CN115039901B - Tobacco spice, preparation method thereof and heating cigarette - Google Patents
Tobacco spice, preparation method thereof and heating cigarette Download PDFInfo
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- CN115039901B CN115039901B CN202210544799.5A CN202210544799A CN115039901B CN 115039901 B CN115039901 B CN 115039901B CN 202210544799 A CN202210544799 A CN 202210544799A CN 115039901 B CN115039901 B CN 115039901B
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- 235000002637 Nicotiana tabacum Nutrition 0.000 title claims abstract description 203
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- 238000010438 heat treatment Methods 0.000 title description 24
- 244000061176 Nicotiana tabacum Species 0.000 title 1
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- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 122
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Images
Classifications
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B3/00—Preparing tobacco in the factory
- A24B3/10—Roasting or cooling tobacco
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/24—Treatment of tobacco products or tobacco substitutes by extraction; Tobacco extracts
- A24B15/26—Use of organic solvents for extraction
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B3/00—Preparing tobacco in the factory
- A24B3/12—Steaming, curing, or flavouring tobacco
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B3/00—Preparing tobacco in the factory
- A24B3/18—Other treatment of leaves, e.g. puffing, crimpling, cleaning
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacture Of Tobacco Products (AREA)
Abstract
The invention relates to the technical field of tobacco flavoring, in particular to tobacco flavor, a preparation method thereof and a heated cigarette. The preparation method of the tobacco flavor comprises the following steps: determining a tobacco leaf curing formula, curing and crushing tobacco leaves, and mixing various tobacco leaf powders according to the tobacco leaf curing formula to obtain tobacco powder; placing the tobacco powder in an extraction kettle, and carrying out enzymolysis and supercritical carbon dioxide extraction on the tobacco powder simultaneously, wherein the enzymolysis adopts flavourzyme; desolventizing the material in the separation kettle to obtain a carbon dioxide extract; desolventizing the material in the extraction kettle to obtain first residue; carrying out ethanol supercritical extraction on the first residue in the extraction kettle; desolventizing the material in the separation kettle, and obtaining an ethanol extract after sedimentation and filtration; mixing the carbon dioxide extract and the ethanol extract to obtain the tobacco flavor. The tobacco flavor prepared by the method has comprehensive flavor-imparting components, good applicability and environmental friendliness in the whole process.
Description
Technical Field
The invention relates to the technical field of tobacco flavoring, in particular to tobacco flavor, a preparation method thereof and a heated cigarette.
Background
The tobacco source perfume mainly comprises tobacco essential oil, tobacco extract and tobacco absolute. The preparation method of the tobacco essential oil mainly adopts a traditional steam distillation method; the tobacco extract is mainly prepared by heating, refluxing, extracting and concentrating ethanol; the tobacco absolute is higher, and is a purer extract obtained by further alcohol precipitation after the tobacco is extracted into paste by ethanol solution. The tobacco source flavor prepared by the method only contains partial tobacco flavor components and cannot reflect the actual tobacco flavor. The tobacco leaf flavor style of different types, varieties and producing places has large difference, the raw material sources of the tobacco source flavors sold in the market are unknown, the commercial tobacco source flavors often have blending marks, and the flavor and the taste are contradictory, so the application difficulty in the product is large, and the tobacco source flavors are only slightly applied to supplement the tobacco flavor in the traditional cigarettes.
The burning mode of the heated cigarette is obviously different from that of the traditional cigarette, so that the core material is flavored mainly by tobacco extract and a few low-boiling point essence and spices, and the flavor components escape along with smoke formed by the atomizing agent after heating. Therefore, the heating cigarette has higher demand for tobacco source flavors and higher quality requirements. At present, although the harm index of the heated cigarettes is greatly lower than that of the traditional cigarettes, the smoking taste is far from that of the heated cigarettes, and the heated cigarettes are mainly characterized by outstanding cooking smell, insufficient tobacco fragrance and the like. The main reason is that the tobacco source spice prepared by the prior method is difficult to exert better effect under the condition of low-temperature short-time heating. Therefore, how to provide a tobacco source spice with outstanding tobacco fragrance, good coordination and strong applicability so as to make up the defect of poor smoking quality of the prior heated cigarettes is a technical problem to be solved in the field.
Disclosure of Invention
In order to solve or partially solve the problems existing in the related art, the invention provides a tobacco flavor, a preparation method thereof and a heated cigarette.
