Preparation method and application of high-aroma tobacco extract

Abstract

The invention discloses a preparation method and application of a high-aroma tobacco extract, and belongs to the technical field of cigarette tobacco. The extract is prepared by the following steps: mixing a fruit extract with a solvent, spraying the mixture onto tobacco, placing in a sealed manner, heating and baking, extracting at low temperature, filtering with an ultrafiltration membrane, concentrating under reduced pressure, and performing molecular distillation. According to the invention, the baking procedure is increased, so that the concentration of aroma substances is well increased, and heat-sensitive substances are better protected. After a proper amount of the high-aroma tobacco extract provided by the invention is added into tobacco shreds of cigarettes, the cigarettes are rich in aroma, free of burnt flavor, good in aftertaste harmony and aroma permeability, and good in application effect and popularization and application prospect.

Description

Technical Field

[0001] The invention belongs to the technical field of cigarettes and tobacco, and particularly relates to a preparation method and application of a high-aroma tobacco extract. Background Art

[0002] Tobacco extract, extracted from tobacco, contains tobacco's natural aroma compounds. Compared to other natural flavors, tobacco extract blends better with cigarettes, enhancing the aroma and adding to the smoke's satisfaction. High-aroma tobacco extracts, rich in volatile and semi-volatile aroma compounds, are prepared and added to cigarettes to transfer small molecule aroma compounds to their original form, minimizing flavor loss and preserving tobacco's unique aroma and flavor to the greatest extent possible.

[0003] In terms of the preparation of tobacco extracts, common extraction methods include solvent extraction, steam distillation, supercritical extraction, etc. For example: Zheng Saijing et al. used supercritical extraction method to prepare extracts from tobacco stems at 120°C and 20MPa pressure and applied them to cigarettes (Tobacco Science and Technology, 2016, 7, 51-59); in CN104450186A, after the sample was processed by ultrasonic crusher, supercritical extraction technology was used to prepare tobacco flavor substances at 40-55°C and 15-25MPa pressure; in CN102349699A and CN102813278A, solvent extraction method was used to prepare extracts under high temperature heating; CN104705777A discloses a cigarette shredded tobacco containing natural compound, in which tobacco extract was prepared by ASE method at 80-110°C with 60-90% ethanol as extraction solvent.

[0004] The above extraction methods show that heating tobacco extracts helps improve the extraction rate, but higher extraction temperatures damage heat-sensitive and easily oxidized substances. Furthermore, tobacco extracts prepared under these conditions contain highly polar, high-boiling-point, and difficult-to-volatile substances. These substances cannot be effectively atomized at the heating temperature of cigarettes and ultimately remain on the electric heating wire, producing a burnt odor and affecting the quality of the cigarettes. Therefore, further improvements to the preparation methods of tobacco extracts are highly necessary. Summary of the Invention

[0005] The purpose of the present invention is to provide a high-aroma tobacco extract prepared at low temperature by improving the preparation method of tobacco extract, thereby overcoming the defects of existing tobacco extracts such as weak aroma and high content of high-boiling point substances to a certain extent.

[0006] The technical solution adopted by the present invention is as follows: A method for preparing a high-aroma tobacco extract comprises the following steps:

[0007] (1) mixing the fruit extract and propylene glycol uniformly, spraying the mixture evenly on the tobacco, sealing the tobacco after spraying, and then baking;

[0008] (2) crushing the material after baking in step (1), adding anhydrous ethanol to extract; after the extraction is completed, separating from the mixture to obtain an extract;

[0009] (3) passing the extract obtained in step (2) through an ultrafiltration membrane, collecting the permeate and removing the solvent to obtain a concentrate;

[0010] (4) The permeate collected in step (3) is concentrated under reduced pressure, the obtained components are molecularly distilled, and the light components are collected to obtain a high-aroma tobacco extract.

[0011] In the preparation method of the above-mentioned high-aroma tobacco extract, in step (1), the fruit extract is one or more of guava extract, orange extract, and apricot extract, and the mass of the fruit extract is 0.3-0.8% of the mass of the tobacco.

[0012] The preparation method of the above-mentioned high-aroma tobacco extract, in step (1), the preparation method of the fruit extract is as follows: after squeezing the fruit juice, the fruit juice is concentrated under reduced pressure to a density of 1.15-1.25g / cm 3 , obtain fruit juice concentrate, add ethanol, heat and reflux, filter and concentrate under reduced pressure to a density of 1.15-1.25g / cm 3 , to obtain the fruit extract.

[0013] In the above-mentioned method for preparing the high-aroma tobacco extract, in step (1), the mass of the propylene glycol is 3-15% of the mass of the tobacco.

