Cigarette aroma style evaluation method based on relative odor activity value of rear nasal cavity smoke aroma type

Abstract

The invention discloses a cigarette aroma style evaluation method based on a relative odor activity value of a rear nasal cavity smoke aroma type. The method comprises the following steps: step (1), capturing rear nasal cavity smoke; (2) carrying out GC-MS (Gas Chromatography-Mass Spectrometer) analysis by using a gas chromatograph-mass spectrometer; and step (3), performing relative score on the aroma types. According to the method disclosed by the invention, smoke components which really generate flavor in a real smoking process are obtained through rear nasal cavity smoke trapping, and the trapping is more accurate than that of a conventional Cambridge filter; according to the method, the contribution and influence of different aroma types on the whole aroma style are quantitatively evaluated by classifying the same aroma types and calculating the ROAV value, the subjectivity of relative sensory evaluation is high, the reproducibility is poor, and the method is more objective and good in reproducibility.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of tobacco analysis, and particularly relates to a cigarette aroma style evaluation method based on relative odor activity value of post-nasal cavity smoke aroma type. BACKGROUND

[0002] As a special consumer product, the quality evaluation of cigarettes has been one of the important research directions in the tobacco industry. The traditional cigarette evaluation method mainly relies on sensory evaluation, that is, professional evaluation personnel subjectively evaluate the aroma, taste, aftertaste and the like of cigarettes. However, this method has certain limitations, such as strong subjectivity of the evaluation results and poor repeatability. In recent years, with the development of analysis technology, more and more researches have begun to try to quantify the quality characteristics of cigarettes through smoke chemical analysis means. However, the current commonly used smoke analysis method mainly detects the total particulate matter captured by the Cambridge filter, which has certain differences from the real cigarette smoke. No matter the whole cycle evaluation method (also known as the large cycle) or the local cycle evaluation method (also known as the small cycle), the smoke is finally slowly discharged from the nasal cavity, and the nasal cavity is the only organ for the perception of aroma substances in the smoke. For the aroma of cigarettes, the aroma in the front nasal cavity mainly includes cigarette smell and cigarette mainstream smoke aroma; the post-nasal aroma is the aroma perceived by people from the post-nasal cavity during smoking, which is the main aroma affecting the taste of cigarettes, and therefore, the composition of the post-nasal smoke plays a decisive role in the sensory quality of cigarette products.

[0003] However, the current industry evaluation system for cigarette aroma style still highly depends on traditional sensory evaluation, and there is an obvious blank for the "aroma style evaluation method based on post-nasal smoke composition analysis", which directly restricts the precise development of cigarette aroma style. Therefore, constructing a cigarette aroma style evaluation method based on post-nasal smoke composition analysis has become a key problem to be solved in the current research field of cigarette sensory quality.

[0004] In order to solve the above problems, the present application is proposed. SUMMARY

[0005] The present application aims at the deficiencies of the prior art, and provides a cigarette aroma style evaluation method based on relative odor activity value of post-nasal cavity smoke aroma type, so as to realize objective evaluation of cigarette style.

[0006] The technical scheme of the present application is as follows:

[0007] A cigarette aroma style evaluation method based on relative odor activity value of post-nasal cavity smoke aroma type, comprising the following steps:

[0008] Step (1), post-nasal smoke capture:

[0009] After the portable post-nasal smoke capture device is built and runs stably, the tester smokes the test cigarette, after one puff, quickly covers the nose with the post-nasal capture device, waits for the post-nasal smoke to be exhaled, and then smokes the second puff, and so on until the cigarette is smoked evenly, and then the capture tube is taken out for smoke analysis;

[0010] Step (2), gas chromatography-mass spectrometry (GC-MS) analysis:

[0011] The capture tube obtained in step (1) is extracted and filtered with methanol-chloroform solvent containing an internal standard, and then analyzed by gas chromatography-mass spectrometry (GC-MS) to obtain the content of aroma components.

[0012] Step (3), relative score of aroma type:

[0013] The aroma components detected by gas chromatography-mass spectrometry (GC-MS) in step (2) are searched to obtain their aroma types and calculate their threshold multiples OAV, and the same aroma types are classified and the relative odor activity value ROAV is calculated, which is the relative score of the style characteristics of the cigarette.

