A heating cigarette aerosol component extraction device and a method for determining the moisture content of heating cigarette aerosol.

Abstract

This invention discloses an extraction device for heated cigarette aerosol components and a method for determining the moisture content of heated cigarette aerosols. The extraction device mainly consists of a collector, a container, and a peristaltic pump. The collector is connected in series with the container and the peristaltic pump via a flexible tube. The main body of the collector is formed by a sealed connection of components A and B, which together form an extraction chamber within the collector. Components A and B are respectively provided with interfaces A and B communicating with the extraction chamber. A filter is placed between interfaces A and B within the extraction chamber. This extraction device can directly capture aerosols released during the smoking process of heated cigarettes using the collector, and can efficiently extract components from the aerosols without opening the collector, reducing the loss of the analyte components in the aerosols during the collection and extraction process, thus minimizing the impact on the measurement results.

Description

Technical Field

[0001] This invention relates to an extraction device for aerosol components of heated cigarettes and a method for determining the moisture content of heated cigarette aerosols, belonging to the field of heated cigarette analysis and detection technology. Background Technology

[0002] The moisture content in heated cigarette aerosol has a significant impact on sensory quality. When the moisture content is low, the cigarette feels noticeably drier during inhalation; when the moisture content is high, the heated cigarette may burn the lips or tongue. Philip Morris International's research indicates that the total total physical mass (TPM) of THS2.2 aerosol is 56.18 mg / cigarette, with a moisture content as high as 44.65 mg / cigarette, accounting for nearly 80%. Since the tar release in traditional cigarettes equals TPM minus nicotine release minus moisture release, accurate determination of the moisture content in aerosols is crucial for assessing the harmfulness of heated cigarettes.

[0003] Currently, the domestic tobacco industry mainly uses YC / T345-2010 "Determination of Moisture Content in Tobacco and Tobacco Products by Gas Chromatography" to determine the moisture release from heated cigarette aerosols. The main process involves removing the Cambridge filter from the collector, adding a certain amount of extraction solution for extraction, and then performing gas chromatography analysis. There is currently no standard for the determination of moisture content in heated cigarette aerosols.

[0004] Wang Kang and colleagues from the Hubei Provincial Tobacco Quality Supervision and Testing Station conducted cigarette smoking experiments following the Canadian deep-smoking model. Cambridge filters, containing the total particulate matter from three cigarette samples, were placed in an extraction bottle. 20 mL of isopropanol extractant containing an internal standard was added, and the mixture was shaken for 40 min. 1 mL of the extract was then transferred to a chromatographic bottle for GC-TCD analysis, determining the moisture content in the heated cigarette aerosol to be approximately 25.83–31.19 mg / cigarette. This method provides a certain approach to determining the moisture content in heated cigarette aerosols. However, because heated cigarettes contain hygroscopic atomizing agents such as glycerol and propylene glycol, the aerosol moisture content is slightly higher than that of traditional cigarettes. Furthermore, since some moisture in the aerosol condenses on the inner wall of the collector, and extraction only extracts moisture from the filter, the measured results may be lower than expected. Additionally, because the collector needs to be opened and the filter removed during testing, some moisture inevitably escapes into the air, further contributing to the lower measured results. Summary of the Invention

[0005] To address the problems existing in the prior art, the first objective of this invention is to provide an extraction device suitable for heated cigarette aerosol components. This device not only enables both collection and extraction to be carried out under relatively closed conditions, reducing the volatilization loss of components in the aerosol during operation, but also enables cyclic extraction, achieving efficient extraction of the analyte components from the aerosol on the collection filter, effectively improving the accuracy of the measurement results. Furthermore, it has a wide range of applications, and can be used to detect the water content in any type of cigarette aerosol, as well as to determine the content of key components such as nicotine, glycerol, and propylene glycol in cigarette aerosol.

[0006] The second objective of this invention is to provide a method for determining the moisture content of heated cigarette aerosols. This method utilizes a special collector to achieve both the collection and extraction of aerosols in the smoke within the same collector, and is completed under relatively closed conditions. It also achieves efficient and cyclical extraction of moisture from the aerosols, effectively avoiding the problem of low measurement results caused by aerosol collection and extraction processes. In addition, this method has the advantages of simple operation and accurate measurement results, and can meet the requirements of rapid and accurate industrial measurement.

