Method for preparing tobacco aroma raw material through heat treatment of extract, product prepared by method and application of tobacco aroma raw material

Abstract

The invention provides a method for preparing a tobacco aroma raw material through heat treatment of an extract and a product and application of the tobacco aroma raw material, and the method comprises the following steps: carrying out heat treatment on the tobacco extract, then extracting with an organic solvent, carrying out solid-liquid separation, and collecting a liquid phase to obtain the tobacco aroma raw material, the pressure intensity of the heat treatment is 0.01 to 6 MPa, the temperature is 50 to 350 DEG C, and the time is 0.1 to 6 hours. According to the method, aroma precursor substances in the tobacco extract are directionally converted into rich aroma components through high-temperature and high-pressure heat treatment under specific conditions, aroma is cured and reproduced, aroma such as sweet aroma, incense and fruit aroma is remarkably enhanced, new aroma which a traditional extract does not have is generated, the quality and value of the aroma are greatly improved, and the method is suitable for industrial production. And a new way is provided for preparing perfume raw materials with different fragrances.

Description

Technical Field

[0001] This invention belongs to the field of tobacco additive preparation technology, specifically relating to a method for preparing tobacco flavoring raw materials by heat treatment of extracts, as well as the products and applications thereof. Background Technology

[0002] The sources of aroma components in tobacco mainly include: (1) primary metabolites: volatile components that are directly synthesized and accumulated during the growth of tobacco leaves, such as terpenes (cephalopanel, β-damasone produced by the degradation of carotene, megastigmatrienone, etc.), aldehydes and alcohols, and some esters; (2) transformation during processing: during the processes of conditioning, fermentation, aging, etc., the macromolecules in tobacco undergo degradation and transformation under the action of enzymes or mild chemical action, such as protein degradation into amino acids, starch degradation into sugars, and sugars and amino acids undergoing preliminary Maillard reactions to generate heterocyclic compounds such as pyrazines and pyrroles; (3) thermal reactions under high temperature combustion or heating: when smoking, tobacco undergoes violent pyrolysis and synthesis reactions at high temperatures, and the Maillard reaction, Streak degradation, caramelization of sugars and other reactions are greatly accelerated, instantly generating a large number of small molecule aroma substances such as furans, ketones, aldehydes and pyrazines, such as furanones and maltol.

[0003] Tobacco extracts are commonly used natural flavorings in cigarettes, primarily enriching aroma components and aroma precursors produced by the first and some second pathways mentioned above. However, the aroma profile of traditional tobacco extracts is greatly constrained by the raw materials and cannot simulate the rich and pleasant mature aroma generated by the third pathway, resulting in limited flavor-enhancing effects and difficulty in improving cigarette quality.

[0004] High-temperature and high-pressure heat treatment technology under closed conditions is an efficient means of organic matter conversion. It can promote hydrolysis, degradation and synthesis reactions. When applied to tobacco extracts with more concentrated components and richer precursors, it can simulate and enhance the thermal reaction of the third pathway in advance at the production end, so as to achieve the targeted reconstruction of aroma. Summary of the Invention

[0005] To address the shortcomings of existing technologies, the present invention aims to provide a method for preparing tobacco aroma raw materials through heat treatment of extracts, as well as the products and applications thereof. The present invention uses a high-temperature and high-pressure process to directionally convert aroma precursors in tobacco extracts into abundant aroma-producing components. The process is simple and efficient, providing a new approach for preparing aroma raw materials with different aromas.

[0006] To achieve this objective, the present invention employs the following technical solution:

[0007] In a first aspect, the present invention provides a method for preparing tobacco flavoring raw materials by heat treatment of an extract, the method comprising:

[0008] The tobacco extract was heat-treated, then extracted with an organic solvent, and the solid-liquid phase was separated and the liquid phase was collected to obtain the tobacco flavoring raw material.

