Evaluation method for spicy–aromatic flavor of cigarette smoke, and applications thereof

Abstract

An evaluation method for the spicy–aromatic flavor of cigarette smoke, and applications thereof. The evaluation method comprises the following steps: (1) collecting total particulate matters of mainstream cigarette smoke from representative spicy-aromatic and non-spicy-aromatic cigarettes, performing GC–MS analysis to obtain the contents of aroma-contributing components in the total particulate matters, and performing partial least squares discriminant analysis on the contents of the aroma-contributing components, so as to obtain VIP values of the aroma-contributing components; (2) collecting the total particulate matter of mainstream cigarette smoke from a cigarette under test, and performing GC–MS analysis to obtain the contents of aroma-contributing components in the cigarette under test; and (3) on the basis of the VIP values and the contents of the aroma-contributing components in the cigarette under test, calculating a spicy–aromatic flavor index Q. The evaluation method can objectively and accurately reflect the spicy–aromatic flavor of cigarette smoke, and avoids subjective errors caused by sensory evaluation, and the situation where an analysis result of aroma-contributing components in tobacco fillers is inconsistent with actual smoking experience, thereby providing a new method for characterization and evaluation of spicy–aromatic flavor of cigarette smoke.

Description

A method for evaluating the spicy aroma and flavor of cigarette smoke and its application Technical Field

[0001] This invention belongs to the field of tobacco analysis technology, specifically relating to an evaluation method for the spicy aroma and flavor of cigarette smoke and its application. Background Technology

[0002] Consumers' consumption patterns of cigarette products dictate that the aroma and flavor characteristics of cigarette smoke are crucial to the formation of cigarette style, and are one of the most important bases for product category construction. Existing research indicates that the overall aroma style of cigarettes is mainly formed by the combined effects of different aroma and flavor characteristics, and each aroma and flavor characteristic is underpinned by a set of material bases that make significant contributions. Currently, sensory evaluation remains the core of the aroma and flavor characteristic evaluation system, but this method lacks objective data support and is time-consuming and labor-intensive to implement. At the molecular level of the material basis, industry researchers have characterized aroma characteristics using indices based on aroma-producing components in tobacco, which has a certain positive effect on the evaluation of aroma characteristics, but it does not fully consider the migration rate of aroma-producing components from tobacco to smoke, or the changes in the types and contents of aroma-producing components during cigarette combustion. Spicy aroma, in particular, can effectively influence consumers' sensory evaluation of cigarette products, making its evaluation especially important.

[0003] Therefore, it is particularly important to identify and extract a set of characteristic aroma components that significantly contribute to the spicy and aromatic flavor of cigarette smoke from numerous chemical components, based on the aroma components of cigarette smoke, using instrumental analysis and detection methods combined with multivariate statistical analysis techniques, so as to achieve an objective and accurate characterization and evaluation of the characteristic aroma of cigarette smoke.

[0004] Summary of the Invention

[0005] To address the shortcomings of existing technologies, the present invention aims to provide a method for evaluating the spicy aroma and flavor of cigarette smoke and its application. The evaluation method provided by this invention can objectively and accurately reflect the spicy aroma and flavor of cigarette smoke, avoiding subjective errors caused by sensory evaluation and discrepancies between the analysis results of aroma components in tobacco and the actual smoking experience. It provides a new method for characterizing and evaluating the spicy aroma and flavor of cigarette smoke, and plays a positive and important role in the rapid evaluation of the spicy aroma and flavor of cigarette smoke and in the research on enhancing the spicy style of cigarettes.

[0006] To achieve this objective, the present invention adopts the following technical solution:

[0007] On the one hand, the present invention provides a method for evaluating the spicy aroma of cigarette smoke, the evaluation method comprising the following steps:

[0008] (1) Collect the total particulate matter of the mainstream smoke of typical spicy cigarettes and typical non-spicy cigarettes, and perform GC-MS (gas chromatography-mass spectrometry) to obtain the content of aroma components in typical spicy cigarettes and typical non-spicy cigarettes. Perform partial least squares discriminant analysis on the content of aroma components to obtain the VIP value (variable weight value) of aroma components.

[0009] (2) Collect the total particulate matter of the mainstream smoke of the cigarette to be tested and perform GC-MS detection to obtain the content of aroma components in the cigarette to be tested;

[0010] (3) Calculate the spiciness and aroma index Q of the cigarette smoke based on the VIP value of the aroma component obtained in step (1) and the content of the aroma component in the cigarette obtained in step (2), and determine the degree of spiciness and aroma of the cigarette smoke.

