A puff-by-puff cigarette smoke capture device and method
By designing an mouth-by-mouth smoke capture device for cigarette smoke, the problem of difficulty in mouth-by-mouth analysis of cigarette smoke is solved, and the rapid and accurate detection of cigarette smoke components is achieved, and the accuracy and reliability of the analysis are improved.
Patent Information
- Application Number
- CN202010975398.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2020-09-16
- Publication Date
- 2025-02-18
- Estimated Expiration
- 2040-09-16
AI Technical Summary
The prior art is difficult to realize the port-by-port aspiration analysis of cigarette smoke, resulting in high detection difficulty and low accuracy.
A port-by-mouth headspace bottle holder, a negative pressure headspace bottle, a cigarette holder and an airflow pipeline were designed to capture the smoke through port-by-mouth headspace and conduct online analysis. Achieve accurate detection of cigarette smoke components.
The device realizes rapid and accurate capture and analysis of cigarette smoke, reduces the loss of volatile semi-volatile components, and improves the accuracy and reliability of the analysis.
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Figure CN111929120B_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the field of analytical chemistry, and in particular relates to a device and method for capturing cigarette smoke by puffing one by one. Background Art
[0002] Smokers' sensory experience of cigarettes mainly comes from cigarette smoke. Smokers feel that there are certain differences in the aroma and taste of each puff of smoke. The reason for this difference can be summarized as a dynamic balance between the tobacco itself, the filter, the cigarette paper, and human factors in the process of smoking. Since smoking a cigarette is a constantly changing process, only by analyzing the smoke components puff by puff can the actual change law of cigarette smoke be accurately revealed. The study of cigarette smoke puff by puff has become a major direction of tobacco chemistry research. In-depth understanding of the content differences and transmission laws of each puff of mainstream cigarette smoke is a research that tobacco scientists have been engaged in.
[0003] In order to achieve puff-by-puff analysis of mainstream cigarette smoke, a device needs to be developed to capture puff-by-puff cigarette smoke. Since gas samples are not easy to collect and preserve, the content of volatile and semi-volatile substances in puff-by-puff smoke is low and difficult to detect. Therefore, it is particularly important to develop a device dedicated to puff-by-puff cigarette smoke capture and component analysis application method. Summary of the invention
[0004] In order to solve the above problems, the present invention provides a puff-by-puff cigarette smoke capture device and method, which has the advantages of being fast, accurate, and easy to operate.
[0005] The technical solution adopted by the present invention is specifically as follows:
[0006] A puff-by-puff cigarette smoke capture device comprises a negative pressure headspace bottle holder, in which a plurality of negative pressure headspace bottles are evenly arranged, and cigarette clamps are arranged on the upper ends of the plurality of negative pressure headspace bottles, one end of the cigarette clamp clamps the cigarette, and the other end is provided with an airflow pipeline, and the airflow pipeline is inserted into the negative pressure headspace bottles in sequence to capture the smoke; each negative pressure headspace bottle captures a puff of cigarette smoke.
[0007] Furthermore, the cigarette holder is provided with a holder regulating valve to adjust the diameter of the holder to 5-9 mm.
[0008] Furthermore, the pressure of the negative pressure headspace bottle is 40-200 kPa, and the volume is 20-60 mL.
[0009] Furthermore, the airflow pipeline has a diameter of 0.2-1 cm and a length of 5-20 cm, and a pointed mouth near the negative pressure headspace bottle end, which is convenient for inserting into the negative pressure headspace bottle cap.
[0010] Furthermore, a plurality of negative pressure headspace bottles are connected via solenoid valves.
[0011] The present invention also relates to a flue gas capture method based on the above device, which is carried out as follows:
[0012] The size of the cigarette holder is adjusted according to the diameter of different cigarettes. While lighting the cigarette, the pointed end of the airflow pipeline is inserted into the negative pressure headspace bottle through one of the negative pressure headspace bottle caps. After continuous collection for 1 to 3 seconds, the airflow pipeline is pulled out and the negative pressure headspace bottle is removed to perform online analysis of the volatile and semi-volatile components of the smoke from the first puff of cigarette.