[0009] The heat treatment pressure is 0.01-6 MPa, for example, 0.01 MPa, 0.05 MPa, 0.1 MPa, 0.5 MPa, 1 MPa, 2 MPa, 3 MPa, 4 MPa, 5 MPa, or 6 MPa; the temperature is 50-350℃, for example, 50℃, 100℃, 150℃, 200℃, 250℃, 300℃, or 350℃; the time is 0.1-6 h, for example, 0.1 h, 0.5 h, 1 h, 1.5 h, 2 h, 2.5 h, 3 h, 3.5 h, 4 h, 4.5 h, 5 h, 5.5 h, or 6 h.

[0010] Other specific point values ​​within the range of the above values ​​can be selected, and will not be elaborated on here.

[0011] This invention uses high-temperature and high-pressure heat treatment under specific conditions to directionally transform aroma precursors in tobacco extracts into rich aroma components, thereby maturing and regenerating the aroma. This significantly enhances aromas such as caramel sweetness, smokiness, and fruitiness, producing new aromas not found in traditional extracts. The aroma quality and value are greatly improved, providing a new approach for preparing aroma raw materials with different aromas.

[0012] Preferably, the pressure of the heat treatment is 1-3 MPa, for example, 1 MPa, 1.2 MPa, 1.5 MPa, 1.7 MPa, 2 MPa, 2.3 MPa, 2.5 MPa, 2.8 MPa, or 3 MPa; the temperature is 100-280℃, for example, 100℃, 120℃, 150℃, 170℃, 200℃, 230℃, 250℃, or 280℃; and the time is 0.5-3 h, for example, 0.5 h, 1 h, 1.2 h, 1.5 h, 1.7 h, 2 h, 2.3 h, 2.5 h, 2.8 h, or 3 h.

[0013] Other specific point values ​​within the range of the above values ​​can be selected, and will not be elaborated on here.

[0014] The heat treatment process is preferably performed within the above parameter range, resulting in tobacco flavoring raw materials with better aroma quality.

[0015] Preferably, the heat treatment comprises two stages:

[0016] The pressure of the first stage heat treatment is 1-2 MPa, for example, it can be 1 MPa, 1.1 MPa, 1.2 MPa, 1.3 MPa, 1.4 MPa, 1.5 MPa, 1.6 MPa, 1.7 MPa, 1.8 MPa, 1.9 MPa or 2 MPa, etc.; the temperature is 100-200℃, for example, it can be 100℃, 110℃, 120℃, 130℃, 140℃, 150℃, 160℃, 170℃, 180℃, 190℃ or 200℃, etc.; the time is 0.2-1 h, for example, it can be 0.2 h, 0.3 h, 0.4 h, 0.5 h, 0.6 h, 0.7 h, 0.8 h, 0.9 h or 1 h, etc.

[0017] The pressure of the second-stage heat treatment is 1-3 MPa, for example, 1 MPa, 1.2 MPa, 1.5 MPa, 1.7 MPa, 2 MPa, 2.3 MPa, 2.5 MPa, 2.8 MPa, or 3 MPa; the temperature is 200-280℃, for example, 200℃, 210℃, 220℃, 230℃, 240℃, 250℃, 260℃, 270℃, or 280℃; and the time is 0.3-2 h, for example, 0.3 h, 0.4 h, 0.5 h, 0.6 h, 0.7 h, 0.8 h, 0.9 h, 1 h, 1.5 h, or 2 h.

[0018] Other specific point values ​​within the range of the above values ​​can be selected, and will not be elaborated on here.

[0019] When the heat treatment process is preferably performed within the parameter range of the two stages mentioned above, the resulting tobacco flavoring raw material will be more delicate and sweet.

[0020] Preferably, the heat treatment is carried out in a sealed container.

[0021] Preferably, the heat treatment process also includes the addition of a catalyst.

[0022] The core role of a catalyst is to regulate the reaction pathways, rates, and product distribution of complex components (sugars, amino acids, polyphenols, alkaloids, etc.) in tobacco extracts at high temperatures by altering the pH environment of the reaction system.

