A method for extracting high-satisfaction, high-aroma tobacco extract and its application in cigarettes
By combining molecular distillation and emulsion membrane extraction, a highly satisfying and aromatic tobacco extract is efficiently extracted from tobacco raw materials, solving the problems of insufficient aroma and resource waste in heated cigarettes, and achieving efficient and environmentally friendly utilization of tobacco components and improvement of smoking quality.
Patent Information
- Application Number
- CN202310616805.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-05-29
- Publication Date
- 2025-11-07
- Estimated Expiration
- 2043-05-29
AI Technical Summary
Existing technologies cannot effectively utilize the water-soluble components in tobacco raw materials, resulting in resource waste. At the same time, heating cigarettes results in insufficient aroma and satisfaction. Traditional extraction methods are energy-intensive, inefficient, and have negative impacts.
An extraction method combining molecular distillation and emulsion membrane extraction is used to extract highly satisfying and aromatic tobacco extracts from tobacco raw materials through a multi-step process, including hot reflux extraction, vacuum concentration, layering, and emulsion separation, selectively enriching the characteristic aroma components of tobacco.
It achieves efficient utilization of tobacco raw materials, improves the aroma concentration and satisfaction of heated cigarettes, reduces off-flavors and irritation, enhances smoking quality, and reduces energy consumption and costs.
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Abstract
Description
TECHNICAL FIELD
[0001] The present application belongs to the technical field of tobacco flavor production, and particularly relates to an extraction method of high-satisfaction and high-aroma tobacco extract and application thereof in cigarettes. BACKGROUND
[0002] Heat-not-burn is a new type of tobacco product that uses a special heat source (200-500℃) to heat and generate smoke by volatilizing flavoring substances to meet the needs of consumers. Compared with traditional cigarettes, most harmful components in the smoke of heat-not-burn cigarettes are reduced by more than 90%, which is an important trend in the future development of the tobacco market. However, compared with traditional cigarettes, heat-not-burn cigarettes have great differences in aroma and taste, and it is difficult to overcome the shortcomings of low smoke density and small strength, which cannot provide consumers with satisfactory smoke volume and satisfaction similar to traditional cigarettes, seriously restricting the development of heat-not-burn cigarettes.
[0003] Therefore, in order to overcome the above-mentioned shortcomings of heat-not-burn cigarettes, a large amount of tobacco extract, such as tobacco water paste or alcohol paste, is usually added to heat-not-burn cigarettes. However, such tobacco extract contains a large amount of macromolecules and high-boiling-point substances, and the content of volatile flavoring components and satisfaction-inducing components is relatively low. Due to the low heating temperature of heat-not-burn cigarettes, the flavoring components in the tobacco extract cannot be completely released during smoking, thus the problem cannot be fundamentally solved. At the same time, it also introduces the problems of offensive odor and irritation, which brings negative effects.
[0004] At present, the methods for separating and enriching volatile flavoring components and satisfaction-inducing components of tobacco mainly include organic solvent (diethyl ether, chloroform, petroleum ether, etc.) extraction, steam distillation, molecular distillation, and supercritical extraction. However, these methods often only enrich the volatile components in the tobacco raw material, while the remaining water-soluble components in the tobacco raw material contain a large amount of latent aroma substances that induce satisfaction, but also contain macromolecular impurities that have a negative impact on cigarette smoking. Therefore, the remaining water-soluble components in the tobacco raw material are often discarded as waste, causing great waste. In addition, the above-mentioned treatments have high energy consumption, low efficiency, high cost, large processing difficulty of equipment, low safety, and large pollution.
[0005] In order to solve the above problems, the present application is proposed. SUMMARY
[0006] The first aspect of the present application provides an extraction method of high-satisfaction and high-aroma tobacco extract, comprising the following steps:
[0007] (1) mixing a certain mass of tobacco raw material with a certain mass percentage concentration of ethanol, and performing two times of hot reflux extraction at 60-90℃, filtering to obtain a tobacco extract.
