Tobacco extract and preparation method therefor, aerosol-generating substrate, electronic atomization device and heat-not-burn cigarette
The tobacco extract, prepared using specific ingredients and physical methods, solves the problems of low tobacco aroma and poor natural harmony, achieving a richer and more harmonious tobacco aroma with excellent sensory effects.
Patent Information
- Authority / Receiving Office
- WO · WO
- Patent Type
- Applications
- Current Assignee / Owner
- SHENZHEN SMOORE TECH LTD
- Filing Date
- 2025-12-16
- Publication Date
- 2026-07-09
AI Technical Summary
Existing tobacco extracts suffer from problems such as low aroma, poor natural harmony, and poor overall sensory experience in applications.
Tobacco extracts are prepared by combining specific proportions of components such as cephalotrimazole, neophytadiene, dihydroactinidone, megastigmatrienone, palmitic acid, and scopolamine with physical methods such as supercritical carbon dioxide extraction, solvent extraction, and purification techniques.
It retains the aroma of tobacco to the greatest extent, with a rich, natural, and harmonious flavor, resulting in a superior overall sensory experience, and it is less prone to carbon buildup.
Smart Images
Figure PCTCN2025142738-FTAPPB-I100001 
Figure PCTCN2025142738-FTAPPB-I100002 
Figure PCTCN2025142738-FTAPPB-I100003
Abstract
Description
A tobacco extract and its preparation method, an aerosol generating matrix, an electronic atomization device, and heated tobacco products.
[0001] Cross-reference to related applications
[0002] This application claims priority to Chinese Patent Application No. 202411979919X, filed on December 30, 2024, entitled "A Tobacco Extract and Its Preparation Method, Aerosol Generating Matrix, Electronic Atomization Device, Heated Tobacco Cigarette", the entire contents of which are incorporated herein by reference. Technical Field
[0003] This application relates to the field of tobacco technology, specifically to a tobacco extract and its preparation method, an aerosol generating matrix, an electronic atomization device, and a heated non-combustible cigarette. Background Technology
[0004] Tobacco extracts primarily originate from tobacco leaves and a large amount of tobacco waste such as low-grade tobacco leaves, stems, and dust. These raw materials, processed through different extraction techniques, yield extracts with varying flavors and characteristics. Tobacco extracts possess complex aroma components that collectively determine their flavor and quality. When applied to tobacco products, they enhance the richness and quality of the aroma. However, existing tobacco extracts suffer from issues such as low smoky aroma, poor natural harmony, and an overall subpar sensory experience. Summary of the Invention
[0005] The purpose of this application is to overcome the shortcomings of existing tobacco extracts, such as low aroma, poor natural harmony, and poor overall sensory quality, and to provide a tobacco extract and its preparation method, an aerosol generating matrix, an electronic atomization device, and heated non-combustible cigarettes.
[0006] To achieve the above objectives, this application adopts the following technical solution:
[0007] This application provides a tobacco extract, the components of which include: cephalotrimazole, neophytadiene, dihydroactinidone, megastigmatrienone, palmitic acid, and scopolamine.
[0008] The mass ratio of cephalothrix trienol, neophytadiene, dihydroactinidone, megastigmatrienone, palmitic acid, and scopolamine is (1-5):(0.01-0.3):(0.01-0.2):(0.01-0.5):(0.01-1.0):(0.01-0.5).
[0009] Optionally, the components of the tobacco extract, based on the dry matter mass of the tobacco extract, are: 1-5 mg / g cephalotrimethylenediol, 0.01-0.3 mg / g neophytadiene, 0.01-0.2 mg / g dihydroactinidone, 0.01-0.5 mg / g megastigmatrienone, 0.01-1.0 mg / g palmitic acid, and 0.01-0.5 mg / g scopolamine.
[0010] In this application, "dry matter" refers to the components of the tobacco extract other than the solvent. The solvent may be ethanol or an aqueous solution of ethanol, and the dry matter includes: cephalotrimethylenediol, neophytadiene, dihydroactinidone, megastigmatrienone, palmitic acid, and scopolamine.
[0011] Optionally, the tobacco extract may also include caryophyllene.
[0012] Optionally, the mass ratio of cephalotrindiol to caryophyllene is (1-5):(0.001-0.05);
[0013] Optionally, the tobacco extract may further comprise, based on the dry matter mass of the tobacco extract, 0.001-0.05 mg / g caryophyllene;
[0014] And / or, the components of the tobacco extract also include guaiacol;
[0015] Optionally, the mass ratio of cephalothrix trienyl alcohol to guaiacol is (1-5):(0.01-0.2);
[0016] Optionally, the tobacco extract may further comprise 0.01-0.2 mg / g guaiacol, based on the dry matter mass of the tobacco extract.
[0017] Optionally, the tobacco extract may also include spirotropin;
[0018] Optionally, the mass ratio of cephalotrimazole and spirochetone is (1-5):(0.001-0.05);
[0019] Optionally, the tobacco extract may further include 0.02-0.2 mg / g spirotropin, based on the dry matter mass of the tobacco extract.
[0020] Optionally, the phenol content in the tobacco extract is less than 0.0001 mg / g, based on the dry matter mass of the tobacco extract;
[0021] And / or, based on the dry matter mass of the tobacco extract, the hydroxyacetone content in the tobacco extract is less than 0.0001 mg / g;
[0022] And / or, based on the dry matter mass of the tobacco extract, the total mass content of N-nitrosonornicotinine (NNN), N'-nitrosonechoicine (NAT), 4-methylnitrosamine-1-3-pyridyl-1-butanone (NNK) and N-nitrosopseudoesequine (NAB) in the tobacco extract is less than 0.01 mg / g;
[0023] Optionally, the total mass content of N-nitrosonornicotinine (NNN), N'-nitrosonechoicine (NAT), 4-methylnitrosamine-1-3-pyridyl-1-butanone (NNK) and N-nitrosopseudoestiline (NAB) in the tobacco extract is less than 0.005 mg / g, based on the dry matter mass of the tobacco extract.