[0023] Preferably, the catalyst accounts for 0.1-5 wt% of the dry weight of the tobacco extract, for example, it can be 0.1%, 0.5%, 1%, 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5% or 5 wt%.

[0024] Other specific point values ​​within the range of the above values ​​can be selected, and will not be elaborated on here.

[0025] Preferably, the catalyst comprises an alkaline catalyst and / or an acidic catalyst.

[0026] Preferably, the alkaline catalyst comprises any one or a combination of at least two of sodium hydroxide, sodium carbonate, sodium bicarbonate, disodium hydrogen phosphate, trisodium phosphate, triethanolamine, choline, arginine hydrochloride, or lysine hydrochloride.

[0027] The alkaline catalyst mainly creates an alkaline environment, which greatly accelerates the Maillard reaction and promotes the generation of a large amount of alkylpyrazines, pyrroles, pyridines, etc. The aroma characteristics are mainly roasted, nutty, and popcorn. The resulting product has a strong, rich, and impactful aroma, which is more suitable for aromas that need to highlight roasted characteristics.

[0028] Preferably, the acidic catalyst comprises any one or a combination of at least two of malic acid, tartaric acid, aminosulfonic acid, phosphoric acid, citric acid, lactic acid, formic acid, or acetic acid.

[0029] Acidic catalysts primarily inhibit the initiation step of the Maillard reaction by protonating amino acids / amines, thereby reducing the formation of alkaline substances such as pyrazines, which have strong roasting and nutty properties but may be irritating. They also catalyze the dehydration and cyclization of sugars, which is more conducive to the formation of substances with caramel sweetness and fruity aromas, such as maltol, furanones (e.g., chicorylone), and cyclopentenone. They gently hydrolyze glycosides, releasing bound aromas. They also hydrolyze esters, increasing acidity, which usually results in a more mellow, rich, and sweet aroma with reduced irritation and off-flavors.

[0030] Preferably, the acidic catalyst includes malic acid, tartaric acid, and aminosulfonic acid.

[0031] The acid catalyst is further preferably a combination of malic acid, tartaric acid and aminosulfonic acid. The three have a synergistic effect and better control of the heat treatment reaction, making the tobacco flavor raw material more delicate and sweet.

[0032] Preferably, the mass ratio of malic acid, tartaric acid and aminosulfonic acid is (1-10):(1-10):(1-10).

[0033] The specific point values ​​in the first (1-10) can be 1, 2, 3, 4, 5, 6, 7, 8, 9 or 10, etc.

[0034] The specific point values ​​in the second (1-10) can be 1, 2, 3, 4, 5, 6, 7, 8, 9 or 10, etc.

[0035] The specific point values ​​in the third (1-10) can be 1, 2, 3, 4, 5, 6, 7, 8, 9 or 10, etc.

[0036] Other specific point values ​​within the range of the above values ​​can be selected, and will not be elaborated on here.

[0037] Preferably, the organic solvent includes any one or a combination of at least two of ethanol, ethylene glycol, glycerol, dichloromethane, or chloroform.

[0038] Preferably, the ratio of the organic solvent to the dry weight of the tobacco extract is (5-10) mL:1 g.

[0039] The specific point values ​​in (5-10) can be 5, 5.5, 6, 6.5, 7, 7.5, 8, 8.5, 9, 9.5 or 10, etc.

[0040] Other specific point values ​​within the range of the above values ​​can be selected, and will not be elaborated on here.

[0041] Preferably, the extraction temperature is 25-35℃, for example, 25℃, 26℃, 27℃, 28℃, 29℃, 30℃, 31℃, 32℃, 33℃, 34℃ or 35℃, etc.; the time is 1-5 h, for example, 1 h, 1.5 h, 2 h, 2.5 h, 3 h, 3.5 h, 4 h, 4.5 h or 5 h, etc.

[0042] Other specific point values ​​within the range of the above values ​​can be selected, and will not be elaborated on here.