[0008] (2) The tobacco extract solution obtained in step (1) is vacuum concentrated at 60-70°C until the density reaches 1.1-1.3 g / cm 3 , to obtain a tobacco concentrated solution.
[0009] (3) The tobacco concentrated solution obtained in step (2) is mixed with ethanol of a certain mass percentage concentration, and then uniformly cooled and stored for 6-24 h to allow the layers to separate. Filtration is performed to obtain an upper alcohol solution and a lower water-soluble extract.
[0010] (4) The upper alcohol solution obtained in step (3) is vacuum concentrated at 60-70°C until no solvent is evaporated, to obtain a tobacco extract.
[0011] (5) The tobacco extract obtained in step (4) is subjected to molecular distillation, and the distillate is collected to obtain a highly aroma-producing tobacco extract A.
[0012] (6) The lower water-soluble extract obtained in step (3) is mixed with an alkali solution, and the pH value is adjusted to 10-14. Filtration is performed using filter cloth to obtain a filtrate.
[0013] (7) A surfactant, a carrier, and an oil phase are mixed in a certain proportion, and then an inner water phase solution is added and stirred in an emulsification container at a stirring speed of 3000-10000 r / min to prepare a stable W / O / W emulsion.
[0014] (8) The filtrate obtained in step (6) is mixed with the W / O / W emulsion obtained in step (7), and then stirred at a speed of 100-400 r / min. After standing, the emulsion phase and the water phase are separated.
[0015] (9) The emulsion phase obtained in step (8) is separated by a microfiltration membrane assembly at room temperature. After the filtrate is allowed to stand and separate into layers, the oil phase is recovered and reused for the preparation of the emulsion in the next cycle, and the water phase filtrate is collected for use.
[0016] (10) The water phase filtrate obtained in step (9) is vacuum concentrated at 60-70°C until the density reaches 1.1-1.3 g / cm 3 , to obtain a highly satisfying tobacco extract B.
[0017] (11) The tobacco extract A and the tobacco extract B are mixed in a mass percentage ratio of (50%-80%):(20%-50%) to obtain the tobacco extract.
[0018] Preferably, the tobacco raw material in step (1) is selected from one or more of tobacco dust, tobacco leaf fragments, tobacco stems, and tobacco shreds, and the specific conditions for the extraction are: an ethanol mass percentage concentration of 20-90%, a mass ratio of the tobacco raw material to ethanol of 1:5-1:20, and two extraction times, each for 2-3 hours.
[0019] Preferably, the specific conditions for the extraction in step (3) are: an ethanol mass percentage concentration of 80-100%, a mass ratio of the tobacco concentrate to ethanol of 1:1-1:10, and a refrigeration temperature of -8 to 4℃.
[0020] Preferably, the specific conditions for the molecular distillation in step (5) are: a vacuum degree of 1×10 -4 -1×10 -3 KPa, a feed temperature of 60-90℃, a distillation temperature of 90-130℃, and a condensation temperature of 20-50℃.
[0021] Preferably, the lye in step (6) is selected from one or more of saturated limestone, a 5%-20% mass percentage concentration sodium hydroxide aqueous solution, a 5%-20% mass percentage concentration potassium hydroxide aqueous solution, a 5%-20% mass percentage concentration sodium carbonate aqueous solution, and a 5%-20% mass percentage concentration potassium carbonate aqueous solution, and the mass ratio of the lower aqueous extract to the lye is 1:1-1:10.
[0022] Preferably, the oil phase in step (7) is selected from one or more of glyceryl triacetate, corn oil, peanut oil, almond oil, coconut oil, and olive oil, the surfactant is sucrose ester and / or glyceryl caprylate, the carrier is pentanedione, the internal aqueous phase solution has a mass percentage concentration of 5-20% and is specifically selected from one or more of lactic acid, malic acid, citric acid, and benzoic acid, the stirring time is 10-60 minutes, and the volume ratio of the oil phase:surfactant:carrier:internal aqueous phase solution is (30-40):(1-5):(1-5):(30-40).