[0007] To achieve the above technical objectives, the present invention adopts the following technical solution:

[0008] This invention provides a heated cigarette aerosol component extraction device, including a collector, a container, and a peristaltic pump. The collector is connected in series with the container and the peristaltic pump via a flexible tube. The main body of the collector is formed by sealing and connecting component A (1-1) and component B (1-2). After the sealing and connection of component A and component B, an extraction chamber is formed inside the collector. Component A and component B are respectively provided with interface A (1-1-2) and interface B (1-2-1) communicating with the extraction chamber. A filter is provided inside the extraction chamber between interface A and interface B.

[0009] The key feature of this invention's heated cigarette aerosol component extraction device lies in its specially designed collector. Compared to traditional collectors, it features a larger extraction chamber, which can accommodate a greater amount of extractant. In particular, the extractant, driven by a peristaltic pump, creates turbulence within the extraction chamber, achieving highly efficient extraction of aerosol components from the filter and significantly improving extraction efficiency. Simultaneously, the combined design of the collector, container, and peristaltic pump enables cyclic extraction of aerosol components from the filter, reducing the amount of extractant used compared to conventional extraction processes and effectively minimizing the loss of analytes during extraction. Furthermore, the collector design is applicable to both the cigarette smoker and the extraction device; the collector does not need to be opened during the entire collection and extraction process, reducing the loss of analytes and errors caused by these processes.

[0010] As a preferred embodiment, component A of the trap has a cavity A (1-1-1) with an opening on one side, and component B has a cavity B (1-2-2) with an opening on one side, and the inner diameter of the opening side of cavity A matches the outer diameter of the opening side of cavity B.

[0011] As a preferred embodiment, component B has a sealing ring on its open side outer wall. Component B is sealed and inserted into component A, allowing cavity A and cavity B to communicate and form a sealed extraction chamber. The filter (1-2-3) is installed inside the open side of cavity B. The sealing ring on the open side outer wall of component B effectively prevents flue gas escape and extractant leakage.

[0012] As a preferred embodiment, hose connector A (1-3) and hose connector B (1-4) are respectively sealed and fitted on interface A and interface B.

[0013] As a preferred embodiment, an iron frame (4) is included, which is used to fix the trap.

[0014] As a preferred embodiment, the trap is horizontally fixed on an iron frame; the trap has one side of hose connector A facing upward and one side of hose connector B facing downward, hose connector A is connected to the peristaltic pump through a hose, and hose connector B is connected to the container (2) through a hose; or, the trap has one side of hose connector B facing upward and one side of hose connector A facing downward, hose connector B is connected to the peristaltic pump through a hose, and hose connector A is connected to the container through a hose.

[0015] As a preferred embodiment, the container is a top-sealed conical flask, and the container is provided with two liquid pipes. One end of each liquid pipe is inserted from the top of the container into the bottom of the container, and the other end of each liquid pipe is connected to a peristaltic pump and a trap respectively via a flexible hose.

[0016] As a preferred embodiment, both components A and B of the collector are made of stainless steel. Compared to traditional flue gas moisture collectors that mostly use polymer materials, the use of stainless steel provides better thermal conductivity, making it easier to condense and collect aerosols in the flue gas.

[0017] As a preferred embodiment, both cavity A and cavity B are conical structures, and the total volume of the extraction chamber formed by them is 3-5 cm³. 3 The conical design of the cavity not only facilitates the condensation and capture of aerogels but also promotes the formation of specific turbulence in the extractant, thereby improving the extraction efficiency of components in the aerosol. The size of the extraction chamber allows it to hold an appropriate amount of extractant, increasing the contact area and time between the extractant and the filter, thus enhancing extraction efficiency.

[0018] This invention also provides a method for determining the moisture content of heated cigarette aerosol, comprising the following steps:

[0019] 1) Install the trap in the smoking machine to capture the aerosols released during the smoking of heated cigarettes;

[0020] 2) After the suction is completed, the trap is disassembled and the extraction device is set up to extract the water in the aerosol captured by the trap in a circulating manner.

[0021] 3) Analyze the extract and calculate the water content in the aerosol.

[0022] The method for determining the moisture content of heated cigarette aerosols provided by this invention, by using a special collector, can complete the collection of aerosols in the smoke and the extraction of moisture from the aerosols in the same collector. The entire process is carried out under relatively closed conditions, which can reduce the detection error of aerosol moisture content. At the same time, the extraction device built using the collector can realize the cyclic extraction of moisture from the aerosols, improve the extraction efficiency, reduce the amount of extractant used, and reduce subsequent detection errors.

[0023] As a preferred embodiment, during the cyclic extraction process, 10-50 ml of extractant is added to the container (2), and the flow rate of the extract is controlled by a peristaltic pump (3) to be 1-5 ml / s, with a cyclic extraction time of 5-30 min.