The invention provides a preparation method of tobacco flavor, which comprises the following steps:
step a), determining a tobacco leaf curing formula, crushing the cured tobacco leaves, and mixing the powder of various tobacco leaves according to the tobacco leaf curing formula to obtain tobacco powder;
step b), placing the tobacco powder in an extraction kettle, and carrying out enzymolysis and supercritical carbon dioxide extraction on the tobacco powder at the same time, wherein the enzymolysis adopts flavourzyme; after extraction, desolventizing the materials in the separation kettle to obtain a carbon dioxide extract; desolventizing the material in the extraction kettle to obtain first residue;
step c), performing ethanol supercritical extraction on the first residue in the extraction kettle; desolventizing the material in the separation kettle, and obtaining an ethanol extract after sedimentation and filtration; leaching and desolventizing the materials in the extraction kettle to obtain second residues;
and d), mixing the carbon dioxide extract and the ethanol extract to obtain the tobacco flavor.
Further, in the step a), the baking temperature is 40-60 ℃, and the baking is carried out until the moisture content of the leaf group is 5-10%; the granularity of the tobacco powder is 20-40 meshes.
Further, in the step b), the pressure of supercritical carbon dioxide extraction is 10MPa to 30MPa, and the temperature is 35 ℃ to 60 ℃; the extraction method comprises the following steps: firstly, static extraction is carried out for 1 to 3 hours, and then the recirculation extraction is carried out for 1 to 3 hours; the mass volume ratio of the tobacco powder to the carbon dioxide fluid is 1g (1 mL-5 mL);
the mass ratio of the flavourzyme to the tobacco powder is (0.001-0.01): 1.
Further, in the step b), the simultaneous enzymolysis and supercritical carbon dioxide extraction of the tobacco powder are specifically:
introducing carbon dioxide fluid and flavourzyme aqueous solution into the extraction kettle; or,
the mixture of the flavourzyme aqueous solution and the tobacco powder is placed in an extraction kettle, and carbon dioxide fluid is introduced into the extraction kettle.
Further, the vacuum degree of desolventizing treatment of the materials in the separating kettle is-0.01 MPa to-0.08 MPa, and the temperature is 48 ℃ to 55 ℃;
the vacuum degree of desolventizing treatment of the materials in the extraction kettle is-0.01 MPa to-0.08 MPa, and the temperature is 58 ℃ to 65 ℃.
Further, in the step c), the supercritical extraction pressure of the ethanol is 8 MPa-20 MPa, the temperature is 240-300 ℃ and the time is 1-3 h; the mass volume ratio of the tobacco powder to the ethanol is 1g (1 mL-5 mL).
Further, the number of times of supercritical extraction of ethanol in the step c) is two, and the pressure of the second extraction is larger than that of the first extraction; and respectively carrying out desolventizing treatment, sedimentation and filtration on the materials in the separation kettle after twice ethanol supercritical extraction, and then merging to obtain ethanol extracts.
Further, the step d) of mixing the carbon dioxide extract and the ethanol extract further comprises the following steps:
the mixture of carbon dioxide extract and ethanol extract is diluted, and the diluent is the mixture of propylene glycol and glycerol.
The invention also provides a tobacco flavor prepared according to the method of any one of the above.
The invention also provides a heating cigarette which comprises the tobacco flavor.
The preparation method of the tobacco flavor provided by the invention can have the following beneficial effects:
1. the tobacco source spice is extracted by taking the leaf group formula as the raw material, so that the product style of the heated cigarette is conveniently determined, the nicotine content in the tobacco source spice is easy to control, and the applicability of the tobacco source spice in the heated cigarette product is improved. The leaf group formula can be combined with sensory evaluation results according to chemical detection data of single tobacco leaves, so that flexible adjustment of the leaf group is realized, and comprehensive utilization of tobacco leaf raw materials is realized while the quality of tobacco source spice is stable.
2. The method fully utilizes the excellent characteristics of the supercritical fluid, firstly uses nonpolar carbon dioxide to extract natural fragrant substances with weak polarity and nonpolar in tobacco powder, and simultaneously adds flavourzyme, and the protein in the tobacco powder is hydrolyzed into small molecular amino acid under the action of the carbon dioxide fluid; and leaching polar components by using ethanol under supercritical conditions, and simultaneously, using the high-temperature environment of the supercritical ethanol to cause the extracted polar components (including amino acid subjected to enzymolysis) to carry out pyrolysis or rearrangement reaction so as to fully generate more aroma compounds, so that the finally obtained tobacco spice integrates the advantages of tobacco essential oil, extract and absolute oil, and overcomes the defect of uneven release of various aroma components when the cigarettes are heated for a short time. The test proves that: the produced tobacco source spice contains furanone, pyrone sweet flavor components, pyrazine, pyridine, pyrrole and other smoke heterocyclic compounds besides natural essential flavor components, has good aroma richness and high aroma content, and can improve the aroma quality, reduce miscellaneous gas and improve the taste when being used for heating cigarettes.
3. The tobacco residue produced by the invention reaches the waste emission standard after the nicotine content is detected, the tobacco residue can also be used for manufacturing core materials of heating cigarettes, the ethanol and the carbon dioxide used in the extraction process can be recycled, and the whole process is environment-friendly.
It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the invention as claimed.