[0024] Optionally, the components of the tobacco extract, based on the dry matter mass of the tobacco extract, include: 0.01-0.3 mg / g neophytadiene, 0.01-0.2 mg / g dihydroactinidone, 0.01-0.5 mg / g megastigmatrienone, 0.01-1.0 mg / g palmitic acid, 0.01-0.5 mg / g scopolamine, 0.001-0.05 mg / g caryophyllene, 0.01-0.2 mg / g guaiacol, and 0.02-0.2 mg / g spirovellone.
[0025] This application provides a method for preparing the tobacco extract described above, comprising the following steps: pulverizing the tobacco extract raw material and then extracting it by physical methods and first concentrating it to obtain a crude extract; then refining the crude extract by physical methods and second concentrating it to obtain the tobacco extract.
[0026] Optionally, the tobacco extract raw material is pulverized to a mesh size of 20-60.
[0027] Optionally, an adsorption treatment step may be included before the second concentration step;
[0028] Optionally, the adsorption material used in the adsorption treatment includes at least one of zeolite, activated carbon, and diatomaceous earth.
[0029] Optionally, the ratio of the adsorbent material to the total mass of the crude extract is (0.05-0.5):1;
[0030] Optionally, the adsorption treatment time is 0.5-2 hours.
[0031] Optionally, the extraction temperature of the physical method is below 80°C;
[0032] Optionally, the extraction temperature of the physical method is 10-80℃.
[0033] Optionally, the physical extraction method includes at least one of supercritical carbon dioxide extraction and solvent extraction.
[0034] Optionally, the supercritical carbon dioxide extraction method includes supercritical carbon dioxide extraction and separation;
[0035] The entrainer used in the supercritical carbon dioxide extraction step is an aqueous ethanol solution with an ethanol content of 70-95%, the extraction pressure is 20-50 MPa, the extraction temperature is 30-60℃, the extraction time is 2-6 h, and the entrainer flow rate is 70-120 L / h.
[0036] The separation pressure in the supercritical carbon dioxide separation step is 5-30 MPa, the separation temperature is 30-50℃, and the separation time is 2-6 h.
[0037] Optionally, the solvent used in the solvent extraction method includes ethanol or an aqueous solution of ethanol, with a solid-liquid ratio of 1:(5-10), a solvent extraction temperature of 10-80℃, a solvent extraction time of 2-24h, and 1-3 solvent extractions.
[0038] Optionally, the ethanol aqueous solution contains 70-90% ethanol by mass.
[0039] Optionally, the ambient humidity during solvent extraction in the solvent extraction method is 50-70%.
[0040] Optionally, the physical purification method includes at least one of solvent extraction purification, fractionation, distillation, and resin purification;
[0041] Optionally, the solvent used in the solvent extraction and purification is an ethanol-water mixed solvent, the volume ratio of the extraction solvent to the crude extract is (1-10):1, the solvent extraction and purification temperature is -20℃ to 0℃, and the solvent extraction and purification time is 5h-12h.
[0042] Optionally, the mass concentration of ethanol in the ethanol-water mixed solvent is 50-95%.
[0043] Optionally, the fractionation temperature is 60-170℃, the fractionation pressure is 0.01-0.5MPa, the fractionation scraper rotation speed is 200-300r / min, and the fractionation time is 30min-3h;
[0044] Optionally, the fractionation step may further include a step of mixing the crude extract with propylene glycol, wherein the volume ratio of the crude extract to propylene glycol is 1:(2-5).
[0045] Optionally, the distillation temperature is 100-200℃, the distillation pressure is 0.01-0.5MPa, and the distillation time is 30min-3h;
[0046] Optionally, the distillation step may further include a step of mixing the crude extract with propylene glycol, wherein the volume ratio of the crude extract to propylene glycol is 1:(2-5).
[0047] Optionally, the elution solvent used in the resin purification is an ethanol-water system, wherein the ethanol mass concentration in the ethanol-water system is 50-95%.
[0048] And / or, the resin used for resin refining includes at least one of macroporous resin and particle exchange resin;
[0049] Optionally, the macroporous resin is an anionic resin or a cationic resin;
[0050] Optionally, the macroporous resin may include D101 macroporous resin or AB-8 macroporous resin.
[0051] Optionally, the first concentration temperature is 40-100℃, and the first concentration vacuum degree is 60-150mbar;
[0052] And / or, the second concentration temperature is 40-100°C, and the second concentration vacuum degree is 70-100 mbar.
[0053] This application provides an aerosol generation matrix, which includes the tobacco extract described above or the tobacco extract prepared by the preparation method described above.
[0054] Optionally, the mass content of tobacco extract in the aerosol generating matrix is 1-50%.
[0055] Optionally, the aerosol generating matrix further includes an atomizing agent;
[0056] Optionally, the atomizing agent accounts for 50-99% of the total mass of the aerosol generating matrix;
[0057] The atomizing agent is selected from at least one of propylene glycol, glycerol, water, and ethanol.
[0058] Optionally, the aerosol generating matrix may also include nicotine;
[0059] The nicotine accounts for 0.5-3% of the total mass of the aerosol-generating matrix.
[0060] Optionally, the aerosol generating matrix further includes organic acids, which account for 0.5-3% of the total mass of the aerosol generating matrix;
[0061] The organic acid is selected from at least one of acetic acid, lactic acid, benzoic acid, malic acid, tartaric acid, citric acid, and levulinic acid; and / or, the aerosol generating matrix further includes a fragrance, which accounts for 0.5-3% of the total mass of the aerosol generating matrix.
[0062] Optionally, the atomizing agent is propylene glycol and glycerol;
[0063] The mass ratio of propylene glycol to glycerol is (3-7):(3-7).
[0064] This application provides the use of the tobacco extract described above or the tobacco extract prepared by the preparation method described above or the aerosol generating matrix described above in atomizing devices and / or heated non-combustible tobacco.
[0065] This application provides an electronic atomizing device, which includes the tobacco extract described above, the tobacco extract prepared by the preparation method described above, or the aerosol generating matrix described above.
[0066] This application provides a heated tobacco product, which includes the tobacco extract described above or the tobacco extract prepared by the preparation method described above or the aerosol generating matrix described above.