[0013] After smoldering for 27 to 59 seconds, insert the pointed end of the airflow pipeline into the negative pressure headspace bottle through the cap of the next negative pressure headspace bottle. After continuous collection for 1 to 3 seconds, pull out the airflow pipeline and remove the negative pressure headspace bottle to perform online analysis of volatile and semi-volatile components in the second puff of cigarette smoke.
[0014] Repeat the above steps to capture the smoke of each puff of a complete cigarette and analyze it with the instrument.
[0015] The present invention also relates to a flue gas capture method based on the above device, which is carried out as follows:
[0016] Adjust the size of the cigarette holder according to the diameter of different cigarettes, close all control valves or solenoid valves, and while lighting the cigarette, insert the pointed end of the airflow pipeline through one of the negative pressure headspace bottle caps into the negative pressure headspace bottle, and continue to capture for 1 to 3 s before pulling out the airflow pipeline; after smoldering for 27 to 59 s, insert the pointed end of the airflow pipeline through another negative pressure headspace bottle cap into the negative pressure headspace bottle, and continue to capture for 1 to 3 s before pulling out the airflow pipeline; repeat the above steps to capture each puff of smoke from a complete cigarette in turn, and remove the negative pressure headspace bottle to perform online analysis of volatile and semi-volatile components in the smoke of each puff of the cigarette.
[0017] The present invention also relates to a flue gas capture method based on the above device, which is carried out as follows:
[0018] Adjust the size of the cigarette holder according to the diameter of different cigarettes, close all control valves or solenoid valves, and while lighting the cigarette, insert the pointed end of the airflow pipeline through one of the negative pressure headspace bottle caps into the negative pressure headspace bottle, and continue to capture for 1 to 3 seconds before pulling out the airflow pipeline; after smoldering for 27 to 59 seconds, insert the pointed end of the airflow pipeline through another negative pressure headspace bottle cap into the negative pressure headspace bottle, and continue to capture for 1 to 3 seconds before pulling out the airflow pipeline; repeat the above steps to capture the smoke of each puff of the whole cigarette in turn, open the control valve or solenoid valve connecting the negative pressure headspace bottles that capture the smoke of each puff, let the smoke mix evenly in the negative pressure headspace bottle, remove the negative pressure headspace bottle to perform online analysis of the volatile and semi-volatile components of the whole cigarette smoke.
[0019] Furthermore, the online analysis was HS-SPME-GC / MS, and the analysis conditions were:
[0020] SPME-headspace conditions: extraction temperature: 40 °C, extraction time: 10-15 min, desorption time: 3 min, extraction head speed: 200-220 rpm;
[0021] Gas chromatography conditions: chromatographic column: DB-5MS capillary column, 30 m×0.32 mm×0.25 μm; injection port temperature: 220 °C; programmed temperature: initial temperature 40 °C, maintained for 1 min, increased to 230 °C at 3-5 °C / min, maintained for 5 min; carrier gas: high-purity helium, constant flow mode, column flow rate 1 mL / min; injection mode: split injection, split ratio 2-5:1;
[0022] Mass spectrometry conditions: ion source: EI source; ionization energy: 70 eV; ion source temperature: 210-220 °C; transfer line temperature: 220 °C; detection mode: full scan monitoring mode, mass scanning range: 30 amu~500 amu; solvent delay: 0.2-0.5 min.
