Characteristic flavor group style strengthening product of smoked plum extract for cigarettes and preparation method of special flavor group style strengthening product

Abstract

The invention relates to a cigarette smoked plum extract characteristic flavor group style strengthening product and a preparation method thereof, and the preparation method comprises the following steps: carrying out multistage membrane separation and two-dimensional liquid chromatographic column separation on a smoked plum extract solution, and respectively collecting each stage of membrane separation intercepted liquid group and two-dimensional liquid chromatographic column separation group; carrying out sensory evaluation on the smoked plum extract, the membrane separation intercepted liquid group at each stage and the two-dimensional liquid chromatographic column separation group, and screening to obtain a flavor group; performing thermal cracking on the flavor group, and screening to obtain flavor substances; and mixing part or all of the flavor groups with part or all of the flavor substances to obtain the cigarette dark plum extract special flavor group style strengthening product. According to the method, the smoked plum extract is subjected to refined processing with the sensory effect as guidance, the smoked plum characteristic flavor group is obtained, flavor substances added to the smoked plum extract are subjected to style strengthening according to the release condition of thermal cracking aroma components of the smoked plum extract, and the smoked plum extract characteristic flavor group style strengthening product for the cigarettes is prepared.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of tobacco flavor, in particular to a tobacco Prunus mume extract characteristic flavor group style enhancement product and a preparation method thereof. BACKGROUND

[0002] Flavor is the basis of cigarette flavoring and the core element of cigarette product research and development. Natural flavor ingredients are complex in composition. On the one hand, the rich composition can give and enhance the flavor style of cigarettes, but on the other hand, due to the existence of some negative ingredients or the suboptimal proportion of characteristic ingredients, it often brings adverse effects to the sensory quality of cigarettes or causes inaccurate and inefficient flavoring and product design.

[0003] Prunus mume extract is one of the commonly used natural flavors in cigarette production, which can make the aroma of cigarettes more delicate and soft, reduce the stimulation, and increase the sweet and smooth feeling and comfortable aftertaste. However, the commercially available Prunus mume extract still has some deficiencies. For example, the characteristic flavors such as fragrance and sweetness are not prominent, and the wax and smoky flavors are slightly heavy, which reduces the freedom of use of Prunus mume extract and limits its use in cigarette flavor formulations.

[0004] Therefore, it is necessary to highlight the various functional characteristics of natural flavors while removing impurities, obtain Prunus mume characteristic flavor groups with multiple functional focuses, improve the functional focus of homologous natural flavors and product diversification, and provide more abundant and effective flavor materials for precise flavoring and digital product design. SUMMARY

[0005] To solve the above technical problems, the present application provides a tobacco Prunus mume extract characteristic flavor group style enhancement product and a preparation method thereof. The present application processes Prunus mume extract in a refined manner based on sensory effects, obtains Prunus mume characteristic flavor groups, and adds flavoring substances to the Prunus mume extract according to the release of thermal cracking aroma components to enhance the style, thereby preparing a tobacco Prunus mume extract characteristic flavor group style enhancement product.

[0006] To achieve this purpose, the present application adopts the following technical solutions:

[0007] In a first aspect, the present application provides a preparation method of a tobacco Prunus mume extract characteristic flavor group style enhancement product, which comprises the following steps:

[0008] (1) subjecting a solution of Prunus mume extract to multi-stage membrane separation and two-dimensional liquid chromatography column separation, and collecting the membrane separation intercept liquid groups and two-dimensional liquid chromatography column separation groups, respectively;

[0009] (2) subjecting the Prunus mume extract, the membrane separation intercept liquid groups and the two-dimensional liquid chromatography column separation groups in step (1) to sensory evaluation, and screening to obtain a flavor group;

[0010] (3) performing thermal cracking on the flavor group in step (2) to obtain flavor substances;

[0011] (4) mixing any one or a combination of at least two of the flavor groups, or any one or a combination of at least two of the flavor substances to obtain the style-enhanced product of the plum extract characteristic flavor group for cigarettes.

