Tobacco extract composition, preparation method therefor, and use thereof

Abstract

A tobacco extract composition, a preparation method therefor, and a use thereof, relating to the technical field of electronic atomization. The tobacco extract composition comprises dihydroactinidiolide, geranyllinalool, maltol, neophytadiene, megastigmatrienone, a cembratriene-diol, guaiacol, and furanone. By weight: dihydroactinidiolide / (geranyllinalool+ maltol)≥0.1. By dry weight: the geranyllinalool content ≥0.01 mg / g; and the maltol content is 0.005–0.05 mg / g. The disclosed extract has a tobacco-like feel, with a strong sweet and natural taste, and provides a pleasant tobacco-like experience. The preparation method therefor comprises: extracting twice at a low temperature to obtain tobacco flavor compounds, extracting twice at a high temperature to obtain smoke flavor compounds, and mixing the tobacco flavor compounds and the smoke flavor compounds in a certain ratio to obtain a tobacco extract composition.

Description

A tobacco extract composition, its preparation method and application

[0001] Cross-references to related applications

[0002] This application claims priority to Chinese Patent Application No. 202411994504X, filed on December 30, 2024, entitled "A Tobacco Extract Composition and Its Preparation Method and Application", the entire contents of which are incorporated herein by reference. Technical Field

[0003] This application belongs to the field of electronic atomization technology, specifically relating to a tobacco extract composition, its preparation method, and its application. Background Technology

[0004] Electronic atomizing devices are electronic products that mimic cigarettes. When people inhale electronic atomizing devices, they inhale an electronic atomizing liquid. Compared to traditional cigarettes, electronic atomizing devices do not require combustion and do not produce harmful substances such as combustion byproducts, meaning they have a lower content of harmful substances compared to traditional cigarettes. However, existing electronic atomizing devices often lack appeal to long-time smokers due to insufficient aroma and poor "smoke-like" experience. Improving the "smoke-like" experience and thus increasing the acceptance of electronic atomizing devices by long-time smokers is a pressing issue that needs to be addressed. Summary of the Invention

[0005] Therefore, the technical problem to be solved by this application is to overcome the defects of insufficient tobacco aroma and poor real tobacco sensation in the prior art of electronic atomization devices, thereby providing a tobacco extract composition, its preparation method and application.

[0006] Therefore, this application provides the following technical solution.

[0007] This application provides a tobacco extract composition comprising dihydroactinol, geranyl linalool, maltol, neophytadiene, megalotrienone, cephalotrimazole, guaiacol, and furanone; by weight: dihydroactinol / (geranyl linalool + maltol) ≥ 0.1; by dry weight of the tobacco extract composition: geranyl linalool content ≥ 0.01 mg / g; maltol content 0.005–0.05 mg / g.

[0008] Optionally, by weight: the range of dihydroactinol / (geranyl linalool + maltol) is 0.1 to 10.

[0009] Optionally, the tobacco extract composition further includes at least one of nicotine, 6-ethyl-5,6-dihydro-2H-pyran-2-one, palmitic acid, scopolamine, spirovehorn, 2-methylbutyric acid, methylcyclopentenolone, and furfuryl alcohol.

[0010] In this application, "dry matter" refers to the components in the tobacco extract composition other than the solvent. The solvent may be an aqueous ethanol solution. The dry matter includes: dihydroactinol, geranyl linalool, maltol, neophytadiene, megalotrienone, cephalothrix trienol, guaiacol, furanone, and may also include: nicotine, 6-ethyl-5,6-dihydro-2H-pyran-2-one, palmitic acid, scopolamine, spirochetone, 2-methylbutyric acid, methylcyclopentenolone, and furfuryl alcohol.

[0011] Optionally, the tobacco extract composition satisfies at least one of the following conditions, with each content calculated based on the dry matter content of the tobacco extract composition:

[0012] (1) The content of cipertrienol is ≥0.5mg / g; optionally, the content of cipertrienol is 0.5~5mg / g;

[0013] (2) The content of 6-ethyl-5,6-dihydro-2H-pyran-2-one is ≥0.01 mg / g; optionally, the content of 6-ethyl-5,6-dihydro-2H-pyran-2-one is 0.01~0.3 mg / g;

[0014] (3) The content of megastigmatrienone is ≥0.1 mg / g; optionally, the content of megastigmatrienone is 0.1 to 0.6 mg / g;

[0015] (4) Palmitic acid content ≥ 0.08 mg / g; optionally, palmitic acid content is 0.08–0.8 mg / g;

[0016] (5) Scopolamine content ≥ 0.05 mg / g; optionally, scopolamine content is 0.05–0.35 mg / g;

[0017] (6) Neophytadiene content ≥ 0.015 mg / g; optionally, neophytadiene content is 0.015–0.16 mg / g;

[0018] (7) The content of dihydroactinol is ≥0.01mg / g; optionally, the content of dihydroactinol is 0.01~0.15mg / g;

[0019] (8) The content of geranylide linalool is 0.01-0.24 mg / g;

[0020] (9) Spirophyrin content ≥ 0.005 mg / g; optionally, spirophyrin content is 0.005~0.05 mg / g;

[0021] (10) The content of 2-methylbutyric acid is 0.005~0.025mg / g;

[0022] (11) The furanone content is 0.002 to 0.08 mg / g; optionally, the furanone includes at least one of 2(H) furanone and 5(H) furanone;

[0023] (12) The content of methylcyclopentenolone is 0.0015~0.025mg / g;

[0024] (13) The furfuryl alcohol content is 0.01–0.1 mg / g;

[0025] (14) The guaiacol content is 0.001~0.015mg / g;

[0026] (15) Nicotine content ≥ 5.5 mg / g; optionally, nicotine content is 5.5 to 20 mg / g.