[0011] Steps (1) and (2) are not in any particular order.

[0012] The aroma-producing components include positively correlated aroma-producing components and negatively correlated aroma-producing components.

[0013] The positively correlated aroma components include any one or a combination of at least two of terpenoid aroma components, long-chain unsaturated fatty acid methyl esters, and positively correlated ketone aroma components. The negatively correlated aroma components include any one or a combination of at least two of nitrogen-containing heterocyclic aroma components, furan aroma components, and negatively correlated ketone aroma components.

[0014] The above method analyzes the aroma components in typical spicy cigarettes, typical non-spicy cigarettes, and the cigarettes under test. It uses partial least squares discriminant analysis to obtain the VIP value, and calculates the spicy aroma index Q by combining it with the content of aroma components. This method can objectively and accurately reflect the spicy aroma of cigarette smoke, avoiding subjective errors caused by sensory evaluation and discrepancies between the analysis results of aroma components in tobacco and the actual smoking experience. It provides a new method for characterizing and evaluating the spicy aroma of cigarette smoke, and plays a positive and important role in the rapid evaluation of the spicy aroma of cigarette smoke and the enhanced research on the spicy style of cigarettes.

[0015] Preferably, the positively correlated aroma components include a combination of terpenoid aroma components, long-chain unsaturated fatty acid methyl esters, and positively correlated ketone aroma components.

[0016] Preferably, the negatively correlated aroma components include a combination of nitrogen-containing heterocyclic aroma components, furan aroma components, and negatively correlated ketone aroma components.

[0017] Preferably, the terpenoid aroma component includes neophytadiene;

[0018] Preferably, the aroma-producing components of the long-chain unsaturated fatty acid methyl esters include methyl linoleate and / or methyl palmitate;

[0019] Preferably, the positively correlated ketone aroma component includes 3-hydroxy-2-butanone;

[0020] Preferably, the nitrogen-containing heterocyclic aroma component includes pyridine;

[0021] Preferably, the furan-type aroma component includes 2-ethylfuran;

[0022] Preferably, the negatively correlated ketone aroma components include cyclopentanone and / or 3-penten-2-one.

[0023] The aforementioned combination of specific aroma components can comprehensively and effectively evaluate the spicy aroma of the cigarette smoke being tested, thereby improving the accuracy of the evaluation.

[0024] Preferably, in the GC-MS detection, the chromatographic column is an HP-5MS.

[0025] Preferably, in the GC-MS detection, the carrier gas flow rate is 0.8-1.2 mL / min, such as 0.8 mL / min, 0.9 mL / min, 1 mL / min, 1.1 mL / min or 1.2 mL / min, but not limited to the values ​​listed above. Other unlisted values ​​within the above range are also applicable.

[0026] Preferably, in the GC-MS detection, the temperature rise procedure is as follows:

[0027] Start at 40-60℃ and hold for 0.7-1.3 min; then increase to 155-175℃ at a rate of 6-10℃ / min and hold for 1.4-2.4 min; then increase to 255-275℃ at a rate of 6-10℃ / min and hold for 12-16 min.

[0028] The specific GC-MS detection conditions described above can effectively improve the accuracy of the detection results, thereby improving the accuracy of the evaluation results.

[0029] Preferably, the formula for calculating the spiciness and aroma index Q in step (3) is as follows: Q = ∑(content of positively correlated aroma-producing component i × VIP) i ) / ∑(content of negatively correlated aroma-producing component j × VIP j );

[0030] In the formula, VIP i This represents the VIP value of the positively correlated aroma-producing component i. j This represents the VIP value of the negatively correlated aroma-producing component j.

[0031] In the above formula, the spicy aroma of cigarette smoke is positively correlated with the index Q. That is, the higher the spicy aroma index Q value of the cigarette smoke to be tested, the more obvious the spicy aroma characteristics of the cigarette smoke.

[0032] On the other hand, the present invention also provides the application of the evaluation method described above in the evaluation and analysis of cigarette smoke aroma.

