A method for simulating the puffing process of heated cigarettes and its application

Abstract

This invention discloses a method for simulating the puff-by-puff process of heated cigarettes, belonging to the field of tobacco quality evaluation technology. It employs a headspace CTC sampler to simulate the puff-by-puff process. First, heated cigarette tobacco is placed in a sampling bottle. Then, the heating device is activated, the sampling bottle is removed from the sample tray and placed into the heating device. After heating is complete, the sampling bottle is immediately removed, the cap is opened, and after the smoke in the sampling bottle has naturally evaporated, the cap is closed again, and the sampling bottle is placed back into the heating device. This simulates the process of taking one puff of heated cigarette. Repeating this process multiple times simulates the process of taking multiple puffs of heated cigarettes. This simulation method avoids the loss of smoke components caused by cumbersome procedures, exhibits good consistency with the puff-by-puff process obtained by traditional methods, and demonstrates high fidelity in simulating the release behavior of smoke components. Using this method to replace traditional methods for evaluating the release behavior of flavoring ingredients in the puff-by-puff smoke of heated cigarettes is simple, time-saving, and labor-saving.

Description

Technical Field

[0001] This invention belongs to the field of tobacco quality evaluation technology, specifically relating to a method for simulating the puffing process of heated cigarettes and its application in evaluating the gas release behavior of puffing heated cigarettes. Background Technology

[0002] Heated cigarettes produce aerosols through heating and distillation, resulting in significant differences in their smoke generation method, smoke-generating medium, and aerosol composition compared to traditional cigarettes. During consumption, the tobacco materials in heated cigarettes are exposed to a lower ambient temperature, generally below 500℃, and the smoke is primarily produced through the pyrolysis of the tobacco materials. Added flavorings are a crucial component of heated cigarette development. Due to their unique heating and release method, the amount and application of flavorings differ significantly from those in traditional cigarettes. The effects and aroma migration behaviors of flavoring substances also vary under different heat sources and heating temperatures in heated cigarettes. Furthermore, the uniformity of flavoring release per puff differs considerably between heated and traditional cigarettes.

[0003] In the analysis of puff-by-puff emissions from novel tobacco products, Han Jingmei et al. studied the puff-by-puff release patterns of key components in e-cigarette aerosols, finding a correlation between the puff-by-puff release amounts of nicotine, glycerol, and propylene glycol and the puff sequence. Wang Le et al., to reveal the temperature distribution and puff-by-puff release patterns of key components in electrically heated cigarettes, analyzed and tested the temperature distribution of the cigarette core and the puff-by-puff residual amounts of key components under different puffing modes, while also detecting and characterizing the volume average temperature and three-dimensional temperature field within the cigarette core. Han Jingmei et al. used electrically heated tobacco products with different lengths of filter tips containing hollow sections, polylactic acid sections, and cellulose acetate sections as research objects, detecting the puff-by-puff release amounts of the main smoke components nicotine, propylene glycol, and glycerol, and analyzing the relative puff-by-puff release amounts and mass fractions of the release amounts. These studies mainly used Cambridge filters to capture smoke, followed by pretreatment and instrumental analysis; the entire experimental process was cumbersome, time-consuming, and labor-intensive. To investigate the changes in the puff-by-puff release of major components in heated cigarette smoke, Gong Shuguo et al. used IQOS and GLO heated cigarettes with two different heating methods as research objects. They modified a rotary smoking machine to achieve puff-by-puff inhalation and smoke capture, established methods for detecting glycerol, nicotine, moisture, and major aroma substances in the smoke, and analyzed the changes in the puff-by-puff release of major components in IQOS and GLO smoke under two modes: Canadian High Cigarette Inhalation (HCI) and ISO standard inhalation. Because using a modified rotary or linear smoking machine to achieve puff-by-puff inhalation and smoke capture of heated cigarettes involves a long inhalation process, and requires sample pretreatment and instrumental analysis of particulate and gaseous substances, it is not only time-consuming and labor-intensive, but also involves numerous steps. Furthermore, the smoke disperses in the air during inhalation, which can easily lead to experimental errors.

