Evaluation method of spicy note of cigarette smoke and application of evaluation method

Abstract

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

Description

Technical Field

[0001] The invention belongs to the technical field of tobacco analysis, and in particular relates to a method for evaluating the spicy 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. 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 does not fully consider 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, spicy aroma can effectively affect consumers' sensory evaluation of cigarette products, and the evaluation of spicy aroma is particularly important.

[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 spicy 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 shortcomings of the prior art, the purpose of the present invention is to provide an evaluation method for the spicy aroma of cigarette smoke and its application. The evaluation method provided by the present invention can objectively and accurately reflect the spicy 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 spicy aroma of cigarette smoke, which has a positive and important role in the rapid evaluation of the spicy aroma of cigarette smoke and the strengthening of the spicy 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 spicy aroma of cigarette smoke, the method comprising the following steps:

[0007] (1) The total particulate matter in mainstream smoke of typical spicy cigarettes and typical non-spicy cigarettes was captured and tested by GC-MS (gas chromatography-mass spectrometry) to obtain the contents of aroma components in typical spicy cigarettes and typical non-spicy cigarettes, and the contents of aroma components were analyzed by 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 spicy 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 spicy aroma degree 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.

[0012] The positively correlated aroma components include any one or a combination of at least two of terpene aroma components, long-chain unsaturated fatty acid methyl esters and positively correlated ketone aroma components, and 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.

[0013] The above method analyzes the aroma components in typical spicy cigarettes, typical non-spicy cigarettes and the cigarettes to be tested, obtains the VIP value by partial least squares discriminant analysis, and calculates the spicy aroma index Q by combining it with the content of the aroma components. It can objectively and accurately reflect the spicy 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 spicy aroma of cigarette smoke, which plays an active and important role in the rapid evaluation of the spicy aroma of cigarette smoke and the strengthening research of the spicy style of cigarettes.

[0014] Preferably, the positively correlated aroma components include a combination of terpene aroma components, long-chain unsaturated fatty acid methyl esters and positively correlated ketone aroma components.

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

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

[0017] Preferably, the long-chain unsaturated fatty acid methyl ester aroma component includes methyl linolenate and / or methyl palmitate;

[0018] Preferably, the positively correlated ketone aroma component includes 3-hydroxy-2-butanone;

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

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

[0021] Preferably, the negatively correlated ketone aroma components include cyclopentanone and / or 3-penten-2-one.

[0022] The above-mentioned specific aroma component combination can comprehensively and effectively evaluate the spicy aroma of the smoke of the tested cigarette, and effectively improve the accuracy of the evaluation.

[0023] Preferably, in the GC-MS detection, the chromatographic column is HP-5MS.

[0024] Preferably, in the GC-MS detection, the carrier gas flow rate is 0.8-1.2 mL / min, for example 0.8 mL / min, 0.9 mL / min, 1 mL / min, 1.1 mL / min or 1.2 mL / min, but is not limited to the above-listed values, and other values ​​not listed within the above numerical range are also applicable.

[0025] Preferably, in the GC-MS detection, the heating program is as follows:

[0026] The initial temperature is 40-60°C and maintained for 0.7-1.3 min; then the temperature is increased to 155-175°C at a rate of 6-10°C / min and maintained for 1.4-2.4 min; then the temperature is increased to 255-275°C at a rate of 6-10°C / min and maintained for 12-16 min.

[0027] 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.

[0028] Preferably, the calculation formula of the spicy aroma index Q in step (3) is as follows:

[0029] Q = ∑ (content of positively correlated aroma component i × VIP i ) / ∑(content of negatively correlated aroma component j×VIP j );

[0030] 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.

[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 are.

[0032] 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.

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

[0034] The invention provides a method for evaluating the spicy aroma of cigarette smoke. The method comprises the following steps: analyzing aroma components in typical spicy cigarettes, typical non-spicy cigarettes and cigarettes to be tested, obtaining a VIP value by using a partial least squares discriminant analysis, and calculating a spicy aroma index Q by combining the VIP value with the content of the aroma components. The method can objectively and accurately reflect the spicy 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 spicy aroma of cigarette smoke, and play an active and important role in rapidly evaluating the spicy aroma of cigarette smoke and strengthening research on the spicy style of cigarettes. DETAILED DESCRIPTION

[0035] 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.

[0036] Example 1

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

[0038] Fragrance component detection:

[0039] 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.

[0040] 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.

[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; program temperature: 50℃ for 1min, then increase to 165℃ at a rate of 8℃ / min, maintain for 1.9min, then increase to 265℃ at a rate of 8℃ / min, maintain for 14min; 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.

[0043] (1) The above method was used to detect the aroma components of typical spicy and non-spicy 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 terpenes (neophytadiene), long-chain unsaturated fatty acid methyl esters (methyl linolenate, methyl palmitate), ketones (3-hydroxy-2-butanone, cyclopentanone, 3-penten-2-one), nitrogen-containing heterocyclic compounds (pyridine), and furans (2-ethylfuran). See the table below.

[0044]

[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 spicy 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 spicy aroma of the cigarette smoke; using a weighted statistical method to calculate the spicy 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 jThe VIP value of negatively correlated aroma component j is shown in the following table. The positively correlated aroma components are neophytadiene, methyl linolenate, methyl palmitate, and 3-hydroxy-2-butanone, and the negatively correlated aroma components are pyridine, 2-ethylfuran, cyclopentanone, and 3-penten-2-one.

