cigarette were significantly reduced compared to the results for the control sample.

Based on these results, it was found that in the case of a cigarette containing flavored tobacco leaf according to the invention, it is possible to better suppress the variability of the menthol mixture between cigarettes and to distribute menthol more evenly in the cigarette rod than in the case of a cigarette obtained by mixing ground menthol particles leaf as a tobacco filler. A cigarette containing flavored tobacco sheet according to the invention, respectively, can suppress the variability of aroma and taste during smoking for each cigarette and the variability of aroma and taste during smoking during the smoking time of the cigarette.

9. Results (cigarette paper)

In the case of cigarette paper, using the experimental methods described above, the following results were obtained.

9-1. The ability to preserve the menthol flavor after aging (evaluation in the case of cigarette paper)

Using the “flavored cigarette paper 1-3 of the invention” and the “control sample of cigarette paper” made as described above, the ability to maintain menthol flavor in cigarette paper after aging was evaluated. The results are shown in FIG. 5.

The cigarette paper was aged for a predetermined period (0 days, 7 days, 14 days or 30 days) under harsh conditions. The menthol content in the cigarette paper was measured by performing a GC-FID assay as described above. In FIG. 5 the results of flavored cigarette paper 1 according to the invention, the results of flavored cigarette paper 2 according to the invention, the results of flavored cigarette paper 3 according to the invention, and the results of the control sample, respectively, are presented as "Carrageenan", "Gellan gum", "Gellan gum + tamarind gum" and “Control sample”. The menthol content (wt.%) Was calculated by the formula: {measured value of the menthol content (mg) / weight of cigarette paper (mg)} × 100. The control sample had a menthol content of approximately 0.7 weight. %, at the time of the beginning of storage (day 0). When the control sample was kept in a thermostat at a temperature of 50 ° C, the menthol content significantly decreased over time and reached almost zero level after the end of a week.

Flavored cigarette paper 1-3 of the invention, on the other hand, had a menthol content of about 1.4 to 1.7 weight. %, at the time of the beginning of storage (day 0), and showed a relatively high menthol content even after aging at 50 ° C in harsh conditions; those. good aroma retention ability was observed.

9-2. The ability to preserve the menthol flavor after aging (evaluation in the case of a cigarette)

Using cigarettes containing a “flavored cigarette paper 1-3 according to the invention” and control cigarettes containing a “control cigarette paper sample”, the ability to maintain menthol flavor in a cigarette after aging was evaluated. The results are shown in FIG. 6.

The cigarette paper was aged for a predetermined period (0 days, 7 days, 14 days or 30 days) under stringent conditions as described above, and then cigarettes were made using cigarette paper as described above. The menthol content in the smoke inhaled by the smoker was measured using a GC-FID test as described above.

In FIG. 6 the results of a cigarette containing flavored cigarette paper 1 according to the invention, the results of a cigarette containing flavored cigarette paper 2 according to the invention, the results of a cigarette containing flavored cigarette paper 3 according to the invention, and the results of a cigarette containing a control sample, respectively, are presented as "Carrageenan", “Gellan gum”, “Gellan gum + tamarind gum” and “Control sample”. In FIG. 6, the menthol content in smoker's inhaled smoke [mg / cigarette] represents the measured amount of menthol (mg) per cigarette.

A cigarette containing a control sample of cigarette paper showed a menthol content in the smoke inhaled by the smoker that corresponds to the level of a cigarette containing flavored cigarette paper of the invention when using cigarette paper aged for 0 days, but the amount of menthol was almost zero when using cigarette paper aged for 7 days.

On the other hand, cigarettes containing flavored cigarette paper 1–3 showed a relatively large amount of menthol in the smoke inhaled by the smoker, and they showed good flavor retention even if cigarette paper was used which was kept at 50 ° C. under harsh conditions.

9-3. The uniformity of the menthol content in the mixture

In the case of 10 cigarettes containing flavored cigarette paper according to the invention, investigated the degree of variability of the content in the mixture of flavoring among cigarettes. In addition, the cigarette rod containing the flavored cigarette paper of the invention was divided into three parts, and the degree of variability of the content of the flavoring mixture among these parts was also examined. The results are presented in table 3, in which the first parameter is presented as “Variability between cigarettes”, and the second parameter is presented as “Variability in the composition of the cigarette”. “Variability in cigarette composition (CV%)” is the average of 10 cigarettes.

