CN106723316B - A kind of composition and the method that tobacco extract is prepared using the composition - Google Patents

A kind of composition and the method that tobacco extract is prepared using the composition Download PDF

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Publication number
CN106723316B
CN106723316B CN201611213727.3A CN201611213727A CN106723316B CN 106723316 B CN106723316 B CN 106723316B CN 201611213727 A CN201611213727 A CN 201611213727A CN 106723316 B CN106723316 B CN 106723316B
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China
Prior art keywords
tobacco
composition
tobacco extract
methyl ether
propyl acetate
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CN201611213727.3A
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Chinese (zh)
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CN106723316A (en
Inventor
李易非
李跃锋
林凯
鹿洪亮
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福建中烟工业有限责任公司
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Priority to CN201611213727.3A priority Critical patent/CN106723316B/en
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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
    • A24B15/00Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/18Treatment of tobacco products or tobacco substitutes
    • A24B15/24Treatment of tobacco products or tobacco substitutes by extraction; Tobacco extracts
    • A24B15/26Use of organic solvents for extraction

Abstract

A kind of method that tobacco extract is prepared the present invention relates to composition and using the composition.The composition, including propyl acetate and eugenol methyl ether, the weight ratio of propyl acetate and eugenol methyl ether is 10~90:10~90.Extract tobacco extract, and gained tobacco extract can effectively be promoted the perfume quantity and harmony of cigarette, reduce the irritation and withered and burnt smell of cigarette, improve Sensory Quality of Cigarette for cigarette from tobacco using above-mentioned composition.

Description

A kind of composition and the method that tobacco extract is prepared using the composition

Technical field

The invention belongs to Field of Tobacco, and in particular to a kind of composition and the side that tobacco extract is prepared using the composition Method.

Background technology

Reconstituted tobacco is one kind raw material based on the tobacco materials such as crumbled tobacco, offal, offal, by reconfiguring processing The product formed, also referred to as reconstituted tobacoo.

Paper process is to prepare the mainstream production technology of reconstituted tobacco at present, including five main workshop sections:Extract section, slurrying Section, section of manufacturing paper with pulp, coating section and baking segment.One typical manufacturing process includes:It is carried out after tobacco material is added water retting first Compression, the hydrotrope in tobacco is detached with insoluble matter (fiber etc.).Then the insoluble matters such as baccy fiber are dispersed in water it Fiber chip base is made by paper machine.Again by the above-mentioned hydrotrope it is concentrated after be coated in chip base, be after dry paper process again Make tobacco leaf.

The hydrotrope generally use Hot water extraction of tobacco is prepared, the method technological process is simple, and cost is relatively low.However, In order to obtain the reconstituted tobacco of high quality, the prior art also needs to preferably prepare the method for tobacco extract and better cigarette Careless extract.

Invention content

Inventor has found, tobacco is extracted using the aqueous solution containing propyl acetate and eugenol methyl ether, Neng Gouyou A variety of aroma components in effect extraction tobacco, gained tobacco extract are used for cigarette, are capable of providing the aesthetic quality of cigarette.

It is an object of the present invention to provide a kind of composition, further object of the present invention is to provide above-mentioned composition Purposes, further object of the present invention is to provide a kind of preparation method of tobacco extract, and further object of the present invention is A kind of tobacco extract is provided, further object of the present invention is to provide the purposes of above-mentioned tobacco extract.

First aspect present invention provides a kind of composition, including propyl acetate and eugenol methyl ether,

The weight ratio of propyl acetate and eugenol methyl ether is 10~90:10~90;

Preferably, the weight ratio of propyl acetate and eugenol methyl ether is 30~60:40~70;

Preferably, the weight ratio of propyl acetate and eugenol methyl ether is 40~50:50~60;

Preferably, the weight ratio of propyl acetate and eugenol methyl ether is 40~45:55~60.

In one embodiment, the composition of any one of present invention, further includes water.

In one embodiment, the composition of any one of present invention, the total weight of propyl acetate and eugenol methyl ether with The weight ratio of water is 1~38:106, preferably 1~15:106, more preferable 1~6:106

In one embodiment, the composition of any one of present invention is used to extract the use of tobacco extract from tobacco On the way.

