CN115633799B - Spice for increasing tobacco fragrance of heated flue-cured cigarettes and preparation method thereof - Google Patents
Spice for increasing tobacco fragrance of heated flue-cured cigarettes and preparation method thereof Download PDFInfo
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- 241000208125 Nicotiana Species 0.000 title claims abstract description 103
- 235000002637 Nicotiana tabacum Nutrition 0.000 title claims abstract description 103
- 235000019504 cigarettes Nutrition 0.000 title claims abstract description 55
- 235000013599 spices Nutrition 0.000 title claims abstract description 29
- 239000003205 fragrance Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000000926 separation method Methods 0.000 claims abstract description 116
- 239000012528 membrane Substances 0.000 claims abstract description 108
- 239000000284 extract Substances 0.000 claims abstract description 49
- 239000012466 permeate Substances 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 14
- 239000000919 ceramic Substances 0.000 claims abstract description 12
- 238000010828 elution Methods 0.000 claims description 81
- 239000012530 fluid Substances 0.000 claims description 48
- 238000004440 column chromatography Methods 0.000 claims description 42
- 239000000796 flavoring agent Substances 0.000 claims description 31
- 235000019634 flavors Nutrition 0.000 claims description 31
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
- 239000003480 eluent Substances 0.000 claims description 18
- 229920005654 Sephadex Polymers 0.000 claims description 17
- 239000012507 Sephadex™ Substances 0.000 claims description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 15
- 239000000741 silica gel Substances 0.000 claims description 15
- 229910002027 silica gel Inorganic materials 0.000 claims description 15
- 238000012856 packing Methods 0.000 claims description 14
- 238000013375 chromatographic separation Methods 0.000 claims description 10
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 10
- 239000000779 smoke Substances 0.000 claims description 8
- 239000011148 porous material Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 230000002708 enhancing effect Effects 0.000 claims description 3
- 238000013329 compounding Methods 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 229940098465 tincture Drugs 0.000 claims description 2
- 238000000552 two-dimensional column chromatography Methods 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 3
- 235000019505 tobacco product Nutrition 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 7
- 229940055329 tobacco leaf extract Drugs 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 6
- 230000001953 sensory effect Effects 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 238000004821 distillation Methods 0.000 description 5
- 238000011156 evaluation Methods 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- 235000019658 bitter taste Nutrition 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000012465 retentate Substances 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 239000003571 electronic cigarette Substances 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 239000000499 gel Substances 0.000 description 2
- XELZGAJCZANUQH-UHFFFAOYSA-N methyl 1-acetylthieno[3,2-c]pyrazole-5-carboxylate Chemical compound CC(=O)N1N=CC2=C1C=C(C(=O)OC)S2 XELZGAJCZANUQH-UHFFFAOYSA-N 0.000 description 2
- 239000002304 perfume Substances 0.000 description 2
- 235000019605 sweet taste sensations Nutrition 0.000 description 2
- 206010013911 Dysgeusia Diseases 0.000 description 1
- 229930091371 Fructose Natural products 0.000 description 1
- RFSUNEUAIZKAJO-ARQDHWQXSA-N Fructose Chemical compound OC[C@H]1O[C@](O)(CO)[C@@H](O)[C@@H]1O RFSUNEUAIZKAJO-ARQDHWQXSA-N 0.000 description 1
- 239000005715 Fructose Substances 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 239000011269 tar Substances 0.000 description 1
- 239000002641 tar oil Substances 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
- 239000000341 volatile oil Substances 0.000 description 1
- 239000001993 wax Substances 0.000 description 1
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- Manufacture Of Tobacco Products (AREA)
Abstract
The invention relates to a spice for increasing the tobacco fragrance of a heated flue-cured cigarette and a preparation method thereof, belonging to the technical field of flavoring of tobacco products. According to the invention, a Zimbabwe tobacco extract solution is subjected to membrane separation by sequentially adopting a 50nm ceramic membrane, a 10nm ceramic membrane and a 1kDa rolled organic membrane, permeate of each stage of membrane separation is used as a raw material of lower stage membrane separation, permeate of the last stage of membrane separation is concentrated and subjected to two-dimensional column chromatography separation, and two-dimensional 40-64min fractions corresponding to one-dimensional 0-38min fractions, two-dimensional 31-42min fractions corresponding to one-dimensional 38-51min fractions, two-dimensional 65-84min fractions corresponding to one-dimensional 51-77min fractions and two-dimensional 55-67min fractions corresponding to one-dimensional 77-200min fractions are collected and compounded with each stage of membrane separation trapped liquid. The method can effectively remove organoleptic components, and fully highlight the characteristics of Zimbabwe tobacco extract.
Description
Technical Field
The invention relates to a spice for increasing the tobacco fragrance of a heated flue-cured cigarette and a preparation method thereof, belonging to the technical field of flavoring of tobacco products.
