阅读说明：本技术 一种烟草提取物及其制备方法和应用、烟草制品 (Tobacco extract, preparation method and application thereof, and tobacco product ) 是由 徐秀娟 史清照 何保江 王丁众 刘珊 刘俊辉 崔凯 屈展 杨春强 宗永立 张建勋 于 2020-05-11 设计创作，主要内容包括：本发明属于烟用香精香料制备技术领域,具体涉及一种烟草提取物及其制备方法和应用、烟草制品。本发明的烟草提取物的制备方法,包括以下步骤：(1)将烟叶粉碎后进行亚临界萃取,除去萃取剂,得烟草浸膏,萃取剂为丁烷或二甲醚；(2)将步骤(1)所得的烟草浸膏醇沉、固液分离,将所得清液浓缩,得烟草浓缩物；(3)将步骤(2)所得的烟草浓缩物进行一级分子蒸馏,将一级分子蒸馏所得重组分进行二级分子蒸馏,所得轻组分即为烟草提取物,所述一级分子蒸馏温度为40-80℃,蒸馏压力为0.001-0.01mbar,所述二级分子蒸馏温度为100-120℃,蒸馏压力为0.001-0.01mbar。该方法工艺简单,适于规模化生产。(The invention belongs to the technical field of preparation of tobacco flavors and fragrances, and particularly relates to a tobacco extract, a preparation method and application thereof, and a tobacco product. The preparation method of the tobacco extract comprises the following steps: (1) crushing tobacco leaves, performing subcritical extraction, and removing an extractant to obtain a tobacco extract, wherein the extractant is butane or dimethyl ether; (2) precipitating the tobacco extract obtained in the step (1) with ethanol, carrying out solid-liquid separation, and concentrating the obtained clear liquid to obtain a tobacco concentrate; (3) and (3) performing primary molecular distillation on the tobacco concentrate obtained in the step (2), performing secondary molecular distillation on the heavy component obtained by the primary molecular distillation, wherein the obtained light component is the tobacco extract, the primary molecular distillation temperature is 40-80 ℃, the distillation pressure is 0.001-0.01mbar, the secondary molecular distillation temperature is 100-120 ℃, and the distillation pressure is 0.001-0.01 mbar. The method has simple process and is suitable for large-scale production.)

1. A preparation method of a tobacco extract is characterized by comprising the following steps:

(1) crushing tobacco leaves, performing subcritical extraction, and removing an extractant to obtain a tobacco extract, wherein the extractant is butane or dimethyl ether;

(2) precipitating the tobacco extract obtained in the step (1) with ethanol, carrying out solid-liquid separation, and concentrating the obtained clear liquid to obtain a tobacco concentrate;

(3) and (3) performing primary molecular distillation on the tobacco concentrate obtained in the step (2), performing secondary molecular distillation on the heavy component obtained by the primary molecular distillation, wherein the obtained light component is the tobacco extract, the primary molecular distillation temperature is 40-80 ℃, the distillation pressure is 0.001-0.01mbar, the secondary molecular distillation temperature is 100-120 ℃, and the distillation pressure is 0.001-0.01 mbar.

2. The method of claim 1, wherein the subcritical extraction temperature in step (1) is 25-50 ℃ and the subcritical extraction time is 0.5-2 h.

3. The method of claim 1, wherein the pressure of the subcritical extraction in the step (1) is a saturated vapor pressure of the extracting agent at the extraction temperature.

4. The method for preparing a tobacco extract according to claim 1, wherein the mass ratio of the tobacco leaves to the extracting agent in the step (1) is 1:8 to 1: 20.

5. The method of claim 1, wherein an entrainer is used in the subcritical extraction in step (1), and the entrainer is ethanol or an ethanol aqueous solution with a volume concentration of 90% or more.

6. The method of claim 5, wherein the entrainer is not greater than 10% by volume of the extraction agent.

7. The method for preparing a tobacco extract as claimed in any one of claims 1 to 6, wherein the alcohol precipitation in the step (2) is: adding ethanol or ethanol water solution with volume concentration of more than 90% into the tobacco extract, heating to 30-50 ℃, keeping for 20-60 min, cooling, and transferring to a refrigerator with temperature of-20-5 ℃ for 8-24 h.

