Spicy essence, preparation method thereof, spicy plate and application of spicy plate

Abstract

The invention relates to the technical field of cigarette perfuming, in particular to spicy essence, a preparation method of the spicy essence, spicy plates and application of the spicy plates. The preparation method comprises the following steps: respectively carrying out cryogenic crushing treatment on each component of spices to obtain corresponding spice powder; respectively placing the spice powder of each component in an environment with constant temperature and humidity; mixing the spice powder of each component according to the proportion to obtain spice mixed powder; performing supercritical CO2 extraction on the spice mixed powder to obtain spice essential oil I and raw material residues; performing microwave-assisted extraction on the raw material residues, and standing and layering an extract to obtain spice essential oil II; and merging the spice essential oil I and the spice essential oil II to obtain the spicy essence. The spicy essence prepared by the method disclosed by the invention has the advantages of high yield, good harmony with tobacco flavor and stable quality.

Description

Technical Field

[0001] The present invention relates to the technical field of cigarette flavoring, in particular to a spicy flavor and a preparation method thereof, a spicy flavor block and an application thereof. Background Art

[0002] Tobacco flavors and fragrances impart character to cigarettes, improve draw quality, and enrich the aroma of tobacco. While synthetic flavors are becoming increasingly common and increasingly important in cigarette flavoring, natural flavors, due to their complex composition and rich aroma, still play an important role in the blending of tobacco flavors and fragrances. Furthermore, as people become more aware of their health, more and more tobacco companies are replacing synthetic flavors with natural flavors to mitigate potential health risks.

[0003] The use of spicy flavors in cigarette flavoring can enhance the aroma of tobacco, reduce dryness, eliminate harshness, increase sweetness, improve aftertaste, mask off-flavors, and impart a distinctive aroma to cigarettes, thereby improving their quality and increasing consumer appeal. Spicy flavors are typically blended from a variety of natural spicy ingredients, such as sweet fennel oil, star anise oil, wild carrot oil, cinnamon oil, clove oil, coriander seed oil, celery seed oil, nutmeg oil, and dill seed oil. The preparation of spicy flavors involves the extraction and blending of these natural spicy ingredients. Currently, the preparation of spicy flavors faces the following challenges: First, the extraction of these natural spicy ingredients currently relies on steam distillation or supercritical CO2 extraction, resulting in low extraction yields. Second, the blending process is closely tied to operator experience, resulting in a high reliance on manual expertise. The resulting spicy flavors often exhibit varying quality depending on the operator. Summary of the Invention

[0004] In order to solve or partially solve the problems existing in the related art, the present invention provides a spicy flavor and a preparation method thereof, a spicy plate and an application thereof.

[0005] The present invention provides a method for preparing a spicy flavor, which comprises: Step a), subjecting each component of the spice to cryogenic grinding treatment at a grinding temperature of -20 to -60°C to obtain corresponding spice powder; Step b), placing the spice powder of each component in a constant temperature and humidity environment, and adjusting the humidity of the spice powder to 10-15%; Step c), mixing the spice powders of the various components according to a proportion to obtain a spice mixture powder; Step d), subjecting the spice mixed powder to supercritical CO2 extraction at an extraction pressure of 10-22 MPa, an extraction temperature of 35-45°C, and an extraction time of 1-5 h to obtain spice essential oil I and a raw material residue; Step e), subjecting the raw material residue to microwave-assisted extraction, and allowing the extract to stand and separate to obtain spice essential oil II; Step f), merging spice essential oil I and spice essential oil II to obtain spicy essence.

[0006] Furthermore, the spices include two or more of the following components: Sichuan pepper, cinnamon bark, dill seeds, clove buds, lemongrass, star anise, tangerine peel, cumin, liquorice, coriander seeds, and celery seeds.

[0007] Furthermore, the spice mixture powder comprises, by weight, 1-5 parts of Sichuan peppercorns, 4-10 parts of cinnamon bark, 1-5 parts of dill seeds, 2-12 parts of clove buds, 2-5 parts of lemongrass, 1-4 parts of star anise, 2-8 parts of dried tangerine peel, 1-8 parts of fennel, 1-5 parts of licorice, and 1-2 parts of coriander seeds.

[0008] Furthermore, the particle size of the spice powder is 20-200 meshes. Furthermore, in step d), the supercritical CO2 extraction is specifically performed by first performing static extraction and then performing cyclic extraction; The static extraction pressure is 10-15 MPa, the extraction temperature is 35-45°C, and the extraction time is 1-2 hours; The pressure of the cyclic extraction is 13-22 MPa, the extraction temperature is 35-45° C., and the extraction time is 1-3 hours.