Background
The heating cigarette product has the outstanding problem of weak tobacco flavor characteristics, and compared with the traditional cigarette, the environment temperature of the tobacco material in the consumption process of the heating cigarette is lower. The temperature of the combustion cone of the traditional cigarette can reach 950 ℃ at most, the cut tobacco of the cigarette can form thousands of products through complicated reaction paths such as distillation, cracking, combustion and the like, for heating the cigarette, the temperature of the tobacco material is generally lower than 500 ℃ when the cigarette is used by consumers, and smoke is mainly generated through the pyrolysis reaction of the tobacco material. The method has the advantages that the release amount of tar and harmful components of the heated cigarette is obviously lower than that of the traditional cigarette, but the heated cigarette has the defect of weak tobacco flavor characteristics.
The tobacco extract is a spice extracted from tobacco leaves serving as raw materials, and has the effects of supplementing characteristic aroma of tobacco and penetrating fuming herbal aroma. Among tobacco extracts obtained from various different tobacco leaves, zimbabwe tobacco extract is always regarded as a top grade product in flavoring of cigarettes due to characteristics of plump fragrance, purity, comfortable aftertaste and the like, and is favored by the cigarette industry, so that the Zimbabwe tobacco extract becomes an indispensable raw material for high-grade cigarettes.
The Zimbabwe tobacco extract can enhance the flue-cured tobacco fragrance, sweet fragrance and baking fragrance, improve sweet taste, increase richness, reduce miscellaneous gases and other various organoleptic characteristics, wherein the increase of the flue-cured tobacco fragrance is the most main characteristic. In the face of the trend of annual decline of the yield of Zimbabwe tobacco leaves, industry researchers take different means to improve the quality and utilization efficiency of Zimbabwe tobacco extract products, such as the preparation of Zimbabwe tobacco essential oil by reduced pressure distillation; preparing Zimbabwe tobacco extract by membrane separation; the Zimbabwe tobacco tar oil is prepared by macroporous adsorption resin, wherein the extract treated by membrane separation or macroporous adsorption resin is mostly used for enhancing the application of the extract in electronic cigarette products. Although these treatments are capable of removing to some extent undesirable components of the extract, such as macromolecular substances like waxes, proteins, etc., the organoleptic characteristics of the extract obtained are not sufficiently outstanding; the application of the Zimbabwe tobacco extract in electronic cigarette products is enhanced by adopting membrane separation or macroporous adsorption resin and the like to treat the Zimbabwe tobacco extract, and the application of the Zimbabwe tobacco extract in heating cigarettes is not high by purposefully removing fructose, glucose and other components beneficial to the traditional cigarette sense.
Disclosure of Invention
The invention aims to provide a preparation method of a spice for increasing the tobacco fragrance of flue-cured tobacco of a heated cigarette, which can fully highlight the characteristics of Zimbabwe tobacco extract and remarkably improve the applicability of the spice in the heated cigarette.
The invention also provides a spice for increasing the tobacco fragrance of the heated flue-cured cigarettes, which is prepared by the preparation method.
In order to achieve the above purpose, the technical scheme adopted by the preparation method for adding the incense layer for heating the flue-cured tobacco fragrance of the cigarettes is as follows:
a preparation method of a spice for increasing the tobacco fragrance of heated tobacco, comprising the following steps:
1) Carrying out first-stage membrane separation on Zimbabwe tobacco extract solution by adopting a ceramic membrane with the pore diameter of 50nm, then carrying out second-stage membrane separation on permeate by adopting a ceramic membrane with the pore diameter of 10nm, and then carrying out third-stage membrane separation on permeate separated by the second-stage membrane by adopting a coiled organic membrane with the interception molecular weight of 1 kDa;
2) Concentrating the permeate liquid of the third-stage membrane separation to obtain concentrated liquid; then carrying out two-dimensional column chromatographic separation on the obtained concentrated solution; the packing of the first dimension chromatographic column is sephadex, and the length-diameter ratio of the sephadex column is 8:1; the packing of the second dimension chromatographic column is C18 reverse phase silica gel, and the length-diameter ratio of the C18 reverse phase silica gel column is 23:1;
During the first dimension column chromatography separation, water is used as an eluent, the flow rate of the eluent corresponding to each 250 pi mL volume column bed is controlled to be 8mL/min, and the fractions of the elution time period from 0min to 38min, the fractions of the elution time period from 38min to 51min, the fractions of the elution time period from 51min to 77min and the fractions of the elution time period from 77min to 200min are respectively collected;
During the second dimension column chromatography separation, enabling the fractions collected during the first dimension column chromatography separation to enter the second dimension column chromatography respectively, taking an ethanol water solution with the ethanol volume fraction of 90% as an eluent, controlling the flow rate of the eluent corresponding to each 46 pi mL volume column bed to be 8mL/min, and collecting the fractions corresponding to the elution time periods of 0 min-38 min in the two dimension column chromatography separation, the fractions corresponding to the elution time periods of 38 min-51 min in the two dimension column chromatography separation, the fractions corresponding to the elution time periods of 31 min-42 min in the two dimension column chromatography separation, the fractions corresponding to the elution time periods of 51min-77min in the two dimension column chromatography separation, and the fractions corresponding to the elution time periods of 77 min-200 min in the two dimension column chromatography separation;
3) And (3) respectively taking the trapped fluid of the first-stage membrane separation in the step (1), the trapped fluid of the second-stage membrane separation, the trapped fluid of the third-stage membrane separation and the fractions of the 40 th to 64 th elution time periods, the fractions of the 31 th to 42 th elution time periods, the fractions of the 65 th to 84 th elution time periods and the fractions of the 55 th to 67 th elution time periods collected in the step (2), and compounding to obtain the composite material.