[0014] Preferably, in step (1), the number of puffs for one cigarette is not less than 3; the number of cigarettes smoked for each brand is not less than 3; and the number of puffs for each cigarette is consistent.

[0015] Preferably, in step (2), the methanol-chloroform solvent is a mixed solution prepared by mixing 5% by volume of methanol and 95% by volume of chloroform; the extraction process is ultrasonic extraction for 10 min; and the methanol-chloroform solvent is added with 5 ug / ml of deuterated naphthalene as an internal standard for quantitative analysis.

[0016] Preferably, in step (2), the GC analysis conditions are as follows: chromatographic conditions: DB-WAX capillary column (30 m x 250 µm x 0.25 µm), stationary phase: polyethylene glycol-PEG; solvent emptying mode, split ratio 20:1; programmed temperature: initial temperature 40℃, hold for 1 min, increase to 230℃ at 8℃ / min, hold for 5 min.

[0017] Mass spectrometry conditions: GC / MS transfer temperature: 260℃; scan mass range: m / z 35-450; solvent delay 3 min, collection mode: Scan and SIM mode, wherein the SIM scan selects ions 107, 108, 136 (internal standard deuterated naphthalene characteristic ion).

[0018] Preferably, in step (2), the content of each component is calculated according to the following formula:

[0019]

[0020] In the formula, C irepresents the content of the measured aroma component; C0represents the threshold value of the aroma component. i represents the peak area of each aroma component; A0represents the peak area of the internal standard; M0represents the mass of the internal standard substance; M represents the mass of the sample.

[0021] Preferably, in step (2), the final content of the aroma component is the average of multiple detections.

[0022] Preferably, in step (3), the OAV is calculated as follows:

[0023]

[0024] In the formula: C i represents the content of the measured aroma component; C0represents the threshold value of the aroma component.

[0025] Preferably, in step (3), the ROAV is calculated as follows:

[0026]

[0027] In the formula: represents the threshold multiple OAV of the aroma type; represents the OAV of the aroma type with the highest threshold multiple OAV.

[0028] The specific structure, working principle, connection relationship of each component, and operation mode of the portable postnasal smoke capturing device are disclosed in detail in the previously applied Chinese invention patent (Patent No. CN202310358241.2). To simplify the expression of this patent and avoid repetitive descriptions of technical content, any reference to the "portable postnasal smoke capturing device" in this patent directly refers to the corresponding technical solution described in the aforementioned CN202310358241.2 patent. The application of this device in this patent does not exceed the technical scope disclosed in the aforementioned prior patent, and its core function remains consistent with the prior patent. The efficient capture of postnasal smoke can be achieved by referring to the prior patent.

[0029] Compared with the prior art, the present application has the following beneficial effects:

[0030] Relative odor activity value (ROAV) is a quantitative indicator for measuring the contribution of aroma components to the overall aroma. It evaluates the importance of aroma components in aroma by calculating the ratio of the concentration of aroma components to their odor threshold value and the percentage of the total overall aroma. By classifying the same aroma type and calculating ROAV, the contribution and influence of different aroma types on the overall aroma style are quantitatively evaluated, thus being more accurate.

[0031] This invention provides a method for evaluating cigarette aroma style based on the relative odor activity value (ROAV) of posterior nasal smoke. This method obtains the smoke components that actually produce flavor during the actual smoking process through posterior nasal smoke capture, which is more accurate than conventional Cambridge filter capture. This method quantifies the contribution and influence of different aroma types on the overall aroma style by classifying the same aroma type and calculating the relative odor activity value (ROAV). Compared with the subjective nature and poor reproducibility of sensory evaluation, this method is more objective and has better reproducibility. Attached Figure Description

[0032] Figure 1 This is the principal component analysis diagram from Example 2. Detailed Implementation

[0033] The present invention will be further described below through embodiments, but is not limited to these embodiments. Experimental methods not specifically described in the embodiments generally use conventional conditions and conditions described in manuals, or conditions recommended by the manufacturer. The general equipment, materials, reagents, etc., used are all commercially available unless otherwise specified.

