WO1994007382A1 - Procede de traitement de tabac vert et produit ainsi obtenu - Google Patents
Procede de traitement de tabac vert et produit ainsi obtenu Download PDFInfo
- Publication number
- WO1994007382A1 WO1994007382A1 PCT/SE1993/000764 SE9300764W WO9407382A1 WO 1994007382 A1 WO1994007382 A1 WO 1994007382A1 SE 9300764 W SE9300764 W SE 9300764W WO 9407382 A1 WO9407382 A1 WO 9407382A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- fraction
- tobacco
- process according
- nicotine
- liquid fraction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Ceased
Links
Classifications
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/24—Treatment of tobacco products or tobacco substitutes by extraction; Tobacco extracts
Definitions
- the present invention relates to a processing method for
- a treating green tobacco plants or parts thereof for obtaining a crude tobacco product also relates to the product obtained by the method.
- Green tobacco plants i.e. immature tobacco plants, or parts of green tobacco plants are normally not used in the manufacture of crude tobacco material. Irrespective of whether the whole of the tobacco plant is used or whether only the leaves of the tobacco plant are used,
- a favourable climate would also allow more than one crop to be harvested each season.
- the present invention relates to the manu ⁇ facture of a crude tobacco material for smokable or smokeless nicotine-containing products of changed compo- sition but with taste and aroma of tobacco.
- the inven ⁇ tion also relates to the product obtained by the pro- cess ,
- One object of the invention is to provide a different and improved product containing reduced amounts of those components which may form undesirable substances when burning.
- Another object of the invention is to enable whole tobacco plants to be used, since this simplifies the process and improves the yield.
- Another object of the invention is to enable green, i.e. immature tobacco, to be used, so as to shorten the tobacco plant cultivation time, thereby enabling tobacco cultivation zones to be extended and several harvests to be obtained during one and the same season.
- Still another object of the invention is to enable the separation of such by-products as those which can be either used directly or processed to form valuable products.
- a further object of the invention is to enable the manufacture of a crude tobacco material of reduced mutagenicity as defined according to Ames test, for instance, and having a low TSNA (Tobacco Specific Nitrosamines) content.
- TSNA tobacco Specific Nitrosamines
- the aforesaid ob ⁇ jects are achieved with a process for treating green tobacco that comprises conversion of the tobacco plant material to a pulp and dividing the pulp into a solid, coarse fraction and a liquid fraction. Suspended or emulsified fine materials in the liquid fraction are removed therefrom, therewith obtaining a pigment-con ⁇ taining leaf nutrient concentrate which, with the aid of various extraction processes, is divided into a plurality of pigment fractions which subsequent to being appropriately processed are wholly or partly returned to the first coarse solid fraction.
- the proteins present in the liquid fraction that remains subsequent to separating the leaf nutrition concentrate therefrom are removed either totally or partially, whereafter the deproteinized liquid fraction is processed while retain ⁇ ing the nicotine, so as to obtain a concentrated liquid phase, so-called brown juice, which contains nicotine, flavourants and colourants.
- This concentrated liquid phase is then returned to the solid, coarse fraction, optionally together with other additives, so as to obtain the desired crude tobacco material.
- US-A-4,343,317 describes a process for treating whole green tobacco leaves, by expressing protoplasmic juice from the leaves and artificially curing the pulp ob ⁇ tained.
- Suitable artificial curing methods are said to be 1) thermal browning by drying at ambient temperature and subsequent heating to a temperature of 190°C for 15 minutes; 2) photobleaching, optionally after pretreating the pulp with steam, alcohol, etc., followed by thermal browning; 3) exposure of the tobacco pulp to SO -gas, so as to remove green pigment and flavourants; and 4) soaking pressed tobacco in an acidic medium (pH 1.5-3.5) and incubating the soaked pulp at elevated temperature, preferably at a temperature of about 50°C, until the green colour has disappeared.
- an acidic medium pH 1.5-3.5
- the expressed juice can be processed to remove different components therefrom, e.g. proteins, and/or to develop the flavourants, and is then returned to the artificially cured pulp.
- one advantage is that whole green tobacco leaves can be used in the process without disintegrating the leaves. As whole green tobacco leaves are used, only a limited removal of protoplasmic juice from the tobacco leaves is obtained and the final product of the present invention cannot therefore be obtained.
- a further disadvantage is the difficulty in the processing operations.
- the earlier mentioned US-A-4,289,147 describes a process for treating tobacco, including green tobacco, in order to obtain a crude tobacco material from which protein, nicotine and green pigment have been removed.
- the tobacco is converted into a pulp which is divided into a liquid fraction and a solid coarse fraction.