[0024] As a preferred embodiment, the circulating extraction method employs a clockwise flow extraction method, a counterclockwise flow extraction method, or a combination of clockwise and counterclockwise flow extraction methods.

[0025] As a preferred embodiment, the extractant is methanol and / or isopropanol.

[0026] As a preferred embodiment, the number of heated cigarettes smoked is less than or equal to 5.

[0027] As a preferred embodiment, the analytical method is internal standard chromatographic analysis, and the chromatogram is gas chromatography or high performance liquid chromatography.

[0028] As a preferred embodiment, in the internal standard method, methanol is used as the internal standard for the extract, dimethylquinoline is used as the internal standard for nicotine, and 1,4-butanediol is used as the internal standard for glycerol and propylene glycol. Since the source of flue gas varies slightly due to differences in the state of tobacco or tobacco products during heating or combustion, it is difficult to prepare flue gas standard references. However, the internal standard method using gas chromatography employs a certain amount of pure substance, which can accurately determine the content of each component in the flue gas when no standard reference is available.

[0029] Compared with existing technologies, the beneficial technical effects of the present invention are as follows:

[0030] 1) The extraction device for heated cigarette aerosol components provided by the present invention uses a specially designed collector, which can not only determine the water content in cigarette aerosol, but also determine the content of key components such as nicotine, glycerol and propylene glycol in cigarette aerosol.

[0031] 2) In the technical solution provided by the present invention, the collection and extraction of aerosols in flue gas are carried out in the same collector by using a special collector and under relatively closed conditions, thereby achieving efficient extraction of water in aerosols and effectively avoiding the problem of low measurement results caused by aerosol collection and extraction. Attached Figure Description

[0032] Figure 1 For heating cigarette aerosol component extraction device;

[0033] 1 is the trap, 2 is the container, 3 is the peristaltic pump, and 4 is the iron frame.

[0034] Figure 2 Cross-sectional views of the various components of the trap;

[0035] 1-1 is component A, 1-2 is component B, 1-3 is hose connector A, 1-4 is hose connector B, 1-1-1 is cavity A, 1-1-2 is interface A, 1-2-1 is interface B, 1-2-2 is cavity B, and 1-2-3 is filter. Detailed Implementation

[0036] The present invention will be further described below with reference to specific embodiments. These embodiments are intended to illustrate the invention and not to further limit it.

[0037] Determination of optimal extraction conditions:

[0038] 1. Experimental Methods

[0039] (1) Preparation of experimental reagents

[0040] Extraction solution: Isopropanol was used as the extraction solution, methanol was used as the internal standard for water with a concentration of 6 mg / ml, dimethylquinoline was used as the internal standard for nicotine with a concentration of 0.2 mg / ml, and 1,4-butanediol was used as the internal standard for glycerol and propylene glycol with a concentration of 2 mg / ml.

[0041] Standard: Prepare an isopropanol solution with a water concentration of 10 mg / ml, a nicotine concentration of 0.4 mg / ml, a glycerol concentration of 10 mg / ml, and a propylene glycol concentration of 10 mg / ml.

[0042] (2) Experimental methods

[0043] Place the Cambridge filter into the trap, press it twice to ensure a tight seal, take 1 ml of standard sample and slowly and evenly spread it onto the Cambridge filter through the small hole at the top of the trap, place it in the measuring device, put 20 ml of extraction solution into the Erlenmeyer flask, and carry out the extraction experiment.

[0044] Moisture blank sample: The result obtained by extracting the sample by placing the Cambridge filter in the trap without adding a standard sample, and following the method described above.

[0045] (3) Selection of extraction time

[0046] The flow rate was set to 300 ml / min, the extract flow direction was clockwise, and the extraction times were 10, 15, 20, 25, and 30 min. After extraction, the water content of the extract in the Erlenmeyer flask was measured, and the results are shown in Table 1. Measured value = water content determined by gas phase - water content of blank sample. As shown in Table 1, the optimal extraction times are 20 and 25 min for orthogonal experimental investigation.

[0047] Table 1. Effect of extraction time on moisture determination results

[0048]

[0049]

[0050] (4) Selection of extractant flow rate

[0051] The extraction time was selected as 30 min, the extract flow direction was clockwise, and the extract flow rate was selected as 100, 150, 200, 250, and 300 ml / min. After extraction, the water content of the extract in the Erlenmeyer flask was measured, and the results are shown in Table 2. Measured value = water content determined by gas phase - water content of blank sample. As shown in Table 2, the optimal extract flow rate is 150 and 200 ml / min for orthogonal experimental investigation.