[0014] In the above-mentioned method for preparing the high-aroma tobacco extract, in step (1), the sealed placement time is 8 to 10 hours.

[0015] In the preparation method of the above-mentioned high-aroma tobacco extract, in step (1), the baking is carried out at 90-130° C. for 0.5-1.5 hours.

[0016] In the preparation method of the above-mentioned high-aroma tobacco extract, in step (2), the extraction temperature is 10-35° C. and the extraction time is 5-10 hours.

[0017] In the above-mentioned method for preparing the high-aroma tobacco extract, in step (4), the parameters for molecular distillation are set as follows: pressure of 0.01 to 0.1 mbar, and distillation temperature of 25° C. to 40° C.

[0018] The high-aroma tobacco extract prepared by the above-mentioned preparation method of the high-aroma tobacco extract is used in the preparation of cigarettes, wherein the mass percentage of the high-aroma tobacco extract is 3-5%.

[0019] A cigarette contains the high-aroma tobacco extract prepared by the above-mentioned preparation method of the high-aroma tobacco extract.

[0020] The main technical idea of ​​the present invention is: first, the fruit extract is mixed with tobacco raw materials, and then the mixture is evenly sprayed on the tobacco to pre-treat the tobacco raw materials to improve the tobacco aroma; and in order to avoid excessively high baking temperature during the baking process, which may cause the tobacco leaves to burn and blacken, bringing about an unpleasant odor, propylene glycol is sprayed on the surface of the tobacco raw materials before baking to affect the smoking experience; the low-temperature extraction technology is used to better protect the aroma-causing substances in the tobacco, retaining the original aroma of the tobacco, so that the smoker can feel more of the smell of the cigarette itself rather than the modulated aroma. After the extract is separated by ultrafiltration membrane, polysaccharides and other macromolecular substances in the extract can be better removed, thereby avoiding the potential threat of macromolecular substances adhering to the heating wire when the cigarette is smoked. The application of ultrafiltration membrane effectively removes macromolecular substances such as sugars and proteins in tobacco and high-boiling point substances, effectively retaining the aroma components in tobacco, while avoiding the occurrence of burning due to excessive concentration of sugar substances in the next distillation process, and the viscosity of the extract, which affects the percentage of the extracted substance; finally, secondary separation is carried out through molecular distillation. At this temperature and pressure, the extracted high-aroma tobacco substances have a fragrance closer to the tobacco itself, a higher aroma purity, and the best sensory evaluation quality; it aims to remove high-boiling point and difficult-to-volatile substances in the extract, enrich volatile aroma substances, thereby better improving its aroma effect, and further reducing the possibility of high-boiling point substances adhering to the cigarette heating wire.

[0021] From the above description of the technical principles, it can be seen that the main technical advantages of the present invention are reflected in the following aspects:

[0022] 1. During baking, the reducing sugars in tobacco react with nitrogen-containing compounds to produce substances such as pyrone and furanone, which enhance the baking aroma.

[0023] 2. The dual separation process of membrane separation and molecular distillation is used to effectively remove macromolecular substances such as sugars and proteins, as well as high-boiling-point substances, while effectively increasing the content of tobacco's characteristic aroma components, such as megastigmatrienone, dihydrodamascone, neophytadiene, benzyl alcohol, phenylethyl alcohol, and farnesyl acetone;

[0024] 3. Preliminary application experiments show that the high-aroma tobacco extract provided by the present invention has a strong baking aroma and tobacco aroma, good permeability, and a clean and comfortable taste.

[0025] In general, the present invention increases the concentration of aroma compounds by a good degree; the use of low-temperature extraction technology better maintains the original aroma characteristics of tobacco, while better protecting heat-sensitive substances; further, the use of membrane separation and molecular distillation processes enables the aroma compounds to be better enriched, while better removing macromolecular substances such as sugars, proteins, resins, and high-boiling-point substances such as long-chain aliphatic hydrocarbons in the tobacco extract. After adding an appropriate amount of the high-aroma tobacco extract provided by the present invention to cigarette shreds, the cigarette can be made to have a rich aroma and good aroma permeability, showing a good application effect and having a good prospect for promotion and application. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] Figure 1 is the total ion chromatogram of tobacco extract;

[0027] Figure 2 This is the total ion current diagram of the molecular distillation extract of Example 2;

[0028] Figure 3 This is the total ion current diagram of the molecular distillation extract of Example 12. DETAILED DESCRIPTION DETAILED DESCRIPTION

[0029] The present invention will be further explained below with reference to the embodiments. Before introducing the specific embodiments, some materials and experimental equipment involved in the following embodiments are briefly described as follows.