[0004] CN105467025A discloses a method for simulating the low-temperature cigarette heating process using pyrolysis and characterizing the smoke using gas chromatography-mass spectrometry (GC-MS). This method involves 8-12 pyrolysis cycles at the same pyrolysis temperature, with each cycle lasting 2-4 seconds, and is relatively complex. CN111965290A discloses a method for analyzing fresh smoke from tobacco products, which involves directly collecting the smoke and then cooling it. However, the smoke disperses into the air during inhalation, which can easily lead to experimental errors. Summary of the Invention

[0005] To address the shortcomings of existing technologies, the present invention aims to provide a simple and feasible method to simulate the puffing process of heated cigarettes, in order to evaluate the gas release behavior of puffing heated cigarettes.

[0006] This invention provides a method for simulating the puff-by-puff process of heated cigarettes, using a headspace CTC sampler to simulate the process, comprising the following steps:

[0007] S1. Place the heated cigarette tobacco in the sampling bottle, cover the bottle cap and set aside, then start the heating device to preheat;

[0008] S2. Place the sampling bottle into the heating device. After heating for a specific time, start the CTC sampler to inject the smoke from the sampling bottle into the GC / MS detector for detection. Immediately after injection, remove the sampling bottle, open the cap, and wait for the smoke in the sampling bottle to dissipate for a period of time. Then, close the cap again and place the bottle back into the heating device for reheating. Repeat this process a specific number of times to simulate the process of smoking a heated cigarette puff by puff.

[0009] Preferably, in step S2, the heating time is 2 to 3 minutes and the heating temperature is 130 to 140°C.

[0010] More preferably, in step S2, the heating time is 2 minutes and the heating temperature is 140°C.

[0011] Preferably, in step S2, the natural evaporation time of the flue gas is 1 minute.

[0012] Another aspect of the present invention provides a method for evaluating the gas release behavior of heated cigarettes in puff-by-puff, which uses a headspace CTC sampler to simulate the smoking process of heated cigarettes, and includes the following steps:

[0013] P1. Using a headspace CTC sampling system, the sampling bottle is a headspace bottle, the tobacco shreds to be tested in the headspace bottle are heated to continuously generate smoke; the tobacco shreds to be tested contain the flavoring raw materials to be tested;

[0014] P2. Using a headspace CTC sampling system, the flue gas generated in step P1 is directly introduced into a gas chromatography-mass spectrometry (GC / MS) instrument for analysis to determine the content of specific fragrance raw materials in the flue gas; GC / MS spectra are obtained and chromatograms are integrated; the release change curve of specific fragrance raw materials is plotted with the peak area of ​​specific fragrance raw materials as the ordinate and the number of suction ports as the abscissa.

[0015] P3. The peak area of ​​the specific fragrance ingredient in each aspiration is compared with the peak area obtained by detecting the same fragrance ingredient using traditional methods. The correlation coefficient is calculated to evaluate the correlation between the two methods and to determine the consistency of the detection conclusions. The formula for calculating the correlation coefficient is as follows:

[0016] ;

[0017] in, The peak area of ​​the specific fragrance ingredient obtained for each extraction using steps P1 and P2. For all suction counts The average value; This refers to the peak area of ​​a specific fragrance ingredient obtained per inhalation using traditional methods. For all suction counts The average value.

[0018] Traditional methods for detecting cigarette smoke emission behavior involve injecting a prepared flavoring solution into unflavored heated cigarettes, inhaling the smoke according to ISO 3308 standards, collecting the smoke using Cambridge filters, then extracting it with ethanol via ultrasonication, centrifuging, and finally analyzing the supernatant using GC / MS. This process is complex and cumbersome, requiring a large number of personnel to monitor the entire process when conducting large-scale cigarette testing. While the results are relatively accurate, the method is slow, inefficient, and consumes significant human and material resources.