[0023] Preferably, the stirring time in step (8) is 10-30 minutes, and the standing time is 10-60 minutes.
[0024] Preferably, the specific conditions for the separation in step (9) are: a microfiltration membrane assembly with a molecular weight cut-off of 200-300 nm is used, and the microfiltration is performed at room temperature under a pressure of 0.08-0.12 MPa.
[0025] The second aspect of the present application provides a use of the high-satisfaction, high-aroma tobacco extract of the first aspect, wherein the tobacco extract is added to a heating cigarette core to form a heating cigarette.
[0026] Preferably, the mass ratio of the tobacco extract to the heating cigarette core is (1:1000)-(50:1000).
[0027] The above technical solutions can be freely combined without contradiction.
[0028] The present application has the following advantages:
[0029] 1. The extraction method of the high satisfaction and high aroma tobacco extract provided by the present application first adopts the technology of combining molecular distillation and emulsion membrane method. At present, the methods for extracting tobacco raw materials such as organic solvent extraction, water vapor distillation or molecular distillation only extract the volatile components in the tobacco raw materials. Although the remaining water-soluble components in the tobacco after extraction contain a large amount of latent aroma substances that can bring satisfaction, they also contain a large amount of macromolecular impurities such as starch, cellulose, pectin and protein that can bring cigarette miscellaneous gas and have a negative impact on cigarette smoking. Therefore, the remaining water-soluble components in the tobacco are often discarded as waste, causing great waste. The extraction method of the extract can selectively enrich the tobacco characteristic aroma components in the remaining water-soluble components in the tobacco raw materials, maximizing the utilization of the tobacco raw materials. Through the molecular distillation process, the distillate rich in free nicotine at a specific temperature range is collected, and the emulsion membrane system is established to selectively separate the water-soluble nicotine salt components, so that the free nicotine and water-soluble nicotine salt in the tobacco raw materials can be obtained at the same time, with high yield, high selectivity and effective enrichment of the alkaloid components in the tobacco.
[0030] 2. The reagents used in the emulsion system of the present application: the oil phase, the surfactant, the carrier and the internal water phase solution are all additives in the list of additives permitted for use in tobacco products in YQ52-2015, effectively solving the problems of the reagents used in the emulsion membrane method reported at present, such as certain toxicity, inability to be added in cigarettes, obvious irritation of the oral cavity, nasal cavity and throat, obvious miscellaneous gas, residual aftertaste and the like. Moreover, these additives used in the present application have a certain contribution to the aroma of cigarettes, and improve the smoking quality of cigarettes while enriching the alkaloid components in the tobacco.
[0031] 3. The emulsion membrane separation method adopted by the present application can selectively separate tobacco alkaloids from tobacco raw materials through the emulsion membrane system formed by the internal water phase, the oil phase, the surfactant and the carrier. The organic solution extraction and the internal water phase counter-extraction process are carried out at the same time to approach complete extraction. The oil phase can be recycled for the preparation of emulsion next time, and the extraction has high yield, high speed, high selectivity, small amount of reagents required, short separation time, simple equipment, environmental protection and safety, and low product cost. It can effectively solve the problems of high energy consumption, low yield and high temperature in the traditional extraction of tobacco alkaloids, and can realize fine separation at room temperature and reduce energy consumption. It is a green and environmentally friendly method with high economic benefits.
[0032] 4、The high satisfaction, high aroma tobacco extract obtained by the unique extraction method is added to the heated cigarette, which has the effects of supplementing tobacco aroma, significantly increasing the sweet aroma, improving the fineness and softness of smoke, improving the richness and fullness of smoke, improving the level and satisfaction of tobacco aroma, and improving the smoking quality. The effect is unpredictable by those skilled in the art. The tobacco extract obtained by the present application fully meets the needs of consumers for heated cigarettes. DETAILED DESCRIPTION
[0033] The application will be further described below in combination with examples.
