Tobacco extract rich in solapalmitate, soladulcide and preparation method and application thereof

Abstract

The present application belongs to the technical field of tobacco flavor, and relates to a preparation method of tobacco characteristic flavor, in particular to a tobacco extract rich in solanone and soladulcidin as well as a preparation method and application thereof. The preparation method comprises the following steps: extracting dried tobacco flower buds with an ethanol aqueous solution or anhydrous ethanol to obtain a flower bud extract; concentrating the flower bud extract to separate layers, removing a lower layer of concentrated liquid to obtain an extract extract; dissolving the extract extract and then performing silica gel column chromatography purification to screen an extract component containing solanone and soladulcidin; and concentrating the extract component and removing a solvent, thereby obtaining the tobacco extract extract rich in solanone and soladulcidin. The extract can significantly improve the aroma quality and fullness of cigarettes, and can improve the smoke of an electronic cigarette and increase the pollen-like sweet smell thereof.

Description

Technical Field

[0001] This invention belongs to the field of tobacco flavoring technology, and relates to a method for preparing characteristic tobacco flavorings, specifically to a tobacco extract rich in solanone and solanedione, its preparation method and application. Background Technology

[0002] The information disclosed in this background section is intended only to enhance understanding of the overall background of the invention and is not necessarily to be construed as an admission or in any way implying that such information constitutes prior art known to those skilled in the art.

[0003] Solanone and norcanedione are unique aroma components of tobacco. Solanone possesses a green, grassy, ​​and sweet aroma, reminiscent of carrots and tea, and its aroma is relatively long-lasting. It can harmonize well with a variety of aromas, while norcanedione excels in thickening and enhancing the resilience of the aroma. The combination of these two can significantly enhance the aroma of cigarettes, making the smoke fuller and greatly improving cigarette quality. However, the content of solanone and norcanedione in tobacco leaves is relatively low, resulting in low levels of these compounds in conventional tobacco extracts, which cannot meet the demand for natural tobacco flavorings in low-tar cigarettes. Various synthetic methods exist both domestically and internationally to produce solanone and norcanedione for tobacco. However, on the one hand, current chemical synthesis methods for solanone and norcanedione are lengthy and costly; on the other hand, the configurations of synthetic solanone and norcanedione differ from those of natural tobacco solanone and norcanedione, resulting in a lack of naturalness and harmony in the flavoring of tobacco products. This makes the extraction of these components from tobacco resources crucial. Summary of the Invention

[0004] To overcome the current situation where the content of solanone and solanidine in tobacco extracts is low, and the naturalness and harmony of chemically synthesized solanone and solanidine are poor, the purpose of this invention is to provide a tobacco extract rich in solanone and solanidine, its preparation method and application. This invention can obtain a tobacco extract paste rich in solanone and solanidine, which can significantly improve the aroma quality and fullness of cigarettes, and can also improve the aroma of e-cigarettes, increasing its pollen-like sweetness.

[0005] To achieve the above objectives, the technical solution of the present invention is as follows:

[0006] In one aspect, a method for preparing a tobacco extract rich in solanone and solanedione includes the following steps:

[0007] The dried tobacco flower buds were extracted using an aqueous ethanol solution or anhydrous ethanol to obtain a flower bud extract.

[0008] The flower bud extract was concentrated until it separated into layers, and the lower layer of concentrate was removed to obtain the extract paste.

[0009] The extract was dissolved and purified by silica gel column chromatography to screen extract fractions containing solanone and solanedione.

[0010] The extract components are concentrated and the solvent is removed to obtain the final product.

[0011] Tobacco inflorescences are a crop that needs to be topped during the flowering period. Currently, most of the toppled tobacco inflorescences are buried, which not only wastes resources but also potentially pollutes the environment. Research in this invention has revealed that tobacco buds contain large amounts of solanone and solanidine, with levels far exceeding those found in tobacco leaves. Therefore, this invention uses dried tobacco buds as raw material, first extracting them with an ethanol-water solution, then sequentially concentrating, separating the lipids and water, and performing chromatographic enrichment to obtain a tobacco extract rich in solanone and solanidine. This method uses tobacco buds instead of tobacco leaves as the raw material for extracting solanone and solanidine, avoiding the resource waste caused by directly burying tobacco inflorescences and the waste associated with using tobacco leaves as raw material. This improves the utilization rate of tobacco leaves in cigarette production, thereby increasing the overall economic benefits of tobacco.

