Method for evaluating woody aroma of cigarette smoke and application thereof

Abstract

The application provides a method for evaluating the woody aroma of cigarette smoke and application thereof, and the method comprises the following steps: (1) capturing the total particulate matter of the mainstream smoke of typical woody type and non-woody type cigarettes, performing GC-MS detection, obtaining the content of aroma components, and performing partial least squares discriminant analysis on the content of aroma components to obtain the VIP value of the aroma components; (2) capturing the total particulate matter of the mainstream smoke of the to-be-tested cigarette, performing GC-MS detection, and obtaining the content of aroma components in the to-be-tested cigarette; (3) calculating the woody aroma index Q according to the VIP value and the content of aroma components in the to-be-tested cigarette. The evaluation method provided by the application can objectively and accurately reflect the woody aroma of cigarette smoke, avoids subjective errors caused by sensory evaluation, and avoids the situation that the analysis results of tobacco aroma components do not correspond to the actual smoking experience, thereby providing a new method for characterizing and evaluating the woody aroma of cigarette smoke.

Description

Technical Field

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

[0002] Consumers' consumption patterns of cigarette products determine the decisive significance of smoke characteristics and aroma in the formation of cigarette style, making these characteristics 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 effect of different smoke characteristics, and each characteristic is underpinned by a set of material bases that make significant contributions. Currently, sensory evaluation remains the core of the characteristic aroma evaluation system, but this method lacks objective data support and is time-consuming and labor-intensive to implement. At the molecular level, industry researchers have characterized aroma characteristics using indices based on aroma-producing components in tobacco, which has a certain positive effect on aroma characteristic evaluation, 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. Woody aromas, in particular, can effectively influence consumers' sensory evaluation of cigarette products, making their evaluation especially important.

[0003] Therefore, it is particularly important to identify and extract a set of characteristic aroma components that significantly contribute to the woody aroma 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. Summary of the Invention

[0004] To address the shortcomings of existing technologies, the present invention aims to provide a method for evaluating the woody aroma of cigarette smoke and its application. The evaluation method provided by this invention can objectively and accurately reflect the woody 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 woody aroma of cigarette smoke, and plays a positive and important role in the rapid evaluation of the woody aroma of cigarette smoke and in the enhanced research on the woody style of cigarettes.

[0005] To achieve this objective, the present invention adopts the following technical solution:

[0006] On the one hand, the present invention provides a method for evaluating the woody aroma of cigarette smoke, the evaluation method comprising the following steps:

[0007] (1) Collect the total particulate matter of the mainstream smoke of typical wood-scented cigarettes and typical non-wood-scented cigarettes, and perform GC-MS (gas chromatography-mass spectrometry) to obtain the content of aroma components in typical wood-scented cigarettes and typical non-wood-scented cigarettes. Perform partial least squares discriminant analysis on the content of aroma components to obtain the VIP value (variable weight value) of aroma components.

[0008] (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;

[0009] (3) Calculate the woody 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 woody aroma in the cigarette smoke.

[0010] Steps (1) and (2) are not in any particular order.

[0011] The aroma-producing components include positively correlated aroma-producing components and negatively correlated aroma-producing components;

[0012] The positively correlated aroma components include any one or a combination of at least two of the following: terpenoid aroma components, positively correlated ketone aroma components, or positively correlated phenolic aroma components. The negatively correlated aroma components include any one or a combination of at least two of the following: nitrogen-containing heterocyclic aroma components, furan aroma components, negatively correlated ketone aroma components, or negatively correlated phenolic aroma components.

[0013] The above method analyzes the aroma components in typical woody cigarettes, typical non-woody cigarettes, and the cigarettes under test. It uses partial least squares discriminant analysis to obtain the VIP value, and combines it with the content of aroma components to calculate the woody aroma index Q. This method can objectively and accurately reflect the woody 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 woody aroma of cigarette smoke, and plays a positive and important role in the rapid evaluation of the woody aroma of cigarette smoke and the enhanced research on the woody style of cigarettes.

[0014] Preferably, the positively correlated aroma components include a combination of terpenoid aroma components, positively correlated ketone aroma components, and positively correlated phenolic aroma components;

[0015] Preferably, the negatively correlated aroma components include a combination of nitrogen heterocyclic aroma components, furan aroma components, negatively correlated ketone aroma components, and negatively correlated phenolic aroma components.