[0067] The beneficial effects of this application are:
[0068] The tobacco extract provided in this application comprises: cephalotrimazole, neophytadiene, dihydroactinidone, megalotrienone, palmitic acid, and scopolamine; the mass ratio of cephalotrimazole, neophytadiene, dihydroactinidone, megalotrienone, palmitic acid, and scopolamine is (1-5):(0.01-0.3):(0.01-0.2):(0.01-0.5):(0.01-1.0):(0.01-0.5). The tobacco extract provided in this application retains the aroma of tobacco to the greatest extent, exhibiting a rich, natural, and harmonious flavor with superior overall sensory appeal. Detailed Implementation
[0069] The following embodiments are provided to better understand this application and are not limited to the preferred embodiments described herein. They do not constitute a limitation on the content and scope of protection of this application. Any product that is the same as or similar to this application, derived by anyone under the guidance of this application or by combining features of this application with other prior art, falls within the scope of protection of this application.
[0070] For experiments not specifically described in the examples, the procedures or conditions should be followed according to the conventional experimental procedures described in the literature in this field. Reagents or instruments whose manufacturers are not specified are all commercially available conventional reagent products.
[0071] This application provides a tobacco extract comprising: cephalotrimazole, neophytadiene, dihydroactinidone, megalotrienone, palmitic acid, and scopolamine; wherein the mass ratio of cephalotrimazole, neophytadiene, dihydroactinidone, megalotrienone, palmitic acid, and scopolamine is (1-5):(0.01-0.3):(0.01-0.2):(0.01-0.5):(0.01-1.0):(0.01-0.5). The tobacco extract provided by this application has the advantage of preserving the aroma of tobacco to the greatest extent, exhibiting a rich, natural, and harmonious aroma with superior overall sensory appeal, and is less prone to carbon buildup.
[0072] The tobacco extract described in this application contains cephalotrindiol (CAS: 57605-80-8), whose main function is to enhance the hay aroma of tobacco and is a core component of tobacco fragrance. The tobacco extract described in this application contains neophytadiene (CAS: 504-96-1), whose main function is to enhance the freshness of tobacco aroma, promote its permeability, increase the duration of the aroma, and make the overall aroma more harmonious. The tobacco extract described in this application contains dihydroactinidiolide (CAS: 17092-92-1), which mainly enhances the freshness and sweetness of tobacco. The tobacco extract described in this application contains megastigmatrienone (CAS: 38818-55-2), which contributes to the hay aroma of tobacco. The tobacco extract described in this application contains n-Hexadecanoic acid (CAS: 57-10-3), which can smooth the smoke and increase its mellowness. The tobacco extract described in this application contains scopolol (CAS: 92-61-5), which can increase the satisfaction and pleasure associated with tobacco.
[0073] In some alternative embodiments, the components of the tobacco extract, based on the dry matter mass of the tobacco extract, include: 1-5 mg / g ceftazidimetrienol, 0.01-0.3 mg / g neophytadiene, 0.01-0.2 mg / g dihydroactinidone, 0.01-0.5 mg / g megastigmatrienone, 0.01-1.0 mg / g palmitic acid, and 0.01-0.5 mg / g scopolamine.
[0074] In some alternative embodiments, the flavor substance further includes at least one of caryophyllene, guaiacol, damasone, and spirovesperidone.
[0075] The tobacco extract described in this application may contain caryophyllene (CAS: 87-44-5), which can increase smoke permeability and enhance the hay aroma and sweetness of tobacco. The tobacco extract described in this application may contain guaiacol (CAS: 88-84-6), which can increase smoke permeability and enhance the hay aroma and sweetness of tobacco. The tobacco extract described in this application may contain spirovetivone (CAS: 54878-25-0), which can enhance the hay aroma of tobacco.
[0076] In some optional embodiments, the tobacco extract further comprises caryophyllene; optionally, the mass ratio of cephalotrindiol to caryophyllene is (1-5):(0.001-0.05); optionally, the tobacco extract further comprises 0.001-0.05 mg / g caryophyllene based on the dry matter mass of the tobacco extract.
[0077] In some optional embodiments, the tobacco extract further comprises guaiacol; optionally, the mass ratio of cepertrienildiol to guaiacol is (1-5):(0.01-0.2); optionally, the tobacco extract further comprises 0.01-0.2 mg / g guaiacol based on the dry matter mass of the tobacco extract.
[0078] In some optional embodiments, the tobacco extract further comprises spirotropin; optionally, the mass ratio of cephalotrindiol to spirotropin is (1-5):(0.001-0.05); optionally, the tobacco extract further comprises 0.02-0.2 mg / g spirotropin based on the dry matter mass of the tobacco extract.
[0079] In some optional embodiments, the phenol content in the tobacco extract is less than 0.0001 mg / g based on the dry matter mass of the tobacco extract; and / or, the hydroxyacetone content in the tobacco extract is less than 0.0001 mg / g based on the dry matter mass of the tobacco extract; and / or, the total mass content of N-nitrosonornicotinine, N'-nitrosoneonicotinine, 4-methylnitrosamine-1-3-pyridyl-1-butanone and N-nitrosopseudoesequine in the tobacco extract is less than 0.01 mg / g based on the dry matter mass of the tobacco extract; optionally, the total mass content of N-nitrosonornicotinine, N'-nitrosoneonicotinine, 4-methylnitrosamine-1-3-pyridyl-1-butanone and N-nitrosopseudoesequine in the tobacco extract is less than 0.005 mg / g based on the dry matter mass of the tobacco extract.
[0080] In some optional embodiments, the tobacco extract further comprises damascone; optionally, the mass ratio of cepertrienol to damascone is (1-5):(0.01-0.1); optionally, the tobacco extract further comprises 0.01-0.1 mg / g damascone based on the dry matter mass of the tobacco extract. The tobacco extract described in this application may contain damascone, which primarily enhances the aroma of tobacco and floral / fruity notes.
[0081] This application provides a method for preparing the tobacco extract described above, comprising the following steps: pulverizing the tobacco extract raw material and then extracting it by physical methods and first concentrating it to obtain a crude extract; then refining the crude extract by physical methods and second concentrating it to obtain the tobacco extract.