[0019] The traditional method for detecting the release behavior of cigarette smoke is as follows: (1) Inject the flavoring raw material solution into unflavored heated cigarettes. The smoking scheme adopts the ISO3308 standard. The first Cambridge filter collects the first puff of smoke from several (e.g., 20) heated cigarettes. The second Cambridge filter collects the second puff of smoke from these heated cigarettes. This process continues until the sixth Cambridge filter collects the sixth puff of smoke from these heated cigarettes. (2) Invert the six Cambridge filters that have been smoked into a 50mL conical flask. Place the wiped cotton into the conical flask as well. Add 20mL of anhydrous ethanol and sonicate at 40℃ and 100W for 40min. After standing for 5min, take the supernatant and filter it with a 0.45μm organic filter membrane. Take 1.5mL of the filtrate into a 2mL brown chromatographic bottle for GC / MS analysis.

[0020] The GC / MS instrument analysis conditions for the above traditional detection methods are as follows: (1) Gas chromatography conditions are as follows: injection port temperature, 250℃; carrier gas, helium; column flow rate, constant flow 1ml / min; injection volume, 1μl; split injection, split ratio 10:1; temperature program, initial temperature 50℃, hold for 2min, then increase to 280℃ at a rate of 8℃ / min, hold for 25min; (2) Mass spectrometry conditions are as follows: electron impact source EI; transfer line temperature, 280℃; ion source temperature, 230℃; ionization energy, 70eV; solvent delay, 7min; scanning mode is full scan mode, scanning mass range 33-400amu.

[0021] The method for evaluating the smoke release behavior of heated cigarettes provided by this invention completely omits the processes of smoking heated cigarettes with a smoking machine and collecting smoke for ethanol extraction, filtration, and centrifugation. It integrates the smoke collection, sampling, and GC / MS detection processes using a headspace CTC sampling system. By directly heating the heated cigarette in the sampling bottle using a heating device, the generated smoke is directly introduced into the GC / MS analyzer through the headspace CTC sampling system for detection. The entire detection process of this invention can be completed by only one person. Apart from a simple operation during the weighing and placement of the heated cigarette tobacco, almost no human intervention is required; only the final experimental data needs to be recorded. The time required by traditional methods (approximately 18-20 hours) is drastically reduced to approximately 8 hours to obtain the test results.

[0022] In the release change curve of the fragrance raw material to be tested obtained by the method of the present invention, the peak area of ​​the fragrance raw material to be tested in each smoke and its average value for all times are selected. At the same time, the peak area of ​​the fragrance raw material to be tested according to the conventional method and its average value for all times are selected. The accuracy of the data obtained by the method of the present invention is calculated according to the above formula, that is, the consistency with the conventional method, to determine whether it can be used to detect the release behavior of a certain fragrance raw material to be tested.

[0023] Preferably, the flavoring ingredient is one or more of menthol, menthyl succinate, ethyl levulinate, γ-heptanol, ethyl phenylacetate, and ethyl cinnamate. When the flavoring ingredient is one of these substances, the detection method of the present invention is consistent with the detection results of traditional methods, meaning that the method of the present invention can completely replace traditional methods and accurately detect the release behavior of the above-mentioned flavoring ingredients in heated cigarette tobacco.

[0024] More preferably, the flavoring material is menthol and menthyl succinate in a weight ratio of (0.25-4):1, and the weight of the flavoring material is 0.05-1% of the heated cigarette. For example, conventionally, the amount of menthol can be selected as 0.05-0.1% of the total weight of the heated cigarette, and the amount of menthyl succinate can be selected as 0.15-0.2% of the total weight of the heated cigarette.