[0027] Optionally, the tobacco extract composition further satisfies at least one of the following conditions, with each content calculated based on the dry matter content of the tobacco extract composition:

[0028] A. Phenol content < 0.015 mg / g; optionally, phenol content < 0.010 mg / g;

[0029] B. Hydroxyacetone content ≤ 0.02 mg / g; optionally, hydroxyacetone content < 0.01 mg / g;

[0030] C. Total nitrosamines < 0.1 mg / g; optionally, nitrosamines include N'-nitrosonornicotinine, 4-(N-methylnitroso)-1-(3-pyridyl)-1-butanone, N′-nitrosopseudoestiline, and N'-nitrosoneonicotinine; further optionally, total nitrosamines < 0.05 mg / g.

[0031] The functions of each component in the tobacco extract composition provided in this application are as follows:

[0032] The presence of nicotine brings greater satisfaction.

[0033] Cembratriene-diols (CAS: 57605-80-8) can enhance the aroma of tobacco and release aroma-producing substances such as solanone and solanesol when heated.

[0034] 6-Ethyl-5,6-dihydro-2H-pyran-2-one (CAS: 19895-35-3) is an important flavor intermediate. When heated above 200°C, it can release furanone, maltol, and other components that bring out the roasted sweetness.

[0035] Megastigmatrienone (CAS: 38818-55-2) can impart a tobacco hay aroma.

[0036] Palmitic acid (n-Hexadecanoic acid / CAS: 57-10-3) can smooth out smoke and increase its mellowness.

[0037] Scopolone (CAS: 92-61-5) can increase tobacco satisfaction and pleasure.

[0038] The main function of neophytadiene (CAS: 504-96-1) is to enhance the aroma of tobacco, promote its permeability, increase the duration of the tobacco aroma, and make the overall aroma more harmonious.

[0039] Dihydroactinidiolide (CAS: 17092-92-1) primarily enhances the aroma and sweetness of tobacco.

[0040] Geraniol (CAS: 1113-21-9) primarily enhances the aroma of tobacco.

[0041] Solavetivone (CAS: 54878-25-0) can enhance the aroma of tobacco hay.

[0042] 2-Methylbutyric acid (2-methyl- / CAS: 116-53-0) can increase smoke permeability and reduce the irritation of smoke.

[0043] Maltol (CAS: 118-71-8) primarily enhances the caramelized sweetness.

[0044] Furanol (2(H)+5(H)) (Furanol / CAS: 3658-77-3&497-23-4) is mainly produced through high temperature and is the main source of the sweetness and caramelization of tobacco.

[0045] Methylcyclopentenolone (CAS: 80-71-7) primarily enhances the caramel sweetness.

[0046] Methylenecyclopropanecarboxylic acid (CAS: 98-00-0) can impart a tobacco roasted aroma and fresh fragrance, but it is easily converted into furfural by heating.

[0047] Guaiacol (CAS: 90-05-1) can enhance the smoky flavor and improve the authentic smoking experience.

[0048] This application provides a method for preparing the above-mentioned tobacco extract composition, comprising the following steps:

[0049] S1: The tobacco raw material is extracted for the first time at 25-60°C to obtain a primary extract. The primary extract is then subjected to a second extraction to obtain tobacco flavor compounds. Optionally, the extraction medium used in the first extraction includes supercritical carbon dioxide.

[0050] S2: Extract tobacco raw materials for the first time at 60-90℃ to obtain a primary extract. Extract the primary extract for the second time at 100-200℃ to obtain a secondary extract. Treat the secondary extract with a porous adsorption material to obtain tobacco flavor compounds.

[0051] S3: Mix the tobacco flavoring agent and the smoke flavoring agent at a mass ratio of 10:1 to 1:10 to obtain the tobacco extract composition.

[0052] Optionally, in step S1, when supercritical carbon dioxide is used as the extraction medium for the first extraction, the extraction pressure is 20–40 MPa, the separation pressure is 5–20 MPa, the extraction temperature is 30–60°C, the separation temperature is 20–40°C, the extraction time is 4–6 h, the carbon dioxide extraction flow rate is 70–100 L / h, and the entrainer includes an ethanol aqueous solution with a concentration ≥80 wt%. Optionally, the mass ratio of the tobacco raw material to the entrainer is 1:3–6.

[0053] Optionally, in step S1, the temperature of the second extraction is -20 to 5°C, the time is 5 to 24 hours, and the mass ratio of the first extract to the extraction medium in the second extraction is 1:2 to 15.

[0054] Optionally, in step S2, the first extraction takes 1.5 to 4 hours, the mass ratio of tobacco raw material to the extraction medium used in the first extraction is 1:8 to 12, and the extraction is performed 1 to 2 times.

[0055] Optionally, in S2, the second extraction method includes any one of microwave dynamic temperature field extraction, thermal reaction extraction, and dry distillation extraction.

