CN113826942B - Preparation method of sun-cured tobacco extract with sweet characteristic and processing method of sun-cured tobacco - Google Patents
Preparation method of sun-cured tobacco extract with sweet characteristic and processing method of sun-cured tobacco Download PDFInfo
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- CN113826942B CN113826942B CN202111270265.XA CN202111270265A CN113826942B CN 113826942 B CN113826942 B CN 113826942B CN 202111270265 A CN202111270265 A CN 202111270265A CN 113826942 B CN113826942 B CN 113826942B
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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
- 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
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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
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/20—Biochemical treatment
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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
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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
- A24B3/14—Forming reconstituted tobacco products, e.g. wrapper materials, sheets, imitation leaves, rods, cakes; Forms of such products
Abstract
The invention provides a preparation method of a dried tobacco extract with sweet characteristic and a processing method of dried tobacco leaves, belonging to the technical field of tobacco flavor and fragrance; (1) extracting tobacco leaf with alcohol, filtering, concentrating the filtrate, and making into sun-cured tobacco concentrated paste; (2) dissolving the sun-cured tobacco concentrated paste, layering, taking the upper layer ointment, adding ethanol 2 for dissolving, adding lead acetate, introducing carbon dioxide, and filtering to obtain sun-cured tobacco filtrate; (3) concentrating the sun-cured tobacco filtrate under reduced pressure to remove ethanol, and preparing a primary paste of sun-cured tobacco absolute oil; (4) vacuum freeze drying for the second time to remove water to obtain dry ointment in the form of sun-cured tobacco solid; (5) performing molecular distillation to obtain light components and heavy components of the sun-cured tobacco extract. The invention can effectively avoid carbonization and coking phenomena in the molecular distillation process, reduce the loss of aroma substances, reduce the green miscellaneous gas and irritation generated by chlorophyll during suction, improve the suction quality and improve the fluidity during molecular distillation.
Description
Technical Field
The invention belongs to the technical field of tobacco flavors and fragrances, and particularly relates to a preparation method of a sweet characteristic sun-cured tobacco extract and a processing method of sun-cured tobacco leaves.
Background
Along with the enhancement of the global smoking control strength, the development environment of tobacco products has been changed greatly and profoundly, the structure of the tobacco products is accelerating to be adjusted towards the development direction of diversification and smokelessness, and the advantages of sun-cured tobacco in traditional cigarettes and novel tobacco products (buccal cigarettes, electronic atomized cigarettes and low-temperature non-combustible cigarettes) are more and more prominent.
The sun-cured tobacco has wide production area and long planting history and almost spreads all over the world. This is the first tobacco variety introduced into china. The tobacco found in the early stage is like yellow flower tobacco, which is called sun-cured tobacco and commonly called soil tobacco. The method for processing the tobacco products is also simpler, generally, the tobacco leaves which are grown mature in the field are picked, tied, hung under eave, aired and dried to form the tobacco leaves, the tobacco leaves are manually made into cigars and tobacco shreds, and the cigars and the tobacco shreds are smoked by a simple smoking set.
The tobacco extract is a dark brown viscous paste, and can be used in tobacco essence to increase natural fragrance of tobacco and improve smoking quality of tobacco. At present, the traditional method is to extract tobacco raw materials by polar solvent and then concentrate the tobacco raw materials into paste or to take clear liquid for concentration after water extract is subjected to alcohol precipitation treatment to obtain the tobacco paste, the tobacco paste obtained by similar process extraction generally has common quality, and the problems of low relative content of aroma components contained in the tobacco paste, large solvent consumption, residue and the like exist, so that the requirements of further development of the tobacco industry can not be met. The tobacco extract is a form of tobacco extract. The tobacco extract can be applied to the technical field of heating non-combustible cigarettes, and is sprayed on a tobacco substrate to adjust the smoke quality of cigarettes.