[0025] Preferably, in step P2, the heating time is 2-3 minutes, the heating temperature is 130-140°C, the temperature of the injection needle is 135-145°C, and the injection volume is 1 μl.

[0026] More preferably, in step P2, the heating time is 2 minutes, the heating temperature is 140°C, and the temperature of the injection needle is 145°C.

[0027] Preferably, in step P3, the natural evaporation time of the flue gas is 1 minute.

[0028] Preferably, in step P2, the gas chromatography conditions for analysis by the gas chromatography-mass spectrometry instrument are as follows: injection port temperature, 250℃; carrier gas, helium; column flow rate, constant flow 1 ml / min; injection volume, 1 μl; split injection, split ratio 10:1; temperature program, initial temperature 50℃, hold for 2 min, then increase to 280℃ at a rate of 8℃ / min, hold for 25 min;

[0029] The mass spectrometry conditions were as follows: electron impact source (EI); transfer line temperature, 280℃; ion source temperature, 230℃; ionization energy, 70 eV; solvent delay, 7 min; full scan mode, scan mass range 33–400 amu.

[0030] Compared with the prior art, the beneficial effects of the present invention are as follows: The simulation method of the present invention directly introduces heated cigarette smoke into the GC / MS instrument, which is simple to operate, does not require smoking machine suction and sample pretreatment process, avoids the loss of smoke components caused by cumbersome operation process, has good consistency with the actual puffing process, and has high authenticity of smoke components; the method of the present invention can effectively replace the traditional method to evaluate the smoke release behavior of heated cigarettes during puffing, which is simple to operate, saves time and effort, and provides accurate and reliable results. Attached Figure Description

[0031] Figure 1 The graph shows the peak area variation trend of menthol release during each puff in Examples 1-4 and Comparative Examples 1-4, simulating the smoking process of heated cigarettes.

[0032] Figure 2 The graph shows the peak area variation trend of menthol monosuccinate released per puff in Examples 1-4 and Comparative Examples 1-4, simulating the smoking process of heated cigarettes.

[0033] Figure 3 The graph shows the peak area variation trend of ethyl levulinate released puff by puff during the simulated smoking process of heated cigarettes in Example 5 and Comparative Example 4.

[0034] Figure 4 The peak area variation trend of γ-heptalactone release during simulated heated cigarette smoking is shown in Example 6 and Comparative Example 4.

[0035] Figure 5 The graph shows the peak area variation trend of ethyl phenylacetate released puff by puff during the simulated smoking process of heated cigarettes in Example 7 and Comparative Example 4.

[0036] Figure 6 The graph shows the peak area variation trend of ethyl cinnamate released puff by puff during the simulated smoking process of heated cigarettes in Example 8 and Comparative Example 4. Detailed Implementation

[0037] The technical solution of the present invention will be clearly and completely described below with reference to specific embodiments. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0038] In the following examples and comparative examples, the headspace CTC injector used was purchased from Agilent Technologies, model RAL RSI 85. The GC / MS analyzer used was purchased from Agilent Technologies, model 5977A-7890B. All reagents and conventional instruments used were readily available through regular purchase.

[0039] Example 1

[0040] The method provided in this embodiment for evaluating the puff-by-puff release behavior of menthol and succinic acid monomenthol (i.e., smoke, flavoring raw materials) during the puff-by-puff inhalation of heated cigarettes uses a headspace CTC sampling system to simulate the heated cigarette inhalation process, and includes the following steps:

[0041] (1) Weigh 0.04g of heated cigarette containing a mixture of menthol and menthol monosuccinate (fragrance raw material) and place it in a headspace vial. After capping the vial, place it on a sample tray. The amount of menthol used is 0.1% of the total weight of the heated cigarette, and the amount of menthol monosuccinate used is 0.2% of the total weight of the heated cigarette, that is, the ratio of menthol to menthol monosuccinate is 0.5:1.

