Evaluation method for nut note of cigarette smoke and application of evaluation method

Abstract

The invention provides a cigarette smoke nut aroma note evaluation method and application thereof, and the evaluation method comprises the following steps: (1) capturing main stream smoke total particulate matters of typical nut aroma type and non-nut aroma type cigarettes, and carrying out GC-MS detection to obtain the content of aroma components in the main stream smoke total particulate matters; carrying out partial least square discriminant analysis on the content of the aroma component to obtain a VIP value of the aroma component; (2) capturing main stream smoke total particulate matters of the to-be-detected cigarette, and performing GC-MS detection to obtain the content of aroma components in the to-be-detected cigarette; and (3) calculating the aroma index Q of the nut aroma according to the VIP value and the content of aroma components in the to-be-detected cigarette. The evaluation method provided by the invention can objectively and accurately reflect the nut aroma note of the cigarette smoke, avoids the subjective error caused by sensory evaluation and the situation that the analysis result of the tobacco shred aroma component does not correspond to the actual smoking experience, and provides a new method for characterization and evaluation of the nut aroma note of the cigarette smoke.

Description

Technical Field

[0001] The invention belongs to the technical field of tobacco analysis, and in particular relates to an evaluation method for nutty aroma of cigarette smoke and an application thereof. Background Art

[0002] The consumption form of cigarette products by consumers determines that the characteristic aroma of smoke is decisive for the formation of cigarette style, and the characteristic aroma of smoke is one of the most important bases for the construction of product categories. Existing relevant studies have shown that the overall aroma style of cigarettes is mainly formed by the joint action of different characteristic aromas of smoke, and behind each characteristic aroma there is a set of material bases with significant contributions. At present, sensory evaluation is still 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 of material basis, researchers in the industry have characterized the aroma characteristics through indexes based on the aroma components in tobacco shreds, which has a certain positive effect on the evaluation of aroma characteristics, but has not fully considered the migration rate of aroma components from tobacco shreds to smoke, as well as the changes in the types and contents of aroma components during cigarette burning. In particular, the nutty aroma can effectively affect consumers' sensory evaluation of cigarette products, and is particularly important for the evaluation of nutty aroma.

[0003] Therefore, based on the aroma components of cigarette smoke, it is particularly important to use instrumental analysis and detection methods combined with multivariate statistical analysis techniques to identify and extract a group of characteristic aroma components that significantly contribute to the nutty aroma of cigarette smoke from numerous chemical components, so as to objectively and accurately characterize and evaluate the characteristic aroma of cigarette smoke. Summary of the invention

[0004] In view of the deficiencies of the prior art, the purpose of the present invention is to provide an evaluation method for the nutty aroma of cigarette smoke and its application. The evaluation method provided by the present invention can objectively and accurately reflect the nutty aroma of cigarette smoke, avoid the subjective error caused by sensory evaluation and the situation that the analysis results of tobacco aroma components do not correspond to the actual smoking experience, and provide a new method for the characterization and evaluation of the nutty aroma of cigarette smoke, which has a positive and important role in the rapid evaluation of the nutty aroma of cigarette smoke and the strengthening of the nutty aroma style of cigarettes.

[0005] In order to achieve the purpose of the invention, the present invention adopts the following technical solutions:

[0006] In one aspect, the present invention provides a method for evaluating the nutty aroma of cigarette smoke, the method comprising the following steps:

[0007] (1) The total particulate matter in mainstream smoke of typical nut-flavored cigarettes and typical non-nut-flavored cigarettes was captured and tested by GC-MS (gas chromatography-mass spectrometry) to obtain the contents of aroma components in the typical nut-flavored cigarettes and typical non-nut-flavored cigarettes, and the contents of aroma components were subjected to partial least squares discriminant analysis to obtain the VIP values ​​(variable weight values) of the aroma components;

[0008] (2) capturing the total particulate matter in the mainstream smoke of the cigarette to be tested, and performing GC-MS detection to obtain the content of the aroma components in the cigarette to be tested;

[0009] (3) calculating the nutty aroma index Q of the smoke of the cigarette to be tested according to the VIP value of the aroma component in step (1) and the content of the aroma component in the cigarette to be tested obtained in step (2), and determining the degree of nutty aroma of the smoke of the cigarette to be tested;

[0010] There is no order distinction between steps (1) and (2).