[0012] Secondly, a tobacco extract rich in solanone and solanedione is obtained by the above preparation method.

[0013] Thirdly, the application of the above-mentioned tobacco extract rich in solanone and solanedione in the flavoring of tobacco products.

[0014] Research has shown that the tobacco extract obtained by the preparation method provided in the first aspect, when added to tobacco products, especially cigarettes, can significantly improve the aroma quality and fullness of cigarettes, and can also enhance the aroma of e-cigarettes, increasing its pollen-like sweetness.

[0015] The beneficial effects of this invention are as follows:

[0016] 1. This invention uses tobacco flower buds, which are originally considered waste, as raw materials to extract tobacco flavoring rich in solanone and solanidine. This not only avoids the waste of resources but also avoids the possibility of environmental pollution caused by direct burial. Thus, it can turn waste into treasure, improve the economic benefits of tobacco planting, and promote increased income for tobacco farmers.

[0017] 2. This invention uses tobacco flower buds as raw materials. Through concentration, lipid-water separation, and chromatographic separation and enrichment, it can extract and retain solanone and solanedione in tobacco flower buds as much as possible, thereby obtaining tobacco extract rich in solanone and solanedione. The operation steps are simple, do not require expensive equipment, and are easy to scale up for production.

[0018] 3. Studies have shown that adding the tobacco extract provided by this invention to tobacco products as an additive can not only coordinate various aromas, but also thicken and increase the toughness of the aroma, thereby significantly increasing the aroma of cigarettes and making the smoke fuller, thus significantly improving the quality of tobacco products. Detailed Implementation

[0019] It should be noted that the following detailed descriptions are exemplary and intended to provide further illustration of the invention. Unless otherwise specified, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains.

[0020] It should be noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of exemplary embodiments according to the invention. As used herein, the singular form is intended to include the plural form as well, unless the context clearly indicates otherwise. Furthermore, it should be understood that when the terms "comprising" and / or "including" are used in this specification, they indicate the presence of features, steps, operations, devices, components, and / or combinations thereof.

[0021] Given that the content of solanone and solanedione in existing tobacco leaves is low, the cost of synthesizing solanone and solanedione is high, and their configurations differ, resulting in a lack of naturalness and harmony in the flavoring of tobacco products, this invention proposes a tobacco extract rich in solanone and solanedione, its preparation method, and its application.

[0022] A typical embodiment of the present invention provides a method for preparing a tobacco extract rich in solanone and solanedione, comprising the following steps:

[0023] The dried tobacco flower buds were extracted using an aqueous ethanol solution or anhydrous ethanol to obtain a flower bud extract.

[0024] The flower bud extract was concentrated until it separated into layers, and the lower layer of concentrate was removed to obtain the extract paste.

[0025] The extract was dissolved and purified by silica gel column chromatography to screen extract fractions containing solanone and solanedione.

[0026] The extract components are concentrated and the solvent is removed to obtain the final product.

[0027] The drying methods for tobacco buds in this invention include freeze-drying, air-drying, sun-drying, programmed temperature drying, and constant temperature drying. In some embodiments, air-drying is used to dry the tobacco buds. Studies have shown that the content of solanone and solanedione in tobacco buds dried by air-drying is significantly higher than that in tobacco buds dried by other methods, and tobacco extracts prepared from air-dried tobacco buds contain more solanone and solanedione.

[0028] In the process of extracting flower bud extract according to this invention, ethanol and water can be mixed in any proportion, for example, the ethanol volume content can be 1-99.99%. The ethanol aqueous solution generally has an ethanol volume content of not less than 80% (when the ethanol volume content is 100%, it is anhydrous ethanol). In some embodiments, the ethanol volume content in the ethanol aqueous solution is not less than 90%, preferably not less than 95%. Studies have shown that when using an ethanol aqueous solution with an ethanol volume content of not less than 90%, the yields of solanone and norsanodione can be significantly improved, especially when the ethanol volume content is not less than 95%, the yields of solanone and norsanodione are even higher.

[0029] In this invention, the extraction temperature for obtaining the flower bud extract is 20–50°C; in some embodiments, the extraction temperature is 20–40°C. Studies have shown that when extracted within the 20–40°C range, the yields of solanone and norsanodione are not significantly different. However, when the extraction temperature reaches 50°C, the yields of solanone and norsanodione from the fireworks raw materials decrease significantly. Preferably, the extraction temperature for the flower bud extract is 20–25°C, under which heating is unnecessary and costs are lower.