[0009] Furthermore, the step e) is specifically as follows: performing alcohol washing on the raw material residue; The raw material residue after alcohol washing is soaked in alkali solution; the material-liquid ratio of the raw material residue to the alkali solution is 1g:3~7ml, and the soaking time is 0.5~5h; The raw material residue and the alkali solution in which it is soaked are subjected to microwave-assisted extraction at a power of 150-700 W, a time of 30 min-120 min, and a temperature of 50-120° C.

[0010] Furthermore, the alcohol washing adopts edible alcohol with a concentration of 50% to 100%, and the alkali solution is a sodium carbonate solution with a concentration of 5% to 10%.

[0011] The present invention also provides a spicy flavor, which is prepared according to any one of the methods described above.

[0012] The present invention also provides a spicy plate, which comprises, by weight, 1 to 10 parts of spicy essence, 0.1 to 2.5 parts of raspberry ketone, 0.2 to 1 part of neroli oil, 0.1 to 5 parts of plum extract, 2 to 5 parts of cooling agent, 2 to 5 parts of water, 5 to 65 parts of ethanol, and 6.5 to 89.6 parts of propylene glycol.

[0013] The present invention also provides an application of the spicy flavor block in flavoring cigarettes, wherein the cigarettes are heat-not-burn cigarettes, electronic cigarettes, or full-granule cigarettes.

[0014] The spicy flavor and preparation method thereof provided by the present invention may have the following beneficial effects: 1. Cryogenic grinding is used to separate the various spice components. On the one hand, cryogenic grinding reduces the surface mechanical strength of the spice, increases the dispersion of the spice powder, improves the surface wall-breaking rate, and increases the specific surface area. This fully exposes the oil cells, increases the extraction of flavor substances, and improves the oil yield of the spice. On the other hand, compared with mechanical grinding, cryogenic grinding avoids the loss of flavor substances caused by heat generation during mechanical grinding, retaining the original spicy flavor of the spice and improving the flavor richness of the extract. Experiments have shown that cryogenic grinding helps to increase oil yield, preserve the original volatile and heat-sensitive components in the spices, and enrich the spice essence with more effective substances.

[0015] 2. Before extraction, the spice powder should be humidified to adjust its water content within the range of 10% to 15%. The appropriate amount of water will act as an entrainer in the subsequent supercritical CO2 extraction process, enhancing the solubility of CO2 and helping to improve the yield.

[0016] 3. This method involves mixing the spice powders of each component according to a specific ratio before extracting them through supercritical CO2. This method achieves a high degree of blending of flavor components and a high degree of reproducibility of plant aromas. Compared to blended essences, the blended spice essences have a more natural and gentle aroma, and the harmony and compatibility between the flavor ingredients are high. Furthermore, this method avoids batch variations caused by factors such as addition order and stirring intensity during compounding, thereby improving quality consistency.

[0017] 4. Supercritical CO2 extraction uses low-pressure extraction. Experiments have shown that low-pressure extraction can reduce the content of pectin, pigments, polysaccharides, polyenamides, cellulose and other substances in the extract, increase the mass fraction of flavor substances in the extract, make the aroma richer and stronger, coordinate with the aroma of tobacco, and enhance the sensory comfort of cigarette smoking.

[0018] 5. Microwave-assisted extraction is used to perform a secondary extraction on the residue from supercritical CO2 extraction to enrich the spicy flavor components and increase the yield. Furthermore, the residue is first subjected to an alcohol wash to remove substances that affect sensory properties, such as polyenamides and cellulose, thereby reducing their negative impact on the sensory properties of cigarettes. Subsequent alkali soaking further breaks down the cell walls of the spice residue, increasing the oil yield of the raw material.

[0019] In summary, the spicy flavor prepared according to the method of this embodiment has the advantages of high yield, good coordination with tobacco aroma, and stable quality.

[0020] It is to be understood that the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the invention. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] The above and other objects, features and advantages of the present invention will become more apparent through a more detailed description of exemplary embodiments of the present invention with reference to the accompanying drawings, wherein like reference numerals generally represent like components throughout the exemplary embodiments of the present invention.

[0022] Figure 1 It is the GC / MS fingerprint of spicy flavor 1 in the embodiment of the present invention. DETAILED DESCRIPTION

[0023] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0024] The terms used in this invention are for the purpose of describing specific embodiments only and are not intended to limit the invention. The singular forms "a," "the," and "the" used in this invention and the appended claims are also intended to include plural forms unless the context clearly indicates otherwise. It should also be understood that the term "and / or" as used herein refers to and includes any or all possible combinations of one or more of the associated listed items.

[0025] It should be understood that although the terms "first", "second", "third", etc. may be used to describe various information in the present invention, such information should not be limited to these terms. These terms are only used to distinguish information of the same type from each other. For example, without departing from the scope of the present invention, the first information may also be referred to as the second information, and similarly, the second information may also be referred to as the first information. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of such features. In the description of the present invention, "plurality" means two or more, unless otherwise clearly and specifically defined.