[0016] Preferably, the terpenoid aroma component includes neophytadiene;

[0017] Preferably, the positively correlated ketone aroma components include solanone and / or 2,3-dihydro-1H-indanone;

[0018] Preferably, the positively correlated phenolic aroma components include 3-ethyl-5-methyl-phenol;

[0019] Preferably, the nitrogen-containing heterocyclic aroma component includes pyridine;

[0020] Preferably, the furan-type aroma component includes 2-ethylfuran;

[0021] Preferably, the negatively correlated ketone aroma component includes 1-hydroxy-2-butanone;

[0022] Preferably, the negatively correlated phenolic aroma components include eugenol;

[0023] Preferably, the aroma-producing components include neophytadiene, solanone, 2,3-dihydro-1H-indone, 3-ethyl-5-methylphenol, pyridine, 2-ethylfuran, 1-hydroxy-2-butanone, and eugenol;

[0024] The aforementioned specific aroma-producing components can comprehensively and effectively evaluate the woody aroma of the cigarette smoke being tested, thus effectively improving the accuracy of the evaluation.

[0025] Preferably, in the GC-MS detection, the chromatographic column is an HP-5MS.

[0026] Preferably, in the GC-MS detection, the carrier gas flow rate is 1.0-1.2 mL / min, such as 1 mL / min, 1.1 mL / min or 1.2 mL / min, but not limited to the values ​​listed above. Other values ​​not listed in the above range are also applicable.

[0027] Preferably, in the GC-MS detection, the temperature rise procedure is as follows:

[0028] Start at 50-60℃ and hold for 1.0-1.4 min; then increase to 160-180℃ at a rate of 8-10℃ / min and hold for 3-4.5 min; then increase to 220-240℃ at a rate of 8-10℃ / min and hold for 13-15 min; then increase to 250-270℃ at a rate of 8-10℃ / min and hold for 9-10 min.

[0029] 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.

[0030] Preferably, the formula for calculating the woody aroma index Q in step (3) is as follows:

[0031] Q = ∑(content of positively correlated aroma component i × VIP) i ) / ∑(content of negatively correlated aroma-producing component j × VIP j );

[0032] 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.

[0033] In the above formula, the woody aroma of cigarette smoke is positively correlated with the index Q. That is, the higher the woody aroma index Q value of the cigarette smoke to be tested, the more obvious the woody aroma characteristics of the cigarette smoke.

[0034] 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.

[0035] Compared with the prior art, the present invention has the following beneficial effects:

[0036] This invention provides a method for evaluating the woody aroma of cigarette smoke. By analyzing the aroma components in typical woody cigarettes, typical non-woody 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 woody aroma index Q. This method can objectively and accurately reflect the woody aroma 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 woody aroma of cigarette smoke, and plays a positive and important role in the rapid evaluation of the woody aroma of cigarette smoke and the enhanced research on the woody style of cigarettes. Detailed Implementation

[0037] 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.

[0038] Example 1

[0039] This embodiment provides a method for evaluating the woody aroma and flavor of cigarette smoke, and the specific steps are as follows:

[0040] Fragrance component analysis:

[0041] 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".

[0042] 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.

[0043] GC-MS analysis conditions:

[0044] Chromatographic column: HP-5MS (30m × 0.25mm × 0.25μm) capillary column; injection port temperature: 240℃; transfer line temperature: 280℃; carrier gas: He, flow rate 1.1mL / min; temperature program: 55℃ for 1.2min, increased to 170℃ at 9℃ / min, held for 4min, increased to 230℃ at 9℃ / min, held for 14min, increased to 260℃ at 9℃ / min, held for 10min; injection volume: 1μL, split ratio: 10:1; 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.

[0045] (1) The aroma components of typical woody and non-woody 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 the aroma components neophytadiene, solanone, 2,3-dihydro-1H-indone, 3-ethyl-5-methylphenol, pyridine, 2-ethylfuran, 1-hydroxy-2-butanone, and eugenol. The results are shown in the table below.