Drawings
The foregoing and other objects, features and advantages of the invention will be apparent from the following more particular descriptions of exemplary embodiments of the invention as illustrated in the accompanying drawings wherein like reference numbers generally represent like parts throughout the exemplary embodiments of the invention.
FIG. 1 is a GC/MS total ion flow diagram of a carbon dioxide extract prepared in example 1 of the present invention;
FIG. 2 is a GC/MS total ion flow diagram of the ethanol extract prepared in example 1 of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used in this specification and the appended claims, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise. It should also be understood that the term "and/or" as used herein refers to and encompasses any or all possible combinations of one or more of the associated listed items.
It should be understood that although the terms "first," "second," "third," etc. may be used in this disclosure to describe various information, these information should not be limited to these terms. These terms are only used to distinguish one type of information from another. For example, first information may also be referred to as second information, and similarly, second information may also be referred to as first information, without departing from the scope of the invention. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature. In the description of the present invention, the meaning of "a plurality" is two or more, unless explicitly defined otherwise.
The invention provides a preparation method of tobacco flavor, which is characterized in that the tobacco flavor components are comprehensively extracted by adjusting the formulation of tobacco leaves under the premise of ensuring that natural tobacco flavor components are not destroyed, and macromolecules are pyrolyzed under the hot environment of heating cigarettes, so that the tobacco flavor with good applicability is obtained. The tobacco flavor prepared by the method is particularly suitable for heating cigarettes.
Specifically, the preparation method of the tobacco flavor provided by the embodiment of the invention comprises the following steps:
step a), determining a tobacco leaf curing formula, crushing the cured tobacco leaves, and mixing the powder of various tobacco leaves according to the tobacco leaf curing formula to obtain tobacco powder;
step b), placing the tobacco powder in an extraction kettle, and carrying out enzymolysis and supercritical carbon dioxide extraction on the tobacco powder at the same time, wherein the enzymolysis adopts flavourzyme; after extraction, desolventizing the materials in the separation kettle to obtain a carbon dioxide extract; desolventizing the material in the extraction kettle to obtain first residue;
step c), performing ethanol supercritical extraction on the first residue in the extraction kettle; desolventizing the material in the separation kettle, and obtaining an ethanol extract after sedimentation and filtration; leaching and desolventizing the materials in the extraction kettle to obtain second residues;
and d), mixing the carbon dioxide extract and the ethanol extract to obtain the tobacco flavor.
The step a) is a pretreatment step before extraction, and the preparation method of the tobacco flavor provided by the invention takes a leaf formula as a raw material, and the leaf formula is dried and crushed into tobacco powder so as to facilitate the subsequent supercritical extraction process. The tobacco leaves of different types and different producing areas have obvious style difference under the influence of factors such as soil, climate, modulation method and the like, and the flue-cured tobacco has three types of fragrance, strong fragrance and intermediate fragrance from the aspect of fragrance; from the quality of tobacco leaves, the chemical components of nicotine, sugar, total nitrogen, potassium, chlorine and the like in the tobacco leaves in different areas and parts are obviously different, and the influence on the characteristics of smoke such as miscellaneous gases, irritation, richness and the like is larger; therefore, any tobacco leaves are singly used, and the tobacco leaves are reasonably proportioned to form a leaf group, so that the advantages can be exerted, the defects are overcome, the tobacco leaf resources are fully utilized, and the tobacco source spice with high comprehensive quality is produced. In view of this, the present invention selects the cured tobacco formulation as the raw material for treatment. The leaf group formula preferably consists of 5-10 single-material tobacco flakes, and is derived from different producing areas, varieties and positions. The tobacco source spice is extracted by adopting the leaf group formula, so that the product style of the heated cigarette can be determined, the nicotine content in the tobacco source spice is easy to control, and the applicability in the heated cigarette product is improved. The leaf group formula can be combined with sensory evaluation results according to chemical detection data of single tobacco leaves, so that flexible adjustment of the leaf group is realized, and comprehensive utilization of tobacco leaf raw materials is realized while the quality of tobacco source spice is stable. In the step, the baking temperature is preferably 40-60 ℃, and the baking is carried out until the moisture content of the leaf group is 5-10%; pulverizing, and sieving; the particle size of the tobacco powder is preferably 20 to 40 mesh.
