A method for detecting the migration of a heating cigarette functional segment additive heated by each puff

Abstract

Provided is a method for detecting the migration of a heating cigarette functional segment additive heated by each puff, comprising the following steps: step S1: determining the temperature of each puff of smoke entering the target heating cigarette functional segment by a thermocouple method and calculating the average temperature of each puff according to the temperature of each puff; step S2: setting a time sequence table according to the average temperature of each puff and collecting the migration of the target heating cigarette functional segment by a detection device according to the time sequence table to obtain a target filter; and step S3: placing the target filter in a static headspace instrument to form a target migration after heating and analyzing the target migration by a gas chromatograph-mass spectrometer, thereby solving the technical problems that the dynamic release behavior of the additive cannot be reflected due to the deviation from the real puff-by-puff smoking process, the migration amount of the functional segment additive cannot be accurately quantified due to the interference of complex components of the tobacco base, and the systematic study on the release rule of each puff cannot be carried out due to the lack of a programmatic control means matched with the dynamic temperature curve of the heating cigarette.

Description

Technical Field

[0001] This patent relates to the field of testing materials for heated non-combustible cigarettes, specifically to a method for detecting the migration of additives in the functional sections of heated cigarettes upon heating. Background Technology

[0002] Heated cigarettes, as an important branch of new tobacco products, have experienced rapid development globally in recent years. Unlike traditional combustible cigarettes, heated cigarettes use an external heating device to heat the tobacco material instead of burning it, allowing nicotine and flavor components to be released at relatively low temperatures, significantly reducing the harmful substances produced by the high-temperature decomposition of tobacco.

[0003] As consumers increasingly demand personalized and differentiated experiences from cigarette products, the aroma of the tobacco sheet material itself alone is no longer sufficient to meet diverse smoking needs. As a result, heated cigarette flavoring technology has emerged and developed rapidly.

[0004] Because the flavoring substances added to tobacco sheets are easily volatilized and dissipated in large quantities during the hot air drying process of sheet production, flavoring the functional sections of heated cigarettes has become the mainstream technical approach for flavoring heated cigarettes.

[0005] Common flavoring methods for functional sections encompass various technical forms: flavoring in the filter section includes flavoring with flavor capsules, flavoring threads, and flavoring with tow; flavoring in the hollow section includes flavoring with O-sticks and flavoring with granules; and flavoring in the cooling section can utilize composite materials. Clarifying the flavoring efficiency and puff-by-puff release patterns of different functional sections and flavoring methods is of significant guiding importance for optimizing the structure of heated cigarettes, adjusting and improving flavor formulations, and reducing product production costs.

[0006] In existing technologies, the detection methods for filter rod additives mainly have the following technical limitations. First, many existing detection methods adopt a scheme of testing the filter tip separately, that is, removing the filter tip from the cigarette and performing heating or solvent extraction analysis separately. This method completely deviates from the elution effect of hot smoke on filter tip additives during actual cigarette smoking, and cannot truly reflect the release behavior and migration pattern of filter rod additives under actual use conditions.

[0007] Secondly, some research methods use smoking machines to simulate the cigarette smoking process, capturing mainstream smoke and then analyzing the target components within it. However, these methods are highly susceptible to interference from the complex chemical components in the smoke. Heated cigarette smoke also contains a large number of pyrolysis and distillation products from tobacco sheets. When there is overlap between the flavoring components added to the tobacco sheets and the functional additives, smoke analysis methods can hardly accurately distinguish and quantify the actual volatilization and migration amounts of the functional additives.

[0008] While some methods for detecting the migration of additives in filter rods have been reported, these methods use a fixed hot air temperature and are only applicable to the analysis of traditional cigarettes, failing to address the technical challenges posed by the working characteristics of heated cigarettes. Furthermore, some existing detection methods do not adequately consider the volatile nature of thermally migrated components and lack effective low-temperature capture methods, leading to the loss of volatile components before analysis and affecting the accuracy of quantitative analysis results.

[0009] For heated cigarettes, the heating characteristics make the existing detection methods even more difficult to apply. First, the heating appliances offered by different manufacturers have different heating temperature profiles and temperature control strategies, which causes the dynamic smoke temperature inside the heated cigarette to exhibit phased changes at different stages of smoking, and the amount of filter rod additives released per puff also fluctuates accordingly.

[0010] Secondly, the distances of different functional sections in heated cigarettes from the heating source are different, and the temperature history experienced by each functional section during the complete heating cycle is not the same. The temperature experienced by the support section, which is close to the heat source, is much higher than that of the filter section, which is far away from the heat source and serves as the end of the smoke. Therefore, the thermal migration behavior of additives in different functional sections will inevitably have significant differences, and it is necessary to specifically measure the actual heating situation of each functional section.

[0011] More importantly, existing methods are limited by their inability to realistically simulate the puff-by-puff state of heated cigarettes. The actual use of heated cigarettes is an intermittent, puff-by-puff process, with each puff's duration, interval, and volume having distinct physical characteristics. Traditional continuous heating or constant-temperature heating modes cannot replicate the temperature changes under these dynamic puffing conditions, making it difficult to conduct systematic research on the puff-by-puff release patterns of filter rod additives. Furthermore, existing analytical methods primarily focus on determining the total amount of additives, lacking effective analytical tools for analyzing the differences in puff-by-puff release of additives under different numbers of puffs.