[0052] Table 2. Effect of extract flow rate on moisture determination results

[0053]

[0054] (5) Selection of the flow direction of the extract

[0055] The extraction time was 30 min, the extract flow rate was 300 ml / min, and the flow direction was selected as clockwise, counterclockwise, clockwise + counterclockwise for 15 min, and counterclockwise + clockwise for 15 min. After extraction, the water content of the extract in the Erlenmeyer flask was measured, and the results are shown in Table 2. Measured value = water content determined by gas phase - water content of blank sample. As shown in Table 3, the counterclockwise and counterclockwise + clockwise flow directions were used as conditions for orthogonal experiments.

[0056] Table 3. Effect of extract flow direction on moisture determination results

[0057]

[0058] (6) Orthogonal experiment

[0059] The results of the single-factor experiments were used to conduct a three-factor, two-level orthogonal experiment, and the results are shown in Table 4. Table 4 shows that the influencing factors are: extraction time > flow direction > extraction flow rate. The preferred extraction conditions are an extraction time of 20 min, a flow rate of 150 ml / min, and a combination of counterclockwise and clockwise rotation.

[0060] Table 4 Results of the orthogonal experiment

[0061]

[0062]

[0063] The following examples all use an extraction method with an extraction time of 20 min, a flow rate of 2.5 ml / s, and an extraction flow direction of 10 min counterclockwise followed by 10 min clockwise.

[0064] Example 1

[0065] Heated cigarettes manufactured by domestic company A were selected. After opening, the cigarettes were equilibrated for 48 hours in a 22°C, 45% moisture balance chamber. Five heated cigarettes were smoked using a heated cigarette smoking machine. A φ44mm Cambridge filter was placed in a custom-designed collector to capture the aerosol. After smoking, the collector was placed in the extraction device designed in this invention for extraction, and the results were compared with the industry standard YC / T345-2010 shaking extraction method. Isopropanol was used as the extractant, methanol was used as the internal standard for water at a concentration of 6 mg / ml, dimethylquinoline was used as the internal standard for nicotine at a concentration of 0.2 mg / ml, and 1,4-butanediol was used as the internal standard for glycerol and propylene glycol at a concentration of 2 mg / ml. The results are shown in Table 5. The results show that the device of this invention measures 14.7% higher moisture content in heated cigarette aerosol than the shaking extraction method, indicating more accurate results. Furthermore, the device of this invention measures the contents of nicotine, glycerol, and propylene glycol similarly to the shaking extraction method.

[0066] Table 5 Comparison of results from oscillation extraction and the method of the present invention.

[0067]

[0068] Example 2

[0069] Heated cigarettes manufactured by domestic company B were selected. After opening, the cigarettes were equilibrated for 48 hours in a 22°C, 45% moisture balance chamber. Five heated cigarettes were smoked using a heated cigarette smoking machine. A φ44mm Cambridge filter was placed in a custom-designed collector to capture the aerosol. After smoking, the collector was placed in the extraction device designed in this invention for extraction, and the results were compared with the industry standard YC / T345-2010 shaking extraction method. Isopropanol was used as the extractant, methanol was used as the internal standard for water at a concentration of 6 mg / ml, dimethylquinoline was used as the internal standard for nicotine at a concentration of 0.2 mg / ml, and 1,4-butanediol was used as the internal standard for glycerol and propylene glycol at a concentration of 2 mg / ml. The results are shown in Table 6. The results show that the device of this invention measures 14.4% higher water content in heated cigarette aerosol than the shaking extraction method, making the results more accurate. Furthermore, the device of this invention measures the contents of nicotine, glycerol, and propylene glycol similarly to the shaking extraction method.

[0070] Table 6 Comparison of results from oscillation extraction and the method of the present invention.

[0071]

[0072] Example 3

[0073] Heated cigarettes manufactured by foreign company C were selected. After opening, the cigarettes were equilibrated for 48 hours in a 22°C, 45% moisture balance chamber. Five heated cigarettes were smoked using a heated cigarette smoking machine. A φ44mm Cambridge filter was placed in a custom-designed collector to capture the aerosol. After smoking, the collector was placed in the extraction device designed in this invention for extraction, and the results were compared with the industry standard YC / T345-2010 shaking extraction method. Isopropanol was used as the extractant, methanol was used as the internal standard for water at a concentration of 6 mg / ml, dimethylquinoline was used as the internal standard for nicotine at a concentration of 0.2 mg / ml, and 1,4-butanediol was used as the internal standard for glycerol and propylene glycol at a concentration of 2 mg / ml. The results are shown in Table 7. The results show that the device of this invention measures 12.6% higher moisture content in heated cigarette aerosol than the shaking extraction method, making the results more accurate. Furthermore, the device of this invention measures the contents of nicotine, glycerol, and propylene glycol similarly to the shaking extraction method.

