CN115806857A - Preparation method of tobacco extract special flavor group - Google Patents
Preparation method of tobacco extract special flavor group Download PDFInfo
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- CN115806857A CN115806857A CN202211130793.XA CN202211130793A CN115806857A CN 115806857 A CN115806857 A CN 115806857A CN 202211130793 A CN202211130793 A CN 202211130793A CN 115806857 A CN115806857 A CN 115806857A
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- 241000208125 Nicotiana Species 0.000 title claims abstract description 111
- 235000002637 Nicotiana tabacum Nutrition 0.000 title claims abstract description 111
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
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- 239000000741 silica gel Substances 0.000 claims description 8
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Abstract
The invention relates to a preparation method of a tobacco extract special flavor group, and belongs to the technical field of tobacco flavors. The method comprises the following steps: separating the tobacco extract solution by 2-15 stages of membranes to obtain membrane separation trapped fluid of each stage and membrane separation permeate of the last stage; the permeation liquid of the last stage of membrane separation is split into two-dimensional fractions with different ultraviolet absorption properties through two-dimensional column chromatography; and performing sensory evaluation on the membrane separation trapped fluid and the two-dimensional flow at each stage, and determining a component capable of highlighting the sensory effect characteristics of the tobacco extract as a characteristic flavor group of the tobacco extract. The method has the comprehensive capability of separating flavor components with different molecular sizes and different molecular polarities, can fully split the flavor components of the tobacco extract, accurately position the characteristic flavor groups of the tobacco extract, and has important significance for refinement and diversification of tobacco extract products.
Description
Technical Field
The invention belongs to the technical field of tobacco flavors, and particularly relates to a preparation method of a tobacco extract special flavor group.
Background
Accurate flavoring and digital product design become the future development trend of cigarette flavoring. The monomer fragrance raw material has great advantages in the aspects of precise fragrance blending and digital product design, does not cause irrelevant interference and is beneficial to embodying the flavor characteristics of the fragrance. However, there is a significant technical bottleneck in the preparation of monomeric fragrance raw materials, and many important monomeric fragrance raw materials still depend on import.
The independent research and development of cigarette flavor raw materials are important components of cigarette blending core technology in the industry and are key factors influencing the high-quality development of enterprises. The independent research and development and self-guarantee capability of the essence and spice core technology for the cigarettes are promoted and improved, the technical bottleneck of monomer spice raw material preparation is broken through, excessive dependence on important monomer spice raw materials is avoided, and the strategic safety of Chinese cigarettes is guaranteed. Therefore, how to break through the technical barrier of independent development of important flavor raw materials has become a hot issue of attention and research in the tobacco industry at present.
The tobacco extract is one of the most important flavor raw materials for blending flavor of Chinese cigarettes, and has the effects of enhancing the characteristic flavor of the tobacco and improving the sensory quality of the cigarettes. The cigarette enterprises can relieve the contradiction of insufficient supply of high-quality tobacco leaf raw materials to a certain extent by reasonably utilizing the tobacco extracts. However, the tobacco extract has complex components and various functions, and sometimes interferes with the aims of accurate flavoring and digital product design while endowing and enhancing the flavor and style of cigarettes. In addition, various flavor characteristics of the tobacco extract coexist, and different from synthetic spices, the flavor characteristics of the tobacco extract are still derived from the combined action of various components, so that the use freedom of the product is reduced to a certain extent.
The existing tobacco extract fine processing technology usually aims at removing impurities, and although the quality of the obtained finished product is improved, the functional focusing degree of the product is insufficient. How to obtain a characteristic flavor group of a tobacco extract with focused functions and multiple components fully highlights the characteristics of the tobacco extract, further improves the diversity of homologous products, provides more abundant and effective supply of flavor raw materials for accurate flavor blending and digital product design, and is a new challenge facing the fine processing industry of the tobacco extract.