[0082] This application uses only physical methods and does not generate any additional harmful substances, making it safer.
[0083] The tobacco extraction raw materials described in this application are not limited and can include tobacco leaves, tobacco stems, tobacco powder, and tobacco and reconstituted tobacco waste, as well as crude tobacco extract or tobacco puree. The type of tobacco used as the tobacco extraction raw material described in this application is also not limited, including but not limited to any one of flue-cured tobacco, Burley tobacco, aromatic tobacco, and cigar tobacco. For example, Burley tobacco leaves can be used as the tobacco extraction raw material.
[0084] In some optional embodiments, the tobacco extract raw material is pulverized to a mesh size of 20-60.
[0085] In some optional embodiments, an adsorption treatment step is included before the second concentration step; optionally, the adsorption treatment uses at least one of zeolite, activated carbon, and diatomaceous earth as the adsorption material; optionally, the ratio of the adsorption material to the total mass of the crude extract is (0.05-0.5):1; optionally, the adsorption treatment time is 0.5-2 hours.
[0086] In some optional embodiments, the extraction temperature of the physical method is below 80°C; alternatively, the extraction temperature of the physical method is 10-80°C.
[0087] In some alternative embodiments, the physical extraction method includes at least one of supercritical carbon dioxide extraction and solvent extraction.
[0088] In some optional embodiments, the supercritical carbon dioxide extraction method includes supercritical carbon dioxide extraction and separation; optionally, the entrainer used in the supercritical carbon dioxide extraction step is an aqueous ethanol solution with an ethanol content of 70-95%, the extraction pressure is 20-50 MPa, the extraction temperature is 30-60℃, the extraction time is 2-6 h, and the entrainer flow rate is 70-120 L / h; optionally, the separation pressure in the supercritical carbon dioxide separation step is 5-30 MPa, the separation temperature is 30-50℃, and the separation time is 2-6 h.
[0089] In some optional embodiments, the solvent used in the solvent extraction method includes ethanol or an aqueous ethanol solution, with a material-to-liquid ratio of 1:(5-10), a solvent extraction temperature of 10-80℃, and a solvent extraction time of 2-24h; the number of solvent extractions is 1-3; optionally, the ethanol aqueous solution has a mass percentage content of 70-90%.
[0090] In some optional embodiments, the physical refining method includes at least one of solvent extraction, fractionation, distillation, and resin refining;
[0091] In some optional embodiments, the solvent extraction and purification uses an ethanol-water mixed solvent, the volume ratio of the extraction solvent to the crude extract is (1-10):1, the solvent extraction and purification temperature is -20℃ to 0℃, and the solvent extraction and purification time is 5h-12h; optionally, the mass concentration of ethanol in the ethanol-water mixed solvent is 50-95%.
[0092] In some optional embodiments, the fractionation temperature is 60-170℃, the fractionation pressure is 0.01-0.5MPa, the fractionation scraper rotation speed is 200-300r / min, and the fractionation time is 30min-3h; optionally, the fractionation step further includes a step of mixing the crude extract with propylene glycol before the fractionation step, wherein the volume ratio of the crude extract to propylene glycol is 1:(2-5).
[0093] In some optional embodiments, the distillation temperature is 100-200℃, the distillation pressure is 0.01-0.5MPa, and the distillation time is 30min-3h; optionally, the distillation step further includes a step of mixing the crude extract with propylene glycol, wherein the volume ratio of the crude extract to propylene glycol is 1:(2-5).
[0094] In some optional embodiments, the elution solvent used for resin purification is an ethanol-water system, wherein the ethanol mass concentration in the ethanol-water system is 50-95%; and / or, the resin used for resin purification includes at least one of macroporous resin and particle exchange resin; optionally, the macroporous resin is an anionic resin or a cationic resin; optionally, the type of macroporous resin includes D101 macroporous resin and AB-8 macroporous resin.
[0095] In some optional embodiments, after the physical extraction step, a first concentration step is further included; optionally, the temperature of the first concentration step is 40-100°C, and the vacuum degree of the first concentration step is 60-150 mbar; optionally, the concentration is increased to 60-85% after the first concentration.
[0096] In some optional embodiments, after the physical purification step, a second concentration step is further included; the temperature of the second concentration step is 40-100°C, and the vacuum degree of the second concentration step is 70-100 mbar; optionally, the concentration is reduced to 40-70% after the second concentration.
[0097] In this application, the concentration in the concentration step refers to the mass percentage of the components other than the solvent in the corresponding mixture, which is detected using an ATAGO handheld concentration meter.
[0098] This application provides an aerosol generation matrix, which includes the tobacco extract described in any one of the above claims or the tobacco extract prepared by the above preparation method;
[0099] In some optional embodiments, the tobacco extract content in the aerosol generating matrix is 1%-50% by mass.
[0100] In some optional embodiments, the aerosol generating matrix further includes an atomizing agent; the atomizing agent in this application is a conventional atomizing agent, including but not limited to at least one selected from propylene glycol, glycerol, water, and ethanol. Optionally, the atomizing agent is propylene glycol and glycerol, and more preferably, the mass ratio of propylene glycol to glycerol is (3-7):(3-7). In some optional embodiments, the mass content of the atomizing agent in the aerosol generating matrix is 50-99%.
[0101] In some alternative embodiments, the aerosol generating matrix further includes at least one of nicotine, organic acid, and fragrance.
[0102] In some alternative embodiments, the nicotine content in the aerosol generating matrix is 0.5-3% by mass.
[0103] In some optional embodiments, the organic acid content in the aerosol generating matrix is 0.5-3% by mass; optionally, the organic acid is selected from at least one of acetic acid, lactic acid, benzoic acid, malic acid, tartaric acid, citric acid, and levulinic acid.
[0104] In some optional embodiments, the flavoring content in the aerosol generating matrix is 0.5-3% by mass. This application does not specifically limit the flavoring; the flavoring type can be food or tobacco, and the source of the flavoring can be purchased externally or prepared in-house. For example, optionally, the flavoring in the aerosol generating matrix can be selected from coffee flavoring (purchased from Hasegawa Biotechnology Co., Ltd.).