[0030] In the process of extracting the tobacco bud extract, the ratio of dried tobacco buds to aqueous ethanol or anhydrous ethanol is 1:5 to 1:15 (g:mL); in some embodiments, the ratio is 1:8 to 1:15. Within this range, the yields of solanone and norsanodione are higher; however, when the ratio is 1:8 to 1:10, the difference in the yields of solanone and norsanodione is not significant.

[0031] In the process of extracting flower bud extract, the extraction time is 5 to 30 minutes. In some embodiments, the extraction time is 10 to 30 minutes. Studies have shown that the yields of solanone and solanedione are higher within this extraction time, and the difference in yield is not significant. Among them, the extraction time is shorter when it is 10 to 20 minutes.

[0032] In some embodiments, the flower bud extract is concentrated under reduced pressure. Reduced pressure concentration uses lower temperatures and consumes less energy. Specifically, the temperature for reduced pressure concentration is 45–50°C.

[0033] In some embodiments, the flower bud extract is concentrated until separation occurs, then allowed to stand at 0–4°C until complete separation, and then the lower layer of concentrate is removed. Specifically, the time for standing until complete separation is achieved is 24–48 hours.

[0034] In some embodiments, dry loading is used when performing silica gel column chromatography purification.

[0035] In some embodiments, during silica gel column chromatography purification, elution is performed sequentially using hexane, a mixture of hexane and ethyl acetate, ethyl acetate, and a mixture of ethyl acetate and ethanol. The volume fraction of hexane in the hexane and ethyl acetate mixture decreases with increasing elution times, while the volume fraction of ethanol in the ethyl acetate and ethanol mixture increases with increasing elution times. Specifically, elution is performed sequentially using hexane, a hexane and ethyl acetate mixture with a hexane volume fraction of 78–82%, a hexane and ethyl acetate mixture with a hexane volume fraction of 38–42%, a hexane and ethyl acetate mixture with a hexane volume fraction of 18–22%, ethyl acetate, an ethyl acetate and ethanol mixture with a ethanol volume fraction of 28–32%, and an ethyl acetate and ethanol mixture with a ethanol volume fraction of 48–52%.

[0036] In one or more embodiments, the eluent fractions of a mixture of n-hexane and ethyl acetate with a volume fraction of 40-0% n-hexane and 0% n-hexane, and the eluent fractions of a mixture of ethyl acetate and ethanol with a volume fraction of 0-50% ethanol, are used as extract components. Studies have shown that this condition can better achieve the enrichment of solanone and norsanodione. Specifically, the eluent fractions obtained from mixtures of n-hexane and ethyl acetate with a volume fraction of 38-42% n-hexane, mixtures of n-hexane and ethyl acetate with a volume fraction of 18-22% n-hexane, mixtures of ethyl acetate and ethanol with a volume fraction of 28-32% ethyl acetate and ethanol, and mixtures of ethyl acetate and ethanol with a volume fraction of 48-52% ethanol are used as extract components.

[0037] In another embodiment of the present invention, a tobacco extract rich in solanone and solanedione is provided, which is obtained by the above preparation method.

[0038] A third embodiment of the present invention provides an application of the above-mentioned tobacco extract rich in solanone and solanedione in the flavoring of tobacco products.

[0039] In some embodiments, the tobacco product is a cigarette or an electronic cigarette.

[0040] Specifically, 4-8 mg of tobacco extract rich in solanone and norsanodione is added per kilogram of tobacco shreds to the cigarette. More specifically, the tobacco extract rich in solanone and norsanodione is dissolved in a solvent and then added to the tobacco shreds to prepare the cigarette. The solvent used to dissolve the tobacco extract rich in solanone and norsanodione is a mixture of propylene glycol, ethanol, and water. In the mixture of propylene glycol, ethanol, and water, the volume fraction of propylene glycol is 18-22%, and the volume fraction of ethanol is 53-57%.

[0041] Specifically, in the e-cigarette, 1-3% of a tobacco extract rich in solanone and norsanodione is added per kilogram of e-cigarette liquid. More specifically, the method of addition is as follows: the tobacco extract rich in solanone and norsanodione is dissolved in a solvent and then added to the e-cigarette liquid. The solvent used to dissolve the tobacco extract rich in solanone and norsanodione is a mixture of propylene glycol, ethanol, and water. In the mixture of propylene glycol, ethanol, and water, the volume fraction of propylene glycol is 73-77%, and the volume fraction of ethanol is 16-20%.

