CN115637196B - Bead-bursting perfume capable of highlighting clear fragrance characteristics of cigarette tea, preparation method of bead-bursting perfume, bead-bursting perfume and cigarette - Google Patents
Bead-bursting perfume capable of highlighting clear fragrance characteristics of cigarette tea, preparation method of bead-bursting perfume, bead-bursting perfume and cigarette Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 17
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- 241000208125 Nicotiana Species 0.000 claims description 19
- 235000002637 Nicotiana tabacum Nutrition 0.000 claims description 19
- 238000013375 chromatographic separation Methods 0.000 claims description 17
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- 229920005654 Sephadex Polymers 0.000 claims description 15
- 239000012507 Sephadex™ Substances 0.000 claims description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 13
- 239000000741 silica gel Substances 0.000 claims description 13
- 229910002027 silica gel Inorganic materials 0.000 claims description 13
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 12
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- GLZPCOQZEFWAFX-UHFFFAOYSA-N Geraniol Chemical compound CC(C)=CCCC(C)=CCO GLZPCOQZEFWAFX-UHFFFAOYSA-N 0.000 description 2
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- 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
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Landscapes
- Tea And Coffee (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention relates to a bead-bursting spice for highlighting the clear fragrance characteristics of cigarette tea, a preparation method thereof, a bead-bursting spice and a cigarette, and belongs to the technical field of flavoring of tobacco products. The method comprises the steps of sequentially adopting a 50kDa, 10kDa and 1kDa coiled organic membrane to carry out membrane separation on green tea extract solution, collecting each stage of separation trapped fluid, taking permeate as a next stage of membrane separation object, concentrating the last stage of membrane separation fluid, carrying out two-dimensional column chromatography separation, collecting fractions of different set elution time periods of first-dimension column chromatography separation, respectively entering each fraction into a second-dimension column chromatography for two-dimensional column chromatography separation, respectively collecting fractions of the set elution time periods when each fraction collected by the first-dimension column chromatography separation corresponds to the second-dimension column chromatography separation, and carrying out combination on the trapped fluid of each stage of membrane separation and each fraction collected when the second-dimension column chromatography separation. The method can effectively remove the organoleptic components in the green tea extract, and fully highlight the characteristics of the green tea extract.
Description
Technical Field
The invention relates to a bead-bursting spice for highlighting the clear fragrance characteristics of cigarette tea, a preparation method thereof, a bead-bursting spice and a cigarette, and belongs to the technical field of flavoring of tobacco products.
Background
The green tea contains nutritional components such as tea polyphenols, catechin, amino acids, vitamins, etc., and also contains a great amount of volatile aroma components such as benzaldehyde, linalool, geraniol, ionone, etc. The green tea extract is widely applied to foods and daily chemicals and plays an important role in flavoring cigarettes. As an important natural perfume for cigarettes, the green tea extract can improve the aroma quality, the mellow and fragrant flavor of cigarettes, improve the moist feel and the aftertaste of the cigarettes, and the like.
The green tea extract is generally prepared by extracting with water or low-concentration ethanol as a solvent through steps of distillation, concentration and the like, but the quality of the green tea extract is uneven, the fluctuation of chemical composition is obvious due to the huge difference of green tea raw materials and the influence of a processing technology, and the sensory effect difference in cigarettes is obvious, so that the problems of unstable quality and the like of cigarette products are caused while the flavoring difficulty of the cigarettes is increased. In addition, the presence of proteins, amino acids, polyphenols, lipids, etc. in green tea extracts often negatively affects the organoleptic quality of the cigarettes. At present, the impurity removal modes of the green tea extract comprise precipitation separation, macroporous adsorption resin separation and the like, and although the active ingredients in the extract can be enriched to a certain extent, the function focusing of the green tea extract is insufficient, and the flavor characteristics are not enough. The tea fragrance consists of tea fragrance and fragrance, improves the quality of green tea extract products, develops tea fragrance perfume with focused functions, fully highlights the characteristics of green tea, and is a problem to be solved in the fine processing of natural perfume for cigarettes.
Disclosure of Invention
The invention aims to provide a preparation method of a flavor for bursting beads, which is capable of highlighting the clear fragrance characteristics of cigarette tea, and can be used for focusing the clear fragrance characteristics of tea and highlighting the green tea characteristics.
