Preparation method and application of tobacco essential oil

Abstract

The invention discloses a preparation method and application of tobacco essential oil, and the preparation method comprises the following steps: (1) drying tobacco leaves until the moisture is less than 5%, and crushing the tobacco leaves into tobacco powder; (2) adding tobacco powder, an extraction solvent and the graphene nano-roll coated ferroferric oxide nano-particle composite material (FG) into an extraction tank for extraction, and cooling and filtering after extraction to obtain a crude extract; wherein the mass ratio of the tobacco powder to the extract solvent is 1: (8-12), and the addition amount of the FG is 0.1% of the total mass; (3) transferring the crude extract into a concentration tank, concentrating under reduced pressure, and removing the organic solvent and water to obtain an extract; and (4) obtaining the tobacco essential oil from the extract by using a membrane separation technology. The tobacco essential oil disclosed by the invention can be well coordinated with cigarette fragrance, obviously improves the smoke quality, softens the cigarette smoke, enriches the fragrance, improves the sweetness and smoothness of cigarettes, reduces irritation and the like, and meanwhile, has the potential of industrial production.

Description

Technical Field

[0001] The invention relates to the technical field of tobacco essential oil, and in particular to a preparation method and application of tobacco essential oil. Background Art

[0002] Tobacco essential oil is a class of compounds extracted from tobacco with the characteristic smell of tobacco. It is volatile and its main components are terpenes, volatile acids, aromatic rings, etc. Adding it to cigarettes can enrich the aroma of cigarettes and improve the sensory quality of cigarettes.

[0003] At present, the main extraction methods of tobacco essential oil are steam distillation, organic solvent extraction and supercritical fluid extraction. The equipment and operation of steam distillation are simple, but since the sample and water are azeotropic during extraction, it is not conducive to the extraction of heat-sensitive substances; supercritical fluid extraction is a new technology developed in recent years, but its extraction rate is low and the extraction of flavor substances is insufficient. Dynamic reciprocating magnetic field assisted extraction combines solvent extraction and magnetic effect, which can effectively improve the magnetic effect of the solvent system under the action of the magnetic field, accelerate solvent extraction, and improve extraction efficiency. The present invention develops tobacco essential oil by strengthening the separation process with the help of an external magnetic field, and has the advantages of high efficiency, easy operation, green and safe, and industrial production. Summary of the invention

[0004] The technical problem to be solved by the present invention is to provide a preparation method of tobacco essential oil and application thereof, aiming to solve the problems that traditional tobacco essential oil extraction methods are low in efficiency, high in cost and unsuitable for heat-sensitive substances.

[0005] The technical problem to be solved by the present invention is achieved through the following technical solutions:

[0006] A method for preparing tobacco essential oil comprises the following steps:

[0007] (1) drying the tobacco leaves in an oven until the moisture content is less than 8%, and then crushing the tobacco leaves into tobacco powder;

[0008] (2) adding cigarette dust, extraction solvent and graphene nanoscroll-wrapped ferroferric oxide nanoparticle composite material (FG) into an extraction tank for extraction, and cooling and filtering after extraction to obtain a crude extract; wherein the mass ratio of cigarette dust to extraction solvent is 1:(8-12), and the amount of FG added is 1‰ of the total mass;

[0009] (3) transferring the crude extract to a concentration tank, concentrating under reduced pressure to remove the organic solvent and water to obtain an extract;

[0010] (4) Using membrane separation technology to obtain tobacco essential oil from the extract.

[0011] Preferably, in the above technical solution, step (1) is specifically as follows: keeping the tobacco leaves in an oven at 40-50° C. for 12-24 hours until the moisture content is less than 8.0%, and then crushing them into 40-50 mesh tobacco powder for later use.

[0012] Preferably, in the above technical solution, in step (2), the extraction solvent is a mixture of ethanol, water and sodium chloride in a mass ratio of 50:45:5; and the extraction conditions are 85° C. for 4 to 10 hours.