Step b) carrying out enzymolysis and supercritical carbon dioxide extraction on the tobacco powder simultaneously. Step c) is a step of continuously performing ethanol supercritical extraction on the first residue after the previous extraction. Carbon dioxide extract and ethanol extract can be obtained through step b) and step c), respectively. Supercritical fluids refer to fluids above their critical temperature and pressure that exhibit many superior characteristics compared to normal liquids, such as similar density, but low viscosity, large diffusion coefficient, strong mass transfer capacity, etc. The method realizes unification of extraction and separation, has the advantages of high efficiency, separability, innocuity, harmlessness, solvent saving and the like, and has incomparable advantages in the aspects of separating natural spice flavor components by traditional methods (distillation, solvent extraction, carbonization and the like). According to the invention, non-and weak-polarity components in the formula tobacco are extracted by supercritical carbon dioxide, enzymolysis of tobacco dust is realized, then tobacco dust residues (namely the first residues) in the last step are extracted by supercritical ethanol, extraction and pyrolysis reaction are realized in a thermal environment of the supercritical ethanol, the obtained extract is subjected to sedimentation and filtration to remove impurities to obtain an ethanol extract, and the carbon dioxide extract and the ethanol extract are mixed to obtain the tobacco source spice.
In the above step b), the enzymolysis and supercritical extraction of the tobacco powder are performed simultaneously. The enzymolysis selects flavourzyme as an enzymolysis agent, can thoroughly degrade the bitter peptide into amino acid and control the bitter taste of the peptide, and on the other hand, the enzyme activity of the enzyme is optimal at the pH value of 6.0-7.0, and is consistent with the acid-base environment of carbon dioxide supercritical extraction, so that the enzyme can be carried out together with the carbon dioxide supercritical extraction and can play a good role in a tobacco powder/carbon dioxide system. The mass ratio of the flavourzyme to the tobacco powder is preferably (0.001-0.01): 1.
The enzymolysis is carried out while carbon dioxide supercritical extraction is carried out, and nonpolar carbon dioxide extracts nonpolar and weakly polar natural components (essential oil components) in the tobacco. During extraction and mass transfer, proteins in the enzymolysis tobacco powder are micromolecular amino acids, most amino acids are remained in tobacco powder residues, and the reaction is carried out under the subsequent ethanol supercritical condition to generate new aroma substances. In the step, the flavourzyme solution can enter the extraction kettle together with the carbon dioxide fluid, and is uniformly mixed with the tobacco powder under the action of the carbon dioxide fluid during static extraction. Or the tobacco powder and the tobacco powder can be added into an extraction kettle in advance, and then carbon dioxide fluid is introduced. Namely, the step can be to introduce a carbon dioxide fluid and an aqueous solution of flavourzyme into the extraction kettle; alternatively, the mixture of the aqueous solution of flavourzyme and tobacco powder is placed in an extraction kettle, and carbon dioxide fluid is introduced into the extraction kettle. The second approach is preferably chosen for time control.
The process conditions for supercritical carbon dioxide extraction are preferably as follows: the supercritical carbon dioxide extraction pressure is 10 MPa-30 MPa, and the temperature is 35-60 ℃; the extraction method comprises the following steps: firstly, static extraction is carried out for 1 to 3 hours, and then the recirculation extraction is carried out for 1 to 3 hours; compared with the cyclic extraction, the static extraction aims to enable the carbon dioxide fluid to fully infiltrate the materials to dissolve the fragrance components, and simultaneously enable the flavourzyme to exert better enzymolysis; the mass volume ratio of the tobacco powder to the carbon dioxide fluid is 1g (1 mL-5 mL).
And after the extraction is finished, desolventizing the separation kettle (extract) and the extraction kettle (extraction residue) respectively, removing carbon dioxide in the extract to obtain a carbon dioxide extract, and removing residual carbon dioxide in residues in the extraction kettle to obtain first residues for subsequent operation. The carbon dioxide after desolventizing can be recycled. Preferably, the vacuum degree of desolventizing treatment of the materials in the separation kettle is-0.01 MPa to-0.08 MPa, and the temperature is 48 ℃ to 55 ℃; the vacuum degree of desolventizing treatment of the materials in the extraction kettle is-0.01 MPa to-0.08 MPa, and the temperature is 58 ℃ to 65 ℃.
Through step b), a carbon dioxide extract enriched in non-polar and weakly polar natural components (essential oil components) of tobacco can be obtained. The extraction residue, i.e., the first residue, still contains more than 70% of polar components such as soluble sugars, nicotine, amino acids, and proteins. The embodiment of the invention continues to carry out the step c), ethanol supercritical extraction is carried out on the first residue, polar components are leached, and simultaneously, the extracted polar components (including amino acid generated in the last step) are subjected to pyrolysis or rearrangement reaction by utilizing the high-temperature environment of supercritical ethanol, so that more aroma compounds are fully generated.