[0012] The present application can obtain a plurality of plum extract characteristic flavor groups with different sensory characteristics by the multi-stage membrane separation and two-dimensional column chromatography separation guided by the senses, and the interference of non-characteristic flavor components is excluded. The diversified functions of the plum extract for cigarettes are highlighted, the product categories of the plum extract are enriched, and the flexibility and precision of the use of cigarette flavoring spices are increased. The multi-stage membrane separation and two-dimensional column chromatography technology are combined and complementary, and the separation process almost does not involve thermal, chemical or biological changes, so that the natural characteristics of the natural spices are maintained. The dextran gel and the reversed-phase silica gel can be repeatedly used, and the efficient production of the two-dimensional column separation groups can be realized by means of the production-level automatic two-dimensional medium-pressure column chromatography equipment.

[0013] Although each group has outstanding style characteristics, there are also some disadvantages such as unbalanced sensory effect and poor richness. The natural spices for cigarettes can fully play their product flavor regulating role only after being burned. The thermal cracking-gas chromatography-mass spectrometry technology is to heat the sample to be tested in a strictly controlled environment, so that it is rapidly cracked into volatile small molecular substances, and the cracking products are directly sent to the gas chromatography-mass spectrometer for analysis. It can simulate the cigarette burning environment to a certain extent, and is suitable for analyzing the flavor substances which have a substantial impact on smoke after the spices are added to the cigarette.

[0014] The characteristic flavor group separation positioning, characteristic flavor substance analysis and screening, and diversified compounding application technology adopted in the present application obtain the style-enhanced product of the plum extract characteristic flavor group for cigarettes, and also provide a reference for the fine processing idea of other natural spices for cigarettes. While highlighting the style characteristics of natural spices, the uncontrollable factors and invalid components of natural spices are minimized, and the quality stability and controllability of the refined products of natural spices are increased, which has practical application value.

[0015] Preferably, the solvent in the solution of the plum extract in step (1) includes ethanol and / or water.

[0016] Preferably, the multi-stage membrane separation of step (1) comprises a combination of at least two of 40-60 nm (e.g., can be 40 nm, 45 nm, 50 nm, 55 nm, 60 nm, etc.) membrane separation, 10-30 nm (e.g., can be 10 nm, 15 nm, 20 nm, 25 nm, 30 nm, etc.) membrane separation, 4-6 nm (e.g., can be 4 nm, 4.5 nm, 5 nm, 5.5 nm, 6 nm, etc.) membrane separation, 1.5-3 nm (e.g., can be 1.5 nm, 2 nm, 2.5 nm, 3 nm, etc.) membrane separation, or 0.1-1 nm (e.g., can be 0.1 nm, 0.2 nm, 0.5 nm, 0.8 nm, 1 nm, etc.) membrane separation.

[0017] In the present application, microfiltration, ultrafiltration, nanofiltration membrane, reverse osmosis membrane are selected for multi-stage separation, and inorganic membranes or organic membranes with different pore sizes can be selected, and the principle of gradually reducing the membrane pore size is followed for step-by-step separation, the permeate of each membrane separation is used as the separation object of the next stage of membrane separation, and the retained liquid obtained by each separation is collected.

[0018] Preferably, the filler of the first-dimensional liquid chromatography column in the two-dimensional liquid chromatography column separation of step (1) comprises Sephadex, and the filler of the second-dimensional liquid chromatography column comprises C18 bonded silica gel.

[0019] Preferably, the detector used in the two-dimensional liquid chromatography column separation of step (1) is an ultraviolet detector.

[0020] Preferably, the detection wavelength of the ultraviolet detector is 200-330 nm (e.g., can be 200 nm, 220 nm, 250 nm, 280 nm, 300 nm, 330 nm, etc.).

[0021] Preferably, the collection of the two-dimensional liquid chromatography column separation group of step (1) comprises: dividing the one-dimensional flow fraction according to the signal of the detector after the first-dimensional liquid chromatography column, combining the flow fractions with similar detector signals, and separately performing the second-dimensional liquid chromatography column separation; and combining the two-dimensional flow fractions according to the signal of the detector after the second-dimensional liquid chromatography column to obtain the two-dimensional liquid chromatography column separation group.

