CN104010526B - Manufacture method containing enhanced ester fragrance component and the tobacco-containing material for contributing to the fragrant composition for inhaling taste and the tobacco product containing the tobacco-containing material manufactured by this method - Google Patents

Manufacture method containing enhanced ester fragrance component and the tobacco-containing material for contributing to the fragrant composition for inhaling taste and the tobacco product containing the tobacco-containing material manufactured by this method Download PDF

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Publication number
CN104010526B
CN104010526B CN201180075975.5A CN201180075975A CN104010526B CN 104010526 B CN104010526 B CN 104010526B CN 201180075975 A CN201180075975 A CN 201180075975A CN 104010526 B CN104010526 B CN 104010526B
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China
Prior art keywords
tobacco
pipe tobacco
ester
acid
curing
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CN104010526A (en
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伊藤研儿
佐藤慎介
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Japan Tobacco Inc
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Japan Tobacco Inc
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    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B3/00Preparing tobacco in the factory
    • A24B3/12Steaming, curing, or flavouring tobacco
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/18Treatment of tobacco products or tobacco substitutes
    • A24B15/28Treatment of tobacco products or tobacco substitutes by chemical substances
    • A24B15/30Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances

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  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacture Of Tobacco Products (AREA)

Abstract

The present invention provides a kind of manufacture method of tobacco-containing material and the tobacco product containing the tobacco-containing material manufactured by methods described, and the manufacture method of the tobacco-containing material includes following process:By the pipe tobacco before the manufacture for tobacco product in air atmosphere and the process that is cured in confined conditions;With the process that polyalcohol is added into the pipe tobacco after the curing step.

Description

Tobacco-containing material containing enhanced ester fragrance component and the composition for contributing to fragrant suction taste Manufacture method and the tobacco product containing the tobacco-containing material manufactured by this method
Technical field
The present invention relates to a kind of system containing enhanced ester fragrance component and the tobacco-containing material for contributing to the fragrant composition for inhaling taste Make method and the tobacco product containing the tobacco-containing material manufactured by this method.
Background technology
Tobacco Leaf after cultivation, harvest passes through the drying process of farmers', the 1 year length to the several years afterwards in raw material factory After phase curing step and the then various working processes such as mixing and chopping in manufacturing works, for tobacco products such as cigarettes Manufacture.After above-mentioned various processing operations, the flaw of Tobacco Leaf can be removed, as the tobacco for giving off a strong fragrance Raw material.Ethanol is added in order to further improve fragrant inhale in taste, the Tobacco Leaf before curing step into raw material factory, then, Common curing step is carried out in bucket, thus improves the fragrant of Tobacco Leaf and inhales taste (patent document 1).This method is the fragrant suction taste of improvement During using curing, therefore the time is longer.In addition, this method due to be manufacture tobacco product before, by Tobacco Leaf for Further working process, therefore, during further working process, contribute to tobacco the fragrant composition for inhaling taste composition because Volatilization of fragrance component etc. and change.
Prior art literature
Patent document
Patent document 1:Japanese Unexamined Patent Application 56-51976 publications
The content of the invention
Invent problem to be solved
In view of the foregoing, it is an object of the present invention to provide a kind of manufacture in a short time and easily enhanced ester The method that the composition of fragrance component and the enhanced composition for contributing to tobacco perfume to inhale taste is not susceptible to the tobacco-containing material of rheological parameters' change with time. In addition, a kind of it is an object of the present invention to provide tobacco product containing the tobacco-containing material manufactured by this method.
The method solved the problems, such as
The present inventor etc. has found, by the pipe tobacco before the manufacture for tobacco product in air atmosphere and in airtight condition It is lower when being cured, the ester fragrance component of pipe tobacco can be strengthened, and when adding polyalcohol into pipe tobacco, ester fragrance component can be suppressed Further generation, thus, the rheological parameters' change with time of the composition of the ester fragrance component of pipe tobacco can be suppressed.And then, the present inventor etc. has found, By changing the treatment conditions of above-mentioned curing, in addition to ester fragrance component, it also can control oxidation product, products of sugar decomposition etc. and help The composition of the composition of taste is inhaled in tobacco perfume, can be manufactured with various fragrant tobacco-containing material for inhaling taste feature, so as to complete this hair It is bright.
I.e., according to the first aspect of the invention, it is possible to provide a kind of manufacture method of tobacco-containing material, it is characterised in that include Following process:By the pipe tobacco before the manufacture for tobacco product in air atmosphere and the work that is cured in confined conditions Sequence;The process that polyalcohol is added into the pipe tobacco after the curing step.
In addition, according to the second aspect of the invention, it is possible to provide a kind of containing the tobacco-containing material manufactured by methods described Tobacco product.
Invention effect
According to the present invention, it is possible to provide a kind of to manufacture in a short time and easily enhanced ester fragrance component and contribute to perfume (or spice) The method that the composition of the composition of suction taste is difficult the tobacco-containing material of rheological parameters' change with time.
Brief description of the drawings
Figure 1A is to represent to make the figure (embodiment 2) of pipe tobacco growing amount of short chain fatty acids methyl esters when various temperature are cured;
Figure 1B is to represent to make the figure (embodiment 2) of pipe tobacco growing amount of aromatic ester when various temperature are cured;
Fig. 2A is to represent to make pipe tobacco in the ethyl crotonate (ethyl in the presence of ethanol and when various temperature are cured Crotonate the figure of growing amount);
Fig. 2 B are to represent to make pipe tobacco in the ethyl palmitate (ethyl in the presence of ethanol and when various temperature are cured Palmitate the figure of growing amount);
Fig. 2 C are to represent to make pipe tobacco in the formic acid menthyl ester in the presence of menthol and when various temperature are cured The figure of the growing amount of (menthyl formate);
Fig. 2 D are to represent to make pipe tobacco in the menthyl acetate in the presence of menthol and when various temperature are cured The figure of the growing amount of (menthyl acetate);
Fig. 2 E are to represent to make pipe tobacco in the isovaleric acid menthyl ester in the presence of menthol and when various temperature are cured The figure of the growing amount of (menthyl isovalerate);
Fig. 2 F are to represent to make pipe tobacco in the menthones (menthone) in the presence of menthol and when various temperature are cured Growing amount figure;
Fig. 2 G are to represent to make pipe tobacco in the benzaldehyde in the presence of phenmethylol and when various temperature are cured (benzaldehyde) figure of growing amount;
Fig. 2 H are the figures of the growing amount for the furfural (furfural) for representing to make pipe tobacco when various temperature are cured;
Fig. 2 I are the figures of the growing amount for the maltol (maltol) for representing to make pipe tobacco when various temperature are cured;
Fig. 2 J are the growing amounts for the methylpyrazine (methylpyrazine) for representing to make pipe tobacco when various temperature are cured Figure;
Fig. 3 A are to represent to make pipe tobacco in the ethyl crotonate in the presence of ethanol and when being cured during various curings The figure of the growing amount of (ethyl crotonate);
Fig. 3 B are to represent to make pipe tobacco in the ethyl palmitate in the presence of ethanol and when being cured during various curings The figure of the growing amount of (ethyl palmitate);
Fig. 3 C are to represent to make pipe tobacco in the formic acid peppermint in the presence of menthol and when being cured during various curings The figure of the growing amount of ester (menthyl formate);
Fig. 3 D are to represent to make pipe tobacco in the acetic acid peppermint in the presence of menthol and when being cured during various curings The figure of the growing amount of ester (menthyl acetate);
Fig. 3 E are to represent to make pipe tobacco thin in the isovaleric acid in the presence of menthol and when being cured during various curings The figure of the growing amount of lotus ester (menthyl isovalerate);
Fig. 4 A are to represent to make ethyl palmitate (ethyl of the pipe tobacco with various pH when curing in the presence of ethanol Palmitate the figure of growing amount);
