Method for identifying and screening characteristic aroma components of cherry extract for cigarettes and method for monitoring aroma quality

Abstract

The invention discloses a cigarette cherry extract characteristic aroma component identification and screening method and an aroma quality monitoring method, and the method comprises the following steps: collecting cigarette cherry extract samples at a preset storage time point, obtaining volatile aroma component information through a GC-IMS detection method, and determining the aroma quality of the cigarette cherry extract according to the types of volatile components and the relative content of the volatile components. The method comprises the following steps: calculating the ROAV value of each volatile component in combination with a sensory threshold, screening out the volatile component types with the ROAV values greater than 1, obtaining the characteristic aroma components of the cherry extract for the cigarettes, and establishing a characteristic aroma fingerprint spectrum of the characteristic aroma components of the cherry extract for the cigarettes by applying analysis software Vocal according to the chromatographic retention time, the ion migration time and the ion strength, thereby obtaining the characteristic aroma fingerprint spectrum of the characteristic aroma components of the cherry extract for the cigarettes. Therefore, a dynamic tracking model of fragrance quality change is formed. The GC-IMS detection method without pretreatment is adopted, more real component information can be reserved, the detection process is rapid and convenient, direct sample injection can be achieved, and the problem of inaccurate detection data caused by complex pretreatment is solved.

Description

Technical Field

[0001] This patent belongs to the technical field of tobacco flavors, and specifically relates to a method for identifying and screening characteristic aroma components of cherry extracts for tobacco and a method for monitoring aroma quality. Background Art

[0002] Cherry extract for tobacco is an important tobacco flavoring, and its aroma quality significantly impacts the style and quality of cigarette products. Typically a dark reddish-brown liquid or paste, it is prepared by crushing cherry fruits, extracting them with a certain concentration of ethanol, and concentrating them. Cherry extract for tobacco imparts a sweet, fruity aroma to tobacco smoke, neutralizing the spiciness of tobacco leaves and enhancing the depth of aroma. It is widely used in the production of tobacco flavors.

[0003] Cherry extract for tobacco has a complex chemical composition. During storage, it is affected by environmental factors such as temperature, humidity, light, and oxygen, which can cause changes in its chemical composition, leading to a decline in aroma quality and affecting its effectiveness in cigarettes. Currently, tobacco flavor and fragrance quality testing methods primarily rely on two main categories: physical and chemical indicators (relative density, refractive index, and acid value) and sensory indicators (appearance and aroma), as determined by the industry standard YC / T164-2012. Aroma is the most important factor affecting the quality of flavor and fragrance products. Sensory evaluation alone is susceptible to human subjectivity, so the introduction of instrumental analysis techniques can more objectively monitor aroma quality. Traditional aroma quality testing, which often relies on GC-MS, requires complex pretreatment and often uses organic solvents for extraction. This process can lead to the loss or degradation of volatile organic compounds (VOCs). Each test takes a long time, and the data is often numerical, failing to quickly and intuitively reflect overall aroma trends. Summary of the Invention

[0004] The purpose of this patent is to provide a method for identifying and screening the characteristic aroma components of cherry extract for tobacco use and a method for monitoring the aroma quality, so as to avoid the losses caused by pre-treatment of the detection method and shorten the detection time.

[0005] In order to solve the above technical problems, this patent adopts the following technical solutions:

[0006] A method for identifying and screening characteristic aroma components of a tobacco cherry extract comprises the following steps:

[0007] Step A: Collecting a sample of the tobacco cherry extract at a predetermined storage time point, and obtaining volatile aroma component information by GC-IMS detection method, wherein the volatile aroma component information includes the type of volatile components and the relative content of the volatile components;

[0008] Step B: Calculate the ROAV value of each volatile component based on the type and relative content of the volatile component and the sensory threshold. The ROAV value calculation formula is as follows:

[0009]

[0010] Wherein, Ci is the relative content of the i-th volatile component (%); Ti is the sensory threshold of the i-th volatile component (μg / kg); Cmax is the relative content of the volatile component that contributes most to the overall flavor (%); Tmax is the sensory threshold of the volatile component that contributes most to the overall flavor (μg / kg);

[0011] Step D: Screening out volatile components with ROAV values ​​greater than 1 to obtain characteristic aroma components of the tobacco cherry extract.

[0012] Furthermore, in step A, GC-IMS detection uses headspace sampling.

[0013] The incubation temperature of headspace injection is 50-70°C, the incubation time is 3-8 min, the incubation speed is 400-600 r / min, the injection needle temperature is 80-90°C, and the injection volume is 90-105 μL.

[0014] Furthermore, GC-IMS detection used a MXT-5 column, a column temperature of 60 °C, an analysis time of 30 min, a carrier gas of N2, an IMS temperature of 45 °C, a drift gas flow rate of 150 mL / min, and an initial carrier gas flow rate of 2 mL / min maintained for 30 min.