According to the preparation method of the spice for increasing the tobacco fragrance of the flue-cured tobacco of the heated cigarettes, the characteristic flavor group obtained by multistage membrane separation and two-dimensional column chromatography of the Zimbabwe tobacco extract solution is compounded, and compared with the original Zimbabwe tobacco extract, the preparation method can effectively remove the organoleptic components in the Zimbabwe tobacco extract, fully highlight the characteristics of the Zimbabwe tobacco extract and improve the applicability of the spice in the heated cigarettes.
The preparation method of the spice for increasing the tobacco fragrance of the heated cigarette flue-cured tobacco has universal applicability to Zimbabwe tobacco extracts of different sources. In the preparation method, the trapped fluid of the first-stage membrane separation, the trapped fluid of the second-stage membrane separation, the trapped fluid of the third-section membrane separation, the fraction of the 40 th to 64 th elution time periods, the fraction of the 31 st to 42 th elution time periods, the fraction of the 65 th to 84 th elution time periods and the fraction of the 55 th to 67 th elution time periods are respectively classified into characteristic flavor groups of Zimbabwe tobacco leaf extract. Wherein, the trapped fluid of the first-stage membrane separation can increase the aroma and richness of the cigarettes; the trapped fluid of the second-stage membrane separation can increase the fineness, softness and smoothness of cigarettes and reduce the bitter taste; the trapped fluid separated by the third section of membrane can obviously increase the concentration of the smoke and the aroma; the flow component in the elution time period from 40min to 64min can obviously increase the tobacco fragrance of the flue-cured tobacco of the cigarettes; the fraction of the elution time period from 31min to 42min can obviously increase sweet taste and reduce bitter taste; the flow fraction in the elution time period from 65min to 84min can increase the strength and fragrance of the cigarettes; the fraction of the elution time period from 55min to 67min can increase the aroma and sweetness of the flue-cured tobacco of the cigarettes.
In order to remarkably increase the characteristics of the tobacco fragrance of the heated tobacco, improve the sweetness and the bitterness, improve the fragrance and the richness, and fine and soft smoothness, increase the smoke concentration and the strength, further, in the step 3), the interception liquid of the first-stage membrane separation, the interception liquid of the second-stage membrane separation, the interception liquid of the third-stage membrane separation, the flow of the elution time period of 40 min-64 min, the flow of the elution time period of 31 min-42 min, the flow of the elution time period of 65 min-84 min and the flow of the elution time period of 55 min-67 min are mixed, and the mass ratio of the flow of the elution time period of 55 min-67 min is 0.1:10-15:0.01-0.03:0.2-0.8:1-2:0.3-0.5:1-3, and more preferably 0.5-1:10-13:0.01-0.02:0.2-0.6:1-2:0.3-0.5:1-2.5.
Further, in the step 1), the Zimbabwe tobacco extract solution is obtained by dissolving Zimbabwe tobacco extract into a solution with a dry matter mass fraction of 10% by adopting an ethanol water solution with an ethanol volume fraction of 50%.
Further, the Zimbabwe tobacco extract is one or any combination of Zimbabwe tobacco extract, zimbabwe tobacco tincture, zimbabwe tobacco absolute and Zimbabwe tobacco extract dry powder.
Further, in the step 2), the dry matter content in the concentrated solution is 8% by mass.
Further, in the step 2), the inner diameter of the first dimension chromatographic column is 50mm, and the packing length of the sephadex in the first dimension chromatographic column is 400mm; in the first dimension column chromatography, the flow rate of the eluent is 8mL/min.
Further, the Sephadex was purchased from GE HEALTHCARE, sweden under the model Sephadex LH-20 and had a particle size range (dry) of 18-111. Mu.m.
Further, the C18 reverse phase silicse:Sup>A gel was se:Sup>A general type C18 filler available from YMC company under the model number YMC ODS-A, and had se:Sup>A particle size of 50. Mu.m.
Further, in the step 2), the inner diameter of the second-dimension chromatographic column is 20mm, and the packing length of the C18 reverse phase silica gel in the second-dimension chromatographic column is 460mm; in the second dimension of column chromatography, the flow rate of the eluent was 8mL/min.