Fig. 4 B are to represent to make ethyl linoleate (ethyl of the pipe tobacco with various pH when curing in the presence of ethanol Linoleate the figure of growing amount);
Fig. 4 C are to represent to make formic acid menthyl ester of the pipe tobacco with various pH when curing in the presence of menthol The figure of the growing amount of (menthyl formate);
Fig. 4 D are to represent to make menthyl acetate of the pipe tobacco with various pH when curing in the presence of menthol The figure of the growing amount of (menthyl acetate);
Fig. 4 E are to represent to make isovaleric acid menthyl ester of the pipe tobacco with various pH when curing in the presence of menthol The figure of the growing amount of (menthyl isovalerate);
Fig. 4 F are to represent to make menthones (menthone) of the pipe tobacco with various pH when curing in the presence of menthol Growing amount figure;
Fig. 4 G are to represent to make benzaldehyde of the pipe tobacco with various pH when curing in the presence of phenmethylol (benzaldehyde) figure of growing amount;
Fig. 4 H are the figures of the growing amount of the phytol (phytol) when representing to make the pipe tobacco curing with various pH;
Fig. 4 I are the figures of the growing amount of the furfural (furfural) when representing to make the pipe tobacco curing with various pH;
Fig. 4 J are the figures of the growing amount of the maltol (maltol) when representing to make the pipe tobacco curing with various pH;
Fig. 4 K are the growing amounts of the methylpyrazine (methylpyrazine) when representing to make the pipe tobacco curing with various pH Figure;
Fig. 5 A are to represent to make to the addition of palmitic acid second of the pipe tobacco of water when curing in the presence of ethanol with various additions The figure of the growing amount of ester (ethyl palmitate);
Fig. 5 B are to represent to make to the addition of linoleic acid second of the pipe tobacco of water when curing in the presence of ethanol with various additions The figure of the growing amount of ester (ethyl linoleate);
Fig. 5 C be represent to make to the addition of formic acid of the pipe tobacco of water when curing in the presence of menthol with various additions it is thin The figure of the growing amount of lotus ester (menthyl formate);
Fig. 5 D be represent to make to the addition of acetic acid of the pipe tobacco of water when curing in the presence of menthol with various additions it is thin The figure of the growing amount of lotus ester (menthyl acetate);
Fig. 5 E are to represent to make to the addition of isovaleric acid of the pipe tobacco of water when curing in the presence of menthol with various additions The figure of the growing amount of menthyl ester (menthyl isovalerate);
Fig. 6 A are to represent to make ethyl palmitate (ethyl of the pipe tobacco when curing in the presence of the ethanol of various concentration Palmitate the figure of growing amount);
Fig. 6 B are to represent to make ethyl linoleate (ethyl of the pipe tobacco when curing in the presence of the ethanol of various concentration Linoleate the figure of growing amount);
Fig. 6 C are to represent to make formic acid menthyl ester (menthyl of the pipe tobacco when curing in the presence of the menthol of various concentration Formate the figure of growing amount);
Fig. 6 D are to represent to make menthyl acetate (menthyl of the pipe tobacco when curing in the presence of the menthol of various concentration Acetate the figure of growing amount);
Fig. 7 A are the figures for representing polyalcohol to the inhibition of the generation of ethyl palmitate (ethyl palmitate);
Fig. 7 B are the figures for representing polyalcohol to the inhibition of the generation of ethyl stearte (ethyl stearate);
Fig. 7 C are the figures for representing polyalcohol to the inhibition of the generation of ethyl linoleate (ethyl linoleate);
Fig. 7 D are the figures for representing polyalcohol to the inhibition of the generation of ethyl linolenate (ethyl linolenate);
Fig. 7 E are the figures for representing polyalcohol to the inhibition of the generation of formic acid menthyl ester (menthyl formate);
Fig. 7 F are the figures for representing polyalcohol to the inhibition of the generation of menthyl acetate (menthyl acetate);
Fig. 7 G are the inhibitions for representing polyalcohol to the generation of isovaleric acid menthyl ester (menthyl isovalerate) Figure;
Fig. 7 H are the figures for representing polyalcohol to the inhibition of the generation of ethyl valerate (ethyl valerate);
Fig. 7 I are to represent that polyalcohol aligns the figure of the inhibition of the generation of ethyl hexanoate (ethyl n-hexanoate);
Fig. 7 J are the figures for representing polyalcohol to the inhibition of the generation of ethyl crotonate (ethyl crotonate);
Fig. 7 K are the figures for representing polyalcohol to the inhibition of the generation of methyl acetate (methyl acetate);
Fig. 7 L are the figures for representing polyalcohol to the inhibition of the generation of benzyl acetate (benzyl acetate);
Fig. 7 M are the inhibitions for representing polyalcohol to the generation of phenethyl acetate (phenylethyl acetate) Figure;
Fig. 8 A are the figures for representing polyalcohol to the inhibition of the generation of ethyl palmitate (ethyl palmitate);
Fig. 8 B are the figures for representing polyalcohol to the inhibition of the generation of ethyl stearte (ethyl stearate);
Fig. 8 C are the figures for representing polyalcohol to the inhibition of the generation of ethyl linoleate (ethyl linoleate);
Fig. 8 D are the figures for representing polyalcohol to the inhibition of the generation of ethyl linolenate (ethyl linolenate);
Fig. 8 E are the figures for representing polyalcohol to the inhibition of the generation of formic acid menthyl ester (menthyl formate);
Fig. 8 F are the figures for representing polyalcohol to the inhibition of the generation of menthyl acetate (menthyl acetate);
Fig. 8 G are the inhibitions for representing polyalcohol to the generation of isovaleric acid menthyl ester (menthyl isovalerate) Figure;
Fig. 8 H are the figures for representing polyalcohol to the inhibition of the generation of ethyl valerate (ethyl valerate);
Fig. 8 I are to represent that polyalcohol aligns the figure of the inhibition of the generation of ethyl hexanoate (ethyl n-hexanoate);
Fig. 8 J are the figures for representing polyalcohol to the inhibition of the generation of ethyl crotonate (ethyl crotonate);
Fig. 8 K are the figures for representing polyalcohol to the inhibition of the generation of benzyl acetate (benzyl acetate);
Fig. 8 L are the inhibitions for representing polyalcohol to the generation of phenethyl acetate (phenylethyl acetate) Figure;
Fig. 9 is the SPME-GCMS spectrum for representing to add various alcohol and the pipe tobacco in 40 DEG C of curings 1 week in yellow kind pipe tobacco Figure;
Figure 10 is the SPME- for representing to add various acid and ethanol and the pipe tobacco in 40 DEG C of curings 1 week in yellow kind pipe tobacco GCMS spectrograms;
Figure 11 A are to represent to add various essential oils or extract spices in yellow kind pipe tobacco and in the cigarette of 40 DEG C of curings 1 week The dichloromethane extraction GCMS spectrograms of silk;
Figure 11 B are to represent to add various essential oils or extract spices in yellow kind pipe tobacco and in the cigarette of 40 DEG C of curings 1 week The SPME-GCMS spectrograms of silk;
Embodiment
Below, the present invention is described in detail, but following explanation does not limit the present invention.
The manufacture method of the tobacco-containing material of the present invention includes following process:By the pipe tobacco before the manufacture for tobacco product The process cured in air atmosphere and in confined conditions;The work of polyalcohol is added into the pipe tobacco after above-mentioned curing step Sequence.Composition generation ester fragrance component and contribute to the fragrant composition for inhaling taste that this method is had in curing step by pipe tobacco, By the addition polyalcohol after, ester fragrance component can be suppressed and contribute to the further generation of the fragrant composition for inhaling taste.Thus Enhanced ester fragrance component can be manufactured and contribute to the composition of the fragrant composition for inhaling taste to be not susceptible to the tobacco-containing material of rheological parameters' change with time.
In addition, according to preferred embodiment, the manufacture method of tobacco-containing material of the invention includes following process:Cigarette will be used for Pipe tobacco before the manufacture of straw-made articles in air atmosphere and in confined conditions, ester fragrance component or contribute to it is fragrant inhale taste into The process cured in the presence of the matrix (such as alcohol) divided;Polyalcohol is added into the pipe tobacco after above-mentioned curing step.Should Both compositions that method is had in curing step by alcohol and pipe tobacco generation particularly ester fragrance component, by being added after Polyalcohol, can suppress the further generation of ester fragrance component.Thus the composition that enhanced ester fragrance component can be manufactured is not susceptible to The tobacco-containing material of rheological parameters' change with time.
In this manual, tobacco it is fragrant inhale taste composition be expressed as respectively " ester fragrance component " and " ester fragrance component with Outer fragrant suction taste composition ".I.e., in this manual, it is expressed as " ester fragrance component and contributing to by the fragrant taste composition of inhaling of tobacco Perfume inhales the composition of taste " in the case of, " the contributing to the fragrant composition for inhaling taste " of the latter refer to " fragrant beyond ester fragrance component inhale taste into Point ", specifically, refer to by oxidation reaction obtain it is fragrant inhale taste composition and by aminocarbonyl reaction obtain it is fragrant inhale taste into Grade.