[0056] Optionally, in step S2, the extraction medium used for the second extraction has a mass of 30% to 50% of the mass of the first extract, and the extraction time for the second extraction is 2 to 5 hours.

[0057] Optionally, in step S2, the mass of the porous adsorbent material is 1.5% to 15% of the secondary extract, and the time for treating the secondary extract with the porous adsorbent material is 2 to 6 hours.

[0058] Optionally, in step S1, the extraction medium used for the second extraction includes ethanol, and also includes at least one of water and propylene glycol; optionally, the mass concentration of ethanol in the extraction medium used for the second extraction is 50% to 90%.

[0059] Optionally, in step S2, the extraction medium used for the first extraction includes an ethanol solution.

[0060] Optionally, in step S2, the extraction medium used for the second extraction includes at least one of water, ethanol, propylene glycol, and glycerol.

[0061] Optionally, the tobacco raw material includes at least one of tobacco leaves, tobacco stems, tobacco powder, tobacco, tobacco waste, tobacco extract, and tobacco pure oil; optionally, when the tobacco raw material is solid, its size is ≤20 mesh.

[0062] Optionally, the porous adsorbent material includes at least one of activated carbon, zeolite, and diatomaceous earth.

[0063] The method for preparing the tobacco extract composition provided in this application typically, but not limited to, includes, for ease of operation, a step of concentrating the obtained primary extract, tobacco flavor compounds, primary extract, and smoke flavor compounds (hereinafter collectively referred to as the respective mixtures) under reduced pressure after each extraction step. The temperature for reduced pressure concentration is 50–70°C, the vacuum pressure is 60–200 mbar, and the concentration is increased to 50%–90%. The concentration refers to the mass percentage of the components other than the solvent in each respective mixture, and can be detected using a concentration meter. In step S1, the apparatus used for the first extraction includes at least one of a supercritical fluid extraction device, a reflux tank, a percolator, and a stirred extraction tank. In step S2, the first extraction method includes at least one of reflux extraction and percolator extraction.

[0064] In the method for preparing the tobacco extract composition provided in this application, typically and non-limitingly, in step S1, after the second extraction, a solid-liquid separation step is further included to separate the obtained tobacco flavor compounds; the solid-liquid separation method includes centrifugation, with a centrifugation time of 10 to 30 minutes, a temperature of -5 to 5°C, and a rotation speed of 7000 to 9000 r.

[0065] In the method for preparing the tobacco extract composition provided in this application, typically and non-limitingly, before treating the secondary extract with a porous adsorbent material in step S2, a step of removing impurities may also be included. The step of removing impurities includes: adding 2 to 4 times its mass of an aqueous ethanol solution (85wt% to 95wt%) to the secondary extract, sonicating for 10 to 20 minutes to disperse it evenly, storing it at -25 to 0°C for 8 to 16 hours, centrifuging for 10 to 20 minutes at centrifugation parameters of -5 to 5°C and 7000 to 9000 rpm, and taking the supernatant obtained by centrifugation for subsequent steps.

[0066] In the preparation method of the tobacco extract composition provided in this application, the tobacco raw materials used are not particularly limited, such as burley tobacco, cigar tobacco, aromatic tobacco, etc.

[0067] This application provides an aerosol generating matrix, comprising a tobacco extract composition, and further comprising at least one of organic acid, flavoring, and atomizing agent; wherein the tobacco extract composition is the above-mentioned tobacco extract composition or a tobacco extract composition prepared by the above-mentioned preparation method.

[0068] Optionally, at least one of the following conditions must also be met:

[0069] 1) The mass of the tobacco extract composition is 1% to 50% of the total aerosol-generating matrix;

[0070] 2) The mass of the atomizing agent is 50% to 99% of the total aerosol generating matrix mass; optionally, the atomizing agent includes at least one of propylene glycol, glycerol, water, and ethanol; ready-made PGVG can be used, wherein the mass ratio of propylene glycol to vegetable glycerol (i.e., glycerol) in the PGVG is 3:7 to 7:3.

[0071] 3) The organic acid accounts for 0-3% of the total aerosol-generating matrix; optionally, the organic acid includes at least one of acetic acid, lactic acid, benzoic acid, malic acid, tartaric acid, citric acid, and levulinic acid.

[0072] 4) The flavoring is 0-3% of the total aerosol-generating matrix; typically, but not limited to, the flavoring type can be food flavoring or tobacco flavoring, which can be purchased directly or made at home.

[0073] 5) The aerosol generating matrix includes additional nicotine, and the content of the additional nicotine is 0 to 3% of the total mass of the aerosol generating matrix.

[0074] This application also provides the use of the above-described tobacco extract composition or the tobacco extract composition prepared by the above-described preparation method or the above-described aerosol generating matrix in an atomizing device.

[0075] The beneficial effects of this application are:

[0076] The tobacco extract composition provided in this application includes dihydroactinol, geranylacetol, maltol, neophytadiene, megastigmatrienone, cephalotrimethylenediol, guaiacol, and furanone; by weight: dihydroactinol / (geranylacetol + maltol) ≥ 0.1; by dry weight of the tobacco extract composition: geranylacetol content ≥ 0.01 mg / g; maltol content 0.005–0.05 mg / g. This tobacco extract composition has a tobacco-like sensation, a strong sweet and natural taste, and a pleasant tobacco experience. Dihydroactinol imparts a natural, sweet tobacco flavor, while maltol and geranylide bring a roasted sweetness and a tobacco-like sensation. Meanwhile, the presence of neophytadiene, megalotrienone, cephalotrimethylenediol, guaiacol, and furanone further enhances the authentic tobacco flavor of the tobacco extract composition. By weight, the ratio of dihydroactinol / (geranylide + maltol) > 0.01, ensuring that the tobacco extract composition, while possessing a certain tobacco-like flavor, is primarily characterized by a sweet and natural taste.