In the above step c), the process conditions of the ethanol supercritical extraction are preferably as follows: the extraction pressure is 8 MPa-20 MPa, the temperature is 240-300 ℃ and the time is 1-3 h; the mass volume ratio of the tobacco powder to the ethanol is 1g (1 mL-5 mL). The temperature range piece is close to the actual heating temperature of the heated cigarettes, and the prepared spice is used for heating the cigarettes, so that the aroma concentration can be improved. Further, the times of ethanol supercritical extraction are two times, the pressure of the second extraction is larger than that of the first extraction, and materials in a separation kettle after the two times of ethanol supercritical extraction are respectively subjected to desolventizing treatment and then combined to obtain ethanol extracts. The ethanol supercritical extraction is carried out twice to realize the full dissolution of the flavor components, and the pressure is increased by the second extraction, so that the nicotine in the tobacco powder is removed. The aim of water leaching of the materials in the extraction kettle is to carry out innocent treatment, so that the content of nicotine in the residue of the tobacco powder reaches the waste discharge standard after detection, and the material can be used for manufacturing core materials of heating cigarettes.
The step c) may specifically be:
introducing absolute ethyl alcohol into the first residue in the extraction kettle, heating to 240-300 ℃, supplementing high-purity nitrogen to reach extraction pressure of 8-20 MPa, opening a receiving valve after extraction, placing ethanol extract into a separation kettle, desolventizing the extraction kettle and the separation kettle at-0.01-0.08 MPa and 50-60 ℃ to obtain a first ethanol extract;
introducing absolute ethyl alcohol into the extraction kettle again, increasing the pressure to be higher than the pressure of the first ethanol supercritical extraction, and opening a material receiving valve to put ethanol extract into the separation kettle after extraction; desolventizing the material in the separation kettle at 50-70 ℃ under-0.01-0.08 MPa to obtain a second ethanol extract; pressurizing, introducing pure water into the materials in the extraction kettle at a flow rate of 4-6 mL/min for leaching, and then desolventizing at 80-90 ℃ under-0.01-0.08 MPa to obtain second residues;
combining the first ethanol extract and the second ethanol extract, settling for 15-20 hours at the temperature of 4-6 ℃, and filtering to obtain the ethanol extract.
The ethanol extract rich in polar components and a plurality of aroma compounds can be obtained through the step c), and finally the carbon dioxide extract and the ethanol extract are mixed according to the step d) to obtain the tobacco flavor. The obtained tobacco flavor integrates the advantages of tobacco essential oil, extract and absolute oil, and overcomes the defect of uneven release of various flavor components when the cigarettes are heated for a short time.
Further, the step d) of mixing the carbon dioxide extract and the ethanol extract further comprises a step of diluting the mixture of the carbon dioxide extract and the ethanol extract, and the diluted mixture can be used for heating the cigarette core material for flavoring according to the process standard. The diluent is a mixture of propylene glycol and glycerol, and the mass ratio of the propylene glycol to the glycerol is preferably (1-3): 1.
From the above, the preparation method of the tobacco flavor provided by the embodiment of the invention has the following advantages:
1. the tobacco source spice is extracted by taking the leaf group formula as the raw material, so that the product style of the heated cigarette is conveniently determined, the nicotine content in the tobacco source spice is easy to control, and the applicability of the tobacco source spice in the heated cigarette product is improved. The leaf group formula can be combined with sensory evaluation results according to chemical detection data of single tobacco leaves, so that flexible adjustment of the leaf group is realized, and comprehensive utilization of tobacco leaf raw materials is realized while the quality of tobacco source spice is stable.
2. The method fully utilizes the excellent characteristics of the supercritical fluid, firstly uses nonpolar carbon dioxide to extract natural fragrant substances with weak polarity and nonpolar in tobacco powder, and simultaneously adds flavourzyme, and the protein in the tobacco powder is hydrolyzed into small molecular amino acid under the action of the carbon dioxide fluid; and leaching polar components by using ethanol under supercritical conditions, and simultaneously, using the high-temperature environment of the supercritical ethanol to cause the extracted polar components (including amino acid subjected to enzymolysis) to carry out pyrolysis or rearrangement reaction so as to fully generate more aroma compounds, so that the finally obtained tobacco spice integrates the advantages of tobacco essential oil, extract and absolute oil, and overcomes the defect of uneven release of various aroma components when the cigarettes are heated for a short time. The test proves that: the produced tobacco source spice contains furanone, pyrone sweet flavor components, pyrazine, pyridine, pyrrole and other smoke heterocyclic compounds besides natural essential flavor components, has good aroma richness and high aroma content, and can improve the aroma quality, reduce miscellaneous gas and improve the taste when being used for heating cigarettes.
3. The tobacco residue produced by the invention reaches the waste emission standard after the nicotine content is detected, the tobacco residue can also be used for manufacturing core materials of heating cigarettes, the ethanol and the carbon dioxide used in the extraction process can be recycled, and the whole process is environment-friendly.
Another embodiment of the present invention also provides a tobacco flavor prepared according to the formulation of the above embodiment. The specific implementation manner is the same as that of the foregoing, and has the same beneficial effects, and will not be repeated.
In addition, another embodiment of the invention also provides a heating cigarette, which comprises the tobacco flavor. The specific implementation manner is the same as that of the foregoing, and has the same beneficial effects, and will not be repeated.