The invention also provides the flavor for the bursting beads, which is prepared by the preparation method of the flavor for the bursting beads, and the bursting beads and the cigarettes which adopt the flavor for the bursting beads, wherein the flavor for the bursting beads is obvious in the fragrance of the cigarette tea.
In order to achieve the above purpose, the technical scheme adopted by the preparation method of the flavor for the bursting beads for highlighting the clear fragrance characteristics of the cigarette tea is as follows:
a preparation method of a flavor for bursting beads for highlighting the clear fragrance characteristics of cigarette tea comprises the following steps:
1) Carrying out first-stage membrane separation on the green tea extract solution by adopting a coiled organic membrane with a molecular weight cutoff of 50kDa, then carrying out second-stage membrane separation on the permeate by adopting a coiled organic membrane with a molecular weight cutoff of 10kDa, and then carrying out third-stage membrane separation on the permeate separated by the second-stage membrane by adopting a coiled organic membrane with a molecular weight cutoff of 1 kDa;
2) Concentrating the permeate liquid separated by the third-stage membrane to obtain concentrated liquid, and then carrying out two-dimensional column chromatographic separation on the concentrated liquid;
the packing of the chromatographic column adopted in the chromatographic separation of the first dimension column is sephadex, and the length-diameter ratio of the sephadex column is 10:1; the packing of the chromatographic column adopted in the second dimension column chromatographic separation is C18 reverse phase silica gel, and the length-diameter ratio of the C18 reverse phase silica gel column is 20:1;
during the first dimension column chromatographic separation, an ethanol water solution with the volume fraction of 50% is taken as an eluent, the flow rate of the eluent corresponding to each 227.8125 pi mL volume of column bed is controlled to be 10mL/min, and the flow fractions of the elution time periods from 0min to 62min, the flow fractions of the elution time periods from 62min to 87min and the flow fractions of the elution time periods from 87min to 200min are respectively collected;
during the second dimension column chromatography separation, enabling the fractions collected during the separation of each first dimension column chromatography to enter the second dimension column chromatography respectively, taking ethanol water solution with the ethanol volume fraction of 95% as eluent, controlling the flow rate of the eluent corresponding to each 78.125 pi mL volume of column bed to be 12mL/min, and collecting the fractions in the 34 th to 58 th elution time periods in the two dimension column chromatography separation process corresponding to the fractions in the 0 th to 62 th elution time periods, the fractions in the 26 th to 40 th elution time periods in the two dimension column chromatography separation process corresponding to the fractions in the 62 th to 87 th elution time periods and the fractions in the 35 th to 42 th elution time periods in the two dimension column chromatography separation process corresponding to the 87 th to 200 th fractions respectively;
3) And (3) 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, the fractions of the 34 th min-58 th min elution time period, the fractions of the 26 th min-40 th elution time period and the fractions of the 35 th min-42 th elution time period collected in the step (2).
According to the preparation method of the flavor for bursting beads for highlighting the clear fragrance characteristics of the cigarette tea, disclosed by the invention, the flavor is obtained by compounding the characteristic flavor groups obtained by multi-stage membrane separation and two-dimensional column chromatography separation of the green tea extract, compared with the original green tea extract, the flavor obtained by compounding can effectively remove the organoleptic components in the green tea extract, the characteristics of the green tea extract are fully highlighted, and the method has general applicability to green tea extracts from different sources.
The trapped fluid of each stage of membrane separation and the flow fractions of each corresponding elution time period collected in the second-dimension column chromatographic separation process in the preparation method of the flavor for bursting beads for highlighting the clear fragrance characteristics of the cigarette tea are all green tea characteristic flavor groups. Wherein, the trapped fluid of the first-stage membrane separation can obviously increase the aroma and the richness of cigarettes; the trapped fluid of the second-stage membrane separation can reduce the bitter taste of cigarettes and increase the sense of fineness, softness and smoothness; the trapped fluid of the third-stage membrane separation can increase the richness of cigarettes; the flow fraction in the elution time period from 34min to 58min collected in the step 2) can obviously increase the faint scent and tea scent of cigarettes, the flow fraction in the elution time period from 26min to 40min can greatly increase the tea scent of cigarettes, and the flow fraction in the elution time period from 35min to 42min can increase the clear and soft flavors of cigarettes.