[0034] Example 1

[0035] Brand A cigarettes were selected as the test cigarettes. After lighting the cigarette and taking a puff, the tester quickly covered their nose with a retronasal trap. After exhaling the smoke through the nose, they took a second puff, and so on. Each cigarette was inhaled evenly for 5 puffs, and 6 cigarettes were used as parallel samples. After adsorption was completed, the trap was removed and ultrasonically extracted with methanol-chloroform solvent (volume ratio 5:95, internal standard 5ug / ml deuterated naphthalene) for 10 min. After filtration, the samples were analyzed by gas chromatography-mass spectrometry (GC-MS). The GC analysis conditions were as follows: chromatographic conditions: DB-WAX capillary column (30m×250µm×0.25µm), stationary phase: polyethylene glycol-PEG; solvent venting mode, split ratio 20:1; temperature program: initial temperature 40℃, hold for 1 min, increase to 230℃ at 8℃ / min, hold for 5 min. Mass spectrometry conditions: GC / MS transfer temperature: 260℃; scan mass range: m / z 35-450; solvent delay 3 min; acquisition mode: Scan and SIM modes, where the SIM scan selected ions 107, 108, and 136 (characteristic ions of internal standard deuterated naphthalene). The contents of the obtained aroma components were determined by aroma type and calculated by OAV. The results are shown in Table 1.

[0036] Table 1. OAV values ​​of aroma components in the posterior nasal cavity of cigarette A

[0037] Serial Number Aroma components Fragrance Threshold multiple 1 Butyl butyrate 109-21-7 Fruity aroma 47.916675 2 2-n-Pentylfuran 3777-69-3 Fruity aroma 1580.459828 3 Styrene 100-42-5 Ointment Fragrance 286.3247692 4 2-Methylbutyric acid-3-methylbutyl ester 27625-35-0 Fruity aroma 1117.571163 5 Isoamyl isovalerate 2050-01-3 Fruity aroma 10541.665 6 Methylheptenone 110-93-0 Fruity aroma 245.0980882 7 2-Ethylhexyl acetate 103-09-3 Fruity aroma 733.9742308 8 (E,E)-2,4-Heptadienal 4313-03-5 perfume 216.4501948 9 Acetic acid 64-19-7 Sour and fragrant 14.52861616 10 Isooctyl acrylate 103-11-7 Ointment Fragrance 84.7222 11 2-Ethylhexanol 104-76-7 Fruity aroma 311.1111 12 Benzaldehyde 100-52-7 Nutty aroma 71.39675585 13 Propionic acid 79-09-4 Sour and fragrant 4.566210046 14 5-Methylfurfural 620-02-0 Caramelized 3.753754054 15 β-Caryophyllene 87-44-5 Spicy 460.069375 16 γ-Velolactone 108-29-2 Milky aroma 0.9166665 17 γ-Butyrolactone 96-48-0 Milky aroma 0.44444445 18 furfuryl alcohol 98-00-0 Baking aroma 7.592593333 19 Shunba soybean acid 503-64-0 Milky aroma 2.638889 20 Anethole 104-46-1 fennel 2306.320183 21 Phenylacetyl alcohol 60-12-8 Floral fragrance 19.69251901 22 Methyl maltol 118-71-8 Caramelized 11.64874194 23 2-Acetylpyrrole 1072-83-9 Baking aroma 0.957768551 24 Anisaldehyde 123-11-5 fennel 2222.222222 25 2-Pyrrolecarboxaldehyde 1003-29-8 Baking aroma 0.534188 26 N-Methyl-2-pyrrolic carboxaldehyde 1192-58-1 Nutty aroma 240.2402432 27 Megastigmatrienone-1, Nicotinone 13215-88-8 Tobacco Scent 77.5034321 28 Eugenol 97-53-0 Spicy 13935.185 29 Nononoic acid, Yangxiu spherical acid 112-05-0 perfume 4.135802222 30 Megastigmatrienone-2, Nicotinone; 13215-88-8 Tobacco Scent 65.98917073 31 p-Vinylguaiacol 7786-61-0 Spicy 5158.728571 32 Methyl palmitate 112-39-0 perfume 14.02778 33 Ethyl palmitate 628-97-7 perfume 7.36111 34 Megastigmatrienone-4, Nicotinone; 13215-88-8 Tobacco Scent 137.3105682 35 Dihydroactinolone 17092-92-1 Bean aroma 400 36 Acacia acetone 762-29-8 Sweet aroma 666.6667 37 Benzoic acid, benzoic acid 65-85-0 Ointment Fragrance 11.94444 38 5-Hydroxymethylfurfural 67-47-0 Caramelized 0.004166667 39 Ethyl vanillin 121-32-4 Milky aroma 36.11111 40 Vanillin 121-33-5 Milky aroma 47.16981132