[0012] In summary, there is an urgent technical need for a method that can realistically simulate the dynamic thermal environment of the functional segment during each puff of heated cigarette, can precisely set the ambient gas temperature of the tested functional segment, can avoid interference from the tobacco sheet substrate smoke, and can independently analyze and detect the migration amount per puff. Summary of the Invention

[0013] This patent aims to solve the technical problems in existing methods for detecting additives in the functional segments of heated cigarettes. These problems include: failing to reflect the dynamic release behavior of additives due to being detached from the actual puffing process; difficulty in accurately quantifying the migration amount of additives due to interference from the complex components of the tobacco base; and the inability to conduct systematic research on the release law of each puff due to the lack of procedural control methods that match the dynamic temperature curve of heated cigarettes. This patent provides the following technical solution: Firstly, a method for detecting the puff-by-puff thermal migration of additives in the functional section of heated cigarettes is provided, comprising the following steps: Step S1: The puff-by-puff temperature of the flue gas entering the target heated cigarette functional section is determined by thermocouple method, and the average temperature per puff is calculated based on the puff-by-puff temperature; Step S2: A time series table is set according to the average temperature per puff, and the target filter is obtained by collecting the migration material from the target heated cigarette functional section through a detection device according to the time series table; Step S3: The target filter is heated in a static headspace analyzer to form the target migration material, and the target migration material is analyzed by gas chromatography-mass spectrometry.

[0014] Further, step S1 includes the following steps: Step S11: Insert the first end of the target heated cigarette functional section through the pin hole using a pin, place the thermocouple sensor into the pin hole, and then seal it with a hot melt glue gun; Step S12: Insert the target heated cigarette functional section into the heating device and then inhale through the smoking machine; Step S13: Record the temperature of each puff during the inhalation cycle and calculate the average temperature of each puff by integration.

[0015] Furthermore, in step S11, the end where the smoke enters the target heated cigarette functional section is the beginning end, and the end where the smoke exits the target heated cigarette functional section is the end end; the pin is inserted into the target heated cigarette functional section from the beginning end until the pin's pillow contacts the obstacle for the second time and is then pulled out, so that the thermocouple sensor is placed in the target heated cigarette functional section along the pin hole and located at the axial center of the target heated cigarette functional section.

[0016] Further, step S2 includes the following steps: Step S21: Set the "stage-duration-target temperature-flow rate" timing table; Step S22: Place the target heated cigarette functional section and filter into the detection device; Step S23: Run the detection device according to the timing table so that the migration formed from the target heated cigarette functional section is enriched on the filter to obtain the target filter.

[0017] Furthermore, in step S21, the stage is the number of suction ports; the target temperature is the average temperature of each port.

[0018] Furthermore, in step S22, the detection device includes a suction mechanism, which is a linear suction machine or a puff-by-puff suction machine; the suction mode of the suction mechanism is the ISO standard suction mode or the Canadian deep suction HCI mode; the suction mode of the suction mechanism is the same as the suction mode of the suction machine in step S12.

[0019] Furthermore, if the suction mechanism is a linear smoking machine, the migration formed within the number of suction ports is concentrated on the same filter; if the suction mechanism is a puff-by-puff smoking machine, the migration formed in a single suction is concentrated on a single filter, and the number of filter plates is equal to the number of suction ports.

[0020] Furthermore, the filter is a Cambridge filter; the filter is placed in the filter holder of the detection device; the target heated cigarette functional section is set between the sealing ring and the filter holder of the detection device, the first end of the target heated cigarette functional section is connected to the sealing ring and the last end of the target heated cigarette functional section is connected to the filter holder, so that the smoke enters from the first end, flows through the target heated cigarette functional section and flows out from the last end.

[0021] Further, in step S3, the parameters of the static headspace analyzer include: sample equilibrium temperature set to 175℃, sample loop volume to 3.0 mL, sample loop temperature set to 180℃, transfer line temperature set to 185℃, sample equilibrium time to 20.0 min, sample vial pressurization pressure to 138 kPa, pressurization time to 0.20 min, gas filling time to 0.20 min, sample loop equilibrium time to 0.05 min, and injection time to 1.0 min; the gas chromatograph uses a VOC elastic fused silica capillary column or equivalent column; the column length is 60 mm, the inner diameter is 0.32 mm, and the film thickness is 1.8 μm; the carrier gas is high-purity helium with a purity of not less than 99.99%; the injection port temperature is set to 200℃; constant flow mode is used, the column flow rate is 2.0 mL / min, and the split ratio is 1:1; the temperature program is: initial temperature 40℃, hold for 2... The temperature was increased to 160℃ at a rate of 4℃ / min, then increased to 210℃ at a rate of 10℃ / min and held for 10 min. The operating temperature was then 250℃ and held for 10 min. The mass spectrometer parameters were as follows: auxiliary interface temperature: 280℃; ionization method: electron impact source with ionization energy of 70 eV; ion source temperature: 230℃; quadrupole temperature: 150℃; solvent delay time: 4.0 min; mass spectrometer used full scan monitoring mode and / or selected ion monitoring mode; the full scan monitoring mode had a scan range of 35 amu to 350 amu; the selected ion monitoring mode selected ions with high specificity and response as quantitative ions, and selected 1-2 other fragment ions as auxiliary qualitative ions.

