Tobacco absolute as well as preparation method and application thereof
Through membrane separation technology, the problem of lack of selectivity in the existing tobacco extract preparation methods is solved, and the preparation of high-quality tobacco clean oil is achieved. It is suitable for cigarette fragrance making and improves the aroma quality.
Patent Information
- Application Number
- CN202411591730.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-08
- Publication Date
- 2025-03-04
AI Technical Summary
In the existing tobacco extract preparation methods, solvent leaching lacks selectivity, causing impurities to enter the product and affect quality.
Using membrane separation technology, mass transfer is carried out between membrane phases by selecting permeability and concentration difference, pressure gradient or potential gradient of polymer membrane as driving force, and tobacco extracts are separated and purified. The specific steps include mixing tobacco fragrance with a high concentration of alcohol solution, leaving it stand to remove the supernatant, concentrated and filtering the filter membrane to obtain tobacco clean oil.
It realizes the high-quality preparation of tobacco extracts, removes ingredients that produce bad flavor to the senses, maintains the original fragrance of raw tobacco, and is suitable for scenting cigarettes, improving the aroma quality.
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Abstract
Description
Technical Field
[0001] The invention relates to the technical field of tobacco, and in particular to a tobacco oil, a preparation method and application thereof. Background Art
[0002] Cigarette production is the process of turning non-standardized tobacco leaf agricultural products into standardized cigarette industrial products. In this process, cigarette flavoring plays a key role in maintaining the stability of sensory quality all year round, and is an important means to improve impurities, increase concentration and improve quality; especially the current market attention and demand for low-tar cigarettes are constantly increasing. While reducing the amount of tar, it also causes a reduction in cigarette flavor substances. The compensation for the loss of tobacco flavor also puts forward more urgent demands for cigarette flavoring. Cigarette flavor raw materials play a vital role as the material basis of cigarette flavoring; tobacco flavor raw materials mainly come from natural extraction, chemical synthesis, biological production, etc. Compared with daily chemical and food flavoring, the flavoring of cigarette products has its own particularity. Tobacco flavor raw materials in natural extraction flavor raw materials are the only flavor raw materials derived from tobacco and can supplement the tobacco flavor of cigarettes. They play a key role in cigarette flavoring, and therefore occupy a core position in tobacco flavor raw materials.
[0003] Traditional tobacco extracts are mainly prepared by solvent extraction, where solvents are added to tobacco leaves for extraction, and tobacco extract products are obtained after concentration and removal of the solvents. The extraction process is mature, simple to operate, and low in cost, but due to the lack of selectivity of solvent extraction, undesirable impurities such as polysaccharides, proteins and other macromolecules are also extracted into the product with the solvent during the preparation process, thereby introducing undesirable sensory flavors. Therefore, the tobacco extract or crude oil products prepared by the extraction method are of low quality. In order to obtain higher quality tobacco extract fragrance raw materials, further refining is required.
[0004] Membrane separation technology is based on the selective permeability of polymer membranes, with concentration difference, pressure gradient or potential gradient as the driving force, and mass transfer between membrane phases, so as to achieve the purpose of separation and purification of different components. Application research in the tobacco industry mainly focuses on the treatment of tobacco flake extracts, and there are few reports on its application in the refining of tobacco extracts. The main application purpose of membrane separation in the preparation of tobacco flakes is concentration, and the flake extract is generally a dilute aqueous phase system. There is a big difference between it and the preparation of tobacco extracts as flavor raw materials: tobacco extracts used as flavor raw materials for the preparation of tobacco flavors are generally alcohol-soluble and have a high viscosity, and the main application appeal is to obtain a good sensory experience and improve the aroma quality. Summary of the invention
[0005] Membrane separation technology is based on the selective permeability of polymer membranes, using concentration difference, pressure gradient or potential gradient as the driving force to carry out mass transfer between membrane phases, thereby achieving the purpose of separation and purification of different components.
[0006] In view of the above-mentioned shortcomings of the prior art, the object of the present invention is to provide a tobacco clean oil and a preparation method and use thereof, so as to solve the problems in the prior art.