- the liquid fraction from which finely particulate material has first been removed and which contains water-soluble plant material, is treated for the removal of proteins and nicotine.
- Pigment is removed from the finely particulate material and divided into green and non-green pigments.
- the coarse fibre fraction which has been decoloured by extraction of green and non-green pigments, is then combined with non-green pigments obtained in earlier stages and the liquid frac ⁇ tion, from which nicotine and protein have been removed.
- the method described in the introduction for treating green tobacco yields a high-grade crude tobacco product which when smoked has strikingly lowered mutagenicity, for instance according to Ames test.
- the process also gives a low TSNA content in the tobacco product. It is also well suited for commercial use.
- the present invention thus relates to a process for treating tobacco plant material so as to obtain crude tobacco material intended for smokable and smoke-free nicotine-containing products which have considerably reduced mutagenicity and a low TSNA content when used, said process comprising
- step (f) suspending the fraction IV obtained from step (c) in alcohol or some other water-miscible solvent and hydrolyzing the suspension, suitably while adding a base, and then evaporating the solvent partially and extracting the residue with non-polar solvent, whereafter a fraction (VIII) containing yellow-orange pigment is separated from a basic fraction (IX) contain- ing green pigment;
- step (h) precipitating from the aqueous phase (XI) obtained in step (g) modified green pigment (XII) which, after suitable treatment, forms chlorophyll-derived colourants and flavourants (XIII) ; and (i) combining the fraction (I) obtained in step (b) , optionally after heating and drying said fraction, with the fractions VII and VIII and optionally also with the fraction X and/or the fraction XIII, thereby obtaining a crude tobacco for the smoking product or the smoke-less product.
- modified green pigment XII
- XIII chlorophyll-derived colourants and flavourants
- Green tobacco is used as the starting material when practicing the inventive process.
- Whole tobacco plants or parts thereof, for instance the leaves, can be used.
- whole tobacco plants are used, especially when the tobacco has been harvested at an early growth stage.
- the plant material is disintegrated in step (a) to form a pulp, optionally with the addition of water.
- Disintegration is effected in a conventional manner, for instance by crushing or grinding the plant material. This disintegration process releases the liquid phase containing water-soluble growth material from the coarse, solid material.
- the disintegration process can be carried out in the presence of suitable additives, such as antioxidants, for instance reducing agents, to prevent oxidation of the polyphenols present.
- step (b) The division in step (b) is effected in a conventional manner.
- the pulp is preferably pressed, so as to sepa ⁇ rate a press juice or green juice (fraction (II) ) from the press cake (fraction (I)).
- Fraction (I) is kept for use in the final process step, and is preferably dried with the purpose of preserving the fraction so as to avoid its quality being impaired due to bacterial and/or mould growth during the storage period, for instance.
- the green juice (fraction (II) ) containing water-soluble plant material and suspended or emulsified fine material may be divided directly in accordance with step (c) into the liquid fraction (III) and the fraction (IV) contain ⁇ ing the fine material.
- the fraction (IV) is normally referred to as leaf nutrient concentrate (LNC) .
- the green juice (fraction (II)) is heated to a temperature of at most 55°C and preferably from 40-45°C prior to step (c) . Heating of the juice results in partial coagulation of fine, green-pigment material, thereby facilitating separation of this material togeth ⁇ er with other substances constituting LNC in the follow ⁇ ing separation step (c) .
- step (c) The separation effected in step (c) is carried out with conventional techniques, for instance centrifugation or filtration.
- conventional techniques for instance centrifugation or filtration.
- centrifugation or filtration In case the aforesaid heat treatment process is carried out, in general moderate centrifugal forces are sufficient to achieve separation.
- Proteins are then removed from the liquid fraction (III) . It is known that proteins give rise to an im ⁇ paired flavour (Schmuck index) when smoking, for instance, a cigarette. Mutagenic substances may also form when burning proteins. It is therefore desirable to remove proteins completely or at least partially from the crude tobacco material. This can be achieved by removing proteins in the form of one or more protein fractions. When the proteins are separated in the form of a single fraction (V) , this is preferably achieved by heating the liquid fraction (III) to a temperature at which all proteins will coagulate, i.e. at a lowest temperature of 52°C and preferably at a temperature of from 75-85°C. The fraction (V) can then be separated, for instance by centrifugation. Alternatively, the proteins can be precipitated by acidification, suitably to a pH-value of 4.5 or less.
- the pH-value of the liquid fraction (VI) which thus contains no proteins or has a reduced protein content, is then adjusted in step (e) to a suitable value, where ⁇ after certain components present in this fraction are optionally oxidized.