[0026] The present invention provides a method for preparing a spicy flavor, which comprises: Step a), subjecting each component of the spice to cryogenic grinding treatment at a grinding temperature of -20 to -60°C to obtain corresponding spice powder; Step b), placing the spice powder of each component in a constant temperature and humidity environment, and adjusting the humidity of the spice powder to 10-15%; Step c), mixing the spice powders of the various components according to a proportion to obtain a spice mixed powder; Step d), subjecting the spice mixed powder to supercritical CO2 extraction at an extraction pressure of 10-22 MPa, an extraction temperature of 35-45°C, and an extraction time of 1-5 h to obtain spice essential oil I and a raw material residue; Step e), subjecting the raw material residue to microwave-assisted extraction, and allowing the extract to stand and separate to obtain spice essential oil II; Step f), merging spice essential oil I and spice essential oil II to obtain spicy essence.

[0027] Step a) involves separately processing the various spice components into powders. Pulverizing the raw materials helps reduce mass transfer resistance during extraction, allowing CO₂ to fully contact the oil cells of the spice raw materials, thereby dissolving the essential oils. Specifically, this step utilizes cryogenic pulverization, which has the following advantages: Firstly, cryogenic pulverization reduces the surface mechanical strength of the spice, increases the dispersion of the spice powder, improves the surface wall breakage rate, and increases the specific surface area, thereby fully exposing the oil cells, increasing the extraction yield of flavor substances and improving the spice oil yield. Secondly, compared to mechanical pulverization, cryogenic pulverization avoids the loss of flavor substances caused by heat generation during mechanical pulverization, preserving the original spicy aroma of the spices and enhancing the flavor richness of the extract. The cryogenic pulverization temperature is preferably between -20°C and -60°C, more preferably between -30°C and -50°C, and most preferably between -30°C and -40°C. The particle size of the spice powder obtained after pulverization is preferably between 20 and 200 mesh, more preferably between 50 and 120 mesh.

[0028] Step b) above involves pre-treating the spice powders of each component. This step aims to control the moisture content of each component within a range of 10% to 15%. The inventors of this application have discovered that, compared to dried materials, materials with a moisture content (i.e., a water content) of 10% to 15% can improve the yield during supercritical CO2 extraction. This is likely because the moisture in the material acts as an entrainer during supercritical CO2 extraction, enhancing CO2 solubility. The spice moisture content is more preferably 11% to 13%, and most preferably 12%. In this step, the constant temperature environment is preferably 20°C to 26°C, and the constant humidity is preferably 55% to 65%.

[0029] Step c) involves mixing the spice powders of each component according to a specific ratio to produce a spice mix. This spice mix serves as the raw material for subsequent extraction. Unlike traditional methods (which extract individual ingredients and then compound the extracts of each component), this method first mixes the spice powders of each component according to a specific ratio before subjecting them to supercritical CO2 extraction. During the extraction process, the volatile components of the different spices interact at the molecular level within the extraction vessel, forming a naturally blended aroma base and achieving better aroma harmony. This also avoids batch variations caused by factors such as addition order and stirring intensity during compounding, thereby improving quality consistency.

[0030] The spices, i.e., the spice mix, preferably include two or more of the following components: Sichuan peppercorns, cinnamon bark, dill seeds, clove buds, lemongrass, star anise, tangerine peel, cumin, liquorice, coriander seeds, and celery seeds. More preferably, the spice mix includes, by weight, 1-5 parts Sichuan peppercorns, 4-10 parts cinnamon bark, 1-5 parts dill seeds, 2-12 parts clove buds, 2-5 parts lemongrass, 1-4 parts star anise, 2-8 parts tangerine peel, 1-8 parts cumin, 1-5 parts liquorice, and 1-2 parts coriander seeds. The most preferred ingredients include: 1-2 parts of Sichuan peppercorns, 4-6 parts of cinnamon bark, 1-2 parts of dill seeds, 6-8 parts of clove buds, 2-3 parts of lemongrass, 1.5-3 parts of star anise, 3-6 parts of dried tangerine peel, 1-3 parts of cumin, 3-4 parts of licorice, and 1-2 parts of coriander seeds.