[0007] To achieve the above object and other related objects, the present invention provides a method for preparing tobacco oil, which comprises the following steps:
[0008] 1) mixing the crude tobacco flavor product with an alcohol solution having a volume fraction of 90% to 95%, allowing the mixture to stand, and collecting the supernatant;
[0009] 2) concentrating the supernatant obtained in step 1) to remove the alcohol solution, and collecting the concentrate;
[0010] 3) filtering the concentrated liquid obtained in step 2) through a filter membrane, and the obtained filtrate is the tobacco pure oil.
[0011] The present invention also provides tobacco clean oil prepared by the above preparation method.
[0012] The present invention also provides the use of the tobacco clean oil in preparing tobacco flavorings.
[0013] The present invention also provides the use of the above tobacco clean oil or the above tobacco flavoring in flavoring cigarettes.
[0014] The present invention also provides a cigarette, which comprises the above-mentioned tobacco clean oil or the above-mentioned tobacco flavoring.
[0015] As described above, the tobacco clean oil of the present invention and its preparation method and use have the following beneficial effects:
[0016] 1) The process is simple, convenient and easy to operate, suitable for industrial production, with the characteristics of low energy consumption, high integration, green and environmental protection;
[0017] 2) The product has good effect, excellent quality, and a strong tobacco flavor. Adding it to the product has a prominent effect of increasing concentration and improving quality;
[0018] 3) Physical separation is performed by membrane filtration to remove components that produce unpleasant flavors to the senses, effectively improving the quality of the clean oil, and maintaining the original aroma of the raw tobacco to the greatest extent, avoiding the introduction of new unpleasant flavors, and effectively protecting heat-sensitive substances;
[0019] 4) The clean oil product prepared by using a high-concentration alcohol solution has a uniform and pure texture and good solubility in a flavor system with ethanol as a solvent, and is easy to be used in cigarette production. BRIEF DESCRIPTION OF THE DRAWINGS
[0020] Figure 1 It is a schematic diagram showing the total scores of the sensory evaluation of the embodiments of the present invention and the comparative examples.
[0021] Figure 2 Shown is a radar chart of sensory evaluation of the embodiments of the invention and the comparative examples. DETAILED DESCRIPTION
[0022] The present invention first provides a method for preparing tobacco oil, which comprises the following steps:
[0023] 1) mixing the crude tobacco flavor product with an alcohol solution having a volume fraction of 90% to 95%, allowing the mixture to stand, and collecting the supernatant;
[0024] 2) concentrating the supernatant obtained in step 1) to remove the alcohol solution, and collecting the concentrate;
[0025] 3) filtering the concentrated liquid obtained in step 2) through a filter membrane, and the obtained filtrate is the tobacco pure oil.
[0026] In certain embodiments of the present invention, in step 1), the crude tobacco flavor product is a tobacco extract.
[0027] The tobacco extract is a product obtained by extracting specific components from tobacco.
[0028] In certain embodiments of the present invention, in step 1), the dosage form of the crude tobacco flavor product is selected from tincture, extract or crude absolute oil.
[0029] The tobacco extract is a concentrated product obtained by extracting aromatic components and other soluble substances in tobacco. The tobacco extract usually has a strong tobacco flavor and aroma, and forms a viscous or semi-solid substance after removing the solvent.
[0030] In certain embodiments of the present invention, in step 1), the alcohol solution is an ethanol solution.
[0031] In certain embodiments of the present invention, in step 1), the volume ratio of the crude tobacco flavor product to the alcohol solution is 1:(4-7). The volume ratio of the crude tobacco flavor product to the alcohol solution is selected from any of the following ranges: 1:(4-5), 1:(5-6), 1:(6-7). Preferably, the volume ratio of the crude tobacco flavor product to the alcohol solution is 1:(4-5).
[0032] In certain embodiments of the present invention, in step 1), the standing time is 16 to 24 hours. The standing time is selected from any of the following ranges: 16 to 18 hours, 18 to 20 hours, 20 to 22 hours, 22 to 24 hours. Preferably, the standing time is 16 to 20 hours. More preferably, the standing time is 18 hours.