[0023] Furthermore, the online analysis was HS-GC / MS, and the analysis conditions were:
[0024] The static headspace conditions were as follows: sample equilibration temperature: 40°C; sample loop: 3.0 mL; sample loop temperature: 40-50°C; transfer line temperature: 100-120°C; sample equilibration time: 10.0 min; sample bottle pressurization pressure: 35 psi; pressurization time: 2 min; gas filling time: 0.4-0.5 min; injection time: 0.20-0.30 min;
[0025] Gas chromatography conditions were as follows: chromatographic column: flexible capillary polyethylene glycol column or equivalent column, 30 m×0.25 mm×0.25 μm; carrier gas: helium, purity ≥99.999%; injection port temperature: 150°C; constant flow mode, column flow rate 1.0 mL / min, split ratio 5:1; programmed temperature rise: initial temperature 40°C, hold for 1 min, increase to 220-230°C at 3-5°C / min, hold for 5 min; column flow rate 1 mL / min;
[0026] The mass spectrometry conditions were as follows: auxiliary interface temperature: 210-220°C; ionization mode: electron bombardment source; ionization energy: 70 eV; ion source temperature: 210°C; quadrupole temperature: 180°C; solvent delay time: 0.1-0.2 min; mass scanning range: 30amu~500 amu.
[0027] Compared with the prior art, the beneficial effects of the present invention are as follows:
[0028] (1) The analysis steps of the present invention are simple. Samples can be analyzed after suctioning one by one. The steps are simple. At the same time, the present invention provides a one-stop suction and capture device, which is easy to promote.
[0029] (2) The present invention has high accuracy, completes capture in a closed system of fixed volume, and realizes direct sampling, which greatly reduces the loss of volatile and semi-volatile components in the smoke during the transfer process and increases the accuracy of the analysis process. The present invention draws smoke from 20 cigarettes one by one, and the analysis results show that the relative standard deviation of the integral area of nicotine, a representative volatile and semi-volatile component in the same smoke, is between 0.21% and 2.54%, and the relative standard deviation of the total integral area of volatile and semi-volatile components in the same smoke is between 0.23% and 2.87%. The device draws full smoke from 20 cigarettes of the same cigarette, and the analysis results show that the relative standard deviation of the integral area of nicotine, a representative volatile and semi-volatile component in the smoke, is between 0.11% and 2.12%, and the relative standard deviation of the total integral area of volatile and semi-volatile components in the smoke is between 0.19% and 2.36%.
[0030] (3) The present invention has low cost. The cigarette holder, airflow pipeline, negative pressure headspace bottle, negative pressure headspace bottle bracket, etc. involved in the device are made of materials that are easily available in the laboratory. It does not require an expensive smoking machine as a suction source, and the cost is low.
[0031] (4) The present invention is environmentally friendly. The device has good sealing performance, and volatile and semi-volatile components are not easy to evaporate. Moreover, the present invention does not involve sample pretreatment with solvents, etc., thus avoiding the loss caused by the volatilization of chemical components in the pretreatment step and realizing the full sampling and analysis of the captured substances by the device. Due to the sealing performance of the capture device and the full sampling of the captured substances, while improving the accuracy of the analysis, the pollution to the environment caused by the capture process is reduced.
[0032] (5) The present invention has wide applicability. The device and method are applicable to cigarettes of different specifications, such as thin, medium, ordinary, and thick, as well as to new tobacco products such as heat-not-burn cigarettes and electronic cigarettes, and are applicable to the capture of cigarette smoke puffed one by one under different smoking modes such as ISO and Canadian deep smoking. It is used to detect volatile and semi-volatile substances in cigarette smoke puffed one by one and volatile and semi-volatile substances in whole smoke, and has the advantages of rapidity, accuracy, and simple operation. BRIEF DESCRIPTION OF THE DRAWINGS
[0033] Figure 1 A schematic structural diagram of a first embodiment of a puff-by-puff cigarette smoke capture device;
[0034] Figure 2 It is a schematic structural diagram of inserting a negative pressure head space bottle according to the first embodiment;
[0035] Figure 3 A schematic structural diagram of a second embodiment of a puff-by-puff cigarette smoke capture device;
[0036] Figure 4 It is a structural schematic diagram of inserting a negative pressure head space bottle in the second embodiment;
[0037] Figure 5 is a chromatogram of smoke component analysis of a puff-by-puff cigarette according to Example 1 of the present invention;
[0038] Figure 6 is a chromatogram of smoke component analysis of a puff-by-puff cigarette according to Example 2 of the present invention;
[0039] Figure 7 is a chromatogram of smoke component analysis of a puff-by-puff cigarette according to Example 3 of the present invention;
[0040] Figure 8 is a chromatogram of smoke component analysis of a puff-by-puff cigarette according to Example 4 of the present invention;
[0041] In the figure: 1-cigarette, 2-cigarette holder, 3-airflow pipeline, 4-negative pressure headspace bottle, 5-negative pressure headspace bottle holder, 6-control valve or solenoid valve. DETAILED DESCRIPTION
[0042] Those skilled in the art will appreciate that the following examples are only used to illustrate the present invention and should not be considered to limit the scope of the present invention. If no specific techniques or conditions are specified in the examples, they are carried out according to the techniques or conditions described in the literature in this area or according to the product instructions. If the manufacturer of the reagents or instruments used is not specified, they are all conventional products that can be purchased.
