Tobacco extract as well as preparation method and application thereof

Abstract

The invention belongs to the technical field of tobacco extraction, and particularly relates to a tobacco extract and a preparation method and application thereof. According to the method, the temperature parameters of the distillation process are precisely regulated and controlled, and the inert gas is adopted as the unique purging medium, so that the natural tobacco extract with harmonious aroma and outstanding fragrance is successfully prepared. The extract is rich in geranyl acetone, beta-damascone, beta-ionone, beta-dihydrodamascone and other core aroma components, and the substances have a synergistic effect, so that the extract is endowed with excellent aroma quality and sensory expression. Performance test results show that a cigarette product added with the extract shows purer and harmonious aroma quality and more abundant and full aroma amount, bad offensive odor such as wood odor and scorched odor is effectively modified and covered, the smoking strength tends to be soft and comfortable, and the unexpected technical effect is shown.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of tobacco extraction, and particularly relates to a method for extracting β-damascenone, β-dihydrodamascenone, β-ionone, geranylacetone and other tobacco flavor components in tobacco by using a distillation technology. BACKGROUND

[0002] Tobacco extract, which is rich in flavor components highly consistent with tobacco original flavor, can directly improve the sensory quality of cigarettes and is a key component in the cigarette flavoring system. Distillation technology, which is simple to operate, is a core means for extracting flavor components from tobacco waste. Through this technology, natural distillates of tobacco original flavor can be collected, and flavor components can be enriched through concentration processing, ultimately preparing an extract that retains the original tobacco flavor and embodies the characteristics of tobacco itself.

[0003] Current mainstream tobacco extraction technologies are generally based on distillation processes, among which the method using superheated steam as the single extraction medium is the most widely used. For example, patent CN119523142A discloses a typical process: tobacco raw materials are placed in a dry distillation device, the equipment is preheated, and then superheated steam is introduced, and a distillation and dry distillation combined process is carried out at a temperature of 100-450°C; after collecting the whole process distillate, purification steps such as ethanol precipitation, coarse filtration and membrane filtration are carried out, and finally an extract rich in key flavor components such as heterocyclic, phenolic and furan is obtained. The product presents obvious roasting, caramel and sweet characteristics, which can effectively enhance the sensory aroma performance of cigarettes.

[0004] To further improve resource utilization and ensure the safety of high-temperature reactions, some advanced schemes introduce a mixed medium system of nitrogen gas and superheated steam. As described in patent CN119193236A, this technology uses waste tobacco leaves after steam distillation or solvent extraction of fresh tobacco leaves as raw materials, which are loaded into a distillation-dry distillation device (loading rate controlled at 30-90%) and continuously introduced into the kettle with a mixture of nitrogen gas (100 mL / min) and superheated steam (400 g / h) during the reaction process. The role of nitrogen is to build an inert atmosphere, effectively isolating oxygen in the external air, preventing the raw materials from being oxidized or combusted at high temperatures, and ensuring the stability and controllability of the pyrolysis process. The method uses a programmed temperature rise (10°C / min to 180°C, then 3°C / min to 350°C), selectively collects the distillate at 200-350°C, and then extracts with an organic solvent (using ethyl acetate-n-hexane mixture or petroleum ether), dehydrates and removes the solvent by rotary evaporation to obtain a tobacco flavor. This method not only realizes the high-value utilization of waste tobacco leaves, but also produces a product with rich roasting, caramel and sweet flavors, which is suitable for the flavoring needs of new tobacco products.

[0005] However, although the above two technical paths have slight differences in operation mode, they still have common core limitations: no matter pure superheated water vapor or its mixed system with nitrogen gas, the core mechanism relies on high-temperature pyrolysis. In this process, superheated water vapor not only acts as a mass transfer carrier, but also as an efficient heat carrier, uniformly transferring heat to the material inside, so that the reaction temperature is accurately maintained in the range of 100-450℃. This temperature range exactly promotes the pyrolysis and Maillard reaction of tobacco macromolecular precursor substances such as cellulose, hemicellulose, protein and pectin, generating roasted, caramelized compounds mainly composed of heterocyclic and phenolic compounds. Therefore, the aroma style of the prepared extract is highly concentrated in the roasting characteristics, with strong irritation, lack of floral, fruity and fresh fragrance, which seriously restricts the adaptability and application efficiency of the extract in cigarette flavoring, and it is difficult to meet the demand of modern cigarette products for complex, coordinated and multi-level aroma profile. SUMMARY

[0006] The purpose of the present application is to provide a tobacco extract with lower irritation, weakened roasting characteristics, and both sweet notes and fresh fragrance, which is specifically realized by the following technical solutions:

[0007] A preparation method of a tobacco extract, comprising the following steps: treating tobacco raw materials by a distillation process at 100-130℃, using an inert gas as a blowing carrier, so that volatile components released by the tobacco under the action of heat are captured and dissolved by an organic solvent, to obtain a tobacco pre-extract; after dehydration treatment of the tobacco pre-extract, filtering and concentrating to obtain a tobacco extract.