[0033] In certain embodiments of the present invention, in step 1), the standing temperature is -18°C to -5°C. The standing temperature is selected from any of the following ranges: -18°C to -15°C, -15°C to -10°C, -10°C to -5°C. Preferably, the standing temperature is -15°C to -10°C. More preferably, the standing temperature is -10°C.
[0034] In certain embodiments of the present invention, in step 2), the concentration temperature is 48°C to 52°C.
[0035] In certain embodiments of the present invention, in step 2), the concentration is performed until no alcohol solution is distilled out;
[0036] In certain embodiments of the present invention, in step 2), the concentration is carried out by concentration under reduced pressure.
[0037] In certain embodiments of the present invention, in step 3), the pore size of the filter membrane is 0.40 μm to 0.65 μm. The pore size of the filter membrane is selected from any of the following ranges: 0.40 μm to 0.45 μm, 0.45 μm to 0.50 μm, 0.50 μm to 0.55 μm, 0.55 μm to 0.60 μm, 0.60 μm to 0.65 μm. Preferably, the pore size of the filter membrane is 0.43 μm to 0.47 μm. More preferably, the pore size of the filter membrane is 0.45 μm.
[0038] In certain embodiments of the present invention, in step 3), the filter membrane is made of nylon or polytetrafluoroethylene (PTFE). Preferably, the filter membrane is made of nylon.
[0039] In certain embodiments of the present invention, in step 3), the filtration pressure is 0.52 kPa to 0.64 kPa. The filtration pressure is selected from any of the following ranges: 0.52 kPa to 0.54 kPa, 0.54 kPa to 0.56 kPa, 0.56 kPa to 0.58 kPa, 0.58 kPa to 0.60 kPa, 0.60 kPa to 0.62 kPa, 0.62 kPa to 0.64 kPa.
[0040] The present invention also provides tobacco clean oil prepared by the above preparation method.
[0041] The present invention also provides the use of the tobacco clean oil in preparing tobacco flavorings.
[0042] The present invention also provides the use of the above tobacco clean oil or the above tobacco flavoring in flavoring cigarettes.
[0043] The present invention also provides a cigarette, which comprises the above-mentioned tobacco clean oil or the above-mentioned tobacco flavoring.
[0044] The following describes the embodiments of the present invention through specific examples, and those skilled in the art can easily understand other advantages and effects of the present invention from the contents disclosed in this specification. The present invention can also be implemented or applied through other different specific embodiments, and the details in this specification can also be modified or changed in various ways based on different viewpoints and applications without departing from the spirit of the present invention.
[0045] Before further describing the specific embodiments of the present invention, it should be understood that the scope of protection of the present invention is not limited to the specific embodiments described below; it should also be understood that the terms used in the examples of the present invention are for describing the specific embodiments rather than for limiting the scope of protection of the present invention; in the present specification and claims, unless otherwise expressly stated herein, the singular forms "a", "an" and "the" include plural forms.
[0046] When the embodiments give numerical ranges, it should be understood that, unless otherwise specified in the present invention, both endpoints of each numerical range and any numerical value between the two endpoints can be selected. Unless otherwise defined, all technical and scientific terms used in the present invention have the same meaning as those generally understood by those skilled in the art. In addition to the specific methods, equipment, and materials used in the embodiments, according to the grasp of the prior art by those skilled in the art and the record of the present invention, any methods, equipment, and materials of the prior art similar or equivalent to the methods, equipment, and materials described in the embodiments of the present invention can also be used to realize the present invention.
[0047] Example 1
[0048] 1) Mix 100L of tobacco extract with 400L of 93% ethanol solvent, stir slowly and thoroughly, and heat at -10℃.
[0049] Let stand for 18 hours, discard the precipitate and take the supernatant;
[0050] 2) Concentrating the supernatant obtained in step 1) under reduced pressure at 50° C., and collecting the concentrate;
[0051] 3) The concentrated liquid obtained in step 2) is filtered at a pressure of 0.60 kPa using a nylon filter membrane with a pore size of 0.45 μm, and the obtained filtrate is the tobacco pure oil.
