FI58049B - FOERFARANDE FOER TILLVARATAGANDE AV AROMAEMNEN UR TOBAK - Google Patents

Description

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Patent · och reglsterstyrelsen '' amöIcm utitgd oeh utUkrHwn pubikurad 29.08.80 (32) (33) (31) Pyrdstty «uolkaut —B * gtrd prlorltat 09.06.71

Federal Republic of Germany-Förb undsrepubliken Tyskland (DE) P 2128779.6

Styrkt (71) H.F. & Ph.F. Reemtsma, Parkstrasse 51 »2000 Hamburg 52, Federal Republic of Germany-Förbundsrepubliken Tyskland (DE) (72) Jurgen Gewe, Hamburg, Federal Republic of Germany-Förbundrepubliken Tyskland (DE) (7 ^) Oy Kolster Ab (5M Method for recovering tobacco flavorings - tobacco For the purposes of this Regulation, the flavoring means tobacco

The invention relates to a process for recovering flavorings from tobacco, in which the tobacco is subjected to an extraction treatment and the obtained extract is freed from undesired substances by treatment as a solvent having a polarity other than that of the extractant.

It is known to extract the tobacco with water and then also with alcohol and to treat the tobacco with these extracts after their possible pre-combination and concentration, which can be continued until a solvent-free residue is obtained. The purpose is to improve the taste of the tobacco treated with the extract or to change the smoke of its smoke to match the tobacco used in the extraction.

In the process according to FR patent 1,206,210, which is the starting point of the present invention, undesired components are removed from the obtained extract so that the extracted substances obtained with a less polar solvent are post-treated more strongly as a polar solvent. It is known from CH patent publication 276 709 to remove essential oils and resins from tobacco dust in the manufacture of tobacco by means of a solvent, apparently alcohol 2,58049, which is evaporated, the residue containing the essential oils and resins can be further purified by distillation and fractionation, also thought to eliminate the harmful or undesired components that came with the solution.

According to DE-A-1,517,252, tobacco is extracted, preferably in crude form, with highly cooled solvents, for example ice-water. The extract is allowed to solidify and dried by a freeze-drying method. A light brown product with a strong odor is formed, which is treated as a powder in amounts of 5 to 10% by weight or as a solution containing an equivalent amount, the aroma and taste of which are to be influenced.

Since the Fermon-treated tobacco to be treated used as a starting material in said process contains about 50% by weight of soluble ingredients and these ingredients must also be extracted for economic reasons, said maximum treatment of smoke-flavored tobacco increases by 10% by weight due to the excess powder. 20% by weight, but the overall taste level increases only by a relatively small amount, about 10%, whereby, however, the condensate content of the smoke of the tobacco products thus modified also increases correspondingly as a result of the increase in this soluble tobacco constituents.

Thus, a substantial and above all neutral increase in the condensate content of the smoke is not achieved.

The prior art further comprises the process according to DE-A-1 109 583, in which the solvent extract obtained from tobacco is reacted with, for example, alcohols and catalysts to obtain organoleptic substances from tobacco. Even with this method, it is not possible to obtain flavorings free of undesirable, non-flavoring, soluble additives.

The object of the invention is to provide a method by which it is possible to isolate natural flavoring substances from tobacco as free as possible from undesirable tracers and to make them as effective as possible, whereby precursors of such natural flavoring substances isolated together or alone are also recovered and converted into flavoring substances.

The invention is characterized in that only those components of the tobacco which are soluble in chloroform are isolated and that the residue remaining after removal of the solvent is heat-treated at 110-18 ° C, the heat treatment being maintained after reaching the treatment temperature for up to 9 hours.

3,58049

The invention is based on the finding that when extracting tobacco with carefully selected extractants, in addition to flavorings, a considerable amount of substances dissolves, which can be activated as flavorings by adding a heat treatment step to the extraction step.

The research underlying the invention has surprisingly shown that only 5 ~ 20% of the solids content of the extract, corresponding to about 2.5 ~ 10% of the dry weight of ordinary tobacco, imparts a taste to the smoke of a tobacco preparation prepared using the extract.

These extract solids also contain a surprisingly large amount of smoke flavor precursors that can be activated by appropriate heating. These activating agents are present in ordinary tobacco unused for flavor enhancement and form a latent flavor reserve that can be utilized in the method of the invention.

The extraction is conveniently carried out at a temperature between 1 + 5 ° and 85 ° C.

Although it has proved advantageous to heat treat the product obtained from the extracts as such, it is in principle also possible to heat the tobacco whose combustion properties are to be influenced after the heat-treated or non-heat-treated products obtained from the extracts have been added to the tobacco. In this case, the quality of the heat source and heat transfer is less relevant to the invention and only the duration of the heat treatment is mainly affected. Furthermore, in special cases, it may also be expedient to subject the tobacco used as a starting material to heat treatment in a suitable manner before extraction or to the extract before reprocessing.

In the following, the invention is presented in more detail by means of examples.

