Method for preparing tobacco absolute oil through enzymolysis treatment of tobacco leaf residues and application of tobacco absolute oil in cigarettes
By enzymatically treating tobacco residues and using compound enzyme preparations and membrane separation technology to prepare tobacco pure oil, the problem of tobacco resource waste has been solved, the aroma and sensory quality of cigarettes have been improved, and high-value utilization and green production of resources have been achieved.
Patent Information
- Application Number
- CN202511285962.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-09-10
- Publication Date
- 2025-12-26
AI Technical Summary
In existing technologies, tobacco residue after supercritical carbon dioxide extraction is considered waste, resulting in resource waste. Furthermore, conventional extraction methods cannot effectively utilize its lignin and cellulose, affecting the high-value utilization of tobacco resources.
Tobacco residue is treated with enzymatic hydrolysis. A mixture of compound enzyme preparations, such as manganese peroxidase, laccase, and lignin peroxidase, combined with acetic acid to adjust the pH value and membrane separation technology, is used to prepare tobacco pure oil, which is then applied to cigarettes to improve the sensory quality of the smoke.
This achieves efficient utilization of tobacco resources, and the prepared tobacco oil significantly enhances the aroma and quantity of cigarettes, reduces off-flavors, improves aftertaste, and enhances the sensory quality of smoke, which aligns with the concept of green production.
Smart Images
Figure CN121196221A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of tobacco technology, and in particular to a method for preparing tobacco oil by enzymatic hydrolysis of tobacco residue and its application in cigarettes. Background Technology
[0002] Tobacco extract is a crucial flavoring ingredient in Chinese cigarettes. It's a refined product extracted and purified from tobacco, containing various volatile and semi-volatile components. Common extraction methods include solvent extraction, supercritical fluid extraction, steam distillation, microwave-assisted extraction, and eutectic solvent extraction. Among these, supercritical carbon dioxide extraction is a highly efficient and environmentally friendly separation technology widely used in the development and research of tobacco flavorings. However, the tobacco residue remaining after supercritical carbon dioxide extraction is typically treated as waste, resulting in significant resource waste. Given the current tight demand for high-quality tobacco leaves, the high-value utilization of tobacco waste resources has become a pressing issue for the tobacco industry.
[0003] The residue left after supercritical fluid extraction of tobacco leaves has extremely low volatile content, making further extraction using common methods largely pointless. However, this residue contains a large amount of lignin and cellulose, and selecting appropriate deep processing techniques for the reuse of lignin and cellulose is an effective solution. Lignin is mainly formed by three typical phenylpropane units (p-hydroxyphenyl, guaiacol, and syringyl) linked by various ether bonds and carbon-carbon bonds. Valuable aroma substances can be produced through biodegradation, and the process is gentle and environmentally friendly.
[0004] Therefore, this invention aims to address the problem of efficient utilization of tobacco waste by providing a method for preparing tobacco purified oil through enzymatic hydrolysis of tobacco residue, and applying the prepared tobacco purified oil to cigarettes to effectively improve the sensory quality of the smoke. Summary of the Invention
[0005] The technical problem to be solved by the present invention is to provide a method for preparing tobacco purified oil by enzymatic hydrolysis of tobacco residue and its application in cigarettes. The method is characterized by simple equipment, green and efficient operation, and the purified oil has outstanding sensory quality and significantly improves the state of the smoke.
[0006] The technical problem to be solved by the present invention is achieved through the following technical solution:
[0007] A method for preparing tobacco pure oil by enzymatic hydrolysis of tobacco residue includes the following steps:
[0008] (1) Raw material pretreatment: Weigh the tobacco leaf fragments after supercritical extraction and add them to the reaction vessel. Add water with a mass of 3-4 times the weight of the tobacco leaf fragments and stir evenly. Adjust the pH of the solution to 5-6 with acetic acid. Seal and heat to 180-200℃ and react for 1-2 hours. Stop heating and cool to room temperature. Transfer the treated solution to a 50℃ oil bath and stir evenly.
[0009] (2) Activation and hydrolysis of compound enzyme preparation: Take 0.5% of the compound enzyme preparation by weight of raw material, add water to completely dissolve to obtain enzyme solution, activate in a 50℃ water bath for 25 min, add the activated enzyme solution to the pretreated raw material, and hydrolyze in a 50℃ constant temperature oil bath for 3-4 h. After the hydrolysis is completed, raise the temperature of the oil bath to 100℃ and continue stirring for 20 min, stop heating and cool to room temperature to obtain material solution A;
[0010] (3) Preparation of tobacco purified oil: After centrifuging the liquid A, take the supernatant as liquid B, add ethanol with a mass of 3 times that of liquid B, stir evenly, use a membrane separation device to separate and remove impurities, collect the membrane separation permeate, and obtain tobacco purified oil.
