CN112011405A - High-nicotine tobacco extract, preparation method thereof and cigarette without burning by heating - Google Patents
High-nicotine tobacco extract, preparation method thereof and cigarette without burning by heating Download PDFInfo
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- CN112011405A CN112011405A CN202010729165.8A CN202010729165A CN112011405A CN 112011405 A CN112011405 A CN 112011405A CN 202010729165 A CN202010729165 A CN 202010729165A CN 112011405 A CN112011405 A CN 112011405A
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- 241000208125 Nicotiana Species 0.000 title claims abstract description 94
- 235000002637 Nicotiana tabacum Nutrition 0.000 title claims abstract description 94
- 239000000284 extract Substances 0.000 title claims abstract description 88
- 235000019504 cigarettes Nutrition 0.000 title claims abstract description 40
- 229960002715 nicotine Drugs 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000010438 heat treatment Methods 0.000 title abstract description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 57
- 239000002994 raw material Substances 0.000 claims abstract description 34
- 241000208134 Nicotiana rustica Species 0.000 claims abstract description 31
- 238000002386 leaching Methods 0.000 claims abstract description 21
- 238000002156 mixing Methods 0.000 claims abstract description 19
- 108090000790 Enzymes Proteins 0.000 claims abstract description 16
- 102000004190 Enzymes Human genes 0.000 claims abstract description 16
- 238000000605 extraction Methods 0.000 claims abstract description 16
- 239000007788 liquid Substances 0.000 claims abstract description 16
- SNICXCGAKADSCV-JTQLQIEISA-N (-)-Nicotine Chemical compound CN1CCC[C@H]1C1=CC=CN=C1 SNICXCGAKADSCV-JTQLQIEISA-N 0.000 claims abstract description 14
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000003960 organic solvent Substances 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000000926 separation method Methods 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 239000003513 alkali Substances 0.000 claims abstract description 11
- 239000012074 organic phase Substances 0.000 claims abstract description 9
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 239000012071 phase Substances 0.000 claims abstract description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 15
- 229940088598 enzyme Drugs 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 108010059892 Cellulase Proteins 0.000 claims description 10
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 10
- 108010059820 Polygalacturonase Proteins 0.000 claims description 10
- 229940106157 cellulase Drugs 0.000 claims description 10
- 108010093305 exopolygalacturonase Proteins 0.000 claims description 10
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 10
- 230000000694 effects Effects 0.000 claims description 9
- 239000007787 solid Substances 0.000 claims description 7
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000003208 petroleum Substances 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 239000000341 volatile oil Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims 1
- 239000003205 fragrance Substances 0.000 abstract description 8
- 239000000243 solution Substances 0.000 description 23
- 238000001816 cooling Methods 0.000 description 9
- 239000000796 flavoring agent Substances 0.000 description 7
- 235000019634 flavors Nutrition 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 230000003113 alkalizing effect Effects 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 238000007873 sieving Methods 0.000 description 3
- 230000000391 smoking effect Effects 0.000 description 3
- 235000013599 spices Nutrition 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000006286 aqueous extract Substances 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- 239000001814 pectin Substances 0.000 description 2
- 229920001277 pectin Polymers 0.000 description 2
- 235000010987 pectin Nutrition 0.000 description 2
- 230000001953 sensory effect Effects 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 244000018633 Prunus armeniaca Species 0.000 description 1
- 235000009827 Prunus armeniaca Nutrition 0.000 description 1
- 240000008866 Ziziphus nummularia Species 0.000 description 1
- 239000000443 aerosol Substances 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000469 ethanolic extract Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 235000011389 fruit/vegetable juice Nutrition 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 238000000622 liquid--liquid extraction Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000011837 pasties Nutrition 0.000 description 1
- 239000011802 pulverized particle Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000004505 smoke cartridge Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229940098465 tincture Drugs 0.000 description 1
- 235000019505 tobacco product Nutrition 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/025—Recovery by solvent extraction
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/0069—Heterocyclic compounds
- C11B9/0092—Heterocyclic compounds containing only N as heteroatom
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacture Of Tobacco Products (AREA)
Abstract
The invention provides a high nicotine tobacco extract, a preparation method thereof and a cigarette which is not combusted by heating, wherein the preparation method of the high nicotine tobacco extract comprises the following steps: mixing the crushed tobacco raw material with water, and adding an enzyme preparation for treatment; mixing and leaching the treated tobacco raw material with a high-concentration ethanol solution, performing solid-liquid separation after leaching to obtain a leaching solution, and filtering the leaching solution to obtain a tobacco clear solution; concentrating the tobacco clear liquid under reduced pressure to obtain a tobacco alcohol extract; adding alkali liquor into the tobacco alcohol extract, stirring uniformly, and mixing with an organic solvent for extraction; and separating the liquid after extraction to obtain an organic phase and a water phase, and concentrating the organic phase under reduced pressure to obtain the high nicotine tobacco extract. The high-nicotine tobacco extract prepared by the invention has higher nicotine content than the conventional tobacco extract, and has obvious tobacco original fragrance and strength. The cigarette added with a small amount of high nicotine tobacco extract without burning is rich in herbal fragrance and strength.