Pipe tobacco used in the present invention can use any kind, for example, can use yellow kind, burley tobaccos kind, Japan The stripped leaf and offal of cigarette kind and the green sheet again being made up of these raw materials." the cigarette being used for before the manufacture of tobacco product Silk " refers to drying process by farmers', afterwards at 1 year of raw material factory to the long-term curing step of several years and then in system The various working processes such as mixing and chopping in factory are made, the pipe tobacco of the preparation for manufacturing tobacco product has been carried out.In tobacco In the case that product is cigarette, " pipe tobacco being used for before the manufacture of tobacco product " is " cigarette before the cigarette working procedure of cigarette Silk ".In the case that pipe tobacco used in the present invention is stripped leaf, can generally have following size:With common thin slice Pipe tobacco meter pipe tobacco width is 0.6~1mm, and length is calculated as 25cm or so with maximum leaf size.In the following description, " it will use Pipe tobacco before the manufacture of tobacco product " is referred to as " pipe tobacco ".
In the present invention, in order to cure, pipe tobacco is placed in air atmosphere and under confined conditions.That is, pipe tobacco is put into In container with air-tightness, placed in the state of the surface of pipe tobacco and atmosphere.Closed container can be arbitrary appearance Amount, but the temperature preferably in controllable container.Pipe tobacco is due to requiring its surface and atmosphere, therefore, not preferably in container Pipe tobacco is pressurized from above by fill up.Pipe tobacco can be for example put into container with about 50~80% degree for accounting for container capacity.
As the cooking conditions of this method, temperature generally can be from the models of room temperature~70 DEG C (specifically 20~70 DEG C) Enclose middle selection (reference picture 1A~1B, 2A~2J).According to Figure 1A and Figure 1B result, with the rising of curing temperature, short chain fat The growing amount increase of fatty acid methyl esters and aromatic ester, therefore, curing temperature can generally be set to 20~70 DEG C, be preferably set to 30~70 DEG C, more preferably it is set to 40~70 DEG C.
Ester fragrance component and the endogenous enzymes for contributing to the fragrant composition for inhaling taste to have during curing by (i) using pipe tobacco The enzyme reaction (such as the back reaction of ester hydrolase) of progress and/or (ii) chemical reaction (for example by dehydration generate ester, Menthol oxide etc. is generated by oxidation reaction, furans, reductones, Pyrazine etc. are generated by aminocarbonyl reaction) To generate.
Therefore, wishing enhanced ester fragrance component and contributing to the fragrant composition for inhaling taste mainly to be generated by (i) enzyme reaction In the case of, temperature can be set to room temperature~50 DEG C (specifically 20~50 DEG C), on the other hand, wish that enhanced ester is fragrant In the case that gas composition and the composition for contributing to perfume to inhale taste are mainly generated by (ii) chemical reaction, temperature can be set to 60~70 ℃.Or, wish enhanced ester fragrance component and contribute to the fragrant composition for inhaling taste to be chemically reacted by (i) enzyme reaction and (ii) In the case of both generations, temperature can be set to room temperature~70 DEG C (specifically 20~70 DEG C).
, generally can be from 1 week~3 months, the scope of such as 1~15 week during curing as the cooking conditions of this method Select (reference picture 3A~3E).
As the cooking conditions of this method, the pH of pipe tobacco generally can between 2~8 arbitrarily setting (reference picture 4A~ 4K).According to Fig. 4 A~4E result, observed in the case where using the pipe tobacco of pH2~7 various ester compositions generation, with And the pipe tobacco used in the inventive method has the value of pH5~6 originally, it is contemplated that the above-mentioned fact, it is desirable that strengthening various esters In the case of fragrance component, regulation processing of the pipe tobacco without implementing pH can be used.In addition, according to Fig. 4 A~4E result, Also the generation of various ester compositions is observed in the case of pipe tobacco using pH2~3, particularly such as formic acid menthyl ester (Fig. 4 C), second Sour menthyl ester (Fig. 4 D) preferentially generates near pH2 like that.Therefore, in the case of it is desirable that strengthening various ester compositions, by inciting somebody to action The pH of pipe tobacco arbitrarily sets to cure between 2~8, can obtain the pipe tobacco of the composition with desired ester fragrance component.
In addition, according to Fig. 4 F~4K result, even in it is desirable that control oxidation reaction product (such as menthones, benzaldehyde Deng), the composition (phytol etc.) that is decomposed using acid, aminocarbonyl reaction product is (comprising reductones such as furans, the maltols such as furfural The Pyrazines such as class, methylpyrazine) etc. contribute to the composition of the fragrant composition for inhaling taste in the case of, the situation phase with ester fragrance component Together, also can by the way that by the pH of pipe tobacco, any setting be cured between 2~8, obtain contributing to desired fragrant suction taste into The pipe tobacco of the composition divided.
It should be noted that the present inventor etc. pass through after the pH and curing step of the pipe tobacco before experimental verification curing step The pH of pipe tobacco do not vary widely.I.e., in the method for the invention, the pH of pipe tobacco does not almost become during curing step Change.
As the cooking conditions of this method, the generation that moisture (humidification) fundamentally suppresses ester fragrance component is added to pipe tobacco, It is therefore preferable that adding water (reference picture 5A~5C) not in pipe tobacco.Pipe tobacco used in the method for the present invention is maintained originally 10~15 weight % moisture.But, if adding water in the pipe tobacco of burley tobaccos kind, menthyl acetate or isovaleric acid peppermint The generation increase (reference picture 5D and 5E) of the ester fragrance component of the short chain fatty acids such as ester.Therefore, (the i.e. moisture under necessary information Addition promote desired ester fragrance component and contribute to the situation of the generation of the fragrant composition for inhaling taste), can also add in pipe tobacco Add water point.Now, moisture that generally can be in pipe tobacco adds moisture in the range of reaching 80 weight %.For example, moisture can be with It is added using the amount relative to pipe tobacco 1g as 0.2~1mL.The addition of moisture is preferably by spraying etc., tobacco manufacturing process Using conventional method by moisture spread all over pipe tobacco it is overall in the way of carry out.
As the cooking conditions of this method, preferably selected from the addition of at least one of alcohol, acid, essential oil and extract spices Cured in the presence of thing.Specifically, additive is added in the forward direction pipe tobacco of curing step.Alcohol, essential oil, extract are fragrant Material can also directly added stoste, can also added in the form of dilution, and acid can be added in the form of the solution containing acid Plus.By adding the additive, it is possible to increase ester fragrance component and contribute to the fragrant composition for inhaling taste matrix components amount, thus make The ester fragrance component of generation and amount increase or the increase species for contributing to the fragrant composition for inhaling taste.
As additive, it can use selected from ethanol, menthol, phenmethylol, isobutanol, n-butanol, isoamyl alcohol, n-hexyl alcohol Deng alcohol;The acid such as isobutyric acid, 3 Methylbutanoic acid, n-caproic acid, octanoic acid;And Rum, peppermint oil, spearmint oil, Japanese peppermint oil, fan Repeatedly at least one of the essential oil or extract spices such as sesame oil, licorice, carob tamarind legume extract, cocoa.Essential oil is carried It is natural goods spices to take thing spices, the matrix (such as alcohol and/or acid) containing ester fragrance component and the composition for contributing to fragrant suction taste. According to the species of these additives, different ester fragrance components and the composition for contributing to perfume to inhale taste can be increased.For example, by adding Plus ethanol, can increase various ethyl ester classes, specifically, ethyl acetate, ethyl crotonate, ethyl hexanoate, ethyl palmitate, Asia The ester of the aliphatic acid such as ethyl oleate and ethanol.Similarly, the alcohol of addition, acid and natural goods spices and cigarette containing them are passed through The combination of the acid, alcohol that contain originally in silk, can strengthen various ester fragrance components.
In addition, composition contained in these additives turns into oxidation, the matrix of aminocarbonyl reaction, as contributing to fragrant suction The composition of taste.For example, by oxidation, menthol, which turns into menthones, phenmethylol, turns into benzaldehyde, benzoic acid, make the fragrant suction of tobacco Taste changes.By aminocarbonyl reaction, contained glucose, fructose, maltose etc. turn into methyl cyclopentene in licorice Other aminocarbonyl reaction products such as alcohol ketone, furfuryl alcohol, maltol, change the fragrant taste of inhaling of tobacco.
In the present invention, the combination of several additives can also be used, such as ethanol and menthol, ethanol and butyric acid Combination.