[0046] Fragrance ingredients VIP value Neophytadiene 1.275 Solanone 1.285 3-Ethyl-5-methylphenol 1.125 2,3-Dihydro-1H-indanone 1.317 1-Hydroxy-2-Butanone 1.506 Eugenol 1.541 Pyridine 1.544 2-Ethylfuran 1.579

[0047] (2) The aroma components of 38 commercially available cigarettes were tested using the above method, and the results are shown in the table below.

[0048]

[0049]

[0050] (3) Calculate the woody aroma index Q of the cigarette smoke of the above 38 commercially available cigarettes. The Q index reflects the woody aroma of the cigarette smoke. The woody aroma index Q of the cigarette smoke to be tested is calculated using a weighted statistical method. The calculation formula is as follows:

[0051] Q = ∑(content of positively correlated aroma component i × VIP) i ) / ∑(content of negatively correlated aroma-producing component j × VIPj );

[0052] 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, solanone, 2,3-dihydro-1H-indone, and 3-ethyl-5-methylphenol. The negatively correlated aroma components are pyridine, 2-ethylfuran, 1-hydroxy-2-butanone, and eugenol.

[0053] The results are shown in the table below.

[0054] Sample Name Q value Sample Name Q value Sample Name Q value JP-1 5.61 JP-14 4.07 JP-27 2.25 JP-2 6.00 JP-15 12.74 JP-28 2.15 JP-3 2.24 JP-16 12.02 JP-29 5.18 JP-4 2.20 JP-17 17.62 JP-30 12.77 JP-5 3.40 JP-18 2.15 JP-31 8.31 JP-6 4.61 JP-19 11.24 JP-32 2.10 JP-7 3.73 JP-20 9.14 JP-33 4.66 JP-8 4.81 JP-21 10.47 JP-34 3.31 JP-9 4.88 JP-22 10.72 JP-35 2.29 JP-10 0.66 JP-23 2.62 JP-36 3.30 JP-11 4.41 JP-24 4.02 JP-37 3.18 JP-12 3.80 JP-25 2.86 JP-38 9.12 JP-13 12.80 JP-26 3.59

[0055] (4) In order to verify that the Q value is closely related to the intensity trend of the woody aroma of cigarette smoke, a group comparison evaluation method was adopted. 18 groups of samples were randomly selected and distributed according to 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 woody aroma of cigarette smoke and can accurately and effectively evaluate the woody aroma of cigarette smoke.

[0056]

[0057] Example 2

[0058] This embodiment provides a method for evaluating the woody aroma and flavor of cigarette smoke. Except for the GC-MS analysis conditions, the specific steps are the same as in Example 1.

[0059] GC-MS analysis conditions:

[0060] 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 180℃ at a rate of 10℃ / min, hold for 4.5 min, increase to 220℃ at a rate of 8℃ / min, hold for 13 min, increase to 270℃ at a rate of 8℃ / min, hold for 10 min; injection volume: 1μL, split ratio: 10:1; 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.

[0061] Example 3

[0062] This embodiment provides a method for evaluating the woody aroma and flavor of cigarette smoke. Except for the GC-MS analysis conditions, the specific steps are the same as in Example 1.

[0063] GC-MS analysis conditions:

[0064] 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: 60℃ for 1.4min, increased to 160℃ at 8℃ / min, held for 3min, increased to 240℃ at 10℃ / min, held for 15min, increased to 250℃ at 8℃ / min, held for 9min; injection volume: 1μL, split ratio: 10:1; 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.

[0065] Example 4

[0066] This embodiment provides a method for evaluating the woody 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.

[0067] Example 5

[0068] This embodiment provides a method for evaluating the woody aroma of cigarette smoke. Except for the heating procedure, the specific steps are the same as in Embodiment 1.

[0069] Hold at 60℃ for 2 min, then increase the temperature to 240℃ at a rate of 20℃ / min, hold for 8 min, and then increase the temperature to 280℃ at a rate of 5℃ / min, hold for 8 min.

[0070] Example 6

[0071] This embodiment provides a method for evaluating the woody aroma of cigarette smoke. The specific steps are the same as in Example 1, except that the aroma-producing components do not contain neophytadiene.