[0042] (2) The heating chamber (i.e., the heating device) is started. After the heating temperature reaches 140℃, the headspace vial is removed from the sample tray and placed into the heating chamber (heating device) using the headspace CTC injection system. After heating for 2 minutes, the flue gas is directly introduced into the gas chromatography-mass spectrometry (GC-MS) instrument through the injection needle for analysis to determine the content of flavoring raw materials in the flue gas. The temperature of the injection needle is 145℃. The conditions for analysis by the GC-MS instrument are:

[0043] Gas chromatography conditions: Injector temperature, 250℃; Carrier gas, helium; Column flow rate, constant flow 1 ml / min; Injection volume, 1 μl; Split injection, split ratio 10:1; Temperature program, initial temperature 50℃, hold for 2 min, then increase to 280℃ at a rate of 8℃ / min, hold for 25 min.

[0044] Mass spectrometry conditions: Electron impact source (EI); transfer line temperature, 280℃; ion source temperature, 230℃; ionization energy, 70 eV; solvent delay, 7 min; full scan mode, scan mass range 33-400 amu;

[0045] (3) After the flue gas is directly introduced into the gas chromatograph-mass spectrometer, the headspace vial is immediately removed, the cap is opened, and the flue gas in the headspace vial is allowed to evaporate naturally for 1 minute before the headspace vial cap is closed and the headspace vial is placed back into the sample tray.

[0046] (4) Repeat steps (2) and (3) 6 times to simulate the process of heating a cigarette and taking 6 puffs;

[0047] (5) Perform chromatographic integration on the GC / MS spectrum of each puff of smoke, and plot the release trend of menthol and succinic acid monomenthol on the puff-by-puff process of heated cigarettes, with the peak areas of menthol and succinic acid monomenthol on the ordinate and the number of puffs on the abscissa.

[0048] (6) The peak areas of menthol and menthyl succinate obtained in each aspiration obtained in step (5) above are compared with the peak areas obtained after detecting menthol and menthyl succinate using the traditional method. The correlation coefficient between the two is calculated according to the following formula to determine the consistency of the detection conclusion.

[0049] ;

[0050] in, This represents the peak area of ​​menthol or menthyl succinate monosuccinate obtained from each aspiration using steps P1 and P2. For all suction counts The average value; This represents the peak area of ​​menthol or menthyl succinate mono-method obtained per aspiration using conventional methods. For all suction counts The average value.

[0051] Ultimately, the correlation coefficient between the two methods for detecting menthol was 0.998, and the correlation coefficient for detecting menthyl succinate was 0.780.

[0052] Example 2

[0053] The method provided in this embodiment for evaluating the puff-by-puff release behavior of menthol and succinic acid monomenthol during the puff-by-puff smoking of heated cigarettes is basically the same as that in Example 1, except that the heating temperature of the heating chamber (i.e. the heating device) in step (2) is 130°C and the temperature of the injection needle is 135°C.

[0054] Ultimately, the correlation coefficient between the two methods for detecting menthol was 0.983, and the correlation coefficient for detecting menthyl succinate was 0.584.

[0055] Example 3

[0056] The method provided in this embodiment for evaluating the puff-by-puff release behavior of menthol and succinic acid monomenthol during the puff-by-puff smoking of heated cigarettes is basically the same as that in Example 1, except that the heating time in step (2) is 3 min.

[0057] Ultimately, the correlation coefficient between the two methods for detecting menthol was 0.968, and the correlation coefficient for detecting menthyl succinate was 0.554.

[0058] Example 4

[0059] The method for evaluating the puff-by-puff release behavior of ethyl levulinate provided in this embodiment is basically the same as that in Example 1, except that 0.04g of heated cigarette containing menthol and menthol monosuccinate is replaced with 0.04g of heated cigarette containing ethyl levulinate. Ultimately, the correlation coefficient between the two methods for detecting ethyl levulinate was 0.991.