[0034] Example 1
[0035] A high satisfaction, high aroma tobacco extract extraction method, comprising the following steps:
[0036] (1) Take 1 kg of tobacco leaf fragments, add 5 kg of 60% ethanol by mass percentage concentration; carry out two hot reflux extractions under the condition of 70℃, the first extraction time is 3h; the second extraction time is 2h; after the two extraction liquids are combined, filter with 400 mesh gauze to obtain a tobacco extraction liquid.
[0037] (2) The tobacco extraction liquid obtained in step (1) is vacuum concentrated at 60℃ until the density reaches 1.2g / cm 3 , to obtain a tobacco concentrate;
[0038] (3) After the tobacco concentrate obtained in step (2) is uniformly mixed with 95% ethanol by mass percentage concentration, the mass ratio of tobacco concentrate to ethanol is 1:5, and the mixture is stored at 4℃ for 12h to stand and stratify, filter to obtain an upper alcohol solution and a lower water-soluble extract;
[0039] (4) The upper alcohol solution obtained in step (3) is vacuum concentrated at 65℃ until no solvent is distilled out, to obtain a tobacco extract;
[0040] (5) The tobacco extract obtained in step (4) is subjected to molecular distillation under the conditions of vacuum degree 1×10 -3 KPa, feed temperature 70℃, distillation temperature 100℃, and condensation temperature 30℃. The distillate is collected to obtain a high-aroma tobacco extract A;
[0041] (6) The lower water-soluble extract obtained in step (3) is uniformly mixed with 5% sodium hydroxide aqueous solution by mass percentage concentration, the mass ratio of lower water-soluble extract to 5% sodium hydroxide aqueous solution by mass percentage concentration is 1:5, the PH value is adjusted to 12, and the filter cloth is filtered to obtain a filtrate;
[0042] (7) Mix triacetin, sucrose ester and pentanedione, add 10% lactic acid solution, and place in an emulsification container. The volume ratio of triacetin, sucrose ester, pentanedione and 10% lactic acid solution is 30:1:1:30. Stir at 10,000 r / min to obtain stable W / O / W emulsion.
[0043] (8) Mix the filtrate obtained in step (6) with the W / O / W emulsion obtained in step (7), and stir at 300 r / min for 20 min. After standing for 30 min, separate the emulsion phase from the water phase.
[0044] (9) Separate the emulsion phase obtained in step (8) by microfiltration membrane assembly with a molecular weight cut-off of 200 nm at room temperature and 0.08 MPa. After standing and layering, recover the oil phase for reuse in the next preparation of emulsion, and collect the water phase filtrate for use.
[0045] (10) Add 10% propylene glycol to the water phase filtrate obtained in step (9), and concentrate under vacuum at 60°C until the density reaches 1.25 g / cm 3 to obtain tobacco extract B with high satisfaction.
[0046] (11) Mix tobacco extract A and tobacco extract B in a mass ratio of 50:50 to obtain the high-satisfaction, high-aroma tobacco extract.
[0047] Example 2
[0048] A method for extracting a high-satisfaction, high-aroma tobacco extract, comprising the following steps:
[0049] (1) Take 1 kg of tobacco leaf fragments and tobacco dust mixture, and add 8 kg of 70% ethanol. Perform two hot reflux extractions at 80°C, with the first extraction time being 3 h and the second extraction time being 2 h. After combining the two extraction solutions, filter with 400-mesh gauze to obtain a tobacco extract.
[0050] (2) Vacuum concentrate the tobacco extract obtained in step (1) at 65°C until the density reaches 1.3 g / cm 3 to obtain a tobacco concentrate.
[0051] (3) Mix the tobacco concentrate obtained in step (2) with anhydrous ethanol, with the mass ratio of tobacco concentrate to ethanol being 1:3. After standing for 12 h at 4°C, filter to obtain an upper alcohol solution and a lower water-soluble extract.
