Preparation method and application of brazilian tobacco absolute

Abstract

The application discloses a preparation method and application of a Brazil tobacco leaf absolute, relates to the field of tobacco flavors, and comprises the following steps: raw material treatment, enzyme treatment, continuous countercurrent ultrasonic extraction, freeze-drying, dewaxing to obtain a tobacco leaf dewaxing product, three-stage molecular distillation refining, and selection of one or more compounds in light components of each stage of distillation as the Brazil tobacco leaf absolute. The application further discloses a composition containing the Brazil tobacco leaf absolute and application of the Brazil tobacco leaf absolute or the composition in cigarettes. The Brazil tobacco leaf absolute and the absolute composition provided by the application effectively improve the stability of the Brazil tobacco leaf absolute and the stability of the Brazil tobacco leaf absolute in finished cigarettes, and the Brazil tobacco leaf absolute can be applied to cigarettes as a "sweet and clean flavor" flavor base module to increase the amount of aroma, improve the quality of aroma, highlight the sweet and clean flavor style, cover up the odor, improve the comfort, and is suitable for high-quality cigarettes.

Description

Technical Field

[0001] This invention relates to the field of tobacco flavoring technology, and particularly to the field of tobacco leaf purified oil, specifically a method for preparing and applying Brazilian tobacco leaf purified oil. Background Technology

[0002] In cigarette production, the addition of flavorings and fragrances can effectively improve the taste and aroma of cigarettes, enhance tobacco fragrance, and increase satisfaction. Since Brazilian tobacco extract is a natural flavoring agent, its safety is assured. Furthermore, research has found that using Brazilian tobacco extract as an endogenous tobacco additive has a unique role in supplementing characteristic tobacco aromas, enhancing the natural tobacco fragrance, and improving the taste of tobacco. However, as an important component of blended tobacco with a sweet aroma profile, there is relatively little research in the industry on the preparation of Brazilian tobacco extract, and precise analysis of the aroma components in the extract and the preparation of purified oil are even rarer. Due to technical limitations, extensive selection of purified oil samples and concentration gradient experiments are required in the laboratory, significantly lengthening the research and development cycle, hindering rapid market response, and preventing precise research and development. At the same time, in the development and maintenance of cigarette blend formulations, there are also cases where the compatibility of some Brazilian tobacco formulations is not high, failing to fully utilize each style of tobacco, resulting in surplus of some varieties and grades of tobacco that are ultimately discarded.

[0003] In existing technologies, the preparation of tobacco extracts generally involves direct extraction from re-dried low-grade tobacco leaves. However, this method makes it difficult to guarantee the quality of the tobacco leaves. Extraction methods typically employ traditional solvent extraction and supercritical fluid extraction. While traditional solvent extraction can effectively enhance the aroma, limitations in extraction efficiency and solvent residue can lead to unpleasant odors, increased roughness, dryness, and astringency on the tongue. Although the widely used supercritical fluid extraction technology improves the purity of the extract, it does not selectively separate aroma-producing components, retaining some substances detrimental to the taste of cigarettes. Summary of the Invention

[0004] This invention addresses the limitations of existing technologies in the preparation of tobacco extracts and tobacco leaf oils, which lead to negative effects such as the inability to selectively separate aroma components and the retention of substances detrimental to cigarette flavor. Furthermore, existing technologies for utilizing Brazilian tobacco leaf oils suffer from deficiencies such as inaccurate extraction and research, slow market response, low adaptability, and inability to fully utilize their rich aroma. Therefore, this invention provides a method for preparing and applying Brazilian tobacco leaf oils.

[0005] This invention is achieved using the following techniques:

[0006] This invention provides a method for preparing purified oil from Brazilian tobacco leaves, comprising the following steps:

[0007] a: Raw material processing

[0008] Remove the stems from the Brazilian BOC-YN raw tobacco leaves.

[0009] b: Enzyme treatment

[0010] Select an acidic protease, neutral protease, cellulase, pectinase, amylase, or a complex enzyme including at least two of the above at a concentration of 0.03wt% to 1.0wt%, preferably at a concentration of 0.03wt% to 0.07wt%. Soak the tobacco leaves treated in step a in the enzyme preparation reaction solution at 40 to 60°C for 0.5 to 2 minutes, preferably at 40 to 55°C for 1 minute, to ensure that the tobacco leaves are in full contact with the enzyme preparation without affecting subsequent treatments.

[0011] After soaking, the tobacco leaves are hung to stand and dehydrate until the moisture content is less than or equal to 25%. The excess enzyme reaction solution is drained from the tobacco leaves. The hanging and standing dehydration treatment time is 0.5 to 1 hour, preferably 40 minutes, which is conducive to the full contact between the tobacco leaves and the enzyme reaction solution.