Description
Technical Field
The invention relates to a tobacco technology, in particular to a high-nicotine tobacco extract, a preparation method thereof and a heating non-combustible cigarette.
Background
The cigarette is a novel tobacco product, the reconstituted tobacco sheet is used as a cigarette cartridge, aerosol containing nicotine and other compounds is generated after the cigarette cartridge is heated within the temperature range of 200-300 ℃, the experience feeling similar to that of smoking a traditional cigarette is met, and the attention of the tobacco market is attracted more and more.
Currently, the styles of the cigarettes which are popular in the market and are not burned by heating are different, and the coating liquid of the cigarette cartridge mainly comprises various cigarette flavors, so that the cigarette style is determined by the cigarette flavors. The tobacco flavor is generally prepared by mixing various natural flavor extracts and tobacco extracts, wherein the natural flavor extracts are extracted from non-tobacco aromatic plants, such as jujube tincture, apricot juice and the like; the latter is extracted directly from tobacco material. The natural spice extract can make the cigarette have characteristic aroma and can obviously increase the aroma amount of the cigarette; the tobacco extract contains fragrant substances such as nicotine and tobacco organic acid, and can increase the concentration, the original fragrance, the strength and the satisfaction of the cigarette; the relative ratio of the two is difficult to balance.
In the tobacco flavor formula of the cigarette cartridge, when the content of the natural flavor extract is too high, the characteristic fragrance of non-tobacco is too obvious, so that the tobacco fragrance of the cigarette can be covered, the cigarette is not strong, and the smoking experience cannot be met. When the content of the tobacco extract is too high, the cigarette lacks characteristic aroma, the nicotine proportion is too large, and the cigarette strength is high; some macromolecular substances extracted from tobacco materials, such as pectin and cellulose, can strongly irritate the mouth and throat when heated, causing discomfort to the smoker. Therefore, in the formula of the cigarette which is not combusted by heating, the natural spice extract with high content is kept, and a certain amount of high-nicotine tobacco extract is added, so that the cigarette can give consideration to characteristic aroma and taste, and the cigarette is very necessary.
Disclosure of Invention
The invention aims to provide a preparation method of a high-nicotine tobacco extract, aiming at solving the problem that the existing tobacco extract can not meet the requirements of heating non-burning cigarettes on characteristic aroma and concentration.
In order to achieve the purpose, the invention adopts the technical scheme that: a preparation method of a high nicotine tobacco extract comprises the following steps:
(1) enzymolysis: mixing the crushed tobacco raw materials with water, and adding an enzyme preparation for enzymolysis reaction;
(2) leaching: mixing and leaching the tobacco raw material subjected to enzymolysis with a high-concentration ethanol solution, performing solid-liquid separation after leaching to obtain a leaching solution, and filtering the leaching solution to obtain a tobacco extracting solution;
(3) concentration: concentrating the tobacco extract under reduced pressure to obtain tobacco alcohol extract;
(4) and (3) extraction: adding alkali liquor into the tobacco alcohol extract, stirring uniformly, and mixing with an organic solvent for extraction;
(5) separation: separating the liquid after extraction to obtain an organic phase and a water phase, and concentrating the organic phase under reduced pressure to obtain an essential oil product which is the high nicotine tobacco extract.
