Preparation method of tobacco leaf flavonoid pigment and application of tobacco leaf flavonoid pigment in cigarettes
The method enhances flavonoid compound extraction and application in cigarette paper, addressing color stability and environmental issues, improving yield and sensory quality by using ethanol extraction and a two-step dyeing process.
Patent Information
- Application Number
- CN202510461386.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-04-14
- Publication Date
- 2025-07-15
AI Technical Summary
The existing yellow cigarette paper dyes are prone to degradation under factors such as light, heat and oxidation, resulting in uneven color and environmental protection problems during the production process, making it difficult to achieve safety, durability and color consistency.
The flavonoid pigment of tobacco leaves is extracted by ethanol extraction, macroporous resin elution and rotary vaporization, and is applied to cigarette paper through two-step impregnation-dirty processes to improve the extraction rate and purity and ensure color uniformity and environmental protection.
It significantly improves the extraction rate of flavonoid pigments in tobacco leaves and the coloring effect of cigarette paper, improves the comfort and sensory quality of cigarettes, reduces miscellaneous air and irritating reactions, and achieves environmentally friendly production.
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Figure CN120310299A_ABST
Abstract
Description
Technical Field
[0001] The present invention belongs to the technical field of cigarette additives, and particularly relates to a preparation method of tobacco leaf flavonoid pigment and its application in cigarettes. Background Art
[0002] In cigarette production, the appearance color of cigarette paper has always been an important indicator for evaluating product quality. As a colorant, it must not only meet strict safety requirements, but also exhibit excellent coloring effects and outstanding color fastness in variable environments and processing processes. This poses extremely high requirements for the selection of colorant raw materials and processing technologies.
[0003] In the past, the coloring of yellow cigarette paper mainly used natural or synthetic pigments such as chrysanthemum yellow and carotenoids. However, these pigments are generally sensitive to factors such as light, heat, and oxidation in practical applications, and are prone to degradation or fading during production, storage, and even combustion, resulting in problems such as uneven color and insufficient color persistence, directly affecting the appearance quality of cigarette paper. Moreover, their application in the cigarette combustion process will produce certain by-products, which will inevitably have a certain negative impact on taste and smoke comfort.
[0004] To address this issue, caramel pigment has been gradually introduced in the industry as an alternative. Caramel pigment is prepared by heating and coking sugars in an acidic environment. It not only has a low cost and excellent heat resistance, but also shows good stability during the production and combustion of cigarette paper, and can impart an ideal yellow tone to cigarette paper. However, since caramel pigment is essentially a mixture formed by the coking of complex sugars, there are certain differences in its composition and color tone between different batches, resulting in difficulties in strictly controlling color consistency and stability. At the same time, the preparation process under high temperature and acidic conditions will also produce a large amount of waste acid and wastewater, causing environmental problems and increasing the environmental burden of the production process.
[0005] Therefore, how to develop a yellow cigarette paper colorant that takes into account both safety and durability, and can ensure uniform color and an environmentally friendly production process has become the key bottleneck in the current technological development.
[0006] To solve the above problems, the present invention is proposed. Summary of the Invention
[0007] To address the deficiencies of traditional yellow pigments in terms of safety and durability, the present invention proposes a method for preparing a flavonoid pigment from tobacco leaves and its application in cigarettes. By using processes such as ethanol extraction, macroporous resin elution, and rotary evaporation to remove alcohol, not only is the traditional extraction process simplified, but also the extraction rate of the flavonoid pigment from tobacco leaves is significantly increased, from the traditional approximately 9% to 15% - 20%. This greatly improves the utilization rate of raw materials and production efficiency. Secondly, when the prepared flavonoid pigment from tobacco leaves is applied to cigarette paper dyeing, not only does it ensure a good coloring effect, but it also does not cause irritation during the smoking process, can effectively reduce the off-flavors of cigarette paper, and maintain the harmony of the aroma of tobacco leaves, thus improving the overall sensory quality of cigarettes.
[0008] The technical solution adopted by the present invention is as follows:
[0009] In the first aspect of the present invention, a method for preparing a flavonoid pigment from tobacco leaves is provided, and the method includes the following steps:
[0010] Step (1): Take tobacco leaves that have been aged for more than two years, bake them under specific conditions, and then pulverize them to obtain raw material powder.