[0077] This application provides a method for preparing the above-mentioned tobacco extract composition, comprising the following steps: S1: Extracting tobacco raw material for the first time at 25-60°C to obtain a primary extract, and then performing a second extraction on the primary extract to obtain tobacco flavor compounds; S2: Extracting tobacco raw material for the first time at 60-90°C to obtain a primary extract, and then performing a second extraction on the primary extract at 100-200°C to obtain a secondary extract, and treating the secondary extract with a porous adsorption material to obtain a smoke flavor compound; S3: Mixing the tobacco flavor compound and the smoke flavor compound at a mass ratio of 10:1 to 1:10 to obtain the tobacco extract composition. The tobacco extract composition prepared by this method has a high content of characteristic tobacco flavor substances and contains certain smoke flavor substances to enhance the authentic tobacco flavor, while having a low content of harmful substances. Detailed Implementation

[0078] 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.

[0079] 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.

[0080] The tobacco used in the embodiments and comparative examples of this application is Burley tobacco.

[0081] In this application, concentration refers to the mass percentage of the components other than the solvent in the corresponding mixture, which is detected using an ATAGO concentration meter.

[0082] Example 1

[0083] This embodiment provides a tobacco extract composition and its preparation method, including the following steps:

[0084] (1) Preparation of tobacco flavorings: The tobacco leaves were pulverized to 20 mesh and then extracted using supercritical carbon dioxide. The specific extraction conditions were: extraction temperature 45℃, extraction pressure 30MPa, carbon dioxide flow rate 90L / h, separation temperature 35℃, separation pressure 10MPa, entrainer 80wt% ethanol, mass ratio of tobacco leaves to entrainer 1:4, and extraction time 5h. The obtained primary extract was concentrated to a concentration of 80% under reduced pressure at 60℃ and 100mbar. Three times the mass of the extract was added to the concentrate and ultrasonically sonicated for 10min to disperse it evenly. After storage at -18℃ for 12h, the extract was centrifuged for 10min to achieve a second extraction. The centrifugation parameters were -4℃ and 8000r. After centrifugation, the supernatant was separated and concentrated to a concentration of 80% under reduced pressure at 60℃ and 100mbar, which is the tobacco flavoring.

[0085] (2) Preparation of tobacco flavor compounds: Tobacco leaves were pulverized to 20 mesh and extracted with 80 wt% ethanol at 80℃ under reflux for 2 h. The mass ratio of tobacco leaves to 80 wt% ethanol was 1:10, and the extraction was performed twice. The extracts were combined to obtain the primary extract, which was concentrated to 60% concentration under reduced pressure at 60℃ and 100 mbar to obtain the concentrate. 10% PG (propylene glycol) and 30% water by mass were added to the concentrate, and the mixture was placed in a stainless steel hot reactor and reacted naturally at 100℃ for 3 h to obtain the secondary extract. After cooling, 90 wt% ethanol (3 times the mass of the concentrate) was added to the secondary extract and ultrasonicated for 10 min to disperse it evenly. The mixture was stored at -18℃ for 12 h, then centrifuged for 10 min at -4℃ and 8000 r. After centrifugation, the supernatant was separated, and 2% zeolite by mass was added to the supernatant and allowed to stand for 5 h. After filtering out the zeolite, the mixture was concentrated to 70% concentration under reduced pressure at 60℃ and 100 mbar to obtain the tobacco flavor compounds.

[0086] (3) Combine the tobacco flavoring obtained in (1) with the smoke flavoring obtained in (2) at a mass ratio of 10:1 to obtain a tobacco extract composition.

[0087] Example 2

[0088] This embodiment provides a tobacco extract composition and its preparation method. The only difference from Example 1 is that in step (3), tobacco flavorings and smoke flavorings are combined in a mass ratio of 1:1 to obtain the tobacco extract composition.

[0089] Example 3

[0090] This embodiment provides a tobacco extract composition and its preparation method. The only difference from Example 1 is that in step (3), tobacco flavorings and smoke flavorings are combined at a mass ratio of 1:10 to obtain the tobacco extract composition.

[0091] Example 4

[0092] This embodiment provides a tobacco extract composition and its preparation method. Compared with Example 1, the difference is that step (2) is as follows: Preparation of tobacco flavoring: tobacco leaves are pulverized to 20 mesh and extracted with 80wt% ethanol at 80℃ under reflux for 2 hours. The mass ratio of tobacco leaves to 80wt% ethanol is 1:10, and the extraction is performed twice. The extracts are combined to obtain the primary extract, which is concentrated to a concentration of 60% under reduced pressure at 60℃ and 100mbar to obtain the concentrate. 10% of its mass of PG (propylene glycol) and 30% of its mass of water are added to the concentrate, and the mixture is placed in a microwave dynamic reactor and reacted naturally at 150℃ for 3 hours to obtain the secondary extract. After cooling, 2% of the mass of the secondary extract of zeolite is added and the mixture is allowed to stand for 5 hours. After filtering out the zeolite, the mixture is concentrated to a concentration of 70% under reduced pressure at 60℃ and 100mbar to obtain the tobacco flavoring.