[0011] The aroma components include positively correlated aroma components and negatively correlated aroma components. The positively correlated aroma components include any one of phenolic aroma components, ketone aroma components, furan aroma components or pyridine aroma components, or a combination of at least two of them. The negatively correlated aroma components include any one of ester aroma components, fatty acid aroma components or fatty acid ester aroma components, or a combination of at least two of them.

[0012] The above method analyzes the aroma components in typical nut-flavored cigarettes, typical non-nut-flavored cigarettes and the cigarettes to be tested, obtains the VIP value by partial least squares discriminant analysis, and calculates the nutty aroma index Q by combining it with the content of the aroma components. The method can objectively and accurately reflect the nutty aroma of cigarette smoke, avoid the subjective error caused by sensory evaluation and the situation where the analysis results of tobacco aroma components do not correspond to the actual smoking experience, and provide a new method for the characterization and evaluation of the nutty aroma of cigarette smoke, which plays a positive and important role in the rapid evaluation of the nutty aroma of cigarette smoke and the strengthening of the nutty aroma style of cigarettes.

[0013] Preferably, the positively correlated aroma components include a combination of phenolic aroma components, ketone aroma components, furan aroma components and pyridine aroma components.

[0014] Preferably, the negatively correlated aroma components include a combination of ester aroma components, fatty acid aroma components and fatty acid ester aroma components.

[0015] Preferably, the phenolic aroma component includes 2-methoxy-4-methylphenol.

[0016] Preferably, the ketone aroma component includes 3-ethyl-2-hydroxy-2-cyclopentene-1-one.

[0017] Preferably, the furan-based aroma component includes furfuryl alcohol.

[0018] Preferably, the pyridine aroma ingredient includes 3,4-dimethylpyridine.

[0019] Preferably, the ester aroma ingredient includes 2,2,4-trimethyl-1,3-pentanediol diisobutyrate.

[0020] Preferably, the fatty acid aroma component includes palmitic acid.

[0021] Preferably, the fatty acid ester aroma component includes methyl linolenate and / or methyl palmitate.

[0022] Preferably, the aroma ingredients include 2-methoxy-4-methylphenol, 3-ethyl-2-hydroxy-2-cyclopentene-1-one, furfuryl alcohol, 3,4-lutidine, 2,2,4-trimethyl-1,3-pentanediol diisobutyrate, palmitic acid, methyl linolenate and methyl palmitate.

[0023] The above-mentioned combination of specific aroma components can comprehensively and effectively evaluate the nutty aroma of the smoke of the tested cigarette, and effectively improve the accuracy of the evaluation.

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

[0025] Preferably, in the GC-MS detection, the carrier gas flow rate is 0.8-1.0 mL / min, such as 0.8 mL / min, 0.9 mL / min or 1.0 mL / min, but is not limited to the above-listed values, and other values ​​not listed within the above numerical range are also applicable.

[0026] Preferably, in the GC-MS detection, the heating program is as follows:

[0027] Take 45-60℃ as the initial temperature and maintain it for 0.8-1.4min; then increase to 150-180℃ at a rate of 7-10℃ / min and maintain it for 1.5-4.5min; then increase to 225-240℃ at a rate of 7-10℃ / min and maintain it for 14-15min; then increase to 250-270℃ at a rate of 8-10℃ / min and maintain it for 9-10min.