[0012] After hanging and dehydrating, the tobacco leaves are centrifuged until the moisture content is 14% to 19%. The centrifugation speed is 500 to 700 r / min and the time is 2 to 5 min. Preferably, the centrifugation speed is 600 r / min and the time is 3 min. Controlling the appropriate centrifugation speed and time ensures the stability of the physical properties (e.g., flexibility) of the tobacco leaves.

[0013] The centrifuged tobacco leaves are stored for aging to allow the enzyme preparation to fully react with the tobacco leaves. The storage process temperature is 30~60℃, the ambient humidity is 60%~80%, and the time is 2~3h. Further, the ambient humidity is 60%~70%. Preferably, the storage process temperature is 50℃, the ambient humidity is 65%, and the time is 2h. The stored tobacco leaves are then subjected to enzyme inactivation treatment.

[0014] In the enzyme preparation soaking process, if the tobacco leaves are soaked in the enzyme preparation reaction solution for too short a time, the tobacco leaves will not be able to fully contact the enzyme preparation reaction solution; if the soaking time is too long, the moisture content of the tobacco leaves will be too high, which will have an adverse effect on subsequent processing. Soaking time is also too long and will affect the content of chemical components (such as nicotine) in the tobacco leaves, making it difficult to control the quality of the tobacco leaves. When using acidic protease, the concentration of the enzyme preparation reaction solution is 0.05 wt%, the pH value of the enzyme preparation reaction solution is 2.0~5.0, and the soaking temperature is 45~55℃; when using neutral protease, the concentration of the enzyme preparation reaction solution is 0.07 wt%, the pH value of the enzyme preparation reaction solution is 6.0~7.5, and the soaking temperature is 55℃; when using pectinase, the concentration of the enzyme preparation reaction solution is 0.07 wt%, the pH value of the enzyme preparation reaction solution is 6.0, and the soaking temperature is 50℃; when using amylase, the concentration of the enzyme preparation reaction solution is 0.03 wt%, the pH value of the enzyme preparation reaction solution is 7.0, and the soaking temperature is 50℃.

[0015] c: Continuous countercurrent ultrasonic extraction

[0016] The tobacco leaves obtained in step b are pulverized into 40-120 mesh powder and fed into the leaching chamber at a rate of 0.1-1.0 kg / 10 min, preferably 0.5 kg / 10 min. The main unit and ultrasonic generator are turned on, and the temperature is adjusted to 60-100℃, preferably 80℃. The ratio of tobacco powder to liquid is 1:(2-8), preferably 1:5 by mass. After running from the bottom of the leaching chamber for 0.2-1 hour, the liquid outlet valve is adjusted to release the liquid evenly. The extraction time is 0.6 hours. The solvent addition flow rate is controlled to maintain the liquid level balance in the leaching chamber. When the continuous countercurrent ultrasonic extraction reaches 10-30 minutes, preferably 20 minutes, 50% ethanol with a concentration of 5% (5% of the tobacco mass) is added to complete the first stage of continuous countercurrent ultrasonic extraction. When the continuous countercurrent ultrasonic extraction reaches a total of 20-60 minutes, preferably 50 minutes, the second stage of continuous countercurrent ultrasonic extraction is completed at 30 minutes. The production process is then stopped, the continuous countercurrent ultrasonic extraction is completed, the residue is discharged, and the leachate is obtained.

[0017] d: freeze-drying

[0018] The extract obtained in step c was freeze-dried under vacuum to obtain crude extract of Brazilian tobacco leaves.

[0019] e: Dewaxing

[0020] Add 95% ethanol (i.e., ethanol concentration of 95%) at a mass ratio of 1:(10~15) to the crude extract of Brazilian tobacco obtained in step d, and stir uniformly at 22~25℃ for 1~2h. Preferably, the mass ratio of 95% ethanol is 1:10, and stir uniformly at 25℃ for 2h. Then centrifuge. Take the supernatant and refrigerate it at 0~4℃ for 8~12h. Preferably, the refrigeration time is 12h. Centrifuge again to obtain a secondary supernatant, which is then concentrated by rotary evaporation on a rotary evaporator until no obvious solvent is evaporated, to obtain the dewaxed tobacco product.

[0021] f: Distillation

[0022] Distillation temperature is the most important factor affecting the extraction, separation and refining effect of tobacco. The components in tobacco extract have different boiling points under high vacuum, and the fractional yield and the relative content of aroma components obtained at different distillation temperatures will vary greatly.