The prior art discloses a plurality of extraction technologies of tobacco leaf extracts, a molecular distillation technology can effectively extract characteristic aroma components which are rich in raw materials, and a published patent with the publication number of CN105533793A discloses a preparation method of a sun-cured red tobacco extract, which mainly comprises the steps of drying, crushing and screening tobacco leaves, extracting alcohol, concentrating, molecular distillation, preparing and the like to obtain the sun-cured red tobacco extract. The published patent No. CN109700068A discloses a method for preparing sun-cured tobacco absolute oil by a floating oil method and application thereof, ethanol with different concentrations is used as an extracting agent and an extractant, the steps of membrane filtration, petroleum ether extraction and the like of the traditional method are abandoned, macromolecular water-soluble substances such as saccharides, proteins and the like are removed by utilizing an oil-water separation principle, and main aroma components in sun-cured tobacco are retained to the maximum extent.
The published Chinese patent with the application number of CN201310703531.2 discloses a preparation method of a tobacco extract and application of the extract in cigarettes, wherein the application comprises the steps of weighing tobacco raw materials, adding ethanol with the concentration of 70-95% according to the mass ratio of 1: 5-1: 10 of the feed liquid, adding phosphoric acid or sulfuric acid with the mass of 0.5-3% of the tobacco raw materials, and carrying out hot reflux extraction for 1-3 hours at the temperature of 60-90 ℃; filtering the obtained product, cooling and settling, taking supernatant, and concentrating under reduced pressure to obtain extract, namely the tobacco extract. Adding the obtained tobacco extract into a cigarette leaf group, wherein the adding amount is 0.05-0.1% of the weight of the leaf group.
The extraction technology of the tobacco extract in the prior art has the following problems; firstly, the higher water content of the raw material of the extract can reduce the concentration of an extraction solvent, so that the water-soluble saccharides, proteins and the like in the extract are higher, and the molecular distillation process is easy to carbonize, foam and the like; secondly, the air-cured tobacco leaves contain a large amount of fat-soluble plant pigments, and the smoke has green miscellaneous gas and irritation during combustion; thirdly, the concentration is carried out in a heating and pressure reducing mode, and certain loss is caused to aroma components and heat-sensitive substances; fourthly, the technical requirement of the membrane treatment process is high, and the equipment cost is high.
Disclosure of Invention
In view of the above, in order to solve the technical problems that the extraction method of the tobacco extract in the prior art has high saccharide and protein content, affects the molecular distillation process, contains a large amount of fat-soluble plant pigment, and has serious loss of aroma substances, the invention provides a preparation method of a sweet characteristic sun-cured tobacco extract and a processing method of sun-cured tobacco leaves.
The invention relates to a preparation method of a sun-cured tobacco extract with sweet characteristic, which comprises the following steps;
(1) carrying out primary vacuum drying treatment on the aired tobacco leaves to obtain raw material tobacco leaves; the sugar content of sun-cured tobacco leaf is less than 10%, and the water content of raw tobacco leaf is 3-6%. Through vacuum freeze drying, firstly, the loss of heat-sensitive aroma substances caused by heating and drying is avoided, secondly, the moisture can be controlled at a very low level, the dilution of the raw material moisture to an extraction solvent is reduced, the content of water-soluble substances such as protein, starch, saccharides and the like in a subsequent extract is reduced, and the phenomena of carbonization and coking in the high-temperature process of molecular distillation are avoided.
(2) Putting the raw material tobacco leaves into an ethanol 1 solution with the mass fraction of 85-95% for ethanol extraction, extracting fat-soluble substances in the tobacco raw materials mainly by using high-concentration ethanol according to a similar compatibility principle, wherein the effective ingredients in the raw material tobacco leaves are mainly the fat-soluble substances, meanwhile, the fat-soluble plant pigments are also dissolved in the ethanol 1, and the specific process of the ethanol extraction is as follows; mixing raw materials of tobacco leaves and ethanol 1 solution according to the mass ratio of 1: 4-6, extracting at 70-85 deg.C for 1-2 h/time for 2-3 times, filtering with 400-mesh filter cloth, and concentrating the filtrate to density of 1.1-1.2g/cm3The concentration process of the filtrate is carried out under the conditions that the temperature is 60-70 ℃ and the vacuum pressure is 150-.