Disclosure of Invention
The invention aims to provide a preparation method of a tobacco extract special flavor group, which can be used for more fully splitting flavor components of a tobacco extract and accurately positioning and obtaining the tobacco extract special flavor group.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a tobacco extract special flavor group comprises the following steps: separating the tobacco extract solution by 2-15 stages of membranes to obtain membrane separation trapped fluid of each stage and membrane separation permeate of the last stage; 2-15 stages of membrane separation are sequentially carried out according to the pore size of the membrane from large to small, wherein the pore size of the membrane is selected from one or two or three of microfiltration, ultrafiltration and nanofiltration;
the permeation liquid of the last stage of membrane separation is split into two-dimensional fractions with different ultraviolet absorption properties through two-dimensional column chromatography;
and performing sensory evaluation on the membrane separation trapped fluid and the two-dimensional flow fractions at each stage, and determining a component capable of highlighting the sensory action characteristics of the tobacco extract as a characteristic flavor group of the tobacco extract.
According to the preparation method of the tobacco extract characteristic flavor group, the tobacco extract is used as a raw material, the technical advantages of membrane separation and column chromatography separation are integrated, the separation process of the tobacco extract is optimized, each functional fraction is split, a set of tobacco extract refining and separating method covering multi-dimensional membrane separation and two-dimensional column chromatography separation is developed, the tobacco extract characteristic flavor group with prominent functions is obtained by combining sensory effect evaluation, and the tobacco extract characteristic flavor group is applied to cigarette flavoring, so that the sensory quality and the product characteristics of the cigarette can be remarkably improved.
The preparation method of the tobacco extract characteristic flavor group has the comprehensive capability of separating flavor components with different molecular sizes and different molecular polarities, can more fully split the flavor components of the tobacco extract and accurately position the tobacco extract characteristic flavor group compared with the traditional processing modes of precipitation separation, activated carbon decoloration, resin impurity removal, single membrane separation, single column chromatography and the like, and has important significance for refinement and diversification of tobacco extract products.
The fractions with consistent ultraviolet absorption properties have similar structures and functions, so that the functional components of the tobacco extract can be split according to the difference of the ultraviolet absorption properties, and functional focusing is realized.
Preferably, in the two-dimensional column chromatography, the filler used in the first-dimensional column chromatography is sephadex, and the filler used in the second-dimensional column chromatography is C18 reverse phase silica gel.
Further preferably, during the first-dimension column chromatographic separation, monitoring the ultraviolet absorption signal of the first-dimension effluent, respectively trapping the one-dimension fractions of different ultraviolet absorption signals by using 2-8 trapping columns, allowing the eluent of the trapping columns to enter a second-dimension column chromatography, monitoring the ultraviolet absorption signal of the second-dimension effluent, and collecting the two-dimension fractions with different ultraviolet absorption properties. More preferably, the ultraviolet detection wavelength of the ultraviolet absorption signal is 230nm and/or 280nm. In experiments, ultraviolet detection wavelengths of 230nm and/or 280nm are selected to better reflect the ultraviolet absorption information of the tobacco extract.
Preferably, the eluent used for the first dimension column chromatography and the second dimension column chromatography is water, ethanol or ethanol water solution.
Further preferably, the second-dimension column chromatography adopts gradient elution, the eluent is 10-90% ethanol water solution, and the concentration of the ethanol water solution is gradually increased along with the time.
Preferably, the tobacco extract is selected from one of Yuyan extract, burley tobacco extract and Virginia tobacco extract.
Preferably, 4-stage membrane separation is adopted, and the 4-stage membrane separation is sequentially a 50nm ceramic membrane, a 12nm ceramic membrane or a 50kDa roll type organic membrane, a 5nm ceramic membrane or a 10kDa ceramic membrane and a 1kDa roll type organic membrane.
Preferably, the concentration of the tobacco extract solution is 10wt% to 20wt%. The concentration is a dry matter mass concentration meter.
Preferably, the items of sensory evaluation include a plurality of the following items: aroma, richness, fineness, softness, mellow, miscellaneous gas, smoke concentration, strength, oral cavity stimulation, oral cavity residue, convergence, throat stimulation, throat dryness, nasal cavity stimulation, sweet taste, sour taste, bitter taste, cool taste, flue-cured tobacco fragrance, sun-cured tobacco fragrance, faint scent, fruit fragrance, spicy fragrance, costustoot, green essence fragrance, flower fragrance, herb fragrance, bean fragrance, cocoa fragrance, milk fragrance, paste fragrance, baking fragrance, tea fragrance and sweet fragrance. By performing sensory evaluation on the items, a tobacco extract flavor group can be obtained more accurately.
Further preferably, the flavor panel comprises at least one of the membrane separation retentate stages and at least one of the two-dimensional fractions.