Further, the pulverized tobacco raw material in the step (1) has a pulverized particle size of 20-80 meshes, and the mass ratio of the pulverized tobacco raw material to water is 1:1.5-1:2.5, preferably 1:2-1: 2.5. The tobacco raw material in the step (1) can adopt a low-grade tobacco raw material or a slightly mildewed tobacco raw material.
Further, the enzyme preparation in the step (1) is a mixture of pectinase and cellulase, and the enzyme activities of the pectinase and the cellulase are respectively 5 ten thousand U and 10 ten thousand U; the mass ratio of the tobacco raw material to the pectinase and the cellulase is 100:0.3-0.7:0.1-0.5, preferably 100:0.5-0.7: 0.3-0.5;
the enzymolysis reaction time is 1-3h, the reaction temperature is 45-55 ℃, the preferable reaction time is 2-3h, and the preferable reaction temperature is 50-55 ℃.
Further, the concentration of the high-concentration ethanol solution in the step (2) is 90-95% (v/v), and the mass ratio of the tobacco raw material to the high-purity ethanol solution is 1:7-1:10, preferably 1:9-1: 10;
the leaching temperature is 55-65 ℃, the leaching time is 1-2h, the preferred leaching temperature is 60-65 ℃, and the preferred leaching time is 1.5-2 h.
Further, in the step (3), the reduced pressure concentration temperature is 65-75 ℃, the vacuum degree is 0.07-0.08Mpa, the cooling temperature of the recovered ethanol is-10-10 ℃, the solid content of the tobacco alcohol extract is 50-70%, and the solid content is the mass percentage content of the solid content of the pasty liquid.
Further, the alkali liquor in the step (4) is NaOH solution, KOH solution or NH3·H2O, and the pH value of the alkali liquor is 12-14; the mass ratio of the tobacco alcohol extract to the alkali liquor is 1:1-3, the stirring time is 5-15min, the preferred mass ratio of the tobacco alcohol extract to the alkali liquor is 1:2.5-3, and the preferred stirring time is 10-15 min.
Further, in the step (4), the organic solvent is one or more of dichloromethane, petroleum ether, ethyl acetate and n-hexane, the mass ratio of the tobacco alcohol extract to the organic solvent is 1:2-5, the extraction time is 0.5-2h, the preferred mass ratio of the tobacco alcohol extract to the organic solvent is 1:4-5, and the preferred extraction time is 1.5-2 h.
Further, in the step (5), the reduced pressure concentration temperature is 20-60 ℃, the vacuum degree is 0.07-0.08Mpa, and the cooling temperature for recovering the organic solvent is-10-10 ℃.
The invention also discloses a high nicotine tobacco extract prepared by the method.
The invention also discloses a cigarette which is not burnt by heating, and the cigarette comprises the high nicotine tobacco extract.
Further, the heat non-combustible cigarette comprises 0.002-0.01 wt% of high nicotine tobacco extract. Further, the tobacco shred of the cigarette which is not combusted by heating is coated with 0.002-0.01 wt% of high nicotine tobacco extract. The formula of the cigarette without burning by heating comprises the high nicotine tobacco extract, so that the use amount of the natural spice extract can be correspondingly increased. The extract can remarkably increase the original fragrance, concentration and strength of the tobacco without affecting the fragrance amount and concentration; the cigarette has the advantages of giving consideration to characteristic aroma and taste, and having the effects of better improving the quality of the cigarette which is not combusted by heating and smoking experience.
The invention discloses a high nicotine tobacco extract and a preparation method thereof, and simultaneously discloses a heating non-burning roll added with the high nicotine tobacco extract, compared with the prior art, the invention has the following advantages:
(1) the nicotine content of the high-nicotine tobacco extract is as high as 8-20 wt%, which is higher than that of the conventional tobacco extract. The invention utilizes the solubility of nicotine to transfer nicotine in tobacco raw materials, tobacco extract, tobacco alcohol extract, alkali liquor and organic solvent in turn, and finally concentrates the organic solvent to enrich most of nicotine and remove the organic solvent, thereby preparing the tobacco extract with high nicotine content, excellent aroma quality and excellent aroma quantity.