The dry matter mass fraction in the present invention refers to the percentage of the solute remaining after the solution has completely removed the solvent to the mass of the solution.
The technical scheme adopted by the spice of the invention is as follows:
A flavor prepared by the method for preparing the flavor for increasing the tobacco flavor of the cured tobacco of the heated cigarettes.
The flavor of the invention can fully highlight the characteristics of the Zimbabwe tobacco extract and increase the characteristics of the flue-cured tobacco flavor of the heated cigarettes by removing the organoleptic bad components in the Zimbabwe tobacco extract. The perfume of the invention is directly added to the cigarette of the heating cigarette when in use.
Detailed Description
The technical scheme of the invention is further described below with reference to the specific embodiments.
The zimbabwe tobacco extract used in example 1, the zimbabwe smoke extract used in example 2, and the zimbabwe tobacco extract used in example 3 are different commercially available zimbabwe tobacco extract products.
The Sephadex used in the examples was purchased from GE HEALTHCARE, sweden under the model Sephadex LH-20 and had a particle size range (dry) of 18-111. Mu.m; the C18 reverse phase silicse:Sup>A gel was used, and was purchased from YMC Co., td., model YMC ODS-A general type C18 filler, and had se:Sup>A particle size of 50. Mu.m.
Example 1
The preparation method of the spice for remarkably increasing the tobacco fragrance of the cured tobacco of the heated cigarettes in the embodiment comprises the following steps of:
1) Dissolving Zimbabwe tobacco leaf extract (recorded as Zimbabwe tobacco leaf extract 1) into a solution with a dry matter mass of 10% by adopting an ethanol water solution with an ethanol volume fraction of 50% to obtain a Zimbabwe tobacco extract solution;
2) Carrying out first-stage membrane separation on Zimbabwe tobacco extract solution by adopting a ceramic membrane with the pore diameter of 50nm, collecting trapped fluid of the first-stage membrane separation, carrying out second-stage membrane separation on permeate of the first-stage membrane separation by adopting a ceramic membrane with the pore diameter of 10nm, then collecting trapped fluid of the second-stage membrane separation, carrying out third-stage membrane separation on permeate of the second-stage membrane separation by adopting a coiled organic membrane with the molecular weight of 1kDa, and collecting trapped fluid of the third-stage membrane separation and permeate of the third-stage membrane separation; the trapped fluid of the first-stage membrane separation is marked as MJ1 trapped fluid, the trapped fluid of the second-stage membrane separation is marked as MJ2 trapped fluid, and the trapped fluid of the third-stage membrane separation is marked as MJ3 trapped fluid; the pressure before membrane separation in the first stage membrane separation, the second stage membrane separation and the third stage membrane separation is 3.0bar, 4.0bar and 3.0bar in sequence, and each stage of membrane separation is carried out at room temperature.
3) Concentrating the collected third-stage membrane separated permeate by reduced pressure distillation to obtain a solution with the dry matter mass of 10%, obtaining a concentrated solution, and carrying out two-dimensional column chromatography separation on the obtained concentrated solution;
The chromatographic column packing adopted in the first dimension column chromatographic separation is sephadex, the inner diameter of the chromatographic column is 50mm, and the length of the sephadex column filled in the chromatographic column is 400mm (the dry mass of the filled sephadex is 100 g); the chromatographic column packing adopted in the second dimension column chromatographic separation is C18 reverse phase silica gel, the inner diameter of the chromatographic column is 20mm, the length of the C18 reverse phase silica gel column filled in the chromatographic column is 460mm (the dry mass of the C18 reverse phase silica gel filled is 65 g);
During the first dimension column chromatographic separation, water is used as an eluent, the flow rate of the eluent is controlled to be 8mL/min, and the elution time is controlled to be 200min, and the fractions of the elution time periods from 0min to 38min, the fractions of the elution time periods from 38min to 51min, the fractions of the elution time periods from 51min to 77min and the fractions of the elution time periods from 77min to 200min are respectively collected during the first dimension column chromatographic separation; the elution time period from 0min to 38min is marked as one-dimensional 1 fraction, the elution time period from 38min to 51min is marked as one-dimensional 2 fraction, the elution time period from 51min to 77min is marked as one-dimensional 3 fraction, and the elution time period from 77min to 200min is marked as one-dimensional 4 fraction;
During the second dimension column chromatography separation, respectively enabling the collected one-dimensional 1 fraction, one-dimensional 2 fraction, one-dimensional 3 fraction and one-dimensional 4 fraction to enter a second dimension column chromatography, taking an ethanol water solution with the ethanol volume fraction of 90% as an eluting solvent, controlling the eluting flow rate to be 8mL/min and the eluting time to be 100min for eluting, respectively collecting the fractions in the eluting time period from 40min to 64min when the one-dimensional 1 fraction corresponds to the two dimension column chromatography separation, the fractions in the eluting time period from 31min to 42min when the one-dimensional 2 fraction corresponds to the two dimension column chromatography separation, the fractions in the eluting time period from 65min to 84min when the one-dimensional 3 fraction corresponds to the two dimension column chromatography separation, and the fractions in the eluting time period from 55min to 67min when the one-dimensional 4 fraction corresponds to the two dimension column chromatography separation; the fractions of the elution time period from 40min to 64min are marked as A1 fraction, the fractions of the elution time period from 31min to 42min are marked as A2 fraction, the fractions of the elution time period from 65min to 84min are marked as A3 fraction, and the fractions of the elution time period from 55min to 67min are marked as A4 fraction;
4) 1 part by weight of MJ1 trapped fluid, 10 parts by weight of MJ2 trapped fluid, 0.01 part by weight of MJ3 trapped fluid, 0.6 part by weight of A1 fraction, 1.5 parts by weight of A2 fraction, 0.3 part by weight of A3 fraction and 1 part by weight of A4 fraction are uniformly mixed to obtain a spice capable of remarkably increasing the smoke flavor characteristics of the heated cigarette flue-cured tobacco, and the spice is denoted as spice I.