Drawings
FIG. 1 is a first dimension column chromatography ultraviolet absorption spectrum of Yuyan extract in example 1 of the present invention;
FIG. 2 shows second dimension column chromatography ultraviolet absorption spectra (fractions A1-A8) of Yu-Yan extract in example 1 of the present invention;
FIG. 3 is a second dimension column chromatography ultraviolet absorption spectrum (fractions B1-B6) of Yuyan extract in example 1 of the present invention;
FIG. 4 is a first dimension column chromatography UV absorption spectrum of burley tobacco extract in example 2 of the present invention;
FIG. 5 shows second dimension column chromatography UV absorption spectra (fractions A1-A6) of burley tobacco extract in example 2 of the present invention;
FIG. 6 shows second dimension column chromatography UV absorption spectra (fractions B1-B6) of burley tobacco extract in example 2 of the present invention;
FIG. 7 is a first dimension column chromatography UV absorption spectrum of a Virginia tobacco extract in example 3 of the present invention;
FIG. 8 shows second dimension column chromatography UV absorption spectra (A1-A4) of Virginia tobacco extract in example 3 of the present invention;
FIG. 9 shows second dimension column chromatography UV absorption spectra (B1-B5) of Virginia tobacco extract in example 3 of the present invention.
Detailed Description
The method takes the tobacco extract as a processing object, comprehensively adopts a multi-stage membrane separation technology and a two-dimensional column chromatography separation technology to separate the tobacco extract, screens each separated fraction, and positions a characteristic flavor group of the tobacco extract through sensory evaluation.
And after multi-stage membrane separation, membrane separation trapped fluid at each stage and membrane separation permeate at the last stage are obtained. The permeate of the last stage of membrane separation can be concentrated according to the condition so as to facilitate the separation of two-dimensional column chromatography. Can be concentrated until the dry matter content of the solution is 8-10 wt%. Reverse osmosis or reduced pressure distillation may be used.
In the first-dimension column chromatography, the separation parameters can be determined by experimental optimization, for example, in the first-dimension column chromatography, the flow rate of the eluent can be 1-20mL/min, and the elution time can be more than 200min. Further, the flow rate of the eluent is 8-10mL/min, and the elution time is 200-400min.
The number of the trapping columns can be set according to the ultraviolet property division condition of the first-dimension column chromatography effluent, and is generally 2-8. For example, for Yuyan extract, burley tobacco extract, virginia tobacco extract, the number of trapping columns may be 4, the termination time for the first trapping column is 46-48min, the termination time for the second trapping column is 55-66min, the termination time for the third trapping column is 73-99min, and the termination time for the fourth trapping column is 200-250min.
The determination process of the separation parameters of the second dimension column chromatography is consistent with the separation of the first dimension column chromatography. For example, the flow rate of the eluent can be 8-10mL/min, and the elution time can be 100-200min.
The present invention is further illustrated by the following examples. Sephadex is available from GE Healthcare, sweden, under the type Sephadex LH-20, with a particle size range (dry) of 18-111 μm. C18 reverse phase silicse:Sup>A gel was purchased from YMC, japan, and was filled with YMC ODS-A general-purpose type C18 filler, and had se:Sup>A particle size of 50 μm.
In the following examples, "%" is a volume percentage unless otherwise specified.
1. Examples of methods for preparing a distinctive flavor panel of tobacco extract
Example 1
The preparation method of the tobacco extract special flavor group of the embodiment comprises the following steps:
(1) Dissolving Yuyan extract with 50vol% ethanol solution to obtain Yuyan extract solution with dry matter content of 20wt%, and centrifuging to remove insoluble substances.
(2) 9000g of centrifuged Yuyan extract solution is subjected to four-stage membrane separation:
the four-stage membrane is sequentially a 50nm ceramic membrane, a 12nm ceramic membrane, a 5nm ceramic membrane and a 1kDa roll-type organic membrane, each stage of membrane separation permeate is used as a raw material for next stage of membrane separation, each stage of membrane separation retentate is retained at the same time, and finally 4 stages of membrane separation retentate and the last stage of membrane separation permeate are obtained, and the 4 stages of membrane separation retentate are sequentially numbered as MJ1 (1356 g), MJ2 (876 g), MJ3 (925 g) and MJ4 (956 g).