(2) During enzyme treatment, pectin and cellulose macromolecular substances contained in the tobacco raw materials are subjected to enzymolysis reaction with pectinase and cellulase to generate micromolecular aroma substances and saccharides, so that the aroma components and the water-soluble sugar content in the raw materials are increased; after the enzymolysis stage is finished, the enzyme preparation can be inactivated by adding an ethanol solution, so that the high-temperature inactivation reaction process is omitted, and the loss of aroma components is avoided; the temperature of the three stages of enzymolysis, extraction and concentration is raised in sequence without cooling, and the energy consumption of the whole production process is low.
(3) The process of replacing nicotine and tobacco aroma substances is implemented by liquid-liquid extraction, the temperature is low in the organic solvent concentration stage, and the aroma components in the extract are greatly reserved.
(4) In the invention, after the enzymolysis reaction, solid-liquid separation is not needed; then adding high-concentration ethanol solution and adding water in the enzymolysis reaction for mixing to form ethanol solution with medium concentration (50-80%, v/v), which meets the requirement of the tobacco ethanol extract; the whole leaching process is high in efficiency and short in time consumption.
(5) The preparation process of the high nicotine tobacco extract has low requirement on the quality of raw materials, and can be used for treating mildewed or low-grade tobacco raw materials.
Detailed Description
The invention is further illustrated by the following examples:
example 1
The embodiment discloses a method for preparing a high-nicotine tobacco extract from a tobacco raw material in a Yunnan Trijing area, which comprises the following specific steps:
(1) crushing the raw materials with the mass m, and sieving the crushed raw materials with a 40-mesh sieve; adding 0.3% m of pectinase (enzyme activity: 5 ten thousand U) and 0.2% m of cellulase (enzyme activity: 10 ten thousand U) into 1.5m of water, uniformly stirring, mixing with the raw materials, and performing enzymolysis reaction; the time of the enzymolysis reaction is 3h, and the temperature is 50 ℃.
(2) Mixing the material after enzymolysis with 7m ethanol solution (90%, v/v), and extracting at 55 deg.C for 1 h; and (4) carrying out solid-liquid separation after extraction, and filtering the liquid to obtain a tobacco extract.
(3) Concentrating the tobacco extract at 65 deg.C under reduced pressure until the solid content is 60% to obtain tobacco alcohol extract; cooling to 0 deg.C, and recovering ethanol.
(4) Alkalizing and extracting: adding 2n NaOH aqueous solution (pH value of 12) into the tobacco alcohol extract, and stirring for 5 min; then mixing with petroleum ether with the mass of 3n, and extracting for 1 h.
(5) Separation: layering the extractive solution, collecting organic phase, and concentrating under reduced pressure at 55 deg.C until no petroleum ether volatilizes to obtain high nicotine tobacco extract; the cooling temperature for recovering petroleum ether was 0 ℃.
The nicotine content of the high nicotine tobacco extract prepared in this example was 16.76 wt%.
Example 2
The embodiment discloses a method for preparing a high-nicotine tobacco extract from tobacco raw materials in Zhaotong area of Yunnan, which comprises the following specific steps:
(1) crushing the raw materials with the mass m, and sieving the crushed raw materials with a 60-mesh sieve; adding 0.4% m of pectinase (enzyme activity: 5 ten thousand U) and 0.5% m of cellulase (enzyme activity: 10 ten thousand U) into 2m of water, uniformly stirring, mixing with the raw materials, and performing enzymolysis reaction; the time of the enzymolysis reaction is 2.5h, and the temperature is 55 ℃.
(2) Mixing the material after enzymolysis with 8m ethanol solution (95%, v/v), and extracting at 55 deg.C for 2 h; and (4) carrying out solid-liquid separation after extraction, and filtering the liquid to obtain a tobacco extract.
(3) Concentrating the tobacco extract at 70 deg.C under reduced pressure until the solid content is 60% to obtain tobacco alcohol extract; cooling to 0 deg.C, and recovering ethanol.