[0043] The present invention will be further described below in conjunction with the accompanying drawings. Example 1
[0044] like Figure 1 As shown, the puff-by-puff cigarette smoke capture device of this embodiment is composed of a cigarette holder 2, an airflow pipeline 3, a negative pressure headspace bottle 4, and a negative pressure headspace bottle support 5. The negative pressure headspace bottle 4 can be an existing negative pressure headspace bottle, and the size meets the headspace sampling standard. For example, the negative pressure headspace bottle has a diameter of 0.8-6 cm, a height of 2-5 cm, and is made of pressure-resistant glass.
[0045] The negative pressure headspace bottle holder 5 fixes the negative pressure headspace bottle, and the negative pressure headspace bottle 4 controls the volume of each puff, and each negative pressure headspace bottle 4 captures a puff of cigarette smoke.
[0046] The cigarette holder 2 is provided with a regulating valve, and the diameter of the holder can be adjusted to 5-9 mm.
[0047] The pressure of the negative pressure headspace bottle 4 is 40-200 kPa, and the volume is 20-60 mL.
[0048] The airflow pipe 3 is made of silica gel, has a diameter of 0.2-1 cm, a length of 5-20 cm, and a pointed mouth near the negative pressure headspace bottle 4, which is convenient for inserting into the negative pressure headspace bottle cap. During use, keep the cigarette horizontal.
[0049] The fume capture method based on the above device is carried out as follows:
[0050] According to the diameter of different sample cigarettes 1, the size of the cigarette holder 2 is adjusted to 5 mm. While lighting the cigarette 1, the pointed end of the airflow tube 3 is inserted into the negative pressure headspace bottle through the cap of one of the 35 mL negative pressure headspace bottles 4. After continuous capture for 1 s, the airflow tube 3 is pulled out, and the negative pressure headspace bottle is removed to perform HS-SPME-GC / MS online analysis of the volatile and semi-volatile components of the smoke from the first puff of cigarette; after smoldering for 59 s, the pointed end of the airflow tube 3 is inserted into the negative pressure headspace bottle through the cap of another 35 mL negative pressure headspace bottle 4. After continuous capture for 1 s, the airflow tube 3 is pulled out, and the negative pressure headspace bottle is removed to perform HS-SPME-GC / MS online analysis of the volatile and semi-volatile components of the smoke from the second puff of cigarette; the above steps are repeated to capture the smoke of each puff of a complete cigarette in turn and enter the instrument for analysis.
[0051] The instrument analysis conditions are:
[0052] SPME-headspace conditions: extraction temperature: 40 °C, extraction time: 10 min, desorption time: 3 min, extraction head speed: 220 rpm.
[0053] Gas chromatography conditions: chromatographic column: DB-5MS capillary column (30 m×0.32 mm×0.25 μm); injection port temperature: 220 °C; program temperature rise: initial temperature 40 °C, hold for 1 min, increase to 230 °C at 3 °C / min, hold for 5 min. Carrier gas: high-purity helium, constant flow mode, column flow rate 1 mL / min; injection mode: split injection, split ratio 5:1.