[0074] Table 7 Comparison of results from oscillation extraction and the method of the present invention.

[0075]

Claims

1. A method for determining the moisture content of heated cigarette aerosol, characterized in that: Includes the following steps: 1) Install the trap in the smoking machine to capture the aerosols released during the smoking of heated cigarettes; 2) After the suction is completed, the trap is disassembled and an extraction device is set up to extract the water in the aerosol captured by the trap in a circulating manner. 3) Analyze the extract and calculate the water content in the aerosol; The extraction device includes a trap (1), a container (2), and a peristaltic pump (3); the trap is connected in series with the container and the peristaltic pump via a hose; The main body of the trap is formed by sealing and connecting component A (1-1) and component B (1-2). After sealing and connecting component A and component B, an extraction chamber is formed inside the trap. Component A and component B are respectively provided with interface A (1-1-2) and interface B (1-2-1) communicating with the extraction chamber. A filter (1-2-3) is provided between interface A and interface B inside the extraction chamber. The trap has a cavity A (1-1-1) with one side open inside component A, and a cavity B (1-2-2) with one side open inside component B. The inner diameter of the opening side of cavity A matches the outer diameter of the opening side of cavity B. A sealing ring is provided on the outer wall of the opening side of component B. Component B is sealed and inserted into component A, so that cavity A and cavity B are connected to form a sealed extraction chamber. The filter (1-2-3) is disposed inside the opening side of cavity B. The container is a top-sealed conical flask. The container is equipped with two liquid pipes. One end of each liquid pipe is inserted from the top of the container into the bottom of the container. The other ends of the two liquid pipes are connected to a peristaltic pump and a trap respectively via flexible hoses. Both cavity A and cavity B are conical structures, and the total volume of the extraction chamber formed by them is 3-5 cm³. 3 .

2. The method for determining the moisture content of heated cigarette aerosol according to claim 1, characterized in that: The interface A and interface B are respectively sealed with hose connector A (1-3) and hose connector B (1-4).

3. The method for determining the moisture content of heated cigarette aerosol according to claim 1, characterized in that: Includes an iron frame (4), which is used to fix the trap.

4. The method for determining the moisture content of heated cigarette aerosol according to claim 3, characterized in that: The trap is horizontally fixed on an iron frame; the trap's hose connector A faces upward and the hose connector B faces downward; the hose connector A is connected to the peristaltic pump (3) via a hose, and the hose connector B is connected to the container (2) via a hose; or, the trap's hose connector B faces upward and the hose connector A faces downward; the hose connector B is connected to the peristaltic pump via a hose, and the hose connector A is connected to the container via a hose.

5. The method for determining the moisture content of heated cigarette aerosol according to claim 1, characterized in that: Both component A and component B of the trap are made of stainless steel.

6. The method for determining the moisture content of heated cigarette aerosol according to claim 1, characterized in that: During the cyclic extraction process, 10-50 ml of extractant is added to the container, and the flow rate of the extract is controlled by a peristaltic pump at 1-5 ml / s, with a cyclic extraction time of 5-30 min.

7. The method for determining the moisture content of heated cigarette aerosol according to claim 1, characterized in that: The circulating extraction method employs a clockwise flow extraction method, a counterclockwise flow extraction method, or a combination of both clockwise and counterclockwise flow extraction methods.

8. The method for determining the moisture content of heated cigarette aerosol according to claim 6, characterized in that: The extractant is methanol and / or isopropanol.

9. The method for determining the moisture content of heated cigarette aerosol according to claim 1, characterized in that: The number of heated cigarettes to be smoked is less than or equal to 5.

10. The method for determining the moisture content of heated cigarette aerosol according to claim 1, characterized in that: The analytical method is internal standard chromatographic analysis, and the chromatogram is gas chromatography or high performance liquid chromatography.

11. The method for determining the moisture content of heated cigarette aerosol according to claim 10, characterized in that: In the internal standard method, the internal standard for the extract is methanol, the internal standard for nicotine is dimethylquinoline, and the internal standards for glycerol and propylene glycol are 1,4-butanediol.

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