[0052] Sample name Q Value Sample name Q Value Sample name Q Value JP-1 7.16 JP-14 5.00 JP-27 5.84 JP-2 8.35 JP-15 22.09 JP-28 4.51 JP-3 2.49 JP-16 31.01 JP-29 5.03 JP-4 2.95 JP-17 19.23 JP-30 17.88 JP-5 3.88 JP-18 9.00 JP-31 5.30 JP-6 5.97 JP-19 11.54 JP-32 3.20 JP-7 4.63 JP-20 13.98 JP-33 5.45 JP-8 6.04 JP-21 16.52 JP-34 2.97 JP-9 5.41 JP-22 15.34 JP-35 3.66 JP-10 17.76 JP-23 5.61 JP-36 3.19 JP-11 5.18 JP-24 9.28 JP-37 2.71 JP-12 4.66 JP-25 8.27 JP-38 13.42 JP-13 14.39 JP-26 8.87 - -

[0053] (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 and smoking evaluation method was used. 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 spicy aroma of cigarette smoke and can accurately and effectively evaluate the spicy aroma of cigarette smoke.

[0054]

[0055] Example 2

[0056] This embodiment provides a method for evaluating the spicy aroma of cigarette smoke. The specific steps are consistent with those of Example 1 except that the GC-MS analysis conditions are as follows.

[0057] GC-MS analysis conditions:

[0058] 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: 40℃ for 1.3min, increase to 155℃ at a rate of 6℃ / min, maintain for 2.4min, then increase to 255℃ at a rate of 6℃ / min, maintain for 16min; 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.

[0059] Example 3

[0060] This embodiment provides a method for evaluating the spicy aroma of cigarette smoke. The specific steps are consistent with those of Example 1 except that the GC-MS analysis conditions are as follows.

[0061] GC-MS analysis conditions:

[0062] 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; program temperature: 60℃ for 0.7min, then increase to 175℃ at a rate of 10℃ / min, maintain for 1.4min, then increase to 275℃ at a rate of 10℃ / min, maintain for 12min; 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.

[0063] Example 4

[0064] This embodiment provides a method for evaluating the spicy aroma of cigarette smoke. The specific steps are the same as those of Embodiment 1 except that the chromatographic column HP-5MS is replaced by DB-35MS.

[0065] Example 5

[0066] This embodiment provides a method for evaluating the spicy aroma of cigarette smoke. The specific steps are consistent with those of Example 1 except that the heating program is as follows.

[0067] Keep at 70℃ for 1 min, increase the temperature to 210℃ at a rate of 24℃ / min, keep for 1 min, then increase the temperature to 280℃ at a rate of 6℃ / min, and keep for 5 min.

[0068] Example 6

[0069] This embodiment provides a method for evaluating the spicy aroma of cigarette smoke. The specific steps are consistent with those of Example 1 except that the aroma component does not contain neophytadiene.

[0070] Example 7

[0071] This embodiment provides a method for evaluating the spicy aroma of cigarette smoke. The specific steps are consistent with those of Example 1 except that the aroma components do not contain methyl linolenate and methyl palmitate.

[0072] Example 8

[0073] This embodiment provides a method for evaluating the spicy aroma of cigarette smoke. The specific steps are consistent with those of Example 1 except that the aroma components do not contain cyclopentanone and 3-penten-2-one.

[0074] Example 9

[0075] This embodiment provides a method for evaluating the intensity of spicy aroma of cigarette smoke. The specific steps are consistent with those of Example 1 except that the aroma component does not contain pyridine.

[0076] Example 10

[0077] This embodiment provides a method for evaluating the intensity of spicy aroma of cigarette smoke. The specific steps are consistent with those of Embodiment 1 except that the aroma component does not contain 3-hydroxy-2-butanone.

[0078] Effect test:

[0079] Seven groups of cigarette samples with different intensities of spicy aroma 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 Cigarette Sensory Flavors", 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 1-10, and the Q values ​​were calculated. The results are as follows:

[0080]

[0081] From the above results, it can be found that the present invention can more accurately, comprehensively and effectively evaluate the spicy aroma of the cigarette smoke 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.

[0082] The applicant declares that the present invention uses the above-mentioned embodiments to illustrate the evaluation method and application of the spicy 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 various 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.

[0083] 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.

[0084] 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 spicy aroma of cigarette smoke, characterized in that: The evaluation method comprises the following steps: (1) The total particulate matter in mainstream smoke of typical spicy cigarettes and typical non-spicy cigarettes was captured and tested by GC-MS to obtain the contents of aroma components in the typical spicy cigarettes and typical non-spicy 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 spicy 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 spicy aroma degree 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 or a combination of at least two of terpene aroma components, long-chain unsaturated fatty acid methyl esters and positively correlated ketone aroma components, and 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 terpene 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 terpene aroma components include neophytadiene; Preferably, the long-chain unsaturated fatty acid methyl ester aroma component includes methyl linolenate and / or methyl palmitate; Preferably, the positively correlated ketone aroma component includes 3-hydroxy-2-butanone.

4. The evaluation method according to any one of claims 1 to 3, characterized in that: The nitrogen-containing heterocyclic aroma-causing ingredients include pyridine; Preferably, the furan-based 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 components include neophytadiene, methyl linolenate, 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 in that: In the GC-MS detection, the chromatographic column is HP-5MS.

7. The evaluation method according to any one of claims 1 to 6, characterized in that: 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 in that: In the GC-MS detection, the temperature rising program is as follows: The initial temperature is 40-60°C and maintained for 0.7-1.3 min; then the temperature is increased to 155-175°C at a rate of 6-10°C / min and maintained for 1.4-2.4 min; then the temperature is increased to 255-275°C at a rate of 6-10°C / min and maintained for 12-16 min.

9. The evaluation method according to any one of claims 1 to 8, characterized in that: The calculation formula of the spicy 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. Application of the evaluation method according to any one of claims 1 to 9 in the evaluation and analysis of cigarette smoke aroma.

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