[0052] Example 2
[0053] 1) Mix 100L of tobacco extract with 400L of 93% ethanol solvent, stir slowly and thoroughly, and heat at -10℃.
[0054] Let stand for 18 hours, discard the precipitate and take the supernatant;
[0055] 2) Concentrating the supernatant obtained in step 1) under reduced pressure at 50° C., and collecting the concentrate;
[0056] 3) The concentrated liquid obtained in step 2) is filtered at a pressure of 0.60 kPa using a nylon filter membrane with a pore size of 0.65 μm, and the obtained filtrate is the tobacco pure oil.
[0057] Example 3
[0058] 1) Mix 100L of tobacco extract with 400L of 93% ethanol solvent, stir slowly and thoroughly, and heat at -10℃.
[0059] Let stand for 18 hours, discard the precipitate and take the supernatant;
[0060] 2) Concentrating the supernatant obtained in step 1) under reduced pressure at 50° C., and collecting the concentrate;
[0061] The concentrated solution obtained in step 2) was filtered at a pressure of 0.60 kPa using a PTFE filter membrane with a pore size of 0.45 μm.
[0062] The obtained filtrate is tobacco pure oil.
[0063] Comparative Example 1
[0064] 1) Mix 100L of tobacco extract with 300L of 93% ethanol solvent, stir slowly and thoroughly, and heat at -10℃.
[0065] Let stand for 18 hours, discard the precipitate and take the supernatant;
[0066] 2) The supernatant obtained in step 1) is concentrated under reduced pressure at 50° C. and the concentrated liquid is collected to obtain the tobacco pure oil.
[0067] Comparative Example 2
[0068] 1) Mix 100L of tobacco extract with 400L of 93% ethanol solvent, stir slowly and thoroughly, and heat at -10℃.
[0069] Let stand for 28 hours, discard the precipitate and take the supernatant;
[0070] 2) The supernatant obtained in step 1) is concentrated under reduced pressure at 50° C. and the concentrated liquid is collected to obtain the tobacco pure oil.
[0071] Comparative Example 3
[0072] 1) Mix 100L of tobacco extract with 400L of 93% ethanol solvent, stir slowly and thoroughly, and heat at -10℃.
[0073] Let stand for 18 hours, discard the precipitate and take the supernatant;
[0074] 2) The supernatant obtained in step 1) is concentrated under reduced pressure at 55° C. and the concentrated liquid is collected to obtain the tobacco pure oil.
[0075] Comparative Example 4
[0076] 1) Mix 100L of tobacco extract with 400L of 93% ethanol solvent, stir slowly and thoroughly, and heat at -10℃.
[0077] Let stand for 18 hours, discard the precipitate and take the supernatant;
[0078] 2) The supernatant obtained in step 1) is concentrated under reduced pressure at 50° C. and the concentrated liquid is collected to obtain the tobacco pure oil.
[0079] Comparative Example 5
[0080] 1) Mix 100L of tobacco extract with 400L of 93% ethanol solvent, stir slowly and thoroughly, and heat at 3000
[0081] Centrifuge at rpm for 15 minutes, discard the precipitate, and take the supernatant;
[0082] 2) The supernatant obtained in step 1) is concentrated under reduced pressure at 50° C. and the concentrated liquid is collected to obtain the tobacco pure oil.
[0083] Application Example 1 Preparation of Cigarettes
[0084] The tobacco pure oil prepared in the above examples and comparative examples was diluted 10 times with 95% ethanol by volume, and injected into blank cigarettes at an addition amount of 10 mg / kg to obtain test cigarette samples. The cigarettes injected with the same amount of 95% ethanol were used as blank cigarette samples, and all cigarette samples were equilibrated in a constant temperature and humidity chamber at 22°C and 60% relative humidity (RH) for 48 hours.
[0085] Application Example 2: Quality evaluation of cigarettes
[0086] All the above cigarette samples were evaluated for sensory quality using the tobacco industry standard YC / T 415-2011 "Sensory Evaluation Method for Tobacco Products".