Second aspect of the present invention provides a kind of preparation method of tobacco extract, includes the following steps:

Tobacco extract is extracted from tobacco using any one of them composition of the present invention.

In one embodiment, the method for any one of present invention, includes the following steps:

Tobacco is extracted using the aqueous solution containing composition any one of of the invention.

Preferably, the sum of the concentration of propyl acetate and eugenol methyl ether in the aqueous solution be 1~38mg/L, preferably 1 ~15mg/L, more preferable 1~6mg/L, more preferable 1~4mg/L.

In one embodiment, the method for any one of present invention, the temperature of extraction are 80~90 DEG C, such as 70~80 ℃。

In one embodiment, the method for any one of present invention, time of extraction are 20~60min, such as 30~ 40min。

In one embodiment, the weight ratio of the method for any one of present invention, tobacco and the aqueous solution is 1:30~ 70, such as 1:50~60.

In one embodiment, the method for any one of present invention, it is further comprising the steps of:It is water-soluble after concentration extraction Liquid collects steaming excess.

In one embodiment, the method for any one of present invention, the concentration are to be concentrated under reduced pressure;

Preferably, the vacuum degree of reduced pressure is 100~400mbar, such as 200~300mbar;

Preferably, 60~80 DEG C of the temperature of reduced pressure, such as 70 DEG C;

Preferably, the concentration volume ratio of reduced pressure is 6~8:1.

In one embodiment, it is concentrated under reduced pressure using Rotary Evaporators.

Preferably, the rotating speed of Rotary Evaporators is 80~130r/min, more preferably 100~120r/min.

In one embodiment, the method for any one of present invention, including following one or multi-step:

A) tobacco leaf is extracted with the aqueous solution containing propyl acetate and eugenol methyl ether, per 10g tobacco leaves 300~700ml institutes Aqueous solution extraction is stated, extraction temperature is 60~80 DEG C, and extraction time is 20~40min, is filtered after extraction, collects filtrate;

B) liquid after extraction is concentrated under reduced pressure, the vacuum degree of reduced pressure is 100~400mbar, and temperature is 60~80 DEG C, Cocnentration factor is 6~8:1, collect steaming excess.

In one embodiment, the method for any one of present invention, the tobacco are tobacco leaf.

Third aspect present invention provides a kind of tobacco extract, is made by method any one of of the invention;

Preferably, in the tobacco extract, the weight ratio of pyridines chemical composition and phenols chemical composition is 12~50: 35~82;More preferably 8~13:85~93;

Preferably, in the tobacco extract, 3- picolines, 3-ethylpyridine, xylenol and eugenol weight Than being 0.5~12:4~20:21~57:30~80, more preferably 3~7:5~9:46.5~49.5:35~40.

Fourth aspect present invention provides the tobacco extract of any one of the present invention for the use for cigarette or electronic cigarette flavoring On the way.

Fifth aspect present invention provides use of the tobacco extract as reconstituted tobacco chip base coating fluid of any one of the present invention On the way.

The present composition it is each into belonging to YQ 52-2015《Tobacco product is permitted workable additive list》Allow The substance of addition meets industry relevant regulations.

In one embodiment, No. CAS of propyl acetate is 109-60-4, and No. CAS of eugenol methyl ether is 93-15- 2。

Beneficial effects of the present invention

One or more embodiments of the present invention have following one or more advantageous effects:

1) composition of the invention from tobacco for extracting tobacco extract, to the extraction efficiency of aroma component in tobacco It is high;

2) composition of the invention is from tobacco for extracting tobacco extract, to pyridines chemical composition in tobacco and/ Or the extraction efficiency of phenols chemical composition is high;

3) composition of the invention imitates the extraction of liposoluble constituent in tobacco for extracting tobacco extract from tobacco Rate is high;

4) preparation method of tobacco extract of the invention is easy, at low cost;

5) composition of the invention from tobacco for extracting tobacco extract so that mainly caused in tobacco extract it is fragrant into Point ratio is optimized, and the ratio of two major class chemical compositions is optimized;

6) tobacco extract of the invention is applied to cigarette, and aesthetic quality during gained cigarette smoking is preferable.