The technical scheme of the invention is further described below with reference to specific examples:
example 1
a. 7 flue-cured tobacco leaves are selected to form a leaf group formula, tobacco flakes are baked at 60 ℃ until the water content is 8%, then the tobacco flakes are crushed to obtain 40-mesh tobacco powder, and all the tobacco powder is weighed and mixed according to the preset leaf group proportion to obtain tobacco powder for standby;
b. weighing 0.2g of flavourzyme, dissolving with 50mL of deionized water, transferring into a beaker containing 200g of tobacco powder, transferring into an extraction kettle after uniformly stirring, and introducing 400mL of CO 2 Performing static extraction on the fluid at 10MPa and 50 ℃ for 1.5h, continuously introducing carbon dioxide, regulating the pressure of the extraction kettle to 30MPa, and controlling the flow rate to be 2.5L/minAfter 2h of cyclic extraction, a receiving valve is opened, the extract is put into a separating kettle and desolventized at-0.01 MPa and 50 ℃ to obtain 4.17g of carbon dioxide extract, materials in the extract are desolventized at-0.01 MPa and 60 ℃ to obtain first residues, the first residues are detected, and the detection results are shown in table 1, and can be seen from table 1: the first residue still contains more than 70% of soluble sugar, nicotine, amino acid and protein polar components;
c. introducing 200mL of absolute ethyl alcohol into the first residue in the extraction kettle, heating to 250 ℃, supplementing high-purity nitrogen to reach extraction pressure of 10MPa, opening a receiving valve after extraction for 2h, placing an ethanol extract into a separation kettle, desolventizing the extraction kettle and the separation kettle at-0.08 MPa and 55 ℃ to obtain 30.43g of first ethanol extract, supplementing the recovered ethanol to 200mL, continuously introducing the ethanol into the extraction kettle, raising the pressure to 15MPa, carrying out supercritical extraction for 1h, collecting the extract, desolventizing at-0.08 MPa and 55 ℃ to obtain 19.85g of second ethanol extract, introducing 200mL of pure water into tobacco powder at a flow rate of 5mL/min under pressure, leaching the tobacco powder at-0.08 MPa and 85 ℃ to obtain second residue, and measuring that the nicotine content before leaching of the second residue is 0.13% and the nicotine content after leaching is 0.02%. Combining the first ethanol extract and the second ethanol extract, settling for 16 hours at 4 ℃ and filtering to obtain 40.24g ethanol extract;
d. mixing the carbon dioxide extract and the ethanol extract, and adding a mixed solvent of propylene glycol and glycerol in a ratio of 2.5:1 to 100g to obtain the tobacco source spice.
The nicotine content of the prepared spice is detected to be about 50mg/g, the nicotine content is only 0.25% after the spice is added according to the proportion of 5% of the mass of the heated cigarette core material, and the nicotine content of the heated cigarette is about 1.2%, so that the proper adding amount can be selected according to the requirement, the aroma mixing difficulty is not increased while the high aroma is ensured, and the spice can be mixed with other monomer spices for use so as to improve the aroma quality.
The chemical composition analysis was performed on the tobacco powder, the first residue and the second residue, and the analysis results are shown in table 1.
Because the carbon dioxide extract and the ethanol extract are mixed and have more components and different content sizes, the chromatographic column is difficult to realize better separation, so that the sample injection analysis is respectively diluted. The carbon dioxide extract and the ethanol extract were diluted 5-fold with absolute ethanol, and the results of GC/MS analysis were shown in Table 2, FIG. 1 and FIG. 2 after passing through a 0.45 μm organic phase filter.
TABLE 1 content of conventional chemical Components for materials of different stages in extraction kettles
| Sample of | Total sugar/% | Reducing sugar/% | Nicotine/% | Chlorine/% | Potassium/% |
| Tobacco powder | 25.39 | 24.75 | 2.81 | 0.54 | 2.56 |
| First residue | 20.52 | 19.66 | 2.15 | 0.47 | 2.13 |
| Second residue (before rinsing) | 5.85 | 4.57 | 0.13 | 0.38 | 1.85 |
| Second residue (after rinsing) | 1.23 | 0.66 | 0.02 | 0.11 | 0.35 |
TABLE 2 composition of tobacco source flavor compounds of the present invention
As can be seen from table 1: the first residue still contains more than 70% of soluble sugar, nicotine, amino acid and protein polar components; about 80% of the water-soluble sugars in the first residue are extracted by ethanol supercritical extraction and continue to participate in the pyrolysis reaction.
As can be seen from table 2: the carbon dioxide extract is mainly a low-polarity component in tobacco, and contains various fatty acids and alkane compounds besides the original aroma component of the tobacco. The ethanol extract contains more aldehyde ketone compounds, especially ketone compounds which generate various cyclopentenyl groups, and the ketone compounds have burnt sweet taste.