[0043] Preferably, the solid-liquid separation method is filtration.

[0044] Preferably, the collection of the liquid phase further includes a concentration and / or drying step.

[0045] Preferably, the process of collecting the liquid phase further includes a molecular distillation step.

[0046] By collecting lighter components through molecular distillation, tobacco aroma raw materials with a more concentrated flavor can be obtained.

[0047] Preferably, the preparation method of the tobacco extract includes any one or a combination of at least two of reflux extraction, distillation extraction, ultrasonic extraction or percolation extraction.

[0048] Preferably, the tobacco extract is prepared by a method comprising the following steps:

[0049] The tobacco raw material and extraction reagent are mixed, refluxed for extraction, solid-liquid separation is performed, the liquid phase is collected, and vacuum distillation is carried out to obtain the tobacco extract.

[0050] Preferably, the tobacco raw material includes any one or a combination of at least two of flue-cured tobacco, sun-cured tobacco, Burley tobacco, aromatic tobacco, Maryland tobacco, or cigar tobacco.

[0051] Preferably, the tobacco raw materials include any one or a combination of at least two of tobacco leaves, tobacco stems, tobacco dust, tobacco scraps, or tobacco processing by-products.

[0052] Preferably, the ratio of the amount of tobacco raw material to the extraction reagent is 1 g:(5-10) mL.

[0053] The specific point values ​​in (5-10) can be 5, 5.5, 6, 6.5, 7, 7.5, 8, 8.5, 9, 9.5 or 10, etc.

[0054] Other specific point values ​​within the range of the above values ​​can be selected, and will not be elaborated on here.

[0055] Preferably, the extraction reagent comprises an organic solvent and / or water.

[0056] Preferably, the organic solvent includes any one or a combination of at least two of methanol, ethanol, dichloromethane, chloroform, or acetone.

[0057] Preferably, the reflux extraction temperature is 75-85℃, for example, 75℃, 76℃, 77℃, 78℃, 79℃, 80℃, 81℃, 82℃, 83℃, 84℃ or 85℃, etc.; the time is 2-5 h, for example, 2 h, 2.5 h, 3 h, 3.5 h, 4 h, 4.5 h or 5 h, etc.

[0058] Other specific point values ​​within the range of the above values ​​can be selected, and will not be elaborated on here.

[0059] Preferably, the process of vacuum distillation further includes a water washing step.

[0060] Washing can remove some water-soluble impurities, thereby enriching fat-soluble aroma precursors that are more suitable for thermal conversion.

[0061] Secondly, the present invention provides a tobacco flavoring raw material prepared by the method described in the first aspect.

[0062] Thirdly, the present invention provides the use of tobacco flavoring raw materials as described in the second aspect in the preparation of cigarettes.

[0063] Compared with the prior art, the present invention has the following beneficial effects:

[0064] (1) Using tobacco extract as raw material, the aroma-related components in tobacco were pre-enriched, avoiding interference from a large number of ineffective components such as cellulose and lignin when processing raw tobacco materials.

[0065] (2) By high temperature and high pressure heat treatment under specific conditions, the aroma precursors in tobacco extracts are directionally converted into rich aroma components, and the aroma is matured and recreated, significantly enhancing the aromas such as caramel sweetness, smoky aroma and fruity aroma, producing new aromas that traditional extracts do not possess, greatly improving the aroma quality and value, and providing a new way to prepare aroma raw materials with different aromas.

[0066] (3) By adjusting the heat treatment conditions and the type of catalyst, the depth and direction of reactions such as Maillard reaction and Stryker degradation can be precisely controlled, thereby achieving directional regulation of aroma style.

[0067] (4) Different aroma styles and physical forms (liquid, extract, powder) can be obtained by different post-processing methods (such as direct filtration, solvent extraction, molecular distillation, etc.), which has high application flexibility. Detailed Implementation

[0068] To further illustrate the technical means and effects of the present invention, the following describes the technical solution of the present invention in conjunction with preferred embodiments of the present invention. However, the present invention is not limited to the scope of the embodiments.