[0042] To enable those skilled in the art to better understand the technical solution of the present invention, the technical solution of the present invention will be described in detail below with reference to specific embodiments.

[0043] Example

[0044] 1. Selection of raw materials rich in solanone and noradrenone

[0045] 1.1 Raw material collection

[0046] Using the Honghua Dajinyuan flue-cured tobacco variety from the Dali tobacco-growing area of ​​Yunnan as a representative example, the inflorescences were collected during the topping stage. During the tobacco leaf maturity stage, tobacco leaves from different parts were collected using conventional production methods.

[0047] 1.2 Drying

[0048] Tobacco leaves were dried using conventional baking methods, with the C3F sample from the middle section after baking and drying selected as a representative sample. Tobacco buds were dried using five different methods: freeze-drying, air-drying, sun-drying, programmed temperature drying, and constant temperature drying. The drying conditions for each method are as follows:

[0049] (1) Freeze drying

[0050] The flower buds of the collected tobacco inflorescences were picked, frozen in liquid nitrogen, and then freeze-dried.

[0051] (2) Dry

[0052] Environmental conditions: The diurnal temperature range should be greater than 7℃, with no high temperature and humidity (temperature above 30℃, humidity above 70%), and natural ventilation. Bundle the collected tobacco inflorescences with the main stem, 8-12 inflorescences per bundle. Hang the bundled inflorescences upside down in the seedling shed, which should be shaded. A kraft paper layer should be placed under the hanging device, with the inflorescences 30cm above the layer. During the drying process, the buds will automatically fall onto the layer. Arrange the buds to a thickness of 2-3cm on the layer, turning them over at least once a day. Continue drying on the layer until the moisture content is less than 10%.

[0053] (3) Sun-dry

[0054] Place the collected tobacco inflorescences on a surface covered with kraft paper, with the inflorescences less than 15-20 cm thick. Sun-dry the inflorescences, turning them every 2-3 hours until all the buds have fallen off. Remove the inflorescence stems, and place the remaining buds on a 3-4 cm thick layer of kraft paper, turning them every 3-4 hours. Continue sun-drying on the kraft paper until the moisture content is less than 10%. Note that on rainy days, move the inflorescences indoors.

[0055] (4) Programmable temperature drying

[0056] The drying equipment used in the test was an electric heating temperature and humidity control device (1.90m×1.35m×1.40m). The drying equipment was equipped with stainless steel mesh trays with a spacing of 35cm between the trays, and 10-mesh nylon mesh was laid on the trays.

[0057] Remove the main stem from the collected tobacco inflorescences, place them in layers on a nylon mesh with a thickness of 6-8 cm, and dry them according to the temperature program in Table 1.

[0058] Table 1. Tobacco inflorescence drying procedure

[0059]

[0060] (5) Constant temperature drying

[0061] The drying equipment used in the test was the same as the programmed temperature drying equipment (1.90m×1.35m×1.40m).

[0062] Remove the main stem from the collected tobacco inflorescences, place them in layers on a tray lined with 10-mesh nylon mesh, 6-8 cm thick, and dry at 57°C until the moisture content is less than 10%.

[0063] All the above drying conditions were repeated three times.

[0064] 1.3 Comparison of solanone and norsanodione content in fireworks raw materials dried by different methods

[0065] Sample processing: After drying, tobacco buds obtained by different drying methods were taken, and at the same time, samples of conventionally roasted red tobacco leaves (C3F) were taken, crushed, and the mass fraction of the target components was determined.

[0066] Methods for determining the content of solanone and norsanodione: Weigh 0.2 g of the pulverized sample and place it in a 45 mL glass centrifuge tube. Add 5 mL of ethyl acetate solution containing 17-alkyl internal standard (100 μg / mL), sonicate at room temperature for 10 min, add 5 mL of deionized water, vortex to mix, incubate at 3000 rpm for 10 min, collect the supernatant, filter through a 0.22 μm filter membrane, and determine by GC / MS. The chromatographic column was HP-MS, 30 m × 250 μm × 0.25 μm, the carrier gas was helium, the flow rate was 1.0 mL / min, the injection port temperature was 260 ℃, the injection mode was split, the injection volume was 1 μL, the split ratio was 5:1, the initial column temperature was 40 ℃, held for 1 min, increased to 260 ℃ at 15 ℃ / min, and held for 5 min. Mass spectrometry transfer line temperature: 280℃; quadrupole temperature: 150℃; EI ion source temperature: 230℃; ionization energy: 70 eV; mass scan range: 30–550 amu. Solanone and norsanodione were qualitatively identified based on NIST library search results and literature data. The mass fractions of solanone and norsanodione were calculated using a semi-quantitative method with 17-alkyl as an internal standard. The results are shown in Table 2.