(3) Adding water into the sun-cured tobacco concentrated paste, wherein the mass ratio of the water to the sun-cured tobacco concentrated paste is (2-4): 1, heating to 40-60 ℃, fully stirring and dissolving to obtain a mixed solution, in the standing process, molecules slowly migrate to an upper layer solution for layering because the density of fat-soluble substances is smaller than that of water, the upper layer forms solid cream which mainly comprises fat-soluble aroma substances, nicotine and the like of active ingredients and fat-soluble chloroplast pigments, the upper layer cream is taken, added with ethanol 2 for dissolving (fully dissolving by stirring at 60-70 ℃), and heated in a waterproof way to dissolve the upper layer cream, the temperature of waterproof heating is 90-95 ℃, and the mass ratio of the ethanol 2 to the upper layer cream is 4-8: 1, adding lead acetate, wherein the adding amount of the lead acetate is 0.01 percent of the mass of the upper-layer ointment, then introducing carbon dioxide, performing cold precipitation, and filtering by using an active carbon material to obtain sun-cured tobacco filtrate. The activated carbon material is one of activated carbon non-woven fabrics with the thickness of 0.2-1.2mm and activated carbon filter cotton with the thickness of 3-8 mm.
The reason for the waterproof heating is that the solubility of the fat-soluble plant pigment in the ethanol is low at normal temperature, the temperature of the whole liquid system needs to be increased by heating, the dissolution rate of the fat-soluble plant pigment is increased, and the waterproof heating aims to prevent the ethanol from heating and splashing.
Dissolving the fat-soluble pigment in ethanol, adding lead acetate to generate precipitate, adsorbing with activated carbon material, and filtering to remove the fat-soluble pigment. And carbon dioxide is introduced to remove the residual lead ions, so that the harm caused by the residual lead ions is avoided.
The small amount of carbon dioxide is used for neutralizing unreacted lead acetate to ensure that lead ions can be completely removed, and in addition, when the lead acetate is left, the lead acetate and carbonate generate lead carbonate precipitate and acetic acid, so that the lead acetate and the acetic acid can react with ethanol to generate a small amount of ethyl acetate, the ethyl acetate is a good solvent and can improve the dissolution of aroma substances, and in addition, the ethyl acetate has fruity flavor and can improve the charm of a final product.
(4) Concentrating the sun-cured tobacco filtrate obtained in the step (3) at 50-70 ℃ and under the pressure of 150-300mba under reduced pressure until no solvent flows out and ethanol is removed, and preparing sun-cured tobacco absolute oil primary paste;
(5) carrying out secondary vacuum freeze drying and dewatering on the sun-cured tobacco absolute oil primary paste in the step (4) to obtain a sun-cured tobacco solid absolute paste; the conditions of the second vacuum freeze drying are as follows: pre-cooling the sun-cured tobacco absolute oil paste at minus 10-minus 30 ℃ for 5-10h, and then carrying out vacuum freeze drying at minus 80-minus 110 ℃ of the cold trap temperature to obtain the sun-cured tobacco solid absolute oil paste with the water content of 2-4%.
(6) And (3) preheating and melting the solid oil paste, and then performing molecular distillation to obtain light components and heavy components of the sun-cured tobacco extract. The conditions of the molecular distillation are as follows: the feeding temperature is 70-80 ℃, the distillation temperature is 120-150 ℃, the condensation temperature is 60-70 ℃, and the vacuum pressure is 4 multiplied by 10-2-4×10-3mbar。
The processing method of the air-cured tobacco leaves based on the foregoing description comprises the following steps: (1) taking fresh tobacco leaves, and carrying out primary tobacco leaf baking, wherein the primary tobacco leaf baking temperature is 38-40 ℃;
(2) redrying the primarily-cured tobacco leaves, wherein the redrying temperature is 40-42 ℃;
(3) spraying a compound enzyme to the redried tobacco leaves for fermentation, wherein the compound enzyme comprises cellulase and protease, the addition amount of the compound enzyme is 2.4-3.8% of the mass of the redried tobacco leaves, and the fermentation temperature is 43-52 ℃; the compound enzyme is sprayed during the fermentation of the tobacco leaves, the conversion amount of organic matters and aroma substances can be increased in the fermentation process, in addition, the content of protein can generate the peculiar smell of feather scorching during the combustion, the combustion characteristic of the tobacco leaves can also be reduced, and the compound enzyme is a precursor of harmful substances such as quinoline, hydrocyanic acid and the like in the smoke. The conversion and degradation of the pigment and cell wall substances are accelerated in the later stage of fermentation, and the generation conversion amount of the aroma substances of the tobacco leaves is improved.