Additive generally can using relative to pipe tobacco as below 10 weight %, be preferably 0.4~10 weight %, more preferably 1~10 weight %, more preferably 1~5 weight % amount are added., can be with phase in the case where adding several additives Each additive is added for the amount that pipe tobacco is below 10 weight %, preferably 1~10 weight %, more preferably 1~5 weight %. The addition of additive with the solution of additive or contains preferably by the conventional method sprayed etc. used in tobacco manufacturing process The solution of additive, which spreads all over the overall mode of pipe tobacco, to be carried out.For example, ethanol preferably using relative to pipe tobacco as 1~10 weight %, more Preferably 1~5 weight %, more preferably 2~4 weight % amount are added (reference picture 6A and 6B).Menthol is preferably with phase It is that 1~10 weight %, more preferably 4~10 weight % amount are added (reference picture 6C and 6D) for pipe tobacco.
Pipe tobacco contains formic acid, acetic acid, valeric acid, myristic acid, palmitic acid, stearic acid, oleic acid, linoleic acid, flax in leaf The aliphatic acid such as acid;The alcohol such as methanol, phenmethylol, benzyl carbinol.Therefore, in the method for the invention, even if not adding alcohol into pipe tobacco, Can also as the composition enhancing methyl acetate contained by pipe tobacco, benzyl acetate, phenethyl acetate, the ester fragrance such as methyl hexadecanoate into Divide and contribute to the fragrant composition for inhaling taste.
In the curing step of this method, in the case of above-mentioned additive is added into pipe tobacco, because additive can conduct Ester fragrance component and contribute to the matrix of the fragrant composition for inhaling taste to use, therefore, ester fragrance component can be further enhanced and contributed to Perfume inhales the composition of taste.
In preferred scheme, prepare more than 2 closed containers, it is under different conditions that pipe tobacco is ripe in each container Change, strengthen the ester fragrance component needed and contribute to the fragrant composition for inhaling taste, pipe blend, thus, can be manufactured a variety of after curing Ester fragrance component and the composition for contributing to perfume to inhale taste obtain enhanced tobacco-containing material.For example, using 2 closed containers, at one Grew tobacco relative to burley tobaccos the ethanol of leaf pipe tobacco addition 2% in closed container, using 20~50 DEG C of temperature and 1~2 week Implement the method for the present invention during curing, carry out the increasing of the main composition for contributing to fragrant suction taste centered on ester fragrance component By force.In another closed container, the temperature using 60~70 DEG C and the maturation period of 5~10 weeks relative to yellow kind tobacco leaf pipe tobacco Between implement the method for the present invention, mainly centered on oxidation product and aminocarbonyl reaction product enhancing contribute to it is fragrant inhale taste into Point.As described above, the ester fragrance component with different compositions can also be strengthened in each closed container and contribute to fragrant suction taste Composition, and mix the pipe tobacco that is obtained by each closed container.A variety of ester fragrance are enhanced with desired composition thus, it is possible to manufacture Composition and the tobacco-containing material for contributing to the fragrant composition for inhaling taste.
In the method for the invention, after curing step, polyalcohol is added into pipe tobacco.As polyalcohol, it can use Propane diols, glycerine or their mixture.Polyalcohol can be added using the amount relative to pipe tobacco as 0.1~5 weight %. It is overall that the addition of polyalcohol spreads all over pipe tobacco preferably by the conventional method used in the tobacco manufacturing processes such as spraying with polyalcohol Mode carry out.
In the past, based on the purpose of the moisture retention of pipe tobacco, fragrance protectiveness is ensured, polyalcohol (such as glycerine) is in pipe tobacco charging The stage of (addition of the first spices) makes an addition to the material of pipe tobacco, therefore, is had no problem in terms of applied to pipe tobacco.
Shown in embodiment as be described hereinafter, polyalcohol has the function for the generation for suppressing ester fragrance component.Therefore, by ripe Polyalcohol is added after chemical industry sequence, can suppress further to generate ester fragrance component, thus, the present invention has institute in curing step The composition of the ester fragrance component of generation is not susceptible to effect as rheological parameters' change with time.
Demonstrated in embodiment as be described hereinafter, method of the invention can change generated ester by changing cooking conditions Fragrance component and the composition for contributing to the fragrant composition for inhaling taste.Therefore, if those skilled in the art, then it may rely on hope The ester fragrance component of generation and the composition for contributing to perfume to inhale taste carry out suitable design cooking conditions.
Because the species according to tobacco material is different, the group for the content component (aliphatic acid, reduced sugar etc.) that pipe tobacco has Into difference, therefore, when the method by the present invention cures pipe tobacco, according to the species of tobacco material difference, ester fragrance component And contribute to the growing amount of the fragrant composition for inhaling taste than different.In view of these generation modes, by selecting the species of tobacco material simultaneously Cooking conditions changing the additive (such as alcohol) added, temperature, time, pH, moisture, can arbitrarily change ester fragrance component And contribute to the composition of the fragrant composition for inhaling taste.
In the method for the invention, as described above, multiple closed containers can also be used and multiple cooking conditions are used. That is, multiple closed containers (such as 2~3 closed containers) can also be prepared, each closed container is real using different cooking conditions The method for applying the present invention, strengthening each closed container has the ester fragrance component of different compositions and contributes to the fragrant composition for inhaling taste simultaneously Mix the pipe tobacco obtained by each closed container.By using multiple closed containers, ester fragrance component can be increased and contribute to perfume (or spice) Inhale the change of the composition of the composition of taste.
As described above, in the case where using a closed container or using in the case of multiple closed containers, by adopting Various cooking conditions are used, various ester fragrance components can be manufactured and contribute to the fragrant composition for inhaling taste to obtain enhanced tobacco material Material.For example it can be manufactured according to the method for the present invention from various ester fragrance components chosen below and contribute to the fragrant composition for inhaling taste Obtain enhanced tobacco-containing material.
1) esters
Short-chain aliphatic ester, such as ethyl crotonate, ethyl hexanoate
Long-chain fatty acid ester, such as ethyl palmitate, ethyl linoleate
Ethyl succinate
Short chain fatty acids menthyl ester, such as formic acid menthyl ester, menthyl acetate, isovaleric acid menthyl ester
Aromatic ester, such as benzyl acetate, phenethyl acetate
2) oxidation product
Menthones, isomenthone
Benzaldehyde, benzoic acid
3) aminocarbonyl reaction product
Furans, such as furfural, acetyl furan, furfuryl alcohol, 5 hydroxymethyl furfural
Reductones, such as methyl cyclopentenyl ketone, maltol, furanone
Pyrazine, such as pyrazine, methylpyrazine, dimethyl pyrazine
4) it is other
Duvatrienediol analyte, phytol analyte, damascenone.
Which kind of fragrant taste of inhaling above-mentioned ester fragrance component and the composition for contributing to perfume to inhale taste contribute to for those skilled in the art For be known, the ethyl hexanoate of such as esters has the style fragrance of flowers, contributes to the fragrance of cigarette, ethyl palmitate Effect with the stimulation for relaxing cigarette.There is salubrious peppermint sample fragrance as the menthones of oxidation product, amino carbonyl is used as The methyl cyclopentenyl ketone of base reaction product contributes to the stronger sweet taste of maple syrup sample, and dimethyl pyrazine helps to bake and bank up with earth sample Fragranced, fragrance.
To by the present invention method manufacture tobacco-containing material for, can as arbitrary tobacco product material, example It can such as be used as cigarette smoking product;It is used as the materials'use of the smokeless tobacco articles such as snuff, chewing tobacco.By this The tobacco-containing material of the method manufacture of invention can integrally be used as the tobacco-containing material in tobacco product, can also be used as tobacco product In the part of tobacco-containing material use.In the tobacco-containing material obtained by the present invention as one of the tobacco-containing material in tobacco product In the case of the use of part, it can be used with arbitrary ratio.
The tobacco-containing material obtained by the method for the present invention is due to the ester fragrance component generated in curing step and contributes to The composition that perfume inhales the composition of taste is difficult rheological parameters' change with time, therefore, in the case of for tobacco product, can feel what is enhanced Perfume inhales taste (with reference to embodiment 10 and 11 described later).
Embodiment
Embodiment 1:Ester fragrance component and the analysis for contributing to the fragrant composition for inhaling taste
Build simply analysis ester fragrance component and contribute to the method for the fragrant composition for inhaling taste.For simply obtaining pipe tobacco The purpose of the overall profile of content component, using band dichloromethane extraction-mass spectrometric gas chromatography (DCM-GCMS).Separately Outside, the analysis of the composition concentrated is needed less for being difficult by the low polarity, low quality or amount of this method detection, using band SPME-mass spectrometric gas chromatography (SPME-GCMS).