[0054] Mass spectrometry conditions: ion source: EI source; ionization energy: 70 eV; ion source temperature: 210 °C; transfer line temperature: 220 °C; detection mode: full scan monitoring mode, mass scanning range: 30 amu~500 amu; solvent delay: 0.5 min.
[0055] The device was used to draw puffs of smoke from 20 identical cigarettes. The analysis results showed that the relative standard deviation of the integrated area of nicotine, a representative volatile and semi-volatile component in the same puff of smoke, was between 0.25% and 2.50%, and the relative standard deviation of the sum of the integrated areas of volatile and semi-volatile components in the same puff of smoke was between 0.28% and 2.67%. Example 2
[0056] The device of this embodiment is the same as that of embodiment 1.
[0057] The fume capture method based on the above device is carried out as follows:
[0058] According to the diameter of different cigarettes 1, the size of the cigarette holder 2 is adjusted to 7 mm. While lighting the cigarette 1, the pointed end of the airflow tube 3 is inserted into the negative pressure headspace bottle through the cap of one of the 55 mL negative pressure headspace bottles 4. After continuous capture for 2 s, the airflow tube 3 is pulled out, and the negative pressure headspace bottle is removed to perform HS-GC / MS online analysis of the volatile and semi-volatile components of the smoke from the first puff of cigarette; after smoldering for 28 s, the pointed end of the airflow tube 3 is inserted into the negative pressure headspace bottle through the cap of another 55 mL negative pressure headspace bottle 4. After continuous capture for 2 s, the airflow tube 3 is pulled out, and the negative pressure headspace bottle is removed to perform HS-GC / MS online analysis of the volatile and semi-volatile components of the smoke from the second puff of cigarette; the above steps are repeated to capture the smoke of each puff of a complete cigarette in turn and enter the instrument for analysis.
[0059] The instrument analysis conditions are:
[0060] The static headspace conditions were as follows: sample equilibration temperature: 40°C; sample loop: 3.0 mL; sample loop temperature: 50°C; transfer line temperature: 120°C; sample equilibration time: 10.0 min; sample bottle pressurization pressure: 35 psi; pressurization time: 2 min; inflation time: 0.4 min; and injection time: 0.30 min.
[0061] The gas chromatography conditions were as follows: chromatographic column: elastic capillary polyethylene glycol column or equivalent column, with specifications of [30 m (length) × 0.25 mm (inner diameter) × 0.25 μm (film thickness)]; carrier gas: helium (He), purity ≥99.999%; inlet temperature: 150 °C; constant flow mode, column flow rate 1.0 mL / min, split ratio 5:1; programmed temperature: initial temperature 40 °C, hold for 1 min, increase to 230 °C at 3 °C / min, hold for 5 min; column flow rate 1 mL / min.
[0062] The mass spectrometry conditions were as follows: auxiliary interface temperature: 220°C; ionization mode: electron impact source (EI); ionization energy: 70 eV; ion source temperature: 220°C; quadrupole temperature: 180°C; solvent delay time: 0.1 min; mass scanning range: 30 amu to 500 amu.
[0063] The device was used to draw puffs of smoke from 20 identical cigarettes. The analysis results showed that the relative standard deviation of the integrated area of nicotine, a representative volatile and semi-volatile component in the same puff of smoke, was between 0.31% and 2.24%, and the relative standard deviation of the sum of the integrated areas of volatile and semi-volatile components in the same puff of smoke was between 0.29% and 2.57%. Example 3
[0064] like Figure 3 As shown, the device for capturing cigarette smoke and whole smoke by puff of the present invention is composed of a cigarette 1, a cigarette holder 2, an airflow pipeline 3, a negative pressure headspace bottle 4, a control valve or a solenoid valve 6, and a negative pressure headspace bottle holder 5. The negative pressure headspace bottle holder 5 fixes the negative pressure headspace bottle, and the negative pressure headspace bottle 4 controls the volume of puff by puff. Each negative pressure headspace bottle 4 captures a puff of cigarette smoke, and the control valve or the solenoid valve 6 controls the connection state between multiple negative pressure headspace bottles 4.