[0052] (4) The upper alcohol solution obtained in step (3) is concentrated under vacuum at 60°C until no solvent is evaporated, to obtain a tobacco extract;
[0053] (5) The tobacco extract obtained in step (4) is subjected to molecular distillation under the conditions of a vacuum degree of 1 x 10 -4 KPa, a feeding temperature of 60°C, a distillation temperature of 110°C, and a condensation temperature of 40°C. The distillate is collected to obtain a highly aroma-producing tobacco extract A;
[0054] (6) The lower water-soluble extract obtained in step (3) is mixed with a 10% sodium carbonate solution to obtain a filtrate, with the mass ratio of the lower water-soluble extract to the 10% sodium carbonate solution being 1:5, and the pH value being adjusted to 11.
[0055] (7) Olive oil, glyceryl caprylate, and pentanedione are mixed, and a 20% benzoic acid solution is added to the mixture, which is then placed in an emulsification container. The volume ratio of the olive oil, glyceryl caprylate, pentanedione, and 20% benzoic acid solution is 40:2:1:30, and high-speed stirring is performed at 8000 r / min to obtain a stable W / O / W emulsion.
[0056] (8) The filtrate obtained in step (6) is mixed with the emulsion obtained in step (7), and stirring is performed at a speed of 200 r / min for 30 min. After standing for 50 min, the emulsion phase and the water phase are separated.
[0057] (9) The emulsion phase obtained in step (8) is separated by a microfiltration membrane assembly with a molecular weight cut-off of 300 nm at room temperature and under a pressure of 0.10 MPa. After the filtrate is allowed to stand and separate into layers, the oil phase is recovered and reused for the preparation of the emulsion, and the water phase filtrate is collected for use.
[0058] (10) The water phase filtrate obtained in step (9) is added with a 10% propylene glycol solution, and vacuum concentration is performed at 70°C until the density reaches 1.2 g / cm 3 , to obtain a highly satisfying tobacco extract B.
[0059] (11) The tobacco extract A and the tobacco extract B are mixed in a mass ratio of 60%:40% to obtain the highly satisfying and highly aroma-producing tobacco extract.
[0060] Example 3
[0061] The tobacco extract prepared in Example 1 is detected by gas chromatography-mass spectrometry (GC-MS) analysis:
[0062] (1) Gas chromatography conditions: Chromatographic column: DB-5MS quartz capillary column (30 m x 0.25 mm, 0.25 μm); programmed temperature: initial temperature of 60 °C, holding for 1 min, increasing to 170 °C at a rate of 8 °C / min, holding for 3 min, increasing to 260 °C at a rate of 12 °C / min, holding for 18 min; injection port temperature: 200 °C; column oven temperature: 60 °C; injection mode: split; column flow: 1 mL / min; purge flow: 3 mL / min; split ratio: 5:1; carrier gas: high-purity helium; injection volume: 1 μL; solvent delay: 2 min.
[0063] (2) Mass spectrometry conditions: ionization mode: EI; electron energy: 70 eV; interface temperature: 250 °C; ion source temperature: 200 °C; acquisition mode: scan; scan range: 40-500 amu.
[0064] (3) Qualitative analysis: qualitative analysis was performed by using mass spectrometry as detector and gas chromatography, and using NIST spectral library retrieval.
[0065] (4) Quantitative analysis: internal standard was 99% naphthalene, and internal standard method was used for semi-quantitative analysis of the aroma components. The content of the aroma components was calculated according to the following formula:
[0066]
[0067] In the formula:
[0068] X - content of each compound, μg / g; As - integral peak area of each compound; Ai - integral peak area of internal standard substance; mi - mass of internal standard substance, g; M - mass of sample, g.
[0069] The specific component content is shown in Table 1.
