CN111528518B - Low-nicotine tobacco extract, preparation method thereof and special tobacco tar for cigarette without burning under heating - Google Patents
Low-nicotine tobacco extract, preparation method thereof and special tobacco tar for cigarette without burning under heating Download PDFInfo
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- CN111528518B CN111528518B CN202010360295.9A CN202010360295A CN111528518B CN 111528518 B CN111528518 B CN 111528518B CN 202010360295 A CN202010360295 A CN 202010360295A CN 111528518 B CN111528518 B CN 111528518B
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- tobacco
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- extraction
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- 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
- A24B15/241—Extraction of specific substances
- A24B15/243—Nicotine
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- 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
- A24B15/10—Chemical features of tobacco products or tobacco substitutes
- A24B15/16—Chemical features of tobacco products or tobacco substitutes of tobacco substitutes
- A24B15/167—Chemical features of tobacco products or tobacco substitutes of tobacco substitutes in liquid or vaporisable form, e.g. liquid compositions for electronic cigarettes
-
- 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
- A24B15/26—Use of organic solvents for extraction
Abstract
The invention provides a low-nicotine tobacco extract, a preparation method thereof and special tobacco tar for a cigarette without burning by heating, wherein the preparation method of the low-nicotine tobacco extract comprises the following steps: extraction: leaching the tobacco raw material by using an ethanol solution, performing solid-liquid separation after leaching to obtain a leaching liquor, and centrifuging the leaching liquor to obtain a tobacco extracting solution; concentration: concentrating the tobacco extract under reduced pressure to obtain tobacco alcohol extract; alkalizing and extracting: adding ammonia water into the tobacco alcohol extract, stirring uniformly, and mixing with an organic solvent for extraction; and (3) purification: separating liquid after extraction to obtain an organic phase and a water phase; mixing the water phase with ethanol solution, stirring, and concentrating under reduced pressure to obtain low nicotine tobacco extract. The preparation method has simple process requirements and high yield, and is suitable for mass production. The tobacco extract prepared by the method has low nicotine content and obvious tobacco fragrance, and can be used for preparing cigarettes which are not combusted by heating.
Description
Technical Field
The invention relates to a tobacco technology, in particular to a low-nicotine tobacco extract, a preparation method thereof and special tobacco tar for a cigarette which is not burnt by heating.
Background
The cigarette heated at low temperature without burning meets the experience of smoking the traditional cigarette by heating the tobacco in the form of cut tobacco, and the harm of tobacco products to human bodies is greatly reduced because the content of harmful substances in smoke is controllable and is lower than that of the common cigarette, thereby attracting more attention of the market.
The styles of the heating non-combustion cigarettes on the market at present mainly comprise original tobacco flavor, mint flavor and fruit flavor. The tobacco tar is formed by mixing various tobacco aroma-producing extracts, can enhance the herbal aroma of the tobacco, obviously increases the aroma amount and concentration of the non-combustible cigarette, and is an important additive for forming the brand style of the cigarette. But the tobacco extract is generally prepared by using water or organic solvent, supercritical CO2And extracting the whole soluble components of the tobacco raw materials by molecular distillation and the like, and introducing high-content nicotine along with aroma substances into the cigarette formula. In the formula of the low-temperature non-burning cigarette, when the amount of the tobacco extract is high, the nicotine proportion is too high, so that the cigarette is stiff and has increased irritation, choking and stinging can be generated in the mouth and the throat, and the harm to a human body is serious; when the amount of the tobacco extract is low, the cigarette cannot give out the herbal fragrance of the tobacco, and the smoking experience cannot be met.
Therefore, it is very important to reduce the nicotine content of the tobacco extract special for the cigarette which is not burnt when being heated.
Disclosure of Invention
The invention aims to provide a preparation method of a low-nicotine tobacco extract, aiming at the problem of higher nicotine content of the tobacco extract in the existing low-temperature non-burning cigarette formula.