[0022] Furthermore, the target heated cigarette functional segment is selected from one or more of the following: cellulose acetate filter segment, hollow segment, or support segment.

[0023] This patent has the following beneficial effects: 1. A method for detecting the puff-by-puff thermal migration of additives in the functional section of heated cigarettes is provided, comprising the following steps: Step S1: Measuring the puff-by-puff temperature of the smoke entering the target heated cigarette functional section using a thermocouple method and calculating the average puff-by-puff temperature; Step S2: Setting a time series table based on the average puff-by-puff temperature and collecting the migration material from the target heated cigarette functional section using a detection device according to the time series table to obtain a target filter; Step S3: Heating the target filter in a static headspace analyzer to form target migration material and analyzing the target migration material using gas chromatography-mass spectrometry. This method solves the technical problems of failing to reflect the dynamic release behavior of additives due to the separation from the actual puff-by-puff process, difficulty in accurately quantifying the migration amount of functional section additives due to interference from the complex components of the tobacco substrate, and inability to conduct systematic research on the puff-by-puff release law due to the lack of procedural control methods that match the dynamic temperature curve of heated cigarettes.

[0024] 2. By using the thermocouple method to determine the puff-by-puff temperature of the flue gas entering the target heated cigarette functional section and calculating the average puff-by-puff temperature, the obtained average puff-by-puff temperature is used as the target temperature for each stage in the time series table. This ensures that the ambient gas temperature of the functional section in the detection method closely matches the flue gas temperature experienced by that functional section under actual smoking conditions. Simultaneously, by setting the number of stages in the time series table to match the number of puffs in the selected smoking mode, the gas supply cycle is synchronized with the smoking cycle. This overcomes the technical limitation of existing methods that cannot accurately reproduce the puff-by-puff state of heated cigarettes, providing a reliable experimental basis for studying the puff-by-puff release law of filter rod additives.

[0025] 3. Because the detection method only installs the selected heated cigarette functional segment between the sealing ring and the filter holder of the measuring device, the target airflow only flows through this functional segment and not through the thin tobacco fragments. Therefore, the captured target migrants come entirely from the thermal release of the functional segment additives, without interference from the complex components of the tobacco substrate. This technical advantage overcomes the technical deficiency of traditional smoke analysis methods, which cannot accurately quantify the migration amount of functional segment additives due to the overlap of components between tobacco segment additives and functional segment additives. This allows the detection results to truly reflect the thermal migration behavior of the functional segment additives themselves.

[0026] 4. In this patent, a time series table containing stages, durations, target temperatures, and flow rates is set based on the average temperature of each puff, and the operation of the measuring device is controlled by this time series table. This allows the temperature of the target airflow to be dynamically adjusted according to the stage-by-stage changes in the smoke temperature during actual smoking. This temperature control method can simulate the differentiated heating curves of different heating appliances and the temperature change history of different functional segments within the same heating cycle. It solves the technical problem that traditional fixed hot air temperature detection methods cannot cope with the dynamic stage-by-stage changes in the temperature of heated cigarettes, and achieves accurate measurement of the migration behavior of additives under stage-by-stage smoke temperatures.

[0027] 5. By employing Cambridge filters in a cold trap environment to capture migrating substances, the low temperature of the cold trap effectively reduces the loss of volatility, ensuring high capture efficiency of the Cambridge filters. After capture, the Cambridge filters are heated in a static headspace spectrometer, allowing the migrating substances to be fully desorbed from the filter and introduced into the gas chromatograph-mass spectrometer with the carrier gas for analysis. The static headspace injection method avoids contamination of the chromatographic system by complex matrices, while gas chromatography-mass spectrometry provides qualitative and quantitative analysis capabilities for the various chemical components in the migrating substances.

[0028] 6. When the aspiration mechanism in the measuring device uses a linear aspirator, the migrations formed within all aspiration ports are enriched on the same Cambridge filter. This mode is suitable for rapidly assessing the total migration of functional additives throughout the entire aspiration cycle. When the aspiration mechanism uses a port-by-port aspirator, the migrations formed in each port are enriched on different Cambridge filters. This mode is suitable for systematically studying the port-by-port release pattern of functional additives as the number of aspiration ports changes. Switching between the two detection modes only requires changing the type of aspiration mechanism and the number of Cambridge filters installed. The operation is simple and can meet the detection needs of different research scenarios.

[0029] 7. By optimizing parameters such as sample equilibrium temperature, sample loop temperature, transfer line temperature, and equilibrium time in the static headspace analyzer, migrating components with different volatility and polarity gradients can be effectively desorbed from the Cambridge filter and enter the chromatographic system. Optimizing the temperature program conditions of gas chromatography and the scanning mode of mass spectrometry enables efficient separation and sensitive detection of complex mixtures of migrating components. The combined use of full-scan monitoring mode and selected ion monitoring mode allows for both screening and identification of unknown components in the migrating material and highly sensitive quantitative analysis of known target components, further expanding the application range of the detection method. Attached Figure Description

[0030] To more clearly illustrate the technical solutions of the embodiments of this patent, the drawings used in the embodiments will be briefly introduced below. It should be understood that the following drawings only show some embodiments of this patent and should not be regarded as a limitation of the scope. For those skilled in the art, other related drawings can be obtained from these drawings without creative effort.