[0060] Example 5

[0061] The method for evaluating the puff-by-puff release behavior of γ-heptalactone during the inhalation of heated cigarettes provided in this embodiment is basically the same as that in Example 1, except that 0.04g of heated cigarettes containing menthol and menthol monosuccinate is replaced with 0.04g of heated cigarettes containing γ-heptalactone. Ultimately, the correlation coefficient between the two methods for detecting γ-heptalactone was 0.926.

[0062] Example 6

[0063] The method for evaluating the puff-by-puff release behavior of ethyl phenylacetate during the puff-by-puff process of heated cigarettes provided in this embodiment is basically the same as that in Example 1, except that 0.04g of heated cigarettes containing menthol and menthyl succinate is replaced with 0.04g of heated cigarettes containing ethyl phenylacetate. Ultimately, the correlation coefficient between the two methods for detecting ethyl phenylacetate was 0.983.

[0064] Example 7

[0065] The method provided in this embodiment for evaluating the puff-by-puff release behavior of ethyl cinnamate in heated cigarettes is basically the same as that in Example 1, except that 0.04g of heated cigarettes containing menthol and menthol monosuccinate is replaced with 0.04g of heated cigarettes containing ethyl cinnamate. Ultimately, the correlation coefficient between the two methods for detecting ethyl phenylacetate was 0.955.

[0066] Comparative Example 1

[0067] The method provided in this comparative example for evaluating the puff-by-puff release behavior of menthol and menthol monosuccinate during the puffing of heated cigarettes is basically the same as that in Example 1, except that the heating temperature of the heating chamber (i.e., the heating device) in step (2) is 120°C and the temperature of the injection needle is 125°C. Ultimately, the correlation coefficient for detecting menthol by the two methods was 0.558, and the correlation coefficient for detecting menthol monosuccinate was -0.820.

[0068] Comparative Example 2

[0069] The method for detecting the puff-by-puff release behavior of menthol and menthol monosuccinate provided in this comparative example is basically the same as that in Example 1, except that the heating temperature of the heating chamber (i.e., the heating device) in step (2) is 150°C and the temperature of the injection needle is 155°C. Ultimately, the correlation coefficient for detecting menthol by the two methods was 0.428, and the correlation coefficient for detecting menthol monosuccinate was 0.223.

[0070] Comparative Example 3

[0071] The method provided in this embodiment for evaluating the puff-by-puff release behavior of menthol and succinic acid monomenthol during the puff-by-puff smoking of heated cigarettes is basically the same as that in Example 1, except that the heating time in step (2) is 1 min.

[0072] Ultimately, the correlation coefficient between the two methods for detecting menthol was 0.989, while the correlation coefficient for detecting menthyl succinate was -0.144.

[0073] Comparative Example 4

[0074] The method for determining the puff-by-puff release behavior of menthol and menthol monosuccinate provided in this comparative example is basically the same as that in Example 1, except that in step (3), after each heating and direct introduction of the smoke into the gas chromatography-mass spectrometry instrument, the headspace vial is immediately removed, the cap is quickly replaced, and the vial is returned to the sample tray. Ultimately, the correlation coefficient for detecting menthol using the two methods was 0.925, and the correlation coefficient for detecting menthol monosuccinate was -0.083.

[0075] Experimental Example: Traditional Methods for Detecting Cigarette Smoke Emission Behavior

[0076] 1. A traditional method for detecting cigarette smoke emission behavior for comparison.

[0077] (1) The fragrance raw materials (menthol, succinate monomenthyl ester, ethyl levulinate, γ-heptanol, ethyl phenylacetate and ethyl cinnamate, 6 kinds of fragrance raw materials were tested separately) were injected into unflavored heated cigarettes. The smoking procedure was carried out according to the ISO3308 standard. The first Cambridge filter collected the first puff of smoke from several (e.g., 20) heated cigarettes, the second Cambridge filter collected the second puff of smoke from these heated cigarettes, and so on, until the sixth Cambridge filter collected the sixth puff of smoke from these heated cigarettes.