In order to achieve the purpose, the invention adopts the technical scheme that: a method for preparing a low nicotine tobacco extract comprises the following steps:
(1) extraction: leaching the tobacco raw material by using an ethanol solution, performing solid-liquid separation after leaching to obtain a leaching liquor, and centrifuging the leaching liquor to obtain a tobacco extracting solution;
(2) concentration: concentrating the tobacco extract under reduced pressure to obtain tobacco alcohol extract, and recovering ethanol;
(3) alkalizing and extracting: adding ammonia water into the tobacco alcohol extract, stirring uniformly, and mixing with an organic solvent for extraction;
(4) and (3) purification: separating the liquid after extraction to obtain an organic phase and a water phase, and distilling the organic phase to recover the organic solvent; mixing the water phase with ethanol solution, stirring, and concentrating under reduced pressure to obtain low nicotine tobacco extract.
Further, the tobacco raw material in the step (1) is prepared by crushing tobacco leaves, and the particle size of the tobacco raw material is 40-80 meshes.
Further, the mass ratio of the tobacco raw material to the ethanol solution in the step (1) is 1:7-1: 10; the concentration of the ethanol solution is 70-80% (v/v).
Further, in the step (1), the leaching temperature is 50-65 ℃, and the leaching time is 1-2 h; the rotation speed of the centrifugal machine adopted by the centrifugation is 2500-.
Further, in the step (2), the reduced pressure concentration temperature is 60-75 ℃, the vacuum degree is 0.07-0.08Mpa, the solid content of the tobacco alcohol extract is 55-65%, and the solid content is the mass percentage content of the solid content of the pasty liquid. In the present invention,% represents a mass percentage unless otherwise specified.
Further, the mass ratio of the tobacco alcohol extract to ammonia water in the step (3) is 1:1-3, the concentration of the ammonia water is 25% -28%, and the stirring time is 5-10 min.
Further, in the step (3), the organic solvent is one or more of petroleum ether, ethyl acetate, dichloromethane and n-hexane, the mass ratio of the tobacco alcohol extract to the organic solvent is 1:2-4, and the extraction time is 0.5-2 h.
Further, the mass ratio of the water phase to the ethanol solution in the step (4) is 1:1-2, the concentration of the ethanol solution is 45-60% (v/v), and the stirring time is 15-30 min. The concentration of ethanol in the step (4) is lower than that of the ethanol solution in the step (1), and because ammonia water and an organic solvent are remained in the water phase after extraction, the ammonia water and the organic solvent can be dissolved in the ethanol solution and can be removed along with the evaporation of ethanol during concentration.
Further, in the step (4), the reduced pressure concentration temperature is 60-75 ℃, the vacuum degree is 0.07-0.08Mpa, and the solid content of the low-nicotine tobacco extract is 58-62%.
The invention also discloses a low-nicotine tobacco extract which is prepared by adopting the preparation method of the low-nicotine tobacco extract. The extract can be used as tobacco oil in the formulation of cigarette without burning under heating.
The invention also discloses special tobacco tar for cigarette which is not combusted by heating, which comprises the low-nicotine tobacco extract. The tobacco tar is applied to a formula of the heating non-combustion cigarette (the proportion of the tobacco tar in the formula of the heating non-combustion cigarette is 30-40 percent, namely the coating rate is 30-40 percent), can obviously increase the aroma amount and the concentration of the cigarette on the premise of not increasing the strength and the irritation, and has the effects of better improving the quality and the experience of the heating non-combustion cigarette.
Further, the special tobacco tar for the heating non-combustion cigarette comprises 30-40 wt% of low-nicotine tobacco extract.
Further, the special tobacco tar for the cigarette which is not combusted by heating comprises the following components in parts by weight:
compared with the prior art, the low-nicotine tobacco extract, the preparation method thereof and the special tobacco tar for heating non-combustible cigarettes have the following advantages:
(1) the preparation method of the low-nicotine tobacco extract is scientific and reasonable. According to the invention, based on the principle of nicotine solubility (alkaline solution < organic solvent), the sequence of nicotine transfer is as follows: tobacco raw material → tobacco alcohol extract → ammonia water → organic solvent, and finally most of nicotine is removed by extraction, so that the tobacco extract with low nicotine, good aroma quality and good aroma quantity is prepared.