[0031] Figure 1 This is a flowchart of the detection method in this patent; Figure 2 This is the temperature profile from Example 1. Detailed Implementation

[0032] The detailed features and advantages of this patent are described below in the specific embodiments. The content is sufficient to enable any person skilled in the art to understand the technical content of this patent and implement it accordingly. Based on the specification, claims and drawings disclosed in this specification, a person skilled in the art can easily understand the related objectives and advantages of this patent.

[0033] It should be noted that in this specification, similar reference numerals and letters in the following figures indicate similar items. Therefore, once an item is defined in one figure, it does not need to be further defined and explained in subsequent figures.

[0034] It should be noted that when an element is referred to as being "fixed to" another element, it can be directly on the other element or there may be an intermediate element. When an element is considered to be "connected to" another element, it can be directly connected to the other element or there may be an intermediate element present. The terms "vertical," "horizontal," "left," "right," and similar expressions used herein are for illustrative purposes only and do not indicate the only possible implementation. The terms "upper," "lower," etc., indicating orientation or positional relationships are defined with reference to the coordinates of the accompanying drawings and are only for the convenience of describing this patent and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation of this patent. The terms "first," "second," etc., are only used to distinguish descriptions and should not be construed as indicating or implying relative importance.

[0035] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this patent belongs. The terminology used herein in the specification of this patent is for the purpose of describing particular embodiments only and is not intended to be limiting of this patent. The term "and / or" as used herein includes any and all combinations of one or more of the associated listed items.

[0036] To make the objectives, technical solutions, and advantages of this patent clearer, the embodiments of this patent will be described in further detail below with reference to the accompanying drawings.

[0037] A method for detecting the thermal migration of additives in the functional section of heated cigarettes is provided, wherein the method is implemented using the aforementioned measuring device for thermal migration of additives in the functional section of heated cigarettes.

[0038] The overall workflow of the detection method includes three main steps: temperature characteristic acquisition, time series table setup and migration collection, and migration analysis. Please refer to [link / reference]. Figure 1 The specific implementation methods for each step are described in detail below, following the step-by-step sequence.

[0039] In step S1, the temperature of each puff of flue gas entering the target heated cigarette functional section is measured by thermocouple method, and the average temperature of each puff is calculated based on the measured temperature of each puff.

[0040] The purpose of this step is to obtain temperature-time relationship data of flue gas before it enters the functional segment under actual suction conditions, so as to provide a basis for setting the subsequent time series table.

[0041] Since the distances of different functional sections in heated cigarettes relative to the heat source are different, the temperature history experienced by each functional section during the complete heating cycle is significantly different. Therefore, it is necessary to measure the temperature of the selected target heated cigarette functional section separately in order to obtain the actual temperature change data of the specific functional section during the actual smoking process.

[0042] Step S1 specifically includes the following sub-steps: In step S11, it is first necessary to determine the direction of the first end and the last end of the target heated cigarette functional section, wherein the end where the smoke enters the target heated cigarette functional section is the first end, and the end where the smoke exits the target heated cigarette functional section is the last end.

[0043] Use a pin to gently insert it into the first end of the target heated cigarette section, extending the insertion direction along the axial direction of the section until the tip of the pin contacts the obstacle for the second time.

[0044] The obstacles referred to here are physical blocking structures existing inside the functional section, such as the end face of the O-rod element in the hollow section, the tightly packed surface of the filament bundle in the filter section, or the end face of the support element in the support section.

[0045] When the pin first contacts the obstacle, it penetrates the surface layer of the first end face of the functional segment. It continues to be inserted until the pin contacts the obstacle for the second time. At this point, the pin has reached the position inside the functional segment where a thermocouple sensor can be installed.

[0046] After the pin is inserted, a pinhole is formed on its insertion path. Then the pin is removed, and one end of the thermocouple sensor is placed into the target heated cigarette functional section along the direction of the pinhole, so that the temperature measuring end of the thermocouple sensor is at the axial center of the functional section.

[0047] After the thermocouple sensor is inserted into the pinhole, the pinhole is sealed with a hot melt glue gun to prevent external air from entering the functional section through the pinhole during subsequent suction, which would affect the accuracy of temperature measurement.

[0048] In step S12, the target heated cigarette functional segment with the implanted thermocouple sensor is placed back into its matching heating device.

[0049] The heating device refers to a commercially available heating device used in conjunction with the heated cigarette product to be tested, such as a center-heating or peripheral-heating electric heating device. After the heating device is turned on, a smoking machine is used to simulate smoking the heated cigarette.

[0050] The smoking machine can be set to either the ISO standard smoking mode or the Canadian deep smoking HCI mode, depending on the testing requirements. Both smoking modes are widely recognized and used standard smoking methods in the field of heated cigarette research.

[0051] The ISO standard aspiration mode uses a bell-shaped aspiration curve, with an aspiration volume of 35ml, an aspiration duration of 2s, and an aspiration interval of 60s.

[0052] The Canadian deep aspiration HCI mode also uses a bell-shaped aspiration curve, but the aspiration volume is 55ml, the aspiration time is 2s, and the aspiration interval is 30s.

[0053] In step S13, the temperature data detected by the thermocouple sensor is continuously recorded during the simulated smoking process. This temperature data is the temperature of each puff of smoke before it enters the target heated cigarette functional section within a complete smoking cycle.