(3) And concentrating the permeate of the last stage of membrane separation by reverse osmosis until the dry matter content of the solution is 8wt% to obtain a concentrated solution.
(4) Taking 50mL of concentrated solution for two-dimensional column chromatographic separation:
firstly, performing first-dimension column chromatographic separation, wherein a filler is sephadex, the inner diameter of a chromatographic column is 45mm, the length of a sephadex column filled in the chromatographic column is 450mm (the dry mass of the filled sephadex is 100 g), an eluent is 10vol% ethanol solution, the flow rate is 8mL/min, the elution time is 400min, and according to the change condition of an ultraviolet absorption signal (the ultraviolet detection wavelength is 230nm and 280nm and is recorded as wavelength A and wavelength B), the effluent of the first-dimension column chromatography is divided into 4 groups of effluents with different ultraviolet absorption properties, as shown in fig. 1, wherein one-dimension A is the ultraviolet absorption spectrum of the effluent of the first-dimension column chromatography with the wavelength of 230nm, and one-dimension B is the ultraviolet absorption spectrum of the first-dimension column chromatography with the wavelength of 280nm.
Specifically, four trapping columns are arranged, and the trapping time is divided into: collecting the effluent of the trap column after 0-46min,46-55min,55-85min and 85-250 min. Eluting the trapping column by using an eluent, enabling the eluent to enter a second-dimension chromatographic column, enabling the chromatographic packing of the second-dimension column to be C18 reverse phase silica gel, enabling the chromatographic packing of the second-dimension chromatographic column to be C18 reverse phase silica gel, enabling the chromatographic column to have an inner diameter of 25mm, enabling the length of the C18 reverse phase silica gel filled in the chromatographic column to be 500mm (the dry mass of the filled C18 reverse phase silica gel is 65 g), enabling the eluent to be an ethanol solution, enabling the elution procedure to be gradient elution (0-100 min) from a 10% ethanol solution (0 min) to a 90% ethanol solution (100 min), enabling the concentration of the ethanol solution to be uniformly increased by 0.8% per minute), enabling the flow rate to be 8mL/min, enabling the separation time to be 100min, collecting separated fractions by using test tubes, collecting 15mL of the eluent by each test tube, after the separation is finished, merging corresponding fractions under the same ultraviolet absorption peak or fractions without ultraviolet absorption or whole fractions under the same ultraviolet absorption peak as a characteristic flavor cluster according to the condition of ultraviolet absorption signals of the two-dimension chromatographic column, and obtaining 14 groups respectively numbered A1-A8 and B1-B6.
Specifically, there are two second-dimension column chromatographs, and the eluents of the first-stage trapping column and the third-stage trapping column sequentially enter the first second-dimension column chromatograph, as shown in fig. 2, wherein two-dimension A1 is an ultraviolet absorption spectrum of the effluent of the first second-dimension column chromatograph with a wavelength of 230nm, two-dimension B1 is an ultraviolet absorption spectrum of the effluent of the first second-dimension column chromatograph with a wavelength of 280nm, the eluents of the second and fourth trapping columns enter a second dimension column chromatography in sequence, as shown in fig. 3, wherein two-dimension A2 is an ultraviolet absorption spectrum of the second dimension column chromatography effluent at a wavelength of 230nm, and two-dimension B2 is an ultraviolet absorption spectrum of the second dimension column chromatography effluent at a wavelength of 280nm. The separation times for the fractions A1 to A8 and B1 to B6 are shown in Table 1 below.
TABLE 1 separation time of A1-A8 and B1-B6
(5) Evaluation of organoleptic characteristics:
preparing MJ1, MJ2, MJ3, MJ4, A1-A8 and B1-B6 into 10wt% dry matter solution with 50vol% ethanol solution, injecting each solution into a reference cigarette with 100ppm injection amount, balancing for 2 days under constant temperature and humidity conditions, and performing sensory characteristic description and scoring on the reference cigarette without additives and the cigarettes with each fraction separated from Yu smoke extract. The evaluation results are shown in table 2, and components MJ1, A1, and A3 capable of highlighting sensory characteristics of the tobacco extract were selected as a special flavor group of the yuyan extract tobacco extract according to the evaluation results.