[0038] The results after fragrance classification and ROAV calculation are shown in Table 2.

[0039] Table 2 ROAV of back of nose smoke aroma of cigarettes

[0040] Fragrance OAV Fragrance Type Total Value ROAV fragrance total value Spicy 19553.98 100 Fruity aroma 14577.8 74.55155 fennel 4528.542 23.15919 Sweet aroma 666.6667 3.409366 Bean aroma 400 2.045619 Ointment Fragrance 382.9914 1.958637 Nutty aroma 311.637 1.593727 Tobacco Scent 280.8032 1.436041 perfume 241.9749 1.237471 Milky aroma 87.28092 0.446359 Floral fragrance 19.69252 0.100708 Sour and fragrant 19.09483 0.097652 Caramelized 15.40666 0.07879 Baking aroma 9.08455 0.046459

[0041] In order to verify the accuracy of the back of nose aroma ROAV, 20 taste experts were selected, and the standard Y / CT497-2014 "Sensory evaluation method of Chinese cigarette style of cigarette" was used for smoking evaluation, the average value of aroma style score was obtained, and the ROAV value was calculated, and the results are shown in Table 3. As can be seen from the table, the sensory evaluation results and the ROAV value results of the back of nose smoke are small.

[0042] Table 3 ROAV value of sensory evaluation

[0043] Fragrance Average aroma score ROAV fragrance total value Spicy 6.5 100 Fruity aroma 4.80 73.84615385 fennel 1.50 23.07692308 Sweet aroma 0.20 3.076923077 Bean aroma 0.13 2 Ointment Fragrance 0.13 2 Nutty aroma 0.10 1.538461538 Tobacco Scent 0.10 1.538461538 perfume 0.10 1.538461538 Milky aroma 0.05 0.769230769 Floral fragrance 0.05 0.769230769 Sour and fragrant 0.10 1.538461538 Caramelized 0.00 0 Baking aroma 0.00 0

[0044] Example 2

[0045] In order to further verify the effectiveness of the method, the A brand cigarette was also selected as the test cigarette, and the smoke was collected according to the national standard "GB / T19609-2004 Determination of total particulate matter and tar in cigarettes by smoking machine for routine analysis", 5 puffs were smoked for each cigarette, 6 parallel groups were smoked for each group, and the Cambridge collection filter was obtained. The subsequent filter processing method and GC-MS, the obtained aroma component content, the aroma type determination and OAV calculation, and the calculation of the ROAV value, and the results are shown in Table 4.

[0046] Table 4 ROAV value collected by standard method

[0047] Fragrance OAV Fragrance Type Total Value ROAV fragrance total value Spicy 143034.4 100 Fruity aroma 51897.33 36.28311 fennel 44114.65 30.84198 Sweet aroma 1445.667 1.010713 Bean aroma 2732.219 1.910183 Ointment Fragrance 1908.297 1.334153 Nutty aroma 1692.398 1.183211 Tobacco Scent 2307.766 1.613434 perfume 772.1 0.5398 Milky aroma 789.4145 0.551905 Floral fragrance 48.24667 0.033731 Sour and fragrant 120.3874 0.084167 Caramelized 73.63384 0.05148 Baking aroma 95.4831 0.066755