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

[0029] Preferably, the calculation formula of the nutty aroma index Q in step (3) is as follows:

[0030] Q = ∑ (content of positively correlated aroma component i × VIPi ) / ∑(content of negatively correlated aroma component j×VIP j );

[0031] In the formula, VIP i represents the VIP value of the positively correlated aroma component i, VIP j Represents the VIP value of negatively correlated aroma component j.

[0032] In the above formula, the nutty aroma of cigarette smoke is positively correlated with the index Q, that is, the higher the nutty aroma index Q value of the cigarette smoke to be tested, the more obvious the nutty aroma characteristics of the cigarette smoke are.

[0033] On the other hand, the present invention also provides the application of the above-mentioned evaluation method in the evaluation and analysis of cigarette smoke aroma.

[0034] Compared with the prior art, the present invention has the following beneficial effects:

[0035] The invention provides an evaluation method for the nutty aroma of cigarette smoke. The method comprises the following steps: analyzing the aroma components in typical nutty flavor cigarettes, typical non-nutty flavor cigarettes and cigarettes to be tested, obtaining a VIP value by using partial least squares discriminant analysis, and calculating a nutty aroma index Q by combining the VIP value with the content of the aroma components. The method can objectively and accurately reflect the nutty aroma of cigarette smoke, avoid the subjective error caused by sensory evaluation and the situation that the analysis result of tobacco aroma components does not correspond to the actual smoking experience, provide a new method for characterizing and evaluating the nutty aroma of cigarette smoke, and play an active and important role in quickly evaluating the nutty aroma of cigarette smoke and strengthening the research on the nutty aroma style of cigarettes. DETAILED DESCRIPTION

[0036] In order to further explain the technical means and effects adopted by the present invention, the technical solution of the present invention is further described below in conjunction with the preferred embodiments of the present invention, but the present invention is not limited to the scope of the embodiments.

[0037] Example 1

[0038] This embodiment provides a method for evaluating the nutty aroma of cigarette smoke, and the specific steps are as follows:

[0039] Fragrance component detection:

[0040] The total particulate matter in the mainstream smoke of cigarettes was captured according to the national standard GB / T19609-2004 Determination of total particulate matter and tar by conventional analytical smoking machine for cigarettes.

[0041] The captured filter disc was placed in a simultaneous distillation extraction device, and distilled and extracted for 2 hours using dichloromethane as solvent. The obtained extract was dried over anhydrous sodium sulfate, concentrated to 1.0 mL in a rotary evaporator, and 50 μL (0.1 mol / L) of anhydrous ethanol solution of benzyl acetate was added and shaken well for GC-MS analysis.

[0042] GC-MS analysis conditions:

[0043] Chromatographic column: HP-5MS (30m×0.25mm×0.25μm) capillary column; injection port temperature: 240℃; transfer line temperature: 280℃; carrier gas: He, flow rate 0.9mL / min; program temperature: 55℃ for 1.2min, then increase to 170℃ at a rate of 9℃ / min, maintain for 4min, then increase to 230℃ at a rate of 9℃ / min, maintain for 14min, then increase to 260℃ at a rate of 9℃ / min, maintain for 10min; injection volume: 1μL, split ratio: 10:1; EI ionization energy: 70eV; ion source temperature: 230℃; quadrupole temperature: 160℃; mass range: 35~455amu. The NIST17 and Wiley275 standard spectral libraries were used for qualitative retrieval, and the internal standard method was used for quantitative determination of the content of some aroma components.

[0044] (1) The above method was used to detect the aroma components of typical nut-flavored and typical non-nut-flavored cigarettes. The partial least squares discriminant analysis (PLS-DA) was performed using the chemometric statistical software SIMCA 14.1 to calculate the VIP values ​​of the aroma components of phenols (2-methoxy-4-methylphenol), ketones (3-ethyl-2-hydroxy-2-cyclopentene-1-one), furans (furfuryl alcohol), pyridines (3,4-dimethylpyridine), esters (2,2,4-trimethyl-1,3-pentanediol diisobutyrate), fatty acids (palmitic acid) and fatty acid esters (methyl linolenate, methyl palmitate). See the table below.