Specific embodiment

In following embodiment, No. CAS of propyl acetate is 109-60-4, and No. CAS of eugenol methyl ether is 93-15-2.

Specific embodiments of the present invention will be referred in detail now.Although this hair is described with reference to these specific embodiments It is bright, it is appreciated that being not intended to limit the invention to these specific embodiments.It can be wrapped on the contrary, these embodiments are intended to covering Include replacement, change or equivalent embodiments in the spirit and range being defined by the claims.In the following description, Elaborate a large amount of details in order to provide complete understanding of the present invention.The present invention can be partly or entirely these be specific It is carried out in the case of details.In other cases, it in order not to which the present invention is made unnecessarily to obscure, is not described in well known Technological operation.

When being used in combination with the " comprising " in this specification and the appended claims or similar language, singulative "the" Including plural reference, unless the context clearly dictates otherwise.Unless otherwise defined, all technologies used herein and section are academic Language has the normally understood identical meanings of general technical staff of the technical field of the invention.

Embodiment 1:

When embodiment 1 prepares tobacco extract, the composition used is the mixture of propyl acetate and eugenol methyl ether, The mass ratio of middle propyl acetate and eugenol methyl ether is 42:58.

Specific the step of preparing tobacco extract, is as follows:

Weigh Dali C12F grade tobacco leaf 30.0g (oven dry weight).

1500ml water is added in into tobacco leaf, also adds in 3mg above-mentioned compositions in water.Above-mentioned tobacco leaf is being contained into composition Aqueous solution in extract, 70 DEG C, extraction time 30min of extraction temperature, magnetic agitation aqueous solution in leaching process, speed of agitator: 1000rpm/min.After extraction, filter and collect filtrate.Take 1200ml filtrate decompressions concentration (G3 Rotary Evaporators, Heidolph companies), the vacuum degree 250mbar of reduced pressure, temperature 70 C, rotating speed 110rpm/min, being concentrated into steaming excess is 200ml, collects steaming excess, this steaming excess is the tobacco extract of embodiment 1.

Embodiment 2

When embodiment 2 prepares tobacco extract, the composition used is the mixture of propyl acetate and eugenol methyl ether, The mass ratio of middle propyl acetate and eugenol methyl ether is 11:89.

Specific the step of preparing tobacco extract, with embodiment 1, obtains the tobacco extract of embodiment 2.

Embodiment 3

When embodiment 3 prepares tobacco extract, the composition used is the mixture of propyl acetate and eugenol methyl ether, The mass ratio of middle propyl acetate and eugenol methyl ether is 89:11.

Specific the step of preparing tobacco extract, with embodiment 1, obtains the tobacco extract of embodiment 3.

Embodiment 4

When embodiment 4 prepares tobacco extract, the composition used is the mixture of propyl acetate and eugenol methyl ether, The mass ratio of middle propyl acetate and eugenol methyl ether is 50:50.

Specific the step of preparing tobacco extract, with embodiment 1, obtains the tobacco extract of embodiment 4.

Comparative example 1

Using art methods, with pure water preparation tobacco extract.

Weigh Dali C12F grade tobacco leaf 30.0g (oven dry weight).

1500ml water is added in into tobacco leaf, does not add above-mentioned composition, other steps obtain comparative example 1 with embodiment 1 Tobacco extract.

Analysis detection 1:Sensory quality assessment

The tobacco extract of Example 1~4 and comparative example 1, respectively equivalent be applied on the cigarette paper of blank cigarette, apply The amount of smearing accounts for 2/10000ths of cigarette weight, and gained cigarette sample number consecutively is A~E.According to standard YC/T498-2014《Reconstruction Tobacco leaf (paper process) sensory evaluation method》Sample evaluation rule, aesthetic quality is carried out to cigarette A~E and is smoked panel test, as a result such as table 1 It is shown.