In the case of a control sample, a cigarette sample was made by mixing 2 weight. % milled particles of a menthol-containing sheet (international patent application WO 2009/142159) with milled tobacco, and making the osmolability uniform, in the same way as when using flavored milled tobacco, as described above.

Table 3 Cigarette paper Variability between cigarettes [CV%] Variability in cigarette composition [CV%] Control sample (ground particles of menthol-coated sheet) 34% 54% Flavored cigarette paper 1 according to the invention 9% 7% Flavored cigarette paper 2 according to the invention eleven% 10% Flavored cigarette paper 3 according to the invention 12% 9%

In the case where the menthol-containing sheet was crushed to obtain the same shape as crushed tobacco and the resulting crushed sheet (2 wt.%) Was mixed with crushed tobacco, the variability between cigarettes (CV%) was 34%, and the variability in the composition cigarettes accounted for 54%. On the other hand, when cigarettes were made using the flavored cigarette paper of the invention, both the variability between the cigarettes and the variability in the composition of the cigarette were significantly reduced compared to the results for the control sample.

Based on these results, it was found that in the case of a cigarette containing a flavored cigarette paper according to the invention, it is possible to better suppress the variability of the menthol mixture between cigarettes and to distribute menthol more evenly in a cigarette than in the case of a cigarette obtained by mixing crushed particles of menthol-containing sheet as a tobacco filler. In the case of cigarettes containing flavored cigarette paper according to the invention, accordingly, it is possible to suppress the variability of aroma and taste during smoking for each cigarette, as well as the variability of aroma and taste during smoking during the smoking time of the cigarette.

10. Temperature-dependent property of the sol-gel transition of a polysaccharide-containing liquid

In this experiment, the temperature-dependent property of the sol-gel transition was investigated for the following polysaccharide-containing liquids (suspensions) (1) - (3).

10-1. Preparation of Polysaccharide-Containing Fluid

(1) Carrageenan-containing liquid

Water 0.1 l.

Kappa-carrageenan (CARRAGEENAN CS-530 / San-Ei Gen F. F. I., Inc.) 5 g.

(2) Gellan Gum Liquid

Water 0.1 l.

Gellan gum (KELCOGEL / San-Ei Gen F. F. I., Inc.) 5 g.

Carrageenan-containing liquid and gellan gum-containing liquid were prepared as described below.

Water (0.1 L) was kept at 70 ° C, and the polysaccharide (5 g) was dissolved in water in small portions so that no lumps formed, while stirring using a high-speed DMM mixer manufactured by Atec Japan Ltd., and the resulting polysaccharide was obtained liquid (suspension).

(3) Liquid containing gellan gum and tamarind gum

Water 10 l.

Gellan Gum (KELCOGEL / San-Ei Gen F. F. I., Inc.) 250 g.

Tamarind gum (VIS TOP D-2032 / San-Ei Gen F. F. I., Inc.) 250 g.

Aqueous solution of 5% lecithin (Sun Lecithin A-1 / Taiyo Kagaku Co., Ltd.) 200 ml.

Menthol (Takasago International Corporation) 2500

A liquid containing gellan gum and tamarind gum was made as described below.

In 10 l (100 parts by weight) of water, which was heated and maintained at 80 ° C, while stirring in a mixer of the PRIMIX TK AUTO MIXER 40 model equipped with a stirring solution rotor at 2000 rpm), 500 g (5 parts by weight) of a mixture of two polysaccharides (gellan gum and tamarind gum), the ratio (mass ratio) of which was described above, were dissolved in water in small portions so that no lumps formed (the required time was approximately 20 minutes). While maintaining the same temperature, 2500 g (25 parts by weight) of 1-menthol were added to the mixture. Instead of a mixer, a PRIMIX T. K. AUTO MIXER 40 model homogenizer was used, equipped with a rotor-stator head at 4000 rpm, and the mixture was emulsified for 10 minutes. Thereafter, 200 ml (2 parts by weight) of an aqueous solution of 5% lecithin was added to the mixture, and stirring was continued. Menthol was dispersed in a mixed aqueous solution of polysaccharides containing gellan gum and tamarind gum.