[0093] Example 5

[0094] This embodiment provides a tobacco extract composition and its preparation method. The only difference from Example 4 is that in step (3), tobacco flavorings and smoke flavorings are combined in a mass ratio of 1:1 to obtain the tobacco extract composition.

[0095] Example 6

[0096] This embodiment provides a tobacco extract composition and its preparation method. The only difference from Example 4 is that in step (3), tobacco flavorings and smoke flavorings are combined at a mass ratio of 1:10 to obtain the tobacco extract composition.

[0097] Example 7

[0098] This embodiment provides a tobacco extract composition and its preparation method. Compared with Example 1, the only difference is that step (2) is as follows: Preparation of tobacco flavoring: tobacco leaves are pulverized to 20 mesh and extracted with 80 wt% ethanol at 80°C under reflux for 2 hours. The mass ratio of tobacco leaves to 80 wt% ethanol is 1:10, and the extraction is performed twice. The extracts are combined to obtain the primary extract, which is concentrated to a concentration of 60% under reduced pressure at 60°C and 100 mbar to obtain the concentrate. 10% of its mass of PG (propylene glycol) and 30% of its mass of water are added to the concentrate, and the mixture is placed in a dry distillation furnace reactor and reacted naturally at 200°C for 3 hours to obtain the secondary extract. After cooling, 2% of the mass of zeolite of the secondary extract is added and the mixture is allowed to stand for 5 hours. After filtering out the zeolite, the mixture is concentrated to a concentration of 70% under reduced pressure at 60°C and 100 mbar to obtain the tobacco flavoring.

[0099] Example 8

[0100] This embodiment provides a tobacco extract composition and its preparation method. The only difference from Example 7 is that in step (3), tobacco flavorings and smoke flavorings are combined in a mass ratio of 1:1 to obtain the tobacco extract composition.

[0101] Example 9

[0102] This embodiment provides a tobacco extract composition and its preparation method. The only difference from Example 7 is that in step (3), tobacco flavorings and smoke flavorings are combined at a mass ratio of 1:10 to obtain the tobacco extract composition.

[0103] Example 10

[0104] This embodiment provides an aerosol generating matrix, the preparation method of which includes: taking 50 parts of the tobacco extract composition obtained in Example 5, 30 parts of propylene glycol (PG), and 20 parts of vegetable glycerin (VG), and mixing them to obtain the aerosol generating matrix.

[0105] Example 11

[0106] This embodiment provides an aerosol generating matrix, the preparation method of which includes: taking 10 parts of the tobacco extract composition obtained in Example 5, 45 parts of propylene glycol (PG), and 45 parts of vegetable glycerin (VG), and mixing them to obtain the aerosol generating matrix.

[0107] Example 12

[0108] This embodiment provides an aerosol generating matrix, the preparation method of which includes: taking 1 part of the tobacco extract composition obtained in Example 5, 30 parts of propylene glycol (PG), and 69 parts of vegetable glycerin (VG), and mixing them to obtain the aerosol generating matrix.

[0109] Example 13

[0110] This embodiment provides an aerosol generating matrix, the preparation method of which includes: taking 10 parts of the tobacco extract composition obtained in Example 5, 3 parts of nicotine, 2 parts of benzoic acid, 42.5 parts of propylene glycol (PG), and 42.5 parts of vegetable glycerin (VG), and mixing them to obtain the aerosol generating matrix.

[0111] Example 14

[0112] This embodiment provides an aerosol generating matrix, the preparation method of which includes: taking 10 parts of the tobacco extract composition obtained in Example 5, 1 part of nicotine, 1 part of lactic acid, 3 parts of apple flavoring (purchased from Hasegawa Biotechnology Co., Ltd.), 42.5 parts of propylene glycol (PG), and 42.5 parts of vegetable glycerin (VG), and mixing them to obtain the aerosol generating matrix.

[0113] Example 15

[0114] This embodiment provides an aerosol generating matrix, the preparation method of which includes: taking 10 parts of the tobacco extract composition obtained in Example 5, 1 part of nicotine, 1 part of lactic acid, 44 parts of propylene glycol (PG), and 44 parts of vegetable glycerin (VG), and mixing them to obtain the aerosol generating matrix.

[0115] Example 16

[0116] This embodiment provides a tobacco extract composition and its preparation method, including the following steps:

[0117] (1) Preparation of tobacco flavorings: The tobacco leaves were pulverized to 20 mesh and then extracted using supercritical carbon dioxide. The specific extraction conditions were: extraction temperature 30℃, extraction pressure 30MPa, carbon dioxide flow rate 90L / h, separation temperature 35℃, separation pressure 10MPa, entrainer 85wt% ethanol, mass ratio of tobacco leaves to entrainer 1:3, and extraction time 6h. The obtained primary extract was concentrated to a concentration of 80% under reduced pressure at 60℃ and 100mbar. Twice the mass of the extract was added to the concentrate and ultrasonically sonicated for 10min to disperse it evenly. After storage at -20℃ for 5h, the extract was centrifuged for 10min to achieve a second extraction. The centrifugation parameters were -4℃ and 8000r. After centrifugation, the supernatant was separated and concentrated to a concentration of 80% under reduced pressure at 60℃ and 100mbar, which is the tobacco flavoring.