[0022] Preferably, the sensory evaluation of step (2) comprises: preparing the Fructus Mume extract, the retained liquid of each stage of membrane separation, and the two-dimensional liquid chromatography column separation group into solutions with the same concentration, then injecting the solutions into cigarettes, and performing sensory evaluation on the cigarettes to screen the flavor group.

[0023] The present application prepares the same concentration solution of the prunus mume extract, each level of membrane separation intercept liquid and two-dimensional liquid chromatography column separation group, and adds it to the blank cigarette without flavoring at a suitable tobacco dosage. The sample cigarette is sealed and stored under constant temperature and humidity for 36-72h, and then the cigarette sensory evaluation is performed to screen multiple characteristic flavor groups with good sensory effect and focusing on different flavor characteristics.

[0024] Preferably, the screening criteria of step (2) is to select the flavor groups with aroma and fruit aroma better than the prunus mume extract raw material.

[0025] Preferably, the temperature of the thermal cracking in step (3) is 500-700℃ (for example, it can be 500℃, 550℃, 600℃, 650℃, 700℃, etc.), and the time is 0.1-1min (for example, it can be 0.1min, 0.2min, 0.5min, 1min, etc.).

[0026] Preferably, the screening criteria of step (3) is to select the thermal cracking product with any one or at least two of fruit aroma, sweet aroma, baking aroma or floral aroma in the food additive list or tobacco additive permitted list to obtain the flavor substances.

[0027] Preferably, the flavor substances in step (3) include furfural, 2-acetyl furan, 5-methyl furfural, benzyl alcohol, benzaldehyde, ethyl benzoate, malonic acid diethyl ester, succinic acid diethyl ester, ethyl tetradecanoate, ethyl laurate and ethyl palmitate.

[0028] Preferably, in step (4), the tobacco prunus mume extract characteristic flavor group style enhancement product includes 70-90 parts (for example, it can be 70 parts, 75 parts, 80 parts, 85 parts, 90 parts, etc.) of the flavor group and 10-30 parts (for example, it can be 10 parts, 15 parts, 20 parts, 25 parts, 30 parts, etc.) of the flavor substances in terms of dry matter mass fraction.

[0029] In the present application, the cigarette flavoring personnel can recompound the various prunus mume characteristic flavor groups and the characteristic flavor substances screened and analyzed according to the appropriate proportion of the tobacco leaf group formula, auxiliary material design parameters and style characteristic requirements to obtain the prunus mume flavor tobacco flavor series products.

[0030] In the second aspect, the present application provides a tobacco prunus mume extract characteristic flavor group style enhancement product prepared by the preparation method of the tobacco prunus mume extract characteristic flavor group style enhancement product according to the first aspect.

[0031] Compared with the prior art, the present application has at least the following beneficial effects:

[0032] The application removes the interference of non-characteristic flavor components, effectively separates and enriches the characteristic flavor groups, enriches the product categories of natural plum flavor, and increases the flexibility of cigarette flavoring. Meanwhile, the characteristic flavor substances which have substantial impact on smoke after being added to cigarettes are obtained by thermal cracking, the characteristic flavor groups and the characteristic flavor substances are compounded, and the plum extract characteristic flavor group style enhancement product with high sensory evaluation is obtained. BRIEF DESCRIPTION OF DRAWINGS

[0033] Figure 1 is a one-dimensional column chromatogram in Example 1.

[0034] Figure 2 is a two-dimensional column A chromatogram in Example 1.

[0035] Figure 3 is a two-dimensional column B chromatogram in Example 1.

[0036] Figure 4 is a two-dimensional column C chromatogram in Example 1.

[0037] Figure 5 is a two-dimensional column D chromatogram in Example 1. DETAILED DESCRIPTION

[0038] The technical solutions of the application will be further described below in combination with the drawings and through specific embodiments. However, the following examples are only simple examples of the application, and do not represent or limit the protection scope of the application, and the protection scope of the application is subject to the claims.