[0067] Comparison of solanone and norsanodione content: Table 2 shows that under air-drying conditions, the content of solanone and norsanodione in tobacco buds was significantly higher than that under other drying methods, being 4.37-4.43, 2.4-3.4, 2.8-4.3, and 3.28-4.98 times higher, respectively, than under freeze-drying, sun-drying, programmed temperature drying, and constant temperature drying conditions. Under different drying methods, the content of solanone and norsanodione in tobacco buds was higher than that in tobacco leaves, with the content of solanone and norsanodione in air-dried tobacco buds being 15.9-19.7 times that in tobacco leaves (C3F). Therefore, air-dried tobacco buds were selected as the raw material for tobacco extracts rich in solanone and norsanodione.

[0068] Table 2. Mass fractions of solanone and norcanedione in tobacco flower buds under different drying methods.

[0069]

[0070]

[0071] 2. Extraction and purification of solanone and norsanodione

[0072] 2.1 Selection of Extraction Conditions

[0073] (1) Solvent selection

[0074] Considering cost and extract safety, different concentrations of ethanol (80%, 90%, 95%, and 100%) were selected as extraction solvents. 10g of dried tobacco buds were extracted three times at room temperature for 10 minutes each time, with a material-to-liquid ratio of 10:1 (g:g). The extracts were combined and mixed thoroughly. 1mL of the extract was dried under nitrogen and dissolved in 1mL of ethyl acetate solution containing a 17-alkyl internal standard (100μg / mL). The solution was filtered through a 0.22μm filter membrane, and the yields of solanone and norsanodione from fireworks raw materials were semi-quantitatively determined by GC / MS. The results are shown in Table 3. Table 3 shows that within the ethanol concentration range of 80-95%, the yields of solanone and norsanodione increased significantly with increasing ethanol concentration. The difference in yield between anhydrous ethanol and 95% ethanol was not statistically significant. Therefore, considering economic efficiency, 95% ethanol was selected as the extraction solvent.

[0075] Table 3. Yields of solanone and norsanodione extracted from fireworks raw materials at different ethanol concentrations (mg / 100g)

[0076]

[0077] (2) Extraction temperature

[0078] 10g of dried tobacco buds were extracted three times at room temperature for 20min each time using 95% ethanol as the solvent at a material-to-liquid ratio of 10:1. The extraction temperatures were set at room temperature (22℃), 30℃, 40℃, and 50℃. The extracts from each treatment were combined, and the yields of solanone and norsanodione from the fireworks raw materials were determined using the same method as in 2.1. The results are shown in Table 4. Table 4 shows that the yields of solanone and norsanodione from the fireworks raw materials did not differ significantly within the range of room temperature to 40℃. At an extraction temperature of 50℃, the yields of solanone and norsanodione from the fireworks raw materials decreased significantly. Therefore, room temperature extraction was chosen to save costs.

[0079] Table 4. Yields of solanone and norsanodione from fireworks raw materials at different extraction temperatures (mg / 100g)

[0080]

[0081] (3) Selection of feed-liquid ratio

[0082] 10g of dried tobacco buds were extracted three times at room temperature for 20min each time using 95% ethanol as the solvent. Four treatments were set with different material-to-liquid ratios: 1:5, 1:8, 1:10, and 1:15. The extracts from each treatment were combined, and the yields of solanone and norsanodione in the fireworks raw materials were determined using the same method as in 2.1. The results are shown in Table 5. As can be seen from Table 5, the yields of solanone and norsanodione were lowest under the material-to-liquid ratio of 1:5. Within the material-to-liquid ratio range of 1:8-1:15, the differences in the yields of solanone and norsanodione were not significant. Therefore, the significant material-to-liquid ratios were 1:8-1:10.