[0045]

[0046] (2) The above method was used to detect the aroma components of 38 types of cigarettes on the market. The results are shown in the following table.

[0047]

[0048]

[0049] (3) Calculating the nutty aroma index Q of the cigarette smoke corresponding to the 38 types of cigarettes on the market, and using the Q index to reflect the nutty aroma of the cigarette smoke; using a weighted statistical method to calculate the nutty aroma index Q of the cigarette smoke to be tested, the calculation formula is:

[0050] Q = ∑ (content of positively correlated aroma component i × VIP i ) / ∑(content of negatively correlated aroma component j×VIP j );

[0051] In the above formula, VIP i represents the VIP value of the positively correlated aroma component i, VIP j The VIP value of negatively correlated aroma component j is shown in the table below. The positively correlated aroma components are 2,2'-isopropyldi(5-methylfuran), 2,3,6-trimethyl-1,4-naphthalenedione, megastigmatrienone C, and megastigmatrienone D. The negatively correlated aroma components are 2,2,4-trimethyl-1,3-pentanediol diisobutyrate, furfural, furfuryl alcohol, and 4-cyclopentene-1,3-dione.

[0052]

[0053]

[0054] (4) In order to verify that the Q value is closely related to the intensity trend of the nutty aroma of cigarette smoke, a group comparison smoking evaluation method was adopted. 18 groups of samples were randomly selected and distributed according to the Q value of high, medium and low. Each group was divided into No. 1, No. 2 and No. 3. The order of Q value was No. 1> No. 2> No. 3. A smoking evaluation team composed of 12 experts conducted comparative smoking evaluation in accordance with the provisions of "GB5606.4-2005 Technical Requirements for Sensory Evaluation of Cigarettes". The results showed that the conclusions of the 6 groups of smoking evaluations were consistent with their Q value trends (see the table below), indicating that the Q value has applicable value in characterizing and evaluating the nutty aroma of cigarette smoke and can accurately and effectively evaluate the nutty aroma of cigarette smoke.

[0055]

[0056] Example 2

[0057] This example provides a method for evaluating the nutty aroma of cigarette smoke. The specific steps are consistent with those of Example 1 except that the GC-MS analysis conditions are as follows.

[0058] GC-MS analysis conditions:

[0059] 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; program temperature: 45℃ for 1.2min, then increase to 150℃ at a rate of 7℃ / min, maintain for 2.5min, then increase to 250℃ at a rate of 7℃ / min, maintain for 17min; injection volume: 2μL, split ratio: 25:1; EI ionization energy: 70eV; ion source temperature: 230℃; quadrupole temperature: 160℃; mass range: 35~455amu. The NIST17 and Wiley275 standard spectral libraries were used for qualitative retrieval, and the internal standard method was used for quantitative determination of the content of some aroma components.

[0060] Example 3

[0061] This example provides a method for evaluating the nutty aroma of cigarette smoke. The specific steps are consistent with those of Example 1 except that the GC-MS analysis conditions are as follows.

[0062] GC-MS analysis conditions:

[0063] 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; program temperature: 60℃ for 1.4min, then increase to 160℃ at a rate of 8℃ / min, maintain for 3min, then increase to 240℃ at a rate of 10℃ / min, maintain for 15min, then increase to 250℃ at a rate of 8℃ / min, maintain for 9min; injection volume: 1μL, split ratio: 10:1; EI ionization energy: 70eV; ion source temperature: 230℃; quadrupole temperature: 160℃; mass range: 35~455amu. The NIST17 and Wiley275 standard spectral libraries were used for qualitative retrieval, and the internal standard method was used for quantitative determination of the contents of some aroma components.