In order to remarkably increase the fragrance-cleaning characteristic of the cigarette tea, promote the green and soft fragrance of the cigarette, improve the fragrance quality, enrich, fine and soft and smooth the softness, reduce the bitter taste and promote the overall sensory effect, further, in the step 3), the components are uniformly mixed by 1 to 2 parts by weight of the trapped fluid separated by the first-stage membrane, 4 to 8 parts by weight of the trapped fluid separated by the second-stage membrane, 10 to 15 parts by weight of the trapped fluid separated by the third-stage membrane, 0.01 to 0.02 part by weight of the fraction in the elution time period from 34min to 58min, 1 to 2 parts by weight of the fraction in the elution time period from 26min to 40min and 0.5 to 0.8 part by weight of the fraction in the elution time period from 35min to 42min, so as to obtain the perfume for the bead explosion. Preferably, in the step 3), the compounding is to uniformly mix 1 to 2 parts by weight of the trapped fluid of the first-stage membrane separation, 5 to 8 parts by weight of the trapped fluid of the second-stage membrane separation, 10 to 14 parts by weight of the trapped fluid of the third-stage membrane separation, 0.01 to 0.02 part by weight of the fraction of the elution time period from 34min to 58min, 1 to 2 parts by weight of the fraction of the elution time period from 26min to 40min and 0.6 to 0.8 part by weight of the fraction of the elution time period from 35min to 42min, thereby obtaining the bead-blasting spice.
The green tea extracts from different sources can be used for preparing the spice for highlighting the fragrance of the cigarette tea by the preparation method. Further, the green tea extract is one or any combination of green tea extract, green tea absolute, green tea tincture and green tea extract dry powder.
Further, in the step 1), the green tea extract solution is a solution with a dry matter mass fraction of 8% -10% obtained by dissolving the green tea extract in an ethanol aqueous solution with an ethanol volume fraction of 50% -70%. Preferably, the green tea extract solution is a solution with a dry matter mass fraction of 8% obtained by dissolving green tea extract in an aqueous ethanol solution with a volume fraction of 50% ethanol.
Further, in the step 2), the mass fraction of the dry matter in the concentrated solution is 8% -10%. Preferably, in step 2), the mass fraction of dry matter in the concentrate is 8%.
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, in the step 2), the C18 reverse phase silicse:Sup>A gel is se:Sup>A YMC ODS-A general type C18 filler available from YMC Co., td., model number, and has se:Sup>A particle size of 50. Mu.m.
Further, in the step 2), the inner diameter of a chromatographic column used for the first dimension column chromatographic separation is 45mm, and the length of a sephadex column filled in the chromatographic column is 450mm; the flow rate of the eluent in the first dimension column chromatography was 10mL/min. The dry mass of the packed dextran gel in the column was 100g.
Further, in the step 2), the inner diameter of a chromatographic column used for the second-dimension column chromatographic separation is 25mm, and the length of a C18 reverse phase silica gel column filled in the chromatographic column is 500mm; the flow rate of the eluent in the second dimension column chromatography is 12mL/min. The dry mass of the C18 reverse phase silica gel column packed in the column was 65g.
The technical scheme adopted by the spice for bursting beads for highlighting the clear fragrance characteristics of the cigarette tea is as follows:
the flavor for the bursting beads, which is prepared by adopting any one of the preparation methods for the flavor for bursting beads, which is used for highlighting the clear fragrance characteristics of the cigarette tea.
The flavor for bursting beads, which is capable of highlighting the clear fragrance characteristics of the cigarette tea, has low content of the organoleptic bad components in the green tea extract, and can fully highlight the characteristics of the green tea extract.
The technical scheme adopted by the explosion bead is as follows:
the bead explosion comprises a shell and tobacco essence, wherein the tobacco essence comprises the bead explosion spice. The bursting beads of the invention can highlight the fragrance of the cigarette tea. The dosage of the tobacco essence is preferably 15-20 mu L/grain.