Table 2 sensory evaluation results of characteristic flavor groups of yuyan extract tobacco extract in example 1
As can be seen from the table 2, the Yuyan extract MJ1 can improve the tobacco fragrance of the reference cigarette, increase the baking aroma, sweetness, aroma, richness, fineness, softness and roundness, and reduce miscellaneous gas; the component A1 obtained by two-dimensional column chromatographic separation can improve the tobacco aroma and baking aroma of reference cigarettes, improve the sweet taste, and increase the aroma, richness and smoke concentration; the component A3 obtained by two-dimensional column chromatographic separation can improve the smoke concentration and the tobacco fragrance of the flue-cured tobacco.
Example 2
The preparation method of the tobacco extract special flavor group of the embodiment comprises the following steps:
(1) Dissolving the burley tobacco extract with 50% ethanol to obtain a burley tobacco extract solution with dry matter content of 15wt%, and filtering to remove insoluble substances.
(2) 9564g of the filtered burley tobacco extract solution was subjected to a four-stage membrane separation:
the four-stage membrane is sequentially a 50nm ceramic membrane, a 50kDa roll-type organic membrane, a 5nm ceramic membrane and a 1kDa roll-type organic membrane, each stage of membrane separation permeate is used as a raw material for next stage of membrane separation, each stage of membrane separation retentate is retained at the same time, and finally 4 stages of membrane separation retentate and a last stage of membrane separation permeate are obtained, and the 4 stages of membrane separation retentate are sequentially numbered as MJ1 (1730 g), MJ2 (59.9 g), MJ3 (2819 g) and MJ4 (2819 g).
(3) And concentrating the permeate of the last stage of membrane separation by using reduced pressure distillation until the dry matter content of the solution is 10wt% to obtain a concentrated solution.
(4) Taking 35mL of concentrated solution for two-dimensional column chromatography separation:
first, a first-dimension column chromatography separation is performed, wherein a filler is sephadex (same specification as example 1), an eluent is water, a flow rate is 8mL/min, an elution time is 200min, and according to the change condition of an ultraviolet absorption signal (ultraviolet detection wavelengths are 230nm and 280nm, and are recorded as wavelength a and wavelength B), the effluent of the first-dimension column chromatography is divided into 4 groups of effluents with different ultraviolet absorption properties, as shown in fig. 4, wherein one-dimension a is an ultraviolet absorption spectrum of the effluent of the first-dimension column chromatography to the wavelength of 230nm, and one-dimension B is an ultraviolet absorption spectrum of the effluent of the first-dimension column chromatography to the wavelength of 280nm. The trapping time of the four trapping columns was divided into: collecting the effluent of the trap column after 0-48min,48-58min,58-73min and 73-200 min.
Eluting the trapping column by using an eluent, enabling the eluent to enter a second-dimension chromatographic column, enabling a chromatographic filler of the second-dimension column to be C18 reverse phase silica gel (the specification is the same as that of example 1), enabling the eluent to be an ethanol solution, enabling the elution procedure to be that the gradient elution is carried out from a 10% ethanol solution (0 min) to a 90% ethanol solution (100 min), enabling the concentration of the ethanol solution to be uniformly increased by 0.8% per minute, enabling the flow rate to be 8mL/min, enabling the separation time to be 100min, collecting separated fractions by using test tubes, enabling each test tube to collect 15mL of eluent, after the separation is finished, combining corresponding fractions under the same ultraviolet absorption peak or fractions without ultraviolet absorption integrally according to the ultraviolet absorption signal conditions of the two-dimension chromatographic column separation fractions (the ultraviolet detection wavelength is 230nm and 280nm and is marked as wavelength A and wavelength B), and obtaining 12 fractions which are respectively marked as A1-A6 and B1-B6.
The two second-dimension column chromatographs are provided, the eluent of the first-stage trapping column and the eluent of the third-stage trapping column enter the first second-dimension column chromatograph in sequence, as shown in figure 5, wherein, the two-dimension A1 is the ultraviolet absorption spectrum of the effluent of the first second-dimension column chromatograph to the wavelength of 230nm, and the two-dimension B1 is the ultraviolet absorption spectrum of the effluent of the first second-dimension column chromatograph to the wavelength of 280 nm; the eluents of the second and fourth trapping columns enter a second dimension column chromatography in sequence, as shown in fig. 6, wherein, the two dimension A2 is the ultraviolet absorption spectrum of the effluent of the second dimension column chromatography with the wavelength of 230nm, and the two dimension B2 is the ultraviolet absorption spectrum of the effluent of the second dimension column chromatography with the wavelength of 280nm.