Example 1 50 g of dry tobacco from a tobacco mixture underlying a commercial cigarette brand was extracted with a solution of 270 g of pure isopropanol and 60 g of water corresponding to 82% by weight of isopropanol and the solvent was azeotroped off. The distillate consisted of 270 g of pure isopropanol and 100 g of water and corresponded to 310 g of 88% by weight of isopropanol. A 39 g aqueous extract residue containing 20 g of water and 19 g of dry matter, corresponding to 38% by weight of tobacco used, was recovered as a solution of 135 g of pure methanol and 10 g of water, corresponding to 82% by weight of methanol. including water in the extraction residue, and partitioned 3 times with 30 g of hexane each time. The amount of substance dissolved in hexane was 1.75 g, which corresponded to 3.5% by weight of tobacco used. The polar phase distillate was removed azeotropically to give a distillate containing 135 g of pure methanol and 17 g of water, corresponding to 152 g of 89% w / w methanol.

The aqueous residue contained 13 g of water and 17.25 g of dry matter and was taken up in 135 g of water and partitioned 3 times with 75 g of chloroform. The proportion of dry matter in the aqueous phase was 16.0 g, corresponding to 32.0 # of tobacco used, and in the chloroform phase, 1.25 g, corresponding to 2.5 # of tobacco used. The solvent-free residue from the chloroform phase was heated at 180 ° C for 5 minutes, developing a rich and excellent tobacco aroma that was superior to the aroma of both the quantity and quality of the tobacco used, giving the smoky taste of the tobacco sweeter and generally more pleasant effect.

Example 2 32 g of an air-conditioned tobacco blend based on a commercial cigarette brand with a moisture content of 15.5 # corresponding to 27 g of dry tobacco was shaken for 2b hours with 360 ml of ethyl acetate, the solvent was repeated and the extraction was repeated until the solvent was colorless. The combined extracts were evaporated to solvent free at 20 torr. The yield was 1.89 g of dry residue corresponding to 7% of the dried tobacco used and the residue was taken up in 25 ml of 85 volumes of aqueous methanol and partitioned 3 times with 8 ml of hexane. The solvent was removed from the hexane phases essentially in vacuo to give 8.86 g of a dry residue corresponding to 3.2% of the dry tobacco used.

The polar phases were evaporated in vacuo until the residue was practically free from methanol and contained a further 1.8 g of water. To this aqueous residue was added an additional 20 g of water, and then partitioned 3 times with 8 ml of chloroform. After separation of the chloroform phase and practically evaporation to dryness, 0.09 g of a residue corresponding to 1.8% of the dry tobacco used were obtained and, after heating for 7 minutes at 165 ° C, it developed a rich and strong tobacco aroma comparable in quality to that of the example. 1.

Example 3 50 g of dry tobacco dust was extracted in a solution of 270 g of pure isopropanol and 60 g of water corresponding to 330 g of 82 wt.% Isopropanol for 71 * hours and the solvent was azeotroped off. The aqueous extraction residue was obtained in 29.25 g and contained 20 g of water and 9.25 g of dry residue corresponding to 18.5% by weight of dry tobacco dust and was taken up in 135 g of pure methanol and 10 g of residual water corresponding to 82 g. 58049% by weight of methanol, taking into account the water contained in the extract residue, and partitioned 3 times with 30 g of hexane each time. The amount of substance dissolved in hexane was 1.5 g, corresponding to 3.0% by weight of tobacco dust used. The polar phase was azeotroped apart to give an aqueous residue containing 13 g of water and 7> 75 g of dry matter. This residue was taken up in 135 g of water and partitioned 3 times with 120 g of chloroform each time.

The dry matter content of the aqueous phase was 2.75 g corresponding to 5 to 5% by weight of the dry tobacco dust used and the dry matter content of the chloroform phase was 5 g corresponding to 10% of the tobacco dust used. The substantially solvent-free chloroform phase residue was heated to 155 ° C to develop a full and sweet tobacco aroma when treated with the starting tobacco and the smoky taste of the treated tobacco was significantly better than that of the untreated tobacco.

Example U

Example 1 was repeated except that the solvent-free residue from the chloroform phase was heated at 110 ° C for 9 hours. In the sensory experiment, the same impression was obtained, however, in that it felt like a beginning, but by no means significant, burnt taste.

Example 5 (Comparative Example corresponding to Example 3 of FR Patent 1,206,210) 50 g of cut tobacco of a commercial cigarette mixture were thoroughly extracted with diethyl ether under normal conditions. The solvent was evaporated to give 2.25 g of a residue which was taken up in 50 ml of hexane and partitioned between an equal volume of hexane-saturated (80%) ethanol solution. The solvent was removed from the polar phase to give 0.85 g of a residue which was taken up in 5 ml of 96 - # ethanol. 2.5 ml of this solution was diluted 1: 1 with water. The resulting diluted solution was used to treat tobacco from which the waxy components had been previously removed. As a result of a sensory comparison experiment (Food Research 13, 19U8, pp. 503-505), it was found that treated tobacco is slightly, yet occasionally, better than otherwise identical but untreated tobacco. The improvement is non-significant.

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