[0078] (2) Place the six Cambridge filters that have been aspirated upside down into a 50mL Erlenmeyer flask, and put the wiped cotton into the Erlenmeyer flask as well. Add 20mL of anhydrous ethanol, sonicate at 40℃ and 100W for 40min. After standing for 5min, take the supernatant, filter it with a 0.45μm organic filter membrane, and take 1.5mL of the filtrate into a 2mL brown chromatographic bottle for GC / MS analysis.

[0079] The GC / MS instrument analysis conditions are as follows:

[0080] ① The gas chromatography conditions are as follows: injection port temperature, 250℃; carrier gas, helium; column flow rate, constant flow 1ml / min; injection volume, 1μl; split injection, split ratio 10:1; temperature program, initial temperature 50℃, hold for 2min, then increase to 280℃ at a rate of 8℃ / min, hold for 25min.

[0081] ②The mass spectrometry conditions are as follows: electron impact source (EI); transfer line temperature, 280℃; ion source temperature, 230℃; ionization energy, 70eV; solvent delay, 7min; scanning mode is full scan mode, and the scanning mass range is 33-400amu.

[0082] 2. Test Results

[0083] The peak areas of the six fragrance raw materials—menthol, menthyl succinate, ethyl levulinate, γ-heptanol, ethyl phenylacetate, and ethyl cinnamate—were obtained using the simulation methods of Examples 1-3 and Comparative Examples 1-5, and the peak areas obtained using the conventional methods described above are shown in Tables 1-6 below.

[0084] Table 1. Detection results of menthol

[0085]

[0086] Table 2. Detection results of menthyl succinate monosuccinate

[0087]

[0088] Table 3. Detection results of ethyl levulinate

[0089]

[0090] Table 4. Detection results of γ-heptanolide

[0091]

[0092] Table 5. Detection results of ethyl phenylacetate

[0093]

[0094] Table 6. Detection results of ethyl cinnamate

[0095]

[0096] Figure 1 , Figure 2 The peak area variation trends of menthol and menthyl succinate monosuccinate released in Examples 1-3 and Comparative Examples 1-5 are shown respectively, corresponding to the data in Tables 1 and 2. Figure 1 As can be seen, in the simulated heated cigarette smoking process of Examples 1-3 of this invention, the puff-by-puff release trends of menthol and menthol monosuccinate are consistent with those measured by the traditional method. Among them, Example 1 has the highest correlation coefficient with the traditional method, that is, the consistency is the best. In Comparative Examples 1-5, the puff-by-puff release trends of menthol and menthol monosuccinate differ from those measured by the traditional method, either one is significantly different or both are inconsistent. Therefore, in step (2), adjusting the heating temperature and heating time, or in step (3), quickly closing the headspace cap after each puff, will affect the accuracy of the final detection results.

[0097] Figure 3-6The figures show the puff-by-puff release trends of ethyl levulinate (Example 4), γ-heptanolone (Example 5), ethyl phenylacetate (Example 6), and ethyl cinnamate (Example 7) during simulated heated cigarette smoking, corresponding to the data in Tables 3-6. As can be seen from the figures, the puff-by-puff release trends of each flavoring ingredient measured using the method of this invention are largely consistent with those measured using traditional methods. The results indicate that the method of this invention can effectively simulate the puff-by-puff process of heated cigarettes, completely replacing traditional methods, and providing a true, effective, and reliable evaluation of the release behavior of these flavoring ingredients in the puff-by-puff smoke of heated cigarettes. It is simple to operate and greatly saves labor and time.

[0098] The above description is merely a specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any variations or substitutions that can be easily conceived by those skilled in the art within the scope of the technology disclosed in the present invention should be included within the scope of protection of the present invention. The scope of protection of the present invention shall be determined by the scope of the claims.