[0064] Example 4

[0065] This example provides a method for evaluating the nutty aroma of cigarette smoke. The specific steps are the same as those of Example 1 except that the chromatographic column HP-5MS is replaced by DB-35MS.

[0066] Example 5

[0067] This embodiment provides a method for evaluating the nutty aroma of cigarette smoke. The specific steps are consistent with those of Example 1 except that the heating program is as follows.

[0068] Keep at 65℃ for 2 min, increase the temperature to 240℃ at a rate of 20℃ / min, keep it for 8 min, then increase the temperature to 280℃ at a rate of 5℃ / min, keep it for 8 min.

[0069] Example 6

[0070] This embodiment provides a method for evaluating the nutty aroma of cigarette smoke. The specific steps are consistent with those of Example 1 except that the aroma component does not contain 3,4-lutidine.

[0071] Example 7

[0072] This embodiment provides a method for evaluating the nutty aroma of cigarette smoke. The specific steps are consistent with those of Example 1 except that the aroma components do not contain 2-methoxy-4-methylphenol and 3-ethyl-2-hydroxy-2-cyclopentene-1-one.

[0073] Example 8

[0074] This embodiment provides a method for evaluating the nutty aroma of cigarette smoke. The specific steps are consistent with those of Example 1 except that the aroma component does not contain 2,2,4-trimethyl-1,3-pentanediol diisobutyrate.

[0075] Example 9

[0076] This embodiment provides a method for evaluating the intensity of nutty aroma in cigarette smoke. The specific steps are consistent with those in Example 1 except that the aroma components do not contain methyl linolenate and methyl palmitate.

[0077] Example 10

[0078] This embodiment provides a method for evaluating the intensity of nutty aroma in cigarette smoke. The specific steps are consistent with those in Example 1 except that the aroma component does not contain furfuryl alcohol.

[0079] Embodiment 11

[0080] This embodiment provides a method for evaluating the intensity of nutty aroma in cigarette smoke. The specific steps are consistent with those in Example 1 except that the aroma components do not contain palmitic acid.

[0081] Effect test:

[0082] Seven groups of cigarette samples with different intensities of nutty aroma in smoke were taken, and a smoking evaluation panel composed of 12 experts conducted comparative smoking evaluation in accordance with the provisions of "GB5606.4-2005 Technical Requirements for Sensory Flavor of Cigarettes", and determined that the intensity was ranked from small to large as A, B, C, D, E, F, and G. Then, the seven groups of cigarettes were rated using the method provided in Examples 1-11, and the Q value was calculated. The results are as follows:

[0083]

[0084]

[0085] From the above results, it can be found that the present invention can more accurately, comprehensively and effectively evaluate the nutty aroma of the smoke of the cigarette to be tested by controlling specific chromatographic parameters and selecting a specific combination of aroma components, thereby effectively improving the accuracy of the evaluation results.

[0086] The applicant declares that the present invention uses the above-mentioned embodiments to illustrate the evaluation method and application of the nutty aroma of cigarette smoke of the present invention, but the present invention is not limited to the above-mentioned embodiments, that is, it does not mean that the present invention must rely on the above-mentioned embodiments to be implemented. Those skilled in the art should understand that any improvement of the present invention, equivalent replacement of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.

[0087] The preferred embodiments of the present invention are described in detail above. However, the present invention is not limited to the specific details in the above embodiments. Within the technical concept of the present invention, a variety of simple modifications can be made to the technical solution of the present invention, and these simple modifications all belong to the protection scope of the present invention.

[0088] 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 further describe various possible combinations.