[0048] As can be seen from Table 4, there is a difference in the size of the aroma contribution between the OAV value collected by the standard method and the back of nose smoke, and the OAV value of the standard method is obviously larger than that of the back of nose smoke, which may be caused by the absorption of the oral cavity and respiratory tract of the smoke. In addition, there is a significant difference between the ROAV value of the standard method and the ROAV value of the sensory evaluation. In order to further visualize the difference, the principal component analysis was used to process the ROAV of the back of nose smoke in Example 1, the sensory evaluation and the standard method in Example 2, and the results are shown in Figure 1 The results show that the sensory evaluation and the back of nose smoke completely overlap, which further indicates the accuracy of the back of nose smoke ROAV value evaluation, and indicates that the method can effectively represent the aroma style of the smoke; in addition, the sensory evaluation and the standard method do not overlap and the distance is large, which indicates that the standard method has certain limitations in the evaluation of the aroma style of the smoke.

[0049] The above has made the exemplary description to the present application, should indicate that, in not departing from the core of the present application, any simple change, modification or other field technicians can not spend the equivalent replacement of creative labor falls into the protection scope of the present application.

Claims

1. A method for evaluating the aroma style of a cigarette based on the relative odor activity value of the postnasal smoke aroma type, characterized by, It comprises the following steps: Step (1), the back of the nose smoke capture: After the portable back of the nose smoke capture device is built and runs stably, the tester smokes the test cigarette, after one puff, quickly covers the nose with the back of the nose capture device, waits for the back of the nose smoke to be exhaled, and then smokes the second puff, and so on, until the cigarette is smoked evenly, and the capture tube is taken out for smoke analysis; Step (2), gas chromatography-mass spectrometry GC-MS analysis: The capture tube obtained in step (1) is extracted and filtered with methanol-chloroform solvent containing an internal standard, and then analyzed by gas chromatography-mass spectrometry GC-MS detection to obtain the content of aroma components; Step (3), relative score of flavor type: The aroma components detected by gas chromatography-mass spectrometry GC-MS in step (2) are searched to obtain their flavor types and calculate their threshold multiple OAV, and the same flavor types are classified and the relative odor activity value ROAV is calculated, which is the relative score of the style characteristics of the cigarette.

2. The method of claim 1, wherein, In step (1), the number of puffs for a cigarette is not less than 3 times; the number of cigarettes smoked for each brand is not less than 3; and the number of puffs for each cigarette is consistent.

3. The method of claim 1, wherein, In step (2), the methanol-chloroform solvent is a mixed solution prepared by mixing 5% by volume of methanol and 95% by volume of chloroform; the extraction process is 10 min of ultrasonic extraction; and the methanol-chloroform solvent is added with 5 ug / ml of deuterated naphthalene as an internal standard for quantitative analysis.

4. The method of claim 1, wherein, In step (2), the GC analysis conditions are: chromatographic conditions: DB-WAX capillary column, stationary phase: polyethylene glycol-PEG; solvent emptying mode, split ratio 20:1; programmed temperature: initial temperature 40℃, hold for 1 min, increase to 230℃ at 8℃ / min, hold for 5 min; Mass spectrometry conditions: GC / MS transmission temperature: 260℃; scanning mass range: m / z 35-450; solvent delay 3 min, collection mode: Scan and SIM mode, wherein the SIM scan selects ions 107, 108, 136.

5. The method of claim 1, wherein, In step (2), the content of each component is calculated as follows: wherein: C i represents the content of the measured aroma component; A i is the peak area of each aroma component; A0 represents the peak area of the internal standard; M0 represents the mass of the internal standard substance; and M is the mass of the sample.

6. The method of claim 1, wherein, In step (2), the final aroma component content is the average value of multiple detections.

7. The method of claim 1, wherein, In step (3), OAV calculation: wherein: C i represents the content of the measured aroma component; Co is the threshold value of the aroma component.

8. The method of claim 1, wherein, In step (3), ROAV calculation: in which: OAVmax represents the OAV of the most odorant odorant of the odorants; OAVmax represents the OAV of the most odorant odorant of the odorants;

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