[0083] Table 5. Yields of solanone and norsanodione from fireworks raw materials with different feed-to-liquid ratios (mg / 100g)

[0084]

[0085] (4) Extraction time selection

[0086] 10g of dried tobacco buds were extracted three times at room temperature using 95% ethanol as the solvent at a material-to-liquid ratio of 10:1. Four extraction times were set: 5 min, 10 min, 20 min, and 30 min. The extracts from each treatment were combined, and the yields of solanone and norsanodione in the fireworks raw material were determined using the same method as in section 2.1. The results are shown in Table 6. Table 6 shows that the yields of solanone and norsanodione were significantly lower at an extraction time of 5 min. Within the extraction time range of 10-30 min, the differences in the yields of solanone and norsanodione were not significant. Therefore, an extraction time of 10-20 min was selected.

[0087] Table 6. Yields of solanone and norsanodione from fireworks raw materials at different extraction times (mg / 100g)

[0088]

[0089] Based on the above experimental results, the extraction conditions for tobacco solanone and solanidone are as follows: using dried tobacco buds as raw material, 95% ethanol as the extraction solvent, a material-to-liquid ratio of 8-10:1, extraction at room temperature, extraction three times consecutively, each time for 10-20 minutes, and then combining the extracts.

[0090] 2.2 Extraction and Concentration Separation

[0091] Based on the above extraction conditions, 5 kg of tobacco buds were used as raw material, 95% ethanol was used as the extraction solvent, the material-to-liquid ratio was 10:1, and extraction was performed at room temperature for 3 consecutive times, 10 min each time. The extracts were combined and concentrated under reduced pressure at 45-50℃ until the concentrate showed stratification. The extract was then allowed to stand at 0-4℃ for 24 h. 0.1 g of the upper (lipid-soluble) and lower (water-soluble) extracts were taken separately and dried under nitrogen. The mass fractions of solanone and norsanodione in the extracts were determined using the same method as in 2.1. No solanone or norsanodione was detected in the lower concentrate, while the mass fractions of solanone and norsanodione in the upper concentrate were 9.52 mg / g and 5.48 mg / g, respectively. The lipid and aqueous layers of the concentrated extract were separated, and the lower concentrate was discarded to obtain 190 g of extract preliminarily enriched with solanone and norsanodione.

[0092] 2.3 Silica gel column chromatography purification

[0093] Take 100g of the lipid-soluble extract obtained above, and use dry loading method to separate and enrich solanone and solanedione by silica gel column chromatography. The specific method is as follows: (1) Mixing: Dissolve the extract in ethanol, stir evenly with 100-200 mesh silica gel at a ratio of 1:1, remove the solvent by rotary evaporation, and obtain silica gel powder adsorbing the extract. (2) Column packing and loading: Take a 10cm diameter vacuum chromatography column (with sand core), and uniformly pack 300g of silica gel (200-300 mesh). Then, carefully and evenly add the silica gel powder (100-200 mesh) adsorbing the extract obtained above to the top layer of the column. (3) Elution: Add 12 times the volume of solvent of the extract (Table 7) in sequence for vacuum filtration and elution. Collect the eluted components separately, and take 1ml of each, filter through a 0.2μm filter membrane, separate them using gas chromatography-mass spectrometry, and identify the target compounds by searching the NIST spectral library. Compare the differences in the content of solanone and solanedione in different components by peak area. According to the test results, components Fr3, Fr4, Fr5, Fr6, and Fr7 contained solanone and norsanodione, with higher contents in components Fr4, Fr5, and Fr6. Fr1, Fr2, Fr8, and Fr9 showed almost no detectable levels of solanone and norsanodione. Fr3, Fr4, Fr5, Fr6, and Fr7 were combined, concentrated, and the solvent was removed to obtain 83.68 g of eluent extract. 0.1 g of this extract was dissolved in 10 mL of ethyl acetate solution containing a 17-alkyl internal standard (100 μg / mL), filtered through a 0.22 μm filter membrane, and semi-quantitatively determined by GC / MS to be 9.17 mg / g and 5.17 mg / g, respectively.

[0094] Table 7. Elution solvent composition for silica gel column chromatography

[0095]

[0096] 3. Flavoring application in tobacco products

[0097] Cigarette Addition: The obtained extract rich in solanone and norsanodione was dissolved in a solvent (20% propylene glycol + 55% ethanol + 25% water) at a mass ratio of 1:100 and added to the reference cigarette. The amount of the target extract added per kilogram of tobacco was 4-8 mg. The same volume of blank solvent was added as a control. Sensory evaluation was carried out according to the sensory technical requirements (GB 5606.4-2005 Cigarette Part 4). As shown in Table 8, the results showed that the target extract could significantly improve the aroma quality, improve the aroma penetration, enrich the tobacco aroma, reduce the irritation, and increase the smoothness, delicacy and sweetness of the smoke.