As can be seen from fig. 1 and 2: the tobacco flavor prepared in this example has both low boiling point aroma compounds and high boiling point aroma precursors. The aroma substance is derived from the same batch of leaf group formula, has good aroma cooperativity, and is convenient for flavoring.
As can be seen from table 2, fig. 1 and fig. 2: the tobacco source spice of the invention has the advantages of filtering out or pyrolyzing polar macromolecular components, high content of herbal aroma substances of the tobacco, various aroma component types, non-polar components and polar components in the extract,
the European Union defines waste tobacco as "toxic and hazardous waste" and prescribes that the nicotine content after innocent treatment by special chemical and biological methods should not exceed 500mg/kg. After 3 times of extraction (one carbon dioxide supercritical extraction and two times of ethanol supercritical extraction), the nicotine content in the residue is about 1300mg/kg, and the nicotine content in the residue is as low as 200mg/kg after leaching by water, so that the residue can be directly treated as waste.
Example 2
6 flue-cured tobacco leaves are selected to form a leaf group formula, tobacco flakes are baked at 60 ℃ until the water content is 8%, crushed, screened by a 20-mesh sieve to obtain tobacco powder, and 200g of the tobacco powder are weighed and mixed according to a preset formula proportion; weighing 0.5g of flavourzyme, dissolving with 50mL of deionized water, transferring all the ingredients into tobacco powder, stirring uniformly, loading the tobacco powder into an extraction kettle, and introducing 800mL of CO 2 Performing static extraction on fluid at 10MPa and 55 ℃ for 2 hours, continuously introducing liquid carbon dioxide, regulating the pressure of an extraction kettle to 30MPa, circularly extracting at a flow rate of 2.5L/min for 2.5 hours, opening a material receiving valve, placing an extract into a separation kettle, desolventizing at-0.01 MPa and 50 ℃ to obtain 4.51g of carbon dioxide extract, desolventizing at-0.01 MPa and 60 ℃ to obtain first residues; introducing 200mL of absolute ethyl alcohol into the first residue in the extraction kettle, heating to 245 ℃, adjusting the extraction pressure to 10MPa, opening a material receiving valve after 2h of extraction to place an ethanol extract into a separation kettle, desolventizing the extraction kettle and the separation kettle at-0.08 MPa and 55 ℃ to obtain 30.43g of first ethanol extract, supplementing the recovered ethanol to 200mL, and continuously introducing the extractExtracting for 1h under supercritical condition with pressure regulated to 15MPa, collecting extractive solution, desolventizing at-0.08 MPa and 55deg.C to obtain 19.64g of second ethanol extract, desolventizing at-0.08 MPa and 85deg.C to obtain second residue, mixing the two extracts, standing at 4deg.C for 8h, and filtering to obtain 39.36g of ethanol extract b; mixing the carbon dioxide extract and the ethanol extract, and adding a mixed solvent of propylene glycol and glycerol in a ratio of 2.5:1 to 100g to obtain the tobacco flavor.
The tobacco source spice prepared by the embodiment is sprayed on the core material of the heating cigarette according to the mass of 5% of the core material, and is rolled into cigarettes, and compared with the heating cigarette added with the commercial tobacco extract with the same proportion, the tobacco source spice prepared by the embodiment has the advantages of prominent fragrance and sweet smell, obviously improved fragrance quantity and fragrance quality, reduced miscellaneous gas and softer smoke.
Example 3
7 flue-cured tobacco leaves are selected to form a leaf group formula, tobacco flakes are baked at 60 ℃ until the water content is 8%, crushed, sieved by a 40-mesh sieve to obtain tobacco powder, and 200g of the tobacco powder are weighed and mixed according to a preset formula proportion; 1.0g of flavourzyme is weighed, dissolved by 50mL of deionized water, fully transferred into tobacco powder, evenly stirred, transferred into an extraction kettle and introduced with 600mL of CO 2 Extracting fluid to 10MPa at 50 ℃ for 1.5h, continuously introducing carbon dioxide to enable the pressure of an extraction kettle to be 30MPa, circularly extracting for 2h at a flow rate of 2.5L/min, opening a material receiving valve, desolventizing a separating kettle at-0.01 MPa and 50 ℃ to obtain 4.29g of carbon dioxide extract, desolventizing materials in the extract at-0.01 MPa and 60 ℃ to obtain first residue, and decompressing and desolventizing tobacco powder to obtain the first residue; introducing 250mL of absolute ethyl alcohol into the first residue in the extraction kettle, heating to 280 ℃, adjusting the extraction pressure to 10MPa, opening a receiving valve after extracting for 2.5h, placing the extract into a separation kettle, desolventizing the extraction kettle and the separation kettle at-0.08 MPa and 55 ℃ to obtain 30.15g of first ethyl alcohol extract, supplementing the recovered ethyl alcohol to 300mL, continuously introducing into the extraction kettle, increasing the pressure to 15MPa for supercritical extraction for 2h, collecting the extract, desolventizing at-0.08 MPa and 55 ℃ to obtain 20.54g of second ethyl alcohol extract, simultaneously obtaining the second residue after desolventizing at-0.08 MPa and 85 ℃, combining the two extracts, standing at 4 ℃ for 8h, and filtering to obtain 39.85g of ethyl alcohol extractTaking a material; finally, mixing the carbon dioxide extract and the ethanol extract, and adding a 3:1 propylene glycol and glycerol mixed solvent to 100g to obtain the tobacco source spice.