1-1. band dichloromethane extraction-mass spectrometric gas chromatography (DCM-GCMS)
Pipe tobacco 0.5g is accurately weighed in glass system screw socket bottle (20mL capacity), with the acetonitrile solution to bromophenethyl alcohol (1mg/mL) 25 μ L are as internal standard substance, and dichloromethane 10mL is as extractant and is capped for addition, at room temperature with 200rpm Oscillation extraction 60 minutes.By the supernatant with moving to GC bottles after 0.45 μm of film filter filtering, using with automatic sampler GCMS is analyzed.The ratio between obtained GC chromatography object component and the peak area to bromophenethyl alcohol are obtained, with obtained value Compare the amount of analysis object component contained in each tobacco sample.
<Analysis condition>
Device:Agilent company systems gas chromatographic analysis device (6890N)
Agilent company systems mass spectrograph (5973N)
Sample size:1 μ L (with pulse, shunt mode does not inject)
Post:Agilent company systems HP-INNOWAX (30m × 0.25mm (0.25 μm of thickness))
Column oven:40 DEG C → 260 DEG C (5 DEG C/min)
Mass spectrograph:TIC patterns (mass number 29~550)
<Analyze object component>
Esters:Methyl hexadecanoate, ethyl myristate, ethyl palmitate, ethyl stearte, ethyl oleate, linoleic acid second It is ester, ethyl linolenate, acetic acid (mono-, di-, three) glyceride, other
Oxidation product:It is the long chain fatty acids such as menthones, isomenthone, benzaldehyde, benzoic acid, palmitic acid, other
Aminocarbonyl reaction product:It is pyruvic alcohol, 3-hydroxy-2-butanone, acetyl pyrrole, HMF 5 hydroxymethyl 2 furaldehyde (5-HMF), other
It is other:Phytol, duvatrienediol, glycerine, propane diols etc..
1-2. band SPME-mass spectrometric gas chromatographies (SPME-GCMS)
Pipe tobacco 0.5g is accurately weighed in SPME bottles (20mL capacity), bottle cap is covered and is sealed, using band SPME certainly The GCMS of dynamic gatherer is analyzed.
In addition, to being added at another SPME bottles to the μ L of acetonitrile solution (1mg/mL) 25 of bromophenethyl alcohol sample similarly Analyzed, obtain analysis the ratio between object component and the peak area to bromophenethyl alcohol, in the hope of more each tobacco sample of value in The amount of contained analysis object component.Therefore, the present invention in determined analysis object component amount (Fig. 2A~2J, Fig. 3 A~ 3E, Fig. 4 A~4K, Fig. 5 A~5E, Fig. 6 A~Fig. 6 D, Fig. 7 A~7M, Fig. 8 A~8L longitudinal axis) represent relative amount.
<Analysis condition>
Device:Agilent company systems gas chromatographic analysis device (6890A)
CTC Analytics SPME automatic leading-in devices (Combi PAL)
Agilent company systems mass spectrograph (5973N)
Sample size:1 μ L (are injected) with pulse without shunt mode
Post:INNOWAX
Column oven:40 DEG C → 250 DEG C (3 DEG C/min)
Mass spectrograph:TIC patterns (mass number 29~550)
<Analyze object component>
Esters:(methyl acetate (C2-Me)), methyl isovalerate (isoC4-Me), methyl valerate (n-C4-Et), caproic acid first Ester (n-C6-Me), methyl phenylacetate, ethyl isovalerate, ethyl valerate, ethyl crotonate, ethyl hexanoate, cognac oil, octanoic acid Ethyl ester, ethyl pelargonate, ethyl caprate, formic acid menthyl ester, menthyl acetate, isovaleric acid menthyl ester, benzyl formate, formic acid benzene second It is ester, benzyl acetate, phenethyl acetate, other
Oxidation product:It is the short chain fatty acids such as acetic acid, benzaldehyde, benzoic acid, phenylacetic acid, other
Aminocarbonyl reaction product:Furfural, acetyl furan, 5 methyl furfural, 2- furancarbinols, methyl cyclopentene alcohol It is ketone, maltol, furanone, pyrazine, methylpyrazine, 2,5-dimethyl pyrazine, 2,6 dimethyl pyrazine, other.
Embodiment 2:The effect of curing temperature during in the absence of alcohol
2-1. curing
It will wind up closed container (glass scre-cap bottle -5mL) the inherent various temperature of the pipe tobacco 1g before process in controllable temperature It is lower to place 1 week.As pipe tobacco, any of yellow kind is produced using Brazil's production burley tobaccos kind or Brazil.As curing temperature, use 5℃、22℃、30℃、40℃、50℃、60℃、70℃.As control, the pipe tobacco for not carrying out maturation process is used.
2-2. analysis
Ester fragrance component is carried out by the method described in embodiment 1 and contributes to the analysis of the fragrant composition for inhaling taste.
2-3. result
The analysis result of short chain fatty acids methyl esters and aromatic ester is shown in Figure 1A and Figure 1B.In Figure 1A and Figure 1B In, left side is the analysis result of burley tobaccos kind, and right side is the analysis result of yellow kind.
In figure ia, C2-Me represents methyl acetate, and isoC4-Me represents methyl isovalerate, and n-C4-Me represents valeric acid first Ester, n-C6-Me represents methyl caproate.
According to Figure 1A result, the rising with temperature, the tendency of the growing amount increase of short chain fatty acids methyl esters are found. Under conditions of 50 DEG C and 60 DEG C, the growing amount of short chain fatty acids methyl esters is especially high.Burley tobaccos kind and yellow kind it is any in, C2-Me (methyl acetate) growing amount highest.In burley tobaccos kind, methyl isovalerate (isoC4-Me) is detected, but in yellow Do not detected in kind.
According to Figure 1B result, with the rising of temperature, particularly methyl phenylacetate (methyl phenylacetate) Growing amount increase.In burley tobaccos kind, confirm in addition to methyl phenylacetate, benzyl acetate (benzylacetate) and second Sour phenethyl ester (phenethylacetate) increases with the growing amount of the rising of temperature.In yellow kind, confirm except benzene second Beyond sour methyl esters, benzyl acetate (benzylacetate), phenyl ethyl formate (phenetylformate), phenethyl acetate (phenethylacetate) increase with the growing amount of the rising of temperature.
Embodiment 3:The effect of curing temperature when there is alcohol
3-1. curing step
It will wind up closed container (glass scre-cap bottle -5mL) the inherent various temperature of the pipe tobacco 1g before process in controllable temperature It is lower to place 1 week.As pipe tobacco, any of yellow kind is produced using Brazil's production burley tobaccos kind or Brazil.As curing temperature, adopt With -40 DEG C, 5 DEG C, 22 DEG C, 30 DEG C, 35 DEG C, 40 DEG C, 45 DEG C, 50 DEG C, 60 DEG C or 70 DEG C.
Before curing, weight of the addition relative to pipe tobacco is injected for 2 weight % ethanol and equivalent to 1 weight by syringe Measure menthol/ethanol solution of % menthol.
3-2. analysis
Ester fragrance component is carried out by the method described in embodiment 1 and contributes to the analysis of the fragrant composition for inhaling taste.
3-3. result
Analysis result is shown in Fig. 2A~2J.In figure, bullet represents burley tobaccos kind, and white round dot represents yellow kind.
According to Fig. 2A~2B result, ethyl crotonate is more than 50 DEG C, preferably more than 60 DEG C, more preferably 60~70 DEG C temperature show higher growing amount;Temperature of the ethyl palmitate more than 20 DEG C, preferably at 20~50 DEG C shows higher Growing amount.
According to Fig. 2 C~2E result, temperature of the formic acid menthyl ester more than 60 DEG C, preferably at 60~70 DEG C shows higher Growing amount;Temperature of the menthyl acetate more than 20 DEG C, preferably at 20~50 DEG C shows higher growing amount;Isovaleric acid peppermint Ester shows higher growing amount in 20~60 DEG C, the temperature preferably at 30~50 DEG C.
According to Fig. 2 F~2G result, temperature of the menthones more than 60 DEG C, preferably at 60~70 DEG C shows higher life Cheng Liang;Temperature of the benzaldehyde more than 20 DEG C, preferably more than 60 DEG C, more preferably at 60~70 DEG C shows higher growing amount.
According to Fig. 2 H~2J result, furfural, maltol and methylpyrazine are more than 60 DEG C, preferably at 60~70 DEG C Temperature shows higher growing amount.In addition, the pipe tobacco of yellow kind preferentially generates furans and reductones, and on the other hand, white rib The pipe tobacco of cigarette kind preferentially generates Pyrazine.
Embodiment 4:The effect during curing when there is alcohol
4-1. curing step
The pipe tobacco 1g before process be will wind up in the inherent 40 DEG C temperature of the closed container (glass scre-cap bottle -5mL) of controllable temperature During degree places various curings.As pipe tobacco, any of yellow kind is produced using Brazil's production burley tobaccos kind or Brazil.It is used as curing Period, using 0,1 week, 2 weeks, 4 weeks, 8 weeks or 12 weeks.