[0054] Specifically, from the moment the heating appliance is turned on, the smoking machine performs sequential suction according to the set suction mode, and the thermocouple sensor records the temperature change curve over time during each suction process in real time.

[0055] After each suction cycle is completed, the corresponding temperature-time curve is fully recorded. Once all suction cycles have been completed, the temperature-time curves of each recorded suction cycle are integrated to obtain the average temperature of each suction cycle, i.e., the average temperature per suction cycle.

[0056] Specifically, the integral formula is: Average temperature = Integral of temperature over time ÷ Total duration

[0057] The average temperature per port reflects the equivalent thermal environment temperature experienced by the functional segment during each suction process, and is the key data for converting the actual suction conditions into the program control parameters of the detection device.

[0058] In step S2, a timing table is set according to the average temperature obtained in step S1, and the migration material of the target heated cigarette functional section is collected by a measuring device according to the timing table to obtain the target filter.

[0059] The purpose of this step is to convert the temperature data obtained during the actual suction process into control commands for the detection device, enabling the detection device to simulate heating of the functional segment according to the same temperature sequence as the actual suction process, thereby reproducing the thermal migration process of the additives in the functional segment under laboratory conditions.

[0060] Step S2 specifically includes the following sub-steps: In step S21, a timing table of "stage-duration-target temperature-flow rate" is set in the control mechanism of the measuring device.

[0061] The number of stages is set according to the number of puffs of the cigarette to be tested. The stage duration and airflow are set according to the puffing time and capacity of the selected puffing mode. The target temperature of each stage in the time sequence table is set according to the average temperature of each puff in S13.

[0062] The number of stages in this timing table is set to the number of puffs in the selected vaping mode. For example, when the Canadian Deep Inhale (HCI) mode is selected, if the heated cigarette has 8 puffs in HCI mode, then the number of stages in the timing table is set to 8 stages.

[0063] Each stage in the timing table corresponds to one suction port. The duration of each stage is set to be consistent with the single-port suction duration in the suction mode. The target temperature of each stage is set to the average temperature of the corresponding number of suction ports measured in step S1. The flow rate of each stage is set to the gas supply flow rate corresponding to the single-port suction capacity in the suction mode.

[0064] With the above settings, the timing table fully records the gas supply time, gas supply temperature, and gas supply flow rate for each suction port within the entire suction cycle. After the timing table is set, it is stored by the timing scheduling module of the control mechanism for later retrieval.

[0065] In step S22, the target heated cigarette functional section and filter are placed into the measuring device.

[0066] Specifically, firstly, a sealing ring with a matching inner diameter is selected based on the outer diameter of the target heated cigarette functional section, and the sealing ring is installed on the connecting pipe at the outlet end of the buffer tank of the measuring device. Then, the first end of the target heated cigarette functional section is inserted into the sealing ring, so that the sealing ring tightly wraps around the outer peripheral wall of the functional section, thereby achieving airtight fixation.

[0067] Connect the end of the target heated cigarette functional section to the inlet of the cold trap chamber of the measuring device to ensure that the gas flowing out of the end of the functional section can directly enter the cold trap chamber without leaking to the outside.

[0068] A filter is installed in the filter holder inside the cold trap chamber. The filter is a Cambridge filter, which is a circular filter made of glass fiber and has high collection efficiency and good chemical inertness.

[0069] The filter is held and fixed in place by the filter holder on the cross-section of the airflow channel inside the cold trap chamber, ensuring that all the airflow passes through the Cambridge filter.

[0070] When the suction mechanism in the measuring device is a linear suction machine, a Cambridge filter is installed in the filter holder.

[0071] When the suction mechanism adopts a sequential suction machine, multiple Cambridge filters are installed in the filter holder in sequence. The number of filters is equal to the number of suction ports in the selected suction mode. The positions of the multiple Cambridge filters are controlled by the moving guide rail or turntable mechanism on the sequential suction machine.

[0072] In step S23, the measuring device is run according to the timing table set in step S21, so that the additives in the target heated cigarette functional section are heated, migrated and enriched on the filter under simulated smoking conditions, and the target filter is obtained.

[0073] The specific operation process is as follows: After the detection program of the measuring device is started, the timing scheduling module in the control mechanism runs sequentially from the first stage according to the timing table.

[0074] When the gas source mechanism is activated, the mass flow controller outputs a constant mass flow rate of air according to the target flow rate value of the current stage. The airflow is divided into two paths and enters the heating chamber and the ambient temperature chamber respectively.

[0075] The feedforward calculation module in the control mechanism calculates the theoretical heating power in real time based on the target temperature, measured inlet temperature, gas specific heat capacity and current flow rate, and outputs it to the heating drive module. The heating drive module controls the heater to heat with the corresponding power.

[0076] The feedback correction module uses the feedback temperature of the temperature sensor after the output valve as the main feedback point and the feedback temperature of the third temperature sensor in the buffer tank as the auxiliary feedback point to perform cascade PID correction calculations, and fine-tunes the output power of the heater so that the actual temperature of the target airflow is stabilized with high precision within ±1 degree Celsius of the target temperature at the current stage.

[0077] During the preheating stage before the temperature reaches the set value, the vent valve is open while the output valve is closed. Gas from the buffer tank is discharged to a safe location via the vent valve and does not enter the functional section.