[0015] Furthermore, the characteristic aroma components of the cherry extract for smoking in step D include ethyl acetate, benzaldehyde, isobutyl butyrate, 2-methyl-3-methylthiofuran, 3-methyl-2-butenal, methyl butyrate, 2-ethylfuran, 2,5-dimethylfuran, isopentanol, 2,3-pentanedione, valeraldehyde, hydroxyacetone, isobutyl formate, 3-methyl-2-butanol, 2-methylvaleraldehyde, butyric acid, butyl acetate, acetaldehyde propylene glycol acetal, isopentyl formate and propyl butyrate.

[0016] This patent further provides a method for monitoring the aroma quality of cherry extract for tobacco during storage based on any one of the above-mentioned methods for identifying and screening characteristic aroma components of cherry extract for tobacco.

[0017] Furthermore, a method for monitoring the aroma quality of cherry extract for tobacco during storage comprises the following steps:

[0018] Step A: Collecting a sample of the tobacco cherry extract at a predetermined storage time point, and obtaining volatile aroma component information by GC-IMS detection. The volatile aroma component information includes the type of volatile component, the relative content of the volatile component, the chromatographic retention time, the ion migration time, and the ion strength;

[0019] Step B: Calculate the ROAV value of each volatile component based on the type and relative content of the volatile component and the sensory threshold. The ROAV value calculation formula is as follows:

[0020]

[0021] Wherein, Ci is the relative content of the i-th volatile component (%); Ti is the sensory threshold of the i-th volatile component (μg / kg); Cmax is the relative content of the volatile component that contributes most to the overall flavor (%); Tmax is the sensory threshold of the volatile component that contributes most to the overall flavor (μg / kg);

[0022] Step D: Screening out volatile components with ROAV values ​​greater than 1 to obtain characteristic aroma components of the tobacco cherry extract;

[0023] Step E: Using the analysis software Vocal, a characteristic aroma fingerprint of the characteristic aroma components of the tobacco cherry extract is established based on the chromatographic retention time, ion migration time, and ion intensity, thereby forming a dynamic tracking model for aroma quality changes.

[0024] Further, step E comprises the following steps:

[0025] Step E1: Use the built-in Reporter of the analysis software Vocal to draw an intuitive two-dimensional spectrum of the aroma components of the smoking cherry extract based on the chromatographic retention time, ion migration time and ion intensity;

[0026] Step E2: Based on the two-dimensional map information, the Gallery Plot plug-in built into the analysis software Vocal and the IMS database are used to establish an aroma fingerprint of the smoking cherry extract;

[0027] Step E3: Retain the data of ethyl acetate, benzaldehyde, isobutyl butyrate, 2-methyl-3-methylthiofuran, 3-methyl-2-butenal, methyl butyrate, 2-ethylfuran, 2,5-dimethylfuran, isopentanol, 2,3-pentanedione, valeraldehyde, hydroxyacetone, isobutyl formate, 3-methyl-2-butanol, 2-methylvaleraldehyde, butyric acid, butyl acetate, acetaldehyde propylene glycol acetal, isopentyl formate and propyl butyrate on the aroma fingerprint to obtain the characteristic aroma fingerprint of the characteristic aroma components of the tobacco cherry extract.

[0028] Furthermore, step E further includes the following steps:

[0029] Step E4: The Gallery Plot plug-in built into the analysis software Vocal is used to quickly calculate the similarity between the tested sample and the standard sample of the tobacco cherry extract, thereby determining whether the aroma quality of the tobacco cherry extract sample is qualified.

[0030] Furthermore, in step E4, the similarity threshold between the tested sample and the standard sample is set to at least 90%, thereby judging that the aroma quality of the tobacco cherry extract sample is qualified.

[0031] Furthermore, in step A, the preset storage time point is the 0th day of the storage period and the cherry extract samples for tobacco are collected every 10 to 15 days starting from the 0th day of the storage period.

[0032] This patent provides a method for identifying and screening characteristic aroma components of cherry extract for tobacco use and a method for monitoring aroma quality. It adopts a GC-IMS detection method that does not require pretreatment, which can retain more real component information. The detection process is fast and convenient, and direct sampling can be performed to avoid inaccurate detection data caused by complex pretreatment.

[0033] This patent can select characteristic aroma components from multiple different varieties or batches of cherry extracts for tobacco use and monitor them. Based on the test results, the aroma quality change trend of cherry extracts for tobacco use can be monitored, and whether the aroma quality of the test sample is qualified can also be directly determined on the software. BRIEF DESCRIPTION OF THE DRAWINGS

[0034] The above content of this patent and the following specific embodiments will be better understood when read in conjunction with the accompanying drawings. It should be noted that the drawings are only examples of the technical solutions claimed.