[0069] Where specific techniques or conditions are not specified in the examples, they shall be performed in accordance with the techniques or conditions described in the literature in this field, or in accordance with the product instructions. Reagents or instruments whose manufacturers are not specified are all conventional products that can be purchased through legitimate channels.

[0070] Example 1

[0071] This embodiment provides a method for preparing tobacco flavoring raw materials, the method comprising:

[0072] Mix 100 g of flue-cured tobacco dust with 750 mL of 75 vol% ethanol aqueous solution, reflux at 80 °C for 4 h, filter, collect the liquid phase, and remove ethanol by vacuum distillation to obtain a dark brown viscous tobacco extract.

[0073] 10 g of tobacco extract was placed in a sealed reactor, and 0.1 g of malic acid, 0.1 g of tartaric acid, and 0.1 g of sulfamic acid were added. Heat treatment was then performed: first, the pressure was set to 1.5 MPa, and the heat treatment was carried out at 150℃ for 0.6 h; then, the pressure was set to 2 MPa, and the heat treatment was carried out at 240℃ for 1.2 h. After cooling, 75 mL of ethanol was added, and extraction was performed at 30℃ for 3 h. The mixture was filtered, the liquid phase was collected, concentrated, and dried to obtain the tobacco aroma raw material.

[0074] Example 2

[0075] This embodiment provides a method for preparing tobacco flavoring raw materials, the method comprising:

[0076] Mix 100 g of flue-cured tobacco dust with 500 mL of 95 vol% ethanol aqueous solution, reflux at 85 °C for 2 h, filter, collect the liquid phase, and remove ethanol by vacuum distillation to obtain a dark brown viscous tobacco extract.

[0077] 10 g of tobacco extract was placed in a sealed reactor, and 0.2 g of malic acid, 0.2 g of tartaric acid, and 0.1 g of sulfamic acid were added. Heat treatment was then performed: first, the pressure was set to 1 MPa, and the heat treatment was carried out at 100℃ for 1 h; then, the pressure was set to 3 MPa, and the heat treatment was carried out at 260℃ for 0.3 h. After cooling, 100 mL of dichloromethane was added, and extraction was carried out at 35℃ for 1 h. The mixture was filtered, the liquid phase was collected, concentrated, and dried to obtain the tobacco flavoring raw material.

[0078] Example 3

[0079] This embodiment provides a method for preparing tobacco flavoring raw materials, the method comprising:

[0080] Mix 100 g of flue-cured tobacco dust with 1000 mL of 50 vol% ethanol aqueous solution, reflux at 75 °C for 5 h, filter, collect the liquid phase, and remove ethanol by vacuum distillation to obtain a dark brown viscous tobacco extract.

[0081] 10 g of tobacco extract was placed in a sealed reactor, and 0.04 g of malic acid, 0.02 g of tartaric acid, and 0.04 g of sulfamic acid were added. Heat treatment was then performed: first, the pressure was set to 2 MPa, and the temperature was 200℃ for 0.2 h; then, the pressure was set to 1 MPa, and the temperature was 200℃ for 2 h. After cooling, 50 mL of chloroform was added, and extraction was carried out at 25℃ for 5 h. The mixture was filtered, the liquid phase was collected, concentrated, and dried to obtain the tobacco flavoring raw material.

[0082] Example 4

[0083] This embodiment provides a method for preparing tobacco flavoring raw materials. The only difference between this method and Example 1 is that the process of "first setting the pressure to 1.5 MPa and heat-treating at 150°C for 0.6 h; then setting the pressure to 2 MPa and heat-treating at 240°C for 1.2 h" is replaced with "first setting the pressure to 2 MPa and heat-treating at 240°C for 1.2 h; then setting the pressure to 1.5 MPa and heat-treating at 150°C for 0.6 h". All other steps remain unchanged.