[0013] Preferably, in the above technical solution, in step (2), the amount of the tobacco dust, the extraction solvent and the FG added is 2 / 3 of the volume of the extraction tank, and after the FG is taken out, it is washed 3-5 times with a 30% ethanol / water solution.

[0014] Preferably, in the above technical solution, in step (3), the temperature of the reduced pressure concentration is 40-60° C., the vacuum pressure is 50-100 Pa, and the concentration of the extract is 1.0-1.2 g / mL.

[0015] Preferably, in the above technical solution, step (4) is specifically as follows: using a 50nm ceramic membrane and a 50kDa rolled organic membrane to separate the tobacco essential oil in sequence, and further concentrating the permeate using reverse osmosis technology to obtain a concentrated solution, and diluting it with 50% ethanol / water to a concentration of 10%, namely the tobacco essential oil.

[0016] Preferably, in the above technical solution, the tobacco leaves are Zimbabwean tobacco leaves.

[0017] The invention discloses a tobacco essential oil, wherein the tobacco essential oil is prepared according to a preparation method of the tobacco essential oil.

[0018] The invention discloses an application of tobacco essential oil in cigarettes.

[0019] Preferably, in the above technical solution, the application is to inject tobacco essential oil into cigarettes to improve the coordination of tobacco aroma, increase the aroma volume and richness, increase the sweetness, and reduce irritation.

[0020] The above technical solution of the present invention has the following beneficial effects:

[0021] The present invention adopts an ethanol-sodium chloride-water solvent system and a dynamic reciprocating magnetic field assisted extraction technology, combined with the use of a reusable graphene nanoscroll-wrapped ferroferric oxide nanoparticle composite material (FG), which not only improves the extraction efficiency and reduces the production cost, but also maintains the heat-sensitive components of tobacco essential oil and optimizes the sensory quality and taste of cigarettes. The Zimbabwe tobacco essential oil can be well coordinated with the cigarette aroma, significantly improve the cigarette quality, soften the cigarette smoke, enrich the aroma, improve the sweetness and fineness of the cigarette, reduce stimulation, etc., and has the potential for industrial production. DETAILED DESCRIPTION

[0022] Various exemplary embodiments of the present invention will now be described in detail. It should be noted that the relative arrangement of components and steps, numerical expressions and numerical values ​​set forth in these embodiments do not limit the scope of the present invention unless otherwise specifically stated.

[0023] Principles of this application:

[0024] Dynamic reciprocating magnetic field assisted extraction

[0025] Ethanol-sodium chloride-water introduces metal ions, which can effectively improve the magnetic effect of the solvent system under the action of the magnetic field, accelerate solvent extraction, and improve extraction efficiency. The extraction rate of Zimbabwe tobacco essential oil prepared by this method is about 1.52%, which effectively saves production costs. The graphene nanoscroll-wrapped ferroferric oxide nanoparticle composite material (hereinafter referred to as FG) is reusable, easy to industrialize, and has good application potential.

[0026] For example, the magnetic field can change the surface tension, viscosity, density, conductivity, etc. of a material system, thereby affecting the physical and chemical properties of the material, thereby achieving the separation of the material system.

[0027] Strong magnetic field assisted efficient extraction of Zimbabwe tobacco leaves to obtain crude extracts, membrane separation to obtain Zimbabwe tobacco extracts. After membrane separation, organic phases with different components were obtained to prepare Zimbabwe essential oil.

[0028] Example 1

[0029] A method for preparing tobacco essential oil comprises the following steps:

[0030] 1. Take 500 g of Zimbabwean tobacco leaves from 2020, keep them in an oven at 45°C for 12 hours, grind them with a grinder, and pass them through a 40-mesh sieve to obtain Zimbabwean tobacco powder;

[0031] 2. Prepare ethanol: water in a ratio of 1:1 (mass ratio) as the extraction solvent W1; the mass ratio of tobacco dust to the extraction solvent is 1:8;

[0032] 3. According to the above ratio, weigh 30 g of Zimbabwean tobacco powder and extraction solvent respectively, add them into the extraction tank, heat to 85°C and extract for 4 hours. After the extraction, cool and filter to obtain Zimbabwe crude extract T1.