[0105] This application provides the use of the tobacco extract described above or the tobacco extract prepared by the preparation method described above or the aerosol generating matrix described above in atomizing devices and / or heated non-combustible tobacco.
[0106] This application provides an electronic atomizing device, which includes the tobacco extract described above, the tobacco extract prepared by the preparation method described above, or the aerosol generating matrix described above.
[0107] This application provides a heated tobacco product, which includes the tobacco extract described above or the tobacco extract prepared by the preparation method described above or the aerosol generating matrix described above.
[0108] The aerosol generating matrix described in this application can be used to add atomizing agents, nicotine, and other flavorings for vaporizing tobacco, and can also be used to heat tobacco to enhance its aroma.
[0109] Furthermore, the aerosol generating matrix of this application can also be used to heat tobacco for flavoring, making the tobacco aroma more intense.
[0110] The present application will be further described in detail below with reference to specific embodiments, which should not be construed as limiting the scope of protection claimed in the present application.
[0111] Example 1
[0112] This embodiment provides a method for preparing a tobacco extract, including the following steps:
[0113] Burley tobacco leaves were pulverized to 30 mesh and then extracted using supercritical carbon dioxide extraction. The entrainer in the supercritical carbon dioxide extraction vessel was a 90% aqueous ethanol solution at a flow rate of 90 L / h. The extraction pressure was 30 MPa, the extraction temperature was 45℃, and the extraction time was 4 h. The separation pressure in the supercritical carbon dioxide extraction vessel was 25 MPa, the separation temperature was 40℃, and the separation time was 4 h. After extraction, the mixture was concentrated to [a specific concentration] at 60℃ and a vacuum of 100 mbar. The crude extract was obtained at a concentration of 80%. The crude extract was mixed with an ethanol aqueous solution with a mass concentration of 90% at a mass ratio of 1:2. The mixture was purified by standing at -20℃ for 5 hours. The solid was then removed by centrifugation at -5℃ and 8000 rpm for 20 minutes. Zeolite of 50% of the total mass of the crude extract was added to the centrifuged liquid. The mixture was allowed to stand for 1 hour and then filtered (600 mesh). The solution was then concentrated to a concentration of 50% at 60℃ and a vacuum of 70 mbar to obtain the tobacco extract.
[0114] Example 2
[0115] This embodiment provides a method for preparing a tobacco extract, including the following steps:
[0116] Burley tobacco leaves were pulverized to 30 mesh and then extracted using supercritical carbon dioxide extraction. The entrainer in the supercritical carbon dioxide extraction vessel was a 90% ethanol aqueous solution, with a flow rate of 90 L / h, an extraction pressure of 30 MPa, an extraction temperature of 45℃, and an extraction time of 4 h. Separation in the supercritical carbon dioxide extraction vessel was carried out at a pressure of 25 MPa, a separation temperature of 40℃, and a separation time of 4 h. After extraction, the extract was concentrated to 80% at 60℃ and a vacuum of 100 mbar to obtain a crude extract. The crude extract was mixed with propylene glycol at a volume ratio of 1:2 and fractionated by molecular distillation for 2 h at a temperature of 100℃, a separation pressure of 0.1 MPa, and a scraper rotation speed of 200 r / min. After fractionation, the light fraction was collected and concentrated to 50% at 60℃ and a vacuum of 100 mbar to obtain the tobacco extract.
[0117] Example 3
[0118] This embodiment provides a method for preparing a tobacco extract, including the following steps:
[0119] Burley tobacco leaves were pulverized to 30 mesh and then extracted using supercritical carbon dioxide extraction. The supercritical carbon dioxide extraction vessel used a 90% ethanol aqueous solution as an entrainer at a flow rate of 90 L / h, an extraction pressure of 30 MPa, an extraction temperature of 45℃, and an extraction time of 4 h. Separation was performed in the supercritical carbon dioxide extraction vessel at a pressure of 25 MPa, a separation temperature of 40℃, and a separation time of 4 h. After extraction, the extract was concentrated to 80% at 60℃ and a vacuum of 100 mbar to obtain a crude extract. The crude extract was then mixed with propylene glycol at a volume ratio of 1:2 and distilled in a distillation column at 200℃ and 0.1 MPa. After distillation, the fraction was collected and concentrated to 50% at 60℃ and a vacuum of 100 mbar to obtain the tobacco extract.
[0120] Example 4
[0121] This embodiment provides a method for preparing a tobacco extract, including the following steps:
[0122] Burley tobacco leaves were pulverized to 10-30 mesh and then extracted using a solvent extraction method. The solvent used in the solvent extraction method was an ethanol-water solution with a mass concentration of 90% (1:10) at an extraction temperature of 10℃, an ambient humidity of 50%, and an extraction time of 24 hours. The extraction was performed once. After extraction, the mixture was filtered (200 mesh) and concentrated to a concentration of 80% under a vacuum of 100 mbar and a temperature of 60℃ to obtain a crude extract. The crude extract was then mixed with propylene glycol at a volume ratio of 1:2 and fractionated for 2 hours at a fractionation temperature of 140℃, a fractionation pressure of 0.5 MPa, and a fractionation scraper speed of 180 r / min. After fractionation, zeolite (50% of the total mass of the purified product) was added to the collected light fraction, and the mixture was allowed to stand for 1 hour. Then, it was filtered (600 mesh) and concentrated to a concentration of 50% under a vacuum of 100 mbar and a temperature of 60℃ to obtain the tobacco extract.
[0123] Example 5
[0124] This embodiment provides a method for preparing a tobacco extract, including the following steps:
[0125] Burley tobacco leaves were pulverized to 10-30 mesh and then extracted using a solvent extraction method. The solvent used in the solvent extraction method was an ethanol-water solution with a mass concentration of 90% ethanol, a material-to-liquid ratio of 1:10, an extraction temperature of 10℃, an ambient humidity of 50% during extraction, an extraction time of 24 hours, and one extraction cycle. After extraction, the mixture was filtered (filter mesh 200 mesh) and concentrated to a concentration of 80% under a vacuum of 100 mbar and 60℃ to obtain a crude extract. The crude extract was mixed with propylene glycol at a volume ratio of 1:2 and then distilled in a distillation column at 140℃ and 0.5 MPa for 2 hours. Zeolite (50% of the total mass of the crude extract) was added to the light fraction obtained from the distillation, and the mixture was allowed to stand for 1 hour. Then, it was filtered (filter mesh 600 mesh) and concentrated to a concentration of 50% under a vacuum of 70 mbar and 60℃ to obtain a tobacco extract.