The technical scheme adopted by the cigarette of the invention is as follows:
a cigarette adopting the explosion beads. The cigarette of the invention adopts the bursting beads, and can highlight the tea fragrance of the cigarette.
Detailed Description
The technical scheme of the invention is further described below with reference to the specific embodiments.
The green tea extract and the green tea extract dry powder adopted in the examples are all commercial products, the adopted Sephadex is purchased from GE Healthcare company in Sweden, the model is Sephadex LH-20, and the particle size range (dry) is 18-111 mu m; the C18 reverse phase silicse:Sup>A gel used 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 flavor for bursting beads for highlighting the clear fragrance characteristics of the cigarette tea in the embodiment comprises the following steps:
1) Dissolving green tea extract into 8% dry matter solution by adopting 70% ethanol water solution to obtain green tea extract solution;
2) Carrying out first-stage membrane separation on the obtained green tea extract solution by adopting a coiled organic membrane with a molecular weight cutoff of 50kDa, marking the cutoff of the first-stage membrane separation as MJ1 cutoff, carrying out second-stage membrane separation on the cutoff of the first-stage membrane separation by adopting a coiled organic membrane with a molecular weight cutoff of 10kDa, marking the cutoff of the second-stage membrane separation as MJ2 cutoff, carrying out third-stage membrane separation on the cutoff of the second-stage membrane separation by adopting a coiled organic membrane with a molecular weight cutoff of 1kDa, marking the cutoff of the third-stage membrane separation as MJ3 cutoff, and collecting the penetration of the third-stage membrane separation; the pressure before membrane separation of 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 permeate liquid of the third-stage membrane separation into a solution with the dry matter mass fraction of 8% by using reduced pressure distillation to obtain a concentrated solution; then carrying out two-dimensional column chromatographic separation on the concentrated solution;
the chromatographic column packing adopted in the chromatographic separation of the first dimension column is sephadex, the inner diameter of the chromatographic column is 45mm, the length of the sephadex column filled in the chromatographic column is 450mm (the dry mass of the filled sephadex is 100 g), the eluent adopted is ethanol water solution with the volume fraction of 50 percent, the flow rate of the eluent is controlled to be 10mL/min, the elution time is 200min, and the elution is respectively carried out by collecting the fractions (marked as one-dimensional 1 fraction) in the elution time period from 0min to 62min, the fractions (marked as one-dimensional 2 fraction) in the elution time period from 62min to 87min and the fractions (marked as one-dimensional 3 fraction) in the elution time period from 87min to 200min in the separation process of the first dimension column; in the second dimension column chromatography separation, enabling a one-dimensional 1 fraction, a one-dimensional 2 fraction and a one-dimensional 3 fraction to respectively enter a second dimension column for separation, wherein the packing of the second dimension column is C18 reversed phase silica gel, the inner diameter of the column is 25mm, the length of the C18 reversed phase silica gel column filled in the column is 500mm (the dry mass of the filled C18 reversed phase silica gel is 65 g), the adopted eluting solvent is ethanol water solution with 95% ethanol volume fraction, the eluting flow rate is controlled to be 12mL/min, the eluting time is 100min, and the elution is respectively carried out to collect fractions (denoted as A1 fraction) of the 34 th min-58 th elution time period in the one-dimensional 1 fraction corresponding to the two-dimensional column chromatography separation, fractions (denoted as A2 fraction) of the 26 th-40 th elution time period in the one-dimensional 2 th fraction corresponding to the two-dimensional column chromatography separation, and fractions (denoted as A3 fraction) of the 35 th-42 th elution time period in the one-dimensional 3 fraction corresponding to the two-dimensional column chromatography separation;
4) Uniformly mixing MJ1 trapped fluid, MJ2 trapped fluid, MJ3 trapped fluid, A1 fraction, A2 fraction and A3 fraction according to the mass ratio of 1:8:12:0.01:1:0.6 to obtain the flavor for the beads, which can remarkably increase the flavor-clearing characteristics of the cigarette tea, and is marked as flavor I.
Example 2
The preparation method of the flavor for bursting beads for highlighting the clear fragrance characteristics of the cigarette tea in the embodiment comprises the following steps:
1) Dissolving the green tea extract dry powder by adopting an ethanol water solution with the ethanol volume fraction of 70%, filtering to remove insoluble matters to obtain a solution with the dry matter content of 8%, and obtaining the green tea extract solution.