[0065] The cigarette holder 2 is provided with a regulating valve, and the diameter of the holder can be adjusted to 5-9 mm.
[0066] The pressure of the negative pressure headspace bottle 4 is 40-200 kPa, and the volume is 20-60 mL; the connection state between the multiple negative pressure headspace bottles 4 is controlled by a control valve or a solenoid valve 6.
[0067] The gas flow pipe 3 is made of silica gel, has a diameter of 0.2-1 cm, a length of 5-20 cm, and a pointed mouth near the negative pressure headspace bottle 4, which is convenient for inserting into the negative pressure headspace bottle cap. Pipes are arranged on both sides of the negative pressure headspace bottle 4, and a solenoid valve 6 is arranged on the pipeline.
[0068] The fume capture method based on the above device is carried out as follows:
[0069] According to the diameter of different sample cigarettes 1, the size of the cigarette holder 2 is adjusted to 5 mm, and all control valves or solenoid valves 6 are closed. While lighting the cigarette 1, the pointed end of the airflow pipeline 3 is inserted into the negative pressure headspace bottle through the cap of one of the 35 mL negative pressure headspace bottles 4, and the airflow pipeline 3 is pulled out after continuous capture for 1 second. After smoldering for 59 seconds, the pointed end of the airflow pipeline 3 is inserted into the negative pressure headspace bottle through the cap of another 35 mL negative pressure headspace bottle 4, and the airflow pipeline 3 is pulled out after continuous capture for 1-3 seconds. Repeat the above steps to capture the smoke of each puff of a complete cigarette in turn, and remove the negative pressure headspace bottle to perform HS-SPME-GC / MS online analysis of volatile and semi-volatile components in the smoke of each puff of the cigarette.
[0070] The instrument analysis conditions are:
[0071] SPME-headspace conditions: extraction temperature: 40 ℃, extraction time: 15 min, desorption time: 3 min, extraction head speed: 200 rpm. Gas chromatography conditions: chromatographic column is DB-5MS capillary column (30 m×0.32 mm×0. 25μm); injection port temperature: 220 ℃; program temperature rise: initial temperature 40 ℃, hold for 1 min, increase to 230 ℃ at 5 ℃ / min, hold for 5 min. Carrier gas: high-purity helium, constant flow mode, column flow rate 1 mL / min; injection mode: split injection, split ratio 2:1. Mass spectrometry conditions: ion source: EI source; ionization energy: 70 eV; ion source temperature: 220 ℃; transfer line temperature: 220 ℃; detection mode: full scan monitoring mode, mass scanning range: 30 amu~500 amu; solvent delay: 0.2 min.
[0072] The device was used to draw smoke from 20 cigarettes, and the analysis results showed that the relative standard deviation of the integral area of nicotine, a representative volatile and semi-volatile component in the same puff of smoke, was between 0.21% and 2.44%, and the relative standard deviation of the total integral area of volatile and semi-volatile components in the same puff of smoke was between 0.36% and 2.87%. The device was used to draw smoke from 20 cigarettes, and the analysis results showed that the relative standard deviation of the integral area of nicotine, a representative volatile and semi-volatile component in the smoke, was between 0.23% and 2.02%, and the relative standard deviation of the total integral area of volatile and semi-volatile components in the smoke was between 0.29% and 2.16%. Example 4
[0073] The device of this embodiment is the same as that of embodiment 3.
[0074] The fume capture method based on the above device is carried out as follows:
[0075] According to the diameter of different cigarettes 1, the size of the cigarette holder 2 is adjusted to 7 mm, all control valves or solenoid valves 5 are closed, and while the cigarette 1 is lit, the pointed end of the airflow pipeline 3 is inserted into the negative pressure headspace bottle through the cap of one of the 55 mL negative pressure headspace bottles 4, and the airflow pipeline 3 is pulled out after continuous capture for 2 s; after smoldering for 28 s, the pointed end of the airflow pipeline 3 is inserted into the negative pressure headspace bottle through the cap of another 55 mL negative pressure headspace bottle 4, and the airflow pipeline 3 is pulled out after continuous capture for 2 s; repeat the above steps to capture the smoke of each puff of the whole cigarette in turn, open the control valve or solenoid valve 5 connecting the negative pressure headspace bottles that capture the smoke of each puff, let the smoke mix evenly in the negative pressure headspace bottle, remove the negative pressure headspace bottle to perform HS-GC / MS online analysis of volatile and semi-volatile components of the whole cigarette smoke.