[0126] Example 6
[0127] This embodiment provides a method for preparing a tobacco extract, including the following steps:
[0128] Burley tobacco leaves were pulverized to 10-30 mesh and then extracted using a solvent extraction method. The solvent used in the solvent extraction method was an 80% ethanol aqueous solution with a material-to-liquid ratio of 1:10. The extraction temperature was 70℃, the ambient humidity was 50%, the extraction time was 2 hours, and the extraction was performed twice. After extraction, the mixture was filtered (200 mesh) and concentrated to a concentration of 70% under a vacuum of 100 mbar at 60℃ to obtain a crude extract. The crude extract was mixed with a 95% ethanol aqueous solution at a mass ratio of 1:2 and allowed to stand at -18℃ for 5 hours to complete the purification process. Then, the mixture was centrifuged at -5℃ and 8000 rpm for 20 minutes to remove solids. Zeolite (50% of the total mass of the crude extract) was added to the centrifuged liquid, and the mixture was allowed to stand for 1 hour. Then, it was filtered (600 mesh) and concentrated to a concentration of 50% under a vacuum of 100 mbar at 60℃ to obtain the tobacco extract.
[0129] Example 7
[0130] This embodiment provides a method for preparing a tobacco extract, including the following steps:
[0131] Burley tobacco leaves were pulverized to 10-30 mesh and then extracted using a solvent extraction method. The solvent used in the solvent extraction method was an ethanol-water solution with a mass concentration of 70% (1:10) at an extraction temperature of 80℃ and an ambient humidity of 70% for 2 hours. The extraction was performed twice. After extraction, the extract was filtered (using a 200-mesh filter) and concentrated to a concentration of 70% under a vacuum of 100 mbar and a temperature of 60℃ to obtain a crude extract. The crude extract was then purified using D101 macroporous resin. The eluent was an ethanol-water solution with a mass concentration of 60% (50% by mass of the crude extract) and zeolite was added to the eluent. The mixture was allowed to stand for 1 hour and then filtered (using a 600-mesh filter). Finally, the extract was concentrated to a concentration of 50% under a vacuum of 100 mbar and a temperature of 60℃ to obtain a tobacco extract.
[0132] Example 8
[0133] This embodiment provides an atomizing formulation, which, by mass parts, includes 1 part of the tobacco extract obtained in Example 1, 49.5 parts of propylene glycol, and 49.5 parts of glycerol.
[0134] Example 9
[0135] This embodiment provides an atomizing formulation, which, by mass parts, includes 20 parts of the tobacco extract obtained in Example 1, 40 parts of propylene glycol, and 40 parts of glycerol.
[0136] Example 10
[0137] This embodiment provides an atomizing formulation, which, by mass parts, includes 10 parts of the tobacco extract obtained in Example 1, 1 part of nicotine, 1 part of lactic acid, 44 parts of propylene glycol, and 44 parts of glycerol.
[0138] Example 11
[0139] This embodiment provides an atomizing formulation, which, by weight, comprises 10 parts of tobacco extract obtained in Example 1, 1 part of nicotine, 1 part of lactic acid, 3 parts of coffee flavoring (purchased from Hasegawa Biotechnology Co., Ltd.), 42.5 parts of propylene glycol, and 42.5 parts of glycerol.
[0140] Comparative Example 1
[0141] This comparative example provides a method for preparing a tobacco extract, comprising the following steps:
[0142] Burley tobacco leaves were pulverized to 30 mesh and then extracted using a solvent extraction method. The solvent used in the solvent extraction method was an 80% ethanol aqueous solution with a material-to-liquid ratio of 1:10. The extraction temperature was 70℃, the ambient humidity was 50%, the extraction time was 2 hours, and the extraction was performed twice. After extraction, the mixture was filtered (filter mesh size 200 mesh) and concentrated to a concentration of 50% under conditions of 60℃ and a vacuum degree of 100 mbar to obtain the tobacco extract.
[0143] Comparative Example 2
[0144] This comparative example provides a method for preparing a tobacco extract, comprising the following steps:
[0145] Burley tobacco leaves were pulverized to 10-30 mesh and then extracted using supercritical carbon dioxide extraction. The entrainer in the supercritical carbon dioxide extraction vessel was an ethanol-water solution with a mass concentration of 90% ethanol, the flow rate of the entrainer was 90 L / h, the extraction pressure was 30 MPa, the extraction temperature was 45℃, and the extraction time was 4 h. The separation pressure in the supercritical carbon dioxide extraction vessel was 25 MPa, the separation temperature was 40℃, and the separation time was 4 h. After extraction, the mixture was concentrated to a concentration of 50% under conditions of 60℃ and a vacuum degree of 100 mbar to obtain the tobacco extract.
[0146] Comparative Example 3
[0147] This comparative example provides a method for preparing a tobacco extract, comprising the following steps:
[0148] The flue-cured tobacco leaves were pulverized to 10-30 mesh and then extracted using a solvent extraction method. The solvent used in the solvent extraction method was an 80% ethanol aqueous solution with a material-to-liquid ratio of 1:10. The extraction temperature was 70℃, the ambient humidity was 50%, the extraction time was 2 hours, and the extraction was performed twice. After extraction, the mixture was filtered (filter mesh size 200 mesh) and concentrated to a concentration of 70% under a vacuum of 100 mbar and 60℃ to obtain a crude extract. The crude extract was then added to water (the mass ratio of crude extract to water was 10:3) and subjected to dry distillation at 200℃ for 2 hours to further concentrate to a concentration of 50% to obtain the tobacco extract.