(4) And infiltrating the fermented tobacco leaves into a mixed solution of pectinase and cellulase, and then drying and airing to obtain the aired tobacco leaves. The plant cell wall of the tobacco leaves has abundant pectin and cellulose, and the tobacco leaves are contacted with pectinase and cellulase in advance, so that the structure of the plant cells on the surface layer of the tobacco leaves is damaged, and the dissolution amount of effective substances can be increased in the alcohol extraction process.
The invention has the following beneficial effects;
(1) the air-cured tobacco leaves and the air-cured tobacco absolute oil primary paste are subjected to vacuum freeze drying, so that firstly, the dilution of raw material water to a solvent is avoided, the content of water-soluble saccharides, protein and the like in an extract is reduced, and the phenomena of carbonization and coking in the molecular distillation process are effectively avoided; secondly, the loss of the fragrant substances is reduced.
(2) The existing activated carbon is utilized to remove a large amount of fat-soluble chlorophyll, so that green miscellaneous gas and irritation generated by the chlorophyll during suction are reduced, the suction quality is improved, and the fluidity during molecular distillation is improved, so that the industrial production is easy to realize.
(3) The better effect of separating and enriching the aroma components is achieved through simple process technology integration.
(4) The extraction rate of light components and heavy components can be effectively improved through the pretreatment of the aired tobacco leaves.
Detailed Description
The present invention will be described in detail with reference to specific embodiments. The experimental methods in which specific conditions are not specified in examples are generally commercially available under the conventional conditions and the conditions described in the manual, or under the general-purpose equipment, materials, reagents and the like used under the conditions recommended by the manufacturer, unless otherwise specified. The starting materials required in the following examples and comparative examples are all commercially available.
The sensory evaluation method comprises the following steps: the blank cigarette without added spice is used as a reference, and the cigarette obtained in the examples and the comparative examples is evaluated according to the technical requirements of GB5606.4-2005 cigarette part 4 sensory requirements.
Example 1
The invention relates to a preparation method of a sun-cured tobacco extract with sweet characteristic, which comprises the following steps;
(1) and carrying out primary vacuum drying treatment on the sun-cured tobacco leaves to obtain raw tobacco leaves, wherein the sugar content of the sun-cured tobacco leaves is 10%, and the water content of the raw tobacco leaves is 3%.