The separation times for the A1-A6 and B1-B6 fractions are shown in Table 3 below.
Table 3 two-dimensional fraction separation time of example 2
| Fraction(s) of | Separation time/min | Fraction(s) of | Separation time/min |
| A1 | 50-81 | B1 | 75-101 |
| A2 | 83-141 | B2 | 103-146 |
| A3 | 150-173 | B3 | 147-166 |
| A4 | 175-201 | B4 | 202-225 |
| A5 | 203-214 | B5 | 227-270 |
| A6 | 216-241 | B6 | 272-293 |
(5) Evaluation of organoleptic characteristics:
injecting each fraction solution onto a reference cigarette at an injection amount of 100ppm, balancing for 2 days under constant temperature and humidity conditions, carrying out sensory characteristic description and scoring on the reference cigarette without adding and the cigarettes with each fraction obtained by adding Yu tobacco extract for separation, wherein the number of evaluators is 11, the evaluation result is shown in table 4, and according to the evaluation result, selecting components MJ1, A3, A5 and B5 capable of highlighting the sensory effect characteristics of the tobacco extract as a special flavor group of the burley tobacco extract.
Table 4 sensory evaluation results of the flavor and taste groups of burley tobacco extracts in example 2
As can be seen from Table 4, the trapped fluid MJ1 obtained by separating the burley tobacco extract through a 50nm membrane can improve the tobacco fragrance of the sun-cured tobacco of the reference cigarette, has outstanding sensory characteristics, and simultaneously has the effects of reducing offensive odor, remarkably improving strength, reducing throat irritation and throat dryness and the like. The component A3 of the burley tobacco extract separated by the two-dimensional column chromatography can obviously increase the sun-cured tobacco fragrance of the reference cigarette and increase the smoke concentration and richness; the component A5 can increase the richness, smoke concentration and strength of the reference cigarette; the component B5 can obviously increase the sweet taste of the reference cigarette and increase the fine, smooth, soft and mellow degree.
Example 3
The preparation method of the tobacco extract special flavor group of the embodiment comprises the following steps:
(1) Dissolving Virginia tobacco extract with 50vol% ethanol solution to obtain Virginia tobacco extract solution with dry matter content of 11wt%, and filtering to remove insoluble substances.
(2) 5467g of the filtered tobacco extract solution from Virginia were subjected to a four-stage membrane separation:
the four-stage membrane sequentially comprises a 50nm ceramic membrane, a 12nm ceramic membrane, a 10kDa ceramic membrane and a 1kDa roll-type organic membrane, permeate of each stage of membrane separation is used as a raw material for the next stage of membrane separation, retentate of each stage of membrane separation is kept simultaneously, 4 stages of membrane separation retentate and permeate of the last stage of membrane separation are finally obtained, and the 4 stages of membrane separation retentate are numbered as MJ1 (487 g), MJ2 (341.4 g), MJ3 (301 g) and MJ4 (179 g) sequentially.
(3) And concentrating the permeate of the last stage of membrane separation by using reduced pressure distillation until the dry mass of the solution is 8.5wt% to obtain a concentrated solution.
(4) Taking 20mL of concentrated solution for two-dimensional column chromatographic separation:
first, a first-dimension column chromatography separation is performed, wherein a filler is sephadex (same as the specification in example 1), an eluant is water, a flow rate is 10mL/min, an elution time is 400min, and according to the change situation of an ultraviolet absorption signal (ultraviolet detection wavelength is 230nm and 280nm, and is recorded as wavelength a and wavelength B), the effluent of the first-dimension column chromatography is divided into 4 groups of effluents with different ultraviolet absorption properties, as shown in fig. 7, wherein one-dimension a is an ultraviolet absorption spectrum of the effluent of the first-dimension column chromatography at a wavelength of 230nm, and one-dimension B is an ultraviolet absorption spectrum of the effluent of the first-dimension column chromatography at a wavelength of 280nm. 4 groups of effluent liquids with different ultraviolet absorption properties enter 4 trapping columns, and the trapping time of the 4 trapping columns is divided into: collecting the effluent of 4 groups of trapping columns after 0-48min, 48-66min, 68-99min and 99-200 min.