2) Carrying out first-stage membrane separation on the prepared green tea extract solution by adopting a coiled organic membrane with a molecular weight cutoff of 50kDa, marking the cutoff of the first-stage membrane separation as MJ1, carrying out second-stage membrane separation on the permeation solution of the first-stage membrane separation by adopting a coiled organic membrane with a molecular weight cutoff of 10kDa, marking the cutoff of the second-stage membrane separation as MJ2, carrying out third-stage membrane separation on the permeation solution of the second-stage membrane separation by adopting a coiled organic membrane with a molecular weight cutoff of 1kDa, marking the cutoff of the third-stage membrane separation as MJ3, and collecting the permeation solution of the third-stage membrane separation; the pressure before membrane separation of 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 permeate liquid separated by the third-stage membrane into a solution with the dry matter mass fraction of 8% by reverse osmosis to obtain a concentrated solution; carrying out two-dimensional column chromatographic separation on the obtained concentrated solution;
the packing of the chromatographic column adopted in the chromatographic separation of the first dimension column is sephadex, the inner diameter of the chromatographic column is 45mm, the length of the sephadex column filled in the chromatographic column is 450mm (the dry mass of the filled sephadex is 100 g), the adopted eluent is ethanol water solution with the volume fraction of 50 percent, the flow rate of the eluent is controlled to be 10mL/min, the elution time is 200min, and the fractions (marked as one-dimensional 1 fraction) in the elution time period from 0min to 62min, the fractions (marked as one-dimensional 2 fraction) in the elution time period from 62min to 87min and the fractions (marked as one-dimensional 3 fraction) in the elution time period from 87min to 200min are respectively collected; in the second dimension column chromatography separation, enabling a one-dimensional 1 fraction, a one-dimensional 2 fraction and a one-dimensional 3 fraction to respectively enter the second dimension column chromatography for separation, wherein the second dimension column packing is C18 reversed phase silica gel, the inner diameter of the chromatographic column is 25mm, the length of the C18 reversed phase silica gel column filled in the chromatographic column is 500mm (the dry mass of the filled C18 reversed phase silica gel is 65 g), the adopted eluting solvent is ethanol water solution with 95% of ethanol volume fraction, the eluting flow rate is controlled to be 12mL/min, the eluting time is 100min, the fractions (denoted as A1 fraction) of the 34 th min-58 th min eluting time period in the one-dimensional 1 fraction corresponding to the two-dimensional column chromatography separation are respectively collected, the fractions (denoted as A2 fraction) of the 26 th-40 th eluting time period in the one-dimensional 3 fraction corresponding to the 35 th-42 th eluting time period (denoted as A3 fraction) in the two-dimensional column chromatography separation;
4) Uniformly mixing MJ1 trapped fluid, MJ2 trapped fluid, MJ3 trapped fluid, A1 fraction, A2 fraction and A3 fraction according to the mass ratio of 2:5:14:0.02:2:0.8 to obtain the flavor for the beads, which can remarkably increase the flavor-clearing characteristics of the cigarette tea, and is marked as flavor II.
Example 3
The preparation method of the flavor for bursting beads for highlighting the clear fragrance characteristics of the cigarette tea in the embodiment comprises the following steps:
steps 1) to 3) are the same as steps 1) to 3) of example 2, and are not repeated here;
in the step 4), the MJ1 trapped fluid, the MJ2 trapped fluid, the MJ3 trapped fluid, the A1 fraction, the A2 fraction and the A3 fraction are uniformly mixed according to the mass ratio of 1.5:6:10:0.01:1.5:0.6 to obtain the bead-blasting spice capable of remarkably increasing the clear aroma characteristic of the cigarette tea, and the bead-blasting spice is denoted as spice III.
In the embodiment of the flavor for bursting beads, which highlights the fragrance of cigarette tea, of the invention, the flavor for bursting beads, which highlights the fragrance of cigarette tea, is prepared by the preparation method of any one of the embodiments 1 to 3, and is not described herein.