Example 2
The preparation method of the spice for remarkably increasing the tobacco fragrance of the heated cigarettes in the embodiment comprises the following steps of:
1) Dissolving Zimbabwe tobacco leaf extract (recorded as Zimbabwe tobacco leaf extract 2) into a solution with a dry matter mass of 10% by adopting an ethanol water solution with an ethanol volume fraction of 50% to obtain a Zimbabwe extract solution;
2) Performing first-stage membrane separation on Zimbabwe extract solution by adopting a ceramic membrane with the aperture of 50nm, collecting trapped fluid of the first-stage membrane separation, performing second-stage membrane separation on permeate of the first-stage membrane separation by adopting a ceramic membrane with the aperture of 10nm, then collecting trapped fluid of the second-stage membrane separation, performing third-stage membrane separation on permeate of the second-stage membrane separation by adopting a coiled organic membrane with the molecular weight of 1kDa, and collecting trapped fluid of the third-stage membrane separation and permeate of the third-stage membrane separation; the trapped fluid of the first and the membrane separation is denoted as MJ1 trapped fluid, the trapped fluid of the second-stage membrane separation is denoted as MJ2 trapped fluid, and the trapped fluid of the third-stage membrane separation is denoted as MJ3 trapped fluid; the pressure before membrane separation in the first stage membrane separation, the second stage membrane separation and the third stage membrane separation is 3.0bar, 4.0bar and 3.0bar in sequence, and each stage of membrane separation is carried out at room temperature;
3) Concentrating the collected permeation solution separated by the third-stage membrane into a solution with the dry matter mass fraction of 10% by reduced pressure distillation to obtain a concentrated solution; performing two-dimensional column chromatography on the obtained concentrated solution; the chromatographic column packing adopted in the first dimension column chromatographic separation is sephadex, the inner diameter of the chromatographic column is 50mm, the length of the sephadex column filled in the chromatographic column is 400mm (the dry mass of the filled sephadex is 100 g); the chromatographic column packing adopted in the second dimension column chromatographic separation is C18 reverse phase silica gel, the inner diameter of the chromatographic column is 20mm, the length of the C18 reverse phase silica gel column filled in the chromatographic column is 460mm (the dry mass of the C18 reverse phase silica gel filled is 65 g);
In the first dimension column chromatography separation, water is used as an eluent, the flow rate of the eluent is controlled to be 8mL/min, the elution time is controlled to be 200min, and the fractions of the elution time periods from 0min to 38min, the fractions of the elution time periods from 38min to 51min, the fractions of the elution time periods from 51min to 77min and the fractions of the elution time periods from 77min to 200min in the first dimension column chromatography separation process are respectively collected; the elution time period of 0min-38min is respectively marked as one-dimensional 1 fraction, the elution time period of 38 min-51 min is marked as one-dimensional 2 fraction, the elution time period of 51 min-77 min is marked as one-dimensional 3 fraction, and the elution time period of 77 min-200 min is marked as one-dimensional 4 fraction;
During the second dimension column chromatography separation, respectively enabling the one-dimensional 1 fraction, the one-dimensional 2 fraction, the one-dimensional 3 fraction and the one-dimensional 4 fraction collected during the first dimension column chromatography separation to respectively enter the second dimension column chromatography, taking an ethanol water solution with the ethanol volume fraction of 90% as an eluting solvent, controlling the eluting flow rate to be 8mL/min and the eluting time to be 100min for column chromatography separation, respectively collecting the fractions of the one-dimensional 1 fraction corresponding to the eluting time period of 40 min-64 min during the two-dimension column chromatography separation, the fractions of the one-dimensional 2 fraction corresponding to the eluting time period of 31 min-42 min during the two-dimension column chromatography separation, the fractions of the one-dimensional 3 fraction corresponding to the eluting time period of 65 min-84 min during the two-dimension column chromatography separation, and the fractions of the one-dimensional 4 fraction corresponding to the eluting time period of 55 min-67 min during the two-dimension column chromatography separation; the fractions of the elution time period from 40min to 64min are respectively marked as A1 fraction, the fractions of the elution time period from 31min to 42min are respectively marked as A2 fraction, the fractions of the elution time period from 65min to 84min are respectively marked as A3 fraction, and the fractions of the elution time period from 55min to 67min are respectively marked as A4 fraction;
4) Uniformly mixing 0.5 part by weight of MJ1 trapped fluid, 11 parts by weight of MJ2 trapped fluid, 0.02 part by weight of MJ3 trapped fluid, 0.2 part by weight of A1 fraction, 1 part by weight of A2 fraction, 0.3 part by weight of A3 fraction and 1.2 parts by weight of A4 fraction to obtain a spice capable of remarkably increasing the smoke aroma characteristics of the heated flue-cured tobacco, and marking as spice II.