[0030] Experimental materials:

[0031] Tobacco raw materials are: provided by the applicant;

[0032] Experimental equipment:

[0033] Molecular short-path distillation apparatus VKL70 (Rida GmbH, Germany);

[0034] Rotary evaporator (Shanghai Yuhua);

[0035] Circulating water vacuum pump SHZ-DIII (Shanghai Yuhua);

[0036] 7890A-5977B MSD gas chromatograph / mass spectrometer (Agilent, USA);

[0037] Ceramic membrane separation test machine (Shandong Bona).

[0038] Oscillator (Shanghai Zhicheng);

[0039] Oven (Binder, Germany);

[0040] Experimental reagents:

[0041] Propylene glycol (Sinopharm Reagent);

[0042] Anhydrous ethanol (Tianjin Kemao);

[0043] Acetic acid (purchased from Aladdin website).

[0044] In the following examples, the method for preparing cigarettes to which the high-aroma tobacco extract is added as a flavoring is conventional.

[0045] Example 1

[0046] The present invention provides a method for preparing a high-aroma tobacco extract, which comprises the following steps:

[0047] (1) mixing the fruit extract at a ratio of 0.3 to 0.8% by weight of the tobacco raw material with propylene glycol at a ratio of 3 to 15% by weight of the tobacco raw material, spraying the mixture evenly on the tobacco, sealing the mixture and placing it for 8 to 10 hours, and then baking it at 90 to 130° C. for 0.5 to 1.5 hours;

[0048] (2) crushing the material after baking in step (1), adding anhydrous ethanol to extract; after the extraction is completed, separating from the mixture to obtain an extract; the extraction temperature during the extraction is 10 to 35° C., and the extraction time is 5 to 10 hours;

[0049] (3) passing the extract obtained in step (2) through an ultrafiltration membrane, collecting the permeate and removing the solvent to obtain a concentrate;

[0050] (4) The permeate collected in step (3) is concentrated under reduced pressure, and the obtained components are molecularly distilled, and the light components are collected; the molecular distillation parameters are set as follows: pressure of 0.01 to 0.1 mbar, and distillation temperature of 25° C. to 40° C. to obtain a high-aroma tobacco extract.

[0051] The high-aroma tobacco extract obtained above is added to cigarettes, with the mass percentage of the high-aroma tobacco extract being 3-5%.

[0052] The fruit extract is guava extract, orange extract or apricot extract.

[0053] Preparation method of guava extract:

[0054] After squeezing the guava juice, filter the guava juice and concentrate it under reduced pressure to a density of 1.20±0.05g / cm 3 , to obtain guava juice concentrate, add 4-6 times the volume of 95% ethanol, heat under reflux for 4 hours, filter, and concentrate under reduced pressure to a density of 1.20±0.05g / cm 3 , to obtain guava extract.

[0055] Preparation method of orange extract:

[0056] After squeezing the orange juice, filter the orange juice and concentrate it under reduced pressure to a density of 1.20±0.05g / cm 3 , and then add 4-6 times the volume of 95% ethanol to obtain orange juice concentrate, heat and reflux for 4 hours, filter, and concentrate under reduced pressure to a density of 1.20±0.05g / cm 3 , to obtain orange extract.

[0057] Preparation method of apricot extract:

[0058] After squeezing apricot juice, filter the apricot juice and concentrate it under reduced pressure to a density of 1.20±0.05g / cm 3 , and then add 4-6 times the volume of 95% ethanol to obtain apricot juice concentrate, heat and reflux for 4 hours, filter, and concentrate under reduced pressure to a density of 1.20±0.05g / cm 3 , to obtain apricot extract.

[0059] Example 2

[0060] The present invention provides a method for preparing a high-aroma tobacco extract, which comprises the following steps:

[0061] (1) Mix the guava extract prepared in Example 1 with propylene glycol at a ratio of 0.6% by weight of the tobacco raw material and 8% by weight of the tobacco raw material. After mixing, spray the mixture evenly onto the tobacco. After spraying, seal the mixture and place it for 9 hours, then heat it to 120°C and bake it for 1 hour.

[0062] (2) crushing the material after baking in step (1), adding anhydrous ethanol to extract; after the extraction is completed, separating from the mixture to obtain an extract; the extraction temperature during the extraction is 30° C. and the extraction time is 9 hours;

[0063] (3) passing the extract obtained in step (2) through an ultrafiltration membrane, collecting the permeate and removing the solvent to obtain a concentrate;

[0064] (4) The permeate collected in step (3) is concentrated under reduced pressure, and the obtained components are molecularly distilled, and the light components are collected to obtain a high-aroma tobacco extract; the molecular distillation parameters are set as follows: pressure is 0.01 mbar, and distillation temperature is 35°C.