Claims

1. A method for evaluating the nutty aroma of cigarette smoke, characterized in that: The evaluation method comprises the following steps: (1) The total particulate matter in mainstream smoke of typical nut-flavored cigarettes and typical non-nut-flavored cigarettes was captured and tested by GC-MS to obtain the contents of aroma components in the typical nut-flavored cigarettes and typical non-nut-flavored cigarettes, and the contents of aroma components were analyzed by partial least squares discriminant analysis to obtain the VIP values ​​of aroma components; (2) capturing the total particulate matter in the mainstream smoke of the cigarette to be tested, and performing GC-MS detection to obtain the content of the aroma components in the cigarette to be tested; (3) calculating the nutty aroma index Q of the smoke of the cigarette to be tested according to the VIP value of the aroma component in step (1) and the content of the aroma component in the cigarette to be tested obtained in step (2), and determining the degree of nutty aroma of the smoke of the cigarette to be tested; Steps (1) and (2) are not sequential; The aroma components include positively correlated aroma components and negatively correlated aroma components. The positively correlated aroma components include any one of phenolic aroma components, ketone aroma components, furan aroma components or pyridine aroma components, or a combination of at least two of them. The negatively correlated aroma components include any one of ester aroma components, fatty acid aroma components or fatty acid ester aroma components, or a combination of at least two of them.

2. The method for evaluating the nutty aroma of cigarette smoke according to claim 1, characterized in that: The positively correlated aroma components include a combination of phenol aroma components, ketone aroma components, furan aroma components and pyridine aroma components; The negatively correlated aroma components include a combination of ester aroma components, fatty acid aroma components and fatty acid ester aroma components.

3. The method for evaluating the nutty aroma of cigarette smoke according to claim 2, characterized in that: The phenolic aroma component includes 2-methoxy-4-methylphenol; The ketone aroma component includes 3-ethyl-2-hydroxy-2-cyclopentene-1-one; The furan-based aroma component includes furfuryl alcohol; The pyridine aroma component includes 3,4-dimethylpyridine.

4. The method for evaluating the nutty aroma of cigarette smoke according to claim 3, characterized in that: The ester aroma component includes 2,2,4-trimethyl-1,3-pentanediol diisobutyrate; The fatty acid aroma component includes palmitic acid; The fatty acid ester aroma component includes methyl linolenate and / or methyl palmitate.

5. The method for evaluating the nutty aroma of cigarette smoke according to claim 4, characterized in that: The aroma ingredients include 2-methoxy-4-methylphenol, 3-ethyl-2-hydroxy-2-cyclopentene-1-one, furfuryl alcohol, 3,4-dimethylpyridine, 2,2,4-trimethyl-1,3-pentanediol diisobutyrate, palmitic acid, methyl linolenate and methyl palmitate.

6. The method for evaluating the nutty aroma of cigarette smoke according to claim 5, characterized in that: In the GC-MS detection, the chromatographic column is HP-5MS.

7. The method for evaluating the nutty aroma of cigarette smoke according to claim 6, characterized in that: In the GC-MS detection, the carrier gas flow rate is 0.8-1.0 mL / min.

8. The method for evaluating the nutty aroma of cigarette smoke according to claim 7, characterized in that: In the GC-MS detection, the temperature rising program is as follows: Take 45-60℃ as the initial temperature and maintain it for 0.8-1.4min; then increase to 150-180℃ at a rate of 7-10℃ / min and maintain it for 1.5-4.5min; then increase to 225-240℃ at a rate of 7-10℃ / min and maintain it for 14-15min; then increase to 250-270℃ at a rate of 8-10℃ / min and maintain it for 9-10min.

9. The method for evaluating the nutty aroma of cigarette smoke according to claim 8, characterized in that: The calculation formula of the nutty aroma index Q in step (3) is as follows: Q = ∑ (content of positively correlated aroma component i × VIP i ) / ∑(content of negatively correlated aroma component j×VIP j ); In the formula, VIP i represents the VIP value of the positively correlated aroma component i, VIP j Represents the VIP value of negatively correlated aroma component j.

10. Use of the method for evaluating nutty aroma of cigarette smoke according to any one of claims 1 to 9 in evaluating and analyzing the aroma of cigarette smoke.

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