[0118] (2) Preparation of tobacco flavor compounds: Tobacco leaves were pulverized to 20 mesh and extracted with 80 wt% ethanol at 90℃ under reflux for 1.5 h. The mass ratio of tobacco leaves to 80 wt% ethanol was 1:8, and the extraction was performed twice. The extracts were combined to obtain the primary extract, which was concentrated to 60% concentration under reduced pressure at 60℃ and 100 mbar to obtain the concentrate. 10% PG (propylene glycol) and 20% water by mass were added to the concentrate, and the mixture was placed in a stainless steel hot reactor and reacted naturally at 100℃ for 2 h to obtain the secondary extract. After cooling, 90 wt% ethanol (3 times the mass of the concentrate) was added to the secondary extract and ultrasonicated for 10 min to disperse it evenly. The mixture was stored at -18℃ for 12 h, then centrifuged for 10 min at -4℃ and 8000 r. After centrifugation, the supernatant was separated, and 1.5% activated carbon by mass was added to the supernatant and allowed to stand for 6 h. After filtering out the activated carbon, the mixture was concentrated to 70% concentration under reduced pressure at 60℃ and 100 mbar to obtain the tobacco flavor compounds.

[0119] (3) Combine the tobacco flavoring obtained in (1) with the smoke flavoring obtained in (2) at a mass ratio of 10:1 to obtain a tobacco extract composition.

[0120] Example 17

[0121] This embodiment provides a tobacco extract composition and its preparation method, including the following steps:

[0122] (1) Preparation of tobacco flavorings: The tobacco leaves were pulverized to 20 mesh and then extracted using supercritical carbon dioxide. The specific extraction conditions were: extraction temperature 60℃, extraction pressure 30MPa, carbon dioxide flow rate 90L / h, separation temperature 35℃, separation pressure 10MPa, entrainer 80wt% ethanol, mass ratio of tobacco leaves to entrainer 1:6, and extraction time 4h. The obtained primary extract was concentrated to a concentration of 80% under reduced pressure at 60℃ and 100mbar. 15 times the mass of the extract was added to the concentrate and ultrasonicated for 10min to disperse it evenly. After storage at 5℃ for 24h, it was centrifuged for 10min to achieve a second extraction. The centrifugation parameters were -4℃ and 8000r. After centrifugation, the supernatant was separated and concentrated to a concentration of 80% under reduced pressure at 60℃ and 100mbar, which is the tobacco flavoring.

[0123] (2) Preparation of tobacco flavor compounds: Tobacco leaves were pulverized to 20 mesh and extracted with 80wt% ethanol at 60℃ under reflux for 4 hours. The mass ratio of tobacco leaves to 80wt% ethanol was 1:12, and the extraction was performed twice. The extracts were combined to obtain the primary extract, which was concentrated to 60% concentration under reduced pressure at 60℃ and 100mbar to obtain the concentrate. 15% PG (propylene glycol) and 35% water by mass were added to the concentrate, and the mixture was placed in a stainless steel hot reactor and reacted naturally at 100℃ for 5 hours to obtain the secondary extract. After cooling, 90wt% ethanol (3 times the mass of the concentrate) was added to the secondary extract and ultrasonicated for 10 minutes to disperse it evenly. The mixture was stored at -18℃ for 12 hours and then centrifuged for 10 minutes at -4℃ and 8000r. After centrifugation, the supernatant was separated, and 15% activated carbon by mass was added to the supernatant and allowed to stand for 2 hours. After filtering out the activated carbon, the mixture was concentrated to 70% concentration under reduced pressure at 60℃ and 100mbar to obtain the tobacco flavor compounds.

[0124] (3) Combine the tobacco flavoring obtained in (1) with the smoke flavoring obtained in (2) at a mass ratio of 10:1 to obtain a tobacco extract composition.

[0125] Comparative Example 1

[0126] This comparative example provides a tobacco extract, which differs from Example 4 in that only step (1) of Example 4 is performed, and the resulting tobacco flavor compound is the tobacco extract in this comparative example.

[0127] Comparative Example 2

[0128] This comparative example provides a tobacco extract, which differs from Example 4 in that only step (2) of Example 4 is performed, and the resulting smoke flavor is the tobacco extract in this comparative example.

[0129] Comparative Example 3

[0130] This comparative example provides a tobacco extract composition and its preparation method. Compared with Example 1, the difference is that in step (2), the reaction temperature in the stainless steel hot reactor is 80°C; in step (3), the tobacco flavoring obtained in (1) and the smoke flavoring obtained in (2) are combined in a mass ratio of 1:1.

[0131] Comparative Example 4

[0132] This comparative example provides a tobacco extract composition and its preparation method. Compared with Example 1, the difference is that in step (2), the reaction temperature in the stainless steel hot reactor is 250°C; in step (3), the tobacco flavoring obtained in (1) and the smoke flavoring obtained in (2) are combined in a mass ratio of 1:1.

