A method for extracting tobacco extract from tobacco extract, the tobacco extract and its uses

Abstract

This invention relates to the field of tobacco extract production technology, and in particular to a method for extracting tobacco extract from tobacco extract, the tobacco extract prepared by this method, and its uses. The extraction method includes: providing a tobacco extract; adjusting excess tobacco extract to an alkaline solution using an alkalinity regulator; adding a complex amino acid compound to the alkaline solution for a mixed reaction; and post-treatment to obtain the tobacco extract. This method, by combining thermal alcoholization technology with the Maillard reaction, not only effectively reduces the discharge of excess tobacco extract and lowers wastewater treatment costs, but also enables the reuse of excess tobacco extract, reduces the total sugar content in the tobacco extract, and increases the content of megastigmatrienone. The tobacco extract prepared by this method is suitable for use in the tobacco product industry.

Description

Technical Field

[0001] This invention relates to the field of tobacco extract production technology, and in particular to a method for extracting tobacco extract from tobacco extract, the tobacco extract prepared by the method, and its uses. Background Technology

[0002] The reconstituted tobacco production process generates an excess of extract. With the gradual implementation of new technologies, the problem of excess extract is intensifying. Directly discharging the excess extract poses a significant challenge to the wastewater treatment capacity of wastewater treatment plants. Furthermore, the extract contains many effective components, such as tobacco aroma components, and direct discharge would result in substantial waste.

[0003] Aroma components in tobacco are an important part of the intrinsic quality of tobacco. Megastigmatrienone is the most abundant carotenoid degradation product among neutral aroma components. It is formed by the degradation of chlorophyll and has a tobacco aroma and spicy base flavor. It significantly enhances the aroma of tobacco, improves the taste, harmonizes the smoke, and reduces irritation. Adding a small amount of this compound to cigarettes can greatly improve the aroma quality of cigarettes, giving them a pleasant aroma similar to cocoa and Burley tobacco. It is an indispensable flavoring in cigarette manufacturing and has important applications in the tobacco industry. It has also been widely used in perfumes, cosmetics, beverages, and food flavorings.

[0004] This application involves the deep processing of tobacco extract, which reduces wastewater treatment costs and reveals the potential application of tobacco extract in tobacco products. Summary of the Invention

[0005] In view of the shortcomings of the prior art described above, the purpose of this invention is to provide a method for extracting tobacco extract from tobacco extract. This method reuses the extract from tobacco leaf production, is simple in processing, low in cost, and suitable for large-scale production. Furthermore, the tobacco extract processed using this method has a lower total sugar content and an increase in aroma components such as megastigmatrienone.

[0006] To achieve the above and other related objectives, the first aspect of the present invention provides a method for extracting tobacco extract from tobacco extract, specifically comprising: 1) providing tobacco extract and adjusting excess tobacco extract to an alkaline solution using an alkaline regulator; 2) adding a complex amino acid mixture to the alkaline solution for a mixed reaction; and 3) post-processing to obtain tobacco extract.

[0007] A second aspect of the present invention provides a tobacco extract prepared by the aforementioned method for extracting tobacco extract from tobacco extract, wherein the tobacco extract contains megastigmatrienone.

[0008] A second aspect of the present invention provides the use of the tobacco extract prepared by the aforementioned method for extracting tobacco extract from tobacco extract in tobacco products, preferably, the use of the tobacco extract in the preparation of electronic cigarettes.

[0009] The beneficial effects of this invention are as follows:

[0010] The method for extracting tobacco extract from tobacco extract of the present invention can effectively reduce the discharge of excess tobacco extract, lower wastewater treatment costs, and simultaneously achieve the reuse of excess tobacco extract, realizing the goal of "turning waste into treasure." Furthermore, the method is simple to operate, has low material costs, and is suitable for large-scale industrial production. In the field of tobacco leaf reprocessing, the method of this application can reduce undesirable components (e.g., total sugar) in the extract and improve the quality of the tobacco extract (e.g., increased aroma components). Attached Figure Description

[0011] Figure 1 TIC diagram of aroma components of the tobacco extract (before alcoholization) prepared in Comparative Example 1 of this application;

[0012] Figure 2 The TIC diagram shows the aroma components of the tobacco extract (after alcoholization) prepared in Example 1 of this application.