[0039] Example 1

[0040] The embodiment provides a preparation method of a plum extract characteristic flavor group style enhancement product for cigarettes, which comprises the following steps:

[0041] (1) Take the plum extract developed and produced by Guangxi China Tobacco Industry Co., Ltd., and measure the optimal solubility in 80% ethanol according to the method of YC / T145.4-1998. Dilute the plum extract with 80% ethanol to a solution with a mass fraction of 8%, centrifuge to remove a small amount of insoluble matter, and take the supernatant for membrane separation operation. Use 50 nm, 5 nm and 2 nm ceramic membranes in sequence for separation, and use the permeate of each membrane separation as the separation object of the next membrane. The process parameters and interception ratio (the ratio of the mass of the interception liquid in each process section to the feed) of each membrane separation are shown in Table 1, and the interception liquid obtained by each separation is collected. Use reverse osmosis (RO) membrane to concentrate the 2 nm membrane permeate, and collect the RO membrane interception liquid.

[0042] Table 1

[0043] Separation process section Pre-membrane pressure / bar Post-membrane pressure / bar Pump frequency / Hz membrane flux / [L / (h·m 2 )]]]> Retention ratio / % 50 nm 2.0 0.2 40 133.6 16.5 5 nm 3.5 2.6 45 52.9 9.5 2 nm 3.5 2.5 45 40.3 10.0 RO 15.3 14.8 45 2.19 35.0

[0044] (2) The RO membrane retentate of the plum extract was separated using a preparative-grade fully automated two-dimensional column chromatography system. This system consists of one one-dimensional separation column, followed by four collection columns, and then two two-dimensional separation columns. The system has a maximum pressure resistance of 5 MPa and a maximum working flow rate of 50 mL / min. UV detectors are connected after both the one-dimensional and two two-dimensional columns, and an automatic fraction collector is also located after the two-dimensional columns.

[0045] In this embodiment, the one-dimensional column chromatography size was 50 mm × 400 mm, the packing material was dextran gel, the eluent was 20% ethanol, the flow rate was 8 mL / min, the elution time was 200 min, and the UV detection wavelengths were 230 nm and 280 nm. Based on the UV absorption signal (see attached...) Figure 1 The eluents from the one-dimensional column chromatography separation at time points of 0–40 min, 40–50 min, 50–74 min, and 74–200 min were introduced into four trapping columns, each 26 mm × 200 mm in size and packed with C18 bonded silica gel. During the trapping process, the eluent from the trapping columns was collected. After trapping, the trapping columns were eluted with a gradient of ethanol from 20% to 95% (ethanol volume percentage increased uniformly by 0.8% per minute until the ethanol volume fraction reached 95%, which was then maintained until the two-dimensional separation was complete). The eluents were then introduced into second-dimensional column chromatography for further separation. The second-dimensional column was 20 mm × 460 mm in size and packed with C18 bonded silica gel. The two-dimensional separation time was 100 min, and the UV detection wavelengths were 230 nm and 280 nm, respectively. The results were based on the UV absorption signals from the second-dimensional column chromatography (see attached image). Figures 2-5 The elution fractions with similar absorption peaks were merged. In addition, considering the actual production application, the continuous fractions with lower yields were also merged, resulting in a total of 9 groups (A1, A2, B1, B2, C1, C2, D1, D2, D3). Together with the effluents from the 4 collection columns (T1 to T4), a total of 13 groups were obtained.

[0046] (3) The dry matter content of the plum extract and each isolated group was determined by freeze-drying. Each isolated group was prepared into solutions of the same concentration and numbered. Using an automatic flavoring injector, each group solution was added to a reference cigarette at a dry matter content of 30 μg / g tobacco. The solutions were then sealed and stored for at least 48 hours at a temperature of (22±1)℃ and a relative humidity of 60%±2%. Sensory evaluation of the sample cigarettes after flavoring injection of the separated plum extract groups was conducted according to YC / T 497—2014 "Sensory Evaluation Method for Chinese-style Cigarettes" (considering production costs, groups with excessively low yields, A2, B2, C2, D2, D3, T1, and T2, were not evaluated).