8. A tobacco extract obtained by the method for producing a tobacco extract according to any one of claims 1 to 7.

9. A smoking article, characterized in that it comprises the tobacco extract according to claim 8.

10. Use of a tobacco extract according to claim 8 in tobacco flavor.

Technical Field

The invention belongs to the technical field of preparation of tobacco flavors and fragrances, and particularly relates to a tobacco extract, a preparation method and application thereof, and a tobacco product.

Background

The tobacco extract is extracted from tobacco, contains tobacco intrinsic aroma components, has the advantages of natural and harmonious aroma, compensation of the intrinsic aroma of the tobacco, prominent style characteristics and the like, and is an irreplaceable aroma raw material for cigarette blending and novel tobacco product development.

The tobacco extract has complex product components, and the problems of low content of aroma components, unclear style and characteristic and the like are caused while the natural feeling and richness are given to the tobacco extract. At present, various separation technologies are applied to the fine processing of tobacco extracts, such as column chromatography, membrane separation, precipitation separation, molecular distillation and the like. The Chinese patent application with application publication number CN101570717A discloses a preparation method of a tobacco extract and application thereof, which sequentially adopts the steps of enzymolysis, ultrasonic extraction, filtration, chromatographic column separation and reduced pressure concentration; the Chinese patent application with the application publication number of CN102894467A discloses a method for preparing a tobacco extract by fermenting an immobilized enzyme preparation and acetic acid bacteria, which can quickly and effectively reduce the content of starch, protein, cellulose, lignin and pectin in the tobacco extract; the Chinese patent application with the application publication number of CN104223356A discloses a method for adsorbing protein macromolecules in a tobacco extract by using a zwitterionic exchange membrane to improve the quality of the tobacco extract; CN103734905A, the Chinese patent application of the invention adopts a method of alkali extraction and acid precipitation to remove proteins in tobacco extracts; the Chinese patent with the publication number of CN105533793B discloses a preparation method of a sun-cured red tobacco extract, which adopts the molecular distillation technology to divide a tobacco extract into four stages and organically combines the light components of the two stages and the four stages.

Although the prior art has conducted extensive research and research on the process of removing macromolecules in the extract, some technical defects still exist. For example: in the aspect of removing the plant wax, the prior art has better removal efficiency on long-chain alkane, but cannot effectively reduce the content of low-carbon alkane; higher fatty acids in tobacco extracts are detrimental to cigarette smoking, mainly manifested by increased irritation and a waxy taste of the smoke, but there is less concern about the removal of such substances in separation techniques; the processes of column chromatography, alkali extraction, acid precipitation and the like are complex, the conditions are not easy to control, and the large-scale production is difficult.

Disclosure of Invention

The invention aims to provide a preparation method of a tobacco extract, which can be used for deeply enriching aroma components in tobacco, has a simple preparation process and is suitable for large-scale production.

The second purpose of the invention is to provide a tobacco extract, which has low content of plant waxy components and higher fatty acid and high content of aroma components and can provide material base for high-quality tobacco products.

A third object of the present invention is to provide a tobacco product which is capable of better retaining the original aroma characteristics of tobacco.

The fourth purpose of the invention is to provide an application of the tobacco extract in tobacco flavor, and the tobacco extract can be used as the tobacco flavor so as to be applied to a plurality of tobacco products such as cigarettes, electronic cigarettes, heating non-burning cigarettes and the like, and provide real, rich and full tobacco original flavor for the tobacco products.

In order to achieve the purpose, the specific technical scheme of the tobacco extract is as follows:

the specific technical scheme of the preparation method of the tobacco extract is as follows:

a preparation method of a tobacco extract comprises the following steps:

(1) crushing tobacco leaves, performing subcritical extraction, and removing an extractant to obtain a tobacco extract, wherein the extractant is butane or dimethyl ether;

(2) precipitating the tobacco extract obtained in the step (1) with ethanol, carrying out solid-liquid separation, and concentrating the obtained clear liquid to obtain a tobacco concentrate;

(3) and (3) performing primary molecular distillation on the tobacco concentrate obtained in the step (2), performing secondary molecular distillation on the heavy component obtained by the primary molecular distillation, wherein the obtained light component is the tobacco extract, the primary molecular distillation temperature is 40-80 ℃, the distillation pressure is 0.001-0.01mbar, the secondary molecular distillation temperature is 100-120 ℃, and the distillation pressure is 0.001-0.01 mbar.