Before curing, the weight added into pipe tobacco relative to pipe tobacco is 2 weight % ethanol and 1 weight % peppermint Alcohol, ethanol is added by syringe, and menthol weighs specified rate with the state of powder and is added.After addition, sealing, fully stir The pipe tobacco in container is mixed, is homogenized.
4-2. analysis
Ester fragrance component is carried out by the method described in embodiment 1 and contributes to the analysis of the fragrant composition for inhaling taste.
4-3. result
Analysis result is shown in Fig. 3 A~3E.In figure, bullet represents burley tobaccos kind, and white round dot represents yellow kind.
According to Fig. 3 A~3B result, ethyl crotonate shows higher more than 5 weeks, during the curing of preferably 5~12 weeks Growing amount;Ethyl palmitate shows higher growing amount during 1~5 week, the curing of preferably 1~2 week.
According to Fig. 3 C~3E result, formic acid menthyl ester, menthyl acetate, isovaleric acid menthyl ester are more than 1 week, preferably 1 Higher growing amount is shown during the curing of~5 weeks.
Embodiment 5:The effect of pipe tobacco pH when there is alcohol
5-1. curing step
In the present embodiment, to roll the pipe tobacco before process as material, various pH pipe tobacco is prepared.Specifically, pH Adjust 1N aqueous sulfuric acids or 1N sodium hydrate aqueous solutions by specified rate of being sprayed in pipe tobacco and uniformly mix to carry out.
Pipe tobacco 1g after pH is adjusted is in the inherent 40 DEG C temperature of the closed container (glass scre-cap bottle -5mL) of controllable temperature Lower placement cures it in 1 week.As pipe tobacco, any of yellow kind is produced using Brazil's production burley tobaccos kind or Brazil.The pH of pipe tobacco Set in the range of 2~10.
Before curing, the weight added into the pipe tobacco after pH adjusted relative to pipe tobacco is 2 weight % ethanol and 1 weight % menthol is measured, ethanol is added by syringe, and menthol weighs specified rate with the state of powder and is added.Addition, it is close It is honored as a queen, is sufficiently stirred for the pipe tobacco in container, is homogenized.
5-2. analysis
Ester fragrance component is carried out by the method described in embodiment 1 and contributes to the analysis of the fragrant composition for inhaling taste.
In addition, for the pH of pipe tobacco, distilled water 10mL is added in pipe tobacco 0.5g, with 30 points of 200rpm oscillation extractions Clock, obtained supernatant is determined using pH meter (Mettler toledo).
5-3. result
Analysis result is shown in Fig. 4 A~4K.In figure, bullet represents burley tobaccos kind, and white round dot represents yellow kind.
According to Fig. 4 A~4B result, ethyl ester class (ethyl palmitate, ethyl linoleate) is using below pH3 (preferably pH2 ~3) or in the case of 4~7 any pipe tobacco show higher growing amount.
According to Fig. 4 C~4E result, formic acid menthyl ester is in the case of using below pH3 (preferably pH2~3) pipe tobacco The higher growing amount of display;Menthyl acetate, isovaleric acid menthyl ester are using below pH3 (preferably pH2~3) or 4~7 any Higher growing amount is shown in the case of pipe tobacco.
According to Fig. 4 F~4G result, the situation of menthones, benzaldehyde in the pipe tobacco using below pH4 (preferably pH2~3) The higher growing amount of lower display.
According to Fig. 4 H result, phytol shows what is decomposed in the case of using below pH4 (preferably pH2~3) pipe tobacco Tendency.
According to Fig. 4 I~4K result, furfural using below pH3 (preferably pH2~3) pipe tobacco in the case of show compared with High growing amount;Maltol shows higher growing amount in the case of using below pH5 (preferably pH2~5) pipe tobacco;Methyl Pyrazine shows higher growing amount in the case of using more than pH7 (preferably pH7~9) pipe tobacco.In addition, the pipe tobacco of yellow kind Preferential generation furans and reductones, on the other hand, the pipe tobacco of burley tobaccos kind preferentially generates Pyrazine.
Embodiment 6:The damping effect of pipe tobacco when there is alcohol
6-1. curing step
In the present embodiment, by the water of various specified rates of spraying in the pipe tobacco before rolling process and uniformly mix to add Plus.
The pipe tobacco 1g of moisture will be with the addition of in the inherent 40 DEG C temperature of the closed container (glass scre-cap bottle -5mL) of controllable temperature Lower place of degree cures it in 1 week.As pipe tobacco, any of yellow kind is produced using Brazil's production burley tobaccos kind or Brazil.It is used as water Divide addition, 0 μ L, 50 μ L, 100 μ L, 200 μ L are used relative to pipe tobacco 0.5g.
Before curing, the weight added into the pipe tobacco for the addition of moisture relative to pipe tobacco is 2 weight % ethanol and 1 weight % menthol is measured, ethanol is added by syringe, and menthol weighs specified rate with the state of powder and is added.Addition, it is close The pipe tobacco being honored as a queen in fully stirring container, is homogenized.
6-2. analysis
The analysis of ester fragrance component is carried out by the method described in embodiment 1.
6-3. result
Analysis result is shown in Fig. 5 A~5E.In figure, bullet represents burley tobaccos kind, and white round dot represents yellow kind.
According to Fig. 5 A~5E result, in the case of adding water in the pipe tobacco of yellow kind, suppress ethyl palmitate, sub- oil The generation of acetoacetic ester, formic acid menthyl ester, menthyl acetate, the generation of isovaleric acid menthyl ester do not find change.On the other hand, white In the case of water being added in the pipe tobacco of rib cigarette kind, menthyl acetate, the generation increase of isovaleric acid menthyl ester.
Embodiment 7:The effect of determining alcohol
7-1. curing step
The pipe tobacco 1g before process be will wind up in the inherent 40 DEG C temperature of the closed container (glass scre-cap bottle -5mL) of controllable temperature Degree, which is placed, cures it in 1 week.As pipe tobacco, any of yellow kind is produced using Brazil's production burley tobaccos kind or Brazil.
Before curing, the ethanol of various concentration and the menthol of various concentration are added into pipe tobacco, ethanol passes through syringe Addition, menthol weighs specified rate with the state of powder and is added.After addition, sealing, the fully pipe tobacco in stirring container, Homogenized.As concentration of alcohol, relative to pipe tobacco, using 1 weight %, 2 weight %, 4 weight %, 10 weight % or 40 weights Measure %.As menthol concentration, relative to pipe tobacco, using 0.4 weight %, 1 weight %, 4 weight %, 10 weight %.
7-2. analysis
The analysis of ester fragrance component is carried out by the method described in embodiment 1.
7-3. result
Analysis result is shown in Fig. 6 A~6D.In figure, bullet represents burley tobaccos kind, and white round dot represents yellow kind.
According to Fig. 6 A~6D result, if using relative to pipe tobacco as 1~5 weight %, more preferably 2~4 weight % amount The ethanol as matrix is added, then ethyl palmitate, the growing amount of ethyl linoleate are significantly increased.In addition, if with relative to Pipe tobacco for 4~10 weight % amount addition as matrix menthol, then formic acid menthyl ester, menthyl acetate growing amount it is notable Increase.
Embodiment 8:The additive effect of polyalcohol
Embodiment 8-A:The additive effect of polyalcohol before curing
8-A1. adds polyalcohol and subsequent curing
Relative to the pipe tobacco before process is rolled, atomization is with 4:1 ratio contains the aqueous solution of glycerine and propane diols and equal Mix evenly, be produced on the pipe tobacco of damping in mixing chamber (22 DEG C, 4 days).The addition of glycerine and propane diols relative to pipe tobacco It is respectively set as 2 weight % and 0.5 weight %.And then, it is 2 weight %'s to be added by syringe injection relative to the pipe tobacco Ethanol and menthol/ethanol solution equivalent to 1 weight % menthols.
The pipe tobacco 1g being processed as above is inherent 40 DEG C in the closed container (glass scre-cap bottle -5mL) of controllable temperature Temperature place cure it within 1 week.As pipe tobacco, any of yellow kind is produced using Brazil's production burley tobaccos kind or Brazil.
8-A2. is analyzed
The analysis of ester fragrance component is carried out by the method described in embodiment 1.