[0133] Comparative Example 5

[0134] This comparative example provides a tobacco extract composition and its preparation method. Compared with Example 1, the difference is that in step (1), the extraction temperature of tobacco leaves using supercritical carbon dioxide extraction is 20°C; in step (2), the reflux extraction temperature is 40°C, and the reaction temperature in the stainless steel hot reactor is 150°C; in step (3), the tobacco flavoring obtained in (1) and the smoke flavoring obtained in (2) are combined at a mass ratio of 1:1.

[0135] Test Example 1 (Component Content Detection)

[0136] Flavor component analysis was performed on the final products obtained from Examples 1-9, 16, and 17, which were comparative examples.

[0137] Take 1 mL of the final product and add dichloromethane at a volume ratio of 1:10 to extract the product. Concentrate the extract to separate the dichloromethane. Dissolve the residue in 1 mL of anhydrous ethanol and filter it through a 0.45 μm filter membrane for later use.

[0138] Detection procedure: Gas chromatography-mass spectrometry (GC-MS (6590-7890)) was used. 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 relative content of each substance in the corresponding final product, based on dry matter mass, was calculated by peak area integration. The results are shown in Tables 1-3.

[0139] Table 1

[0140] Table 2

[0141] Table 3

[0142] Test Example 2 (Sensory Assessment)

[0143] Sensory evaluations were performed on the final products obtained from the examples and comparative examples.

[0144] The final products obtained in the examples and comparative examples were packaged into the same type of cartridge (T65B-1); if the final product is a tobacco extract composition, the atomizing liquid was first prepared by mass percentage of 10% tobacco extract composition and 90% PGVG (5:5).

[0145] Five expert evaluators conducted a blind sensory evaluation using the same model of electronic atomizer (RELX 5th generation). The vaping operation followed the general sensory evaluation standards for electronic atomizers (3 seconds of vaping per sample, with an interval of at least 10 minutes between samples). Scoring ranged from 1 to 10 points, using a positive scoring principle. The scoring dimensions emphasized the intensity of the tobacco aroma, its naturalness and tobacco-like sensation, as well as a comprehensive sensory evaluation. The intensity of the tobacco aroma primarily focused on a sweet tobacco flavor. Single sensory dimension (x) scoring criteria: 10 points maximum, x ≤ 3 points - weak, 3 < x < 7 points - average, x ≥ 7 points - strong. Overall sensory dimension (y) scoring criteria: 10 points maximum, y ≤ 3 points - poor, 3 < y < 7 points - average, y ≥ 7 points - excellent. The average scores were calculated and presented in Table 4.

[0146] Table 4

[0147] As can be seen from Tables 1-4, compared with the examples, the tobacco extract compositions obtained in the comparative examples do not meet the requirements of this application, by mass: dihydroactinol / (geranyl linalool + maltol) ≥ 0.1, geranyl linalool content ≥ 0.01 mg / g, and maltol content 0.005-0.05 mg / g; resulting in a poor and uncoordinated true tobacco flavor, an indistinct sweet flavor, and ultimately a poor overall sensory experience.

[0148] 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 composition, characterized in that, Including dihydroactinol, geranyl linalool, maltol, neophytadiene, megastigmatrienone, cephalotrimazole, guaiacol, and furanone; By mass: dihydroactinol / (geranyl linalool + maltol) ≥ 0.1; Based on the dry matter weight of the tobacco extract composition, the content of geranylide linalool is ≥0.01 mg / g; the content of maltol is 0.005–0.05 mg / g.

2. The tobacco extract composition according to claim 1, characterized in that, By mass: the range of dihydroactinol / (geranyl linalool + maltol) is 0.1–10; And / or, the tobacco extract composition further includes at least one of nicotine, 6-ethyl-5,6-dihydro-2H-pyran-2-one, palmitic acid, scopolamine lactone, spirotropin, 2-methylbutyric acid, methylcyclopentenolone, and furfuryl alcohol.

3. The tobacco extract composition according to claim 2, characterized in that, The following conditions must be met, and the content of each ingredient is based on the dry matter content of the tobacco extract composition: (1) The content of cipertrienol is ≥0.5mg / g; optionally, the content of cipertrienol is 0.5~5mg / g; (2) The content of 6-ethyl-5,6-dihydro-2H-pyran-2-one is ≥0.01 mg / g; optionally, the content of 6-ethyl-5,6-dihydro-2H-pyran-2-one is 0.01~0.3 mg / g; (3) The content of megastigmatrienone is ≥0.1 mg / g; optionally, the content of megastigmatrienone is 0.1 to 0.6 mg / g; (4) Palmitic acid content ≥ 0.08 mg / g; optionally, palmitic acid content is 0.08–0.8 mg / g; (5) Scopolamine content ≥ 0.05 mg / g; optionally, scopolamine content is 0.05–0.35 mg / g; (6) Neophytadiene content ≥ 0.015 mg / g; optionally, neophytadiene content is 0.015–0.16 mg / g; (7) The content of dihydroactinol is ≥0.01mg / g; optionally, the content of dihydroactinol is 0.01~0.15mg / g; (8) The content of geranylide linalool is 0.01-0.24 mg / g; (9) Spirophyrin content ≥ 0.005 mg / g; optionally, spirophyrin content is 0.005~0.05 mg / g; (10) The content of 2-methylbutyric acid is 0.005~0.025mg / g; (11) The furanone content is 0.002 to 0.08 mg / g; optionally, the furanone includes at least one of 2(H) furanone and 5(H) furanone; (12) The content of methylcyclopentenolone is 0.0015~0.025mg / g; (13) The furfuryl alcohol content is 0.01–0.1 mg / g; (14) The guaiacol content is 0.001~0.015mg / g; (15) Nicotine content ≥ 5.5 mg / g; optionally, nicotine content is 5.5 to 20 mg / g.

