CN111366663A - Cigarette smoke circulating extraction device and method - Google Patents
Cigarette smoke circulating extraction device and method Download PDFInfo
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- CN111366663A CN111366663A CN201811604819.3A CN201811604819A CN111366663A CN 111366663 A CN111366663 A CN 111366663A CN 201811604819 A CN201811604819 A CN 201811604819A CN 111366663 A CN111366663 A CN 111366663A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N2030/042—Standards
- G01N2030/045—Standards internal
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
Abstract
The invention relates to the technical field of detection of cigarette smoke components, in particular to a cigarette smoke circulating extraction device and method. The invention discloses a cigarette smoke circulation extraction device, which comprises a smoke catcher, a liquid pipeline and a power device, wherein the smoke catcher is connected with the liquid pipeline through a pipeline; the flue gas catcher is provided with an inlet and an outlet and is connected with the liquid pipeline to form a closed loop, and the closed loop is used for containing an extraction solution; the power device drives the extraction solution to move clockwise or anticlockwise in the closed loop or alternatively move clockwise and anticlockwise. The invention also provides a cigarette smoke circulation extraction method based on the device. The invention provides a cigarette smoke circulation extraction device and a method, which solve the technical problems of inaccurate measurement result and complicated operation steps of the existing cigarette smoke measurement method.
Description
Technical Field
The invention relates to the technical field of detection of cigarette smoke components, in particular to a cigarette smoke circulating extraction device and method.
Background
The cigarette smoke is a complex mixed system formed by a series of chemical reactions of gasifying, decomposing, dehydrating, aromatizing, oxidizing, reducing and the like of chemical components in tobacco under the combustion condition or gasifying, condensing and the like at a certain temperature. The mainstream smoke generally consists of a particulate phase and a gas phase, wherein the analysis of the particulate phase components is usually carried out by capturing the particulate phase components of the cigarette smoke by a smoke catcher, and then taking out the glass fiber filter from a glass fiber filter holder and placing the glass fiber filter in an extraction bottle for solvent extraction.
The calculation method of the Total Particulate Matter (TPM) is the weight difference of the smoke catcher before and after pumping, and the determination method of the chemical components in the total particulate matter is the method of taking out a glass fiber filter and adding a solvent for extraction. However, the particle phase matter contains part of volatile components, and the problems of loss of the volatile components and residue of the trap exist in the process of opening the smoke trap and taking out the glass fiber filter disc. Taking a cigarette which is not combusted by heating as an example, the moisture accounts for more than 70% of the total particulate matter, and serious moisture loss and moisture residue exist in the process of taking out the glass fiber filter disc, so that the moisture measurement result is low, and further, the calculated NFDPM (nicotine and moisture subtracted from the total particulate matter) value is high, and the NFDPM value is called as tar in the traditional cigarette. The traditional method for measuring the aroma components needs to concentrate the extract by nitrogen blowing or rotary evaporation and the like, the operation is troublesome, and the low-boiling-point aroma components are easy to lose.
Therefore, the technical problems to be solved urgently by the technical personnel in the field are that the existing cigarette smoke measuring method has inaccurate measuring result and complicated operation steps.
Disclosure of Invention
The invention provides a cigarette smoke circulation extraction device and a method, which solve the technical problems of inaccurate measurement result and complicated operation steps of the existing cigarette smoke measurement method.
The invention provides a cigarette smoke circulation extraction device, which comprises a smoke catcher, a liquid pipeline and a power device, wherein the smoke catcher is connected with the liquid pipeline;
the flue gas catcher is provided with an inlet and an outlet and is connected through the liquid pipeline to form a closed loop, and the closed loop is used for containing an extraction solution;
the power device drives the extraction solution to move clockwise or anticlockwise in the closed loop or alternatively move clockwise and anticlockwise.
Preferably, the liquid pipeline comprises a liquid inlet pipeline and a liquid outlet pipeline;
one end of the flue gas catcher is connected with the first end of the power device through the liquid inlet pipeline;
the other end of the flue gas catcher is connected with the second end of the power device through the liquid outlet pipeline;
the flue gas catcher, the liquid inlet pipeline, the liquid outlet pipeline and the power device form the closed loop;
a liquid inlet valve for injecting an extraction solution is arranged on the liquid inlet pipeline;
and a liquid outlet valve for taking out the extraction solution is arranged on the liquid outlet pipeline.