[0035] Figure 1 This is the GC-IMS characteristic fingerprint of the cherry extract for smoking in this patent (gas chromatography retention time (ordinate, unit is s), ion migration time (abscissa, unit is ms));

[0036] Figure 2 This is the characteristic aroma fingerprint of the cherry extract for tobacco in this patent;

[0037] Figure 3 This is a model diagram for dynamically tracking the aroma quality changes of the cherry extract for tobacco in this patent (graphic data 98 ​​is the similarity between the test sample 1 and the standard sample; graphical data 95 is the similarity between the test sample 2 and the standard sample);

[0038] Figure 4 This is a model diagram for dynamically tracking the aroma quality changes of the cherry extract for tobacco in Example 1;

[0039] Figure 5 This is a model diagram for dynamically tracking aroma quality changes of cherry extract for tobacco in Example 2;

[0040] Figure 6 This is a model diagram for dynamically tracking the aroma quality changes of the cherry extract for tobacco in Example 3. DETAILED DESCRIPTION

[0041] The detailed features and advantages of this patent are described in detail below in the specific implementation method. The content is sufficient to enable any technical personnel in this field to understand the technical content of this patent and implement it accordingly. Based on the description, claims and drawings disclosed in this specification, technical personnel in this field can easily understand the relevant purposes and advantages of this patent.

[0042] In this specification and claims, reference will be made to various terms which, unless otherwise indicated, shall be defined to have the following meanings:

[0043] The terms "include" or "have" have the same meaning as "contain", and also include other forms of the term, such as the gerund form and the singular form in English, meaning including but not limited to, and are not intended to exclude, for example, other elements, components, integers or steps.

[0044] All numbers used to express amounts of ingredients, properties (e.g., weight average molecular weight), reaction conditions, and the like should be considered to be modified in all instances by the term "within the inevitable error range" or "about." Therefore, the numerical values ​​set forth herein are approximate and may vary depending on the desired properties sought to be obtained by the present invention. At the very least, and not intended to limit the scope of the claims, the doctrine of equivalents should be applied, for example, each numerical value should at least be construed in light of the number of reported significant digits and by applying ordinary rounding techniques.

[0045] All other terms used herein that are not specifically defined in this patent are intended to have the general meanings understood by ordinary technicians in the field to which they belong, and in particular, ordinary technicians in the field can directly and unambiguously determine the meaning of how to implement the technical solution of this patent after reading the claims, description and drawings of this patent.

[0046] Even if there are incomplete descriptions, omissions or ambiguities in the grammar, text, punctuation, graphics, symbols, etc. in the claims, description and drawings of this patent, ordinary technicians in this field can still reach the only correct understanding by reading the claims, description and drawings as a whole without excessive reasoning or experimentation, and effectively exclude various incorrect understandings that are not aimed at achieving the purpose of this patent.

[0047] Ordinary technical personnel in the relevant field will give priority to reading the patent claims, specifications and drawings to reasonably interpret the terms; secondly, they will choose to refer to the relevant definitions in other documents published by the applicant before the application date to reasonably interpret the terms; thirdly, they will choose to reasonably interpret the terms by referring to the references cited in this patent; finally, they will choose to reasonably interpret the terms by combining the technical dictionaries, technical manuals, reference books, textbooks, national or industry technical standards, etc. commonly used by technical personnel in the relevant technical field.

[0048] The entire contents of all references cited in this application are incorporated into this specification by reference to the extent that they are not inconsistent with the contents disclosed in this application. It is obvious to those skilled in the art that products (devices, components, equipment, compounds, compositions, materials, etc.) and methods (processes, steps, conditions, parameters, equipment and test methods, equipment, etc.) other than those specifically described in this specification can be applied to the implementation of the invention fully disclosed in this specification without resorting to excessive experimentation. This patent intends to cover all functional equivalents known in the art of the methods, devices, equipment components, materials, processes and techniques specifically described in this specification.

[0049] In addition, throughout this specification, references are made to various publications. To more fully describe the state of the art in the field to which the presently disclosed subject matter pertains, the disclosures of these publications are incorporated herein by reference in their entirety. To the extent that the content of a published document is contained in a statement citing such document, the published document is also individually and specifically incorporated herein by reference.

[0050] The various components used in this patent can be prepared by various known methods that are well disclosed in the chemical literature.

[0051] Before disclosing and describing the materials, compounds, compositions, articles, devices and methods of the present invention, it should be understood that the following aspects are not limited to specific synthetic methods or specific reagents, as these can, of course, vary. It should also be understood that the terminology used herein is for the purpose of describing specific aspects only and is not intended to be limiting.