[0033] Compared with the prior art, the present invention has the following beneficial effects:

[0034] This invention provides a method for evaluating the spicy aroma and flavor of cigarette smoke. By analyzing the aroma components in typical spicy cigarettes, typical non-spicy cigarettes, and the cigarette to be tested, partial least squares discriminant analysis is used to obtain the VIP value, which is then combined with the content of the aroma components to calculate the spicy aroma and flavor index Q. This method can objectively and accurately reflect the spicy aroma and flavor of cigarette smoke, avoiding subjective errors caused by sensory evaluation and discrepancies between the analysis results of the aroma components in tobacco and the actual smoking experience. It provides a new method for characterizing and evaluating the spicy aroma and flavor of cigarette smoke, and plays a positive and important role in the rapid evaluation of the spicy aroma and flavor of cigarette smoke and the enhanced research on the spicy style of cigarettes. Detailed Implementation

[0035] To further illustrate the technical means and effects of the present invention, the following describes the technical solution of the present invention in conjunction with preferred embodiments of the present invention. However, the present invention is not limited to the scope of the embodiments.

[0036] Example 1

[0037] This embodiment provides a method for evaluating the spicy and aromatic flavor of cigarette smoke, and the specific steps are as follows:

[0038] Fragrance component analysis:

[0039] The method for collecting total particulate matter in the mainstream smoke of cigarettes is in accordance with the national standard GB / T19609-2004 "Determination of total particulate matter and tar in cigarettes using a conventional analysis smoking machine".

[0040] The collected filter was placed in a simultaneous distillation and extraction apparatus and simultaneously distilled and extracted with dichloromethane as solvent for 2 hours. The resulting extract was dried with anhydrous sodium sulfate and concentrated to 1.0 mL in a rotary evaporator. 50 μL (0.1 mol / L) of anhydrous ethanol solution of benzoyl acetate was added and shaken well for GC-MS analysis.

[0041] GC-MS analysis conditions:

[0042] Chromatographic column: HP-5MS (30m × 0.25mm × 0.25μm) capillary column; injection port temperature: 240℃; transfer line temperature: 280℃; carrier gas: He, flow rate 1.0mL / min; temperature program: hold at 50℃ for 1 min, increase to 165℃ at a rate of 8℃ / min, hold for 1.9 min, then increase to 265℃ at a rate of 8℃ / min, hold for 14 min; injection volume: 2μL, split ratio: 25:1; EI ionization energy: 70eV; ion source temperature: 230℃; quadrupole temperature: 160℃; mass range: 35~455amu. Qualitative analysis was performed using NIST17 and Wiley275 standard libraries, and quantification was performed using the internal standard method to obtain the content of some aroma components.

[0043] (1) The aroma components of typical spicy and non-spicy cigarettes were detected using the above methods. Partial least squares discriminant analysis (PLS-DA) was performed using the chemometrics statistical software SIMCA 14.1 to calculate the VIP values ​​of aroma components such as terpenes (neoptiadiene), long-chain unsaturated fatty acid methyl esters (methyl linoleate, methyl palmitate), ketones (3-hydroxy-2-butanone, cyclopentanone, 3-penten-2-one), nitrogen-containing heterocyclic compounds (pyridine), and furans (2-ethylfuran). The results are shown in the table below.

[0044] (2) The aroma components of 38 commercially available cigarettes were tested using the above method, and the results are shown in the table below.

[0045] (3) Calculate the spiciness and aroma index Q of the cigarette smoke of the above 38 commercially available cigarettes. The Q index reflects the spiciness and aroma of the cigarette smoke. The spiciness and aroma index Q of the cigarette smoke to be tested is calculated using a weighted statistical method. The calculation formula is: Q=∑(content of positively correlated aroma component i × VIP) i ) / ∑(content of negatively correlated aroma-producing component j × VIP j );

[0046] In the above formula, VIP i This represents the VIP value of the positively correlated aroma-producing component i. j The VIP value represents the negatively correlated aroma component j. The positively correlated aroma components are neophytadiene, methyl linoleate, methyl palmitate, and 3-hydroxy-2-butanone. The negatively correlated aroma components are pyridine, 2-ethylfuran, cyclopentanone, and 3-penten-2-one. The results are shown in the table below.

[0047] (4) In order to verify that the Q value is closely related to the intensity trend of the spicy aroma of cigarette smoke, a group comparison evaluation method was adopted. 18 groups of samples were randomly selected and distributed according to the high, medium and low Q values. Each group was divided into No. 1, No. 2 and No. 3. The order of Q value was No. 1 > No. 2 > No. 3. The evaluation group composed of 12 experts conducted comparative evaluation according to the provisions of "GB5606.4-2005 Sensory Technical Requirements for Cigarettes". The results showed that the evaluation conclusions of 6 groups were consistent with the trend of their Q values ​​(see the table below). This indicates that the Q value has applicable value in characterizing and evaluating the spicy aroma of cigarette smoke and can accurately and effectively evaluate the spicy aroma of cigarette smoke.