(2) The nicotine is transferred by liquid-liquid extraction, the temperature in the concentration stage is low, and the loss of the aroma components of the extract is small; the consumption of nicotine, ammonia water and organic solvent is low, the pollution is small and the recovery rate is high after the tobacco extract is concentrated into alcohol extract.
(3) In the alkalization stage, ammonia water with weak alkalinity and low boiling point is used and is heated to decompose to generate ammonia water and water. The tobacco extract is heated in the final concentration stage to almost completely remove ammonia gas, and the sensory quality of the final product is not affected.
(4) The nicotine content of the low-nicotine tobacco extract is low, can be as low as 0.05-0.2 wt%, and is far lower than 2-5 wt% of the nicotine content of the common tobacco extract. The tobacco tar prepared by the low-nicotine tobacco extract can be added into a large amount of cigarettes which are not combusted under heating, so that the cigarettes can obviously retain the herbal fragrance of the cigarettes, the fragrance quality is improved without increasing strength and irritation basically, and the harm to a human body is light.
Detailed Description
The invention is further illustrated by the following examples:
example 1
The embodiment discloses a method for preparing a low-nicotine tobacco extract from tobacco raw materials in the Pitch area of Guizhou, which comprises the following specific steps:
(1) extraction: crushing the tobacco raw material with the mass m, sieving the crushed tobacco raw material with a 40-mesh sieve, mixing the crushed tobacco raw material with an ethanol solution (70 percent, v/v) with the mass of 7m, and extracting the mixture for 1 hour at the temperature of 50 ℃; and (4) carrying out solid-liquid separation after extraction, and centrifuging the liquid for 5min at the rotation speed of 2500rpm to obtain the tobacco extract.
(2) Concentration: concentrating the tobacco extractive solution at 60 deg.C under reduced pressure until the solid content is 60%, to obtain tobacco ethanol extract, and recovering ethanol.
(3) Alkalizing and extracting: adding ammonia water (with concentration of 25%) with mass of 2n into the tobacco alcohol extract with mass of n, and stirring for 5 min; then mixing with petroleum ether with the mass of 3n, and extracting for 1 h.
(4) And (3) purification: separating liquid after extraction to obtain an organic phase and a water phase, and distilling the organic phase to recover petroleum ether; mixing the water phase with 3n ethanol solution, and stirring for 15 min; concentrating under reduced pressure at 60 deg.C to obtain tobacco extract with low nicotine content of 60%.
The content of nicotine in the tobacco extract obtained by the invention is 0.10 wt%, and the tobacco extract can be added into a formula of a heating non-combustible cigarette as tobacco tar in a large amount, so that the aroma amount and concentration of the cigarette can be obviously increased on the premise of not increasing strength and irritation, and the tobacco extract has the effects of better improving the quality and experience of the heating non-combustible cigarette.
Example 2
The embodiment discloses a method for preparing a low-nicotine tobacco extract from tobacco raw materials in Guizhou Zunyi areas, which comprises the following specific steps:
(1) extraction: crushing the tobacco raw material with the mass m, sieving the crushed tobacco raw material with a 60-mesh sieve, mixing the crushed tobacco raw material with an ethanol solution (75 percent, v/v) with the mass of 8m, and extracting the mixture for 1.5 hours at the temperature of 60 ℃; and (4) carrying out solid-liquid separation after extraction, and centrifuging the liquid for 10min at the rotating speed of 3000rpm to obtain the tobacco extracting solution.
(2) Concentration: concentrating the tobacco extractive solution at 65 deg.C under reduced pressure until the solid content is 65%, to obtain tobacco ethanol extract, and recovering ethanol.
(3) Alkalizing and extracting: adding ammonia water (with concentration of 26%) with mass of 1.5n into the tobacco alcohol extract with mass of n, and stirring for 5 min; then mixed with ethyl acetate with the mass of 3n, and extracted for 2 h.