[0052] This patent provides a method for identifying and screening characteristic aroma components of cherry extract for tobacco use and a method for monitoring aroma quality, which includes the following steps:

[0053] S1. Sample preparation

[0054] The cherry extract sample for tobacco use was prepared according to the method described in Chinese patent document CN102952634B, which includes the following steps:

[0055] (1) After cleaning commercial cherries, crush them in a crusher for 5 minutes to obtain cherry pulp;

[0056] (2) Extracting the cherry pulp with 90% ethanol under reflux: Add 5 times the total weight of 90% ethanol to the cherry pulp, extract under reflux at 92±2°C for 2.5 hours, filter while hot, and use the residue in the next step. Keep the extraction filtrate A for later use.

[0057] (3) The filter residue of step (2) was reflux-extracted with 30% ethanol: 6 times the total weight of 30% ethanol was added to the filter residue; reflux-extraction was performed twice at a temperature of 95±2°C, the first time for 1.5 hours and the second time for 1 hour; the two extracts were combined and the combined extract was concentrated at a temperature of 30-45°C to a density of 1.180±0.006 g / cm 3 , the result is cherry concentrate B;

[0058] (4) Add 3 times the weight of the extraction filtrate A of step (2) to the cherry concentrate B, mix well, place in a -10°C to 5°C environment, naturally settle for 12h to 36h, filter at room temperature, and concentrate the obtained filtrate under reduced pressure at a pressure of -0.08MPa to 0.1MPa and a temperature of 30 to 45°C to make the density of the concentrated solution reach 0.950±0.006g / cm 3 , the result is cherry extract for smoking.

[0059] S2. GC-IMS analysis

[0060] GC-IMS technology combines gas chromatography with ion migration technology, offering both high resolution and high sensitivity. After GC separation, the sample is ionized by IMS to form ions, and volatile components are distinguished based on differences in migration time. In this patent, the tobacco cherry extract sample is generally a liquid and can be directly weighed and injected. The tobacco cherry extract sample is collected at a preset storage time point and injected directly without pretreatment. 0.5 g is weighed and placed in a 20 mL headspace injection vial. GC-IMS is used to obtain a three-dimensional spectrum of the volatile aroma components (retention time - migration time - signal intensity).

[0061] GC-IMS detection conditions include:

[0062] use Gas phase ion mobility spectrometry (GAS, Germany) was used. Headspace injection conditions were: incubation temperature 60°C, incubation time 5 min, incubation speed 500 rpm, injection needle temperature 85°C, injection volume 100 μL. GC-IMS conditions were: MXT-5 column (15 m × 0.53 mm, 1.0 μm), column temperature 60°C, analysis time 30 min, carrier gas high-purity N2 (purity ≥99.999%), IMS temperature 45°C, drift gas rate 150 mL / min, carrier gas rate: initial 2 mL / min, maintained for 30 min.

[0063] S3. Feature fingerprint map construction

[0064] according to The characteristic fingerprint of tobacco cherry extract was established based on the GC-IMS test results.

[0065] (1) The built-in Reporter of the analysis software Vocal was used to draw an intuitive two-dimensional map of the aroma components of the cherry extract for smoking, including gas chromatography retention time (vertical axis, unit is s), ion migration time (horizontal axis, unit is ms) and ion intensity (each point represents a volatile component, white indicates a low content, red indicates a high content, the darker the color, the higher the content. The ion intensity of each aroma component is intuitively displayed with visual color depth. The ion intensity refers to the current signal intensity generated by a specific ion hitting the Faraday disk (detector) in the migration tube, which indirectly reflects the concentration of the compound in the sample). The results are as follows. Figure 1 shown.

[0066] (2) Based on the two-dimensional map information, the built-in Gallery Plot plug-in of the analysis software Vocal and the IMS database were used to establish the characteristic aroma fingerprint of the tobacco cherry extract. The results are as follows: Figure 2 and as shown in Table 1.

[0067] Table 1: Qualitative results of characteristic aroma of cherry extract for tobacco

[0068]

[0069]

[0070] (3) The corresponding ROAV value was calculated using the relative content and sensory threshold of each volatile component. The results are shown in Table 2. The relative content of each volatile component was calculated by peak area normalization method, and the sensory threshold was obtained by consulting professional manuals such as "ODOURTHRESHOLD" or scientific database retrieval. The ROAV value is used to define the component that contributes most to the overall flavor of the sample. (Ethyl acetate) ROAV max The value of the compound is 100, and the other compounds are calculated according to the formula:

[0071]

[0072] Wherein, Ci is the relative content (%) of the i-th volatile compound; Ti is the sensory threshold (μg / kg) of the i-th volatile compound; Cmax is the relative content (%) of the volatile compound that contributes most to the overall flavor; Tmax is the sensory threshold (μg / kg) of the volatile compound that contributes most to the overall flavor.