[0076] The instrument analysis conditions are:
[0077] Static headspace conditions were as follows: sample balance temperature: 40°C; sample loop: 3.0 mL; sample loop temperature: 40°C; transfer line temperature: 100°C; sample balance time: 10.0 min; sample bottle pressurization pressure: 35 psi; pressurization time: 2 min; filling time: 0.5 min; injection time: 0.20 min. Gas chromatography conditions were as follows: chromatographic column: elastic capillary polyethylene glycol column or equivalent column, specifications [30 m (length) × 0.25 mm (inner diameter) × 0.25 μm (film thickness)]; carrier gas: helium (He), purity ≥ 99.999%; injection port temperature: 150°C; constant flow mode, column flow rate 1.0 mL / min, split ratio 5:1; program temperature rise: initial temperature 40°C, hold for 1 min, increase to 220°C at 5°C / min, hold for 5 min; column flow rate 1 mL / min. The mass spectrometry conditions were as follows: auxiliary interface temperature: 210°C; ionization mode: electron impact source (EI); ionization energy: 70 eV; ion source temperature: 210°C; quadrupole temperature: 180°C; solvent delay time: 0.2 min; mass scanning range: 30 amu to 500 amu.
[0078] The device was used to draw smoke from 20 cigarettes, and the analysis results showed that the relative standard deviation of the integral area of nicotine, a representative volatile and semi-volatile component in the same puff of smoke, was between 0.29% and 2.54%, and the relative standard deviation of the total integral area of volatile and semi-volatile components in the same puff of smoke was between 0.25% and 2.87%. The device was used to draw smoke from 20 cigarettes, and the analysis results showed that the relative standard deviation of the integral area of nicotine, a representative volatile and semi-volatile component in the smoke, was between 0.11% and 2.11%, and the relative standard deviation of the total integral area of volatile and semi-volatile components in the smoke was between 0.19% and 2.30%.
[0079] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims
1. A puff-by-puff cigarette smoke capture device, characterized in that: The invention comprises a negative pressure headspace bottle support (5), wherein a plurality of negative pressure headspace bottles (4) are evenly arranged in the negative pressure headspace bottle support (5), and a cigarette clamp (2) is arranged at the upper end of the plurality of negative pressure headspace bottles (4), wherein one end of the cigarette clamp (2) clamps the cigarette, and the other end is provided with an airflow pipeline (3), and the airflow pipeline (3) is inserted into the negative pressure headspace bottles (4) in sequence to capture smoke; each negative pressure headspace bottle (4) captures a mouthful of cigarette smoke; the cigarette clamp (2) is provided with a clamp regulating valve, and the diameter of the regulating clamp is 5-9 mm; the pressure of the negative pressure headspace bottle (4) is 40-200 kPa, and the volume is 20-60 mL; the diameter of the airflow pipeline (3) is 0.2-1 cm, the length is 5-20 cm, and the end near the negative pressure headspace bottle (4) is a pointed mouth, which is convenient for inserting into the negative pressure headspace bottle cap; and the plurality of negative pressure headspace bottles (4) are connected by a solenoid valve (6).