[0065] The high-aroma tobacco extract obtained above was added to cigarettes, and the mass percentage of the high-aroma tobacco extract was 4.5%.

[0066] Example 3

[0067] The present invention provides a method for preparing a high-aroma tobacco extract, which comprises the following steps:

[0068] (1) The orange extract prepared in Example 1 was mixed with propylene glycol at a ratio of 0.6% by weight of the tobacco raw material and evenly sprayed onto the tobacco. After spraying, the mixture was sealed and placed for 8 hours, and then baked at 100°C for 0.8 hours.

[0069] (2) crushing the material after baking in step (1), adding anhydrous ethanol to extract; after the extraction is completed, separating from the mixture to obtain an extract; the extraction temperature during the extraction is 20° C. and the extraction time is 9 hours;

[0070] (3) passing the extract obtained in step (2) through an ultrafiltration membrane, collecting the permeate and removing the solvent to obtain a concentrate;

[0071] (4) The permeate collected in step (3) is concentrated under reduced pressure, and the obtained components are molecularly distilled, and the light components are collected; the molecular distillation parameters are set as follows: pressure is 0.08 mbar, and distillation temperature is 35°C.

[0072] The high-aroma tobacco extract obtained above was added to cigarettes, and the mass percentage of the high-aroma tobacco extract was 4%.

[0073] Example 4

[0074] The present invention provides a method for preparing a high-aroma tobacco extract, which comprises the following steps:

[0075] (1) Apricot extract was mixed with propylene glycol at a ratio of 0.3% by weight of the tobacco raw material and 15% by weight of the tobacco raw material. The mixture was evenly sprayed on the tobacco. After spraying, the mixture was sealed and placed for 9 hours, and then baked at 100°C for 0.5 hours.

[0076] (2) crushing the material after baking in step (1), adding anhydrous ethanol to extract; after the extraction is completed, separating from the mixture to obtain an extract; the extraction temperature during the extraction is 10° C. and the extraction time is 10 h;

[0077] (3) passing the extract obtained in step (2) through an ultrafiltration membrane, collecting the permeate and removing the solvent to obtain a concentrate;

[0078] (4) The permeate collected in step (3) is concentrated under reduced pressure, and the obtained components are molecularly distilled, and the light components are collected to obtain a high-aroma tobacco extract; the molecular distillation parameters are set as follows: pressure is 0.01 mbar, and distillation temperature is 40°C.

[0079] The high-aroma tobacco extract obtained above was added to cigarettes, and the mass percentage of the high-aroma tobacco extract was 4.1%.

[0080] Example 5

[0081] The present invention provides a method for preparing a high-aroma tobacco extract, which comprises the following steps:

[0082] (1) Mix the guava extract prepared in Example 1 with propylene glycol at a ratio of 0.8% by weight of the tobacco raw material and evenly spray the mixture onto the tobacco. After spraying, seal the mixture and place it for 10 hours, then bake it at 120°C for 0.8 hours.

[0083] (2) crushing the material after baking in step (1), adding anhydrous ethanol to extract; after the extraction is completed, separating from the mixture to obtain an extract; the extraction temperature during the extraction is 20° C. and the extraction time is 8 hours;

[0084] (3) passing the extract obtained in step (2) through an ultrafiltration membrane, collecting the permeate and removing the solvent to obtain a concentrate;

[0085] (4) The permeate collected in step (3) is concentrated under reduced pressure, and the obtained components are molecularly distilled, and the light components are collected to obtain a high-aroma tobacco extract; the molecular distillation parameters are set as follows: pressure is 0.06 mbar, and distillation temperature is 30°C.

[0086] The high-aroma tobacco extract obtained above was added to cigarettes, and the mass percentage of the high-aroma tobacco extract was 4.4%.

[0087] Example 6

[0088] The present invention provides a method for preparing a high-aroma tobacco extract, which comprises the following steps:

[0089] (1) Mix the guava extract prepared in Example 1 with propylene glycol at a ratio of 0.3% by weight of the tobacco raw material and evenly spray the mixture onto the tobacco. After spraying, seal the mixture and place it for 8 hours, then bake it at 90°C for 0.5 hours.

[0090] (2) crushing the material after baking in step (1), adding anhydrous ethanol to extract; after the extraction is completed, separating from the mixture to obtain an extract; the extraction temperature during the extraction is 10° C. and the extraction time is 5 hours;

[0091] (3) passing the extract obtained in step (2) through an ultrafiltration membrane, collecting the permeate and removing the solvent to obtain a concentrate;

[0092] (4) The permeate collected in step (3) is concentrated under reduced pressure, and the obtained components are molecularly distilled, and the light components are collected to obtain a high-aroma tobacco extract; the molecular distillation parameters are set as follows: pressure is 0.1 mbar, and distillation temperature is 25°C.