According to the preparation method of the tobacco extract, long-chain alkane is removed through subcritical extraction, alcohol precipitation, separation and concentration, the content of low-carbon alkane and high-grade fatty acid in the tobacco extract is reduced through two-stage molecular distillation, the offensive odor and irritation of the tobacco extract are reduced, and the sensory quality of the tobacco extract is improved. The butane and the dimethyl ether with low toxicity and recoverability are selected as the extracting agents, so that the mass transfer speed in the extraction process can be improved, the harm caused by an organic solvent can be reduced, the cost is saved, and the large-scale production is facilitated.

Preferably, in order to fully leach out the aroma components in the tobacco leaves, the temperature of the subcritical extraction is 25-50 ℃, and the time of the subcritical extraction is 0.5-2 h.

In order to further improve the extraction rate, the pressure of the subcritical extraction is the saturated vapor pressure of the extractant at the extraction temperature.

Preferably, the mass ratio of the tobacco leaves to the extracting agent is 1:8-1: 20.

Preferably, an entrainer is also used in the subcritical extraction, and the entrainer is ethanol or ethanol water solution with the volume concentration of more than 90%.

Preferably, the volume of entrainer is no more than 10% of the extractant.

The alcohol precipitation, solid-liquid separation and concentration process specifically comprises the following steps: adding ethanol or ethanol water solution with volume concentration of more than 90% into the tobacco extract, heating to 30-50 ℃, keeping for 20-60 min to fully dissolve the ethanol or ethanol water solution, cooling to room temperature, and transferring to a refrigerator with the temperature of-20 to-5 ℃ to freeze for 8-24 h. Filtering at low temperature to obtain filtrate or centrifuging to obtain supernatant, and concentrating the filtrate or supernatant under reduced pressure to remove ethanol to obtain tobacco concentrate.

The rotation speed of the centrifugation is 4000rpm, and the time is 10-30 min.

The alcohol dosage of the alcohol precipitation is 5-10 times of the quality of the tobacco extract.

The specific technical scheme of the tobacco extract is as follows:

the tobacco extract obtained by the preparation method of the tobacco extract.

The tobacco extract has low content of plant waxy components such as low-carbon alkane, long-chain alkane and the like, and low content of high-carbon fatty acid which is unfavorable for cigarette smoking, and can provide material basis for high-quality tobacco products and improve the sensory quality of the tobacco products.

The tobacco product of the invention has the specific technical scheme that:

a tobacco product comprising the tobacco extract.

The tobacco product prepared by using the tobacco extract can better keep the original aroma characteristics of tobacco and bring better sensory experience to consumers.

The specific technical scheme of the application of the tobacco extract in the tobacco flavor comprises the following steps:

the application of the tobacco extract in tobacco flavor, in particular to the tobacco extract which can be used as the raw material of the tobacco flavor in tobacco products commonly used in the field, such as cigarettes, electronic cigarettes, heating non-burning cigarettes and the like. The tobacco extract can be applied to cigarettes in different modes according to the characteristics of the cigarettes, electronic cigarettes and non-burning cigarettes by heating, and has the effects of enhancing the quality and the quantity of aroma, enriching the aroma of the cigarettes, increasing the concentration and the permeability of smoke and the like.

Detailed Description

The application of the method of the present invention will be specifically described with reference to the following examples. It should be noted that the examples given in this specification are only for the purpose of facilitating understanding of the present invention, and they are not intended to be limiting, i.e., the present invention may be embodied in other forms than those shown in the specification. Therefore, any technical solutions formed by equivalent substitution or equivalent transformation fall within the protection scope of the present invention.