2. A flue gas capture method based on the device of claim 1, characterized in that: The process is as follows: the size of the cigarette holder (2) is adjusted according to the diameter of the cigarette (1), all the solenoid valves (6) are closed, and while the cigarette (1) is lit, the pointed end of the airflow tube (3) is inserted into the negative pressure headspace bottle (4) through the cap of one of the negative pressure headspace bottles (4), and the airflow tube (3) is pulled out after continuous collection for 1 to 3 seconds. After smoldering for 27 to 59 seconds, the pointed end of the airflow tube (3) is inserted into the negative pressure headspace bottle (4) through the cap of another negative pressure headspace bottle (4), and the airflow tube (3) is pulled out after continuous collection for 1 to 3 seconds. The above steps are repeated to capture the smoke of each puff of a complete cigarette in turn, and the negative pressure headspace bottle (4) is removed to perform online analysis of the volatile and semi-volatile components of the smoke of each puff of the cigarette.
3. A flue gas capture method based on the device of claim 1, characterized in that: The size of the cigarette holder (2) is adjusted according to the diameter of different cigarettes (1), and all electromagnetic valves (6) are closed. While lighting the cigarette (1), the pointed end of the airflow pipeline (3) is inserted into the negative pressure headspace bottle (4) through the cap of one of the negative pressure headspace bottles (4), and the airflow pipeline (3) is pulled out after continuous capture for 1 to 3 seconds. After smoldering for 27 to 59 seconds, the pointed end of the airflow pipeline (3) is inserted into the negative pressure headspace bottle through the cap of another negative pressure headspace bottle (4), and the airflow pipeline (3) is pulled out after continuous capture for 1 to 3 seconds. The above steps are repeated to capture the smoke of each puff of the whole cigarette in turn, and the electromagnetic valve (6) connecting the negative pressure headspace bottles (4) that capture the smoke of each puff is opened to allow the smoke to be evenly mixed in the negative pressure headspace bottle (4). The negative pressure headspace bottle (4) is removed to perform online analysis of the volatile and semi-volatile components of the whole smoke of the cigarette.
4. The flue gas capture method according to claim 2 or 3, characterized in that: The online analysis was HS-SPME-GC / MS, and the analysis conditions were: SPME-headspace conditions: extraction temperature: 40 °C, extraction time: 10-15 min, desorption time: 3 min, extraction head speed: 200-220 rpm; Gas chromatography conditions: chromatographic column: DB-5MS capillary column, 30 m×0.32 mm×0.25 μm; injection port temperature: 220 °C; program temperature rise: initial temperature 40 °C, hold for 1 min, increase to 230 °C at 3-5 °C / min, hold for 5 min; Carrier gas: high-purity helium, constant flow mode, column flow rate 1 mL / min; injection method: split injection, split ratio 2-5:1; Mass spectrometry conditions: ion source: EI source; Ionization energy: 70 eV; ion source temperature: 210-220 ℃; transfer line temperature: 220 ℃; detection mode: full scan monitoring mode, mass scanning range: 30 amu~500 amu; solvent delay: 0.2-0.5 min.
5. The flue gas capture method according to claim 2 or 3, characterized in that: The online analysis was HS-GC / MS, and the analysis conditions were: The static headspace conditions were as follows: sample equilibration temperature: 40°C; sample loop: 3.0 mL; sample loop temperature: 40-50°C; transfer line temperature: 100-120°C; sample equilibration time: 10.0 min; sample bottle pressurization pressure: 35 psi; pressurization time: 2 min; gas filling time: 0.4-0.5 min; injection time: 0.20-0.30 min; Gas chromatography conditions were as follows: chromatographic column: elastic capillary polyethylene glycol column or equivalent column, 30 m × 0.25 mm × 0.25 μm; Carrier gas: helium, purity ≥99.999%; injection port temperature: 150°C; constant flow mode, column flow rate 1.0 mL / min, split ratio 5:1; program Heating: Initial temperature 40℃, hold for 1 min, increase to 220-230℃ at 3-5℃ / min, hold for 5 min; column flow rate 1 mL / min; The mass spectrometry conditions were as follows: auxiliary interface temperature: 210-220°C; ionization mode: electron bombardment source; ionization energy: 70 eV; ion source temperature: 210°C; quadrupole temperature: 180°C; solvent delay time: 0.1-0.2 min; mass scanning range: 30 amu~500 amu.
Citation Information
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