[0073] Table 2 Thresholds and ROAV values ​​of characteristic aroma components of cherry extract for tobacco

[0074]

[0075]

[0076] Note: The thresholds in the table are based on the aroma threshold in water; “—” indicates that it was not found.

[0077] According to the principle that the ROAV value is greater than 1, the key aroma components of cherry extract for tobacco are determined to include ethyl acetate, benzaldehyde, phenylacetaldehyde, isobutyl butyrate, methyl butyrate, isobutyl formate, isoamyl formate, propyl butyrate, 2-methyl-3-methylthiofuran, 3-methyl-2-butenal, 2-ethylfuran, 2,5-dimethylfuran, 2,3-pentanedione, valeraldehyde, hydroxyacetone, 2-methylvaleraldehyde, acetaldehyde propylene glycol acetal and other aroma components, which together give cherry extract for tobacco a rich and strong fruity aroma.

[0078] S4. Dynamic monitoring and quality evaluation

[0079] (1) Based on the characteristic fingerprint of the cherry extract for tobacco constructed in step S2, non-critical aroma components were eliminated, and the Gallery Plot plug-in built into the analysis software Vocal was used to establish a dynamic tracking model for aroma quality changes, thereby realizing aroma quality change trend monitoring of the cherry extract for tobacco. Among them, during the storage period, at intervals of time, such as on the 0th, 15th, 30th and 45th days of storage, the cherry extract samples for tobacco are repeatedly subjected to GC-IMS detection to update the data of the characteristic aroma components of ethyl acetate, benzaldehyde, isobutyl butyrate, 2-methyl-3-methylthiofuran, 3-methyl-2-butenal, methyl butyrate, 2-ethylfuran, 2,5-dimethylfuran, isopentanol, 2,3-pentanedione, valeraldehyde, hydroxyacetone, isobutyl formate, 3-methyl-2-butanol, 2-methylvaleraldehyde, butyric acid, butyl acetate, acetaldehyde propylene glycol acetal, isopentyl formate and propyl butyrate, thereby realizing a dynamic tracking model for changes in aroma quality.

[0080] (2) The built-in Gallery Plot plug-in of the application analysis software Vocal can quickly calculate the similarity between the tested sample and the standard sample, such as Figure 3 The aroma quality of the sample was determined to be qualified. The cherry extract sample stored on the 0th day was used as the standard sample. The relative content of each aroma component in the standard sample is shown in Table 2.

[0081] This patent adopts a GC-IMS detection method that does not require pretreatment, which can retain more real component information. The detection process is fast and convenient, and samples can be directly injected, avoiding inaccurate detection data caused by complex pretreatment.

[0082] In addition, this patent screens and identifies the characteristic aroma components of cherry extract for tobacco use, and clarifies the characteristic aroma components of ethyl acetate, benzaldehyde, isobutyl butyrate, 2-methyl-3-methylthiofuran, 3-methyl-2-butenal, methyl butyrate, 2-ethylfuran, 2,5-dimethylfuran, isopentanol, 2,3-pentanedione, valeraldehyde, hydroxyacetone, isobutyl formate, 3-methyl-2-butanol, 2-methylvaleraldehyde, butyric acid, butyl acetate, acetaldehyde propylene glycol acetal, isopentyl formate and propyl butyrate from a variety of aroma components, which facilitates the subsequent establishment of aroma quality change trend monitoring for the characteristic aroma components, and can also directly determine whether the aroma quality of the test sample is qualified on the software, making the detection more convenient and quick.

[0083] Example 1

[0084] 1. Sample preparation and GC-IMS analysis:

[0085] The first batch of tobacco cherry extract samples were placed in a sealed container and stored at 25°C and 60% RH. At 0 days, 15 days, 30 days, and 45 days of storage, 0.5 g was weighed and placed in a 20 mL headspace injection vial for GC-IMS analysis.

[0086] GC-IMS detection conditions include:

[0087] use Gas phase ion mobility spectrometry (GAS, Germany) was used. Headspace injection conditions were: incubation temperature 60°C, incubation time 5 min, incubation speed 500 rpm, injection needle temperature 85°C, injection volume 100 μL. GC-IMS conditions were: MXT-5 column (15 m × 0.53 mm, 1.0 μm), column temperature 60°C, analysis time 30 min, carrier gas high-purity N2 (purity ≥99.999%), IMS temperature 45°C, drift gas rate 150 mL / min, carrier gas rate: initial 2 mL / min, maintained for 30 min.

[0088] The tobacco cherry extract sample stored on the 0th day was used as the standard sample. The relative contents of the aroma components in the standard sample are shown in Table 2. The tobacco cherry extract samples stored on the 15th, 30th, and 45th days were used as the tested samples for comparison with the standard sample.