- a suitable pH-range is from 3 to 4, and particularly a pH-value of 3, which can be obtained by adding phosphoric acid.
- other acids can be used, such as citric acid, succinic acid and other organic acids.
- Oxidation is effected by adding an oxidant at room temperature or preferably at a higher temperature, e.g. a temperature in the region of 30-100°C, preferably 70-
- a suitable oxidant is H O .
- Other oxidants that
- organic peracids can be used are organic peracids.
- the oxidation process results in at least partial oxida ⁇ tion of aromatics to obtain a quinoid-type structure. This corresponds to the oxidation that occurs during conventional curing of tobacco by air-drying the tobacco.
- the leaf nutrient concentrate (LNC), i.e. fraction (IV), is processed in accordance with the invention in the steps (f)-(h) to recover valuable products, which can be returned to the fraction (I) and/or used in some other way.
- the green pigment when processed the green pigment also produces a valuable product (fraction (XIII)).
- the fraction (IV) is suspended in step (f) in alcohol, e.g. methanol, ethanol or isopropanol, or in some other water-miscible solvent.
- alcohol e.g. methanol, ethanol or isopropanol
- This solubilizes the leaf pig ⁇ ments and decolourizes LNC, which becomes suitable as animal feed rich in protein and starch.
- green pigment is insoluble in water, the dissolved pigments are hydrolyzed, e.g. at ambient temperature, by adding a base, for instance an alkali hydroxide, such as potassium hydroxide.
- the alcohol used is suitably etha ⁇ nol, e.g. in an amount which gives a solution containing 60-85 % ethanol by volume.
- the residue is extracted with a non-polar solvent, e.g. heptane.
- a non-polar solvent e.g. heptane.
- the isolated fraction (VIII) thus contains yellow-orange pigment dissolved in the non-polar sol ⁇ vent.
- Extraction is suitably effected at ambient tem ⁇ perature.
- the hydrolysis is also carried out at ambient temperature, even though an elevated tempera ⁇ ture may be used, for instance to accelerate the process of hydrolysis.
- aqueous solvent fraction (IX) containing dissolved green pigment is then extracted with a polar, water- immiscible solvent, to separate a polar pigment (frac ⁇ tion (X)).
- a suitable solvent is ethyl acetate.
- water-immiscible solvent it is meant that the solvent is essentially immiscible with water. Solvents which are included in this term may thus be miscible with water to a certain extent, namely up to about 10%.
- the polar pigment is comprised of xanthophyll.
- a modified green pigment is then precipitated from the remaining aqueous fraction (XII) comprising green pig ⁇ ment, with the aid of some suitable precipitating agent, such as iron compounds including ferric nitrate, ferric citrate, ferric acetate, ferric formate, ferric oxide and corresponding ferrous compounds under acidic condi- tions.
- suitable precipitating agent such as iron compounds including ferric nitrate, ferric citrate, ferric acetate, ferric formate, ferric oxide and corresponding ferrous compounds under acidic condi- tions.
- This precipitation may cause the green colour to convert to another colour, e.g. black when the precipitation process is effected with an iron compound.
- This modified "green pigment” is then further processed, whereby chlorophyll-derived colourants and flavourants (fraction (XIII)) are obtained.
- This processing of the modified "green pigment” involves oxidation and esterification. Initially the black precipitate is solubilized in acetic acid to which H 2 0 2 is added, and the mixture is refluxed at 108-110°C for 30 minutes, and is then cooled. To the same mixture, propanol is added for esterification in the presence of a small amount of sulfuric acid. The resulting solution contains chlorophyll derivatives with a reddish brown colour and is neutralized to a pH of 6 to 7 with a base, such as potassium hydroxide.
- a base such as potassium hydroxide.
- the final step of the inventive method involves combin ⁇ ing the fraction (I) with the brown juice (fraction (VII)) and optionally also with other fractions obtained in previous method steps.
- it can be achieved by spraying the brown juice and/or other liquid fractions over the fraction (I) while mixing said frac ⁇ tion and said juice and/or other liquid fractions to- gether, e.g. by rotation.
- An elevated temperature of 80- 100°C is preferably used.
- Non-liquid fractions which are to be returned to the fraction (I) are dissolved in an appropriate solvent, for instance an alcohol, such as ethanol, and then sprayed over the fraction (I) , as des ⁇ cribed above.
- the solid phase (fraction I) was washed with water, and diluted with three to four times as much water while stirring, and then was again passed through a screw press so as to obtain a solid phase and a liquid phase, this latter phase being discarded.
- the solid phase was fluffed, and optionally disintegrated, in a refiner, prior to being dried to 90% dry solids with heat, in a conventional manner.