[0023] The dewaxed tobacco product obtained in step d is purified by three-stage molecular distillation. The dewaxed tobacco product is subjected to first-stage molecular distillation at 115–135°C, with a vacuum of 0.5–1.5 mbar, a scraper rotation speed of 250–350 rpm, and a feed rate of 400–600 g / h. The heavy phase from the first-stage distillation fraction is then subjected to second-stage molecular distillation at 135–155°C, with a vacuum of 0.05–0.1 mbar, a scraper rotation speed of 200–400 rpm, and a feed rate of 600–800 g / h. The heavy phase from the secondary distillation product is subjected to tertiary molecular distillation at 150-170℃, with a vacuum of 0.03-0.08 mbar, a scraper rotation speed of 200-400 rpm, and a feed rate of 700-900 g / h. The light components from the primary, secondary, and tertiary distillations are obtained. One or more of the light components from each distillation stage are selected as Brazilian tobacco pure oil. Preferably, the distillation component with the best sensory evaluation is selected as Brazilian tobacco pure oil. Specifically, the light component from the secondary distillation stage is selected as Brazilian tobacco pure oil.

[0024] Preferably, the molecular distillation start temperature is 125℃, the temperature for the first-stage molecular distillation is 125℃, the vacuum degree is 0.5mbar, the scraper rotation speed is 300rpm, and the feed rate is 600g / h; the temperature for the second-stage molecular distillation is 145℃, the vacuum degree is 0.05mbar, the scraper rotation speed is 300rpm, and the feed rate is 800ml / h; the temperature for the third-stage molecular distillation is 160℃, the vacuum degree is 0.03mbar, the scraper rotation speed is 300rpm, and the feed rate is 900g / h.

[0025] This invention provides a composition containing Brazilian tobacco pure oil, comprising Brazilian tobacco pure oil, and further comprising any one or more of the following: limonene, isoamyl isovalerate, 1% phenylethanol, menthone, benzyl alcohol, linalool, anisaldehyde, triacetin, dihydrodamascone, perilla frutescens, benzyl benzoate, 1% damascone, 1% phenylethanol, 1% ethyl acetate, 1% stigmasterone, 10% carotenoid degradation products, 1% iris extract, propylene glycol, and glycerol. Wherein, 1% phenylethanol represents a diluted concentration of 1% phenylethanol; similarly, 1% damascone, 1% phenylethanol, 1% ethyl acetate, 1% stigmasterone, 10% carotenoid degradation products, and 1% iris extract all represent their diluted concentrations. By combining aroma substances with Brazilian tobacco pure oil, the aroma intensity can be increased, the aroma quality improved, a "sweet and clean" aroma style highlighted, impurities masked, and comfort enhanced.

[0026] Preferred components include 5-10 parts Brazilian tobacco pure oil, 0.05-0.1 parts limonene, 0.05-0.1 parts isoamyl isovalerate, 0.2-0.4 parts 1% phenylethanol, 1-2 parts menthone, 0.03-0.06 parts benzyl alcohol, 0.005-0.01 parts linalool, 0.005-0.01 parts anisaldehyde, 0.2-0.4 parts triacetin, 5-8 parts dihydrodamascone, 0.1-0.2 parts perilla scape, and 0. 1-0.2 parts benzyl benzoate, 0.14-0.28 parts 1% damascone, 0.2-0.4 parts 1% phenylethanol, 0.05-0.1 parts 1% ethyl acetate, 0.01-0.03 parts 1% megastigmatrienone, 0.3-0.6 parts 10% carotenoid degradation products, 0.15-0.3 parts 1% iris extract, 3-8.2 parts dihydrodamascone, 40-60 parts propylene glycol, 27-35 parts glycerol, wherein the parts are by weight.

[0027] Preferably, the composition includes 8 parts Brazilian tobacco pure oil, 0.05 parts limonene, 0.05 parts isoamyl isovalerate, 0.2 parts 1% phenethyl alcohol, 1 part menthone, 0.03 parts benzyl alcohol, 0.01 parts linalool, 0.01 parts anisaldehyde, 0.2 parts triacetin, 5 parts dihydrodamascone, 0.2 parts perilla stigma, 0.2 parts benzyl benzoate, 0.14 parts 1% damascone, 0.2 parts 1% phenethyl alcohol, 0.05 parts 1% ethyl acetate, 0.01 parts 1% megastigmatrienone, 0.3 parts 10% carotenoid degradation product, 0.15 parts 1% iris extract, 5 parts dihydrodamascone, 47 parts propylene glycol, and 32.2 parts glycerol, wherein the parts are by weight.