Example 4
The explosive bead of the embodiment comprises a shell and tobacco essence wrapped in the shell, wherein the tobacco essence is the essence I prepared in the embodiment 1, the dosage of the tobacco essence in the explosive bead is 15 mu L/particle, and the particle size of the explosive bead is 3.3mm.
Example 5
The explosive beads of the embodiment comprise a shell and tobacco essence wrapped in the shell, wherein the tobacco essence is the essence II prepared in the embodiment 2, the dosage of the tobacco essence in the explosive beads is 18 mu L/particle, and the particle size of the explosive beads is 3.5mm.
Example 6
The explosive beads of the embodiment comprise a shell and tobacco essence wrapped in the shell, wherein the tobacco essence is the essence II prepared in the embodiment 3, the dosage of the tobacco essence in the explosive beads is 20 mu L/particle, and the particle size of the explosive beads is 3.4mm.
Example 7
The cigarette of this embodiment includes a cigarette section and a filter tip, and 1 explosive bead is placed in the filter tip, and the explosive bead used is the explosive bead of embodiment 4.
Example 8
The cigarettes of this example differ from those of example 7 only in that: the bursting beads used in this example were the bursting beads of example 5.
Example 9
The cigarettes of this example differ from those of example 7 only in that: the bursting beads used in this example were the bursting beads of example 6.
Comparative example 1
The bursting beads of this comparative example differ from the bursting beads of example 1 only in that: the tobacco flavor in the explosive beads of the comparative example is obtained by dissolving the green tea extract adopted in the example 1 with 70% ethanol by volume fraction to 5% solution by mass fraction of dry matter, and the dosage of the tobacco flavor in the explosive beads is 15 mu L/granule.
Comparative example 2
The bursting beads of this comparative example differ from the bursting beads of example 2 only in that: the tobacco essence in the explosive beads of the comparative example is obtained by dissolving the green tea extract dry powder adopted in the example 2 into a solution with the dry matter mass fraction of 5% by adopting an ethanol water solution with the ethanol volume fraction of 70%, and the dosage of the tobacco essence in the explosive beads is 18 mu L/grain.
Experimental example
The flavor for bead blasting prepared in examples 1 to 3, the green tea extract (green tea extract) used in example 1 and the green tea extract (green tea extract dry powder, abbreviated as green tea powder in table 1) used in example 2 were each prepared in the optimal amounts for bead blasting (i.e., bead blasting of examples 4 to 6 and comparative examples 1 to 2), 1 particle was added to a reference cigarette filter tip, sensory evaluation was performed by referring to YC/T497-2014 "method for sensory evaluation of style of chinese cigarette", and suction evaluation was performed by 10 professional cigarette sensory evaluators, and the results are shown in table 1.
Table 1 sensory evaluation results
As can be seen from the data in Table 1, compared with the reference cigarettes and green tea extracts, after the cigarettes are added with the explosive beads taking the spice I, the spice II and the spice III as the tobacco essence, the tea aroma, the faint scent and the green flavor of the reference cigarettes can be obviously improved, and indexes such as the aroma, the richness, the fineness, the softness and the roundness of the reference cigarettes are improved to different degrees. These results show that the perfume of the invention can obviously improve the fragrance of the cigarette tea and effectively improve the sensory quality of the cigarettes.