10-2. results

The temperature of the polysaccharide-containing liquid (70 ° C) was reduced to 25 ° C for approximately 900 seconds (0.05 ° C / s). After that, the temperature rose to 70 ° C for approximately 900 seconds. The nature of the change in viscosity (fluidity) of the polysaccharide-containing liquid as a function of the temperature change described above was measured using a RheoStress 1 rheometer manufactured by Thermo-Haake Ltd.

The results of the carrageenan-containing liquid are shown in FIG. 7A and 7B, the results of gellan gum-containing liquid are shown in FIG. 8A and 8B, and the results of a liquid containing gellan gum and tamarind gum are shown in FIG. 9A and 9B.

As shown in FIG. 7A, when the temperature of the liquid containing carrageenan was reduced to 25 ° C, the viscosity remained low until the temperature reached approximately 50 ° C, which represents the temperature of the sol-gel transition, but the viscosity rapidly increased at a temperature below the transition temperature (gelation) . As the temperature of the resulting gel increased, the gel hardly turned back into sol, even if the gel was heated to a higher temperature than the transition temperature, as shown in FIG. 7B. Thus, the state of the gel could be maintained. As shown in FIG. 8A, when the temperature of the gellan gum-containing liquid decreased to 25 ° C, the viscosity remained low until the temperature reached approximately 50 ° C (fluidity remained high), but the viscosity rapidly decreased at 40 ° C or lower temperature (gelation phenomenon) . As the temperature of the resulting gel increased, the gel hardly turned back to sol, even if the gel was heated to a temperature higher than the gelation temperature (40 ° C), as shown in FIG. 8B. Thus, the state of the gel could be maintained until the temperature became sufficiently high.

As shown in FIG. 9A, when the temperature of the liquid containing gellan gum and tamarind gum decreased to 25 ° C, the viscosity remained low until the temperature reached approximately 40 ° C, but the viscosity rapidly increased at 35 ° C or lower temperature (gelation phenomenon) . As the temperature of the resulting gel increased, the gel hardly turned back to sol, even if the gel was heated to a temperature higher than the gelation temperature (35 ° C), as shown in FIG. 9B. Thus, the state of the gel could be maintained until the temperature became sufficiently high.

Based on these results, it was found that upon a single cooling of the suspension containing the polysaccharide described above to cause gelation, the gel was hardly converted back to sol, even if the temperature then increased, and the state of the gel could be maintained. Using this property of the polysaccharide according to the invention, the suspension of the starting material was subjected to preliminary cooling before it was dried. As a result of this, it is difficult to initiate the formation of a polysaccharide sol contained in the suspension of the starting material, which was subjected to preliminary cooling, even if the temperature of the suspension increased during drying, and thus, the evaporation of menthol coated with such a polysaccharide is difficult.

Claims (7)

1. The aromatic component of a cigarette obtained by:
applying the aromatic composition in a sol state to the surface of the cigarette component, the aromatic composition comprising a flavoring agent, water and a polysaccharide selected from the group consisting of carrageenan, gellan gum and a combination of gellan gum and tamarind gum; then
cooling the aroma composition component of the cigarette to a temperature of 0 to 40 ° C. to cause gelation of the aroma composition; and then
drying by heating the aroma-containing component of the cigarette. 2. The flavor component of the cigarette according to claim 1, wherein the drying by heating is performed so that the surface temperature of the aromatic composition is maintained in the range from 70 to 100 ° C. 3. The flavor component of a cigarette according to claim 1 or 2, which is a cigarette paper. 4. The flavor component of a cigarette according to claim 1 or 2, which is a tobacco filler. 5. The flavor component of the cigarette according to claim 4, wherein the tobacco filler is ground tobacco. 6. The flavor component of a cigarette according to claim 4, wherein the tobacco filler is leaf tobacco. 7. A cigarette containing an aromatic component of a cigarette according to any one of paragraphs. 1-6.

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