[0031] The above step d) is the process of performing the first extraction of the spice mixed powder. Supercritical CO2 extraction is used to perform mixed supercritical extraction on the spice raw materials. It is highly efficient and can quickly extract the target product under high pressure conditions, reducing the number of extractions and improving production efficiency. In addition, compared with other extraction methods, the extraction temperature of supercritical CO2 extraction is low, which is conducive to the preservation of active components in the spices and the protection of heat-sensitive components and volatile components. Spices with different components are mixed and then extracted, and the degree of fusion of flavor components is high, and the degree of restoration of plant flavor is high. Compared with the formulated essence, the aroma of the mixed extracted spicy essence is more natural and soft, and the coordination and compatibility between the fragrance raw materials are high. In this step, the extraction pressure is 10-22 MPa, the extraction temperature is 35-45°C, and the extraction time is 1-5 hours. Low-pressure extraction is used in this application, which facilitates the extraction of light components of spices, reduces the content of pectin, pigments, polysaccharides, polyenamides, cellulose, and other substances in the extract, and increases the mass fraction of flavor substances in the extract, making the aroma richer and more intense, coordinating with the tobacco aroma, and improving the sensory comfort of cigarette smoking. At the same time, the presence of moisture in the raw materials improves extraction efficiency and yield.

[0032] In step d), the supercritical CO2 extraction is preferably performed as follows: static extraction is performed first, followed by cyclic extraction; the static extraction pressure is 10-15 MPa, the extraction temperature is 35-45°C, and the extraction time is 1-2 hours; the cyclic extraction pressure is 13-22 MPa, the extraction temperature is 35-45°C, and the extraction time is 1-3 hours. More preferably, the static extraction pressure is 10-13 MPa, the extraction temperature is 42-45°C, and the extraction time is 1-2 hours; the cyclic extraction pressure is 14-15 MPa, the extraction temperature is 42-45°C, and the extraction time is 2 hours. The flow rate of the cyclic extraction is preferably 2.0-2.5 L / min.

[0033] Step d) can obtain spice essential oil I and raw material residue; step e) is a step of performing secondary extraction on the raw material residue, using microwave-assisted extraction to further extract the flavor components in the raw material residue to enrich the components of the spicy flavor.

[0034] The inventors of this application have discovered that while microwave-assisted extraction of raw material residues can increase the types and content of flavor components to a certain extent, it also suffers from issues such as poor taste and extraction yield after the spicy flavoring is added to cigarettes. To alleviate this problem, step e) is preferably: The raw material residue is subjected to alcohol washing; The raw material residue after alcohol washing is soaked in alkali solution; the material-liquid ratio of the raw material residue to the alkali solution is 1g:3~7ml, and the soaking time is 0.5~5h; The raw material residue and the alkali solution soaked therein are subjected to microwave-assisted extraction.

[0035] That is, before the raw material residue is subjected to microwave-assisted extraction, the steps of alcohol washing and alkali solution soaking are first performed. Among them, alcohol washing can remove some substances that affect the sensory effects of the raw material residue, such as polyenamide and cellulose, and reduce the negative impact of these substances on the sensory organs of cigarettes. Alkali solution soaking can further break the cell walls of the spice residue and improve the oil yield of the raw material. Alcohol washing preferably uses edible alcohol with a concentration of 50% to 100%, and the alkali solution is preferably a sodium carbonate solution with a concentration of 5% to 10%. Those skilled in the art will understand that the above concentrations are all mass concentrations. Alkali solution also serves as an extractant. In this embodiment, the material-liquid ratio of the raw material residue to the alkali solution is controlled to be 1g:3~7ml, that is, a very small amount of solvent is used for microwave extraction, which is also called solvent-free microwave extraction. During the extraction process, the heat accumulation inside the spice cells exceeds its transmission capacity, causing the cells to rupture faster and more thoroughly, thereby improving the yield of the raw material residue. Furthermore, the power of microwave-assisted extraction is controlled to be 150-700 W, the time is 30 min-120 min, and the temperature is 50-120 °C to ensure efficient extraction of essential oils while avoiding adverse effects on the quality of plant materials and their essential oils.

[0036] After step e), spice essential oil II can be obtained. Finally, according to step f), spice essential oil I and spice essential oil II are combined to obtain spicy essence.

[0037] Another embodiment of the present invention provides a spicy flavor, prepared according to the method described in the above embodiment. The specific implementation method is the same as that described above and is not further described here. The density of the spicy flavor is preferably 1.2-1.5 g / mL. The spicy flavor preferably includes any one or more of the following ingredients: citronellal, citronellol, geraniol, geranyl acetate, propylphenol, p-anisaldehyde, cinnamaldehyde, anethole, terpineol acetate, eugenol, β-caryophyllene, α-caryophyllene, bornyl acetate, and 1,8-cineole.

[0038] Another embodiment of the present invention provides a spicy flavor block, comprising, by weight, 1-10 parts spicy flavor essence, 0.1-2.5 parts raspberry ketone, 0.2-1 part neroli oil, 0.1-5 parts plum extract, 2-5 parts cooling agent, 2-5 parts water, 5-65 parts ethanol, and 6.5-89.6 parts propylene glycol. Accordingly, an embodiment of the present invention also provides the use of the spicy flavor block in flavoring cigarettes, such as heat-not-burn cigarettes, electronic cigarettes, or full-granule cigarettes.