[0093] The high-aroma tobacco extract obtained above was added to cigarettes, and the mass percentage of the high-aroma tobacco extract was 3.6%.

[0094] Example 7

[0095] The present invention provides a method for preparing a high-aroma tobacco extract, which comprises the following steps:

[0096] (1) Mix the guava extract prepared in Example 1 with propylene glycol at a ratio of 0.4% by weight of the tobacco raw material and 5% by weight of the tobacco raw material. After mixing, spray the mixture evenly on the tobacco. After spraying, seal and place for 8 hours, and then bake at 100°C for 0.5 hours.

[0097] (2) crushing the material after baking in step (1), adding anhydrous ethanol to extract; after the extraction is completed, separating from the mixture to obtain an extract; the extraction temperature during the extraction is 20° C. and the extraction time is 5 hours;

[0098] (3) passing the extract obtained in step (2) through an ultrafiltration membrane, collecting the permeate and removing the solvent to obtain a concentrate;

[0099] (4) The permeate collected in step (3) is concentrated under reduced pressure, and the obtained components are molecularly distilled, and the light components are collected to obtain a high-aroma tobacco extract; the molecular distillation parameters are set as follows: pressure is 0.1 mbar, and distillation temperature is 25°C.

[0100] The high-aroma tobacco extract obtained above was added to cigarettes, and the mass percentage of the high-aroma tobacco extract was 3.8%.

[0101] Example 8

[0102] The present invention provides a method for preparing a high-aroma tobacco extract, which comprises the following steps:

[0103] (1) Mix the guava extract prepared in Example 1 with propylene glycol at a ratio of 0.5% by weight of the tobacco raw material and evenly spray the mixture onto the tobacco. After spraying, seal the mixture and place it for 8 hours, then bake it at 100°C for 0.5 hours.

[0104] (2) crushing the material after baking in step (1), adding anhydrous ethanol to extract; after the extraction is completed, separating from the mixture to obtain an extract; the extraction temperature during the extraction is 20° C. and the extraction time is 5 hours;

[0105] (3) passing the extract obtained in step (2) through an ultrafiltration membrane, collecting the permeate and removing the solvent to obtain a concentrate;

[0106] (4) The permeate collected in step (3) is concentrated under reduced pressure, and the obtained components are molecularly distilled, and the light components are collected to obtain a high-aroma tobacco extract; the molecular distillation parameters are set as follows: pressure is 0.1 mbar, and distillation temperature is 25°C.

[0107] The high-aroma tobacco extract obtained above was added to cigarettes, and the mass percentage of the high-aroma tobacco extract was 3.9%.

[0108] Example 9

[0109] The present invention provides a method for preparing a high-aroma tobacco extract, which comprises the following steps:

[0110] (1) Mix the guava extract prepared in Example 1 at a ratio of 0.6% by weight of the tobacco raw material with propylene glycol at a ratio of 10% by weight of the tobacco raw material, spray the mixture evenly on the tobacco, seal the mixture and place it for 9 hours, and then bake it at 110°C for 1 hour;

[0111] (2) crushing the material after baking in step (1), adding anhydrous ethanol to extract; after the extraction is completed, separating from the mixture to obtain an extract; the extraction temperature during the extraction is 25° C. and the extraction time is 8 hours;

[0112] (3) passing the extract obtained in step (2) through an ultrafiltration membrane, collecting the permeate and removing the solvent to obtain a concentrate;

[0113] (4) The permeate collected in step (3) is concentrated under reduced pressure, and the obtained components are molecularly distilled, and the light components are collected to obtain a high-aroma tobacco extract; the molecular distillation parameters are set as follows: pressure is 0.05 mbar, and distillation temperature is 30°C.

[0114] The high-aroma tobacco extract obtained above was added to cigarettes, and the mass percentage of the high-aroma tobacco extract was 4.0%.

[0115] Example 10

[0116] The present invention provides a method for preparing a high-aroma tobacco extract, which comprises the following steps:

[0117] (1) Mix the guava extract prepared in Example 1 at a ratio of 0.7% by weight of the tobacco raw material with propylene glycol at a ratio of 10% by weight of the tobacco raw material, spray the mixture evenly on the tobacco, seal the mixture and place it for 9 hours, and then bake it at 110°C for 1 hour;

[0118] (2) crushing the material after baking in step (1), adding anhydrous ethanol to extract; after the extraction is completed, separating from the mixture to obtain an extract; the extraction temperature during the extraction is 25° C. and the extraction time is 8 hours;

[0119] (3) passing the extract obtained in step (2) through an ultrafiltration membrane, collecting the permeate and removing the solvent to obtain a concentrate;

[0120] (4) The permeate collected in step (3) is concentrated under reduced pressure, and the obtained components are molecularly distilled, and the light components are collected to obtain a high-aroma tobacco extract; the molecular distillation parameters are set as follows: pressure is 0.05 mbar, and distillation temperature is 35°C.