[0047] The sensory evaluation results (Table 2) show that the sensory effects of the groups obtained by membrane separation and column chromatography separation of Fructus Mume extract are quite different, and the good and poor groups are obviously distinguished. The 50 nm cut-off group retains the overall characteristics of the flavor before separation, and has better effects in improving the cigarette aroma and fruit aroma, and masking the offensive odor; the RO membrane cut-off group has better overall effect than the flavor before separation, and the smoke state, comfort and characteristic aroma are obviously improved, especially in improving the smoke fruit aroma and sweet aroma; the group B1 obtained by two-dimensional column chromatography separation has significant effects in increasing the smoke sweetness and fruit aroma, and the smoke state and comfort are also good. The other groups all show different degrees of increasing the irritation, residual feeling and convergence (such as the 2 nm cut-off group, the A1 group, the C1 group, the D1 group and the T3 group), reducing the aroma of the reference cigarette, and increasing the offensive odor (such as the D1 group, the T3 group and the T4 group).

[0048] Therefore, the 50 nm cut-off group, the RO membrane cut-off group and the column chromatography B1 group of Fructus Mume extract membrane separation are used as the characteristic flavor groups of Fructus Mume.

[0049] Table 2

[0050] Note: The scores of "smoke concentration", "throat irritation" and "nasal cavity irritation" of each evaluation cigarette are all 6.0, the score of "strength" is 5.5, and the score of "freshness" is 1.5, the scores of "spicy aroma", "woody aroma" and "green aroma" are all 1.0, the score of "roasted aroma" is 2.5, and the scores of "cooling taste", "sun-cured tobacco aroma", "floral aroma", "herbal aroma", "bean aroma", "cocoa aroma", "milk aroma" and "cream aroma" are all 0.

[0051] (4) The three characteristic flavor groups were respectively subjected to thermal cracking-gas chromatography-mass spectrometry analysis. NIST20 library was used for qualitative analysis, the samples with matching degree higher than 80% were determined, the peak area normalization method was used for semi-quantitative analysis, each sample was determined twice and the average value was taken.

[0052] Cracking conditions: EGA / PY-3030D cracking instrument (FRONTIER LAB, Japan); cracking temperature: 600℃; cracking time: 0.2 min; connecting port temperature: 280℃; sample addition amount: 1 μL.

[0053] GC-MS conditions: 7890A-5975C gas chromatography-mass spectrometry (Agilent, USA); chromatographic column: DB-5MS capillary column (30 m x 0.25 mm x 0.25 μm); carrier gas: He; flow rate: 1.0 mL / min; split ratio: 50:1; programmed temperature: 40℃ for 3 min, increased to 240℃ at a rate of 10℃ / min, and then increased to 280℃ at a rate of 20℃ / min, and maintained for 15 min; GC-MS transfer line temperature: 280℃, ionization mode: EI; ion source temperature: 230℃; quadrupole temperature: 150℃; ionization energy: 70 eV; solvent delay time: 4.5 min; mass scan range 29-450 a.m.u.

[0054] The pyrolysis products and aroma performance of the three characteristic flavor groups are shown in Table 3, and a total of 55 pyrolysis products were detected. From the structure of the compounds, the proportion of esters, heterocyclic compounds, and phenolic compounds is high, in addition to cyclopentenone, aromatic hydrocarbons, acids, alcohols, aldehydes, etc. The aroma types of the pyrolysis products are mainly fruity, sweet, smoked, caramel, nutty, and wax, etc. Some of the above ingredients are also inherent aroma components of tobacco, and therefore, the plum extract applied to cigarette flavoring can coordinate with tobacco aroma and enrich the aroma, especially increase the fruity aroma.

[0055] Table 3

[0056]

[0057]

[0058]

[0059] Note: The aroma characteristics refer to the website information of http: / / perflavory.com / and https: / / www.chembk.com / cn; “—” indicates no aroma characteristics reported; “ / ” indicates not detected.

[0060] (5) This example comprehensively considers the advantages and disadvantages of the sensory characteristics of the plum characteristic flavor group, selects substances that can be used as synthetic flavoring agents for tobacco from the thermal cracking characteristic flavor substances, and obtains a compounding scheme (see Table 4 for details).