[0008] As a preference, in the distillation process, the addition amount of tobacco is 1 / 5-3 / 5 of the volume of the distillation bottle.

[0009] As a preference, the inert gas is nitrogen, and the flow rate of the inert gas is 50-500 mL / min.

[0010] As a preference, the dehydration treatment comprises adding anhydrous sodium sulfate to the organic solvent.

[0011] As a preference, the mass ratio of the tobacco pre-extract to the anhydrous sodium sulfate is (2-10):1.

[0012] As a preference, the concentration is one or more of rotary evaporation and nitrogen blowing.

[0013] As a preference, the pore size of the filter membrane used in the filtering is 0.2-0.5 μm.

[0014] A tobacco extract prepared by any one of the above preparation methods.

[0015] As preferred, the tobacco extract comprises beta-damascenone, megastigmatrienone, beta-dihydrodamascenone, beta-ionone, geranylacetone and nicotine.

[0016] The use of the above-mentioned tobacco extract in cigarettes.

[0017] Compared with the prior art, the present application has the following beneficial effects:

[0018] The present application successfully prepares a natural tobacco extract with coordinated aroma and prominent original aroma by precisely regulating the temperature parameters of the distillation process and using inert gas as the only purging medium. The extract is rich in core aroma components such as geranylacetone, beta-damascenone, beta-ionone, beta-dihydrodamascenone, etc. These substances synergistically give the extract excellent aroma quality and sensory performance. Among them, beta-damascenone, as a key component of tobacco characteristic aroma, significantly enhances the fruity note of the extract, bringing obvious sweetness, aroma fullness and tobacco smoothness; beta-dihydrodamascenone effectively softens the smoke, enriches the aroma levels, and enhances the overall delicacy and high-end feel; beta-ionone further enhances the fullness and persistence of the aroma, optimizes the aftertaste after smoking, and synergistically improves the smoothness of the smoke; and the introduction of geranylacetone adds fresh natural green and floral notes to the extract, significantly improving the complexity and naturalness of the aroma. The synergistic effect of these key components highlights the characteristics of the extract derived from tobacco and returning to the original aroma. Performance test results show that the cigarette product added with the extract of the present application exhibits more pure and coordinated aroma quality and more abundant aroma amount, and the undesirable odors such as woody and dry gas are effectively modified and masked, and the smoking strength is also more comfortable and comfortable. What is particularly outstanding is that sample 4 achieved a key breakthrough in sensory evaluation: its irritability was significantly reduced, the roasting characteristics were significantly weakened, there was no sharp feeling during smoking, the heavy roasting odor was significantly reduced, and instead of clear and transparent tobacco original aroma, natural sweet notes and delicate fragrance, the overall smoke was delicate and soft, and the comprehensive sensory quality was significantly improved. This achievement shows that by simply regulating the process temperature, the limitation of traditional pyrolysis process on aroma style can be broken through, and the transformation from single roasting to multi-coordinated original aroma can be realized, providing a natural solution with better performance for tobacco flavoring. BRIEF DESCRIPTION OF DRAWINGS

[0019] The drawings will be briefly introduced as follows:

[0020] Figure 1 Flow chart for preparing waste tobacco extract;

[0021] Figure 2 Schematic diagram of distillation of tobacco waste

[0022] Figure 3Gas chromatography-mass spectrometry of the tobacco extract for sample 1. (A) Total ion current chromatogram, (B) β-damascenone and megastigmatrienone selected ion chromatogram, (C) β-dihydrodamascenone and β-ionone selected ion chromatogram, (D) geranylacetone selected ion chromatogram.

[0023] Figure 4 Purge and trap-gas chromatography-mass spectrometry of sample 2 and sample 3. (A) Total ion current chromatogram, (B) β-damascenone selected ion chromatogram, (C) β-dihydrodamascenone and β-ionone selected ion chromatogram, (D) geranylacetone selected ion chromatogram. DETAILED DESCRIPTION

[0024] The present application will be further described in the following detailed description of specific embodiments. Those skilled in the art will be able to implement the present application based on the description and drawings. Furthermore, the embodiments of the present application described in the following description are only part of the embodiments of the present application, and not all of the embodiments of the present application. Therefore, all other embodiments obtained by those skilled in the art based on the embodiments in the present application without creative labor should be within the scope of protection of the present application.