[0078] When the temperature sensor after the output valve detects that the temperature has stabilized at the target temperature for the current stage, the control mechanism closes the vent valve and opens the output valve. The target airflow flows through the output valve, passes through the sealing ring, and enters the first end of the target heated cigarette function section.

[0079] As the target airflow flows through the functional section, it heats and carries away the flavorings and fragrances added to the functional section, causing them to flow out from the end of the functional section and forming an airflow containing the target migrated substances.

[0080] The airflow containing the target pollutants enters the cold trap chamber. In the low-temperature environment, the volatility of the pollutants decreases, and they are captured and trapped by the Cambridge filters on the filter holder. Under the synchronous control of the control mechanism, the suction mechanism initiates suction at the same time rhythm as the gas supply cycle, simulating a suction machine applying suction force to the downstream pipeline according to a preset suction curve, ensuring that the airflow passes through the entire system according to the set flow path and velocity.

[0081] When the duration of the current stage ends, the timing module automatically switches to the control target of the next stage. The target temperature is switched to the average temperature of each inlet corresponding to the next suction inlet. The above process is executed cyclically until all stages in the timing table have been completed.

[0082] When the suction mechanism is a linear suction machine, the target airflow containing the migrating material formed in all suction ports flows through the same Cambridge filter. The target migrating material is enriched on the same Cambridge filter. The Cambridge filter removed after the program is completed is the target filter representing the total amount of functional segment additives migrated during the entire suction cycle.

[0083] When the suction mechanism is a port-to-port type suction machine, the target airflow containing the migrating material generated by each port flows through its own independent Cambridge filter. The migrating material corresponding to the first port is captured on the first Cambridge filter, the migrating material corresponding to the second port is captured on the second Cambridge filter, and so on. After the program is completed, each Cambridge filter removed represents the independent migration amount of the additive in the functional segment under a specific number of suction ports.

[0084] In step S3, the target filter obtained in step S2 is placed in a static headspace analyzer and heated to desorb the target migrants trapped on the target filter from the filter substrate and form gaseous target migrants. Then, the gaseous target migrants are qualitatively and quantitatively analyzed by gas chromatography-mass spectrometry.

[0085] The purpose of this step is to convert the migrating components trapped on the Cambridge filter into a gaseous sample that can be analyzed by a chromatography-mass spectrometry system, and to achieve accurate identification and content determination of each migrating component through chromatographic separation and mass spectrometry detection.

[0086] After removing the target filter from the filter holder in the cold trap chamber of the measuring device, place the entire target filter into the sample vial of the static headspace analyzer, seal the sample vial, and place it in the heating equilibrium zone of the static headspace analyzer.

[0087] The static headspace analyzer operates according to the set parameters, heating the sample vial to allow the target migrants captured on the target filter to fully volatilize and enter the gas phase space of the sample vial.

[0088] The preferred parameters for the static headspace analyzer are as follows: sample equilibrium temperature set at 175℃, sample ring volume at 3.0 mL, sample ring temperature set at 180℃, transfer line temperature set at 185℃, sample equilibrium time at 20.0 min, sample vial pressurization pressure at 138 kPa, pressurization time at 0.20 min, gas filling time at 0.20 min, sample ring equilibrium time at 0.05 min, and sample injection time at 1.0 min.

[0089] Under the above conditions, the migrating components on the target filter are fully desorbed from the filter substrate and diffused into the gas phase space inside the sample vial, achieving gas-solid two-phase equilibrium.

[0090] After the static headspace analyzer has finished running, the gaseous target migratings in the gas phase space inside the sample vial are introduced into the gas chromatography system along with the carrier gas for separation and analysis.

[0091] The optimal analytical conditions for gas chromatography are as follows: A VOC flexible fused silica capillary column or equivalent column is used, with a length of 60 mm, an inner diameter of 0.32 mm, and a film thickness of 1.8 μm. High-purity helium is used as the carrier gas, with a purity of not less than 99.99%. The injection port temperature is set to 200℃. Constant flow mode is used, with a column flow rate of 2.0 mL / min and a split ratio of 1:1.

[0092] The programmed temperature rise conditions were as follows: initial temperature 40℃, hold for 2 min, increase to 160℃ at a rate of 4℃ / min, then increase to 210℃ at a rate of 10℃ / min, hold for 10 min. The final operating temperature was 250℃, held for 10 min.

[0093] The components separated by gas chromatography were sequentially analyzed by a mass spectrometer. The optimal analytical parameters for the mass spectrometer were as follows: auxiliary interface temperature set to 280℃; electron impact ionization method with an ionization energy of 70 eV; ion source temperature set to 230℃; quadrupole temperature set to 150℃; and solvent delay time set to 4.0 min.

[0094] The mass spectrometer employs a combination of full-scan monitoring and selected ion monitoring modes for data acquisition. In full-scan monitoring mode, the scanning range is 35 amu to 350 amu, which covers the molecular ion peaks and characteristic fragment ion peaks of most fragrance and flavor components, enabling the screening and identification of unknown components in the migrated material.

[0095] In the selected ion monitoring mode, for each target compound's mass spectrometric ion fragments, ions with high specificity and response intensity are selected as quantitative ions, and one or two other fragment ions are selected as auxiliary qualitative ions to achieve highly sensitive quantitative analysis of known target components.