[0048] Example 2

[0049] This embodiment provides a method for evaluating the spicy aroma and flavor of cigarette smoke. Except for the GC-MS analysis conditions, the specific steps are the same as in Example 1.

[0050] GC-MS analysis conditions:

[0051] Chromatographic column: HP-5MS (30m × 0.25mm × 0.25μm) capillary column; injection port temperature: 240℃; transfer line temperature: 280℃; carrier gas: He, flow rate 0.8mL / min; temperature program: hold at 40℃ for 1.3min, increase to 155℃ at a rate of 6℃ / min, hold for 2.4min, then increase to 255℃ at a rate of 6℃ / min, hold for 16min; injection volume: 2μL, split ratio: 25:1; EI ionization energy: 70eV; ion source temperature: 230℃; quadrupole temperature: 160℃; mass range: 35~455amu. Qualitative analysis was performed using NIST17 and Wiley275 standard libraries, and quantification was performed using the internal standard method to obtain the content of some aroma components.

[0052] Example 3

[0053] This embodiment provides a method for evaluating the spicy aroma and flavor of cigarette smoke. Except for the GC-MS analysis conditions, the specific steps are the same as in Example 1.

[0054] GC-MS analysis conditions:

[0055] Chromatographic column: HP-5MS (30m × 0.25mm × 0.25μm) capillary column; injection port temperature: 240℃; transfer line temperature: 280℃; carrier gas: He, flow rate 1.2mL / min; temperature program: hold at 60℃ for 0.7min, increase to 175℃ at a rate of 10℃ / min, hold for 1.4min, then increase to 275℃ at a rate of 10℃ / min, hold for 12min; injection volume: 2μL, split ratio: 25:1; EI ionization energy: 70eV; ion source temperature: 230℃; quadrupole temperature: 160℃; mass range: 35~455amu. Qualitative analysis was performed using NIST17 and Wiley275 standard libraries, and quantification was performed using the internal standard method to obtain the content of some aroma components.

[0056] Example 4

[0057] This embodiment provides a method for evaluating the spicy aroma of cigarette smoke. The specific steps are the same as in Example 1, except that the HP-5MS chromatographic column is replaced with a DB-35MS column.

[0058] Example 5

[0059] This embodiment provides a method for evaluating the spicy aroma and flavor of cigarette smoke. Except for the heating procedure, the specific steps are the same as in Embodiment 1.

[0060] Hold at 70℃ for 1 min, then increase the temperature to 210℃ at a rate of 24℃ / min, hold for 1 min, then increase the temperature to 280℃ at a rate of 6℃ / min, and hold for 5 min.

[0061] Example 6

[0062] This embodiment provides a method for evaluating the spicy aroma of cigarette smoke. The specific steps are the same as in Example 1, except that the aroma-causing components do not contain neophytadiene.

[0063] Example 7

[0064] This embodiment provides a method for evaluating the spicy aroma of cigarette smoke. The specific steps are the same as in Example 1, except that the aroma-producing components do not contain methyl linoleate and methyl palmitate.

[0065] Example 8

[0066] This embodiment provides a method for evaluating the spicy aroma of cigarette smoke. The specific steps are the same as in Example 1, except that the aroma-causing components do not contain cyclopentanone and 3-penten-2-one.

[0067] Example 9

[0068] This embodiment provides a method for evaluating the intensity of the spicy aroma of cigarette smoke. The specific steps are the same as in Example 1, except that the aroma-causing components do not contain pyridine.

[0069] Example 10

[0070] This embodiment provides a method for evaluating the intensity of the spicy aroma of cigarette smoke. The specific steps are the same as in Example 1, except that the aroma-causing components do not contain 3-hydroxy-2-butanone.

[0071] Effect test:

[0072] Seven additional cigarette samples with different intensities of spicy aroma were selected and compared by a 12-member expert evaluation panel according to the provisions of "GB5606.4-2005 Sensory Technical Requirements for Cigarettes". The intensities were determined to be ranked from lowest to highest as A, B, C, D, E, F, and G. The seven groups of cigarettes were then rated using the methods provided in Examples 1-10, and the Q value was calculated. The results are as follows:

[0073] The results above show that by controlling specific chromatographic parameters and selecting specific aroma component combinations, this invention can more accurately, comprehensively, and effectively evaluate the spicy aroma of the cigarette smoke being tested, thus effectively improving the accuracy of the evaluation results.