[0061] Table 4

[0062]

[0063]

[0064] Example 2

[0065] The present example provides a preparation method of a tobacco plum extract characteristic flavor group style strengthening product, comprising the following steps:

[0066] (1) Using a certain commercially available Fructus Mume extract as raw material, its solubility in 60% ethanol was determined to be optimal according to the method of YC / T 145.4-1998. The Fructus Mume extract was diluted with 60% ethanol to a solution with a mass fraction of 7%, and the insoluble matter was removed by centrifugation using an industrial high-speed tubular centrifuge (rotating speed 16000 rpm). The clear liquid was collected for multi-stage membrane separation production. 50 nm, 2 nm, and reverse osmosis membranes were used in sequence.

[0067] In this example, a full-automatic continuous multi-stage membrane separation platform was used for multi-stage membrane separation production of Fructus Mume extract. The platform consisted of five membrane separation machine groups, namely inorganic ultrafiltration machine group, organic ultrafiltration machine group, inorganic nanofiltration machine group, organic nanofiltration machine group, and reverse osmosis machine group. The outlet pipeline of the inorganic ultrafiltration machine group was connected to the upper inlet of the inorganic nanofiltration machine group by flange interface and food-grade PP hose, and the outlet pipeline of the inorganic nanofiltration machine group was connected to the inlet of the reverse osmosis machine group, realizing the connection and simultaneous use of the three machine groups. When the inorganic ultrafiltration machine group was used for 50 nm membrane separation process, the permeate directly flowed into the inorganic nanofiltration machine group. When the amount of 50 nm permeate in the inorganic nanofiltration machine group exceeded the minimum circulating volume of the equipment, the inorganic nanofiltration machine group was started, and the 2 nm membrane separation process was started at the same time. Similarly, when the amount of 2 nm permeate in the reverse osmosis machine group exceeded the minimum circulating volume of the equipment, the reverse osmosis machine group was started, and the three machine groups worked simultaneously. The process parameters of the three-stage membrane separation process are shown in Table 5, and the mass, refractive index, relative density, and yield of each membrane separation group are shown in Table 6.

[0068] Table 5

[0069]

[0070] Table 6

[0071]

[0072] (2) The RO membrane retention group of Fructus Mume extract was further separated using a production-level full-automatic two-dimensional column chromatography separation platform. The one-dimensional column of the equipment was 30×60 cm, followed by four trapping columns of 20×20 cm, and then four two-dimensional separation columns of 20×40 cm. The system had a maximum pressure resistance of 2 MPa and a maximum working flow rate of 2 L / min. UV detectors were connected after the one-dimensional column and the four two-dimensional columns, and an automatic fraction collector was also connected after the two-dimensional columns.

[0073] The one-dimensional filler was dextran gel, the loading volume was 2000 mL (1860 g), the eluent was 10% ethanol, the flow rate was 200 mL / min, and the UV detection wavelengths were 230 nm and 270 nm, respectively. The effluent of the one-dimensional column chromatography in the time periods of 0-54 min, 54-83 min, and 83-200 min was introduced into the first three trapping columns, respectively, and the trapping column filler was reversed-phase silica gel. The effluent of the trapping column was collected during the trapping process. After the trapping was completed, the trapping column was eluted with a gradient of ethanol with a volume fraction of 10% to 95% (the volume fraction of ethanol increased at a uniform speed of 0.8% per minute, and the volume fraction of ethanol was kept at 95% until the end of two-dimensional separation), and the eluent was introduced into the second-dimensional column chromatography for separation; the second-dimensional column chromatography filler was reversed-phase silica gel, the two-dimensional separation time was 200 min, and the UV detection wavelengths were 230 nm and 270 nm, respectively. According to the UV absorption signal of the second-dimensional column chromatography, the elution fractions corresponding to the similar absorption peaks were combined, and the continuous fractions with low yield were also combined by considering the actual production and application, and a total of 9 groups (A1, A2, B1, B2, C1, C2, T1, T2, and T3) were obtained.

[0074] (3) The dry matter content of the plum extract and the separated groups was determined. The separated groups were configured into solutions with the same concentration and numbered, and the solutions of the groups were added to reference cigarettes by using an automatic flavor injection instrument at a dosage of 30 μg / g of tobacco. The reference cigarettes were stored in a sealed environment at a temperature of (22±1) ℃ and a relative humidity of 60%±2% for 48 h or more. The sample cigarettes after the plum extract and the separated groups were flavored were subjected to sensory evaluation according to YC / T 497-2014 “Sensory evaluation method for Chinese cigarettes” (some groups with low yield were not evaluated considering the production cost).