[0096] Qualitative identification of each chemical component in the migrating precipitate is achieved by comparing the retention times and mass spectra of each component's chromatographic peaks with standards or standard libraries. A standard curve for the target component is established, and its content in the migrating precipitate is calculated based on the peak area of ​​each component's chromatographic peak.

[0097] The application of the detection method of the present invention will be further explained below through specific embodiments.

[0098] Example 1

[0099] The detection method of this invention is used to detect the thermal migration of flavoring components added to the hollow O-section of heated cigarettes. In this embodiment, the Canadian deep-puff HCI mode is selected as the simulated puffing mode, with 8 puffs.

[0100] First, following step S1, implant the thermocouple sensor into the head end of the hollow O-rod segment of the cigarette to be tested. After inserting the cigarette into the matching heating device, use a smoking machine in HCI mode to inhale, and record the thermocouple temperature data during the inhalation cycle as follows: Figure 2 As shown in Table 1, the average temperature of each of the eight suction ports was obtained through integral calculation.

[0101] Then, following the method in step S2, the average temperature of each of the 8 suctions is sequentially set to the target temperature of the 8 stages in the time sequence table, with each stage lasting 2 seconds, the gas supply capacity being 55 ml, and the suction interval being 30 seconds.

[0102] The hollow O-rod segment to be tested and all filter rod segments after the hollow segment are installed as a whole between the sealing ring and the inlet of the cold trap chamber of the measuring device. Cambridge filters are placed in the filter holder. The suction mechanism in the measuring device adopts a linear suction machine.

[0103] After the detection program was completed, the Cambridge filter that was removed contained all the target mitochondria that had migrated from the hollow O-rod segment additives during the eight suction processes.

[0104] The Cambridge filter was placed in a static headspace analyzer and heated to equilibrium under the preferred conditions of the static headspace analyzer. The gaseous target precipitates were then introduced into a gas chromatograph-mass spectrometer for analysis, as shown in Table 2.

[0105] Table 1. Average Temperature Results

[0106] Table 2 Target Migrant Analysis Results

[0107] Analysis results show that the detection method of this invention can identify multiple characteristic components originating from the flavoring added to the hollow O-bar segment from the migrants captured by the Cambridge filter. The chromatographic peaks of each component are clearly distinguishable, and there is no co-eluting problem of tobacco substrate interference components. This embodiment verifies the technical effect of the detection method of this invention in effectively capturing and accurately qualitatively analyzing the migrating components of functional segment additives while eliminating tobacco substrate interference. The migration component chromatograms obtained by this embodiment can intuitively reflect the overall migration behavior of each flavoring component in the hollow O-bar flavoring formula during a complete smoking cycle, providing direct experimental basis for the optimization and adjustment of the flavoring formula.

[0108] Example 2

[0109] The detection method of this invention is used to detect the puff-by-puff thermal migration of flavoring components added to the hollow O-section of heated cigarettes. In this embodiment, the temperature measurement in step S1 and the setting of the time sequence table in step S2 are the same as in embodiment 1.

[0110] The difference lies in the fact that the suction mechanism of the measuring device in step S2 adopts a sequential suction machine, in which eight Cambridge filters are installed in sequence in the filter holder inside the cold trap chamber, and the positions of the eight Cambridge filters are controlled by the moving guide rails on the sequential suction machine.

[0111] After installing the hollow O-bar segment to be tested and all subsequent filter rod segments as a whole, the testing program is started. The target airflow containing the migrating material formed by the first suction flows through the first Cambridge filter, so that the migrating material corresponding to the first suction is captured on the first Cambridge filter.

[0112] After the first suction cycle, the moving guide rail of the sequential suction machine moves, causing the second Cambridge filter to move to the effective collection position in the airflow channel. The migrating material corresponding to the second suction cycle is then collected on the second Cambridge filter.

[0113] This process continues until all eight aspirations are completed, with the migrating material from each of the eight aspirations being captured on eight separate Cambridge filters.

[0114] Eight Cambridge filters were placed in a static headspace analyzer and heated, and then sequentially introduced into a gas chromatograph-mass spectrometer for analysis. The content of the target migrating component corresponding to each aspiration was obtained, as shown in Table 3.

[0115] Table 3 Content of Target Migrating Components

[0116] By comparing and analyzing the puff-by-puff data, the migration and release patterns of the main components in the additives at different puff counts can be clearly observed. For example, the migration and release of D-limonene peaks during the second and third puffs, and then decreases with each subsequent puff. This puff-by-puff release pattern provides a scientific explanation for the differences in aroma consistency before and after smoking in flavored products of this functional segment, and also points the way to specifically adjusting the flavor formulation to improve the aroma decay problem at the end. This embodiment verifies the unique technical advantages of the detection method of the present invention in independent puff-by-puff collection and puff-by-puff release pattern analysis. This method can provide indispensable experimental data support for the refined research and development of flavoring technology for heated cigarette functional segments.

[0117] This patent specification uses directional terms such as "front," "rear," "upper," "lower," "left," "right," "side," "top," and "bottom" to describe various example structural parts and components of this patent. However, the use of these terms is merely for illustrative purposes and is based on the orientation of the examples shown in the accompanying drawings. Since the embodiments disclosed in this patent can be arranged in different orientations, these directional terms are for illustrative purposes only and should not be considered as limitations. For example, "upper" and "lower" are not necessarily limited to directions opposite to or the same as the direction of gravity.