[0013] Explanation of markings in the diagram:

[0014] 1. Megastigmatrienone 1; 2. Megastigmatrienone 2; 3. Megastigmatrienone 3; 4. Megastigmatrienone 4. Detailed Implementation

[0015] The method for extracting tobacco extract from tobacco extract according to the present invention includes the following steps:

[0016] 1) Provide tobacco extract, and use an alkaline regulator to adjust the excess tobacco extract into an alkaline solution;

[0017] Specifically, the tobacco extract is selected from excess tobacco extract, and the concentrate from the production site meets the process requirements for excess extract. For example, in the reconstituted tobacco production process, the excess extract from the extraction process is concentrated, or the excess concentrate from the concentration process generally has a density of 1.08–1.28 g / cm³. 3 .

[0018] More specifically, in the reconstituted tobacco production process, the excess extract from the extraction process, after concentration treatment, or the excess concentrate from the concentration process, has a density of 1.185±0.005 g / cm³. 3 The excess extract contains high levels of tobacco aroma compounds, such as solanone, dihydroactinolone, and megastigmatrienone.

[0019] The alkalinity adjuster is selected from potassium hydroxide and / or sodium hydroxide, preferably potassium hydroxide. The pH of the alkaline solution is 7.5–9.5, and the pH can be selected from 7.5–7.9, 7.9–8.9, or 8.9–9.5. This provides an alkaline environment to meet the requirements of subsequent mixing reactions with complex amino acids.

[0020] 2) Add the complex amino acid mixture to the alkaline solution and react.

[0021] Specifically, the mixed reaction is selected from thermal aging reaction and / or Maillard reaction. Preferably, the thermal aging process commonly used in the tobacco preparation field is introduced into the Maillard reaction. After treatment under certain reaction conditions, tobacco extract with reduced total sugar content and increased content of aroma substances, such as megastigmatrienone, in the tobacco extract are obtained.

[0022] Specifically, the amount of compound amino acids added is 0.1–0.5 wt%, which means the mass of the compound amino acids added is 0.1–0.5% of the mass of the alkaline solution after alkalinity adjustment. 0.1–0.2% or 0.2–0.5% can be selected. The amount of compound amino acids added needs to be appropriate to ensure full participation in the reaction, achieving the goal of reducing total sugar and increasing aroma compounds through the complex Maillard reaction.

[0023] Preferably, the compound amino acid is selected from at least two of proline, glutamic acid, aspartic acid, alanine, glycine, phenylalanine, and tryptophan, and is appropriately formulated according to the different tobacco extracts. Optionally, the compound amino acid contains proline, and the mass fraction of proline accounts for more than 28% of the total mass of the compound amino acid. Optionally, the compound amino acid contains proline and glutamic acid, and the mass fraction of proline and glutamic acid accounts for more than 50% of the total mass of the compound amino acid. Optionally, the compound amino acid contains proline, glutamic acid, and aspartic acid, and the mass fraction of proline, glutamic acid, and aspartic acid accounts for more than 70% of the total mass of the compound amino acid. In a preferred embodiment, the composite amino acid is a complex of proline, glutamic acid, aspartic acid, alanine, glycine, phenylalanine, and tryptophan, and the mass ratio of the composite amino acid to proline, glutamic acid, aspartic acid, alanine, glycine, phenylalanine, and tryptophan is (18-30):(8-14):(8-13):(5-7):(2-6):(2-5):1. More preferably, the mass ratio of the composite amino acid to proline, glutamic acid, aspartic acid, alanine, glycine, phenylalanine, and tryptophan is 150:82:70:43:32:29:7.

[0024] Specifically, the reaction temperature for the mixed reaction is 70–90℃, and the reaction time is 24–72h, which can be selected according to actual needs. The temperature can be 70–80℃ or 80–90℃, and the reaction time can be 24–36h, 36–48h, or 48–72h.

[0025] 3) Post-processing to obtain tobacco extract.

[0026] Specifically, the post-processing involves alcohol precipitation of the solution after the mixing reaction in step 2) to obtain tobacco extract.

[0027] The alcohol precipitation process specifically involves: the pretreated solution after the mixing reaction in step 2); adding an alcohol solution to the pretreated solution under stirring to perform alcohol extraction; and then allowing it to stand, separate into layers, and concentrate to obtain tobacco extract. The stirring speed is generally 200-400 r / min.

[0028] Preferably, the pretreatment solution needs to be cooled to an initial temperature of 3–8°C, which can be 3–4°C, 4–6°C, or 6–8°C. The mass ratio of the pretreatment solution to the alcohol solution is (2–8):1, which can be (2–3):1, (3–4):1, (4–5):1, or (5–8):1. The alcohol solution is preferably an aqueous ethanol solution with an ethanol concentration of 95–100% added to the pretreatment solution.