[0070] Table 1 Volatile components and relative content analysis of tobacco extract prepared in Example 1
[0071]
[0072]
[0073] As can be seen from Table 1, the tobacco extract prepared by the method of Example 1 can enrich a large amount of tobacco characteristic aroma components. The component with the highest content is nicotine, the pyrolysis product of which produces resin-like aroma, and nicotine has obvious promoting effect on the sensory quality of cigarettes, so that the consumer can obtain satisfaction. The content of neophytadiene in the tobacco extract is only less than that of nicotine, and neophytadiene is a chlorophyll degradation product, has fresh aroma, can reduce the irritability of smoke through combustion of alcohol and smoke, and has strong influence on the taste of fine and soft smoke, improvement of aftertaste, and reduction of irritation. Neophytadiene can effectively increase the richness of smoke. Giganteonitrone A, giganteonitrone B, giganteonitrone C, giganteonitrone D, isophorone oxide, geranylacetone, dihydroactinidiolide and the like have important role in improving the aroma quality of cigarettes, can obviously increase the amount of aroma, reduce the odor and irritability, improve the aftertaste, and endow the cigarettes with the characteristic aroma of tobacco. Solanone is a very key aroma substance in tobacco, is produced by biochemical degradation of cembranoids in tobacco, can significantly enhance the tobacco aroma, improve the taste, harmonize the smoke, and reduce the irritation. Aroma substances such as palmitic acid, linolenic acid, and linoleic acid can adjust the acidity and alkalinity of tobacco, increase the richness and harmony of smoke.
[0074] Comparative Example 1
[0075] A method for extracting a tobacco extract, 5 times petroleum ether is added to tobacco fragments, and twice hot reflux extraction is performed at 60°C. The extract is concentrated to 1.2 g / cm 3 at 65°C and 80 kPa to obtain a petroleum ether extracted tobacco extract.
[0076] Comparative Example 2
[0077] A method for extracting a tobacco extract, steps 1-5 are the same as those in Example 1 to obtain a molecularly distilled tobacco extract.
[0078] Comparative Example 3
[0079] A method for extracting a tobacco extract, steps 1-3 are the same as those in Example 1, the lower water-soluble extract is taken out and prepared into a tobacco extract according to steps 7-10, wherein step 7 is changed to: sulfurized kerosene, Span 80 and secondary octanol are mixed, and after 5% sulfuric acid aqueous solution is added, the mixture is placed in an emulsification container, and the volume ratio of the three kinds of solvents is 89:5:3:89. The tobacco extract is obtained.
[0080] Example 4
[0081] In order to compare the influence of different processes on the components of the tobacco extract, the tobacco extracts prepared by Example 1, Comparative Example 1, Comparative Example 2 and Comparative Example 3 of the present application are respectively subjected to aroma component analysis according to the method of Example 3, and the total amount of tobacco alkaloids and aroma substances is statistically analyzed. The results are shown in Table 2.
[0082] Table 2 statistical results of different tobacco extract ingredient content
[0083]
[0084] The results show that the total amount of aroma-producing substances in the tobacco extract obtained by the method of the present application is the highest (10146.677 μg / g), which is significantly higher than that of the traditional petroleum ether extraction method, i.e. Comparative Example 1 (7682.822 μg / g). It is also higher than that of the tobacco extract prepared only by molecular distillation method, i.e. Comparative Example 2 (9028.214 μg / g), indicating that the method of the present application can accumulate a large amount of tobacco characteristic aroma-producing components, and realizes the full utilization of tobacco raw materials. In addition, the content of tobacco alkaloids in the tobacco extract obtained by the present application is also the highest (47.59%), and is higher than that of the existing emulsion membrane method, i.e. Comparative Example 3 (30.28%). This is because nicotine in tobacco exists in free state and nicotine salt, and the method used in the present application can separate free nicotine, while accumulating water-soluble nicotine salt, and has high yield, which can effectively accumulate alkaloid components in tobacco.