[0039] This spicy flavor block is suitable for both traditional and heated cigarettes, offering a rich, fresh spicy aroma complemented by a sweet fruity aroma. The rich aroma creates a delicate, rich smoke that harmonizes with the tobacco flavor, providing high oral comfort and a more comprehensive experience for consumers. This spicy flavor block is particularly suitable for heated cigarettes, and the specific operation can be as follows: The spicy and fragrant block is added in an amount of 3-5% and sprayed on roller-pressed reconstituted tobacco leaves to make heated cigarettes.

[0040] The spicy flavor and preparation method thereof provided by the embodiments of the present invention have the following advantages: 1. Cryogenic grinding is used to separate the various spice components. On the one hand, cryogenic grinding reduces the surface mechanical strength of the spice, increases the dispersion of the spice powder, improves the surface wall-breaking rate, and increases the specific surface area. This fully exposes the oil cells, increases the extraction of flavor substances, and improves the oil yield of the spice. On the other hand, compared with mechanical grinding, cryogenic grinding avoids the loss of flavor substances caused by heat generation during mechanical grinding, retaining the original spicy flavor of the spice and improving the flavor richness of the extract. Experiments have shown that cryogenic grinding helps to increase oil yield, preserve the original volatile and heat-sensitive components in the spices, and enrich the spice essence with more effective substances.

[0041] 2. Before extraction, the spice powder should be humidified to adjust its water content within the range of 10% to 15%. The appropriate amount of water will act as an entrainer in the subsequent supercritical CO2 extraction process, enhancing the solubility of CO2 and helping to improve the yield.

[0042] 3. This method involves mixing the spice powders of each component according to a specific ratio before extracting them through supercritical CO2. This method achieves a high degree of blending of flavor components and a high degree of reproducibility of plant aromas. Compared to blended essences, the blended spice essences have a more natural and gentle aroma, and the harmony and compatibility between the flavor ingredients are high. Furthermore, this method avoids batch variations caused by factors such as addition order and stirring intensity during compounding, thereby improving quality consistency.

[0043] 4. Supercritical CO2 extraction uses low-pressure extraction. Experiments have shown that low-pressure extraction can reduce the content of pectin, pigments, polysaccharides, polyenamides, cellulose and other substances in the extract, increase the mass fraction of flavor substances in the extract, make the aroma richer and stronger, coordinate with the aroma of tobacco, and enhance the sensory comfort of cigarette smoking.

[0044] 5. Microwave-assisted extraction is used to perform a secondary extraction on the residue from supercritical CO2 extraction to enrich the spicy flavor components and increase the yield. Furthermore, the residue is first subjected to an alcohol wash to remove substances that affect sensory properties, such as polyenamides and cellulose, thereby reducing their negative impact on the sensory properties of cigarettes. Subsequent alkali soaking further breaks down the cell walls of the spice residue, increasing the oil yield of the raw material.

[0045] In summary, the spicy flavor prepared according to the method of this embodiment has the advantages of high yield, good coordination with tobacco aroma, and stable quality.

[0046] The technical solution of the present invention will be further described below in conjunction with specific embodiments: Example 1 (1) The spice raw materials (peppercorns, cinnamon bark, dill seeds, clove buds, lemongrass, star anise, tangerine peel, cumin, licorice, and coriander seeds) were placed in a low-temperature freezing device, with liquid nitrogen as the freezing source, the crushing temperature was -30°C, the crushing particle size was 120 mesh, and the crushed spice powder was stored in a constant humidity environment with the humidity controlled at 12%; (2) Take 1 part of Sichuan peppercorns, 4 parts of cinnamon bark, 1 part of dill seeds, 6 parts of clove buds, 2 parts of lemongrass, 1.5 parts of star anise, 3 parts of dried tangerine peel, 1 part of cumin, 3 parts of liquorice, and 1 part of coriander seeds, mix them evenly, and the obtained spice mixture is set aside; (3) The spice mixture powder was transferred into a reactor, and CO2 fluid was introduced. Static extraction was carried out at 10 MPa and 42 °C for 1 h. Carbon dioxide was continued to be introduced, and the pressure of the extraction reactor was adjusted to 14 MPa. After 2 h of cyclic extraction at a flow rate of 2.5 L / min, the receiving valve was opened. After the extraction was completed, spice essential oil I and raw material residue were obtained; (4) The raw material residue was washed with 70% edible alcohol, and the solid-liquid ratio (w:v) of the raw material residue and edible alcohol was 1g:5ml; then 5% sodium carbonate solution was sprayed and added, and the solid-liquid ratio (w:v) of the raw material residue and sodium carbonate solution was 1g:3ml. The soaking time was 30 min. The raw material residue and the soaking alkali solution were placed in a microwave extraction device for microwave-assisted solvent-free extraction. The extraction temperature was set to 90℃, the microwave power was 350W, and the extraction time was 45min. After extraction, the mixture was allowed to stand and separate, and the upper layer was taken to obtain spice essential oil II.