4. The tobacco extract composition according to any one of claims 1 to 3, characterized in that, It also meets at least one of the following conditions, with each content calculated based on the dry matter content of the tobacco extract composition: A. Phenol content < 0.015 mg / g; optionally, phenol content < 0.010 mg / g; B. Hydroxyacetone content ≤ 0.02 mg / g; optionally, hydroxyacetone content < 0.01 mg / g; C. Total nitrosamines < 0.1 mg / g; optionally, nitrosamines include N'-nitrosonornicotinine, 4-(N-methylnitroso)-1-(3-pyridyl)-1-butanone, N′-nitrosopseudoestiline, and N'-nitrosoneonicotinine; further optionally, total nitrosamines < 0.05 mg / g.

5. A method for preparing a tobacco extract composition according to any one of claims 1 to 4, characterized in that, Includes the following steps: S1: The tobacco raw material is extracted for the first time at 25-60°C to obtain a primary extract. The primary extract is then subjected to a second extraction to obtain tobacco flavor compounds. Optionally, the extraction medium used in the first extraction includes supercritical carbon dioxide. S2: Extract tobacco raw materials for the first time at 60-90℃ to obtain a primary extract. Extract the primary extract for the second time at 100-200℃ to obtain a secondary extract. Treat the secondary extract with a porous adsorption material to obtain tobacco flavor compounds. S3: Mix the tobacco flavoring agent and the smoke flavoring agent at a mass ratio of 10:1 to 1:10 to obtain the tobacco extract composition.

6. The preparation method according to claim 5, characterized in that, In step S1, when supercritical carbon dioxide is used as the extraction medium for the first extraction, the extraction pressure is 20–40 MPa, the separation pressure is 5–20 MPa, the extraction temperature is 30–60°C, the separation temperature is 20–40°C, the extraction time is 4–6 h, the carbon dioxide extraction flow rate is 70–100 L / h, and the entrainer includes an ethanol-water solution with a concentration ≥80 wt%. Optionally, the mass ratio of the tobacco raw material to the entrainer is 1:3–6. And / or, in S1, the temperature of the second extraction is -20 to 5°C, the time is 5 to 24 hours, and the mass ratio of the first extract to the extraction medium in the second extraction is 1:2 to 15; And / or, in S2, the first extraction time is 1.5 to 4 hours, the mass ratio of tobacco raw material to the extraction medium used in the first extraction is 1:8 to 12, and the number of extractions is 1 to 2. And / or, in S2, the second extraction method includes any one of microwave dynamic temperature field extraction, thermal reaction extraction, and dry distillation extraction; And / or, in S2, the mass of the extraction medium used in the second extraction is 30% to 50% of the mass of the first extract, and the extraction time is 2 to 5 hours; And / or, in S2, the mass of the porous adsorbent material is 1.5% to 15% of the secondary extract, and the time for treating the secondary extract with the porous adsorbent material is 2 to 6 hours.

7. The preparation method according to claim 6, characterized in that, In step S1, the extraction medium used for the second extraction includes ethanol, and also includes at least one of water and propylene glycol; optionally, the mass concentration of ethanol in the extraction medium used for the second extraction is 50% to 90%. And / or, in S2, the extraction medium used for the first extraction includes an ethanol solution; And / or, in S2, the extraction medium used for the second extraction includes at least one of water, ethanol, propylene glycol, and glycerol; And / or, the tobacco raw material includes at least one of tobacco leaves, tobacco stems, tobacco powder, tobacco, tobacco waste, tobacco extract, and tobacco pure oil; optionally, when the tobacco raw material is solid, the size is ≤20 mesh; And / or, the porous adsorbent material includes at least one of activated carbon, zeolite, and diatomaceous earth.

8. An aerosol generation matrix, characterized in that, The composition includes tobacco extract, and also includes at least one of organic acids, flavorings, and atomizing agents; The tobacco extract composition is the tobacco extract composition as described in any one of claims 1 to 4 or the tobacco extract composition prepared by the preparation method as described in any one of claims 5 to 7.

9. The aerosol generation matrix according to claim 8, characterized in that, It also meets at least one of the following conditions: 1) The mass of the tobacco extract composition is 1% to 50% of the total aerosol-generating matrix; 2) The mass of the atomizing agent is 50% to 99% of the total aerosol generating matrix; optionally, the atomizing agent includes at least one of propylene glycol, glycerol, water, and ethanol; 3) The organic acid accounts for 0-3% of the total aerosol-generating matrix; optionally, the organic acid includes at least one of acetic acid, lactic acid, benzoic acid, malic acid, tartaric acid, citric acid, and levulinic acid. 4) The mass of the fragrance is 0-3% of the total mass of the aerosol-generating matrix; 5) The aerosol generating matrix includes additional nicotine, and the content of the additional nicotine is 0 to 3% of the total mass of the aerosol generating matrix.

10. The use of a tobacco extract composition as described in any one of claims 1 to 4, or a tobacco extract composition prepared by any one of claims 5 to 7, or an aerosol generating matrix as described in claim 8 or 9, in an atomizing device.

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