[0085] Example 5
[0086] Cigarette sensory evaluation: The tobacco extracts obtained by the present application Example 1, Comparative Example 1, Comparative Example 2, Comparative Example 3 were respectively diluted by 0.5% per heated cigarette core, and added to the heated cigarette core section, to obtain cigarette-Example 1 (50 pieces), cigarette-Comparative Example 1 (50 pieces), cigarette-Comparative Example 2 (50 pieces), cigarette-Comparative Example 3 (50 pieces). The blank cigarette (50 pieces) without adding flavor was used as a control. All the above cigarettes were placed in a constant temperature and humidity box (temperature 22±1℃, humidity 60±2%) for 48h, and evaluated by experts with cigarette evaluation qualification according to "GB5606.4-2005 Cigarette Part 4 Sensory Technical Requirements", "YC / T 497-2014 Sensory Evaluation Method of Chinese Cigarette Style in Cigarette". The evaluation results are shown in Tables 3, 4 and 5:
[0087] Table 3 tobacco extract cigarette evaluation results
[0088]
[0089] Table 4 tobacco extract cigarette comfort characteristic evaluation results
[0090]
[0091] Table 5 tobacco extract cigarette smoke characteristic evaluation results
[0092]
[0093] The results show that the tobacco extract obtained by the application has the effects of supplementing tobacco flavor, obviously increasing sweet and pure tobacco flavor, improving tobacco smoke fineness and softness, improving smoke richness and fullness, improving tobacco flavor level and satisfaction, covering the smell of burning, leaving a pure and natural aftertaste, and improving the smoking quality of the heated cigarette.
[0094] As can be seen from Tables 3, 4 and 5, the heated cigarette added with the tobacco extract of the application has outstanding tobacco flavor, significantly improves smoke concentration and strength, has comfortable aftertaste, significantly reduces miscellaneous smell, and greatly improves irritation. The tobacco extract in Comparative Examples 1-3 has no above effects.
[0095] This is because the petroleum ether used in Comparative Example 1 is extremely volatile, flammable and explosive, has great processing difficulty, low safety, and great pollution, and has kerosene smell, which easily brings miscellaneous smell to the extracted tobacco extract. The tobacco extract prepared by the molecular distillation method in Comparative Example 2 has full tobacco flavor, natural aftertaste, and reduced miscellaneous smell, but has a lack of satisfaction for the heated cigarette. The solvent used in the current emulsion liquid membrane method in Comparative Example 3 is sulfided kerosene, Span 80, secondary octanol and sulfuric acid, which all have certain toxicity and cannot be added in the cigarette, and obviously cause oral cavity, nasal cavity and throat irritation, and oral cavity residue aftertaste.
[0096] Therefore, the extraction method provided by the application can not only enrich the high-aroma aroma components in the tobacco raw material, but also enrich the high-satisfaction components, thereby improving the added value of the tobacco raw material.
[0097] The above is only a specific embodiment of the application, but the protection scope of the application is not limited thereto, and any person skilled in the art can easily think of changes or replacements within the technical range disclosed by the application, which should be covered in the protection scope of the application.
Claims
1. A method for extracting a high-satisfying, high- aroma tobacco extract, characterized by, The method comprises the following steps: (1) mixing a certain mass of tobacco raw material with a certain mass percentage concentration of ethanol, and performing twice hot reflux extraction at 60-90℃, filtering to obtain a tobacco extract; (2) The tobacco extract solution obtained in step (1) is vacuum concentrated at 60-70°C until the density reaches 1.1-1.3 g / cm 3 , to obtain a tobacco concentrated solution; (3) uniformly mixing the tobacco concentrate obtained in step (2) with a certain mass percentage concentration of ethanol, and then placing it in a refrigerator for 6-24h to stand and separate into layers, filtering to obtain an upper alcohol solution and a lower water-soluble extract; (4) vacuum concentrating the upper alcohol solution obtained in step (3) at 60-70℃ until no solvent is evaporated, to obtain a tobacco extract; (5) performing molecular distillation on the tobacco extract obtained in step (4), and collecting the distillate, to obtain a high-fragrance tobacco extract