[0028] This invention provides the application of Brazilian tobacco leaf pure oil in cigarettes. The cigarettes selected have high sensory quality. Brazilian tobacco leaf pure oil is used as the flavor base of the "sweet and refreshing" tobacco functional segment in the proprietary product. It can also replace the tobacco pure oil module in the original flavoring or be directly added to the tobacco shreds.

[0029] This invention provides the application of a composition containing Brazilian tobacco leaf extract in cigarettes. The composition containing Brazilian tobacco leaf extract is used as the flavor base of the "sweet and refreshing" tobacco functional segment in proprietary products, and can also replace the tobacco extract module in the original flavoring, or be directly added to tobacco shreds.

[0030] The present invention provides the application of a composition containing Brazilian tobacco leaf purified oil in cigarettes, wherein the amount of Brazilian tobacco leaf purified oil added is 0.001%~0.005%.

[0031] Preferably, the amount of Brazilian tobacco pure oil added to the blank cigarette is 0.003%.

[0032] Compared with the prior art, the present invention has the following beneficial effects:

[0033] This invention discloses a method for preparing and applying Brazilian tobacco leaf purified oil. The invention uses discarded Brazilian tobacco leaves with poor leaf compatibility (generally referring to a single type of tobacco that, when its content is increased, exhibits a high aroma and quantity, but also brings off-flavors, irritation, and reduced strength) as the research object. First, the tobacco leaves are enzymatically treated to initially improve their quality. Then, a crude extract of the tobacco leaves is obtained using continuous countercurrent ultrasonic extraction. The crude extract is then dewaxed and further separated using molecular distillation under different preset separation conditions to obtain a high-quality, highly stable Brazilian tobacco leaf purified oil suitable for cigarettes. Aroma components with a sweet and refreshing aroma are also screened out.

[0034] By combining the stylistic characteristics of Brazilian tobacco leaves, this invention addresses the practical problems in tobacco formulation development and maintenance. Using preset sensory requirements as the evaluation index, the purified oil distillation components are separated according to the molecular free path from low to high. This determines that the components provided by this invention are the optimal formulation. At the same time, it effectively screens out the molecular distillation components that best meet the requirements for targeted aroma enhancement, determines their compound ratio and dosage, and provides a theoretical basis for clarifying the sensory impact of aroma-enhancing components.

[0035] The Brazilian tobacco leaf purified oil and purified oil composition provided by this invention effectively improve the stability of Brazilian tobacco leaf purified oil and its stability in finished cigarettes. When used as a "sweet aroma" flavor base module in cigarettes, it can increase the aroma volume, improve the aroma quality, highlight the sweet aroma style, mask off impurities, and improve comfort, making it suitable for high-quality cigarettes.

[0036] This invention combines the selected distilled components with "sweet aroma" and "caramelized sweet aroma" characteristics, and uses natural or synthetic fragrance raw materials as aids to create a fragrance base module that simultaneously possesses the aroma characteristics of "sweet aroma" and "caramelized sweet aroma".

[0037] When the flavoring formula of the Brazilian tobacco leaf pure oil provided by this invention is applied to cigarettes, it can significantly improve the sensory quality of cigarettes, effectively remove the burnt smell in the smoke, and produce a clear, rich aroma with a comfortable taste. It also adds the natural aroma of tobacco, as well as a sweet and refreshing aroma, and a hay-like aroma, which are not found in cigarettes containing other additives. Implementation

[0038] Specific embodiments of the present invention will be described below. Example 1

[0039] The present invention discloses a method for preparing Brazilian tobacco leaf purified oil, comprising the following steps:

[0040] a: Raw material processing

[0041] Remove the stems from the Brazilian BOC-YN raw tobacco leaves.

[0042] b: Enzyme treatment

[0043] The tobacco leaves treated in step a are soaked in the enzyme preparation reaction solution at 55°C for 1 minute to ensure that the tobacco leaves are in full contact with the enzyme preparation without affecting subsequent treatments.

[0044] Hang the soaked tobacco leaves to dehydrate for 40 minutes.

[0045] The tobacco leaves after hanging and dehydration are centrifuged at a speed of 600 r / min for 3 min to ensure the stability of the physical properties (such as flexibility) of the tobacco leaves.

[0046] The centrifuged tobacco leaves are stored for aging to allow the enzyme preparation to fully react with the tobacco leaves. The storage process is carried out at a temperature of 50°C, an ambient humidity of 65%, and a time of 2 hours. The stored tobacco leaves are then subjected to enzyme inactivation treatment.