(4) And (3) purification: separating the liquid after extraction to obtain an organic phase and a water phase, and distilling the organic phase to recover ethyl acetate; mixing the water phase with 3n ethanol solution, and stirring for 30 min; concentrating under reduced pressure at 70 deg.C to obtain tobacco extract with low nicotine content of 60%.
The content of nicotine in the tobacco extract obtained by the invention is 0.08 wt%, and the tobacco extract can be added into a formula of a heating non-combustible cigarette as tobacco tar in a large amount, so that the aroma amount and concentration of the cigarette can be obviously increased on the premise of not increasing strength and irritation, and the tobacco extract has the effects of better improving the quality and experience of the heating non-combustible cigarette.
Example 3
The embodiment discloses a method for preparing a low-nicotine tobacco extract from tobacco raw materials in Yuxi region of Yunnan, which comprises the following specific steps:
(1) extraction: pulverizing tobacco raw material with mass m, sieving with 40 mesh sieve, mixing with 10m ethanol solution (75%, v/v), and extracting at 55 deg.C for 1.5 hr; and (4) carrying out solid-liquid separation after extraction, and centrifuging the liquid for 5min at the rotation speed of 3500rpm to obtain a tobacco extracting solution.
(2) Concentration: concentrating the tobacco extractive solution at 65 deg.C under reduced pressure until the solid content is 55%, to obtain tobacco ethanol extract, and recovering ethanol.
(3) Alkalizing and extracting: adding ammonia water (concentration is 28%) with mass of 1.5n into the tobacco alcohol extract with mass of n, and stirring for 10 min; then mixed with n-hexane with the mass of 2.5n, and extracted for 1.5 h.
(4) And (3) purification: separating the liquid after extraction to obtain an organic phase and a water phase, and distilling the organic phase to recover n-hexane; mixing the water phase with 3n ethanol solution, and stirring for 20 min; concentrating under reduced pressure at 70 deg.C to solid content of 65% to obtain low nicotine tobacco extract.
The content of nicotine in the tobacco extract obtained by the invention is 0.11 wt%, and the tobacco extract can be added into a formula of a heating non-combustible cigarette as tobacco tar in a large amount, so that the aroma amount and concentration of the cigarette can be obviously increased on the premise of not increasing strength and irritation, and the tobacco extract has the effects of better improving the quality and experience of the heating non-combustible cigarette.
Example 4
The embodiment discloses a method for preparing a low-nicotine tobacco extract by taking burley tobacco as a raw material, which comprises the following specific steps:
(1) extraction: crushing the tobacco raw material with the mass m, sieving the crushed tobacco raw material with a 60-mesh sieve, mixing the crushed tobacco raw material with an ethanol solution (80 percent, v/v) with the mass of 10m, and extracting the mixture for 2 hours at 65 ℃; and (4) carrying out solid-liquid separation after extraction, and centrifuging the liquid for 10min at the rotating speed of 6000rpm to obtain the tobacco extracting solution.
(2) Concentration: concentrating the tobacco extractive solution at 60 deg.C under reduced pressure until the solid content is 65%, to obtain tobacco ethanol extract, and recovering ethanol.
(3) Alkalizing and extracting: adding ammonia water (with concentration of 25%) with mass of 2n into the tobacco alcohol extract with mass of n, and stirring for 5 min; then mixing with petroleum ether with the mass of 1.5n, and extracting for 1 h.
(4) And (3) purification: separating liquid after extraction to obtain an organic phase and a water phase, and distilling the organic phase to recover petroleum ether; mixing the water phase with 3n ethanol solution, and stirring for 15 min; concentrating under reduced pressure at 65 deg.C to solid content of 55% to obtain low nicotine tobacco extract.
The content of nicotine in the tobacco extract obtained by the invention is 0.15 wt%, and the tobacco extract can be added into a formula of a heating non-combustible cigarette as tobacco tar in a large amount, so that the aroma amount and concentration of the cigarette can be obviously increased on the premise of not increasing strength and irritation, and the tobacco extract has the effects of better improving the quality and experience of the heating non-combustible cigarette.