1 cigarette sample aesthetic quality's grade form of table

As shown in Table 1, the sense organ marking of cigarette E is 68.0 points, and the sense organ marking of cigarette A~D is 69.5~72.0 points.Tool Body, cigarette A~D is promoted in terms of perfume quantity and harmony, is decreased in terms of irritation and withered and burnt smell, wherein, cigarette The marking highest of branch A, perfume quantity and harmony rise significantly, and irritation and withered and burnt smell reduce significantly.It is described above, embodiment 1~4 tobacco extract is used for cigarette, can effectively promote the perfume quantity and harmony of cigarette, reduce cigarette irritation and Withered and burnt smell improves Sensory Quality of Cigarette.

Analysis detection 2:Gaschromatographic mass spectrometry detects

It is respectively caused in gas chromatography mass spectrometry (GC/MS) further detection 1 two groups of tobacco extracts of embodiment 1 and comparative example Fragrant ingredient.

To meet detection sample requirement, the tobacco of embodiment 1 and comparative example 1 is extracted respectively with dichloromethane (polarity 3.4) Extract, add methylene chloride 200ml per 200ml tobacco extracts, extracts 3 times, merges and collects 3 extract liquor (dichloromethane Phase), 500ml is taken, is concentrated under reduced pressure (G3 Rotary Evaporators, Heidolph companies), 39 DEG C, vacuum degree 750mbar of thickening temperature, is turned After fast 110rpm/min, 2.0ml is concentrated into, obtains detection sample.

Gaschromatographic mass spectrometry condition is as follows:Chromatographic column DB-5MS (30m × 0.25mm × 0.25 μm);Carrier gas He (99.999%);Flow velocity 1.0ml/min;290 DEG C of injector temperature;1.0 μ L of sample size;Sample introduction pattern is split sampling;Shunting Sample introduction is than 10:1;Temperature program is 45 DEG C (2min), and 5 DEG C/min rises to 200 DEG C, and 3 DEG C/min rises to 250 DEG C, and 5 DEG C/min rises to 300℃(10min);Ion source is electron bombardment (EI);Electron energy 70eV;250 DEG C of ion source temperature.Transmission line temperature 300 ℃;Analyzer is level four bars mass analyzer;Scan pattern is full scan;40~500amu of mass scan range;Solvent delay 4.5min。

According to gaschromatographic mass spectrometry testing result, analyze and calculate tobacco extract obtained by every gram of tobacco leaf (oven dry weight) In several main aroma components mass content and ratio, it is as shown in table 2 below:

Table 2

As shown in table 2, compared to comparative example 1, main aroma component has increase in the leaf tobacco extract of embodiment 1.Example Such as, 3- picolines extraction efficiency increases by 361.5%, and 3-ethylpyridine extraction efficiency increases by 634.3%, xylenol extraction efficiency Increase by 291.8%, eugenol extraction efficiency increases by 256.8%.It follows that the addition is used in tobacco leaf extraction process After agent, the extraction efficiency of main aroma component significantly improves.

In addition, for the normalization percentage of above-mentioned several main aroma components, embodiment 1 is compared with comparative example 1,3- first The ratio of yl pyridines and 3-ethylpyridine increases, and the ratio of eugenol decreases.It follows that use of the present invention group The extraction efficiency that tobacco extract prepared by object extraction not only increases main aroma component is closed, also optimizes main aroma component Ratio, which is used for cigarette, can effectively promote the perfume quantity and harmony of cigarette, reduces the irritation of cigarette And withered and burnt smell, improve Sensory Quality of Cigarette.

Further, according to the detection data of gaschromatographic mass spectrometry, to each aroma component for detecting according to pyridines and phenol Two class chemical composition of class carries out Classifying Sum, and specifically, pyridines chemical composition includes 3- picolines, 3-ethylpyridine, 3, 4- and picoline and 4- ethylpyridines;Phenol generalization, which studies, point to be included:Xylenol, eugenol, guaiacol and phenol.

Two class chemical composition contents and ratio comparison are as shown in table 3 below in the tobacco extract of embodiment 1 and comparative example 1.

Table 3

As shown in table 3, in the tobacco extract of embodiment 1, pyridine compounds and their extraction efficiency increases in tobacco leaf 182.9%, phenolic compound extraction efficiency increases by 388.7%.From the foregoing, it will be observed that it is extracted using tobacco prepared by the present composition Object, the content of two major class chemical composition of pyridines and phenols is significantly increased in product.