(2) Putting the raw material tobacco leaves into an ethanol 1 solution with the mass fraction of 85 percent for ethanol extraction, wherein the specific process of the ethanol extraction is as follows; mixing the raw materials of tobacco leaves and ethanol 1 solution according to the mass ratio of 1: 4, extracting for 3 times at 70 deg.C for 1 h/time, filtering with 400-mesh filter cloth, and concentrating the filtrate to density of 1.1g/cm3The filtrate concentration process is carried out under the conditions of 60 ℃ and 150mbar vacuum pressure;
(3) adding water into the sun-cured tobacco concentrated paste, wherein the mass ratio of the water to the sun-cured tobacco concentrated paste is 2: 1, heating to 40 ℃, fully stirring and dissolving to obtain a mixed solution, standing, layering the solution, taking the upper-layer ointment, adding ethanol 2 for dissolving (fully dissolving by stirring at 65 ℃), heating in a water-proof way to dissolve the upper-layer ointment, wherein the water-proof heating temperature is 90 ℃, and the mass ratio of the ethanol 2 to the upper-layer ointment is 4: 1, adding lead acetate, wherein the adding amount of the lead acetate is 0.01 percent of the mass of the upper-layer ointment, then introducing carbon dioxide, performing cold precipitation, and filtering by using an active carbon material to obtain sun-cured tobacco filtrate. The activated carbon material is an activated carbon non-woven fabric with the thickness of 0.2 mm;
(4) concentrating the sun-cured tobacco filtrate obtained in the step (3) at 50 ℃ and under 150mba pressure until no solvent flows out to remove ethanol, and preparing a primary paste of sun-cured tobacco absolute oil;
(5) and (5) carrying out secondary vacuum freeze drying and water removal on the primary paste of the sun-cured tobacco absolute oil in the step (4) to obtain a sun-cured tobacco solid absolute ointment, wherein the conditions of the secondary vacuum freeze drying are as follows: pre-cooling the sun-cured tobacco absolute oil primary paste for 15h at minus 10 ℃, and then carrying out vacuum freeze drying at the temperature of minus 80 ℃ of a cold trap, wherein the water content of the prepared sun-cured tobacco solid absolute oil paste is 2%;
(6) and (3) preheating and melting the solid oil paste, and then performing molecular distillation to obtain light components and heavy components of the sun-cured tobacco extract. The conditions of the molecular distillation are as follows: the feeding temperature is 70 ℃, the distillation temperature is 120 ℃, the condensation temperature is 60 ℃, and the vacuum pressure is 4 multiplied by 10-2mbar。
The processing method of the air-cured tobacco leaves based on the foregoing description comprises the following steps:
(1) taking fresh tobacco leaves, and carrying out primary tobacco leaf baking, wherein the primary tobacco leaf baking temperature is 38 ℃;
(2) redrying the primarily-cured tobacco leaves, wherein the redrying temperature is 40 ℃;
(3) spraying a compound enzyme to the redried tobacco leaves for fermentation, wherein the compound enzyme comprises cellulase and protease, the addition amount of the compound enzyme is 2.4% of the mass of the redried tobacco leaves, and the fermentation temperature is 43 ℃;
(4) and infiltrating the fermented tobacco leaves into a mixed solution of pectinase and cellulase, and then drying and airing to obtain the aired tobacco leaves.
Analyzing the light components and the heavy components of the sun-cured tobacco obtained in the embodiment, the content of heterocyclic components of the light components of the sun-cured tobacco is high, accounting for 55.0%, and the light components are mainly nicotine; secondly, the acid accounts for 20.7 percent, the content of alcohol and ketone is 16.6 percent, and the sweet feeling effect is obviously improved; the acid component content of the heavy components of the sun-cured tobacco is high and reaches 72.7 percent, and the heavy components mainly comprise acetic acid and 3-methylvaleric acid; the second is hydrocarbons, accounting for 16.0%.
Example 2
The invention relates to a preparation method of a sun-cured tobacco extract with sweet characteristic, which comprises the following steps;
(1) and carrying out primary vacuum drying treatment on the sun-cured tobacco leaves to obtain raw material tobacco leaves, wherein the sugar content of the sun-cured tobacco leaves is 9%, and the water content of the raw material tobacco leaves is 6%.