[0149] Test Example 1
[0150] The tobacco extracts obtained in Examples 1-7 and Comparative Examples 1-3 were respectively mixed with dichloromethane at a volume ratio of 1:10 for extraction. The extract was concentrated and the dichloromethane was recovered to obtain a concentrate. The concentrate was dissolved in 1 mL of methanol and filtered through a 0.45 μm filter membrane to obtain a pretreated sample for later use.
[0151] Detection method: The pretreated samples were sent to the detection equipment, GC-MS (6590-7890). The injection port temperature was 250℃, the initial temperature was 40℃, and it was held for 2 min; the temperature was increased to 150℃ at 3℃ / min and held for 5 min; the temperature was increased to 300℃ at 5℃ / min and held for 5 min; finally, the temperature was increased to 320℃ at 10℃ / min and held for 10 min. The results were calculated using peak area integration.
[0152] The contents of each component in the tobacco extract dry matter corresponding to the tobacco extracts obtained in Examples 1-7 and Comparative Examples 1-3 are shown in Table 1 and Table 1 Continued.
[0153] Table 1
[0154] Table 1 (continued)
[0155] Test Example 2
[0156] The tobacco extracts of Examples 1-7 and Comparative Examples 1-3 were mixed with propylene glycol and glycerol to form an atomized formulation, wherein the tobacco extract accounted for 10% of the total mass of the atomized formulation, propylene glycol accounted for 45% of the total mass of the atomized formulation, and glycerol accounted for 45% of the total mass of the atomized formulation.
[0157] The aforementioned atomizing formulations and those from Examples 8-11 were respectively loaded into identical e-cigarette cartridges (RELX 5th Generation Phantom Cartridges). Five expert evaluators conducted a blind sensory evaluation using identical e-cigarette devices (RELX 5th Generation Phantom Devices). The vaping operation involved 3 seconds of vaping for each sample, with an evaluation interval of at least 10 minutes between samples. The evaluation was based on the scoring criteria in Table 2, focusing on the intensity of the smoke aroma, natural harmony, smoke-like sensation, and overall sensory evaluation. A positive scoring principle was adopted, with higher scores for better results, ranging from 1 to 10 points. The average scores were statistically analyzed, and the specific results are shown in Table 3.
[0158] The above-mentioned atomizing formulation and the atomizing formulations of Examples 8-11 were respectively loaded into the same type of e-cigarette cartridge (RELX 5th generation cartridge). After 200 puffs with a smoking machine at the same power, the carbon deposit height on the ceramic membrane was measured. The smoking machine's puffing conditions were 3 seconds of puffing, 27 seconds of rest, and each puff volume was 55 mL. The test results are shown in Table 3.
[0159] Table 2
[0160] Table 3
[0161] Obviously, the above embodiments are merely illustrative examples for clear explanation and are not intended to limit the implementation. Those skilled in the art will recognize that other variations or modifications can be made based on the above description. It is neither necessary nor possible to exhaustively list all possible implementations here. However, obvious variations or modifications derived therefrom are still within the scope of protection of this invention.
Claims
1. A tobacco extract, characterized in that, The components of the tobacco extract include: cephalotrimazole, neophytadiene, dihydroactinidone, megastigmatrienone, palmitic acid, and scopolamine. The mass ratio of cephalothrix trienol, neophytadiene, dihydroactinidone, megastigmatrienone, palmitic acid, and scopolamine is (1-5):(0.01-0.3):(0.01-0.2):(0.01-0.5):(0.01-1.0):(0.01-0.5).
2. The tobacco extract according to claim 1, characterized in that, The components of the tobacco extract, based on the dry matter mass of the tobacco extract, include: 1-5 mg / g cephalotrimethylenediol, 0.01-0.3 mg / g neophytadiene, 0.01-0.2 mg / g dihydroactinidone, 0.01-0.5 mg / g megastigmatrienone, 0.01-1.0 mg / g palmitic acid, and 0.01-0.5 mg / g scopolamine.
3. The tobacco extract according to claim 1 or 2, characterized in that, The tobacco extract also includes caryophyllene; Optionally, the mass ratio of cephalotrindiol to caryophyllene is (1-5):(0.001-0.05); Optionally, the tobacco extract may further comprise, based on the dry matter mass of the tobacco extract, 0.001-0.05 mg / g caryophyllene; And / or, the components of the tobacco extract may also include guaiacene; Optionally, the mass ratio of cephalothrix trienyl alcohol to guaiacol is (1-5):(0.01-0.2); Optionally, the tobacco extract may further comprise 0.01-0.2 mg / g guaiacol, based on the dry matter mass of the tobacco extract.
4. The tobacco extract according to any one of claims 1-3, characterized in that, The components of the tobacco extract also include spirotropin; Optionally, the mass ratio of cephalotrimazole and spirochetone is (1-5):(0.001-0.05); Optionally, the tobacco extract may further include 0.02-0.2 mg / g spirotropin, based on the dry matter mass of the tobacco extract.
5. The tobacco extract according to any one of claims 1-4, characterized in that, The phenol content in the tobacco extract is less than 0.0001 mg / g, based on the dry matter mass of the tobacco extract. And / or, based on the dry matter mass of the tobacco extract, the hydroxyacetone content in the tobacco extract is less than 0.0001 mg / g; And / or, based on the dry matter mass of the tobacco extract, the total mass content of N-nitrosonornicotinine, N'-nitrosonecholine, 4-methylnitrosamine-1-3-pyridyl-1-butanone and N-nitrosopseudoestiline in the tobacco extract is less than 0.01 mg / g; Preferably, the total mass content of N-nitrosonornicotinine, N'-nitrosonecholine, 4-methylnitrosamine-1-3-pyridyl-1-butanone and N-nitrosopseudoestiline in the tobacco extract is less than 0.005 mg / g, based on the dry matter mass of the tobacco extract.
6. The tobacco extract according to any one of claims 1-5, characterized in that, The components of the tobacco extract, based on the dry matter mass of the tobacco extract, include: 1-5 mg / g cephalotrimethylenediol, 0.01-0.3 mg / g neophytadiene, 0.01-0.2 mg / g dihydroactinidone, 0.01-0.5 mg / g megastigmatrienone, 0.01-1.0 mg / g palmitic acid, 0.01-0.5 mg / g scopolamine, 0.001-0.05 mg / g caryophyllene, 0.01-0.2 mg / g guaiacolene, and 0.02-0.2 mg / g spirovellone.