Claims

1. A method of assessing the puff-by-puff smoke delivery behaviour of a heated cigarette, characterised in that, The method comprises the following steps: P1. Using a headspace CTC sampling system, a sampling bottle is selected as a headspace bottle, and a method of simulating the process of puffing a heated cigarette is adopted to heat the test tobacco in the headspace bottle and continuously generate smoke; the test tobacco contains a to-be-tested flavor raw material; The method of simulating the process of puffing a heated cigarette is as follows: P1-1. The heated tobacco is placed in the sampling bottle, and the bottle cap is closed before use. The heating device is started to preheat; P1-2. The sampling bottle is placed in the heating device, and after being heated for a specific time, the CTC sampler is started to sample. The smoke in the sampling bottle is introduced into the GC / MS detector for detection. After sampling, the sampling bottle is taken out, the bottle cap is opened, and after the smoke in the sampling bottle is volatilized for a period of time, the bottle cap is closed again, the sampling bottle is placed in the heating device for heating again, and the process is repeated for a specific number of times to simulate the process of puffing a heated cigarette. The heating time is 2-3 min, the heating temperature is 130-145 DEG C, the temperature of the sampling needle is 135-145 DEG C, and the sampling amount is 1 μl; P2. The smoke generated in step P1 is directly introduced into a gas chromatograph mass spectrometer for analysis by using a headspace CTC sampling system to determine the content of the to-be-tested flavor raw material in the smoke. A GC / MS spectrum is obtained, and chromatogram integration is performed. The peak area of the to-be-tested flavor raw material is taken as the vertical coordinate, and the number of puffs is taken as the horizontal coordinate to draw a release change curve of the to-be-tested flavor raw material; P3. The peak area of the to-be-tested flavor raw material in each puff is compared with the peak area obtained by detecting the to-be-tested flavor raw material by using a traditional method. The correlation coefficient is calculated to evaluate the correlation between the two, and the consistency of the detection conclusion is determined. The formula for calculating the correlation coefficient is as follows: ； wherein is the peak area of the test flavor raw material of each puff obtained by the method of steps P1, P2, is the average value of the for all puff numbers; is the peak area of the test flavor raw material of each puff obtained by the conventional method, is the average value of the for all puff numbers, the test flavor raw material being one or more of menthol, monomenthyl succinate, ethyl levulinate, gamma-heptalactone, ethyl phenylacetate, ethyl cinnamate.

2. The method for evaluating the release behavior of each puff of the heated cigarette according to claim 1, wherein, The weight ratio of the flavor raw material (0.25-4):1 is menthol and succinic acid monomenthyl ester, and the weight of the flavor raw material is 0.05-1% of the heated cigarette.

3. The method for evaluating the release behavior of each puff of the heated cigarette according to claim 1, wherein, In step P1-2, the heating time is 2 min, the heating temperature is 140 DEG C, and the temperature of the sampling needle is 145 DEG C.

4. The method for evaluating the release behavior of each puff of heated cigarette smoke according to claim 1, wherein, In step P1-2, the volatilization time of the smoke is 1 min.

5. The method for evaluating the release behavior of each puff of heated cigarette smoke according to claim 1, wherein In step P2, the gas chromatograph conditions of the gas chromatograph mass spectrometer for analysis are as follows: the injection port temperature is 250 DEG C; the carrier gas is helium; the column flow is constant 1 ml / min; the injection amount is 1 μl; the split injection is 10:1; the temperature program is that the initial temperature is 50 DEG C, maintained for 2 min, then increased to 280 DEG C at a rate of 8 DEG C / min, and maintained for 25 min; The mass spectrometry conditions are as follows: the electron impact source EI; the transfer line temperature is 280 DEG C; the ion source temperature is 230 DEG C; the ionization energy is 70 eV; the solvent delay is 7 min; the scanning mode is full scan, and the scanning mass range is 33-400 amu. ​

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