[0075] The sensory evaluation results (Table 7) show that the 50 nm cutoff group of membrane separation, the RO membrane cutoff group, and the column chromatography A1 and B1 groups can be used as the characteristic flavor groups of plum.

[0076] Table 7

[0077]

[0078]

[0079] Note: The scores of the indicators of “cool taste”, “sun-cured tobacco aroma”, “floral aroma”, “herbal aroma”, “bean aroma”, “cocoa aroma”, “milk aroma”, and “cream aroma” of each evaluation cigarette are 0.

[0080] (4) The four characteristic flavor groups were subjected to pyrolysis-gas chromatography-mass spectrometry analysis, and the specific experimental conditions were the same as those in Example 1. The pyrolysis products and aroma performance of the four characteristic flavor groups are shown in Table 8, and a total of 59 pyrolysis products were detected.

[0081] Table 8

[0082]

[0083]

[0084] Note: The aroma characteristics refer to the information from the websites of http: / / perflavory.com / and https: / / www.chembk.com / cn; “—” means no aroma characteristics reported; “ / ” means not detected.

[0085] (5) Application of the complex of characteristic flavor group and characteristic flavor substances: considering the advantages and disadvantages of the sensory characteristics of the characteristic flavor group of Fructus Mume, the compounds that can be used as tobacco flavor were selected from the characteristic flavor substances of thermal cracking, and the complex was prepared according to the scheme in Table 9.

[0086] Table 9

[0087]

[0088]

[0089] Comparative Example 1

[0090] The present comparative example provides a preparation method of a tobacco Fructus Mume extract characteristic flavor group style strengthening product, steps (1)-(4) refer to Example 1, and the complexing scheme provided in step (5) only contains the 50 nm cut-off group, the RO cut-off group and the column chromatography B1 group, and the component allocation ratio refers to Example 1.

[0091] Test Example

[0092] The complexing products provided by Comparative Example 1 and Examples 1-2, and the Fructus Mume extract used in Examples 1-2 were configured into solutions with the same concentration, and the solutions were added to reference cigarettes by an automatic flavoring injection instrument with a dosage of 30 μg / g of dry matter of tobacco shred. The sample cigarettes after flavoring injection were stored in an environment with a temperature of (22±1) ℃ and a relative humidity of 60%±2% for 48 h or more. The sample cigarettes after flavoring injection were subjected to sensory evaluation according to YC / T 497—2014 “Sensory evaluation method for Chinese-style cigarettes”. The change values of each evaluation index compared with the reference cigarettes are shown in Table 10.

[0093] Table 10

[0094]

[0095]

[0096] It can be seen from the test results that the characteristic flavor groups of Fructus Mume are located through the sensory-guided multi-stage membrane combined two-dimensional column separation, and the endogenous characteristic substances are screened through the thermal cracking analysis, and the effect of the Fructus Mume extract refined product is significantly improved by the optimized compounding scheme, and the sensory evaluation effect of the product is better than any characteristic flavor group and better than the original flavor. The compounding product of example 1 can significantly improve the fruit aroma, sweet aroma, aroma, richness, fine soft and round feeling of the cigarette compared with the original extract, and can increase the sweetness, mask the odor, reduce the stimulation and convergence feeling to a certain extent, and the smoke state, comfort and characteristic aroma are improved. The compounding product of example 2 has more obvious advantages in improving the cigarette aroma, richness, sweetness, fruit aroma, sweet aroma and baking aroma compared with the original extract, and can also improve the comfort of the cigarette, reduce the stimulation, dryness and convergence feeling, and is coordinated with the tobacco aroma.

[0097] It can be seen from the comparison of the sensory evaluation of the compounding product of example 1 and the compounding product of comparative example 1 that when only the characteristic flavor group is contained in the formula and the flavor substances obtained by thermal cracking are lacking, the sensory effect is decreased.