[0084] Example 5

[0085] This embodiment provides a method for preparing tobacco flavoring raw materials. The only difference between this method and Example 1 is that the process of "first setting the pressure to 1.5 MPa and heat-treating at 150°C for 0.6 h; then setting the pressure to 2 MPa and heat-treating at 240°C for 1.2 h" is replaced with "setting the pressure to 1.5 MPa and heat-treating at 150°C for 1.8 h". All other steps remain unchanged.

[0086] Example 6

[0087] This embodiment provides a method for preparing tobacco flavoring raw materials. The only difference between this method and Embodiment 1 is that the process of "first setting the pressure to 1.5 MPa and heat-treating at 150°C for 0.6 h; then setting the pressure to 2 MPa and heat-treating at 240°C for 1.2 h" is replaced with "setting the pressure to 2 MPa and heat-treating at 240°C for 1.8 h". All other steps remain unchanged.

[0088] Example 7

[0089] This embodiment provides a method for preparing tobacco flavoring raw materials. The only difference between this method and Example 1 is that the process of "first setting the pressure to 1.5 MPa and heat-treating at 150°C for 0.6 h; then setting the pressure to 2 MPa and heat-treating at 240°C for 1.2 h" is replaced with "setting the pressure to 6 MPa and heat-treating at 250°C for 0.1 h". All other steps remain unchanged.

[0090] Example 8

[0091] This embodiment provides a method for preparing tobacco flavoring raw materials. The only difference between this method and Example 1 is that the process of "first setting the pressure to 1.5 MPa and heat-treating at 150°C for 0.6 h; then setting the pressure to 2 MPa and heat-treating at 240°C for 1.2 h" is replaced with "setting the pressure to 0.01 MPa and heat-treating at 50°C for 6 h". All other steps remain unchanged.

[0092] Example 9

[0093] This embodiment provides a method for preparing tobacco flavoring raw materials, which differs from Example 1 only in that: malic acid is not added, and its reduction is proportionally allocated to tartaric acid and aminosulfonic acid, while the remaining steps remain unchanged.

[0094] Example 10

[0095] This embodiment provides a method for preparing tobacco flavoring raw materials, which differs from Example 1 only in that: tartaric acid is not added, and its reduction is proportionally allocated to malic acid and aminosulfonic acid, while the remaining steps remain unchanged.

[0096] Example 11

[0097] This embodiment provides a method for preparing tobacco flavoring raw materials, which differs from Example 1 only in that: sulfamic acid is not added, and its reduced amount is proportionally allocated to malic acid and tartaric acid, while the remaining steps remain unchanged.

[0098] Example 12

[0099] This embodiment provides a method for preparing tobacco flavoring raw materials, which differs from Example 1 only in that malic acid, tartaric acid and aminosulfonic acid are not added, while the other steps remain unchanged.

[0100] Comparative Example 1

[0101] This comparative example provides a method for preparing tobacco flavoring raw materials. The only difference between this method and Example 1 is that the process of "first setting the pressure to 1.5 MPa and heat-treating at 150°C for 0.6 h; then setting the pressure to 2 MPa and heat-treating at 240°C for 1.2 h" is replaced with "setting the pressure to 8 MPa and heat-treating at 400°C for 0.05 h". All other steps remain unchanged.

[0102] Comparative Example 2

[0103] This comparative example provides a method for preparing tobacco flavoring raw materials. The only difference between this method and Example 1 is that the process of "first setting the pressure to 1.5 MPa and heat-treating at 150°C for 0.6 h; then setting the pressure to 2 MPa and heat-treating at 240°C for 1.2 h" is replaced with "setting the pressure to 0.008 MPa and heat-treating at 40°C for 7 h". All other steps remain unchanged.

[0104] Comparative Example 3

[0105] This comparative example provides a method for preparing tobacco flavoring raw materials, the method comprising:

[0106] Mix 100 g of flue-cured tobacco dust with 750 mL of 75 vol% ethanol aqueous solution, reflux at 80 °C for 4 h, filter, collect the liquid phase, and remove ethanol by vacuum distillation to obtain a dark brown viscous tobacco extract.