[0011] Preferably, in the above technical solution, in step (1), the sealing heating temperature is 200℃ and the reaction time is 2h.
[0012] Preferably, in the above technical solution, in step (2), the compound enzyme preparation is a mixture of manganese peroxidase (MnP), laccase and lignin peroxidase (LiP), and the mass ratio of the three is 1:(2-3):(2-3).
[0013] Preferably, in the above technical solution, in step (2), the mass ratio of manganese peroxidase (MnP), laccase and lignin peroxidase (LiP) in the compound enzyme preparation is 1:2:2, 1:3:3 or 1:2.5:3.
[0014] Preferably, in the above technical solution, in step (3), the ethanol concentration is 95%, and the membrane material used in the membrane separation device is cellulose acetate (CA) or polyacrylonitrile (PAN).
[0015] Application of a tobacco purified oil prepared according to the above method in cigarettes.
[0016] Preferably, in the above technical solution, the application involves adding tobacco oil at a ratio of 0.08 wt% to the cigarette tobacco shreds by spraying during the cigarette feeding process, producing cigarette products using conventional cigarette manufacturing methods, and then balancing the moisture content of the cigarette products for 24 hours under conditions of 60% ± 2% humidity and 25 ± 1℃.
[0017] The above-described technical solution of the present invention has the following beneficial effects:
[0018] (1) Efficient utilization of resources: Using tobacco residue that is often discarded after supercritical extraction as raw material, we fully explore the value of lignin and cellulose contained therein to prepare tobacco pure oil, realize the high value of tobacco waste resources, and alleviate the problem of tight demand for high-quality tobacco leaves.
[0019] (2) The process is green and simple: the equipment requirements are low, only conventional equipment such as stainless steel reactor, oil bath, and membrane separation device are needed; the enzymatic hydrolysis is mild and there are no highly polluting reagents throughout the process, which is in line with the concept of green production and the operation process is simple and easy to implement.
[0020] (3) Excellent product quality and application effect: The prepared tobacco pure oil, when added to cigarettes, can significantly improve the aroma quality and aroma quantity, reduce impurities, reduce irritation, improve aftertaste, effectively improve the sensory quality of cigarette smoke, and meet the needs of Chinese cigarette flavoring. Attached Figure Description
[0021] The accompanying drawings, which are incorporated in and form part of this specification, illustrate embodiments of the invention and, together with their description, serve to explain the principles of the invention.
[0022] Figure 1 The images show the GC-MS diagrams of the three tobacco oils from Examples 1-3 of this invention. Detailed Implementation
[0023] Various exemplary embodiments of the present invention will now be described in detail with reference to the accompanying drawings. It should be noted that, unless otherwise specifically stated, the relative arrangement, numerical expressions, and values of the components and steps set forth in these embodiments do not limit the scope of the invention.
[0024] Unless otherwise specified, the experimental methods used in the following examples are conventional methods, and the materials and reagents used are commercially available. Unless otherwise specified, the equipment used in the experiments is well known to those skilled in the art.
[0025] Example 1
[0026] A method for preparing tobacco pure oil by enzymatic hydrolysis of tobacco residue and its application in cigarettes includes the following steps:
[0027] (1) Raw material pretreatment:
[0028] Weigh 50g of supercritical extracted tobacco leaf fragments and add them to a stainless steel reactor. Add 150g of water, stir well, and adjust the pH of the solution to 5 with acetic acid. Seal the reactor and heat it to 180℃. React for 1 hour, then stop heating and cool to room temperature. Transfer the treated solution to a 50℃ oil bath and stir well.
[0029] (2) Activation and enzymatic hydrolysis of compound enzyme preparations:
[0030] Take 0.5% of the raw material mass of the compound enzyme preparation, dissolve it completely in water to obtain an enzyme solution, and activate it in a 50℃ water bath for 25 min. The compound enzyme preparation is a mixture of manganese peroxidase (MnP), laccase, and lignin peroxidase (LiP) triple enzyme preparations in a mass ratio of 1:2:2. Add the dissolved and activated enzyme solution dropwise to the pretreated raw material, and continue enzymatic hydrolysis in a constant temperature 50℃ oil bath for 3 h. After the enzymatic hydrolysis is completed, raise the temperature of the oil bath to 100℃ and continue stirring for 20 min. Then stop heating and cool to room temperature, and record this as solution A.