7. A method for preparing the tobacco extract according to any one of claims 1-6, characterized in that, Includes the following steps: The tobacco extract raw material is crushed and then extracted and concentrated by physical methods to obtain a crude extract; then the crude extract is refined and concentrated by physical methods to obtain the tobacco extract.
8. The method for preparing the tobacco extract according to claim 7, characterized in that, The second concentration step is preceded by an adsorption treatment step; Optionally, the adsorption material used in the adsorption treatment includes at least one of zeolite, activated carbon, and diatomaceous earth.
9. The method for preparing the tobacco extract according to claim 7 or 8, characterized in that, The extraction temperature of the physical method is below 80℃; Preferably, the extraction temperature of the physical method is 10-80℃.
10. The method for preparing the tobacco extract according to any one of claims 7-9, characterized in that, The physical extraction method includes at least one of supercritical carbon dioxide extraction and solvent extraction.
11. The method for preparing the tobacco extract according to claim 10, characterized in that, The supercritical carbon dioxide extraction method includes supercritical carbon dioxide extraction and separation; The entrainer used in the supercritical carbon dioxide extraction step is an aqueous ethanol solution with an ethanol content of 70-95%, the extraction pressure is 20-50 MPa, the extraction temperature is 30-60℃, the extraction time is 2-6 h, and the entrainer flow rate is 70-120 L / h. The separation pressure in the supercritical carbon dioxide separation step is 5-30 MPa, the separation temperature is 30-50℃, and the separation time is 2-6 h.
12. The method for preparing the tobacco extract according to claim 10, characterized in that, The solvent extraction method uses ethanol or an aqueous ethanol solution as the solvent, with a solid-liquid ratio of 1:(5-10), an extraction temperature of 10-80℃, an extraction time of 2-24 hours, and 1-3 extractions. Optionally, the ethanol aqueous solution contains 70-90% ethanol by mass.
13. The method for preparing the tobacco extract according to any one of claims 7-12, characterized in that, The physical refining method includes at least one of solvent extraction refining, fractionation, distillation, and resin refining.
14. The method for preparing the tobacco extract according to claim 13, characterized in that, The solvent extraction and purification process uses an ethanol-water mixed solvent as the extraction solvent, with a volume ratio of extraction solvent to crude extract of (1-10):
1. The solvent extraction and purification temperature is -20℃ to 0℃, and the solvent extraction and purification time is 5h-12h. Optionally, the mass concentration of ethanol in the ethanol-water mixed solvent is 50-95%.
15. The method for preparing the tobacco extract according to claim 13, characterized in that, The fractionation temperature is 60-170℃, the fractionation pressure is 0.01-0.5MPa, the fractionation scraper speed is 200-300r / min, and the fractionation time is 30min-3h. Optionally, the fractionation step may further include a step of mixing the crude extract with propylene glycol, wherein the volume ratio of the crude extract to propylene glycol is 1:(2-5).
16. The method for preparing the tobacco extract according to claim 13, characterized in that, The distillation temperature is 100-200℃, the distillation pressure is 0.01-0.5MPa, and the distillation time is 30min-3h; Optionally, the distillation step may further include a step of mixing the crude extract with propylene glycol, wherein the volume ratio of the crude extract to propylene glycol is 1:(2-5).
17. The method for preparing the tobacco extract according to claim 13, characterized in that, The elution solvent used in the resin purification is an ethanol-water system, in which the ethanol mass concentration is 50-95%. And / or, the resin used for resin refining includes at least one of macroporous resin and particle exchange resin; Optionally, the macroporous resin is an anionic resin or a cationic resin; Optionally, the macroporous resin may include D101 macroporous resin or AB-8 macroporous resin.
18. The method for preparing the tobacco extract according to any one of claims 7-17, characterized in that, The first concentration temperature is 40-100℃, and the first concentration vacuum degree is 60-150mbar; And / or, the second concentration temperature is 40-100°C, and the second concentration vacuum degree is 70-100 mbar.
19. An aerosol generation matrix, characterized in that, The aerosol generating matrix includes the tobacco extract according to any one of claims 1-6 or the tobacco extract prepared by the preparation method according to any one of claims 7-18.
20. The aerosol generation matrix according to claim 19, characterized in that, The mass content of tobacco extract in the aerosol generating matrix is 1-50%.
21. The aerosol generating matrix according to claim 19 or 20, characterized in that, The aerosol generating matrix also includes an atomizing agent; Optionally, the atomizing agent accounts for 50-99% of the total mass of the aerosol generating matrix; The atomizing agent is selected from at least one of propylene glycol, glycerol, water, and ethanol.
22. The aerosol generating matrix according to any one of claims 19-21, characterized in that, The aerosol generating matrix also includes nicotine; The nicotine accounts for 0.5-3% of the total mass of the aerosol-generating matrix.
23. The aerosol generating matrix according to any one of claims 19-22, characterized in that, The aerosol generating matrix also includes organic acids, which account for 0.5-3% of the total mass of the aerosol generating matrix; The organic acid is selected from at least one of acetic acid, lactic acid, benzoic acid, malic acid, tartaric acid, citric acid, and levulinic acid; and / or, the aerosol generating matrix further includes a fragrance, which accounts for 0.5-3% of the total mass of the aerosol generating matrix.
24. The aerosol generating matrix according to any one of claims 19-23, characterized in that, The atomizing agent is propylene glycol and glycerol; The mass ratio of propylene glycol to glycerol is (3-7):(3-7).
25. An electronic atomizing device, characterized in that, The electronic atomizing device includes the tobacco extract according to any one of claims 1-6, or the tobacco extract prepared by the preparation method according to any one of claims 7-18, or the aerosol generating matrix according to any one of claims 19-24.
26. A heated non-combustible cigarette, characterized in that, The heated non-combustible cigarette includes the tobacco extract according to any one of claims 1-6, or the tobacco extract prepared by the preparation method according to any one of claims 7-18, or the aerosol generating matrix according to any one of claims 19-24.