Eluting the trapping column by using an eluent, enabling the eluent to enter a second-dimension chromatographic column, enabling a chromatographic filler of the second-dimension column to be C18 reverse phase silica gel (the specification is the same as that of example 1), enabling the eluent to be an ethanol solution, enabling the elution procedure to be that the gradient elution is carried out from a 10% ethanol solution (0 min) to a 90% ethanol solution (100 min), enabling the concentration of the ethanol solution to be uniformly increased by 0.8% per minute, enabling the flow rate to be 8mL/min, enabling the separation time to be 100min, collecting separated fractions by using test tubes, enabling each test tube to collect 15mL of eluent, after the separation is finished, combining corresponding fractions under the same ultraviolet absorption peak or fractions without ultraviolet absorption integrally according to the ultraviolet absorption signal conditions of the two-dimension chromatographic column separation fractions (the ultraviolet detection wavelength is 230nm and 280nm and is marked as wavelength A and wavelength B), and obtaining 9 fractions which are respectively marked as A1-A4 and B1-B5.
The two second-dimension column chromatographs are provided, and the eluents of the first-stage trapping column and the third-stage trapping column enter the first second-dimension column chromatograph in sequence, as shown in fig. 8, wherein, the two-dimension A1 is the ultraviolet absorption spectrum of the effluent of the first second-dimension column chromatograph to the wavelength of 230nm, and the two-dimension B1 is the ultraviolet absorption spectrum of the effluent of the first second-dimension column chromatograph to the wavelength of 280 nm; the eluents of the second and fourth trapping columns enter a second dimension column chromatography in sequence, as shown in fig. 9, wherein two-dimension A2 is an ultraviolet absorption spectrum of the second dimension column chromatography effluent at a wavelength of 230nm, and two-dimension B2 is an ultraviolet absorption spectrum of the second dimension column chromatography effluent at a wavelength of 280nm.
The separation times for the A1-A4 and B1-B5 fractions are shown in Table 5 below.
Table 5 two-dimensional fraction separation time of example 3
| Fractions of the invention | Time of separation | Fractions of the invention | Time of separation |
| A1 | 49-72 | B1 | 101-121 |
| A2 | 74-141 | B2 | 123-192 |
| A3 | 149-172 | B3 | 202-224 |
| A4 | 174-241 | B4 | 226-262 |
| B5 | 264-293 |
(5) Evaluation of organoleptic characteristics:
MJ1, MJ2, MJ3, MJ4, A1-A4 and B1-B5 are prepared into 10wt% of solution with 50vol% of ethanol solution, each solution is injected onto a reference cigarette in 50ppm of injection amount, the solution is balanced for 2 days under constant temperature and humidity conditions, sensory characteristics of the reference cigarette without adding and the cigarettes with each fraction obtained by adding Yu cigarette extract separation are described and classified, an evaluator is 11 persons, the evaluation result is shown in table 6, and according to the evaluation result, the components of MJ1, MJ2, MJ3, A1 and A3 which can highlight the sensory characteristics of the tobacco extract are selected as a special flavor group of the Virginia tobacco extract.
Table 6 sensory evaluation results of characteristic flavor groups of the virginia tobacco extract in example 3
As can be seen from table 6, MJ1 can significantly improve the reference cigarette baking aroma and the flue-cured tobacco aroma, significantly improve the aroma and richness, and reduce miscellaneous gases, oral cavity irritation, oral cavity residue, throat irritation, dry sensation and nasal cavity irritation; MJ2 can remarkably improve the baking aroma of a reference cigarette, reduce the bitter taste, increase the tobacco aroma of a flue-cured tobacco, improve the delicate, soft and round feeling, and reduce the oral cavity stimulation and the dry feeling; the trapped fluid obtained by MJ3 can improve the tobacco fragrance and the acid taste of the flue-cured tobacco of the reference cigarette, reduce the bitter taste, improve the fragrance, be fine, smooth, soft and round, reduce the miscellaneous gas and reduce the oral cavity stimulation and the nasal cavity stimulation; the component A1 can obviously improve the tobacco fragrance of reference cigarettes, improve the baking aroma and the sweet aroma, obviously increase the aroma, richness, fineness, softness and smoothness and reduce the miscellaneous gas; the component A3 can increase the tobacco aroma, baking aroma and sweet aroma of reference cigarette and flue-cured tobacco, and increase sweet taste.