[0047] c: Continuous countercurrent ultrasonic extraction

[0048] The tobacco leaves obtained in step b are pulverized into 80-mesh powder and fed into the leaching chamber at a rate of 0.5 kg / 10 min. The main unit and ultrasonic generator are turned on, and the temperature is adjusted to 80°C. The ratio of tobacco powder to liquid is 1:5. After running from the bottom of the leaching chamber for 0.6 h, the liquid outlet valve is adjusted to release the liquid evenly and maintain the liquid level balance in the leaching chamber. When the continuous countercurrent ultrasonic extraction reaches 20 min, 5% ethanol with a concentration of 50% is added, accounting for 5% of the mass of tobacco dust, to complete the first stage of continuous countercurrent ultrasonic extraction. When the continuous countercurrent ultrasonic extraction reaches a total of 50 min, that is, the second stage of continuous countercurrent ultrasonic extraction for 30 min, the production process is stopped, the continuous countercurrent ultrasonic extraction is completed, the slag is discharged, and the leachate is obtained.

[0049] d: freeze-drying

[0050] The extract obtained in step c was freeze-dried under vacuum to obtain crude extract of Brazilian tobacco leaves.

[0051] e: Dewaxing

[0052] Add 95% ethanol at a mass ratio of 1:10 to the crude extract of Brazilian tobacco obtained in step d and stir evenly at 25°C for 2 hours, then centrifuge. Take the supernatant and refrigerate it in a refrigerator at 0-4°C for 12 hours. Centrifuge again to obtain a secondary supernatant, which is then concentrated by rotary evaporation until no obvious solvent is evaporated, thus obtaining the dewaxed tobacco product.

[0053] f: Distillation

[0054] The dewaxed tobacco product obtained in step d was purified by three-stage molecular distillation. The dewaxed tobacco product was subjected to first-stage molecular distillation at 125℃ with a vacuum of 0.5 mbar, a scraper speed of 300 rpm, and a feed rate of 600 g / h. The heavy phase of the first-stage distillation product was subjected to second-stage molecular distillation at 145℃ with a vacuum of 0.05 mbar, a scraper speed of 300 rpm, and a feed rate of 800 g / h. The heavy phase of the second-stage distillation product was subjected to third-stage molecular distillation at 160℃ with a vacuum of 0.03 mbar, a scraper speed of 300 rpm, and a feed rate of 900 g / h. The light fraction from the second-stage distillation was used as Brazilian tobacco oil. Example 2

[0055] The present invention discloses a method for preparing Brazilian tobacco leaf purified oil, comprising the following steps:

[0056] Steps a to e are the same as in Example 1. In step f, except that the light fraction of the first distillation is taken as the purified oil of Brazilian tobacco leaves, the other steps are the same as in Example 1. Example 3

[0057] The present invention discloses a method for preparing Brazilian tobacco pure oil, comprising the following steps: steps a to e are the same as in Example 1; in step f, except that the light fraction of the third distillation is taken as Brazilian tobacco pure oil, the remaining steps are the same as in Example 1.

[0058] The Brazilian tobacco oil obtained in Examples 1-3 was added to blank cigarettes at a concentration of 0.003%, with a blank control group as a comparative example. The sensory quality was evaluated according to the Chinese cigarette sensory style evaluation method, referring to the cigarette sensory quality evaluation criteria in "YC / T497-2014 - Sensory Evaluation Method for Chinese Cigarette Style", including: aroma style, flavor style, comfort characteristics, and smoke characteristics. The results are shown in the table below.

[0059]

[0060] Based on comprehensive statistical scoring, compared with the blank group, Example 1 achieved the highest overall evaluation across all indicators. The resulting purified oil exhibited a light and hay-like aroma, with a clear and bright fragrance, a moderate to high aroma intensity, a relatively full and rounded smoke appearance, moderate transparency, and a relatively soft and delicate aroma. Therefore, Example 1 (i.e., using the light fraction from secondary distillation as Brazilian tobacco purified oil) was selected for comparison of the content of major aroma compounds before and after molecular distillation. The results are shown in the table below:

[0061]

[0062] Comparison of aroma components before and after distillation revealed that the relative contents of γ-butyrolactone, solanone, megastigmatrienone, and dihydroactinolone all increased by more than four times. These substances have typical tobacco aroma characteristics, with a sweet and refreshing aroma that can effectively enrich the tobacco aroma and improve the satisfaction during smoking. Therefore, the pure oil of Brazilian tobacco leaves obtained by using Brazilian BOC-YN raw tobacco leaves as raw material through enzyme treatment, continuous countercurrent ultrasonic extraction technology, dewaxing process, and molecular distillation technology has good performance when used as the "sweet and refreshing aroma" component. Example 4