[0031] (3) Preparation of tobacco purified oil and its application in cigarettes:
[0032] After centrifuging the cooled liquid A to room temperature, take the supernatant to obtain liquid B. Add 95% ethanol with a mass of 3 times that of liquid B, stir well, and use a membrane separation device to separate and remove impurities. Collect the membrane separation permeate to obtain tobacco pure oil, which is denoted as pure oil 1#.
[0033] The obtained tobacco oil was added to the cigarette tobacco at a ratio of 0.08 wt% via spraying during the feeding process (the blank control sample used only alcohol). The cigarette product was then manufactured using conventional methods in the field. The moisture content was equilibrated (60% ± 2% humidity, 25 ± 1℃) for 24 hours. Sensory evaluation was conducted by a panel of qualified tasters. The evaluation results and component analysis are shown in Tables 1 and 2, respectively. Figure 1 .
[0034] Example 2
[0035] A method for preparing tobacco pure oil by enzymatic hydrolysis of tobacco residue and its application in cigarettes includes the following steps:
[0036] (1) Raw material pretreatment:
[0037] Weigh 50g of tobacco leaf fragments after supercritical extraction and add them to a stainless steel reactor. Add 200g of water, stir well, and adjust the pH of the solution to 6 with acetic acid. Seal the reactor and heat it to 200℃. React for 2 hours, then stop heating and cool to room temperature. Transfer the treated solution to a 50℃ oil bath and stir well.
[0038] (2) Activation and enzymatic hydrolysis of compound enzyme preparations:
[0039] Take 0.5% of the raw material mass of the compound enzyme preparation, dissolve it completely in water to obtain an enzyme solution, and activate it in a 50℃ water bath for 25 min. The compound enzyme preparation is a mixture of manganese peroxidase (MnP), laccase, and lignin peroxidase (LiP) triple enzyme preparations in a mass ratio of 1:3:3. Add the dissolved and activated enzyme solution dropwise to the pretreated raw material, and continue enzymatic hydrolysis in a constant temperature 50℃ oil bath for 4 h. After the enzymatic hydrolysis is completed, raise the temperature of the oil bath to 100℃ and continue stirring for 20 min. Then stop heating and cool to room temperature, and record this as solution A.
[0040] (3) Preparation of tobacco purified oil and its application in cigarettes:
[0041] After centrifuging the cooled liquid A to room temperature, take the supernatant to obtain liquid B. Add 95% ethanol with a mass of 3 times that of liquid B, stir well, and use a membrane separation device to separate and remove impurities. Collect the membrane separation permeate to obtain tobacco pure oil, which is denoted as pure oil 2#.
[0042] The obtained tobacco oil was added to the cigarette tobacco at a ratio of 0.08 wt% via spraying during the feeding process (the blank control sample used only alcohol). The cigarette product was then manufactured using conventional methods in the field. The moisture content was equilibrated (60% ± 2% humidity, 25 ± 1℃) for 24 hours. Sensory evaluation was conducted by a panel of qualified tasters. The evaluation results and component analysis are shown in Tables 1 and 2, respectively. Figure 1 .
[0043] Example 3
[0044] A method for preparing tobacco pure oil by enzymatic hydrolysis of tobacco residue and its application in cigarettes includes the following steps:
[0045] (1) Raw material pretreatment:
[0046] Weigh 50g of tobacco leaf fragments after supercritical extraction and add them to a stainless steel reactor. Add 200g of water, stir well, and adjust the pH of the solution to 5 with acetic acid. Seal the reactor and heat it to 200℃. React for 2 hours, then stop heating and cool to room temperature. Transfer the treated solution to a 50℃ oil bath and stir well.
[0047] (2) Activation and enzymatic hydrolysis of compound enzyme preparations:
[0048] Take 0.5% of the raw material mass of the compound enzyme preparation, dissolve it completely in water to obtain an enzyme solution, and activate it in a 50℃ water bath for 25 min. The compound enzyme preparation is a mixture of manganese peroxidase (MnP), laccase, and lignin peroxidase (LiP) triple enzyme preparations in a mass ratio of 1:2.5:3. Add the dissolved and activated enzyme solution dropwise into the pretreated raw material, and continue enzymatic hydrolysis in a constant temperature 50℃ oil bath for 3 h. After the enzymatic hydrolysis is completed, raise the temperature of the oil bath to 100℃ and continue stirring for 20 min. Then stop heating and cool to room temperature, and record this as solution A.