Claims (9)
1. A preparation method of a flavor for bursting beads for highlighting the clear fragrance characteristics of cigarette tea is characterized by comprising the following steps: the method comprises the following steps:
1) Carrying out first-stage membrane separation on the green tea extract solution by adopting a coiled organic membrane with a molecular weight cutoff of 50kDa, then carrying out second-stage membrane separation on the permeate by adopting a coiled organic membrane with a molecular weight cutoff of 10kDa, and then carrying out third-stage membrane separation on the permeate separated by the second-stage membrane by adopting a coiled organic membrane with a molecular weight cutoff of 1 kDa;
2) Concentrating the permeate liquid separated by the third-stage membrane to obtain concentrated liquid, and then carrying out two-dimensional column chromatographic separation on the concentrated liquid;
the packing of the chromatographic column adopted in the chromatographic separation of the first dimension column is sephadex, and the length-diameter ratio of the sephadex column is 10:1; the packing of the chromatographic column adopted in the second dimension column chromatographic separation is C18 reverse phase silica gel, and the length-diameter ratio of the C18 reverse phase silica gel column is 20:1;
during the first dimension column chromatographic separation, an ethanol water solution with the volume fraction of 50% is taken as an eluent, the flow rate of the eluent corresponding to each 227.8125 pi mL volume of column bed is controlled to be 10mL/min, and the flow fractions of the elution time periods from 0min to 62min, the flow fractions of the elution time periods from 62min to 87min and the flow fractions of the elution time periods from 87min to 200min are respectively collected;
during the second dimension column chromatography separation, enabling the fractions collected during the separation of each first dimension column chromatography to enter the second dimension column chromatography respectively, taking ethanol water solution with the ethanol volume fraction of 95% as eluent, controlling the flow rate of the eluent corresponding to each 78.125 pi mL volume of column bed to be 12mL/min, and collecting the fractions in the 34 th to 58 th elution time periods in the two dimension column chromatography separation process corresponding to the fractions in the 0 th to 62 th elution time periods, the fractions in the 26 th to 40 th elution time periods in the two dimension column chromatography separation process corresponding to the fractions in the 62 th to 87 th elution time periods and the fractions in the 35 th to 42 th elution time periods in the two dimension column chromatography separation process corresponding to the fractions in the 87 th to 200 th elution time periods respectively;
3) The method comprises the steps of 1) mixing the trapped fluid of the first-stage membrane separation, the trapped fluid of the second-stage membrane separation, the trapped fluid of the third-stage membrane separation, the fractions of the 34 th min-58 th min elution time period, the fractions of the 26 th min-40 th min elution time period and the fractions of the 35 th min-42 th min elution time period collected in 2);
the compounding is that 1-2 parts by weight of trapped fluid of first-stage membrane separation, 4-8 parts by weight of trapped fluid of second-stage membrane separation, 10-15 parts by weight of trapped fluid of third-stage membrane separation, 0.01-0.02 parts by weight of fractions in an elution time period from 34min to 58min, 1-2 parts by weight of fractions in an elution time period from 26min to 40min and 0.5-0.8 parts by weight of fractions in an elution time period from 35min to 42min are uniformly mixed.
2. The method for preparing the flavor for bursting beads, which is characterized by highlighting the clear flavor characteristics of the cigarette tea according to claim 1, which is characterized in that: the green tea extract is one or any combination of green tea extract, green tea absolute, green tea tincture and green tea extract dry powder.
3. The method for preparing the flavor for bursting beads, which is characterized by highlighting the clear flavor characteristics of the cigarette tea according to claim 1, which is characterized in that: in the step 1), the green tea extract solution is a solution with a dry matter mass fraction of 8% -10% obtained by dissolving green tea extract in an ethanol water solution with an ethanol volume fraction of 50% -70%.
4. The method for preparing the flavor for bursting beads, which is characterized by highlighting the clear flavor characteristics of the cigarette tea according to claim 1, which is characterized in that: in the step 2), the mass fraction of the dry matter in the concentrated solution is 8% -10%.
5. The method for preparing the flavor for bursting beads, which is characterized by highlighting the clear flavor characteristics of the cigarette tea according to claim 1, which is characterized in that: in the step 2), the inner diameter of a chromatographic column used for the chromatographic separation of the first dimension column is 45mm, and the filling length of the sephadex in the chromatographic column is 450mm; the flow rate of the eluent in the first dimension column chromatography was 10mL/min.
6. The method for preparing the flavor for bursting beads, which is characterized by highlighting the clear flavor characteristics of the cigarette tea according to claim 1, which is characterized in that: in the step 2), the inner diameter of a chromatographic column used for the chromatographic separation of the second dimension column is 25mm, and the filling length of C18 reverse phase silica gel in the chromatographic column is 500mm; the flow rate of the eluent in the second dimension column chromatography is 12mL/min.
7. A flavor for popping beads prepared by the method for preparing a flavor for popping beads which is characterized in that the flavor for popping cigarette tea is emphasized according to any one of claims 1 to 6.
8. The utility model provides a explode pearl, includes shell and tobacco essence, its characterized in that: the tobacco flavor comprises the bead-blasting flavor according to claim 7.
9. A cigarette employing the bead of claim 8.
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