[0025] Example 1

[0026] A method for preparing a tobacco extract, comprising the following steps:

[0027] Distillation extraction. Accurately weigh 5 g of discarded tobacco sample (sample 1) and uniformly fill it into a 50 mL distillation flask, at this time the sample volume accounts for about 2 / 5 of the total volume of the distillation flask (ensure that the sample is loosely distributed to avoid local accumulation affecting heat and mass transfer). Place the distillation flask in a constant temperature oil bath, and connect the distillation flask branch pipe to the gas flow meter (nitrogen inlet) through a silica gel tube, while the branch pipe end extends to the receiving device (a 50 mL conical flask, pre-added with 30 mL of analytical pure ethanol for absorbing the distillation product). Start the nitrogen generator, adjust the gas flow meter to maintain a stable nitrogen flow rate of 200 mL / min, and continuously introduce it into the distillation flask for 10 min to exclude air in the device (to avoid oxygen interference with the pyrolysis reaction of tobacco components). Turn on the oil bath and set the temperature to 100°C, start timing after the oil bath temperature stabilizes, and maintain constant temperature heating for 120 min; during the distillation process, the nitrogen carries the volatile components of the tobacco into the conical flask, which are absorbed by the ethanol solution to form a tobacco pre-extract mixture.

[0028] Purification and concentration. After the distillation, turn off the oil bath and nitrogen, take out the conical flask, observe and record the volume of the tobacco pre-extract (due to the evaporation of part of the ethanol in the gas flow during the distillation process, the final collection amount is about 20 mL). Add 2 g of pre-dried anhydrous sodium sulfate to the conical flask, place it on the digital shaker, and shake for 5 min to make the anhydrous sodium sulfate fully absorb the moisture in the mixed solution (ensure complete dehydration to avoid water affecting subsequent filtration and concentration). Transfer the mixed solution after shaking to a centrifuge tube and place it in a high-speed centrifuge with a speed of 2000 rpm for 5 min (separate the anhydrous sodium sulfate particles after adsorbing water to avoid clogging the filter membrane). Take out the supernatant after centrifugation, and use a 0.45 μm organic phase filter membrane to perform vacuum filtration (the filter membrane is activated by soaking in ethanol before use), to remove residual small particle impurities, and obtain a clear filtrate. Transfer the clear filtrate to a 50 mL rotary evaporation flask, and connect the rotary evaporator: set the constant temperature water bath temperature to 35°C, the vacuum degree to 0.08-0.09 MPa, and the rotation rate to 60 rpm, and perform vacuum concentration; Observe the liquid volume in the evaporation flask closely, and when the concentration is 2 mL, turn off the rotary evaporator and stop the concentration to obtain the target tobacco extract, which is immediately sealed and stored away from light until GC / MS analysis.

[0029] GC / MS analysis conditions. The chromatographic column is a DB-5MS capillary column (5% phenyl-95% dimethyl polysiloxane as stationary phase, specifications 30 m x 0.25 mm x 0.25 μm, to ensure effective separation of weakly polar components); the carrier gas is high-purity helium (purity 99.999%), using constant flow mode, column flow 1.0 mL / min; the injection port temperature is 250°C (to avoid sample residue or decomposition in the injection port); the injection volume is 2 μL (to ensure moderate signal strength and avoid overload); the injection mode is split injection with a split ratio of 10:1 (to reduce the impact of injection volume fluctuations on separation); the temperature program is as follows: initial temperature 50°C, hold for 2 min (to allow low-boiling-point components in the sample to fully vaporize); then linearly increase the temperature to 250°C at a rate of 5°C / min, hold for 10 min (to ensure that high-boiling-point components are completely eluted and avoid residue). In the mass spectrometry conditions, the ion source is an electron impact ionization source (EI) with an electron energy of 70 eV (standard ionization energy to facilitate obtaining characteristic mass spectra); the ion source temperature is 230°C (to maintain stable operation of the ion source and reduce background interference); the quadrupole rod temperature is 150°C (to ensure ion transmission efficiency and improve detection sensitivity); the interface temperature is 230°C (to match the column outlet temperature and avoid component condensation at the interface); the mass scan range is 35-500 amu (covering the molecular weight range of main tobacco flavor components such as phenols, furans, and esters).