[0098] Table 8. Statistical Table of Sensory Quality Inspection of Cigarettes

[0099]

[0100] Adding to e-cigarettes: The obtained extract rich in solanone and norsanodione was dissolved in a solvent (75% propylene glycol + 18% ethanol + 7% water) at a mass ratio of 5:100 and added to the e-cigarette liquid at a rate of 1-3% per kilogram of e-cigarette liquid. A blank solvent of the same volume was added as a control. Sensory evaluation was conducted according to the enterprise standard Q / SZ 105 002—2024, as shown in Table 9. The results showed that the extract could significantly improve the aroma of e-cigarettes: the aroma quality was improved, the fullness of the smoke was increased, the smoothness and delicacy were improved, the irritation was reduced, and the sweetness was increased, but the effect on satisfaction was not obvious.

[0101] Table 9 Sensory Quality Evaluation Indicators and Scales for Heated Cigarettes

[0102]

[0103]

[0104] The above description is merely a preferred embodiment of the present invention and is not intended to limit the invention. Various modifications and variations can be made to the present invention by those skilled in the art. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the scope of protection of the present invention.

Claims

1. A method for preparing a tobacco extract rich in solanone and solanedione, characterized in that, Includes the following steps: The dried tobacco flower buds were extracted using an aqueous ethanol solution or anhydrous ethanol to obtain a flower bud extract. The flower bud extract was concentrated until it separated into layers, and the lower layer of concentrate was removed to obtain the extract paste. The extract was dissolved and purified by silica gel column chromatography to screen extract fractions containing solanone and solanedione. The extract components are concentrated and the solvent is removed to obtain the final product; The method for drying tobacco flower buds is air drying; The volume content of ethanol in the aqueous ethanol solution is not less than 95%; The temperature for extracting the flower bud extract is 20~25℃; The mixture was eluted sequentially with hexane, a mixture of hexane and ethyl acetate with a volume fraction of 78-82% hexane, a mixture of hexane and ethyl acetate with a volume fraction of 38-42% hexane, a mixture of hexane and ethyl acetate with a volume fraction of 18-22% hexane, ethyl acetate, a mixture of ethyl acetate and ethanol with a volume fraction of 28-32% ethanol, and a mixture of ethyl acetate and ethanol with a volume fraction of 48-52% ethanol. The eluents obtained from the following solutions are used as extract components: a mixture of n-hexane and ethyl acetate with a volume fraction of 38-42% n-hexane, a mixture of n-hexane and ethyl acetate with a volume fraction of 18-22% n-hexane, a mixture of ethyl acetate and ethanol with a volume fraction of 28-32% ethyl acetate and ethanol, and a mixture of ethyl acetate and ethanol with a volume fraction of 48-52% ethanol. The ratio of dried tobacco buds to aqueous ethanol or anhydrous ethanol is 1:8 to 1:

15. The extraction time for flower bud extract is 10-30 minutes.

2. The method for preparing the tobacco extract rich in solanone and norsanodione as described in claim 1, characterized in that, The flower bud extract was concentrated under reduced pressure; the temperature for reduced pressure concentration was 45~50℃.

3. The method for preparing the tobacco extract rich in solanone and norsanodione as described in claim 1, characterized in that, The flower bud extract was concentrated until it separated into layers, and then allowed to stand at 0-4 ℃ until it completely separated into layers. The lower layer of concentrate was then removed. The time for complete separation is 24-48 hours.

4. The method for preparing the tobacco extract rich in solanone and norsanodione as described in claim 1, characterized in that, The ratio of dried tobacco buds to aqueous ethanol or anhydrous ethanol is 1:8 to 1:10; or, the extraction time for the bud extract is 10 to 20 minutes.

5. A tobacco extract rich in solanone and solanedione, characterized in that, Obtained by the preparation method described in any one of claims 1 to 4.

6. The use of the tobacco extract rich in solanone and solanedione as described in claim 5 in the flavoring of tobacco products.

7. The application as described in claim 6, characterized in that, The tobacco product is either a cigarette or an electronic cigarette.

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