[0029] More preferably, the alcohol solution is added to the pretreatment solution by dropwise addition at a rate of 0.15–0.25 L / min, with an alcohol precipitation time of 4–10 hours. The supernatant is then collected and concentrated at 30–45°C to obtain tobacco extract, with a concentration of 1.142–1.342 g / cm³. 3 .

[0030] In addition, this application also discloses a method for detecting megastigmatrienone in tobacco extract obtained by the above extraction method. Take 10 ml of tobacco extract, add 40 μL of 10 mg / mL phenethyl acetate internal standard solution, then add 20 ml of methyl tert-butyl ether, sonicate for 1 h, then place on a constant temperature shaker, shake for 4 h, let stand overnight, centrifuge, take the supernatant, add an appropriate amount of anhydrous sodium sulfate, concentrate in a rotary concentrator at 40 °C to 1 mL, take out and filter for GC / MS analysis.

[0031] The gas chromatography conditions were as follows: the column was a DB-Waxlter capillary column; the thermal desorption and gas chromatography transfer line temperature was 240℃; the carrier gas was high-purity helium with a purity ≥99.999%; the flow rate was 0.8-1.2 mL / min; splitless injection was used; the temperature program was: 40℃ held for 2 min, then increased to 230℃ at a rate of 3℃ / min and held for 20 min; the total analysis time was 85.33 min.

[0032] The mass spectrometry conditions were as follows: ion source temperature 230℃, quadrupole temperature 150℃, ionization method EI source, ionization energy 70eV, scanning mode full scan, and mass scan range m / z: 29~450amu.

[0033] The following specific examples illustrate the implementation of the present invention. Those skilled in the art can easily understand other advantages and effects of the present invention from the content disclosed in this specification. The present invention can also be implemented or applied through other different specific embodiments, and various details in this specification can also be modified or changed based on different viewpoints and applications without departing from the spirit of the present invention.

[0034] Furthermore, it should be understood that one or more method steps mentioned in this invention do not preclude the existence of other method steps before or after the combined steps, or the insertion of other method steps between these explicitly mentioned steps, unless otherwise stated. It should also be understood that, unless otherwise stated, the numbering of each method step is merely a convenient tool for identifying each method step, and not for limiting the order of the method steps or limiting the scope of implementation of this invention. Changes or adjustments to their relative relationships, without substantially altering the technical content, should also be considered as within the scope of implementation of this invention.

[0035] Example 1

[0036] 240g of excess tobacco extract from the reconstituted tobacco production process was taken, and its density was measured to be 1.182g / cm³. 3 Add an appropriate amount of potassium hydroxide to adjust the pH to 8.9, then add 0.2 wt% of a complex amino acid, with the specific mass ratio of each amino acid being: proline:glutamic acid:aspartic acid:alanine:glycine:phenylalanine:tryptophan = 150:82:70:43:32:29:7. Mix and react at 90℃ for 72 hours. Take 200g of the obtained extract and add 518g of 95% ethanol for alcohol precipitation, with the ethanol dropping rate being 0.15-0.25L / min, the initial temperature of the extract being 5℃, and alcohol precipitation for 8 hours. Take the supernatant and concentrate it at 40℃ using a rotary condenser to obtain tobacco extract with a density of 1.245g / cm³. 3 .

[0037] Comparative Example 1

[0038] Take 200g of excess tobacco extract and add 518g of 95% ethanol for alcohol precipitation. The ethanol is added at a rate of 0.15–0.25 L / min, the initial temperature of the extract is 5℃, and the precipitation lasts for 8 hours. Collect the supernatant and concentrate it at 40℃ using a rotary condenser to obtain tobacco extract with a density of 1.241 g / cm³. 3 .

[0039] Test Example 1

[0040] The total sugar content in excess tobacco extract, tobacco extract (before alcoholization) of Comparative Example 1, and tobacco extract (after alcoholization) of Example 1 were determined according to national standard YC / T159-2002. The results are shown in Table 1 below:

[0041] Table 1. Changes in total sugar content of excess tobacco extract, pre-aging tobacco extract, and post-aging tobacco extract.

[0042] Serial Number sample Total sugar / % 1 Excess tobacco extract 9.46 3 Tobacco extract (before alcoholization) in Example 1 18.73 4 Comparative Example 1: Tobacco extract (after alcoholization) 6.29

[0043] As shown in Table 1, the total sugar content of the tobacco extract prepared by the extraction process of this application is reduced by 33.5% compared to the tobacco extract, and by 66.42% compared to the tobacco extract (before aging) prepared by the process of this application. It can be inferred that this is due to the participation of sugars in the Maillard reaction during the thermal aging process.