[0121] The high-aroma tobacco extract obtained above was added to cigarettes, and the mass percentage of the high-aroma tobacco extract was 4.1%.

[0122] Example 11

[0123] The present invention provides a method for preparing a high-aroma tobacco extract, which comprises the following steps:

[0124] (1) Mix the guava extract prepared in Example 1 with propylene glycol at a ratio of 0.7% by weight of the tobacco raw material and evenly spray the mixture onto the tobacco. After spraying, seal the mixture and place it for 9 hours, then bake it at 120°C for 1.5 hours.

[0125] (2) crushing the material after baking in step (1), adding anhydrous ethanol to extract; after the extraction is completed, separating from the mixture to obtain an extract; the extraction temperature during the extraction is 25° C. and the extraction time is 9 hours;

[0126] (3) passing the extract obtained in step (2) through an ultrafiltration membrane, collecting the permeate and removing the solvent to obtain a concentrate;

[0127] (4) The permeate collected in step (3) is concentrated under reduced pressure, and the obtained components are molecularly distilled, and the light components are collected to obtain a high-aroma tobacco extract; the molecular distillation parameters are set as follows: pressure is 0.05 mbar, and distillation temperature is 35°C.

[0128] The high-aroma tobacco extract obtained above was added to cigarettes, and the mass percentage of the high-aroma tobacco extract was 4.3%.

[0129] Example 12

[0130] The present invention provides a method for preparing a high-aroma tobacco extract, which comprises the following steps:

[0131] (1) Mix the guava extract prepared in Example 1 at a ratio of 0.7% by weight of the tobacco raw material with propylene glycol at a ratio of 10% by weight of the tobacco raw material, spray the mixture evenly on the tobacco, seal the mixture and place it for 9 hours, and then bake it at 120°C for 1 hour;

[0132] (2) crushing the material after baking in step (1), adding anhydrous ethanol to extract; after the extraction is completed, separating from the mixture to obtain an extract; the extraction temperature during the extraction is 30° C. and the extraction time is 9 hours;

[0133] (3) passing the extract obtained in step (2) through an ultrafiltration membrane, collecting the permeate and removing the solvent to obtain a concentrate;

[0134] (4) The permeate collected in step (3) is concentrated under reduced pressure, and the obtained components are molecularly distilled, and the light components are collected to obtain a high-aroma tobacco extract; the molecular distillation parameters are set as follows: pressure is 0.01 mbar, and distillation temperature is 35°C.

[0135] The high-aroma tobacco extract obtained above was added to cigarettes, and the mass percentage of the high-aroma tobacco extract was 4.5%.

[0136] Example 13

[0137] The present invention provides a method for preparing a high-aroma tobacco extract, which comprises the following steps:

[0138] (1) Mix the guava extract prepared in Example 1 at a ratio of 0.8% by weight of the tobacco raw material with propylene glycol at a ratio of 15% by weight of the tobacco raw material, spray the mixture evenly on the tobacco, seal the mixture and place it for 10 hours, and then bake it at 130°C for 1.5 hours;

[0139] (2) crushing the material after baking in step (1), adding anhydrous ethanol to extract; after the extraction is completed, separating from the mixture to obtain an extract; the extraction temperature during the extraction is 35° C. and the extraction time is 10 hours;

[0140] (3) passing the extract obtained in step (2) through an ultrafiltration membrane, collecting the permeate and removing the solvent to obtain a concentrate;

[0141] (4) The permeate collected in step (3) is concentrated under reduced pressure, and the obtained components are molecularly distilled, and the light components are collected to obtain a high-aroma tobacco extract; the molecular distillation parameters are set as follows: pressure is 0.01 mbar, and distillation temperature is 30°C.

[0142] The high-aroma tobacco extract obtained above was added to cigarettes, and the mass percentage of the high-aroma tobacco extract was 4.5%.