(4) Alkalizing and extracting: adding NaOH aqueous solution (pH value is 13) with mass n into the tobacco alcohol extract with mass n, and stirring for 15 min; then mixing with n-hexane with the mass of 2n, and extracting for 1 h.
(5) Separation: layering the extractive solution, collecting organic phase, and concentrating under reduced pressure at 55 deg.C until no n-hexane volatilizes to obtain high nicotine tobacco extract; the cooling temperature for recovering n-hexane was-10 ℃.
The nicotine content of the high nicotine tobacco extract prepared in this example was 13.16 wt%.
Example 3
The embodiment discloses a method for preparing a high-nicotine tobacco extract by using tobacco raw materials in a Guizhou Zunyi area, which comprises the following specific steps:
(1) crushing the raw materials with the mass m, and sieving the crushed raw materials with a 40-mesh sieve; adding 0.6% m pectinase (enzyme activity: 5 ten thousand U) and 0.5% m cellulase (enzyme activity: 10 ten thousand U) into 2m water, stirring, mixing with the raw materials, and performing enzymolysis; the time of the enzymolysis reaction is 3h, and the temperature is 50 ℃.
(2) Mixing the material after enzymolysis with 9m ethanol solution (95%, v/v), and extracting at 60 deg.C for 1 h; and (4) carrying out solid-liquid separation after extraction, and filtering the liquid to obtain a tobacco extract.
(3) Concentrating the tobacco extract at 65 deg.C under reduced pressure until the solid content is 60% to obtain tobacco alcohol extract; cooling to-5 deg.C, and recovering ethanol.
(4) Alkalizing and extracting: adding KOH aqueous solution (with the pH value of 13) with the mass of n into the tobacco alcohol extract with the mass of n, and stirring for 10 min; then mixed with dichloromethane with the mass of 3n, and extracted for 1.5 h.
(5) Separation: layering the extractive solution, collecting organic phase, and concentrating under reduced pressure at 50 deg.C until no dichloromethane volatilizes to obtain high nicotine tobacco extract; the cooling temperature for the recovery of methylene chloride was-5 ℃.
The high nicotine tobacco extract prepared in this example had a nicotine content of 14.34 wt%.
Examples 4 to 6
Examples 4-6 disclose three types of cigarettes which are not combusted by heating, and the three types of cigarettes which are not combusted by heating are added with different contents of the high nicotine tobacco extract in example 1, and the specific addition amounts are shown in table 1.
The control example was an aqueous extract of tobacco material prepared by substantially the same method as the steps (1) and (2) of example 1, except that no enzyme preparation was added in step (1) and the extraction solution of step (2) was water (instead of the ethanol solution in the original example), in response to the addition of the aqueous extract of tobacco material described in example 1.
Sensory evaluation comparative experiments were conducted for examples 4 to 6 and comparative example 1, respectively, and the results are shown in Table 1.
TABLE 1 sensory evaluation results
The result shows that the tobacco extract prepared by the embodiment is applied to the smoke cartridge of the novel heating non-combustion cigarette, is coordinated with smoke, keeps the style of the cigarette, can enhance the herbal fragrance of the cigarette, can obviously improve the strength and satisfaction of the heating non-combustion cigarette, and improves the taste.
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 (10)
1. A preparation method of a high nicotine tobacco extract is characterized by comprising the following steps:
(1) enzymolysis: mixing the crushed tobacco raw materials with water, and adding an enzyme preparation for enzymolysis reaction;
(2) leaching: mixing and leaching the tobacco raw material subjected to enzymolysis with a high-concentration ethanol solution, performing solid-liquid separation after leaching to obtain a leaching solution, and filtering the leaching solution to obtain a tobacco extracting solution;
(3) concentration: concentrating the tobacco extract under reduced pressure to obtain tobacco alcohol extract;
(4) and (3) extraction: adding alkali liquor into the tobacco alcohol extract, stirring uniformly, and mixing with an organic solvent for extraction;
(5) separation: separating the liquid after extraction to obtain an organic phase and a water phase, and concentrating the organic phase under reduced pressure to obtain an essential oil product which is the high nicotine tobacco extract.