[0033] 4. The Zimbabwe crude extract was transferred to a concentration tank, and the organic solvent and water in the extract were removed by vacuum distillation using a rotary evaporator to obtain Zimbabwe extract, wherein the vacuum concentration temperature was 40° C., the vacuum pressure was 80 Pa, and the concentration of the Zimbabwe extract was 1.0 g / mL.

[0034] 5. The Zimbabwe extract was separated by membrane to obtain Zimbabwe tobacco essential oil with an extraction rate of 1.24%.

[0035] Specifically, a 50 nm ceramic membrane and a 50 kDa rolled organic membrane were used to separate the Zimbabwe essential oil, and the permeate was further concentrated using reverse osmosis technology to obtain a concentrate, which was diluted to a concentration of 10% using 50% ethanol / water, namely, Zimbabwe tobacco essential oil A1.

[0036] 6. Use an essence and flavor injector to add Zimbabwe tobacco essential oil A1 to a blank heated cigarette, with the added amount being 0.8% of the weight of the tobacco shreds. After the injection, keep the mixture in a constant temperature and humidity environment for 48 hours to obtain a sample cigarette Y1.

[0037] Example 2

[0038] 1. Prepare a solution with a mass ratio of ethanol-water-sodium chloride of 50:45:5 as the extraction solvent W2; the mass ratio of tobacco dust and extract solvent is 1:10; the amount of FG added is 1‰ of the total mass, and it is wrapped with filter cloth.

[0039] 2. According to the above proportions, weigh 30 g of Zimbabwean tobacco powder, extraction solvent W2 and FG respectively, add them into the extraction tank, heat to 85°C and extract for 4 hours. After the extraction, cool and filter to obtain Zimbabwean crude extract T2.

[0040] 3. The Zimbabwe crude extract T2 was transferred to a concentration tank, and the organic solvent and water in the extract were removed by vacuum distillation using a rotary evaporator to obtain Zimbabwe extract, wherein the vacuum concentration temperature was 40° C., the vacuum pressure was 80 Pa, and the concentration of the Zimbabwe extract was 1.0 g / mL.

[0041] 4. The Zimbabwe extract was separated by membrane to obtain Zimbabwe tobacco essential oil with an extraction rate of 1.52%.

[0042] Specifically, a 50 nm ceramic membrane and a 50 kDa rolled organic membrane were used to separate the Zimbabwe essential oil, and the permeate was further concentrated using reverse osmosis technology to obtain a concentrate, which was diluted to a concentration of 10% using 50% ethanol / water, namely, Zimbabwe tobacco essential oil A2.

[0043] 5. Use an essence and flavor injector to add Zimbabwe tobacco essential oil A2 to a blank heated cigarette, with the added amount being 0.8% of the weight of the tobacco shreds. After the injection, keep the mixture in a constant temperature and humidity environment for 48 hours to obtain a sample cigarette Y2.

[0044] Example 3

[0045] 1. Prepare a solution with a mass ratio of ethanol-water-sodium chloride of 50:45:5 as the extraction solvent W2; the mass ratio of tobacco dust and extract solvent is 1:10; the amount of FG added is 1‰ of the total mass, and it is wrapped with filter cloth.

[0046] 2. According to the above proportions, weigh 30 g of Zimbabwean tobacco powder, extraction solvent W2 and FG respectively, add them into the extraction tank, heat to 85°C and extract for 4 hours. After the extraction, cool and filter to obtain Zimbabwean crude extract T2.

[0047] 3. The Zimbabwe crude extract T2 was transferred to a concentration tank, and the organic solvent and water in the extract were removed by vacuum distillation using a rotary evaporator to obtain Zimbabwe extract, wherein the vacuum concentration temperature was 40° C., the vacuum pressure was 80 Pa, and the concentration of the Zimbabwe extract was 1.0 g / mL.