(2) Putting the raw material tobacco leaves into an ethanol 1 solution with the mass fraction of 95% for ethanol extraction, wherein the specific process of the ethanol extraction is as follows; mixing the raw materials of tobacco leaves and ethanol 1 solution according to the mass ratio of 1: 6, extracting for 2 times at 85 deg.C for 2 h/time, filtering with 400-mesh filter cloth, and concentrating the filtrate to density of 1.2g/cm3The filtrate concentration process is carried out under the conditions that the temperature is 70 ℃ and the vacuum pressure is 200 mbar;
(3) adding water into the sun-cured tobacco concentrated paste, wherein the mass ratio of the water to the sun-cured tobacco concentrated paste is 4: 1, heating to 60 ℃, fully stirring and dissolving to obtain a mixed solution, standing, layering the solution, taking the upper-layer ointment, adding ethanol 2, dissolving (fully dissolving by stirring at 70 ℃), heating in a water-proof way to dissolve the upper-layer ointment, wherein the heating temperature in the water-proof way is 95 ℃, and the mass ratio of the ethanol 2 to the upper-layer ointment is 8: 1, adding lead acetate, wherein the adding amount of the lead acetate is 0.01 percent of the mass of the upper-layer ointment, then introducing carbon dioxide, performing cold precipitation, and filtering by using an active carbon material to obtain sun-cured tobacco filtrate. The activated carbon material is activated carbon non-woven fabric with the thickness of 1.2 mm;
(4) concentrating the sun-cured tobacco filtrate obtained in the step (3) at 70 ℃ and under the pressure of 300mba under reduced pressure until no solvent flows out to remove ethanol, and preparing a primary paste of sun-cured tobacco absolute oil;
(5) and (5) carrying out secondary vacuum freeze drying and water removal on the primary paste of the sun-cured tobacco absolute oil in the step (4) to obtain a sun-cured tobacco solid absolute ointment, wherein the conditions of the secondary vacuum freeze drying are as follows: pre-cooling the sun-cured tobacco absolute oil primary paste at minus 30 ℃ for 10h, and then carrying out vacuum freeze drying at minus 110 ℃ of a cold trap temperature to obtain the sun-cured tobacco solid absolute oil paste with the water content of 4%;
(6) and (3) preheating and melting the solid oil paste, and then performing molecular distillation to obtain light components and heavy components of the sun-cured tobacco extract. The conditions of the molecular distillation are as follows: the feeding temperature is 80 ℃, the distillation temperature is 150 ℃, the condensation temperature is 70 DEG CAir pressure 4X 10-3mbar。
The processing method of the air-cured tobacco leaves based on the foregoing description comprises the following steps:
(1) taking fresh tobacco leaves, and carrying out primary tobacco leaf baking, wherein the primary tobacco leaf baking temperature is 40 ℃;
(2) redrying the primarily-cured tobacco leaves, wherein the redrying temperature is 42 ℃;
(3) spraying a compound enzyme to the redried tobacco leaves for fermentation, wherein the compound enzyme comprises cellulase and protease, the addition amount of the compound enzyme is 3.8% of the mass of the redried tobacco leaves, and the fermentation temperature is 52 ℃;
(4) and infiltrating the fermented tobacco leaves into a mixed solution of pectinase and cellulase, and then drying and airing to obtain the aired tobacco leaves.
Example 3
The invention relates to a preparation method of a sun-cured tobacco extract with sweet characteristic, which comprises the following steps;
(1) and carrying out primary vacuum drying treatment on the sun-cured tobacco leaves to obtain raw material tobacco leaves, wherein the sugar content of the sun-cured tobacco leaves is 10%, and the water content of the raw material tobacco leaves is 5%.
(2) Putting the raw material tobacco leaves into an ethanol 1 solution with the mass fraction of 90 percent for ethanol extraction, wherein the specific process of the ethanol extraction is as follows; mixing the raw materials of tobacco leaves and ethanol 1 solution according to the mass ratio of 1: 5, extracting for 3 times at 80 deg.C for 2 h/time, filtering with 400-mesh filter cloth, and concentrating the filtrate to density of 1.15g/cm3The filtrate concentration process is carried out under the conditions that the temperature is 65 ℃ and the vacuum pressure is 180 mbar;
(3) adding water into the sun-cured tobacco concentrated paste, wherein the mass ratio of the water to the sun-cured tobacco concentrated paste is 3: 1, heating to 50 ℃, fully stirring and dissolving to obtain a mixed solution, standing, layering the solution, taking the upper ointment, adding ethanol 2, dissolving (fully dissolving by stirring at 65 ℃), heating in a water-proof way to dissolve the upper ointment, wherein the water-proof heating temperature is 92 ℃, and the mass ratio of the ethanol 2 to the upper ointment is 6: 1, adding lead acetate, wherein the adding amount of the lead acetate is 0.01 percent of the mass of the upper-layer ointment, then introducing carbon dioxide, performing cold precipitation, and filtering by using an active carbon material to obtain sun-cured tobacco filtrate. The activated carbon material is activated carbon filter cotton with the thickness of 3 mm;