[0044] Test Example 2

[0045] Megastigrinone in excess tobacco extract, tobacco extract (before alcoholysis), and tobacco extract (after alcoholysis) from Example 1 were determined using gas chromatography-mass spectrometry (GC-MS) and relative internal standard method. The results are shown in Table 2 below.

[0046] First, the method for detecting megastigmatrienone in tobacco extract described in this application was used to detect megastigmatrienone in tobacco extract (before alcoholization) and tobacco extract (after alcoholization), with the processing methods and detection conditions being consistent for both. Specifically: 10 ml of tobacco extract was taken (both before and after alcoholization were taken for subsequent processing and analysis), 40 μL of 10 mg / mL phenethyl acetate internal standard solution was added, followed by 20 ml of methyl tert-butyl ether. The mixture was ultrasonically extracted for 1 h, then placed on a constant temperature shaker and shaken for 4 h. After standing overnight, the mixture was centrifuged, and the supernatant was collected. An appropriate amount of anhydrous sodium sulfate was added, and the mixture was concentrated to 1 mL at 40 °C in a rotary concentrator. The solution was then filtered and prepared for GC / MS analysis.

[0047] The gas chromatography conditions were as follows: the column was a DB-Waxlter capillary column; the thermal desorption and gas chromatography transfer line temperature was 240℃; the carrier gas was high-purity helium with a purity ≥99.999%; the flow rate was 0.8-1.2 mL / min; splitless injection was used; the temperature program was: 40℃ held for 2 min, then increased to 230℃ at a rate of 3℃ / min and held for 20 min; the total analysis time was 85.33 min.

[0048] The mass spectrometry conditions were as follows: ion source temperature 230℃, quadrupole temperature 150℃, ionization method EI source, ionization energy 70eV, scanning mode full scan, and mass scan range m / z: 29~450amu.

[0049] The TIC diagram of the meso-aroma components in tobacco extract (before aging) is shown below. Figure 1 As shown, only the chromatographic peak of megastigmatrienone 4 is observed; the TIC chromatogram of the aroma components in tobacco extract (after alcoholization) is shown below. Figure 2 As shown, chromatographic peaks of four isomers, namely mesostachinoide 1, mesostachinoide 2, mesostachinoide 3 and mesostachinoide 4, were observed.

[0050] Table 2. Changes in the content of megastigmatrienone in excess tobacco extract, pre-alcoholized tobacco extract, and post-alcoholized tobacco extract.

[0051]

[0052]

[0053] As shown in Table 2, only megastigmatrienone 4 was detected in tobacco extract (before aging), while all four megastigmatrienones were detected in tobacco extract (after aging), and the content was much higher than that in tobacco extract (before aging).

[0054] Example 2

[0055] Take 240g of the same excess tobacco extract as in Example 1, and measure its density to be 1.182g / cm³. 3 Add an appropriate amount of potassium hydroxide to adjust the pH to 7.9, then add 0.5 wt% of a complex amino acid, with the specific mass ratio of each amino acid being: proline:glutamic acid:aspartic acid:alanine:glycine:phenylalanine:tryptophan = 150:82:70:43:32:29:7. Mix and react at 80℃ for 72 hours. Take 200g of the obtained extract and add 518g of 95% ethanol for alcohol precipitation, with the ethanol dropping rate being 0.15-0.25L / min, the initial temperature of the extract being 5℃, and alcohol precipitation for 8 hours. Take the supernatant and concentrate it at 40℃ using a rotary condenser to obtain tobacco extract with a density of 1.242g / cm³. 3 .

[0056] Comparative Example 2

[0057] Take 200g of excess tobacco extract and add 518g of 95% ethanol for alcohol precipitation. The ethanol is added at a rate of 0.15–0.25 L / min, the initial temperature of the extract is 5℃, and the precipitation lasts for 8 hours. Collect the supernatant and concentrate it at 40℃ using a rotary condenser to obtain tobacco extract with a density of 1.241 g / cm³. 3 .

[0058] Test Example 3

[0059] The total sugar content in excess tobacco extract, tobacco extract (before aging), and tobacco extract (after aging) from Example 2 was determined according to national standard YC / T159-2002. The results are shown in Table 3 below:

[0060] Table 3. Changes in total sugar content of excess tobacco extract, pre-aging tobacco extract, and post-aging tobacco extract.