In addition, for the normalization percentage of above-mentioned two major class chemical composition, embodiment 1 is compared with comparative example 1, pyridines The ratio of compound decreases, and the ratio of phenolic compound increased.It is made it follows that being extracted using the present composition Standby tobacco extract not only increases the extraction efficiency of two major class chemical compositions, also optimizes the ratio of two major class chemical compositions Example, the tobacco extract are used for cigarette, can effectively promote the perfume quantity and harmony of cigarette, reduce the irritation of cigarette and withered Burnt gas improves Sensory Quality of Cigarette.

For the composition that above-described embodiment uses, lipophilic group and hydrophily base are included in their chemical constitution Group, wherein, lipophilic group can be combined with liposoluble constituent in tobacco leaf, and hydrophilic radical can be combined with water, and then form water packet The physical form of oil, is dissolved in water liposoluble constituent in tobacco leaf.Tobacco is extracted from tobacco using the composition of the present invention Extract can not only improve the extraction efficiency to effective aroma component in tobacco and two major class chemical compositions, additionally it is possible to excellent Change the ratio of effective aroma component and two major class chemical compositions.The tobacco extract is used for cigarette, can effectively promote cigarette Perfume quantity and harmony reduce the irritation and withered and burnt smell of cigarette, improve Sensory Quality of Cigarette.

Finally it should be noted that:The above embodiments are merely illustrative of the technical scheme of the present invention and are not intended to be limiting thereof;To the greatest extent The present invention is described in detail with reference to preferred embodiments for pipe, those of ordinary skills in the art should understand that:Still It can modify to the specific embodiment of the present invention or equivalent replacement is carried out to some technical characteristics;Without departing from this hair The spirit of bright technical solution should all cover in the claimed technical solution range of the present invention.

Claims (34)