Example 3
The preparation method of the spice for remarkably increasing the tobacco fragrance of the heated cigarettes in the embodiment comprises the following steps of:
1) Dissolving Zimbabwe tobacco leaf extract (marked as Zimbabwe tobacco leaf extract 3) into a solution with a dry matter mass of 10% by adopting an ethanol water solution with an ethanol volume fraction of 50% to obtain a Zimbabwe extract solution;
2) Performing first-stage membrane separation on Zimbabwe tobacco extract solution by adopting a ceramic membrane with the aperture of 50nm, collecting trapped fluid of the first-stage membrane separation, performing second-stage membrane separation on permeate of the first-stage membrane separation by adopting a ceramic membrane with the aperture of 10nm, then collecting trapped fluid of the second-stage membrane separation, performing third-stage membrane separation on permeate of the second-stage membrane separation by adopting a coiled organic membrane with the molecular weight of 1kDa, and collecting trapped fluid and permeate of the third-stage membrane separation; the trapped fluid separated by the first-stage membrane is denoted as MJ1 trapped fluid, the trapped fluid separated by the second-stage membrane is denoted as MJ2 trapped fluid, and the trapped fluid separated by the third-stage membrane is denoted as MJ3 trapped fluid; the pressure before membrane separation in the first stage membrane separation, the second stage membrane separation and the third stage membrane separation is 3.0bar, 4.0bar and 3.0bar in sequence, and each stage of membrane separation is carried out at room temperature;
3) Concentrating the permeate liquid separated by the third-stage membrane into a solution with the dry matter mass of 10% by using reduced pressure distillation to obtain concentrated liquid, and then carrying out two-dimensional column chromatography on the obtained concentrated liquid;
The chromatographic column packing adopted in the first dimension column chromatographic separation is sephadex, the inner diameter of the chromatographic column is 50mm, the length of the sephadex column filled in the chromatographic column is 400mm (the dry mass of the filled sephadex is 100 g); the chromatographic column packing adopted in the second dimension column chromatographic separation is C18 reverse phase silica gel, the inner diameter of the chromatographic column is 20mm, the length of the C18 reverse phase silica gel column filled in the chromatographic column is 460mm (the dry mass of the C18 reverse phase silica gel filled is 65 g);
during the first dimension column chromatography separation, water is used as an eluent, the flow rate of the eluent is controlled to be 8mL/min, the elution time is controlled to be 200min, and the fractions of the elution time periods from 0min to 38min, the fractions of the elution time periods from 38min to 51min, the fractions of the elution time periods from 51min to 77min and the fractions of the elution time periods from 77min to 200min are collected during the first dimension column chromatography separation; the elution time period from 0min to 38min is marked as one-dimensional 1 fraction, the elution time period from 38min to 51min is marked as one-dimensional 2 fraction, the elution time period from 51min to 77min is marked as one-dimensional 3 fraction, and the elution time period from 77min to 200min is marked as one-dimensional 4 fraction;
During the second dimension column chromatography separation, respectively enabling the collected one-dimensional 1 fraction, one-dimensional 2 fraction, one-dimensional 3 fraction and one-dimensional 4 fraction to enter a second dimension column chromatography, taking an ethanol water solution with the ethanol volume fraction of 90% as an eluting solvent, controlling the eluting flow rate to be 8mL/min and the eluting time to be 100min for column chromatography separation, respectively collecting fractions in the eluting time period of 40 min-64 min when the one-dimensional 1 fraction corresponds to the two dimension column chromatography separation, fractions in the eluting time period of 31min-42min when the one-dimensional 2 fraction corresponds to the two dimension column chromatography separation, fractions in the eluting time period of 65 min-84 min when the one-dimensional 3 fraction corresponds to the two dimension column chromatography separation, and fractions in the eluting time period of 55 min-67 min when the one-dimensional 4 fraction corresponds to the two dimension column chromatography separation; the fractions of the elution time period from 40min to 64min are marked as A1 fraction, the fractions of the elution time period from 31min to 42min are marked as A2 fraction, the fractions of the elution time period from 65min to 84min are marked as A3 fraction, and the fractions of the elution time period from 55min to 67min are marked as A4 fraction;
4) Uniformly mixing 0.7 part by weight of MJ1 trapped fluid, 13 parts by weight of MJ2 trapped fluid, 0.02 part by weight of MJ3 trapped fluid, 0.3 part by weight of A1 fraction, 2 parts by weight of A2 fraction, 0.5 part by weight of A3 fraction and 2.5 parts by weight of A4 fraction to obtain a spice capable of remarkably increasing the smoke aroma characteristics of the heated flue-cured tobacco, and marking as spice III.