[0049] (3) Preparation of tobacco purified oil and its application in cigarettes:
[0050] After centrifuging the cooled liquid A to room temperature, take the supernatant to obtain liquid B. Add 95% ethanol with a mass of 3 times that of liquid B, stir well, and use a membrane separation device to separate and remove impurities. Collect the membrane separation permeate to obtain tobacco pure oil, which is designated as pure oil 3#.
[0051] The obtained tobacco oil was added to the cigarette tobacco at a ratio of 0.08 wt% via spraying during the feeding process (the blank control sample used only alcohol). The cigarette product was then manufactured using conventional methods in the field. The moisture content was equilibrated (60% ± 2% humidity, 25 ± 1℃) for 24 hours. Sensory evaluation was conducted by a panel of qualified tasters. The evaluation results and component analysis are shown in Tables 1 and 2, respectively. Figure 1 .
[0052] Table 1. Sensory quality evaluation results of test samples and blank control samples
[0053]
[0054]
[0055] As can be seen from Table 1, when the tobacco purified oil obtained by this invention is added to cigarettes, the aroma quality and aroma quantity of the cigarettes are significantly improved, the off-flavor of the smoke is reduced, and the irritation is decreased; the aftertaste is more comfortable, indicating that the addition of the obtained tobacco purified oil can mask the off-flavor of the tobacco itself, improve the taste, and enhance the quality of the smoke.
[0056] Although the present invention has been disclosed above with reference to embodiments, it is not intended to limit the present invention. Any person skilled in the art can make various different choices and modifications without departing from the spirit and scope of the present invention. Therefore, the scope of protection of the present invention is defined by the claims and their equivalents.
Claims
1. A method for preparing tobacco pure oil by enzymatic hydrolysis of tobacco leaf residue, characterized in that, Includes the following steps: (1) Raw material pretreatment: Weigh the tobacco leaf fragments after supercritical extraction and add them to the reaction vessel. Add water with a mass of 3-4 times the weight of the tobacco leaf fragments and stir evenly. Adjust the pH of the solution to 5-6 with acetic acid. Seal and heat to 180-200℃ and react for 1-2 hours. Stop heating and cool to room temperature. Transfer the treated solution to a 50℃ oil bath and stir evenly. (2) Activation and hydrolysis of compound enzyme preparation: Take 0.5% of the compound enzyme preparation by weight of raw material, add water to completely dissolve to obtain enzyme solution, activate in a 50℃ water bath for 25 min, add the activated enzyme solution to the pretreated raw material, and hydrolyze in a 50℃ constant temperature oil bath for 3-4 h. After the hydrolysis is completed, raise the temperature of the oil bath to 100℃ and continue stirring for 20 min, stop heating and cool to room temperature to obtain material solution A; (3) Preparation of tobacco purified oil: After centrifuging the liquid A, take the supernatant as liquid B, add ethanol with a mass of 3 times that of liquid B, stir evenly, use a membrane separation device to separate and remove impurities, collect the membrane separation permeate, and obtain tobacco purified oil.
2. The method according to claim 1, characterized in that, In step (1), the sealing heating temperature is 200℃ and the reaction time is 2h.
3. The method according to claim 1, characterized in that, In step (2), the compound enzyme preparation is a mixture of manganese peroxidase, laccase and lignin peroxidase, with a mass ratio of 1:(2-3):(2-3).
4. The method according to claim 3, characterized in that, In step (2), the mass ratio of manganese peroxidase, laccase and lignin peroxidase in the compound enzyme preparation is 1:2:2, 1:3:3 or 1:2.5:
3.
5. The method according to claim 1, characterized in that, In step (3), the ethanol concentration is 95%, and the membrane material used in the membrane separation device is cellulose acetate or polyacrylonitrile.
6. The use of a tobacco pure oil prepared according to any one of claims 1-5 in cigarettes.
7. The application according to claim 6, characterized in that, The application involves adding tobacco oil at a ratio of 0.08 wt% to the tobacco shreds during the cigarette feeding process by spraying. The cigarette product is then manufactured using conventional cigarette manufacturing methods, and subsequently, the cigarette product is subjected to moisture balancing for 24 hours at a humidity of 60% ± 2% and a temperature of 25 ± 1℃.