First, the specific embodiment of the preparation method of the tobacco extract of the present invention

Example 1

The preparation method of the tobacco extract of this example is as follows:

(1) crushing tobacco leaves to 100 meshes, transferring the tobacco leaves to a subcritical extraction kettle, adding dimethyl ether, extracting for 2 hours at 25 ℃ under the condition that the mass ratio of tobacco leaf powder to dimethyl ether is 1:8 and the entrainer is 95% ethanol (the using amount is 5% of the volume of dimethyl ether), and the extraction pressure is the saturated vapor pressure of dimethyl ether at the temperature, and performing reduced pressure evaporation after the extraction is finished to obtain tobacco extract;

(2) adding 95% ethanol 5 times the mass of the tobacco extract obtained in the step (1), heating to 30 ℃, and keeping for 60min to fully dissolve the tobacco extract; then cooling to room temperature, and transferring to a refrigerator with the temperature of-20 ℃ for freezing for 8 h; filtering at low temperature to obtain filtrate, and concentrating the filtrate under reduced pressure until no ethanol is present to obtain tobacco concentrate;

(3) transferring the tobacco concentrate obtained in the step (2) into a molecular distillation feed tank, performing primary molecular distillation at 60 ℃ under the condition of 0.001mbar, and respectively collecting light components and heavy components; performing secondary molecular distillation on the heavy component at 120 deg.C and 0.001mbar, and collecting light component to obtain tobacco extract.

Example 2

The preparation method of the tobacco extract of this example is as follows:

(1) crushing tobacco leaves to 100 meshes, transferring the tobacco leaves to a subcritical extraction kettle, adding dimethyl ether, extracting the tobacco leaves for 0.5h at 40 ℃ by using absolute ethyl alcohol (the using amount is 10% of the volume of the dimethyl ether) as an entrainer according to the mass ratio of 1:10 and the volume of the dimethyl ether, and performing reduced pressure evaporation after the extraction is finished to obtain a tobacco extract;

(2) adding 10 times of anhydrous ethanol into the tobacco extract obtained in the step (1), heating to 50 ℃, and keeping for 20min to fully dissolve the tobacco extract; then cooling to room temperature, and transferring to a refrigerator with the temperature of-5 ℃ for freezing for 24 h; centrifuging at low temperature (4000rpm, 10min), and concentrating the supernatant under reduced pressure until ethanol is removed to obtain tobacco concentrate;

(3) transferring the tobacco concentrate obtained in the step (2) into a molecular distillation feed tank, performing primary molecular distillation at 80 ℃ under the condition of 0.01mbar, and respectively collecting light components and heavy components; performing secondary molecular distillation on the obtained heavy component at 100 deg.C and 0.01mbar, and collecting light component to obtain tobacco extract.

Example 3

The preparation method of the tobacco extract of this example is as follows:

(1) crushing tobacco leaves to 50 meshes, transferring the tobacco leaves to a subcritical extraction kettle, adding butane, extracting for 1h at 50 ℃ under the condition that the ratio of tobacco leaf powder to butane is 1:20, wherein the extraction pressure is the saturated vapor pressure of butane at the temperature, and decompressing and evaporating after the extraction is finished to obtain tobacco extract;

(2) adding absolute ethyl alcohol with the mass being 8 times that of the tobacco extract obtained in the step (1), heating to 40 ℃, and keeping for 40min to fully dissolve the absolute ethyl alcohol; then cooling to room temperature, and transferring to a refrigerator with the temperature of-15 ℃ for freezing for 12 h; centrifuging at low temperature (4000rpm, 10min), and concentrating the supernatant under reduced pressure until ethanol is removed to obtain tobacco concentrate;

(3) transferring the tobacco concentrate obtained in the step (2) into a molecular distillation feed tank, performing primary molecular distillation at 40 ℃ under the condition of 0.001mbar, and respectively collecting light components and heavy components; performing secondary molecular distillation on the heavy component at 120 deg.C and 0.01mbar, and collecting light component to obtain tobacco extract.

Second, specific examples of the tobacco extract of the present invention

Example 4

The tobacco extract of this example was obtained by the preparation method of example 1.

Example 5

The tobacco extract of this example was obtained by the preparation method of example 2.

Example 6

The tobacco extract of this example was obtained by the preparation method of example 3.

Third, the tobacco product of the present invention

Example 7

The tobacco product of the embodiment is a cigarette, and specifically, the tobacco extract of the embodiment 4 is diluted with 95% ethanol to a mass concentration of 10%, and is injected into a blank cigarette with an automatic injection and flavoring device, wherein the injection amount is 1 μ L/cigarette, so that the cigarette product is obtained.