[0047] (5) Spice essential oil I and spice essential oil II are combined to obtain spicy essence 1.

[0048] Comparative Example 1 The only difference from Example 1 is that in step (1), the various spice raw materials are pulverized at room temperature, and other experimental conditions are the same, to obtain spicy essence 2.

[0049] Comparative Example 2 The only difference from Example 1 is that the composition of the spice raw materials and the ratio of the spice mixed powder are different. Specifically, in step (1), the spice raw materials include: Sichuan peppercorns, cinnamon bark, clove buds, lemongrass, star anise, tangerine peel, cumin, liquorice, and coriander seeds; in step (2), the ratio of the spice mixed powder is: 6 parts of Sichuan peppercorns, 2 parts of cinnamon bark, 1 part of clove buds, 8 parts of lemongrass, 0.5 parts of star anise, 1 part of tangerine peel, 9 parts of cumin, 6 parts of liquorice, and 3 parts of coriander seeds. Other experimental conditions are the same, and spicy essence 3 is obtained.

[0050] Example 2 (1) The spice raw materials (peppercorns, cinnamon bark, dill seeds, clove buds, lemongrass, star anise, tangerine peel, cumin, licorice and coriander seeds) were placed in a low-temperature freezing device, with liquid nitrogen as the freezing source, the crushing temperature was -40 ° C, the crushing particle size was 50 mesh, and the crushed spice powder was stored in a constant humidity environment with the humidity controlled at 12%; (2) Take 2 parts of Sichuan peppercorns, 6 parts of cinnamon bark, 2 parts of dill seeds, 8 parts of clove buds, 3 parts of lemongrass, 3 parts of star anise, 6 parts of dried tangerine peel, 3 parts of cumin, 4 parts of liquorice, and 2 parts of coriander seeds, and mix them evenly to obtain a spice mixture for later use; (3) The spice mixture powder was transferred into a reactor, and CO2 fluid was introduced. Static extraction was carried out at 13 MPa and 45 °C for 1 h. Carbon dioxide was continued to be introduced, and the pressure of the extraction reactor was adjusted to 15 MPa. After 2 h of cyclic extraction at a flow rate of 2.0 L / min, the receiving valve was opened. After the extraction was completed, spice essential oil I and raw material residue were obtained; (4) The raw material residue was rinsed with 75% edible alcohol, and the solid-liquid ratio of the raw material residue to the edible alcohol was 1g:5ml; then 10% sodium carbonate solution was sprayed and added, and the solid-liquid ratio (w:v) of the raw material residue to the sodium carbonate solution was 1g:4ml. The soaking time was 60min. The raw material residue and the soaking alkali solution were placed in a microwave extraction device for microwave-assisted solvent-free extraction. The extraction temperature was set to 70℃, the microwave power was 400W, and the extraction time was 60min. After extraction, the mixture was allowed to stand for stratification, and the upper layer was taken to obtain spice essential oil II.

[0051] (5) Spice essential oil I and spice essential oil II are combined to obtain spicy essence 4.

[0052] Comparative Example 3 The only difference from Example 2 is that the CO2 supercritical fluid extraction conditions in step (3) are adjusted to: extraction temperature 50°C, extraction pressure 30 MPa, and static extraction at 45°C for 2 hours. The other experimental conditions are consistent with Example 2, and spicy flavor 5 is obtained.

[0053] Comparative Example 4 The only difference from Example 2 is that the extraction step of step (4) is omitted, and the spice essential oil I obtained in step (3) is the spicy flavor, which is recorded as spicy flavor 6. Comparative Example 5 The only difference from Example 2 is that in step (4), the sodium carbonate solution is replaced with an equal volume of pure water. The other experimental conditions are the same as those in Example 2, and spicy flavor 7 is obtained.

[0054] Comparative Example 6 The only difference from Example 2 is that in step (4), the step of rinsing the raw material residue with edible alcohol is omitted, and 10% sodium carbonate solution is directly sprayed into the raw material residue. The other experimental conditions are consistent with those of Example 2, and spicy flavor 8 is obtained.

[0055] Test Example 1 The extraction was repeated three times in each of the above examples and comparative examples, and the yields of spicy flavors 1 to 8 were calculated. The specific formula is shown in formula (1), and the experimental results of the specific yields are shown in Table 1.