[0063] The composition containing Brazilian tobacco pure oil disclosed in this invention comprises 8 parts Brazilian tobacco pure oil, 0.05 parts limonene, 0.05 parts isoamyl isovalerate, 0.2 parts 1% phenethyl alcohol, 1 part menthone, 0.03 parts benzyl alcohol, 0.01 parts linalool, 0.01 parts anisaldehyde, 0.2 parts triacetin, 5 parts dihydrodamascone, 0.2 parts perilla stigma, 0.2 parts benzyl benzoate, 0.14 parts 1% damascone, 0.2 parts 1% phenethyl alcohol, 0.05 parts 1% ethyl acetate, 0.01 parts 1% megastigmatrienone, 0.3 parts 10% carotenoid degradation product, 0.15 parts 1% iris extract, 5 parts dihydrodamascone, 47 parts propylene glycol, and 32.2 parts glycerol. Example 5

[0064] The composition containing Brazilian tobacco pure oil disclosed in this invention comprises 5 parts Brazilian tobacco pure oil, 0.05 parts limonene, 0.05 parts isoamyl isovalerate, 0.2 parts 1% phenethyl alcohol, 1 part menthone, 0.03 parts benzyl alcohol, 0.01 parts linalool, 0.01 parts anisaldehyde, 0.2 parts triacetin, 5 parts dihydrodamascone, 0.2 parts perilla stigma, 0.2 parts benzyl benzoate, 0.14 parts 1% damascone, 0.2 parts 1% phenethyl alcohol, 0.05 parts 1% ethyl acetate, 0.01 parts 1% megastigmatrienone, 0.3 parts 10% carotenoid degradation product, 0.15 parts 1% iris extract, 5 parts dihydrodamascone, 50 parts propylene glycol, and 32.2 parts glycerol. Example 6

[0065] The composition containing Brazilian tobacco pure oil disclosed in this invention comprises 8 parts Brazilian tobacco pure oil, 0.05 parts limonene, 0.05 parts isoamyl isovalerate, 0.2 parts 1% phenethyl alcohol, 1 part menthone, 0.03 parts benzyl alcohol, 0.01 parts linalool, 0.01 parts anisaldehyde, 0.2 parts triacetin, 5 parts dihydrodamascone, 0.2 parts perilla stigma, 0.2 parts benzyl benzoate, 0.14 parts 1% damascone, 0.2 parts 1% phenethyl alcohol, 0.05 parts 1% ethyl acetate, 0.01 parts 1% megastigmatrienone, 0.3 parts 10% carotenoid degradation product, 0.15 parts 1% iris extract, 8.2 parts dihydrodamascone, 47 parts propylene glycol, and 29 parts glycerol. Example 7

[0066] The composition containing Brazilian tobacco pure oil disclosed in this invention comprises 10 parts Brazilian tobacco pure oil, 0.05 parts limonene, 0.05 parts isoamyl isovalerate, 0.2 parts 1% phenethyl alcohol, 1 part menthone, 0.03 parts benzyl alcohol, 0.01 parts linalool, 0.01 parts anisaldehyde, 0.2 parts triacetin, 5 parts dihydrodamascone, 0.2 parts perilla stigma, 0.2 parts benzyl benzoate, 0.14 parts 1% damascone, 0.2 parts 1% phenethyl alcohol, 0.05 parts 1% ethyl acetate, 0.01 parts 1% megastigmatrienone, 0.3 parts 10% carotenoid degradation product, 0.15 parts 1% iris extract, 5 parts dihydrodamascone, 45 parts propylene glycol, and 32.2 parts glycerol.

[0067] The stability of the purified oil compositions in Examples 4-7 was observed after standing for 1 week. The control group was a blank control. The specific observation results were that the control group showed obvious stratification, the purified oil composition in Example 4 was stable, the purified oil composition in Example 5 showed slight stratification, the purified oil composition in Example 6 showed slight stratification, and the purified oil composition in Example 7 showed obvious stratification. Example 8

[0068] The application of a Brazilian tobacco leaf oil-containing composition in cigarettes disclosed in this invention includes the following steps in its preparation method:

[0069] Brazilian tobacco pure oil was prepared according to the method in Example 1. Eight parts of Brazilian tobacco pure oil were mixed with 0.05 parts limonene, 0.05 parts isoamyl isovalerate, 0.2 parts 1% phenylethanol, 1 part menthone, 0.03 parts benzyl alcohol, 0.01 parts linalool, 0.01 parts anisaldehyde, 0.2 parts triacetin, 5 parts dihydrodamascone, 0.2 parts perilla stigma, 0.2 parts benzyl benzoate, 0.14 parts 1% damascone, 0.2 parts 1% phenylethanol, 0.05 parts 1% ethyl acetate, 0.01 parts 1% megastigmatrienone, 0.3 parts 10% carotenoid degradation product, 0.15 parts 1% iris extract, 5 parts dihydrodamascone, 47 parts propylene glycol, and 32.2 parts glycerol to obtain a Brazilian tobacco pure oil composition. This composition was then added to blank cigarettes at a concentration of 0.003% to produce cigarettes. Example 9