[0011] Step (2): Mix the raw material powder obtained in step (1) with 50% ethanol in a predetermined ratio, and use ultrasonic-assisted extraction technology to extract 2 - 3 times under specified conditions. After combining and concentrating the filtrates obtained each time, a crude extract of the flavonoid pigment from tobacco leaves is obtained.
[0012] Step (3): Load the crude extract of the flavonoid pigment from tobacco leaves prepared in step (2) onto AB-8 macroporous resin for adsorption, elute it with 60% ethanol at an elution rate of 1 / 3 column volume per minute, gradually collect the eluate rich in yellow components, concentrate the collected eluate by rotary evaporation, use a Buchner funnel to filter and collect the solid part, and then place the collected solid part in an empty drying oven to dry to obtain the flavonoid pigment from tobacco leaves.
[0013] Preferably, in step (1), the tobacco leaves are baked at a controlled temperature of 70 - 80°C for 8 - 10 hours.
[0014] Preferably, in step (2), the raw material powder is fully mixed with 50% ethanol at a ratio of 1 g:10 mL, and ultrasonic-assisted extraction is carried out at room temperature for 2 - 3 times, 1 - 2 hours each time. Then, first use a sterile gauze for rough filtration to collect the liquid part, and then use a Buchner funnel to filter and collect the filtrate. Put the obtained filtrate into a rotary evaporation flask and perform vacuum rotary evaporation until no alcohol flows out to obtain the crude extract of the flavonoid pigment from tobacco leaves.
[0015] Preferably, in step (3), before loading the crude extract of tobacco leaf flavonoid pigment, the AB-8 macroporous resin is first packed into a column by wet packing method for standby. The loading ratio of the crude extract of tobacco leaf flavonoid pigment to the AB-8 macroporous resin is 1 g of crude extract: 10 - 20 mL of resin volume.
[0016] Preferably, in step (3), the rotary evaporation temperature is 40 °C and the rotation speed is 100 revolutions per minute.
[0017] In the second aspect of the present invention, there is provided an application of the tobacco leaf flavonoid pigment obtained by the preparation method described in the first aspect in cigarettes. The cigarette contains a cigarette paper with tobacco leaf flavonoid pigment prepared by the following method:
[0018] (1) Mix dried sour papaya with distilled water at a ratio of 3 g: 100 ml, and perform ultrasonic treatment for 1 h under the temperature control condition of 50 °C. Collect the solution part to obtain the mordant for standby;
[0019] (2) Use distilled water as the solvent to prepare the tobacco leaf flavonoid pigment powder into a dye with a concentration of 10%;
[0020] (3) First, immerse the blank cigarette paper in the aforementioned dye for 20 s, remove the excess liquid and let it dry naturally, then immerse it in the aforementioned mordant for 10 s again, remove the excess liquid and let it dry naturally to obtain the cigarette paper with tobacco leaf flavonoid pigment. The quantitative relationship between the blank cigarette paper and the aforementioned dye and mordant is 37 g of blank cigarette paper: 100 ml of the aforementioned dye: 5 ml of the aforementioned mordant.
[0021] In addition, the aforementioned natural drying means standing in an environment of 25 ± 2 °C and relative humidity of 50% ± 5% until there is no visible liquid on the surface; the blank cigarette paper is an undyed cigarette paper that meets the GB / T 23230 - 2009 standard.
[0022] Preferably, the cigarette containing the cigarette paper with tobacco leaf flavonoid pigment is tested by the sensory evaluation method of GB5606.4 - 2005. Its irritation, comfort and taste scores have no difference from those of the undyed cigarette paper. It can effectively reduce the foreign odor of the cigarette paper without irritation, and the scores of the cigarette aroma coordination and aftertaste are significantly improved.
[0023] The present invention has the following beneficial effects:
[0024] 1. By using the ultrasonic-assisted extraction technology combined with 50% ethanol solvent, the present invention optimizes the dissolution efficiency of tobacco leaf flavonoid pigment. The extraction rate is increased from about 9% of the traditional process to 15% - 20%, and the raw material utilization rate is nearly doubled, reducing the production cost. In addition, the present invention also adopts the AB-8 resin purification process to achieve the efficient separation and enrichment of tobacco leaf flavonoid pigment, avoiding the problems of uneven dyeing caused by impurity residues in the traditional process and affecting the smoking effect of cigarettes.
[0025] 2. The present invention adopts a two-step process of impregnation and mordanting, and specifically selects tobacco leaf flavonoid pigment powder with distilled water as the solvent to prepare a 10% concentration as the dye, achieving uniform dyeing of cigarette paper and avoiding the phenomena of uneven color, spots or color difference in the traditional dyeing process.