- the resultant solid material i.e. the treated fraction (I)
- the fraction (I) was divided into two further fractions, namely a fibrous, long fraction, called Fibre A in the table below, (120 kg) , and a small tobacco fraction (110 kg) .
- the former fraction was used as a reference materi ⁇ al for evaluating smoking properties. The results from these evaluations are set forth in Table I below.
- Green juice (fraction II) from the first pressing pro ⁇ cess was adjusted to a pH of 5.15 with phosphoric acid and heated to 45°C. This temperature was maintained for about ten minutes, whereafter the precipitated fine material, the leaf nutrient concentrate (fraction IV) (240 kg, 28% dry solids) , was separated by decanting from the aqueous phase (III) , also designated yellow juice.
- Carbon dioxide (g) was added to the resultant aqueous phase until saturation was reached, the Fl-proteins precipitating or crystallizing and being separated from the juice by centrifugation or filtration.
- the remaining, soluble proteins were coagulated, by adjusting the pH of the juice to 3.5 with phosphoric acid (the juice was allowed to stand for about one hour and the F2-proteins were then separated from the liquid phase (fraction VI) , i.e. the brown juice, by centrifu- gation or filtration.
- the pH-value of the brown juice was adjusted to 3 by adding phosphoric acid, and 30-percent hydrogen peroxide was added (200:1, based on volume), whereafter the brown juice was heated at 80°C over night.
- the brown juice was concentrated to a dry solids content of 50% (fraction VII) , and could then be stored for later use. This concentrated brown juice (fraction VII) is designated BJ A in the following.
- the green juice (fraction II) from the first pressing process was adjusted to a pH of 3.5, by adding phosphoric acid, and was then heated to a temperature of 75°C, this temperature being maintained for about fif ⁇ teen minutes, whereafter the precipitated fine material (175 kg, 28% dry solids) (fraction (IV) + (V)) was separated by decanting said material from the aqueous phase (the brown juice) (fraction (VI)).
- the brown juice (VI)) was adjusted to a pH-value of 3 with phosphoric acid, and 30-percent hydrogen peroxide was added (200:1, based on volume), whereafter the brown juice was heated to a temperature of 80°C, this tempera ⁇ ture being maintained over night.
- the brown juice was then concentrated to 80% dry solids and could then be stored for later use.
- This concentrated brown juice fraction (VII)
- BJ B was added to the long fibrous material.
- Fibre A obtained from Example 1, in a propor ⁇ tion of 4 kg dry solids brown juice to 10 kg dry solids of solid material, whereafter the material obtained was dried to 14-18% dry solids and filterless cigarettes were manufactured in a conventional cigarette machine.
- Cigarettes were also manufactured from the fibrous, long material obtained above from the fully grown plants (Fibre B) .
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacture Of Tobacco Products (AREA)
Abstract
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| AU51221/93A AU5122193A (en) | 1992-10-01 | 1993-09-22 | A method for treating green tobacco and the product obtained thereby |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SE9202876-0 | 1992-10-01 | ||
| SE9202876A SE501394C2 (sv) | 1992-10-01 | 1992-10-01 | Förfaranden för behandling av grön tobak och därmed erhållen produkt |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| WO1994007382A1 true WO1994007382A1 (fr) | 1994-04-14 |
Family
ID=20387355
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/SE1993/000764 Ceased WO1994007382A1 (fr) | 1992-10-01 | 1993-09-22 | Procede de traitement de tabac vert et produit ainsi obtenu |
Country Status (3)
| Country | Link |
|---|---|
| AU (1) | AU5122193A (fr) |
| SE (1) | SE501394C2 (fr) |
| WO (1) | WO1994007382A1 (fr) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0967898A4 (fr) * | 1996-08-05 | 2000-01-05 | Jonnie R Williams | Procede de traitement du tabac pour reduire la teneur en nitrosamines et produits ainsi fabriques |