The tobacco flavor prepared by the embodiment is sprayed on the heated cigarette core material by 5% of the mass of the tobacco flavor core material, and is rolled into cigarettes, and compared with the heated cigarettes added with the commercial tobacco extracts in the same proportion, the tobacco flavor prepared by the embodiment has the advantages of prominent fragrance and sweet smell, obviously improved aroma and quality, reduced miscellaneous gases and softer smoke.
The foregoing description of embodiments of the invention has been presented for purposes of illustration and description, and is not intended to be exhaustive or limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the various embodiments described. The terminology used herein was chosen in order to best explain the principles of the embodiments, the practical application, or the improvement of technology in the marketplace, or to enable others of ordinary skill in the art to understand the embodiments disclosed herein.
Claims (8)
1. A method for preparing tobacco flavor, which is characterized by comprising the following steps:
step a), determining a tobacco leaf curing formula, crushing the cured tobacco leaves, and mixing the powder of various tobacco leaves according to the tobacco leaf curing formula to obtain tobacco powder;
step b), placing the tobacco powder in an extraction kettle, and carrying out enzymolysis and supercritical carbon dioxide extraction on the tobacco powder at the same time, wherein the enzymolysis adopts flavourzyme; after extraction, desolventizing the materials in the separation kettle to obtain a carbon dioxide extract; desolventizing the material in the extraction kettle to obtain first residue;
step c), performing ethanol supercritical extraction on the first residue in the extraction kettle; the supercritical extraction pressure of the ethanol is 8MPa to 20MPa, the temperature is 240 ℃ to 300 ℃ and the time is 1h to 3h; the mass volume ratio of the tobacco powder to the ethanol is 1g (1 mL-5 mL); the times of ethanol supercritical extraction are two times, and the pressure of the second extraction is larger than that of the first extraction; respectively carrying out desolventizing treatment, sedimentation and filtration on materials in a separation kettle after twice ethanol supercritical extraction, and then merging to obtain ethanol extracts; leaching and desolventizing the materials in the extraction kettle to obtain second residues;
and d), mixing the carbon dioxide extract and the ethanol extract to obtain the tobacco flavor.
2. The method for preparing tobacco flavor according to claim 1, wherein in the step a), the baking temperature is 40-60 ℃, and the moisture content of the leaf group is 5-10%; the granularity of the tobacco powder is 20-40 meshes.
3. The method for preparing tobacco flavor according to claim 1, wherein,
in the step b), the supercritical carbon dioxide extraction pressure is 10 MPa-30 MPa, and the temperature is 35-60 ℃; the extraction method comprises the following steps: firstly, static extraction is carried out for 1 to 3 hours, and then the recirculation extraction is carried out for 1 to 3 hours; the mass volume ratio of the tobacco powder to the carbon dioxide fluid is 1g (1 mL-5 mL);
the mass ratio of the flavourzyme to the tobacco powder is (0.001-0.01): 1.
4. A method for preparing a tobacco flavor according to claim 3, characterized in that in step b), the simultaneous enzymolysis and supercritical carbon dioxide extraction of the tobacco powder is specifically:
introducing carbon dioxide fluid and flavourzyme aqueous solution into the extraction kettle; or,
the mixture of the flavourzyme aqueous solution and the tobacco powder is placed in an extraction kettle, and carbon dioxide fluid is introduced into the extraction kettle.
5. The method for preparing tobacco flavor according to claim 1, wherein,
the vacuum degree of desolventizing treatment of the materials in the separation kettle is-0.01 MPa to-0.08 MPa, and the temperature is 48 ℃ to 55 ℃;
the vacuum degree of desolventizing treatment of the materials in the extraction kettle is-0.01 MPa to-0.08 MPa, and the temperature is 58 ℃ to 65 ℃.
6. The method of claim 1, wherein the step d) of mixing the carbon dioxide extract and the ethanol extract further comprises the steps of:
the mixture of carbon dioxide extract and ethanol extract is diluted, and the diluent is the mixture of propylene glycol and glycerol.
7. A tobacco flavor, characterized in that it is prepared according to the method of any one of claims 1 to 6.
8. A heated cigarette comprising the tobacco flavor of claim 7.
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