[0056] ×100% formula (1) In formula (1), y is the yield of spicy flavor, m is the mass of spice mixed powder, unit is g, m1 is the mass of spice essential oil I, unit is g, and m2 is the mass of spice essential oil II, unit is g.

[0057] The yields of the above-mentioned spicy flavors are calculated and are listed in Table 1: Table 1 Yield of spicy flavors by different extraction methods (%)

[0058] According to Table 1: The results of Example 1 and Comparative Example 1 show that cryogenic crushing helps to improve the oil yield.

[0059] The results of Example 2 and Comparative Example 4 show that further microwave extraction of the supercritical extraction residue is helpful to improve the oil yield of spices.

[0060] The results of Example 2 and Comparative Example 4 show that soaking the spice residue in alkaline solution helps to increase the oil yield of the raw material.

[0061] Test Example 2 Spicy Flavors 1 to 8 were diluted with an appropriate amount of ethanol and added to blank cigarettes at a ratio of 0.12% using a flavoring injector. The cigarettes were then equilibrated for 48 hours in a constant temperature and humidity chamber (relative humidity 60±5%, temperature 20±2°C). The cigarettes were scored according to the GB5606.4-2005 Cigarette Sensory Quality Evaluation Standards. Ten professional technicians with national or provincial qualifications in cigarette sensory quality evaluation were evaluated. The evaluation criteria are shown in Table 2. Cigarettes made from cut tobacco without the addition of extracts served as a control, and the gloss score was not considered. The smoking results are shown in Table 3.

[0062] Table 2 GB5606.4--2005 Cigarette Sensory Quality Evaluation Standard

[0063] Table 3 Sensory evaluation results of Examples 1-2 and Comparative Examples 1-6

[0064] The results show that: 1. The spicy characteristics of the olfactory characteristics of spicy flavors 1 to 8 are obvious; especially spicy flavors 1 and 4, which have good smoke permeability, obvious spicy aroma, harmonious aroma, rich and full smoke, good layering, and a natural feel; 2. According to spicy flavor 1 and spicy flavor 2, deep cold grinding helps to retain the original volatile components and heat-sensitive components in spices, so that the spicy flavor has more effective substances.

[0065] 3. According to Spicy Flavor 1 and Spicy Flavor 3, the spice formula of Example 1 is more coordinated with the tobacco aroma.

[0066] 4. According to spicy flavors 4 and 5, it can be seen that during supercritical extraction, higher pressure causes more polyenamides, sugars, pigments and other substances in spicy flavors to dissolve, affecting the coordination with the tobacco aroma.

[0067] 5. According to spicy flavor 4 and spicy flavor 6, further microwave extraction of supercritical extraction residue can enrich the flavor substances of spicy flavor.

[0068] 6. According to spicy flavor 4 and spicy flavor 8, alcohol washing can remove some substances that affect sensory effects, such as polyenamide and cellulose in the raw material residue, thereby improving the sensory experience and reducing oral residue.

[0069] 7. In summary, deep-cold grinding, spice blending, low-pressure environment during supercritical extraction, solvent-free microwave extraction, and elution with sodium carbonate solution can enhance the smoke richness of spicy flavors, harmonize with the aroma of the tobacco, reduce irritation to the oral and nasal cavities, and improve the aftertaste of the mouth, making them particularly suitable for highlighting the style characteristics of cigarettes.

[0070] Test Example 3 The spicy flavor 1 obtained above was subjected to GC / MS analysis, and the fingerprint was obtained by searching and analyzing the NIST general library. Figure 1 Its main chemical components and relative percentages are shown in Table 4.

[0071] Table 4 Description and content analysis of the main volatile components in spicy flavor 1

[0072] As shown in Table 4, Spicy Flavor 1 exhibits a strong, fresh, spicy aroma, supplemented by sweet, woody, floral, and light herbal notes. Its main components are eugenol, cinnamaldehyde, eugenyl acetate, β-caryophyllene, linalool, and carvone. In addition to the main volatile components mentioned in the table, other volatile components are present at lower levels, including benzoic acid, camphene, styrene, β-pinene, vanillin, β-ocimene, phenylacetaldehyde, nonanal, pentadecanal, citronellal, octyl acetate, phenylethyl acetate, dianthin, and carveol. These compounds enhance the fruity, sweet, floral, and woody notes of the spicy flavor and reduce irritation and dryness.