[0030] Please refer to the attached Figure 3It can be observed that the tobacco extract prepared in this application not only contains nicotine, but also is enriched with typical tobacco aroma substances such as β-damascone, megastigmatrienone, β-dihydrodamascone, β-ionone, and geraniol acetone. It can present a distinct tobacco aroma, and has the advantages of low irritation and weakened roasting characteristics. At the same time, it has both sweetness and fragrance, which meets the needs of diverse aromas.

[0031] Example 2

[0032] This embodiment uses the tobacco extract prepared in Example 1 to prepare aroma-rich cigarette paper, including the following steps:

[0033] Two blank cigarette papers, each 5cm × 5cm in size, from the same batch were selected (to ensure substrate consistency and reduce background interference). One paper was used as a blank control sample and labeled as Sample 2; the other was used as a test sample and labeled as Sample 3. For Sample 3, 50μL of the tobacco extract prepared in Example 1 was accurately transferred using a micropipette and evenly dropped onto the surface of the cigarette paper (dropped in three points along the diagonal of the cigarette paper to avoid local liquid accumulation). The sample was then placed in a constant temperature and humidity environment (25±1℃, 50±5%) for 30 minutes to ensure that the extract was fully adsorbed on the surface of the cigarette paper and that there was no solvent residue. After equilibration, the sample was sealed and stored together with Sample 2 for subsequent analysis.

[0034] Purge and trap analysis conditions. High-purity helium (≥99.999%) was used as the purge gas, with a flow rate precisely controlled at 40 mL / min using a gas flow meter to ensure stable gas flow during the purge process and avoid component residue or loss. Purge temperature: 40℃ (temperature controlled by a constant-temperature water bath with an accuracy of ±0.5℃, simulating the normal storage environment of cigarette paper to avoid premature volatilization of components due to high temperatures); trap temperature: room temperature (25±1℃, utilizing the adsorption of volatile components by the trap packing material to achieve enrichment of the target component); desorption temperature: 260℃ (programmed temperature control with a heating rate of 100℃ / min for rapid desorption of the trapped target component and reduction of peak broadening); baking temperature: 280℃ (after desorption, the trap is baked at high temperature to remove residual impurities and avoid cross-contamination); transfer line and six-way valve temperature: both set to 260℃ (matching the desorption temperature to prevent condensation of the target component during transfer and ensure complete entry of the component into the subsequent chromatographic system). Purging time: 30 min (to ensure that the volatile components adsorbed on the surface of the cigarette paper are fully carried to the trap by helium gas, achieving efficient enrichment); Dry purging time: 6 min (after purging, helium gas is continuously introduced to remove residual moisture and low-boiling-point impurities in the trap, improving detection accuracy); Desorption time: 2 min (to ensure that the captured target components are completely desorbed, avoiding component residues affecting quantitative results); Baking time: 10 min (to thoroughly clean the trap, ensuring no memory effect in the next experiment).

[0035] Gas chromatography-mass spectrometry (GC-MS) analysis conditions. For chromatography, the column selection was as follows: a DB-WAX capillary column (stationary phase: polyethylene glycol, dimensions: 60m × 0.32mm × 0.25μm) was used. This column exhibits excellent separation performance for polar and moderately polar components, effectively separating aroma components such as β-damascone and ionone from tobacco extracts. Carrier gas and flow rate: High-purity helium (purity ≥99.999%) was used as the carrier gas, and the column flow rate was controlled at 2mL / min in constant flow mode to ensure peak resolution and retention time stability. Injector temperature: 250℃ (to avoid sample condensation or decomposition at the injection port and ensure complete vaporization of components); split injection with a split ratio of 10:1 (to reduce the impact of injection volume fluctuations on separation performance and avoid column overload); injection volume: automatically injected by the purge-and-trap system, with the injection volume matched to the desorption capacity of the trap, requiring no manual adjustment. Temperature program: Initial temperature 40℃, hold for 5 min (to allow low-boiling-point components to fully vaporize and initially separate, avoiding peak overlap); linearly increase the temperature to 200℃ at a rate of 2.5℃ / min (slow heating to achieve fine separation of medium-boiling-point components); then rapidly increase the temperature to 230℃ at a rate of 20℃ / min, hold for 10 min (to promote complete elution of high-boiling-point components, avoiding column residue). In the mass spectrometry, the ion source type was electron impact ionization (EI), with an electron energy of 70 eV (standard ionization energy, beneficial for obtaining characteristic mass spectra of the target components, facilitating qualitative retrieval); the EI source temperature was 230℃ (to maintain stable operation of the ion source and reduce background ion interference); the transfer line temperature was 240℃ (matched to the column outlet temperature to ensure effective ion transfer to the quadrupole); the quadrupole temperature was 150℃ (to ensure the separation efficiency of the quadrupole and improve mass resolution); and the mass scan range was 35~500 amu (covering the molecular weight range of the main aroma components in tobacco extracts, such as nicotine and megastigmatrienones). Furthermore, this embodiment also used the aforementioned cigarette paper coated with cigarette extracts to prepare cigarettes (sample 4), and the cigarette preparation employed existing technology.