[0143] Comparative Example

[0144] To demonstrate the technical effect of the high-aroma tobacco extract provided by the present invention, the inventors prepared the tobacco extract using a conventional heating extraction method. The specific extraction process is as follows:

[0145] 1 kg of flue-cured tobacco raw material was extracted by solvent extraction method, with anhydrous ethanol as the solvent, a solid-liquid ratio of 1:10, and heated under reflux for 2 h, and extracted twice;

[0146] After the extraction is completed, the extract is filtered out with a 400-mesh filter cloth, and the extract is concentrated under reduced pressure until there is no solvent to obtain tobacco extract;

[0147] Add 10 times of anhydrous ethanol to the extract, and after it is fully dissolved, place the solution in a refrigerator (-5°C) and freeze it for 20 hours. After the insoluble matter is fully precipitated, filter the filtrate and concentrate it under reduced pressure until there is no solvent to obtain tobacco oil.

[0148] The tobacco clean oil obtained above was added to cigarettes, and the mass percentage of the tobacco clean oil was 19%.

[0149] Example 14 Experimental detection

[0150] Sensory evaluation

[0151] The tobacco extracts provided in Examples 2 to 13 and the comparative example were injected at a dosage of 0.02% into a blank cigarette sample of a certain brand without flavoring or additives. Referring to the sensory evaluation method for finished cigarettes in GB 5606.4-2005, professional sensory quality judges conducted an intrinsic quality evaluation. The evaluation results are shown in the following table:

[0152] Table 1 Sensory evaluation table

[0153] sample luster aroma coordination Miscellaneous gases Stimulate Aftertaste Total score Comparative Example 4.5 28.0 4.5 10.5 17.0 21.5 86.0 Example 2 4.5 29.5 5.0 11.0 18.0 22.5 90.5 Example 3 4.5 28.5 5.0 10.5 18.0 22.0 88.5 Example 4 4.5 28.5 5.0 10.5 17.5 21.5 87.5 Example 5 4.5 29.0 5.0 11.0 18.0 22.0 89.5 Example 6 4.5 28.0 5.0 10.5 17.5 21.5 87.0 Example 7 4.5 28.5 5.0 11.0 17.5 22.0 88.5 Example 8 4.5 29.0 5.0 11.0 17.5 22.0 89.0 Example 9 4.5 29.0 5.0 10.5 17.5 22.0 88.5 Example 10 4.5 29.0 5.0 11.0 18.0 22.0 89.5 Example 11 4.5 29.0 5.0 11.0 17.5 22.0 89.0 Example 12 4.5 29.5 5.0 11.0 18.0 22.0 90.0 Example 13 4.5 29.0 5.0 11.0 18.0 22.0 89.5

[0154] After multiple test analyses and sensory evaluations by professionals, the experimental conditions most significantly impacting yield, combined with the mass percentage of high-aroma tobacco extract, were extraction temperature and extraction time. The experimental conditions that significantly impacted the extract's aroma quality were the fruit extract ratio, propylene glycol ratio, molecular distillation pressure, and molecular distillation temperature. Combining the mass percentage of high-aroma tobacco extract, i.e., the tobacco extract ratio, yielded similar results but with relatively optimal conditions. We ultimately selected the experimental conditions of Examples 2 and 12, which yielded tobacco extracts with superior aroma and effectiveness. The experimental conditions were: tobacco raw material mass ratio of 0.6%-0.7%; propylene glycol ratio of 8%-10%; sealed and standing for 9 hours after spraying; baking temperature of 120°C; baking time of 1 hour; extraction temperature of 30°C; extraction time of 9 hours; molecular distillation pressure of 0.01 mbar; molecular distillation temperature of 35°C; and a high-aroma tobacco extract mass percentage of 4.5%.

[0155] Example 15 Analysis of extract components

[0156] The molecular distillation extracts obtained in Example 2 and Example 12 were analyzed and evaluated using GC-MS.

[0157] GC conditions: DB-5MS column (60 m × 0.25 mm × 0.25 μm), injection port temperature 280°C; temperature program: initial temperature 50°C, hold for 2 min, increase to 280°C at 4°C / min, hold for 20 min; helium flow rate: 1.0 mL / min; injection volume 1 μL; split ratio 5:1;

[0158] MS conditions were as follows: EI temperature 280°C, quadrupole temperature 150°C, ionization voltage 70 eV, solvent delay 4.8 min, and scan range 30–550 AMU. The collected mass spectra were searched against the NIST14 spectral library.

[0159] Pre-injection treatment: Take 1 ml of 0.1042 mg / ml phenylethyl acetate (solvent: dichloromethane) and dilute to volume with 95% ethanol in a 10 ml volumetric flask to form the diluent with internal standard. Dilute the extract 10-fold with the diluent before GC-MS analysis.