[0061] Serial Number sample Total sugar / % 1 Excess tobacco extract 9.46 3 Tobacco extract (before alcoholization) in Example 2 18.73 4 Comparative Example 2: Tobacco extract (after alcoholization) 8.79

[0062] As shown in Table 3, the total sugar content of the tobacco extract prepared by the extraction process of this application is reduced by 7.1% compared with the tobacco extract, and the total sugar content is reduced by 53.07% compared with the tobacco extract (before aging) obtained without this process.

[0063] Test Example 4

[0064] The megastigmatrienone in the tobacco extract of Comparative Example 2 (before alcoholization) and the tobacco extract of Example 2 (after alcoholization) were determined using the same method as in Test Example 2. The results are shown in Table 4 below.

[0065] Table 4. Changes in the content of megastigmatrienone in excess tobacco extract, pre-alcoholized tobacco extract, and post-alcoholized tobacco extract.

[0066] Serial Number Fragrance ingredients Tobacco extract (before aging) μg / g Tobacco extract (after alcoholization) μg / g 1 Megastigmatrienone 1 - 0.23 2 Megastigmatrienone 2 - 0.92 3 Megastigmatrienone 3 - 0.27 4 Megastigmatrienone 4 0.20 1.04

[0067] As shown in Table 4, under the same processing conditions and detection methods, only a small amount of megastigmatrienone 4 was detected in tobacco extract (before aging), while all four megastigmatrienones were detected in tobacco extract (after aging), and the content was much higher than that in tobacco extract (before aging). It can be inferred that this was due to the degradation of carotenoids promoted by the thermal aging process.

[0068] In summary, the present invention provides a method for extracting tobacco extract from tobacco extract. The tobacco extract prepared by this method has a low total sugar content and a high content of megastigmatrienone, making it suitable for flavoring and adding to electronic cigarettes and tobacco products.

[0069] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention in any form or substance. It should be noted that those skilled in the art can make various improvements and additions without departing from the method of the present invention, and these improvements and additions should also be considered within the scope of protection of the present invention. Any modifications, alterations, and equivalent changes made by those skilled in the art based on the above-disclosed technical content without departing from the spirit and scope of the present invention are equivalent embodiments of the present invention. Furthermore, any modifications, alterations, and evolutions made to the above embodiments based on the essential technology of the present invention still fall within the scope of the technical solution of the present invention.

Claims

1. A method for extracting tobacco extract from tobacco extract, specifically comprising: 1) Provide tobacco extract, which is adjusted to an alkaline solution using an alkalinity regulator; the tobacco extract is a concentrate obtained from excess extract during the reconstituted tobacco production process, or excess concentrate obtained during the concentration process, with a density of 1.08–1.28 g / cm³. 3 ; 2) Add a complex amino acid to the alkaline solution for a mixed reaction; the amount of the complex amino acid added is 0.1-0.5 wt%; the reaction conditions for the mixed reaction are: reaction temperature of 80-90℃, reaction time of 24-72h; the mixed reaction is a thermal alcoholysis reaction and a Maillard reaction; the mass ratio of the complex amino acid, proline, glutamic acid, aspartic acid, alanine, glycine, phenylalanine, and tryptophan is (18-30):(8-14):(8-13):(5-7):(2-6):(2-5):1; 3) Post-treatment to obtain tobacco extract; the post-treatment is to perform alcohol precipitation on the solution after the mixing reaction in step 2) to obtain tobacco extract.

2. The method for extracting tobacco extract from tobacco extract as described in claim 1, characterized in that, Step 1) includes at least one of the following technical features: a1. The alkalinity regulator is selected from potassium hydroxide and / or sodium hydroxide; a2. The pH of the alkaline solution is 7.5 to 9.

5.

3. The method for extracting tobacco extract from tobacco extract as described in claim 1, characterized in that, The alcohol precipitation process specifically involves: providing a pretreated solution after the mixing reaction in step 2); adding an alcohol solution to the pretreated solution under stirring to perform alcohol extraction; and then allowing it to stand, separate layers, and concentrate to obtain tobacco extract.

4. The method for extracting tobacco extract from tobacco extract as described in claim 3, characterized in that, Includes at least one of the following technical features: c1. The initial temperature of the pretreatment solution is 3-8℃; c2. The mass ratio of the pretreatment solution to the alcohol solution is (2-8):1; c3. The alcohol solution is an aqueous ethanol solution; c4. The alcohol solution has a concentration of 95-100%; c5. The alcohol solution is added to the pretreatment solution by dropping, at a rate of 0.15–0.25 L / min.

5. The tobacco extract prepared by the method for extracting tobacco extract from tobacco extract as described in any one of claims 1-4.

6. Use of the tobacco extract as described in claim 5 in tobacco products.

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