(4) concentrating the sun-cured tobacco filtrate obtained in the step (3) at 65 ℃ and 180mba under reduced pressure until no solvent flows out to remove ethanol, and preparing a primary paste of sun-cured tobacco absolute oil;
(5) and (5) carrying out secondary vacuum freeze drying and water removal on the primary paste of the sun-cured tobacco absolute oil in the step (4) to obtain a sun-cured tobacco solid absolute ointment, wherein the conditions of the secondary vacuum freeze drying are as follows: pre-cooling the sun-cured tobacco absolute oil primary paste for 8h at minus 20 ℃, and then carrying out vacuum freeze drying at the temperature of minus 100 ℃ of a cold trap, wherein the water content of the prepared sun-cured tobacco solid absolute oil paste is 3%;
(6) and (3) preheating and melting the solid oil paste, and then performing molecular distillation to obtain light components and heavy components of the sun-cured tobacco extract. The conditions of the molecular distillation are as follows: the feeding temperature is 75 ℃, the distillation temperature is 140 ℃, the condensation temperature is 65 ℃, and the vacuum pressure is 1 multiplied by 10-2mbar。
The processing method of the air-cured tobacco leaves based on the foregoing description comprises the following steps:
(1) taking fresh tobacco leaves, and carrying out primary tobacco leaf baking at the temperature of 39 ℃;
(2) redrying the primarily-cured tobacco leaves, wherein the redrying temperature is 41;
(3) spraying a compound enzyme to the redried tobacco leaves for fermentation, wherein the compound enzyme comprises cellulase and protease, the addition amount of the compound enzyme is 3.2% of the mass of the redried tobacco leaves, and the fermentation temperature is 48 ℃;
(4) and infiltrating the fermented tobacco leaves into a mixed solution of pectinase and cellulase, and then drying and airing to obtain the aired tobacco leaves.
Example 4
The embodiment is similar to the embodiment 3, and is different from the embodiment 3 in that the mass ratio of water to the sun-cured tobacco concentrated paste in the step (3) is 4: 1, the activated carbon material is activated carbon filter cotton with the thickness of 8 mm.
Comparative example
Comparative example tobacco extract was extracted by the technical method disclosed in CN201310703531.2, and the purity of the tobacco raw material and ethanol used were the same as in example 1.
The light components in the examples 1 to 4 and the extract in the comparative example are used as tobacco essence to be added into a non-burning cigarette, and after the cigarette is prepared, more than 7 persons with smoking qualification certificates in the tobacco industry are asked to smoke, and the results are as follows;
the invention has the following beneficial effects:
(1) the air-cured tobacco leaves and the air-cured tobacco absolute oil primary paste are subjected to vacuum freeze drying, so that firstly, the dilution of raw material water to a solvent is avoided, the content of water-soluble saccharides, protein and the like in an extract is reduced, and the phenomena of carbonization and coking in the molecular distillation process are effectively avoided; secondly, the loss of the fragrant substances is reduced.
(2) The existing activated carbon is utilized to remove a large amount of fat-soluble chlorophyll, so that green miscellaneous gas and irritation generated by the chlorophyll during suction are reduced, the suction quality is improved, and the fluidity during molecular distillation is improved, so that the industrial production is easy to realize.
(3) The good effect of separating and enriching aroma components is achieved through simple process technology integration, the content of heterocyclic components of the light components of the sun-cured tobacco is high, and the heterocyclic components account for 55.0 percent and are mainly nicotine; secondly, the acid accounts for 20.7 percent, the content of alcohol and ketone is 16.6 percent, and the sweet feeling effect is obviously improved; the acid component content of the heavy components of the sun-cured tobacco is high and reaches 72.7 percent, and the heavy components mainly comprise acetic acid and 3-methylvaleric acid; the second is hydrocarbons, accounting for 16.0%.
(4) The extraction rate of light components and heavy components can be effectively improved through the pretreatment of the air-cured tobacco leaves.