[0089] 2. Dynamic monitoring

[0090] The Gallery Plot plug-in built into the analysis software Vocal was used to monitor 21 aroma components, including ethyl acetate, benzaldehyde, isobutyl butyrate, 2-methyl-3-methylthiofuran, 3-methyl-2-butenal, methyl butyrate, 2-ethylfuran, 2,5-dimethylfuran, isopentanol, 2,3-pentanedione, valeraldehyde, hydroxyacetone, isobutyl formate, 3-methyl-2-butanol, 2-methylvaleraldehyde, butyric acid, butyl acetate, acetaldehyde propylene glycol acetal, isopentyl formate, and propyl butyrate, at intervals to monitor the aroma quality change trend of cherry extract for tobacco use. The results are as follows: Figure 4 shown.

[0091] Example 2

[0092] 1. Sample preparation and GC-IMS analysis:

[0093] The second batch of cherry extract samples were placed in a sealed container and stored at 25°C and 60% RH. At 0 days, 15 days, 30 days, 45 days, and 60 days of storage, 0.5 g was weighed and placed in a 20 mL headspace injection vial for GC-IMS analysis.

[0094] GC-IMS detection conditions include:

[0095] use Gas phase ion mobility spectrometry (GAS, Germany) was used. Headspace injection conditions were: incubation temperature 60°C, incubation time 5 min, incubation speed 500 rpm, injection needle temperature 85°C, injection volume 100 μL. GC-IMS conditions were: MXT-5 column (15 m × 0.53 mm, 1.0 μm), column temperature 60°C, analysis time 30 min, carrier gas high-purity N2 (purity ≥99.999%), IMS temperature 45°C, drift gas rate 150 mL / min, carrier gas rate: initial 2 mL / min, maintained for 30 min.

[0096] The tobacco cherry extract sample stored on the 0th day was used as the standard sample. The relative contents of the aroma components in the standard sample are shown in Table 2. The tobacco cherry extract samples stored on the 15th, 30th, and 45th days were used as the tested samples for comparison with the standard sample.

[0097] 2. Quality evaluation

[0098] The 21 aroma components, including ethyl acetate, benzaldehyde, isobutyl butyrate, 2-methyl-3-methylthiofuran, 3-methyl-2-butenal, methyl butyrate, 2-ethylfuran, 2,5-dimethylfuran, isoamyl alcohol, 2,3-pentanedione, valeraldehyde, hydroxyacetone, isobutyl formate, 3-methyl-2-butanol, 2-methylvaleraldehyde, butyric acid, butyl acetate, acetaldehyde propylene glycol acetal, isoamyl formate and propyl butyrate, were monitored. The Gallery Plot plug-in built into the analysis software Vocal was used to quickly calculate the similarity between the tested sample and the standard sample, which was 95%, higher than the threshold set at 90%. The aroma quality of the tested sample was determined to be qualified. The results are as follows: Figure 5 Shown is a sample of tobacco cherry extract on the 15th day of storage.

[0099] Example 3

[0100] 1. Sample preparation and GC-IMS analysis:

[0101] The third batch of cherry extract samples were placed in a sealed container and stored at 25°C and 60% RH. On the 0th day and every 15 days of storage, 0.5 g was weighed and placed in a 20 mL headspace injection vial for GC-IMS analysis.

[0102] GC-IMS detection conditions include:

[0103] use Gas phase ion mobility spectrometry (GAS, Germany) was used. Headspace injection conditions were: incubation temperature 60°C, incubation time 5 min, incubation speed 500 rpm, injection needle temperature 85°C, injection volume 100 μL. GC-IMS conditions were: MXT-5 column (15 m × 0.53 mm, 1.0 μm), column temperature 60°C, analysis time 30 min, carrier gas high-purity N2 (purity ≥99.999%), IMS temperature 45°C, drift gas rate 150 mL / min, carrier gas rate: initial 2 mL / min, maintained for 30 min.

[0104] The tobacco cherry extract sample stored on the 0th day was used as the standard sample. The relative contents of the aroma components in the standard sample are shown in Table 2. The tobacco cherry extract samples stored on the 15th, 30th, 45th, ... 135th days were used as the tested samples for comparison with the standard sample.

[0105] 2. Quality evaluation

[0106] The 21 aroma components, including ethyl acetate, benzaldehyde, isobutyl butyrate, 2-methyl-3-methylthiofuran, 3-methyl-2-butenal, methyl butyrate, 2-ethylfuran, 2,5-dimethylfuran, isoamyl alcohol, 2,3-pentanedione, valeraldehyde, hydroxyacetone, isobutyl formate, 3-methyl-2-butanol, 2-methylvaleraldehyde, butyric acid, butyl acetate, acetaldehyde propylene glycol acetal, isoamyl formate and propyl butyrate, were monitored. The Gallery Plot plug-in built into the analysis software Vocal was used to quickly calculate the similarity between the tested sample and the standard sample, which was 69%, lower than the threshold value of 90%. Combined with sensory evaluation, it was found that the cherry fruit aroma and burnt sweet aroma of the tested sample were significantly weakened, and the aroma quality of the tested sample was judged to be unqualified. The results are as follows: Figure 6 Shown is a sample of tobacco cherry extract on day 135 of storage.