[0070] In the preparation of Brazilian tobacco oil in Example 8, step c, continuous countercurrent ultrasonic extraction, was replaced by traditional solvent extraction. All other steps were completely consistent with those in Example 8, and cigarettes were produced. Example 10

[0071] In the preparation of Brazilian tobacco pure oil in Example 8, step e (dewaxing) is omitted. The crude extract of Brazilian tobacco obtained in step d is directly purified by three-stage molecular distillation. The remaining steps are completely consistent with those in Example 8, and cigarettes are produced. Example 11

[0072] In the preparation of Brazilian tobacco pure oil in Example 8, step f, distillation, was not performed. The obtained tobacco dewaxing product was directly mixed, and the remaining steps were completely consistent with those in Example 8 to produce cigarettes. Example 12

[0073] In the preparation of Brazilian tobacco pure oil in Example 8, the light fraction of primary distillation was used as Brazilian tobacco pure oil, and the remaining steps were completely consistent with those in Example 8, and cigarettes were made. Example 13

[0074] In the preparation of Brazilian tobacco pure oil in Example 8, the light component of the third distillation was used as Brazilian tobacco pure oil, and the remaining steps were completely consistent with those in Example 8, and cigarettes were made.

[0075] A mixture of 0.05 parts limonene, 0.05 parts isoamyl isovalerate, 0.2 parts 1% phenethyl alcohol, 1 part menthone, 0.03 parts benzyl alcohol, 0.01 parts linalool, 0.01 parts anisaldehyde, 0.2 parts triacetin, 5 parts dihydrodamascone, 0.2 parts perilla sap, 0.2 parts benzyl benzoate, 0.14 parts 1% damascone, 0.2 parts 1% phenethyl alcohol, 0.05 parts 1% ethyl acetate, 0.01 parts 1% megastigmatrienone, 0.3 parts 10% carotenoid degradation products, 0.15 parts 1% iris extract, 5 parts dihydrodamascone, 10 parts propylene glycol, and 32.2 parts glycerol was used to prepare a composition free of Brazilian tobacco oil. This composition served as a blank control group and was used to manufacture cigarettes.

[0076] Thirty-three professional sensory evaluators were randomly selected to conduct sensory quality evaluations on the cigarettes obtained in Examples 8-13 and Comparative Example 1 according to the sensory style evaluation method for Chinese-style cigarettes. The sensory quality evaluation criteria for cigarettes in "YC / T497-2014 Sensory Evaluation Method for Chinese-style Cigarettes" were referenced, including: aroma style, flavor style, comfort characteristics, and smoke characteristics. The sensory quality evaluation scores are shown in the table below.

[0077]

[0078] The data in the table above shows the sensory quality evaluation scores of the cigarettes obtained in Examples 8-13, indicating that the sensory quality of the cigarettes in the embodiments of the present invention has been significantly improved. Among them, Example 8 has the highest sensory quality score and the best flavor. Based on the specific feedback from professional sensory evaluators, the sensory experience of the cigarette obtained in Example 8 during smoking is mainly reflected in: a relatively obvious tobacco aroma and a sweet, refreshing fragrance, as well as a hint of hay, and a delicate and smooth smoke. Simultaneously, the refining process through molecular distillation effectively removes the burnt or scorched smell from the smoke, resulting in a clear, rich aroma and a comfortable taste.

[0079] The scope of protection claimed by this invention is not limited to the specific embodiments described above. Moreover, for those skilled in the art, this invention can have various modifications and alterations. Any modifications, improvements, and equivalent substitutions made within the concept and principles of this invention should be included within the scope of protection of this invention.