[0074] The applicant declares that this invention illustrates the method for evaluating the spicy aroma and flavor of cigarette smoke and its application through the above embodiments. However, this invention is not limited to the above embodiments, meaning that this invention does not necessarily rely on the above embodiments for implementation. Those skilled in the art should understand that any improvements to this invention, equivalent substitutions of raw materials for the product, addition of auxiliary components, and selection of specific methods all fall within the protection and disclosure scope of this invention.

[0075] The preferred embodiments of the present invention have been described in detail above. However, the present invention is not limited to the specific details in the above embodiments. Within the scope of the technical concept of the present invention, various simple modifications can be made to the technical solution of the present invention, and these simple modifications all fall within the protection scope of the present invention.

[0076] It should also be noted that the various specific technical features described in the above specific embodiments can be combined in any suitable manner without contradiction. In order to avoid unnecessary repetition, the present invention will not describe the various possible combinations separately.

Claims

1. A method for evaluating the spicy note of cigarette smoke, characterized by, The evaluation method includes the following steps: (1) Collect the total particulate matter of the mainstream smoke of typical spicy cigarettes and typical non-spicy cigarettes, and perform GC-MS detection to obtain the content of aroma components in typical spicy cigarettes and typical non-spicy cigarettes. Perform partial least squares discriminant analysis on the content of aroma components to obtain the VIP value of aroma components. (2) Collect the total particulate matter of the mainstream smoke of the cigarette to be tested and perform GC-MS detection to obtain the content of aroma components in the cigarette to be tested; (3) Calculate the spiciness and aroma index Q of the cigarette smoke based on the VIP value of the aroma component obtained in step (1) and the content of the aroma component in the cigarette obtained in step (2), and determine the degree of spiciness and aroma of the cigarette smoke. Steps (1) and (2) are not in any particular order; The aroma-producing components include positively correlated aroma-producing components and negatively correlated aroma-producing components; The positively correlated aroma components include any one or a combination of at least two of terpenoid aroma components, long-chain unsaturated fatty acid methyl esters, and positively correlated ketone aroma components. The negatively correlated aroma components include any one or a combination of at least two of nitrogen-containing heterocyclic aroma components, furan aroma components, and negatively correlated ketone aroma components.

2. The evaluation method according to claim 1, characterized in that, The positively correlated aroma components include a combination of terpenoid aroma components, long-chain unsaturated fatty acid methyl esters, and positively correlated ketone aroma components; Preferably, the negatively correlated aroma components include a combination of nitrogen-containing heterocyclic aroma components, furan aroma components, and negatively correlated ketone aroma components.

3. The evaluation method according to claim 1 or 2, characterized in that, The terpenoid aroma components include neophytadiene; Preferably, the aroma-producing components of the long-chain unsaturated fatty acid methyl esters include methyl linoleate and / or palmitic acid methyl ester. Methyl acetate; Preferably, the positively correlated ketone aroma component includes 3-hydroxy-2-butanone.

4. The evaluation method according to any one of claims 1-3, characterized in that, The nitrogen-containing heterocyclic aroma components include pyridine; Preferably, the furan-type aroma component includes 2-ethylfuran; Preferably, the negatively correlated ketone aroma components include cyclopentanone and / or 3-penten-2-one.

5. The evaluation method according to claim 3 or 4, characterized in that... The aroma-producing components include neophytadiene, methyl linoleate, methyl palmitate, 3-hydroxy-2-butanone, pyridine, 2-ethylfuran, cyclopentanone, and 3-penten-2-one.

6. The evaluation method according to any one of claims 1 to 5, characterized by, In the GC-MS detection, the chromatographic column was HP-5MS.

7. The evaluation method according to any one of claims 1 to 6, characterized by, In the GC-MS detection, the carrier gas flow rate is 0.8-1.2 mL / min.

8. The evaluation method according to any one of claims 1 to 7, characterized by, In the GC-MS detection, the temperature rise procedure is as follows: Start at 40-60℃ and hold for 0.7-1.3 min; then increase to 155-175℃ at a rate of 6-10℃ / min and hold for 1.4-2.4 min; then increase to 255-275℃ at a rate of 6-10℃ / min and hold for 12-16 min.

9. The evaluation method according to any one of claims 1 to 8, characterized by, The formula for calculating the spiciness and aroma index Q in step (3) is as follows: Q = ∑(content of positively correlated aroma component i × VIP) i ) / ∑(content of negatively correlated aroma-producing component j × VIP j ); In the formula, VIP i This represents the VIP value of the positively correlated aroma-producing component i. j This represents the VIP value of the negatively correlated aroma-producing component j.

10. The application of an evaluation method according to any one of claims 1-9 in the evaluation and analysis of cigarette smoke aroma.

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