Example 5
The embodiment discloses tobacco tar special for cigarette heating and non-combustion, which comprises any one of the low-nicotine tobacco extracts in the embodiments 1-4.
The special tobacco tar for the non-burning cigarette comprises the following components in parts by weight:
the special tobacco tar for the non-combustible heating cigarette accounts for 30 wt% of the formula of the non-combustible heating cigarette. The cigarette prepared by the embodiment has good quality and experience.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (3)
1. A preparation method of a low-nicotine tobacco extract is characterized by comprising the following steps:
(1) extraction: leaching the tobacco raw material by using an ethanol solution, performing solid-liquid separation after leaching to obtain a leaching liquor, and centrifuging the leaching liquor to obtain a tobacco extracting solution; the mass ratio of the tobacco raw material to the ethanol solution is 1:7-1: 10; the concentration of the ethanol solution is 70-80%; the leaching temperature is 50-65 ℃, and the leaching time is 1-2 h; the rotation speed of the centrifugal machine adopted by the centrifugation is 2500-;
(2) concentration: concentrating the tobacco extract under reduced pressure to obtain tobacco alcohol extract; the reduced pressure concentration temperature is 60-75 ℃, the vacuum degree is 0.07-0.08Mpa, and the solid content of the tobacco alcohol extract is 55-65%;
(3) alkalizing and extracting: adding ammonia water into the tobacco alcohol extract, stirring uniformly, and mixing with an organic solvent for extraction; the mass ratio of the tobacco alcohol extract to ammonia water is 1:1-3, the concentration of the ammonia water is 25% -28%, and the stirring time is 5-10 min; the organic solvent is one or more of petroleum ether, ethyl acetate, dichloromethane and n-hexane, the mass ratio of the tobacco alcohol extract to the organic solvent is 1:2-4, and the extraction time is 0.5-2 h;
(4) and (3) purification: separating liquid after extraction to obtain an organic phase and a water phase; mixing the water phase with an ethanol solution, uniformly stirring, and concentrating under reduced pressure to obtain a low-nicotine tobacco extract, wherein the mass ratio of the water phase to the ethanol solution is 1:1-2, the concentration of the ethanol solution is 45-60%, and the stirring time is 15-30 min; the reduced pressure concentration temperature is 60-75 deg.C, vacuum degree is 0.07-0.08Mpa, and the solid content of the low nicotine tobacco extract is 58-62%.
2. A low nicotine tobacco extract, characterized by being produced by the method for producing a low nicotine tobacco extract according to claim 1.
3. A tobacco tar, which is used for a cigarette and does not burn when heated, comprising the low-nicotine tobacco extract according to claim 2.
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| CN202010360295.9A CN111528518B (en) | 2020-04-30 | 2020-04-30 | Low-nicotine tobacco extract, preparation method thereof and special tobacco tar for cigarette without burning under heating |
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| CN202010360295.9A CN111528518B (en) | 2020-04-30 | 2020-04-30 | Low-nicotine tobacco extract, preparation method thereof and special tobacco tar for cigarette without burning under heating |
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| CN113170917A (en) * | 2021-04-30 | 2021-07-27 | 深圳市澳湾科技有限公司 | Electronic cigarette tobacco tar prepared from real tobacco |
| CN113881501A (en) * | 2021-11-08 | 2022-01-04 | 鹰潭华宝香精有限公司 | Preparation method for reducing nicotine content in refined Yunyan tobacco extract |
| CN114605384B (en) * | 2022-03-02 | 2023-11-21 | 湖南省烟草公司郴州市公司 | Method for extracting nicotine |
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| CN109512014A (en) * | 2017-09-18 | 2019-03-26 | 湖南中烟工业有限责任公司 | A method of the extraction nicotine from tobacco |
| CN110663992A (en) * | 2018-06-29 | 2020-01-10 | 平昌县响滩小学 | Tobacco extract preparation method, prepared tobacco extract and application |
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| GB754772A (en) * | 1954-05-24 | 1956-08-15 | Plate Ges Mit Beschraenkter Ha | Aromatic, mild tobacco with reduced nicotine content and process for the production thereof |
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