[0160] Result Analysis

[0161] from Figure 1-Figure 3 As can be seen from Table 1, the volatile components of the comparative tobacco extract are primarily concentrated in the 5-65 min range, containing a large number of heterocyclic compounds, primarily nicotine, followed by alcohols, ketones, and esters, as well as smaller amounts of lactones, terpenes, hydrocarbons, and acids. The overall peak shape in the chromatogram is shifted, and higher concentrations of larger molecular weight aliphatic compounds such as linolenic acid, linoleic acid, aliphatic hydrocarbons, and other non-volatile substances are more pronounced. Important tobacco flavor compounds such as megastigmatrienone, neophytadiene, and 4-hydroxy-β-dihydrodamascone may be affected, potentially affecting the aroma quality of the product. The extracts obtained in Example 2 and Example 12 had chromatographic peaks concentrated in the 25-55 min region, moderate retention time, relatively few non-volatile substances, obvious peak heights, and rich aroma substances. In addition to containing a large amount of nicotine, common aroma substances in tobacco, such as alcohols, aldehydes, ketones, esters, and lactones, can be detected at high levels. Representative components include DDMP, megastigmatrienone, neophytadiene, and 4-hydroxy-β-dihydrodamascone.

[0162] Table 2 Analysis of aroma substances

[0163]

[0164]

[0165]

[0166]

[0167]

[0168]

[0169] The sensory quality evaluation combined with the GC-MS analysis results demonstrate that, compared to the prior art, the present invention, through improved extraction technology, provides a significantly enhanced tobacco aroma, good aftertaste and harmony, a pure and comfortable mouthfeel, and no burnt taste during prolonged or continuous puffing. In terms of overall improved smoking taste, Examples 2 and 12 demonstrate superior results. Besides ensuring the aroma component content of the high-aroma tobacco extract, the extraction conditions are also optimized.

[0170] The present invention may be summarized in other specific forms that do not violate the spirit or main features of the present invention. Therefore, no matter from which point of view, the above embodiments of the present invention can only be regarded as illustrative of the present invention and not limiting the present invention. The claims indicate the scope of the present invention, while the above description does not indicate the scope of the present invention. Therefore, any changes within the meaning and scope equivalent to the claims of the present invention should be considered as included within the scope of the claims.

Claims

1. A method for preparing a high-aroma tobacco extract, characterized in that: The following steps are involved: (1) mixing the fruit extract and propylene glycol uniformly, spraying the mixture evenly on the tobacco, sealing the tobacco after spraying, and then baking; (2) crushing the material after baking in step (1), adding anhydrous ethanol to extract; after the extraction is completed, separating from the mixture to obtain an extract; (3) passing the extract obtained in step (2) through an ultrafiltration membrane, collecting the permeate and removing the solvent to obtain a concentrate; (4) The permeate collected in step (3) is concentrated under reduced pressure, the obtained components are molecularly distilled, and the light components are collected to obtain a high-aroma tobacco extract.

2. The method for preparing the high-aroma tobacco extract according to claim 1, wherein In step (1), the fruit extract is one or more of guava extract, orange extract, and apricot extract, and the mass of the fruit extract is 0.3-0.8% of the mass of the tobacco.

3. The method for preparing the high-aroma tobacco extract according to claim 1, wherein In step (1), the preparation method of the fruit extract is as follows: after squeezing the fruit juice, the fruit juice is concentrated under reduced pressure to a density of 1.15-1.25 g / cm 3 , obtain fruit juice concentrate, add ethanol, heat and reflux, filter and concentrate under reduced pressure to a density of 1.15-1.25g / cm 3 , to obtain the fruit extract.

4. The method for preparing the high-aroma tobacco extract according to claim 1, wherein In step (1), the mass of the propylene glycol is 3-15% of the mass of the tobacco.

5. The method for preparing the high-aroma tobacco extract according to claim 1, wherein In step (1), the sealed placement time is 8 to 10 hours.

6. The method for preparing the high-aroma tobacco extract according to claim 1, wherein: In step (1), the baking is carried out at 90-130° C. for 0.5-1.5 h.

7. The method for preparing the high-aroma tobacco extract according to claim 1, wherein: In step (2), the extraction temperature is 10-35° C. and the extraction time is 5-10 h.

8. The method for preparing the high-aroma tobacco extract according to claim 1, wherein: In step (4), the parameters for molecular distillation are set as follows: pressure of 0.01 to 0.1 mbar, and distillation temperature of 25° C. to 40° C.

9. Use of the high-aroma tobacco extract prepared by the method for preparing the high-aroma tobacco extract according to any one of claims 1 to 8 in the preparation of cigarettes, characterized in that: The mass percentage of the high-aroma tobacco extract is 3-5%.

10. A cigarette, characterized in that A high-aroma tobacco extract prepared by the method for preparing the high-aroma tobacco extract according to any one of claims 1 to 8.

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