[0026] 3. When the tobacco leaf flavonoid pigment of the present invention is applied to cigarettes, there is no difference in the irritation, comfort and taste scores of the cigarettes compared with those made of untreated cigarette paper. The reasons for the significant improvement in the scores of the cigarette aroma coordination and aftertaste are presumably that the polyphenol components in the tobacco leaf flavonoid pigment can neutralize the lignin derivatives generated by the combustion of cigarette paper, thus reducing the intensity of off-flavors. In addition, the tobacco leaf flavonoid pigment prepared by the method of the present invention synergistically interacts with the aroma components of tobacco leaves (such as solanesol and neophytadiene), thus improving the cigarette aroma coordination and aftertaste in the sensory evaluation, making the overall comfort of the cigarettes containing the tobacco leaf flavonoid pigment of the present invention better than that of untreated cigarettes.
[0027] 4. The present invention specifically selects sour papaya as the raw material for the mordant, which can significantly improve the smoking quality of the cigarettes finally containing the tobacco leaf flavonoid pigment of the present invention on the premise of ensuring the dyeing effect. The main reason may be that substances such as polyphenols, organic acids, and enzymes (such as papain) in the mordant extracted from sour papaya form stable complexes with the tobacco leaf flavonoid pigment, promoting the combination between the tobacco leaf flavonoid and the cigarette paper fiber and improving the color fastness. At the same time, in the dyeing system, the active substances in the sour papaya extract may have certain chemical or physical interactions with the tobacco leaf flavonoid, jointly improving the coloring effect and weakening the adverse stimulation that may be caused by the colorant itself. In addition, the polyphenols, organic acids, enzymes and other components in the mordant prepared with sour papaya as the raw material may also help to neutralize or mask some undesirable off-flavors in the cigarettes, making the overall taste and cigarette aroma more coordinated.
[0028] 5. The present invention selects tobacco leaves that have been aged for more than two years and baked at a certain temperature and time as the raw material for preparing the tobacco leaf flavonoid pigment, in order to enable some precursor substances in the tobacco leaves to undergo reactions such as the Maillard reaction, generating flavonoid pigment molecules that are more easily extracted and have stable coloring, thereby improving the coloring effect. In addition, low-temperature baking can also reduce the moisture content in the raw materials, facilitating the contact between the solvent and the target components during the extraction process, and thus improving the extraction rate and purity. In addition, low-temperature baking also helps to volatilize or decompose some impurities and bad volatile components, which not only makes the color of the extract more pure, but also reduces the discomfort and irritation that may occur during smoking, improving the overall smoking experience.
[0029] 6. Through a series of innovative extraction and dyeing processes, the present invention not only realizes the efficient, safe, and environmentally friendly extraction of flavonoid pigments from tobacco leaves, but also successfully applies them to the coloring of cigarette paper, improving the appearance quality of products and the blending effect of cigarette smoke after combustion, thereby providing a new coloring solution for cigarette production. Description of the Drawings
[0030] Figure 1 It is a finished product diagram of a cigarette after applying the flavonoid pigment of tobacco leaves prepared by the method of the present invention in a specific embodiment;
[0031] Figure 2 For Figure 1 Pictures collected at different time periods during the combustion and inhalation process of the shown cigarette sample. Detailed Description of the Invention
[0032] The following further elaborates on the present invention in detail in conjunction with the drawings and embodiments, but the drawings and embodiments do not limit the technical solutions of the present invention.
[0033] Example 1
[0034] This example provides a method for preparing flavonoid pigment of tobacco leaves, including the following steps:
[0035] Step (1): Take tobacco leaves that have been aged for more than two years, bake them at a controlled temperature of 75 °C for 9 h, grind them into powder, collect the powder with a particle size less than or equal to 90 mesh, and obtain the raw material powder;
[0036] Step (2): Use 50% ethanol as the extraction solution, mix it with the raw material powder at a ratio of 1 g:40 ml of 50% ethanol, then perform ultrasonic treatment for 1 hour, first filter it with gauze, and then perform suction filtration with a Buchner funnel (using a 200-mesh filter paper), collect the filtrate, place it in a rotary evaporation flask, and perform rotary evaporation at a rotary evaporation temperature of 40 °C and a rotation speed of 100 revolutions per minute until no liquid flows out to remove the excess alcohol, and obtain the crude extract of flavonoid pigment of tobacco leaves;
[0037] Step (3): Use the wet method to pack the column, pack AB-8 macroporous resin into the column (the height of AB-8 macroporous resin after packing the column is 20 cm), elute it with 60% ethanol at an elution speed of 1 / 3 column volume per minute, collect the solution with a deeper yellow color, perform rotary evaporation at 40 °C, with a rotation speed of 100 revolutions per minute, until no liquid flows out, collect the rotary evaporation solution, then use a Buchner funnel to filter the crystals in the tobacco pigment, and dry it in a vacuum drying oven at 50 °C to obtain the flavonoid pigment of tobacco leaves.