[0073] Test Example 4 The spicy flavor was designed into a spicy plate, whose raw material composition, by weight, included: 1 part spicy flavor, 0.5 part raspberry ketone, 0.2 part neroli oil, 1 part plum extract, 2 parts cooling agent, 3 parts water, 60 parts ethanol, and 32.3 parts propylene glycol. The spicy plate, prepared by combining these ingredients, was sprayed onto roller-pressed reconstituted tobacco leaves at a 5% addition rate. The resulting heated cigarettes were then heated to 300-350°C in an electric heater. A panel of seven experts evaluated the smoke in the presence of the spicy plate and those without it, comparing the samples in terms of aroma, harmony, smoke concentration, softness and refinement, aftertaste, and off-flavors. The expert evaluation results are shown in Table 5.

[0074] Table 5 Sensory evaluation results of heated cigarettes

[0075] As can be seen from Table 5, the spicy plate prepared in this experimental example has a rich and fresh spicy aroma, supplemented by fruity, floral and woody aromas. The smoke is rich, the smoke permeability and fineness are improved, the oral comfort is improved, the residue is not obvious, and it has good coordination with the tobacco aroma, improves the inhalation taste, enhances the aroma quality, and the smoke is fine and coordinated with the tobacco aroma, giving consumers a more comprehensive experience.

[0076] While various embodiments of the present invention have been described above, the above descriptions are intended to be illustrative, non-exhaustive, and not limited to the disclosed embodiments. Many modifications and variations will be apparent to those skilled in the art without departing from the scope and spirit of the described embodiments. The terminology used herein is selected to best explain the principles of the embodiments, their practical applications, or improvements to existing technologies, or to enable others skilled in the art to understand the embodiments disclosed herein.

Claims

1. A method for preparing a spicy flavor, characterized in that: include: Step a), subjecting each component of the spice to cryogenic grinding treatment at a grinding temperature of -20 to -60°C to obtain corresponding spice powder; Step b), placing the spice powder of each component in a constant temperature and humidity environment, and adjusting the humidity of the spice powder to 10-15%; Step c), mixing the spice powders of the various components according to a proportion to obtain a spice mixture powder; Step d), subjecting the spice mixed powder to supercritical CO2 extraction at an extraction pressure of 10-22 MPa, an extraction temperature of 35-45°C, and an extraction time of 1-5 h to obtain spice essential oil I and a raw material residue; Step e), subjecting the raw material residue to microwave-assisted extraction, and allowing the extract to stand and separate to obtain spice essential oil II; Step f), merging spice essential oil I and spice essential oil II to obtain spicy essence.

2. The preparation method according to claim 1, characterized in that The spices include two or more of the following components: pepper, cinnamon bark, dill seeds, clove buds, lemongrass, star anise, tangerine peel, cumin, liquorice, coriander seeds, and celery seeds.

3. The preparation method according to claim 2, characterized in that The spice mixture powder comprises, by weight, 1-5 parts of peppercorns, 4-10 parts of cinnamon bark, 1-5 parts of dill seeds, 2-12 parts of clove buds, 2-5 parts of lemongrass, 1-4 parts of star anise, 2-8 parts of tangerine peel, 1-8 parts of cumin, 1-5 parts of liquorice, and 1-2 parts of coriander seeds.

4. The preparation method according to claim 1, characterized in that The particle size of the spice powder is 20-200 meshes.

5. The preparation method according to claim 1, characterized in that In the step d), the supercritical CO2 extraction is specifically performed by first performing static extraction and then performing cyclic extraction; The static extraction pressure is 10-15 MPa, the extraction temperature is 35-45°C, and the extraction time is 1-2 hours; The pressure of the cyclic extraction is 13-22 MPa, the extraction temperature is 35-45° C., and the extraction time is 1-3 hours.

6. The preparation method according to claim 1, characterized in that The step e) is specifically as follows: performing alcohol washing on the raw material residue; Soak the raw material residue after alcohol washing in alkali solution; the material-liquid ratio of the raw material residue to the alkali solution is 1g:3~7ml, and the soaking time is 0.5~5h; The raw material residue and the alkali solution in which it is soaked are subjected to microwave-assisted extraction at a power of 150-700 W, a time of 30 min-120 min, and a temperature of 50-120° C.

7. The preparation method according to claim 6, characterized in that The alcohol washing adopts edible alcohol with a concentration of 50% to 100%, and the alkali solution is a sodium carbonate solution with a concentration of 5% to 10%.

8. A spicy flavor, characterized in that It is prepared according to the method according to any one of claims 1 to 7.

9. A spicy plate, characterized in that: The composition includes, by weight, 1-10 parts of spicy flavor, 0.1-2.5 parts of raspberry ketone, 0.2-1 parts of neroli oil, 0.1-5 parts of plum extract, 2-5 parts of cooling agent, 2-5 parts of water, 5-65 parts of ethanol, and 6.5-89.6 parts of propylene glycol.

10. Use of the spicy flavor block according to claim 9 in flavoring cigarettes, wherein the cigarettes are heat-not-burn cigarettes, electronic cigarettes, or full-grain cigarettes.

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