[0098] The applicant declares that the above is only a specific embodiment of the present application, but the protection scope of the present application is not limited thereto, and those skilled in the art should understand that any changes or replacements within the technical scope disclosed by the present application can be easily thought by any person skilled in the art in the technical field, and all fall within the protection scope and disclosure scope of the present application.

Claims

1. A method for preparing a product with enhanced flavor profiles from dried plum extract for tobacco, characterized in that, The preparation method includes the following steps: (1) The solution of dried plum extract was subjected to multi-stage membrane separation and two-dimensional liquid chromatography column separation, and the throttling liquid groups of each stage of membrane separation and the two-dimensional liquid chromatography column separation groups were collected respectively; (2) Sensory evaluation was conducted on the plum extract, the membrane separation interception liquid group and the two-dimensional liquid chromatography column separation group in step (1) to screen out the flavor group; (3) The flavor groups in step (2) are subjected to thermal decomposition and the flavor substances are screened to obtain flavor substances; (4) Mix any one or at least two of the flavor groups and any one or at least two of the flavor substances to obtain the flavor group-enhanced product of the tobacco plum extract.

2. The preparation method according to claim 1, characterized in that, The solvent in the solution of the plum extract in step (1) includes ethanol and / or water.

3. The preparation method according to claim 1 or 2, characterized in that, The multi-stage membrane separation in step (1) includes a combination of at least two of the following: 40-60nm membrane separation, 10-30nm membrane separation, 4-6nm membrane separation, 1.5-3nm membrane separation, or 0.1-1nm membrane separation.

4. The preparation method according to any one of claims 1-3, characterized in that, In step (1), the packing material of the first-dimensional liquid chromatography column in the two-dimensional liquid chromatography column separation includes dextran gel, and the packing material of the second-dimensional liquid chromatography column includes C18 bonded silica gel.

5. The preparation method according to any one of claims 1-4, characterized in that, The detector used for separation in step (1) of the two-dimensional liquid chromatography column is an ultraviolet detector; Preferably, the detection wavelength of the ultraviolet detector is 200-330nm.

6. The preparation method according to any one of claims 1-5, characterized in that, The collection of the two-dimensional liquid chromatography column separation group in step (1) includes: dividing the one-dimensional flow based on the signal of the detector after the first-dimensional liquid chromatography column, merging the flow with similar detector signals, and performing second-dimensional liquid chromatography column separation respectively; merging the two-dimensional flow based on the signal of the detector after the second-dimensional liquid chromatography column to obtain the two-dimensional liquid chromatography column separation group.

7. The preparation method according to any one of claims 1-6, characterized in that, The sensory evaluation in step (2) includes: preparing the plum extract, the membrane separation intercepting liquid at each stage and the two-dimensional liquid chromatography column separation group into solutions of the same concentration, then injecting them into cigarettes, performing sensory evaluation on the cigarettes, and screening to obtain flavor groups; Preferably, the screening criteria in step (2) are: selecting the flavor groups by membrane separation thresholds and two-dimensional liquid chromatography column separation groups that have aroma and fruitiness exceeding those of the raw material of dried plum extract.

8. The preparation method according to any one of claims 1-7, characterized in that, The thermal decomposition in step (3) is carried out at a temperature of 500-700℃ for 0.1-1 min. Preferably, the screening criteria in step (3) are: selecting pyrolysis products that have any one or at least two of the aroma characteristics of fruity aroma, sweet aroma, baking aroma or floral aroma from the list of food additives or the list of permitted tobacco additives to obtain flavor substances; Preferably, the flavoring substance in step (3) includes furfural, 2-acetylfuran, 5-methylfurfural, benzyl alcohol, benzaldehyde, ethyl benzoate, diethyl malonate, diethyl succinate, ethyl tetradecanoate, ethyl laurate, and ethyl palmitate.

9. The preparation method according to any one of claims 1-8, characterized in that, Step (4): Based on dry matter mass parts, the flavor group enhancement product of the tobacco plum extract includes 70-90 parts of flavor group and 10-30 parts of flavor substance.

10. A product with enhanced flavor profile of tobacco plum extract prepared by the method described in any one of claims 1-9.

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