| US6202649B1 (en) | 1996-12-02 | 2001-03-20 | Regent Court Technologies | Method of treating tobacco to reduce nitrosamine content, and products produced thereby |
| US6311695B1 (en) | 1996-06-28 | 2001-11-06 | Regent Court Technologies | Method of treating tobacco to reduce nitrosamine content, and products produced thereby |
| USRE38123E1 (en) | 1996-06-28 | 2003-05-27 | Regent Court Technologies, Llc. | Tobacco products having reduced nitrosamine content |
| US6805134B2 (en) | 1999-04-26 | 2004-10-19 | R. J. Reynolds Tobacco Company | Tobacco processing |
| WO2020148704A1 (fr) * | 2019-01-18 | 2020-07-23 | R. J. Reynolds Tobacco Company | Purification de protéines rubisco dérivées de plantes |
| CN113826942A (zh) * | 2021-10-29 | 2021-12-24 | 云南中烟新材料科技有限公司 | 一种甜感特征晾晒烟提取物的制备方法及晾晒烟叶的加工方法 |
| CN117617543A (zh) * | 2023-12-19 | 2024-03-01 | 山东中烟工业有限责任公司 | 一种提升茄衣烟叶颜色均匀度的发酵介质 |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9420825B2 (en) * | 2012-02-13 | 2016-08-23 | R.J. Reynolds Tobacco Company | Whitened tobacco composition |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4289147A (en) * | 1979-11-15 | 1981-09-15 | Leaf Proteins, Inc. | Process for obtaining deproteinized tobacco freed of nicotine and green pigment, for use as a smoking product |
| US4343317A (en) * | 1980-12-09 | 1982-08-10 | Philip Morris Incorporated | Method of treating green tobacco |
-
1992
- 1992-10-01 SE SE9202876A patent/SE501394C2/sv not_active IP Right Cessation
-
1993
- 1993-09-22 AU AU51221/93A patent/AU5122193A/en not_active Abandoned
- 1993-09-22 WO PCT/SE1993/000764 patent/WO1994007382A1/fr not_active Ceased
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4289147A (en) * | 1979-11-15 | 1981-09-15 | Leaf Proteins, Inc. | Process for obtaining deproteinized tobacco freed of nicotine and green pigment, for use as a smoking product |
| US4343317A (en) * | 1980-12-09 | 1982-08-10 | Philip Morris Incorporated | Method of treating green tobacco |
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| USRE38123E1 (en) | 1996-06-28 | 2003-05-27 | Regent Court Technologies, Llc. | Tobacco products having reduced nitrosamine content |
| US6311695B1 (en) | 1996-06-28 | 2001-11-06 | Regent Court Technologies | Method of treating tobacco to reduce nitrosamine content, and products produced thereby |
| US6338348B1 (en) | 1996-06-28 | 2002-01-15 | Regent Court Technologies | Method of treating tobacco to reduce nitrosamine content, and products produced thereby |
| US6135121A (en) * | 1996-06-28 | 2000-10-24 | Regent Court Technologies | Tobacco products having reduced nitrosamine content |
| EP0967898A4 (fr) * | 1996-08-05 | 2000-01-05 | Jonnie R Williams | Procede de traitement du tabac pour reduire la teneur en nitrosamines et produits ainsi fabriques |
| US6202649B1 (en) | 1996-12-02 | 2001-03-20 | Regent Court Technologies | Method of treating tobacco to reduce nitrosamine content, and products produced thereby |
| US6425401B1 (en) | 1996-12-02 | 2002-07-30 | Regent Court Technologies Llc | Method of treating tobacco to reduce nitrosamine content, and products produced thereby |
| US6805134B2 (en) | 1999-04-26 | 2004-10-19 | R. J. Reynolds Tobacco Company | Tobacco processing |
| US7404406B2 (en) | 1999-04-26 | 2008-07-29 | R. J. Reynolds Tobacco Company | Tobacco processing |
| US6895974B2 (en) | 1999-04-26 | 2005-05-24 | R. J. Reynolds Tobacco Company | Tobacco processing |
| WO2020148704A1 (fr) * | 2019-01-18 | 2020-07-23 | R. J. Reynolds Tobacco Company | Purification de protéines rubisco dérivées de plantes |
| US11523623B2 (en) | 2019-01-18 | 2022-12-13 | R.J. Reynolds Tobacco Company | Plant-derived protein purification |
| CN113826942A (zh) * | 2021-10-29 | 2021-12-24 | 云南中烟新材料科技有限公司 | 一种甜感特征晾晒烟提取物的制备方法及晾晒烟叶的加工方法 |
| CN113826942B (zh) * | 2021-10-29 | 2022-06-21 | 云南中烟新材料科技有限公司 | 一种甜感特征晾晒烟提取物的制备方法及晾晒烟叶的加工方法 |
| CN117617543A (zh) * | 2023-12-19 | 2024-03-01 | 山东中烟工业有限责任公司 | 一种提升茄衣烟叶颜色均匀度的发酵介质 |
Also Published As
| Publication number | Publication date |
|---|---|
| SE501394C2 (sv) | 1995-02-06 |
| SE9202876D0 (sv) | 1992-10-01 |
| SE9202876L (sv) | 1994-04-02 |
| AU5122193A (en) | 1994-04-26 |
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