8-A3. results
Analysis result is shown in Fig. 7 A~7M.Fig. 7 A~7M is represented successively since left:
The situation (-) of polyalcohol (glycerine and propane diols) is not added with the pipe tobacco of yellow kind;
The situation (+) of polyalcohol (glycerine and propane diols) is with the addition of in the pipe tobacco of yellow kind;
The situation (-) of polyalcohol (glycerine and propane diols) is not added with the pipe tobacco of burley tobaccos kind;
The situation (-) of polyalcohol (glycerine conjunction propane diols) is not added with the pipe tobacco of burley tobaccos kind.
Yellow kind and burley tobaccos kind it is any in, by adding polyalcohol, although how much differences of amount, but aobvious Show the tendency for the generation for suppressing various esters.
Embodiment 8-B:Cure the polyalcohol additive effect after 1 week
8-B1. is cured and the further curing added under the conditions of polyalcohol afterwards
Weigh the pipe tobacco 1g before rolling process respectively in screw socket bottle and SPME bottles, add 1 weight % ethanol, peppermint Alcohol or phenmethylol.Ethanol and phenmethylol are added by syringe, specified rate menthol is weighed with the state of powder and added Plus.The pipe tobacco in container is sufficiently stirred for after addition, sealing, is homogenized.
Cure it within 1 week in 40 DEG C of temperature placement the pipe tobacco 1g being processed as above.Then, noted by syringe Enter to the screw socket bottle for being placed with the pipe tobacco through curing and add propane diols in SPME bottles, and then, being placed in 40 DEG C of temperature makes it in 1 week Curing.Addition concentration is set to 0,0.5,1,2,5 weight %.As pipe tobacco, yellow kind is produced using Brazil.
8-B2. is analyzed
The analysis of ester fragrance component is carried out to sample by the method described in embodiment 1.
8-B3. results
Fig. 8 A~8L chart is represented successively since left:
The pipe tobacco (0 week contrast (CTL-0W)) that is not cured,
Only carried out initial 1 week curing 1 week cure pipe tobacco (1W),
Cure after 1 week, be not added with propane diols, then carry out curing in 1 week cure within 2 weeks pipe tobaccos (PG0-2W),
Cure after 1 week, add 0.5 weight % propane diols, then carry out 1 week curing 2 weeks cure pipe tobaccos (PG0.5-2W),
Cure after 1 week, add 1 weight % propane diols, then carry out 1 week curing 2 weeks cure pipe tobaccos (PG1-2W),
Cure after 1 week, add 2 weight % propane diols, then carry out 1 week curing 2 weeks cure pipe tobaccos (PG2-2W),
Cure after 1 week, add 5 weight % propane diols, then carry out point for curing pipe tobacco (PG5-2W) for 2 weeks of curing in 1 week Analyse result.
Fig. 8 A~8D represents with the addition of the ethyl ester class of the various long chain fatty acids in the pipe tobacco maturation process of 1 weight % ethanol Behavior.In Fig. 8 A~8D, compared with 1 week cures pipe tobacco (1W), the various ethyl ester classes in pipe tobacco (PG0-2W) are cured within 2 weeks Growing amount tails off, and it is consistent with the tendency of the rheological parameters' change with time behavior shown in Fig. 3 B.It with the addition of 2 weeks curing pipe tobaccos of propane diols In (PG0.5-2W, PG1-2W, PG2-2W and PG5-2W), no matter its concentration, by ester growing amount at 2 weeks and the third two are not added with 2 weeks of alcohol cure pipe tobacco (PG0-2W) compared to less, by adding propane diols, the tendency of display suppression ester reaction of formation.
Fig. 8 E~8G represents with the addition of the peppermint of the various short chain fatty acids in 1 weight % menthol pipe tobacco maturation process The behavior of esters.In Fig. 8 E~8G, compared with 1 week cures pipe tobacco (1W), cure in pipe tobacco (PG0-2W) within 2 weeks, various peppermints The growing amount increase of esters, it is consistent with the tendency of the rheological parameters' change with time behavior shown in Fig. 3 C~E.It with the addition of 2 weeks of propane diols Cure in pipe tobacco (PG0.5-2W, PG1-2W, PG2-2W and PG5-2W), no matter its concentration, by ester growing amount at 2 weeks and not That adds propane diols cures pipe tobacco (PG0-2W) for 2 weeks compared to less, by adding propane diols, shows and suppresses inclining for ester reaction of formation To.
Fig. 8 H~8J represents to add the ethyl ester class of the various short chain fatty acids in the pipe tobacco maturation process of 1 weight % ethanol Behavior.In Fig. 8 H~8J, compared with 1 week cures pipe tobacco (1W), cure in pipe tobacco (PG0-2W) within 2 weeks, the life of various ethyl ester classes Into amount increase, it is consistent with the tendency of the rheological parameters' change with time behavior shown in Fig. 3 A.It with the addition of 2 weeks curing pipe tobaccos of propane diols In (PG0.5-2W, PG1-2W, PG2-2W and PG5-2W), no matter its concentration, by ester growing amount at 2 weeks and the third two are not added with 2 weeks of alcohol cure pipe tobacco (PG0-2W) compared to less, by adding propane diols, the tendency of display suppression ester reaction of formation.
Fig. 8 K represent to add the behavior of the benzyl acetate in the pipe tobacco maturation process of 1 weight % phenmethylols.In Fig. 8 K, 1 Week curing pipe tobacco (1W) is roughly the same with the benzyl acetate growing amount that 2 weeks cure pipe tobacco (PG0-2W), with the addition of 2 weeks of propane diols Cure also almost without difference in pipe tobacco (PG0.5-2W, PG1-2W, PG2-2W and PG5-2W), but concentration is added with propane diols Increase, show it is fraction of suppress ester reaction of formation tendency.
Fig. 8 L represent the behavior for the phenethyl acetate being not added with the pipe tobacco maturation process of alcohol.1 week curing pipe tobacco (1W) and 2 The phenethyl acetate substantially equal amount of week curing pipe tobacco (PG0-2W), with the addition of 2 weeks curing pipe tobacco (PG0.5- of propane diols 2W, PG1-2W, PG2-2W and PG5-2W) in also almost without difference, but add with propane diols the increase of concentration, display is a little Suppression ester reaction of formation tendency.
According to result above, by adding polyalcohol, although how much differences of amount, but display suppresses the life of various esters Into tendency.
Embodiment 9:Add the behavior of fragrance component when various alcohol are cured
9-1. curing step
Before curing, the pipe tobacco 1g of various alcohol will be with the addition of in the closed container (glass scre-cap bottle -5mL) of controllable temperature Being placed in 40 DEG C of temperature cures it in 1 week.As pipe tobacco, yellow kind is produced using Brazil.As control, using being not added with alcohol Pipe tobacco.
The species of the alcohol of addition and addition concentration are shown in following.
The weight % of isobutanol 2
The weight % of n-butanol 2
The weight % of isoamyl alcohol 2
The weight % of n-hexyl alcohol 2
The weight % of propane diols 2
The weight % of phenmethylol 2.
9-2. analysis
The analysis of ester fragrance component is carried out by the method described in embodiment 1.
9-3. result
The dichloromethane extraction GCMS and SPME-GCMS chromatograms that the curing tobacco sample of various alcohol will be with the addition of are shown in Fig. 9. Confirm the generation of ester corresponding with the species of the alcohol of addition.
In fig .9, " C1 " represents formic acid esters, and " C2 " represents acetic acid esters, and " C5 " represents valerate, and " C6 " represents capronate.
Embodiment 10:Add the behavior of fragrance component when various acid are cured with ethanol
10-1. curing steps
Before curing, both various acid and ethanol are added, pipe tobacco is cured similarly to Example 9.By the sour of addition Species and addition concentration and the addition concentration of ethanol are shown in following.Following addition concentration is with the weight % tables relative to pipe tobacco Show.
The weight % of 1 weight %+ ethanol of isovaleric acid 1
The weight % of 1 weight %+ ethanol of 3 methylvaleric acid 1
The weight % of 1 weight %+ ethanol of n-caproic acid 1
The weight % of 1 weight %+ ethanol of caprylic acid 1.
10-2. is analyzed
The analysis of ester fragrance component is carried out by the method described in embodiment 1.
10-3. results
The SPME-GCMS chromatograms that the curing tobacco sample of various acid and ethanol will be with the addition of are shown in Figure 10.Confirm and add Plus sour corresponding ethyl ester generation.
In Fig. 10, in the case where with the addition of isovaleric acid and ethanol, the generation of ethyl isovalerate is confirmed, with the addition of In the case of 3 methylvaleric acid and ethanol, the generation of 3 methylvaleric acid ethyl ester is confirmed, in the situation of addition n-caproic acid and ethanol Under, the generation of n-caproic acid ethyl ester being confirmed, in the case where with the addition of caprylic acid and ethanol, the life of caprylic acid ethyl ester is confirmed Into.