The present invention is not limited to the above-described specific embodiments, and various modifications and variations are possible. Any modifications, equivalents, improvements and the like made to the above embodiments in accordance with the technical spirit of the present invention should be included in the scope of the present invention.
Claims (7)
1. A preparation method of a sun-cured tobacco extract with a sweet characteristic is characterized by comprising the following steps;
(1) carrying out first vacuum freeze drying treatment on the aired tobacco leaves to obtain raw material tobacco leaves, wherein the sugar content of the aired tobacco leaves is less than 10%, and the water content of the raw material tobacco leaves is 3-6%;
(2) putting the raw material tobacco leaves into an ethanol 1 solution with the mass fraction of 85-95% for ethanol extraction, then filtering, and concentrating the filtrate to the density of 1.1-1.2g/cm3Preparing sun-cured tobacco concentrated paste, wherein the specific alcohol extraction process is as follows; mixing the raw materials of tobacco leaves and ethanol 1 solution according to the mass ratio of 1: 4-6, extracting at 70-85 deg.C for 1-2 h/time for 2-3 times;
(3) adding water into the sun-cured tobacco concentrated paste to dissolve to obtain a mixed solution, standing, layering the solution, taking the upper layer ointment, adding ethanol 2 to dissolve, heating in water to dissolve the upper layer ointment, adding lead acetate, wherein the addition amount of the lead acetate is 0.01% of the mass of the upper layer ointment, introducing carbon dioxide, performing cold precipitation, and filtering with an active carbon material to obtain sun-cured tobacco filtrate;
(4) concentrating the sun-cured tobacco filtrate obtained in the step (3) under reduced pressure to remove ethanol, and preparing a sun-cured tobacco absolute oil primary paste;
(5) carrying out secondary vacuum freeze drying and dewatering on the sun-cured tobacco absolute oil primary paste in the step (4) to obtain a sun-cured tobacco solid absolute paste;
(6) and (3) preheating and melting the solid oil paste, and then performing molecular distillation to obtain light components and heavy components of the sun-cured tobacco extract.
2. The method for preparing the sun-cured tobacco extract with sweet feeling characteristics according to claim 1, wherein the filtrate concentration process in the step (2) is carried out at the temperature of 60-70 ℃ and the vacuum pressure of 150-.
3. The preparation method of the sun-cured tobacco extract with the sweet characteristic according to claim 1, wherein the mass ratio of the water to the sun-cured tobacco concentrated paste in the step (3) is 2-4: 1.
4. the preparation method of the sweet characteristic sun-cured tobacco extract according to claim 3, wherein the heating temperature in a water-proof way is 90-95 ℃, and the mass ratio of the ethanol 2 to the upper ointment is 4-8: 1.
5. the preparation method of the sun-cured tobacco extract with the sweet characteristic according to claim 1, wherein the activated carbon material is one of activated carbon non-woven fabrics with the thickness of 0.2-1.2mm and activated carbon filter cotton with the thickness of 3-8 mm.
6. The method for preparing the sun-cured tobacco extract with the sweet feeling characteristics according to claim 1, wherein the molecular distillation conditions are as follows: the feeding temperature is 70-80 ℃, the distillation temperature is 120-150 ℃, the condensation temperature is 60-70 ℃, and the vacuum pressure is 4 multiplied by 10-2-4×10-3mbar。
7. The preparation method of the sun-cured tobacco extract with the sweet characteristic according to claim 1, wherein the processing method of the sun-cured tobacco leaves comprises the following steps: (1) taking fresh tobacco leaves, and carrying out primary tobacco leaf curing at the temperature of 38-40 ℃;
(2) redrying the primarily-cured tobacco leaves, wherein the redrying temperature is 40-42 ℃;
(3) spraying a compound enzyme to the redried tobacco leaves for fermentation, wherein the compound enzyme comprises cellulase and protease, the addition amount of the compound enzyme is 2.4-3.8% of the mass of the redried tobacco leaves, and the fermentation temperature is 43-52 ℃;
(4) and infiltrating the fermented tobacco leaves into a mixed solution of pectinase and cellulase, and then drying and airing to obtain the aired tobacco leaves.
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