[0072] Example 7

[0073] This embodiment provides a method for evaluating the woody aroma of cigarette smoke. The specific steps are the same as in Example 1, except that the aroma-producing components do not contain solanone and 2,3-dihydro-1H-indene.

[0074] Example 8

[0075] This embodiment provides a method for evaluating the woody aroma of cigarette smoke. The specific steps are the same as in Example 1, except that the aroma-causing components do not contain 1-hydroxy-2-butanone.

[0076] Example 9

[0077] This embodiment provides a method for evaluating the intensity of the woody aroma in cigarette smoke. The specific steps are the same as in Example 1, except that the aroma-causing components do not contain eugenol.

[0078] Example 10

[0079] This embodiment provides a method for evaluating the intensity of the woody aroma in cigarette smoke. The specific steps are the same as in Example 1, except that the aroma-causing components do not contain 3-ethyl-5-methyl-phenol.

[0080] Example 11

[0081] This embodiment provides a method for evaluating the intensity of the woody aroma in cigarette smoke. The specific steps are the same as in Example 1, except that the aroma-causing components do not contain 2-ethylfuran.

[0082] Example 12

[0083] This embodiment provides a method for evaluating the intensity of woody aroma in cigarette smoke. The specific steps are the same as in Example 1, except that the aroma-causing components do not contain pyridine.

[0084] Effect test:

[0085] Seven additional cigarette samples with different intensities of woody aroma in their smoke were evaluated by a panel of 12 experts according to the "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 graded using the methods provided in Examples 1-12, and the Q-values ​​were calculated. The results are as follows:

[0086]

[0087]

[0088] The results above show that by controlling specific chromatographic parameters and selecting specific aroma-producing component combinations, this invention can more accurately, comprehensively, and effectively evaluate the woody aroma of cigarette smoke, thus effectively improving the accuracy of the evaluation results.

[0089] The applicant declares that this invention illustrates the method for evaluating the woody aroma 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, additions of auxiliary components, and selection of specific methods, etc., all fall within the protection and disclosure scope of this invention.

[0090] 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.

[0091] 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 woody aroma and flavor of cigarette smoke, characterized in that, The evaluation method includes the following steps: (1) Collect the total particulate matter of the mainstream smoke of typical wood-scented cigarettes and typical non-wood-scented cigarettes, and perform GC-MS detection to obtain the content of aroma components in typical wood-scented cigarettes and typical non-wood-scented 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 woody 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 woody aroma in 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, positively correlated ketone aroma components, or positively correlated phenolic 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, negatively correlated ketone aroma components, or negatively correlated phenolic aroma components. The terpenoid aroma components include neophytadiene; the positively correlated ketone aroma components include solanone and / or 2,3-dihydro-1H-indan-1-one; the positively correlated phenolic aroma components include 3-ethyl-5-methylphenol; The nitrogen-containing heterocyclic aroma components include pyridine; the furan aroma components include 2-ethylfuran; the negatively correlated ketone aroma components include 1-hydroxy-2-butanone; and the negatively correlated phenolic aroma components include eugenol.

2. The evaluation method according to claim 1, characterized in that, The aroma-producing components include neophytadiene, solanone, 2,3-dihydro-1H-indone, 3-ethyl-5-methylphenol, pyridine, 2-ethylfuran, 1-hydroxy-2-butanone, and eugenol.

3. The evaluation method according to claim 1, characterized in that, In the GC-MS detection, the chromatographic column was HP-5MS.

4. The evaluation method according to claim 1, characterized in that, In the GC-MS detection, the carrier gas flow rate is 1.0-1.2 mL / min.

5. The evaluation method according to claim 1, characterized in that, The temperature rise procedure for the GC-MS detection is as follows: Start at 50-60℃ and hold for 1.0-1.4 min; then increase to 160-180℃ at a rate of 8-10℃ / min and hold for 3-4.5 min; then increase to 220-240℃ at a rate of 8-10℃ / min and hold for 13-15 min; then increase to 250-270℃ at a rate of 8-10℃ / min and hold for 9-10 min.

6. The evaluation method according to claim 1, characterized in that, The formula for calculating the woody 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.

7. The application of an evaluation method according to any one of claims 1-6 in the evaluation and analysis of cigarette smoke aroma.

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