[0118] It should also be noted that the various specific technical features described in the above specific embodiments can be combined in any suitable way without contradiction. In order to avoid unnecessary repetition, this patent will not describe the various possible combinations separately.

[0119] Furthermore, various implementations of this patent can be combined in any way, and as long as they do not violate the spirit of this patent, they should also be regarded as the content disclosed in this patent.

Claims

1. A method for detecting the thermal migration of additives in the functional sections of heated cigarettes, characterized in that, Includes the following steps: Step S1: Measure the temperature of each puff of flue gas entering the target heated cigarette section using the thermocouple method, and calculate the average temperature per puff based on the measured temperature. Step S2: Set a timing table according to the average temperature of each cigarette and collect the migration material of the target heated cigarette functional section through a detection device according to the timing table to obtain the target filter; Step S3: The target filter is placed in a static headspace analyzer and heated to form target migrations, which are then analyzed by gas chromatography-mass spectrometry.

2. The detection method according to claim 1, characterized in that, Step S1 includes the following steps: Step S11: Insert the first end of the target heated cigarette functional section through the pinhole using a pin, place the thermocouple sensor into the pinhole, and then seal it with a hot melt glue gun. Step S12: Insert the target heated cigarette functional section into the heating device and then inhale through the smoking machine; Step S13: Record the temperature of each inlet during the suction cycle and calculate the average temperature of each inlet by integration.

3. The detection method according to claim 2, characterized in that, In step S11, the end where the smoke enters the target heated cigarette functional section is the beginning end, and the end where the smoke exits the target heated cigarette functional section is the end end. The pin is inserted into the target heated cigarette functional section from the beginning end until the pin's pillow contacts the obstacle for the second time and is then pulled out, so that the thermocouple sensor is placed in the target heated cigarette functional section along the pin hole and located at the axial center of the target heated cigarette functional section.

4. The detection method according to claim 2, characterized in that, Step S2 includes the following steps: Step S21: Set the "Stage-Duration-Target Temperature-Flow Rate" timing table; Step S22: Place the target heated cigarette functional section and filter into the detection device; Step S23: Run the detection device according to the timing table so that the migration formed from the target heated cigarette functional section is enriched on the filter to obtain the target filter.

5. The detection method according to claim 4, characterized in that, In step S21, the stage is the number of suction ports; the target temperature is the average temperature per port.

6. The detection method according to claim 5, characterized in that, In step S22, the detection device includes a suction mechanism, which is a linear smoking machine or a puff-by-puff smoking machine; the suction mode of the suction mechanism is the ISO standard suction mode or the Canadian deep suction HCI mode; the suction mode of the suction mechanism is the same as the suction mode of the smoking machine in step S12.

7. The detection method according to claim 6, characterized in that, If the suction mechanism is a linear smoking machine, the migration material formed within the number of suction ports is concentrated on the same filter; if the suction mechanism is a puff-by-puff smoking machine, the migration material formed in a single suction is concentrated on a single filter, and the number of filter sheets is equal to the number of suction ports.

8. The detection method according to claim 4, characterized in that, The filter is a Cambridge filter; the filter is placed in the filter holder of the detection device; the target heated cigarette functional section is located between the sealing ring of the detection device and the filter holder, the first end of the target heated cigarette functional section is connected to the sealing ring and the last end of the target heated cigarette functional section is connected to the filter holder, so that the smoke enters from the first end, flows through the target heated cigarette functional section and flows out from the last end.

9. The detection method according to claim 1, characterized in that, In step S3, the parameters of the static headspace analyzer include: sample equilibrium temperature set to 175℃, sample loop volume to 3.0 mL, sample loop temperature set to 180℃, transfer line temperature set to 185℃, sample equilibrium time to 20.0 min, sample vial pressurization pressure to 138 kPa, pressurization time to 0.20 min, gas filling time to 0.20 min, sample loop equilibrium time to 0.05 min, and sample injection time to 1.0 min. The gas chromatograph uses a chromatographic column, which is a VOC elastic fused silica capillary column or an equivalent column. The chromatographic column has a length of 60 mm, an inner diameter of 0.32 mm, and a film thickness of 1.8 μm. High-purity helium with a purity of not less than 99.99% is used as the carrier gas. The injection port temperature is set to 200℃. The constant flow mode is used with a column flow rate of 2.0 mL / min and a split ratio of 1:

1. The temperature program is as follows: Initial temperature 40℃, hold for 2 min, increase to 160℃ at a rate of 4℃ / min, increase to 210℃ at a rate of 10℃ / min, hold for 10 min, then run at 250℃ and hold for 10 min. The parameters of the mass spectrometer are as follows: auxiliary interface temperature: 280℃; ionization method: electron impact source, ionization energy: 70eV; ion source temperature: 230℃; quadrupole temperature: 150℃; solvent delay time: 4.0 min; the mass spectrometer adopts full scan monitoring mode and / or selected ion monitoring mode; the scanning range of the full scan monitoring mode is 35 amu to 350 amu; the selected ion monitoring mode selects ions with high specificity and response as quantitative ions, and selects 1 to 2 other fragment ions as auxiliary qualitative ions.

10. The detection method according to claim 1, characterized in that, The target heated cigarette functional segment is selected from one or more of the following: cellulose acetate filter segment, hollow segment, or support segment.

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