Example 4
The perfume of this embodiment is prepared by any one of the methods of embodiments 1 to 3, and will not be described here.
Comparative example 1
The flavor of this comparative example was obtained by uniformly mixing 2 parts by weight of MJ1 retentate, 8 parts by weight of MJ2 retentate, 0.01 part by weight of MJ3 retentate, 0.06 part by weight of A1 fraction, 0.5 part by weight of A2 fraction, 0.1 part by weight of A3 fraction, and 4 parts by weight of A4 fraction in example 1, and was designated as flavor IV.
Comparative example 2
The flavor of this comparative example was prepared by replacing the 1kDa rolled organic film with the 5kDa rolled organic film in the method for preparing a flavor for enhancing the tobacco flavor of cured cigarettes of example 1, and was designated as flavor V.
Experimental example 1
The flavor I, flavor II, flavor III, flavor IV, flavor V prepared in examples and comparative examples, and solutions of 3 zimbabwe leaf extracts employed in examples 1 to 3, each of which was prepared by preparing zimbabwe leaf extract into a solution having a dry matter mass fraction of 5% using an aqueous ethanol solution having a volume fraction of 50% as a solvent, were injected into blank heated cigarettes in an amount of 50ppm, and sensory evaluation was performed by 10 professional cigarette sensory evaluation staff with reference to YC/T497-2014 "style sensory evaluation method of cigarette chinese style", and the result of suction evaluation is shown in table 1.
Table 1 sensory evaluation results
As can be seen from the data in Table 1, compared with the blank heated cigarettes and 3 Zimbabwe tobacco extracts, the flavor I, the flavor II and the flavor III can obviously improve the tobacco flavor of the cured tobacco of the blank heated cigarettes after being added into the cigarettes, and meanwhile, the indexes such as aroma, richness, fineness, softness, smoothness and smoothness are improved to different degrees, the bitter taste is reduced, and the sensory effect on the heated cigarettes is better than that of the flavor IV and the flavor V. These results show that the flavor of the heated cigarette tobacco can be obviously improved, and the sensory quality of the cigarette can be effectively improved.
Claims (7)
1. A preparation method of a spice for increasing the tobacco fragrance of heated tobacco is characterized by comprising the following steps: the method comprises the following steps:
1) Carrying out first-stage membrane separation on Zimbabwe tobacco extract solution by adopting a ceramic membrane with the pore diameter of 50nm, then carrying out second-stage membrane separation on permeate by adopting a ceramic membrane with the pore diameter of 10nm, and then carrying out third-stage membrane separation on permeate separated by the second-stage membrane by adopting a coiled organic membrane with the interception molecular weight of 1 kDa;
2) Concentrating the permeate liquid of the third-stage membrane separation to obtain concentrated liquid; then carrying out two-dimensional column chromatographic separation on the obtained concentrated solution; the packing of the first dimension chromatographic column is sephadex, and the length-diameter ratio of the sephadex column is 8:1; the packing of the second dimension chromatographic column is C18 reverse phase silica gel, and the length-diameter ratio of the C18 reverse phase silica gel column is 23:1;
During the first dimension column chromatography separation, water is used as an eluent, the flow rate of the eluent corresponding to each 250 pi mL volume column bed is controlled to be 8mL/min, and the fractions of the elution time period from 0min to 38min, the fractions of the elution time period from 38min to 51min, the fractions of the elution time period from 51min to 77min and the fractions of the elution time period from 77min to 200min are respectively collected;
During the second dimension column chromatography separation, enabling the fractions collected during the first dimension column chromatography separation to enter the second dimension column chromatography respectively, taking an ethanol water solution with the ethanol volume fraction of 90% as an eluent, controlling the flow rate of the eluent corresponding to each 46 pi mL volume column bed to be 8mL/min, and collecting the fractions corresponding to the elution time periods of 0 min-38 min and 40 min-64 min respectively, the fractions corresponding to the elution time periods of 38 min-51 min and 31 min-42 min respectively, the fractions corresponding to the elution time periods of 51 min-77 min and 65 min-84 min respectively, and the fractions corresponding to the elution time periods of 77 min-200 min respectively;
3) Respectively compounding the trapped fluid of the first-stage membrane separation in the step 1), the trapped fluid of the second-stage membrane separation, the trapped fluid of the third-stage membrane separation and the fractions of the 40 th to 64 th elution time periods, the fractions of the 31 th to 42 th elution time periods, the fractions of the 65 th to 84 th elution time periods and the fractions of the 55 th to 67 th elution time periods collected in the step 2);
In the step 3), the mass ratio of the trapping liquid of the first-stage membrane separation, the trapping liquid of the second-stage membrane separation, the trapping liquid of the third-stage membrane separation, the fraction of the 40 th to 64 th elution time periods, the fraction of the 31 st to 42 th elution time periods, the fraction of the 65 th to 84 th elution time periods and the fraction of the 55 th to 67 th elution time periods which are compounded is 0.1-1:10-15:0.01-0.03:0.2-0.8:1-2:0.3-0.5:1-3.