Claims

1. A method for preparing purified oil from Brazilian tobacco leaves, characterized in that: Includes the following steps: a: Raw material processing Remove the stems from Brazilian BOC-YN raw tobacco leaves; b: Enzyme treatment The tobacco leaves treated in step a are soaked in an enzyme preparation reaction solution at a temperature of 40-60℃ for 0.5-2 minutes; the soaked tobacco leaves are hung to stand and dehydrate until the moisture content is less than or equal to 25%, and the hanging and standing dehydration treatment time is 40 minutes to 1 hour; the hung and dehydrated tobacco leaves are centrifuged until the moisture content is 14%-19%; the centrifuged tobacco leaves are stored for aging, and the stored tobacco leaves are subjected to enzyme inactivation treatment; c: Continuous countercurrent ultrasonic extraction The tobacco leaves obtained in step b are pulverized into 40-120 mesh powder and fed into the leachation chamber at a rate of 0.1-1.0 kg / 10 min. The temperature is adjusted to 60-100℃, and the ratio of tobacco powder to liquid is 1:(2-8). After running from the bottom of the leachation chamber for 0.2-1 h by mass, the liquid is discharged evenly by adjusting the outlet valve. When the continuous countercurrent ultrasonic extraction reaches 10-30 min, 5% ethanol (5% of the tobacco powder mass) is added to complete the first stage of continuous countercurrent ultrasonic extraction. When the continuous countercurrent ultrasonic extraction reaches a total of 20-60 min, the production process is stopped, the continuous countercurrent ultrasonic extraction is completed, the residue is discharged, and the leachate is obtained. d: freeze-drying The extract obtained in step c was freeze-dried under vacuum to obtain crude extract of Brazilian tobacco leaves; e: Dewaxing Add 95% ethanol at a mass ratio of 1:(10~15) to the crude extract of Brazilian tobacco obtained in step d and stir at 22~25℃ for 1~2h, then centrifuge; take the supernatant and refrigerate at 0~4℃ for 8~12h, then centrifuge again to obtain a secondary supernatant. Concentrate the supernatant until no obvious solvent is distilled off to obtain the dewaxed tobacco product. f: Distillation The tobacco dewaxed product obtained in step e is purified by three-stage molecular distillation. The tobacco dewaxed product is subjected to one-stage molecular distillation at 115~135℃. The vacuum degree during distillation is 0.5~1.5mbar, the scraper rotation speed is 250~350rpm, and the feed rate is 400~600g / h. The heavy phase of the product from the first distillation fraction was subjected to second molecular distillation at 135~155℃. The vacuum degree during distillation was 0.05~0.1mbar, the scraper speed was 200~400rpm, and the feed rate was 600~800g / h. The heavy phase in the product of the second distillation fraction was subjected to tertiary molecular distillation at 150~170℃. The vacuum degree during distillation was 0.03~0.08mbar, the scraper speed was 200~400rpm, and the feed rate was 700~900g / h. Obtain its primary distillation light components, secondary distillation light components and tertiary distillation light components, and select one or more of the light components from each distillation stage as Brazilian tobacco pure oil.

2. The method for preparing Brazilian tobacco leaf purified oil according to claim 1, characterized in that: In step b, when acidic protease is selected, the concentration of the enzyme preparation reaction solution is 0.05 wt%, the pH value of the enzyme preparation reaction solution is 2.0~5.0, and the soaking temperature is 45~55℃; when neutral protease is selected, the concentration of the enzyme preparation reaction solution is 0.07 wt%, the pH value of the enzyme preparation reaction solution is 6.0~7.5, and the soaking temperature is 55℃; when pectinase is selected, the concentration of the enzyme preparation reaction solution is 0.07 wt%, the pH value of the enzyme preparation reaction solution is 6.0, and the soaking temperature is 50℃; when amylase is selected, the concentration of the enzyme preparation reaction solution is 0.03 wt%, the pH value of the enzyme preparation reaction solution is 7.0, and the soaking temperature is 50℃. The centrifugation speed is 500~700 r / min, the time is 2~5 min, the storage temperature is 30~60℃, the ambient humidity is 60%~80%, and the time is 2~3 h.

3. The method for preparing Brazilian tobacco leaf purified oil according to claim 1, characterized in that: In step f, the temperature of the primary molecular distillation is 125℃, the vacuum degree is 0.5mbar, the scraper rotation speed is 300rpm, and the feed rate is 600g / h. The temperature for secondary molecular distillation was 145℃, the vacuum degree was 0.05mbar, the scraper rotation speed was 300rpm, and the feed rate was 800ml / h. The temperature for tertiary molecular distillation is 160℃, the vacuum degree is 0.03mbar, the scraper rotation speed is 300rpm, and the feed rate is 900g / h.

4. The method for preparing Brazilian tobacco leaf purified oil according to claim 1, characterized in that: In step f, the light fraction from the secondary distillation is used as the purified oil from Brazilian tobacco leaves.

5. The application of the Brazilian tobacco pure oil prepared by any one of the preparation methods described in claims 1 to 4 in cigarettes.

6. The application according to claim 5, characterized in that: The amount of Brazilian tobacco oil added is 0.001% to 0.005%.

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