Embodiment 11:The behavior of fragrance component when addition essential oil or extract spices are cured
11-1. curing steps
Before curing, various essential oils or extract spices are added, pipe tobacco is cured similarly to Example 9.By addition The species and addition concentration of essential oil or extract spices are shown in following.Following addition concentration is with the weight % tables relative to pipe tobacco Show.
Cinnamon leaves oil (Cinnamon leaf oil) 1 weight %
The weight % of rosemary oil (Rosemary oil) 1
The weight % of peppermint oil (Peppermint oil) 1
The weight % of spearmint oil (Spearmint oil) 1
Carob tamarind legume extract (St.John ' s bread extract) 1 weight %
The weight % of licorice (Licorice extract) 1.
11-2. is analyzed
The analysis of ester fragrance component is carried out by the method described in embodiment 1.
11-3. results
The dichloromethane extraction GCMS and SPME-GCMS chromatograms that the curing tobacco sample of various acid and ethanol will be with the addition of are shown In Figure 11 A and 11B.The composition of contained alcohol and acid, confirms the life of various esters in essential oil or extract spices based on addition Into.It can be seen from the result, by adding various essential oils and extract spices, the pipe tobacco constituted with various esters can be obtained.
In Figure 11 A, " C14 " represents ethyl myristate, and " C16 " represents ethyl palmitate, and " C18 " represents stearic acid second Ester.In addition, in Figure 11 B, " C2 " represents ethyl acetate, " C5 " represents ethyl valerate, and " C6 " represents ethyl hexanoate.
Embodiment 12:The sense evaluation of snuff
The preparation of 12-1. sense evaluation samples and evaluation gimmick
Before curing, weight of the addition relative to pipe tobacco is injected for 2 weight % ethanol and equivalent to 1 weight by syringe Measure menthol/ethanol solution of % menthols.By obtained pipe tobacco 1g controllable temperature closed container (glass scre-cap bottle- 5mL) inherent 40 DEG C of placements cure it in 1 week.As pipe tobacco, yellow kind, Japan's production burley tobaccos kind or Greece are produced using Malawi Produce any of Japan's cigarette kind.
The pipe tobacco 0.2g of curing is loaded to the pipe (φ 8mm i.d.) of propylene, the acetate mistake of 4mm width at two ends Filter tip is capped, and the outside of propylene tubulation is rolled with rubber heater, is heated to 40 DEG C as examination and is inhaled sample.
Sense evaluation sucks above-mentioned examination by 5 special commentators and inhales sample, fragrance, taste that the different band to tobacco material is come The difference that road, body sexuality are felt is evaluated.
12-2. results
The result of sense evaluation is shown in following.In sample is inhaled in above-mentioned examination, (use with compareing and do not carried out maturation process The examination of pipe tobacco inhale sample) enhancing when, the fragrant taste of inhaling that commentator experiences is described below.
1) Malawi's production yellow kind
Fruit, the fragrance of herbal medicine sample, sweet taste are relatively strong, suction with cigarette sample is felt.
Stimulate few, happy nice and cool menthol sense occur.
2) Japan's production burley tobaccos kind
Dry fruit, white wine sample fragrance are stronger, and there is also sweet taste.
The residual Japan production distinctive jerky fragrance of burley tobacco leaf, but it is weaker.
3) Greece produces Japan's cigarette kind
The sweet taste of flowers, suction feel stronger, occur the cooling feeling of menthol strongly.
Stimulate and weaken, the residual of the green aroma of Japan's cigarette is weaker.
Embodiment 13:The sense evaluation of cigarette
The preparation of 13-1. sense evaluation samples and evaluation gimmick
Pipe tobacco is cured similarly to Example 10, pipe tobacco is made.To it not enter in the low peppermint alcohol type cigarettes of Seven star The pipe tobacco of the fragrant addition of row two is extracted out, and the 800mg pipe tobaccos are loaded into obtained smoke pipe, examination is set to and smokes cigarette.
The cigarette sample is inhaled by 5 special commentator's examinations, the outer fragrant, suction taste effect that the different band to tobacco material is come Difference is evaluated.
13-2. results
The result of sense evaluation is shown in following.In above-mentioned examination smokes cigarette, with compareing (using not carrying out maturation process The examination of pipe tobacco smoke cigarette) compared to enhancing when, the fragrant taste of inhaling that commentator feels is described below.
1) yellow kind
Outer perfume (or spice):White wine, Rum sample fragrance it is stronger.
Inhale taste:The texture of cigarette matter is thinner, soft.There is fruity sample sweet taste.
The creeping chill enhancing of menthol, continuation is also high.Also there is effect of promoting the production of body fluid.
Stimulate and weaken.
2) burley tobaccos kind
Outer perfume (or spice):The grape dry sample of curing, the fragrance of the fruity of brandy sample are stronger.
Inhale taste:Burley tobaccos sample fragrance is produced while the sweet taste of dry fruit sample, menthol sense is weaker.
3) Japan's cigarette kind
Outer perfume (or spice):Rum, grape dry sample fragrance are stronger, it may have the fragrance of the green herbal medicine in Japan's cigarette ocean.
With the sour smelly weaker of the distinctive fermentation sense of Japan's cigarette.
Inhale taste:With Rum, grape dry sample fragrance, ferment smelly weaker.Promote the production of body fluid effect, stimulate it is slightly strong.
More than, according to various embodiments, embodiment, the present invention is described, but the present invention is not implemented by these Mode, embodiment limitation.The maturation process using pipe tobacco that the present inventor etc. have found first controls ester fragrance component and helped In the method for the fragrant composition for inhaling taste, by changing additive, the maturation process bars such as content component, alcohol or acid contained in pipe tobacco Part, has formulated the pipe tobacco that taste feature is inhaled with target perfume.In addition, the present invention can be shown in Application Example tobacco varieties or contain The additives such as the natural tobacco materials of these tobacco varieties, the ethanol used, menthol also can widely apply day from that need not say Right tobacco-containing material and the perfumery containing alcohol, acid.

Claims (11)

1. a kind of manufacture method of tobacco-containing material, it includes following process:
Dry the Tobacco Leaf after harvest, the process for obtaining dry Tobacco Leaf;
Cure the Tobacco Leaf of above-mentioned drying, the process of the Tobacco Leaf cured;
By the Tobacco Leaf chopping of above-mentioned curing, the process for obtaining pipe tobacco;
By the above-mentioned pipe tobacco before the manufacture for tobacco product is in air atmosphere and is cured in confined conditions, obtain The process of the pipe tobacco of curing;With
The process that polyalcohol is added into the pipe tobacco of the curing.
2. according to the method described in claim 1, wherein, the process of the pipe tobacco cured selected from alcohol, acid and is being extracted Carried out in the presence of at least one of thing spices additive.
3. method according to claim 1 or 2, wherein, in the process of the pipe tobacco cured, make the pipe tobacco Cured in room temperature~70 DEG C.
4. method according to claim 1 or 2, wherein, in the process of the pipe tobacco cured, make the pipe tobacco The time of curing 1 week~3 months.
5. method according to claim 1 or 2, wherein, in the process of the pipe tobacco cured, the pipe tobacco PH is 2~8.
6. method according to claim 2, wherein, the additive is alcohol, and the alcohol is selected from ethanol, menthol, benzene At least one of methanol, isobutanol, n-butanol, isoamyl alcohol, n-hexyl alcohol.
7. method according to claim 2, wherein, the additive is acid, and the acid is selected from isobutyric acid, 3- methyl fourths At least one of acid, n-caproic acid, octanoic acid.
8. method according to claim 2, wherein, the additive is extract spices, and the extract spices is essence Oil.
9. method according to claim 2, wherein, the additive is extract spices, and the extract spices is choosing Carried from Rum, peppermint oil, spearmint oil, Japanese peppermint oil, rosemary oil, licorice, carob tamarind legume extract, cocoa Take at least one of thing.
10. method according to claim 2, wherein, the additive is alcohol, the alcohol using relative to pipe tobacco as 0.4~ 10 weight % amount is added.
11. a tobacco articles, it contains the tobacco-containing material manufactured by method according to any one of claims 1 to 10.
CN201180075975.5A 2011-12-26 2011-12-26 Manufacture method containing enhanced ester fragrance component and the tobacco-containing material for contributing to the fragrant composition for inhaling taste and the tobacco product containing the tobacco-containing material manufactured by this method Expired - Fee Related CN104010526B (en)

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