[0107] Take 10 g of tobacco extract, add 0.1 g of malic acid, 0.1 g of tartaric acid and 0.1 g of aminosulfonic acid, reflux at 80℃ for 4.8 h, filter, collect the liquid phase, distill under reduced pressure to remove ethanol, and obtain the tobacco flavoring raw material.

[0108] Comparative Example 4

[0109] This comparative example provides a method for preparing tobacco flavoring raw materials, the method comprising:

[0110] 10 g of flue-cured tobacco dust and 75 mL of 75 vol% ethanol aqueous solution were mixed and placed in a sealed reactor. 0.1 g of malic acid, 0.1 g of tartaric acid, and 0.1 g of sulfamic acid were added, and the mixture was subjected to heat treatment: first, the pressure was set at 1.5 MPa and the temperature was 150℃ for 0.6 h; then, the pressure was set at 2 MPa and the temperature was 240℃ for 1.2 h. After cooling, 75 mL of ethanol was added, and the mixture was extracted at 30℃ for 3 h. The mixture was filtered, the liquid phase was collected, concentrated, and dried to obtain the tobacco aroma raw material.

[0111] Test case

[0112] The components of the tobacco extract involved in Example 1, and the tobacco flavoring raw materials prepared in Examples 1-12 and Comparative Examples 1-4 were analyzed using gas chromatography-mass spectrometry (GC-MS). The detection conditions were as follows: Column: DB-5MS (60 m × 1.0 μm × 0.25 mm); Temperature program: initial temperature 60℃, increased to 250℃ at 2℃ / min, then increased to 290℃ at 5℃ / min, held for 20 min; Injection volume: 1 μL; Split ratio: 10:1; Injector temperature: 290℃; Carrier gas: He; Flow rate: 1.5 mL / min; Transfer line temperature: 290℃; Ionization mode: EI; Ion source temperature: 230℃; Ionization energy: 70 eV; Quadrupole temperature: 150℃; Mass spectrometry scan range: 26-1000 amu. Using benzoyl acetate as an internal standard, a semi-quantitative method was used to analyze the content of aroma-causing components and aroma activity values ​​(OAV) corresponding to different aromas, and to calculate the total aroma activity values ​​(OAV) of caramel sweet, milky, bean, sour, nutty, spicy, smoky, floral and fruity aromas.

[0113] As shown in Table 1, Examples 1-3 and Comparative Examples 3-4 demonstrate that the high-temperature and high-pressure heat treatment of tobacco extracts in this invention is fundamentally different from conventional heat extraction of tobacco extracts and raw materials. It enables the maturation and reconstruction of aroma, significantly enhancing aromas such as caramel sweetness, smokiness, and fruitiness, producing new aromas not found in traditional extracts. Comparative Examples 1-2 show that a good aroma enhancement effect is achieved only under heat treatment conditions of 0.01-6 MPa pressure, 50-350℃ temperature, and 0.1-6 h time. Examples 7-8 show that heat treatment conditions of 1-3 MPa pressure, 100-280℃ temperature, and 0.5-3 h time can significantly improve the aroma quality of tobacco flavoring raw materials. Examples 4-6 show that a specific two-stage heat treatment can make the obtained tobacco flavoring raw materials more delicate and sweet. Example 12 shows that the addition of a catalyst can promote the forward reaction of the heat treatment. As can be seen from Examples 9-11, malic acid, tartaric acid and aminosulfonic acid in the acid catalyst have a synergistic effect, which can better control the heat treatment reaction process and make the obtained tobacco flavor raw material more delicate and sweet.