Claims (11)
1. A preparation method of a tobacco extract special flavor group is characterized by comprising the following steps: separating the tobacco extract solution by 2-15 stages of membranes to obtain membrane separation trapped fluid of each stage and membrane separation permeate of the last stage; 2-15 stage membrane separation is carried out in sequence from large to small according to the membrane aperture, wherein the membrane aperture is one or two or three of microfiltration, ultrafiltration and nanofiltration;
the permeation liquid of the last stage of membrane separation is split into two-dimensional fractions with different ultraviolet absorption properties through two-dimensional column chromatography;
and performing sensory evaluation on the membrane separation trapped fluid and the two-dimensional flow at each stage, and determining a component capable of highlighting the sensory effect characteristics of the tobacco extract as a characteristic flavor group of the tobacco extract.
2. The method of claim 1, wherein the first dimension of the two-dimensional column chromatography is performed using sephadex and the second dimension of the two-dimensional column chromatography is performed using C18 reverse phase silica gel.
3. The method of claim 2, wherein during the first-dimension column chromatography separation, the first-dimension effluent is monitored for uv absorption signals, 2-8 trapping columns are used to trap one-dimension fractions with different uv absorption signals, respectively, the eluate from the trapping columns enters the second-dimension column chromatography, the uv absorption signals of the second-dimension effluent are monitored, and the two-dimension fractions with different uv absorption properties are collected.
4. The method of claim 3, wherein the UV absorbance signal is at a UV detection wavelength of 230nm and/or 280nm.
5. The method of claim 2, wherein the eluent used in the first dimension column chromatography and the second dimension column chromatography is water, ethanol, or aqueous ethanol.
6. The method of claim 5, wherein the second dimension column chromatography uses gradient elution with an eluent of 10-90% aqueous ethanol, the concentration of which gradually increases over time.
7. The method of claim 1, wherein said tobacco extract is selected from the group consisting of Yuyan extract, burley tobacco extract, and Virginia tobacco extract.
8. The method of preparing a tobacco extract flavor profile according to claim 1 or 7, wherein a 4-stage membrane separation is used, wherein the 4-stage membrane separation is sequentially a 50nm ceramic membrane, a 12nm ceramic membrane or a 50kDa roll-up organic membrane, a 5nm ceramic membrane or a 10kDa ceramic membrane, a 1kDa roll-up organic membrane.
9. The method of preparing a tobacco extract flavor profile of claim 1, wherein the concentration of the tobacco extract solution is between 10wt% and 20wt%.
10. The method of claim 1, wherein the sensory evaluation items comprise a plurality of the following items: aroma, richness, fineness, softness, mellow, miscellaneous gas, smoke concentration, strength, oral cavity stimulation, oral cavity residue, convergence, throat stimulation, throat dryness, nasal cavity stimulation, sweet taste, sour taste, bitter taste, cool taste, flue-cured tobacco fragrance, sun-cured tobacco fragrance, faint scent, fruit fragrance, spicy fragrance, costustoot, green essence fragrance, flower fragrance, herb fragrance, bean fragrance, cocoa fragrance, milk fragrance, paste fragrance, baking fragrance, tea fragrance and sweet fragrance.
11. The method of preparing a tobacco extract flavor panel of claim 1 or claim 10, wherein the flavor panel comprises at least one of the membrane separation retentate fractions and at least one of the two-dimensional fractions.
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| CN102445497A (en) * | 2010-10-15 | 2012-05-09 | 福建中烟工业有限责任公司 | Method for evaluating cigarette flavor compensation technology |
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| CN114532581A (en) * | 2022-03-10 | 2022-05-27 | 浙江中烟工业有限责任公司 | Preparation method and application of acidic flavor components with characteristics of Canadian tobacco smoke |
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| CN102445497A (en) * | 2010-10-15 | 2012-05-09 | 福建中烟工业有限责任公司 | Method for evaluating cigarette flavor compensation technology |
| CN106353419A (en) * | 2016-08-16 | 2017-01-25 | 国家烟草质量监督检验中心 | Method for measuring aroma components in main stream smoke of cigarettes |
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