[0048] 4. The Zimbabwe extract was diluted with 50% ethanol / water to a concentration of 10% to obtain Zimbabwe extract G3 with an extraction rate of 36.50%.

[0049] 5. Use an essence and flavor injector to add Zimbabwe tobacco extract G3 to the blank heated cigarette, with the added amount being 0.8% of the weight of the tobacco shreds. After the injection, keep the mixture in a constant temperature and humidity environment for 48 hours to obtain a sample cigarette Y3.

[0050] The sample cigarettes of Examples 1-3 were evaluated, and the results are shown in Table 1.

[0051] Table 1 Evaluation results

[0052]

[0053] In summary, the tobacco essential oil prepared in the present application is used in the field of heated cigarettes, which can not only effectively give the heated cigarettes the original tobacco aroma, but also improve the taste and flavor of the heated cigarettes, improve the overall aroma quality, and reduce irritation and residue.

[0054] Although the present invention has been disclosed as above by the embodiments, it is not intended to limit the present invention. Any person skilled in the art may make various choices and modifications without departing from the spirit and scope of the present invention. Therefore, the protection scope of the present invention is limited by the claims and their equivalents.

Claims

1. A method for preparing tobacco essential oil, characterized in that, The following steps are involved: (1) drying the tobacco leaves until the moisture content is less than 5%, and crushing them into tobacco powder; (2) adding cigarette dust, extraction solvent and graphene nanoscroll-wrapped ferroferric oxide nanoparticle composite material (FG) into an extraction tank for extraction, and cooling and filtering after extraction to obtain a crude extract; wherein the mass ratio of cigarette dust to extraction solvent is 1:(8-12), and the amount of FG added is 1‰ of the total mass; (3) transferring the crude extract to a concentration tank, concentrating under reduced pressure to remove the organic solvent and water to obtain an extract; (4) Using membrane separation technology to obtain tobacco essential oil from the extract.

2. The preparation method of tobacco essential oil according to claim 1, characterized in that, Step (1) is specifically as follows: keeping the tobacco leaves in an oven at 40-50° C. for 12-24 hours until the moisture content is less than 5.0%, and then crushing the tobacco leaves into 40-50 mesh tobacco powder for later use.

3. The preparation method of tobacco essential oil according to claim 1, characterized in that, In step (2), the extraction solvent is a mixture of ethanol, water and sodium chloride in a mass ratio of 50:45:5; the extraction condition is 85° C. for 4 to 10 hours.

4. The preparation method of tobacco essential oil according to claim 1, characterized in that, In step (2), the amount of the tobacco dust, the extraction solvent and the FG added is 2 / 3 of the volume of the extraction tank, and after the FG is taken out, it is washed 3-5 times with a 30% ethanol / water solution.

5. The preparation method of tobacco essential oil according to claim 1, characterized in that, In step (3), the temperature of the reduced pressure concentration is 40-60° C., the vacuum pressure is 50-100 Pa, and the concentration of the extract is 1.0-1.2 g / mL.

6. The preparation method of tobacco essential oil according to claim 1, characterized in that, Step (4) is specifically as follows: using a 50nm ceramic membrane and a 50kDa rolled organic membrane to separate the tobacco essential oil in turn, and further concentrating the permeate using reverse osmosis technology to obtain a concentrated solution, which is diluted to a concentration of 10% using 50% ethanol / water, namely, tobacco essential oil.

7. The preparation method of tobacco essential oil according to claim 1, characterized in that, The tobacco leaves are Zimbabwean tobacco leaves.

8. A tobacco essential oil, characterized in that The tobacco essential oil is prepared according to the preparation method of tobacco essential oil according to any one of claims 1-7.

9. Use of the tobacco essential oil prepared according to any one of the preparation methods of claims 1 to 7 or the tobacco essential oil according to claim 8 in cigarettes.

10. The use according to claim 9, characterized in that: The application is to inject tobacco essential oil into cigarettes to improve the coordination of tobacco aroma, increase the amount and richness of aroma, increase sweetness and reduce irritation.

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