2. The method for preparing the spice for increasing the tobacco fragrance of the cured tobacco of the heated cigarettes according to claim 1, wherein the method comprises the following steps of: in the step 1), the Zimbabwe tobacco extract solution is obtained by dissolving Zimbabwe tobacco extract into a solution with a dry matter mass fraction of 10% by adopting an ethanol water solution with an ethanol volume fraction of 50%.
3. The method for preparing the spice for increasing the tobacco fragrance of the cured tobacco of the heated cigarettes according to claim 2, wherein the method comprises the following steps of: the Zimbabwe tobacco extract is one or any combination of Zimbabwe tobacco extract, zimbabwe tobacco tincture, zimbabwe tobacco absolute oil and Zimbabwe tobacco extract dry powder.
4. The method for preparing the spice for increasing the tobacco fragrance of the cured tobacco of the heated cigarettes according to claim 1, wherein the method comprises the following steps of: in the step 2), the mass percentage of dry matters in the concentrated solution is 8%.
5. The method for preparing the spice for increasing the tobacco fragrance of the cured tobacco of the heated cigarettes according to claim 1, wherein the method comprises the following steps of: in the step 2), the inner diameter of the first dimension chromatographic column is 50mm, and the packing length of the sephadex in the first dimension chromatographic column is 400mm; in the first dimension column chromatography, the flow rate of the eluent is 8mL/min.
6. The method for preparing the spice for increasing the tobacco fragrance of the cured tobacco of the heated cigarettes according to claim 1, wherein the method comprises the following steps of: in the step 2), the inner diameter of the second-dimension chromatographic column is 20mm, and the packing length of the C18 reverse phase silica gel in the second-dimension chromatographic column is 460mm; in the second dimension of column chromatography, the flow rate of the eluent was 8mL/min.
7. A flavor prepared by the method for preparing a flavor for enhancing the smoke flavor of a cured tobacco of a heated cigarette according to any one of claims 1 to 6.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102759588A (en) * | 2012-07-16 | 2012-10-31 | 上海烟草集团有限责任公司 | Method for separating and preparing key acid flavor components in cigarette mainstream smoke and application of key acid volatile components |
| CN103436363A (en) * | 2013-09-03 | 2013-12-11 | 华宝食用香精香料（上海）有限公司 | Preparation method of aroma substance in Zimbabwe tobacco extractive as well as products and application of aroma substance |
| CN105520189A (en) * | 2015-12-30 | 2016-04-27 | 立场电子科技发展（上海）有限公司 | Method for preparing tobacco juice of electronic cigarettes by adopting Zimbabwean tobacco extract |
| CN106010797A (en) * | 2016-07-25 | 2016-10-12 | 中国烟草总公司郑州烟草研究院 | Malt coke-sweet flavor prepared from coked malt and application thereof in electronic cigarettes |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2008537130A (en) * | 2005-04-21 | 2008-09-11 | シムライズ・ゲゼルシヤフト・ミツト・ベシユレンクテル・ハフツング・ウント・コンパニー・コマンジツト・ゲゼルシヤフト | Method for separating perfume and sensory evaluation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102759588A (en) * | 2012-07-16 | 2012-10-31 | 上海烟草集团有限责任公司 | Method for separating and preparing key acid flavor components in cigarette mainstream smoke and application of key acid volatile components |
| CN103436363A (en) * | 2013-09-03 | 2013-12-11 | 华宝食用香精香料（上海）有限公司 | Preparation method of aroma substance in Zimbabwe tobacco extractive as well as products and application of aroma substance |
| CN105520189A (en) * | 2015-12-30 | 2016-04-27 | 立场电子科技发展（上海）有限公司 | Method for preparing tobacco juice of electronic cigarettes by adopting Zimbabwean tobacco extract |
| CN106010797A (en) * | 2016-07-25 | 2016-10-12 | 中国烟草总公司郑州烟草研究院 | Malt coke-sweet flavor prepared from coked malt and application thereof in electronic cigarettes |
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