[0114] Table 1

[0115]

[0116] This invention illustrates, through the above embodiments, a method for preparing tobacco flavoring raw materials by heat treatment of extracts, as well as the products and applications thereof. However, this invention is not limited to the above embodiments, meaning that this invention does not necessarily rely on the above embodiments for implementation. Those skilled in the art should understand that any improvements to this invention, equivalent substitutions of the raw materials in the products of this invention, the addition of auxiliary components, and the selection of specific methods, all fall within the protection and disclosure scope of this invention.

[0117] The preferred embodiments of the present invention have been described in detail above. However, the present invention is not limited to the specific details in the above embodiments. Within the scope of the technical concept of the present invention, various simple modifications can be made to the technical solution of the present invention, and these simple modifications all fall within the protection scope of the present invention.

[0118] It should also be noted that the various specific technical features described in the above specific embodiments can be combined in any suitable manner without contradiction. In order to avoid unnecessary repetition, the present invention will not describe the various possible combinations separately.

Claims

1. A method of preparing a tobacco flavoring material by heat-treating an extract, characterized in that, The method comprises: The tobacco extract is subjected to heat treatment, then extracted with an organic solvent, solid-liquid separation, collection of the liquid phase, to obtain the tobacco flavor raw material; The heat treatment has a pressure of 0.01-6 MPa, a temperature of 50-350℃, and a time of 0.1-6 h.

2. The method of claim 1, wherein, The heat treatment has a pressure of 1-3 MPa, a temperature of 100-280℃, and a time of 0.5-3 h.

3. The method according to claim 1 or 2, characterized in that, The heat treatment comprises two stages: The first stage of heat treatment has a pressure of 1-2 MPa, a temperature of 100-200℃, and a time of 0.2-1 h; The second stage of heat treatment has a pressure of 1-3 MPa, a temperature of 200-280℃, and a time of 0.3-2 h.

4. The method according to any one of claims 1-3, characterized in that, The heat treatment further comprises adding a catalyst; Preferably, the catalyst accounts for 0.1-5wt% of the dry weight of the tobacco extract; Preferably, the catalyst comprises a basic catalyst and / or an acidic catalyst; Preferably, the basic catalyst comprises any one or a combination of at least two of sodium hydroxide, sodium carbonate, sodium bicarbonate, disodium hydrogen phosphate, trisodium phosphate, triethanolamine, choline, arginine hydrochloride, or lysine hydrochloride; Preferably, the acidic catalyst comprises any one or a combination of at least two of malic acid, tartaric acid, sulfamic acid, phosphoric acid, citric acid, lactic acid, formic acid, or acetic acid; Preferably, the acidic catalyst comprises malic acid, tartaric acid, and sulfamic acid.

5. The method according to any one of claims 1-4, characterized in that, The organic solvent comprises any one or a combination of at least two of ethanol, ethylene glycol, glycerol, dichloromethane, or chloroform; Preferably, the ratio of the organic solvent to the dry weight of the tobacco extract is (5-10) mL:1 g; Preferably, the extraction has a temperature of 25-35℃ and a time of 1-5 h; Preferably, the solid-liquid separation is filtration; Preferably, the collection of the liquid phase is followed by a step of concentration and / or drying.

6. The method according to any one of claims 1-5, characterized in that, The tobacco extract is prepared by a method comprising:

7. The method according to any one of claims 1 to 6, characterized in that, The tobacco raw material and an extraction reagent are mixed, subjected to reflux extraction, solid-liquid separation, collection of the liquid phase, and reduced-pressure distillation, to obtain the tobacco extract. The tobacco raw material and the extraction reagent are used in a ratio of 1 g:(5-10) mL; 8. The method of claim 7, wherein, Preferably, the extraction reagent comprises an organic solvent and / or water; Preferably, the organic solvent comprises any one or a combination of at least two of methanol, ethanol, dichloromethane, chloroform, or acetone; Preferably, the reflux extraction has a temperature of 75-85℃ and a time of 2-5 h.

9. The tobacco flavor raw material prepared by the method of any one of claims 1-8.

10. Use of the tobacco flavor raw material of claim 9 in the preparation of cigarettes. ​

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