A; (6) uniformly mixing the lower water-soluble extract obtained in step (3) with a lye, adjusting the pH value to 10-14, and filtering with a filter cloth to obtain a filtrate; (7) mixing a surfactant, a carrier and an oil phase according to a certain proportion, adding an inner water phase solution, and then placing it in an emulsifying container for stirring, wherein the volume ratio of the oil phase, the surfactant, the carrier and the inner water phase solution is (30-40):(1-5):(1-5):(30-40), the stirring speed is 3000-10000 r / min, and the stirring time is 10-60min, to prepare a stable W / O / W emulsion; the oil phase is selected from one or more of triacetin, corn oil, peanut oil, almond oil, coconut oil and olive oil, the surfactant is sucrose ester and / or glyceryl caprylate, the carrier is pentanedione, the mass percentage concentration of the inner water phase solution is 5-20%, and the inner water phase solution is selected from one or more of lactic acid, malic acid, citric acid and benzoic acid; (8) uniformly mixing the filtrate obtained in step (6) with the W / O / W emulsion obtained in step (7), stirring at a speed of 100-400 r / min, and then standing and separating into layers to separate the emulsion phase and the water phase; (9) separating the emulsion phase obtained in step (8) through a microfiltration membrane assembly at room temperature, standing and separating the filtrate into layers, recovering the oil phase for re-preparing the emulsion in the next time, and collecting the water phase filtrate for use; (10) The aqueous phase filtrate obtained in step (9) is added with propylene glycol at a mass percentage concentration of 10%, and vacuum concentration is carried out at 60-70°C until the density reaches 1.1-1.3 g / cm 3 , i.e. a tobacco extract B with high satisfaction. (11) mixing the tobacco extract A and the tobacco extract B according to a mass percentage ratio of (50%-80%):(20%-50%) to obtain the tobacco extract.
2. The extraction method of a high satisfaction, high aroma tobacco extract according to claim 1, characterized by, The tobacco raw material in step (1) is selected from one or more of tobacco dust, tobacco leaf fragments, tobacco stems and tobacco shreds, and the specific extraction conditions are as follows: the mass percentage concentration of ethanol is 20-90%, the mass ratio of the tobacco raw material to ethanol is 1:5-1:20, and the extraction time is 2-3h each time.
3. The extraction method of a high satisfaction, high aroma tobacco extract according to claim 1, characterized by, The specific extraction conditions in step (3) are as follows: the mass percentage concentration of ethanol is 80-100%, the mass ratio of the tobacco concentrate to ethanol is 1:1-1:10, and the refrigeration temperature is-8~4℃.
4. The extraction method of a high satisfaction, high aroma tobacco extract according to claim 1, characterized by, The specific conditions of the molecular distillation in step (5) are as follows: vacuum degree 1 x 10 -4 -1 x 10 -3 KPa, feed temperature 60-90°C, distillation temperature 90-130°C, and condensation temperature 20-50°C.
5. The extraction method of a high satisfaction, high aroma tobacco extract according to claim 1, characterized by, The alkali solution in step (6) is selected from one or more of saturated lime water, a 5-20% by mass sodium hydroxide aqueous solution, a 5-20% by mass potassium hydroxide aqueous solution, a 5-20% by mass sodium carbonate aqueous solution, and a 5-20% by mass potassium carbonate aqueous solution, and the mass ratio of the lower aqueous extract to the alkali solution is 1:1-1:
10.
6. The extraction method of a high satisfaction, high aroma tobacco extract according to claim 1, characterized by, The stirring time in step (8) is 10-30 min, and the standing time is 10-60 min.
7. The extraction method of a high satisfaction, high aroma tobacco extract according to claim 1, characterized by, The separation in step (9) is performed at room temperature under a pressure of 0.08-0.12 MPa using a microfiltration membrane assembly with a molecular weight cut-off of 200-300 nm.
8. Use of the high-satisfaction, high- aroma tobacco extract obtained by the extraction method according to claim 1, characterized in that, The tobacco extract is added to a heating cigarette core to produce a heating cigarette.
9. Use according to claim 8, characterized in that, The mass ratio of the tobacco extract to the heating cigarette core is (1:1000)-(50:1000).
Citation Information
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