[0087] The absolute oils prepared in the above examples and comparative examples were subjected to sensory evaluation. Figure 1 It can be seen from the total scores of the sensory evaluation of the examples and the comparative examples that the total scores of the samples of Example 1, Example 2 and Example 3 are significantly higher than those of the other comparative examples, among which the sensory evaluation effect of the sample of Example 1 is the best
[0088] By comparison Figure 2From the sensory evaluation radar chart of the examples and comparative samples, it can be clearly seen that in terms of the various evaluation indicators of aroma characteristics (including aroma quality, aroma quantity, impurities, concentration and permeability), taste characteristics (such as fineness, softness, irritation and residual feeling) and aroma style (flue-cured tobacco aroma and fragrance), Example 1 performs best, followed by Example 2 and Example 3. For Comparative Examples 1 to 5, the prepared clean oil is the preliminary tobacco clean oil prepared without membrane separation operation. Compared with the sensory scores of Examples 1, 2 and 3, these tobacco clean oils that have not been subjected to membrane separation operation are significantly inferior in sensory effects. Therefore, it can be concluded that the clean oils prepared by Examples 1, 2 and 3 after membrane separation operation are superior to tobacco clean oils that have not been subjected to such operation in terms of sensory quality.
[0089] The above examples are for the purpose of illustrating the embodiments disclosed by the present invention and are not to be construed as limiting the present invention. In addition, the various modifications listed herein and the variations of the methods in the invention are obvious to those skilled in the art without departing from the scope and spirit of the present invention. Although the present invention has been specifically described in conjunction with various specific preferred embodiments of the present invention, it should be understood that the present invention should not be limited to these specific embodiments. In fact, various modifications as described above that are obvious to those skilled in the art to obtain the invention should be included within the scope of the present invention.
Claims
1. A method for preparing tobacco oil, characterized in that: The preparation method comprises the following steps: 1) mixing the crude tobacco flavor product with an alcohol solution having a volume fraction of 90% to 95%, allowing the mixture to stand, and collecting the supernatant; 2) concentrating the supernatant obtained in step 1) to remove the alcohol solution, and collecting the concentrate; 3) filtering the concentrated liquid obtained in step 2) through a filter membrane, and the obtained filtrate is the tobacco pure oil.
2. The method for preparing tobacco clean oil according to claim 1, characterized in that: Step 1) includes any one or more of the following conditions: 1) The crude tobacco flavor product is a tobacco extract; 2) the dosage form of the crude tobacco flavor product is selected from tincture, extract or crude absolute oil; 3) The alcohol solution is an ethanol solution.
3. The method for preparing tobacco clean oil according to claim 1, characterized in that: Step 1) includes any one or more of the following conditions: 1) The volume ratio of the crude tobacco flavor product to the alcohol solution is 1:(4-7); 2) The standing time is 16 to 24 hours; 3) The standing temperature is -18℃~-5℃.
4. The method for preparing tobacco clean oil according to claim 1, characterized in that: Step 2) includes any one or more of the following conditions: 1) The concentration temperature is 48°C to 52°C; 2) The concentration method is reduced pressure concentration.
5. The method for preparing tobacco clean oil according to claim 1, characterized in that: Step 3) includes any one or more of the following conditions: 1) The pore size of the filter membrane is 0.40 μm to 0.65 μm; 2) The filter membrane is made of nylon or polytetrafluoroethylene.
6. The method for preparing tobacco clean oil according to claim 1, characterized in that: The filtration pressure in step 3) is 0.52 kPa to 0.64 kPa.
7. The tobacco clean oil prepared by the preparation method according to any one of claims 1 to 6.
8. Use of the tobacco clean oil according to claim 7 in preparing tobacco flavoring.
9. Use of the tobacco clean oil according to claim 7 or the tobacco flavoring according to claim 8 in flavoring cigarettes.
10. A cigarette, characterized in that: The cigarette comprises the tobacco clean oil according to claim 7 or the tobacco flavoring according to claim 8.