[0107] This patent provides a method for monitoring the aroma quality of cherry extract for tobacco during storage. The method can monitor the characteristic aroma components of ethyl acetate, benzaldehyde, isobutyl butyrate, 2-methyl-3-methylthiofuran, 3-methyl-2-butenal, methyl butyrate, 2-ethylfuran, 2,5-dimethylfuran, isopentanol, 2,3-pentanedione, valeraldehyde, hydroxyacetone, isobutyl formate, 3-methyl-2-butanol, 2-methylvaleraldehyde, butyric acid, butyl acetate, acetaldehyde propylene glycol acetal, isopentyl formate and propyl butyrate in multiple different varieties or batches of cherry extract for tobacco. By utilizing the high separation and high sensitivity characteristics of GC-IMS technology, the detection results obtained can realize the monitoring of the changing trend of the aroma quality of cherry extract for tobacco.

[0108] In addition, this patent can further apply the Gallery Plot plug-in built into the analysis software Vocal to quickly calculate the similarity between the tested sample and the standard sample of the tobacco cherry extract, and directly determine whether the aroma quality of the tested sample is qualified on the software.

[0109] In the above description of exemplary embodiments / embodiments of this patent, various features of this patent are sometimes grouped together in a single embodiment / embodiment or its drawings and description for the purpose of simplifying the disclosure and aiding understanding of one or more of the various inventive aspects. However, except for explicitly stated contrary guidance or obvious technical contradiction or exclusion, the description method of this patent should not be interpreted as reflecting an intention that the claimed invention requires more features than expressly stated in each claim. Instead, the claims reflect that the inventive aspects lie in less than all features of a single aforementioned disclosed embodiment / embodiment. Therefore, the claims following the detailed description are hereby expressly incorporated into this detailed description, with each claim existing independently as a separate embodiment / embodiment of this patent.

[0110] The terms and expressions used in this specification are intended to be illustrative rather than limiting, and in the use of these terms and expressions, there is no intention to exclude any equivalents of the features shown and described or portions thereof, but it should be recognized that various variations are possible within the scope of the protection claimed in this patent. It should therefore be understood that although this patent is specifically disclosed through preferred embodiments, exemplary embodiments, and optional features, those skilled in the art may adopt variations or modifications of the concepts disclosed in this specification, and such variations and modifications are therefore considered to be within the scope of this patent as defined by the appended claims. The specific embodiments given in this specification are examples of useful embodiments of this patent, and it is obvious to those skilled in the art that many variations of the devices, device components, and method steps disclosed in this specification can be used to implement this patent.

[0111] The foregoing description of the specific embodiments fully discloses the general features of this patent so that others can easily modify and / or adapt such specific embodiments for various applications by applying knowledge within the technical scope of the art without undue experimentation and without departing from the general concept of this patent. Therefore, based on the teachings and guidance given herein, it is intended that such adaptations and modifications be included within the meaning and range of equivalents of the disclosed embodiments. It should be understood that the words or terms used herein are for descriptive purposes only and are not intended to be limiting, and thus the words or terms of this specification will be interpreted by those skilled in the art based on the above teachings and guidance.

[0112] Additionally, the scope of this patent should not be limited by any of the above-described exemplary embodiments, but should be defined only in accordance with the following claims and their equivalents.

Claims

1. A method for identifying and screening characteristic aroma components of cherry extract for tobacco, characterized in that: The following steps are involved: Step A: Collecting a sample of the tobacco cherry extract at a preset storage time point, and obtaining volatile aroma component information by GC-IMS detection method, wherein the volatile aroma component information includes the type of volatile components and the relative content of the volatile components; Step B: Calculate the ROAV value of each volatile component based on the type of volatile component and the relative content of the volatile component in combination with the sensory threshold. The ROAV value calculation formula is as follows: Wherein, Ci is the relative content of the i-th volatile component (%); Ti is the sensory threshold of the i-th volatile component (μg / kg); Cmax is the relative content of the volatile component that contributes most to the overall flavor (%); Tmax is the sensory threshold of the volatile component that contributes most to the overall flavor (μg / kg); Step D: Screening out the volatile component types with the ROAV value greater than 1 to obtain the characteristic aroma components of the cherry extract for smoking.