[0038] Application Example 1
[0039] This application example provides the application of the flavonoid pigment of tobacco leaves prepared in Example 1 in cigarettes.
[0040] First, prepare the tobacco leaf flavonoid pigment cigarette paper. The specific steps are as follows:
[0041] (1) Weigh 3 g of dried sour papaya, cut it into small pieces, add it to 100 ml of distilled water, and then ultrasonically treat it for 1 h under the condition of temperature control at 50 °C. Collect the solution part to obtain the mordant.
[0042] (2) Weigh 10 g of the tobacco leaf flavonoid pigment powder prepared in Example 1, dissolve it in 100 ml of distilled water, and obtain the dye after full dissolution. Set it aside for later use.
[0043] (3) First, immerse the blank cigarette paper in the aforementioned dye for 20 s, remove the excess liquid, and let it dry naturally. Then, immerse it in the aforementioned mordant for 10 s again, remove the excess liquid, and let it dry naturally to obtain the tobacco leaf flavonoid pigment cigarette paper, which is marked as the 1# cigarette paper sample. The quantitative relationship between the blank cigarette paper and the aforementioned dye and mordant is 37 g of blank cigarette paper: 100 ml of the aforementioned dye: 5 ml of the aforementioned mordant.
[0044] At the same time, prepare 4 parallel samples according to the above method, and mark them as the 2# cigarette paper sample, 3# cigarette paper sample, 4# cigarette paper sample, and 5# cigarette paper sample in sequence, as Figure 1 shown.
[0045] Test Example 1
[0046] (1) Sensory evaluation test
[0047] First, make the 1#-5# cigarette paper samples into cigarette products by conventional means, and mark them as the 1# cigarette sample - 5# cigarette sample respectively. Then, organize 7 sensory evaluation experts to evaluate the above 5 cigarette samples according to GB5606.4-2005 and take the average value. The results are shown in Table 1 below:
[0048] Table 1 Sensory evaluation results
[0049]
[0050] Among them, the color and luster in the above table refer to whether there are visible changes in the appearance color and luster of the cigarette paper observed by the sensory evaluation experts during the burning process. If there are, it is unstable; if not, it is stable.
[0051] As Figure 2 shown, the pictures successively show the appearance changes of the cigarette from ignition, burning to inhalation. It can be seen that during the burning process of the cigarette, the appearance color and luster of the cigarette paper with tobacco leaf flavonoid pigment have no obvious changes under high temperature conditions, verifying that the tobacco leaf flavonoid pigment prepared by the present invention has good thermal stability and adhesion performance.
[0052] It can be seen that the cigarette paper samples from No. 1 to No. 5 have no negative impact on the irritation, comfort and taste of cigarettes, and show excellent effects in terms of blending cigarette aroma and enhancing aftertaste.
[0053] (2) Accelerated stability test
[0054] Under normal circumstances, after the cigarette is taken out of the cigarette case, it will be smoked immediately. Therefore, this accelerated stability test mainly simulates long-term storage (simulating 1 year), and the acceleration conditions are: 40°C ± 2°C, 75% RH ± 5% RH; the test objects are: cigarette paper samples from No. 1 to No. 5.
[0055] During the accelerated test, samples are taken once a week at 0 days (initial), 7 days, 14 days, 21 days, and 28 days. Then, the L*, a*, and b* values are measured using a color difference meter (HunterLab), and ΔE is calculated according to the ISO 5631 standard. The test results are shown in Table 2 below:
[0056] Table 2 ΔE test results during the accelerated test
[0057]
[0058]
[0059] At the same time, in this embodiment, the ΔE fluctuation between batches of the cigarette paper samples from No. 1 to No. 5 is also tested with the No. 1 cigarette paper sample as the reference object. The test results are shown in Table 3 below:
[0060] Table 3 ΔE test results between batches of the cigarette paper samples from No. 1 to No. 5
[0061]
[0062] Among them: in Table 2 and Table 3, the judgment criteria are: ΔE < 2.0 indicates color stability, and ΔE ≥ 3.0 indicates obvious visible differences to the naked eye.