1. it is a kind of for extracting the composition of tobacco extract from tobacco, including propyl acetate, eugenol methyl ether and water,
The weight ratio of propyl acetate and eugenol methyl ether is 10~90:10~90;
The weight ratio of the total weight and water of propyl acetate and eugenol methyl ether is 1~38:106
2. the weight ratio of composition according to claim 1, propyl acetate and eugenol methyl ether is 30~60:40~70.
3. the weight ratio of composition according to claim 1, propyl acetate and eugenol methyl ether is 40~50:50~60.
4. the weight ratio of composition according to claim 1, propyl acetate and eugenol methyl ether is 40~45:55~60.
5. the total weight of composition according to claim 1, propyl acetate and eugenol methyl ether and the weight ratio of water for 1~ 15:106
6. the total weight of composition according to claim 1, propyl acetate and eugenol methyl ether and the weight ratio of water for 1~ 6:106
7. claim 1~6 any one of them composition is for the purposes of the extraction tobacco extract from tobacco.
8. a kind of preparation method of tobacco extract, includes the following steps:
Tobacco extract is extracted from tobacco using claim 1~6 any one of them composition.
9. according to the method described in claim 8, include the following steps:
Tobacco is extracted using the aqueous solution of the composition containing any one of claim 1~6.
10. according to the method described in claim 9, the sum of the concentration of propyl acetate and eugenol methyl ether in the aqueous solution is 1~38mg/L.
11. according to the method described in claim 9, the sum of the concentration of propyl acetate and eugenol methyl ether in the aqueous solution is 1~15mg/L.
12. according to the method described in claim 9, the sum of the concentration of propyl acetate and eugenol methyl ether in the aqueous solution is 1~6mg/L.
13. according to the method described in claim 9, the temperature of extraction is 80~90 DEG C.
14. according to the method described in claim 9, the temperature of extraction is 70~80 DEG C.
15. according to the method described in claim 9, the time of extraction is 20~60min.
16. according to the method described in claim 9, the time of extraction is 30~40min.
17. according to the method described in claim 9, the weight ratio of tobacco and the aqueous solution is 1:30~70.
18. according to the method described in claim 9, the weight ratio of tobacco and the aqueous solution is 1:50~60.
It is 19. according to the method described in claim 9, further comprising the steps of:Aqueous solution after concentration extraction, collects steaming excess.
20. according to the method for claim 19, the concentration is to be concentrated under reduced pressure.
21. according to the method for claim 20, the vacuum degree of reduced pressure is 100~400mbar.
22. according to the method for claim 20, the vacuum degree of reduced pressure is 200~300mbar.
23. according to the method for claim 20, the temperature of reduced pressure is 60~80 DEG C.
24. according to the method for claim 20, the temperature of reduced pressure is 70 DEG C.
25. according to the method for claim 20, the concentration volume ratio of reduced pressure is 6~8:1.
26. according to claim 9~25 any one of them method, including following one or multi-step:
A) tobacco leaf is extracted with the aqueous solution containing propyl acetate and eugenol methyl ether, per 10g tobacco leaves water described in 300~700ml Solution extracts, and extraction temperature is 60~80 DEG C, and extraction time is 20~40min, is filtered after extraction, collects filtrate;
B) liquid after extraction is concentrated under reduced pressure, the vacuum degree of reduced pressure is 100~400mbar, and temperature is 60~80 DEG C, concentration Than being 6~8:1, collect steaming excess.
27. the method according to claim 8~25, the tobacco is tobacco leaf.
28. a kind of tobacco extract is made by the method for any one of claim 8~27.
29. tobacco extract according to claim 28, in the tobacco extract, pyridines chemical composition and phenol generalization The weight ratio studied point is 5~15:75~95.
30. tobacco extract according to claim 28, in the tobacco extract, pyridines chemical composition and phenol generalization The weight ratio studied point is 8~13:85~93.
31. tobacco extract according to claim 28, in the tobacco extract, 3- picolines, 3-ethylpyridine, The weight ratio of xylenol and eugenol is 0.5~12:4~20:21~57:30~80.
32. tobacco extract according to claim 28, in the tobacco extract, pyridines chemical composition and phenol generalization The weight ratio studied point is 3~7:5~9:46.5~49.5:35~40.
33. claim 28~32 any one of them tobacco extract is used for the purposes for cigarette or electronic cigarette flavoring.
34. claim 28~32 any one of them tobacco extract is used as the purposes of reconstituted tobacco chip base coating fluid.
CN201611213727.3A 2016-12-26 2016-12-26 A kind of composition and the method that tobacco extract is prepared using the composition CN106723316B (en)

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Publication number Priority date Publication date Assignee Title
EP0908108A2 (en) * 1997-10-08 1999-04-14 Japan Tobacco Inc. Method for producting a heat-irreversibly coagulated glucan sheet containing a leaf tobacco extract and method for producing a tobacco flavor-generating medium using a heat-irreversibly coagulated glucan sheet
EP0908109A2 (en) * 1997-10-09 1999-04-14 Japan Tobacco Inc. Method for producing a tobacco flavor-tasting article
CN104872814A (en) * 2015-05-05 2015-09-02 昌宁德康生物科技有限公司 Production method for extracting tobacco leaf clean oil

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Publication number Priority date Publication date Assignee Title
WO2002090479A1 (en) * 2001-05-04 2002-11-14 The Procter & Gamble Company Perfumed particles and articles containing the same
JP2004535223A (en) * 2001-05-04 2004-11-25 ザ プロクター アンド ギャンブル カンパニー Air freshening compositions, articles containing them, and methods
WO2015029977A1 (en) * 2013-08-27 2015-03-05 日本たばこ産業株式会社 Tobacco raw material, method for manufacturing same, and tobacco product

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0908108A2 (en) * 1997-10-08 1999-04-14 Japan Tobacco Inc. Method for producting a heat-irreversibly coagulated glucan sheet containing a leaf tobacco extract and method for producing a tobacco flavor-generating medium using a heat-irreversibly coagulated glucan sheet
EP0908109A2 (en) * 1997-10-09 1999-04-14 Japan Tobacco Inc. Method for producing a tobacco flavor-tasting article
CN104872814A (en) * 2015-05-05 2015-09-02 昌宁德康生物科技有限公司 Production method for extracting tobacco leaf clean oil

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