[0036] Comparative Example 1

[0037] The difference between this comparative example and the cigarettes prepared in Example 2 is that the cigarette paper surface was not coated with the tobacco extract prepared in this application.

[0038] Performance testing

[0039] To verify the effect of tobacco extract on improving the smoking quality of cigarettes, this study conducted sensory evaluation tests on cigarettes containing the tobacco extract prepared in Example 2 (experimental group) and blank cigarettes without the extract (comparative example 1, control sample). The evaluation experiment was conducted by a panel of 10 professionally trained and certified sensory evaluators. The two cigarettes were comprehensively evaluated using a blind tasting method in a standard tasting environment with constant temperature (22±1℃) and constant humidity (60±5%RH). The evaluation dimensions focus on the core sensory indicators of cigarettes, specifically including: aroma quality (purity, harmony, and style characteristics of aroma), aroma quantity (fullness and intensity of aroma release), off-flavors (degree of off-flavors other than the natural aroma of tobacco), strength (physiological impact of smoke on the mouth and throat), irritation (spiciness and stinging sensation of smoke on the mucous membranes), and aftertaste (comfort and cleanliness of the mouth after smoking). Each dimension is scored independently on a scale of 1 to 9 (1 being the worst and 9 being the best). The final result is the average score of 10 evaluators. The specific data is shown in Table 1.

[0040] Table 1. Evaluation results of the control sample and the cigarette sample with added tobacco extract.

[0041]

[0042] When the waste tobacco extract prepared in this invention is applied to cigarette paper (corresponding to sample 4), compared with the control cigarette sample without the extract, it shows significant optimization in core sensory indicators: the aroma is purer and more harmonious, the aroma is fuller and more abundant, the off-flavors (such as woody and burnt smells) are effectively masked, and the strength is more in line with the needs of comfortable smoking; most importantly, sample 4 successfully achieved the goal of lower irritation and weakened roasting characteristics - there is no obvious sharpness when smoking, the original strong roasting flavor is greatly reduced, while the natural tobacco aroma is clearly revealed, and it also has a natural sweetness and a light and elegant fragrance. The smoke is more delicate and soft overall, which comprehensively improves the smoking quality and sensory comfort of cigarettes.

Claims

1. A method for preparing a tobacco extract, characterized in that, Includes the following steps: Tobacco raw materials are processed using a distillation process at 100-130℃, with an inert gas as the purge carrier, so that the volatile components released by the tobacco under heat are captured and dissolved by an organic solvent to obtain a tobacco pre-extract; the tobacco pre-extract is then dehydrated, filtered, and concentrated to obtain a tobacco extract.

2. The method for preparing a tobacco extract according to claim 1, characterized in that, In the distillation process, the amount of tobacco added is 1 / 5 to 3 / 5 of the volume of the distillation flask.

3. The method for preparing a tobacco extract according to claim 1, characterized in that, The inert gas is nitrogen, and the flow rate of the inert gas is 50~500 mL / min.

4. The method for preparing a tobacco extract according to claim 1, characterized in that, The dehydration process includes adding anhydrous sodium sulfate to an organic solvent.

5. The method for preparing a tobacco extract according to claim 4, characterized in that, The mass ratio of the tobacco pre-extract to the anhydrous sodium sulfate is (2~10):

1.

6. The method for preparing a tobacco extract according to claim 1, characterized in that, The concentration is achieved through one or more methods, such as rotary evaporation and nitrogen blowing.

7. The method for preparing a tobacco extract according to claim 1, characterized in that, The filtration process uses a filter membrane with a pore size of 0.2~0.5μm.

8. A tobacco extract, characterized in that, It is prepared by the preparation method according to any one of claims 1 to 7.

9. A tobacco extract according to claim 8, characterized in that, The tobacco extract includes β-damascone, megastigmatrienone, β-dihydrodamascone, β-ionone, geraniol acetone, and nicotine.

10. The application of a tobacco extract as described in claim 8 in cigarettes.

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