Fourth, specific examples of the application of the tobacco extract of the present invention in tobacco products

Example 8

In the embodiment, the tobacco extract is used for preparing the electronic cigarette liquid, specifically, the propylene glycol is used as a solvent, the tobacco extract in the embodiment 5 is diluted to 5% and applied to the electronic cigarette liquid, the tobacco fragrance can be obviously supplemented during smoking, the cigar style characteristic is obvious, the sweet and greasy feeling is low, and no residue is left in the oral cavity.

Fifth, example of experiment

Experimental example 1

A certain amount of the first-order molecular distillation light component, the second-order molecular distillation heavy component and the tobacco extract obtained in example 1 were accurately weighed, dissolved in absolute ethanol, and then an internal standard (phenylethyl acetate) was added, and component analysis was performed by GC-MS, with the following instrument conditions:

chromatographic conditions are as follows: a chromatographic column: DB-5MS capillary column (30m 0.25mm 0.25 μm); sample inlet temperature: 250 ℃; carrier gas: high purity helium gas; the flow rate is 1.0 mL/min; sample introduction amount: 1 mu L of the solution; the split ratio is 10: 1; temperature programming: keeping the temperature at 50 deg.C for 2min, heating to 270 deg.C at a heating rate of 5 deg.C/min, and keeping for 10 min.

Mass spectrum conditions: an ionization mode: EI; ion source temperature: 230 ℃; electron energy: 70 eV; quadrupole temperature: 150 ℃; electron multiplier voltage: 1.89 kV; the mass scanning range is 33-500 amu; the scanning mode is as follows: full scanning; solvent retardation: 7.0 min.

TABLE 1 type and content of light fraction of first-order molecular distillation and low-carbon alkane in tobacco extract

From the experimental results, most of the low-carbon alkane is enriched in the light component obtained after the first-stage molecular distillation by the preparation method of the tobacco extract, so that the content of the low-carbon alkane in the tobacco extract is greatly reduced and is only 0.4393 mg/g; in addition, the content of high-carbon fatty acids such as linolenic acid and linoleic acid in the tobacco concentrate and the tobacco extract is analyzed, the content of the two in the tobacco concentrate is 13.6057mg/g and 25.6921mg/g respectively, and the content of the two in the obtained tobacco extract is reduced to 4.2163mg/g and 9.4097mg/g respectively through two-stage molecular distillation.

Experimental example 2

The tobacco concentrate and the tobacco extract after the secondary molecular distillation of example 2 were analyzed for the aroma components by the analysis method of example 1, wherein the analysis results of the ketone compounds are shown in table 2.

TABLE 2 content of ketone-type aroma components in tobacco concentrate and tobacco extract

Note: in the table, megastigmatrienone-1, megastigmatrienone-2 and megastigmatrienone-3 represent three isomers of megastigmatrienone, respectively.

From the above results, it can be seen that the content of the aroma components in the tobacco extract is greatly increased and the total amount of the ketone aroma components reaches 49.1827mg/g after the treatment by the method of the present invention. Wherein, the content of megastigmatrienone-2 is improved by 7.73 times, geranylacetone is 2 times of that in tobacco concentrate, and farnesylacetone is 6.36 times of that in original.

Experimental example 3

The tobacco concentrate of example 3, and the tobacco extract after the secondary molecular distillation, were diluted with 95% ethanol to a mass concentration of 10% and injected into blank cigarettes with an automatic injection and flavor machine at an injection rate of 1 μ L/cigarette. After the injection, the cigarettes were put into cigarette packs, sealed at 22 ℃. + -. 2 ℃ and RH 60%. + -. 5% and left for 1 week, and then the perfuming effect was evaluated.

TABLE 3 sensory evaluation results

Note that when the average score is greater than 11.2, the index is obviously improved, and the higher the score is, the higher the improvement degree is.

Evaluation results show that after two-stage molecular distillation, the aroma quality and the aroma quantity of the tobacco extract are obviously improved, miscellaneous gases are reduced, the fineness and the softness of smoke are increased, and the residue and the irritation are reduced; meanwhile, the fragrance, the flower fragrance and the cream fragrance are more prominent.