2. The method for preparing a high nicotine tobacco extract according to claim 1, wherein the pulverized tobacco raw material in the step (1) has a particle size of 20-80 mesh, and the mass ratio of the pulverized tobacco raw material to water is 1:1.5-1: 2.5.
3. The method for preparing a high nicotine tobacco extract as claimed in claim 1, wherein the enzyme preparation in step (1) is a mixture of pectinase and cellulase, and the enzyme activities of the pectinase and cellulase are 5 ten thousand U and 10 ten thousand U, respectively; the mass ratio of the tobacco raw material to the pectinase and the cellulase is 100:0.3-0.7: 0.1-0.5;
the enzymolysis reaction time is 1-3h, and the reaction temperature is 45-55 ℃.
4. The method for preparing the high nicotine tobacco extract according to claim 1, wherein the concentration of the high concentration ethanol solution in the step (2) is 90-95% (v/v), and the mass ratio of the tobacco raw material to the high purity ethanol solution is 1:7-1: 10;
the leaching temperature is 55-65 ℃, and the leaching time is 1-2 h.
5. The method for preparing the high nicotine tobacco extract according to claim 1, wherein the reduced pressure concentration temperature in the step (3) is 65-75 ℃, the vacuum degree is 0.07-0.08Mpa, and the solid content of the tobacco alcohol extract is 50-70%.
6. The method for preparing the high nicotine tobacco extract according to claim 1, wherein the alkali solution in the step (4) is NaOH solution, KOH solution or NH3·H2O, and the pH value of the alkali liquor is 12-14; the mass ratio of the tobacco alcohol extract to the alkali liquor is 1:1-3, and the stirring time is 5-15 min.
7. The method for preparing the high nicotine tobacco extract according to claim 1, wherein the organic solvent in step (4) is one or more of dichloromethane, petroleum ether, ethyl acetate and n-hexane, the mass ratio of the tobacco alcohol extract to the organic solvent is 1:2-5, and the extraction time is 0.5-2 h.
8. The method for preparing the tobacco extract with high nicotine as claimed in claim 1, wherein the concentration under reduced pressure in step (5) is carried out at 20-60 ℃ under a vacuum of 0.07-0.08 Mpa.
9. A high nicotine tobacco extract, prepared by the method of any one of claims 1 to 8.
10. A heat-not-burn cigarette comprising the high nicotine tobacco extract of claim 9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010729165.8A CN112011405A (en) | 2020-07-27 | 2020-07-27 | High-nicotine tobacco extract, preparation method thereof and cigarette without burning by heating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010729165.8A CN112011405A (en) | 2020-07-27 | 2020-07-27 | High-nicotine tobacco extract, preparation method thereof and cigarette without burning by heating |
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| CN105542957A (en) * | 2015-12-09 | 2016-05-04 | 无锡华海香料有限公司 | Preparation method of natural flavor for tobacco and application of flavor |
| CN106235415A (en) * | 2016-08-05 | 2016-12-21 | 广西中烟工业有限责任公司 | A kind of cigarette perfume (or spice) tobacco juice for electronic smoke |
| CN106387990A (en) * | 2016-11-22 | 2017-02-15 | 中国烟草总公司郑州烟草研究院 | High-nicotine tobacco extract and application thereof |
| CN106509981A (en) * | 2016-11-22 | 2017-03-22 | 中国烟草总公司郑州烟草研究院 | Preparation method of high-nicotine tobacco extract |
| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105542957A (en) * | 2015-12-09 | 2016-05-04 | 无锡华海香料有限公司 | Preparation method of natural flavor for tobacco and application of flavor |
| CN106235415A (en) * | 2016-08-05 | 2016-12-21 | 广西中烟工业有限责任公司 | A kind of cigarette perfume (or spice) tobacco juice for electronic smoke |
| CN106387990A (en) * | 2016-11-22 | 2017-02-15 | 中国烟草总公司郑州烟草研究院 | High-nicotine tobacco extract and application thereof |
| CN106509981A (en) * | 2016-11-22 | 2017-03-22 | 中国烟草总公司郑州烟草研究院 | Preparation method of high-nicotine tobacco extract |
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