[0063] Conclusion: As can be seen from Table 2 and Table 3, the tobacco leaf flavonoid pigment cigarette paper prepared by the method of the present invention has stable properties during storage, and the color difference between batches is small, which is suitable for mass production.
[0064] The above is only the specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any person skilled in the art within the technical scope disclosed by the present invention can easily think of changes or substitutions, which should all be covered within the protection scope of the present invention. Therefore, the protection scope of the present invention should be subject to the protection scope of the claims.
Claims
1. A method for preparing flavonoid pigments from tobacco leaves, characterized in that, The method includes the following steps: Step (1): Take tobacco leaves that have been aged for over two years, bake them under specific conditions, and then crush them to obtain raw material powder. Step (2): Mix the raw material powder obtained in step (1) with 50% ethanol in a predetermined ratio, and use ultrasonic-assisted extraction technology to extract 2 - 3 times under specified conditions. After combining and concentrating the filtrates obtained each time, a crude extract of tobacco leaf flavonoid pigment is obtained. Step (3): Load the tobacco leaf flavonoid pigment prepared in step (2) onto AB-8 macroporous resin for adsorption, and elute it with 60% ethanol at an elution rate of 1 / 3 column volume per minute. Gradually collect the eluate rich in yellow components. After concentrating the collected eluate by rotary evaporation, use a Buchner funnel to filter and collect the solid part, and then place the collected solid part in an empty drying oven to dry to obtain the tobacco leaf flavonoid pigment.
2. The preparation method of a tobacco leaf flavonoid pigment according to claim 1, wherein In step (1), the tobacco leaves are baked at a controlled temperature of 70 - 80 °C for 8 - 10 h.
3. The preparation method of a tobacco leaf flavonoid pigment according to claim 1, characterized in that, In step (2), the raw material powder is fully mixed with 50% ethanol at a ratio of 1 g:10 mL, and ultrasonic-assisted extraction is carried out 2 - 3 times at room temperature for 1 - 2 h each time. First, use sterile gauze for rough filtration to collect the liquid part, and then use a Buchner funnel to filter and collect the filtrate. Put the obtained filtrate into a rotary evaporation flask and carry out vacuum rotary evaporation until no alcohol flows out to obtain a crude extract of tobacco leaf flavonoid pigment.
4. The preparation method of a tobacco leaf flavonoid pigment according to claim 1, wherein, In step (3), before loading the crude extract of tobacco leaf flavonoid pigment, first load the AB-8 macroporous resin into a column by wet packing method for standby. The loading ratio of the crude extract of tobacco leaf flavonoid pigment to the AB-8 macroporous resin is 1 g of crude extract:10 - 20 mL of resin volume.
5. The preparation method of a tobacco leaf flavonoid pigment according to claim 1, characterized in that, In step (3), the rotary evaporation temperature is 40 °C and the rotation speed is 100 revolutions per minute.
6. Use of the tobacco leaf flavonoid pigment obtained by the preparation method according to any one of claims 1-5 in cigarettes, characterized in that, The cigarette contains cigarette paper with tobacco leaf flavonoid pigment prepared by the following method: (1) Mix dried sour papaya with distilled water at a ratio of 3 g:100 ml, and carry out ultrasonic treatment for 1 h under a controlled temperature of 50 °C, and collect the solution part to obtain a mordant for standby. (2) Use distilled water as a solvent to prepare a 10% concentration dye with tobacco leaf flavonoid pigment powder for standby. (3) First, immerse the blank cigarette paper in the aforementioned dye for 20 s, remove the excess liquid and let it dry naturally, and then immerse it in the aforementioned mordant for 10 s again, remove the excess liquid and let it dry naturally to obtain the cigarette paper with tobacco leaf flavonoid pigment.
7. The application according to claim 6, characterized in that, The cigarette containing the cigarette paper with tobacco leaf flavonoid pigment is tested by GB5606.4 - 2005 sensory evaluation. Its irritation, comfort and taste scores are not different from those of the non-stained cigarette paper, and it can effectively reduce the off-odor of the cigarette paper without irritation. The scores of cigarette aroma coordination and aftertaste are significantly improved.