2. The method for identifying and screening characteristic aroma components of cherry extract for tobacco according to claim 1, characterized in that: In step A, the GC-IMS detection adopts headspace sampling, The incubation temperature of the headspace injection is 50-70° C., the incubation time is 3-8 min, the incubation speed is 400-600 r / min, the injection needle temperature is 80-90° C., and the injection volume is 90-105 μL.

3. The method for identifying and screening characteristic aroma components of cherry extract for tobacco according to claim 2, characterized in that: The GC-IMS detection uses a MXT-5 chromatographic column, a column temperature of 60°C, an analysis time of 30 min, a carrier gas of N2, an IMS temperature of 45°C, a drift gas flow rate of 150 mL / min, and an initial carrier gas flow rate of 2 mL / min maintained for 30 min.

4. The method for identifying and screening characteristic aroma components of cherry extract for tobacco according to claim 1, characterized in that: The characteristic aroma components of the tobacco cherry extract in step D include ethyl acetate, benzaldehyde, isobutyl butyrate, 2-methyl-3-methylthiofuran, 3-methyl-2-butenal, methyl butyrate, 2-ethylfuran, 2,5-dimethylfuran, isopentanol, 2,3-pentanedione, valeraldehyde, hydroxyacetone, isobutyl formate, 3-methyl-2-butanol, 2-methylvaleraldehyde, butyric acid, butyl acetate, acetaldehyde propylene glycol acetal, isopentyl formate and propyl butyrate.

5. A method for monitoring the aroma quality of cherry extract for tobacco during storage, characterized in that: The following steps are involved: Step A: Collecting a sample of the tobacco cherry extract at a preset storage time point, and obtaining volatile aroma component information by GC-IMS detection method, wherein the volatile aroma component information includes the type of volatile component, the relative content of the volatile component, the chromatographic retention time, the ion migration time and the ion strength; Step B: Calculate the ROAV value of each volatile component based on the type of volatile component and the relative content of the volatile component in combination with the sensory threshold. The ROAV value calculation formula is as follows: Wherein, Ci is the relative content of the i-th volatile component (%); Ti is the sensory threshold of the i-th volatile component (μg / kg); Cmax is the relative content of the volatile component that contributes most to the overall flavor (%); Tmax is the sensory threshold of the volatile component that contributes most to the overall flavor (μg / kg); Step D: screening out the volatile component types with the ROAV value greater than 1 to obtain the characteristic aroma components of the smoking cherry extract; Step E: Using the analysis software Vocal, a characteristic aroma fingerprint of the characteristic aroma components of the smoking cherry extract is established according to the chromatographic retention time, the ion migration time and the ion intensity, thereby forming a dynamic tracking model for aroma quality changes.

6. The method for monitoring the aroma quality of cherry extract for tobacco during storage according to claim 5, characterized in that: The step E comprises the following steps: Step E1: using the built-in Reporter of the analysis software Vocal to draw an intuitive two-dimensional spectrum of the aroma components of the smoking cherry extract according to the chromatographic retention time, the ion migration time and the ion intensity; Step E2: Based on the two-dimensional map information, the Gallery Plot plug-in built into the analysis software Vocal and the IMS database are used to establish an aroma fingerprint of the smoking cherry extract; Step E3: Retain the data of ethyl acetate, benzaldehyde, isobutyl butyrate, 2-methyl-3-methylthiofuran, 3-methyl-2-butenal, methyl butyrate, 2-ethylfuran, 2,5-dimethylfuran, isopentanol, 2,3-pentanedione, valeraldehyde, hydroxyacetone, isobutyl formate, 3-methyl-2-butanol, 2-methylvaleraldehyde, butyric acid, butyl acetate, acetaldehyde propylene glycol acetal, isopentyl formate and propyl butyrate on the aroma fingerprint to obtain the characteristic aroma fingerprint of the characteristic aroma components of the tobacco cherry extract.

7. The method for monitoring the aroma quality of cherry extract for tobacco during storage according to claim 6, characterized in that: The step E further comprises the following steps: Step E4: The Gallery Plot plug-in built into the analysis software Vocal is used to quickly calculate the similarity between the tested sample of the cherry extract for smoking and the standard sample, and determine whether the aroma quality of the cherry extract for smoking is qualified.

8. The method for monitoring the aroma quality of cherry extract for tobacco during storage according to claim 7, characterized in that: In step E4, the similarity threshold between the tested sample and the standard sample is set to at least 90%, thereby judging that the aroma quality of the tobacco cherry extract sample is qualified.

9. The method for monitoring the aroma quality of cherry extract for tobacco during storage according to claim 5, characterized in that: In the step A, the preset storage time point is the 0th day of the storage period and the cherry extract sample is collected every 10 to 15 days from the 0th day of the storage period.

Images