Preferably, the flue gas collector further comprises a closed container, and the flue gas collector is arranged in the closed container;
the closed containers are connected through the liquid pipeline to form the closed loop.
More preferably, one end of the closed container is connected with the first end of the power device through the liquid inlet pipeline;
the other end of the closed container is connected with the second end of the power device through the liquid outlet pipeline;
the closed container, the liquid inlet pipeline, the liquid outlet pipeline and the power device form the closed loop.
The invention also provides a cigarette smoke circulation extraction method, which comprises the following steps:
step 1: smoking cigarettes by using a smoking machine, and trapping smoke particulate matters of the cigarettes by using a smoke catcher;
step 2: taking down a smoke catcher from a smoking machine, wherein the smoke catcher is provided with an inlet and an outlet and is connected through a liquid pipeline to form a closed loop for containing an extraction solution;
the power device drives the extraction solution to do clockwise motion or anticlockwise motion or alternating motion of the clockwise motion and the anticlockwise motion in the closed loop, so that the extraction solution performs circulation extraction on the cigarette smoke particle phase substances in the smoke catcher to obtain extraction liquid;
and step 3: the extract was taken out and subjected to gas chromatography.
Preferably, the step 2 further comprises a closed container, and the flue gas trap is arranged in the closed container;
the closed containers are connected through the liquid pipeline to form the closed loop.
More preferably, the cigarette includes a conventional cigarette, a heat non-burning cigarette and an electronic cigarette.
Further preferably, the cigarette is a cigarette which is not burned by heating.
More preferably, the smoking machines comprise linear smoking machines and carousel smoking machines.
Further preferably, the smoking machine is a linear smoking machine.
Preferably, the extraction solution is an internal standard solution;
the solvent of the internal standard solution comprises one or more of methanol, ethanol, isopropanol, dichloromethane, ethyl acetate and acetonitrile.
More preferably, the solvent of the internal standard solution is isopropanol.
Preferably, the flue gas catcher comprises a catcher and a glass fiber filter sheet arranged in the catcher;
the diameter of the glass fiber filter disc is 1-150 mm.
More preferably, the diameter of the glass fiber filter sheet is 44mm or 92 mm.
Preferably, each of said glass fiber filters traps between 2 and 20 cigarettes.
More preferably, each glass fiber filter traps 5 cigarettes.
Preferably, the time of the circulation extraction is 1-180 min.
More preferably, the time of the loop extraction is 60 min.
Preferably, the volume of the extraction solution is 2-100 mL.
It should be noted that the volume of the extraction solvent depends on the volume of the piping loop, and is preferably 20mL in the present invention.
According to the technical scheme, the extraction solution is injected into the closed loop, the power device is started, the power device drives the extraction solution to flow in the closed loop and performs circular extraction on the cigarette smoke particulate matters in the smoke catcher, the smoke catcher is directly installed in the device without opening the smoke catcher, the loss of target objects in the opening process and the influence of test results caused by pollution in the operation process are avoided, and the extraction accuracy is improved. In addition, the cigarette smoke circulation extraction method provided by the invention can ensure more sufficient extraction, higher extraction efficiency, shortened extraction time and solvent saving by keeping the fluidity of the extraction solution in the closed loop.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic view of a first structure of a cigarette smoke circulating extraction device in embodiment 1 of the present invention;
FIG. 2 is a second schematic structural diagram of a cigarette smoke circulating extraction device in embodiment 1 of the present invention;
FIG. 3 is a schematic view of a first structure of a cigarette smoke circulating extraction device in embodiment 2 of the present invention;
fig. 4 is a second structural schematic diagram of the cigarette smoke circulating extraction device in embodiment 2 of the present invention;
wherein the reference numbers are as follows:
the device comprises a flue gas catcher 1, a hose 2, a power device 3, a liquid inlet valve 4, a liquid outlet valve 5 and a closed container 6.
Detailed Description
The invention provides a cigarette smoke circulation extraction device and a method, which solve the technical problems of inaccurate measurement result and complicated operation steps of the existing cigarette smoke measurement method.
In order to make the objects, features and advantages of the present invention more obvious and understandable, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the embodiments described below are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The cigarette smoke circulation extraction device and method provided by the embodiment of the invention are further explained below.
Example 1
Referring to fig. 1 and fig. 2, an embodiment of the present invention provides a cigarette smoke circulating extraction apparatus, including a smoke catcher 1, a liquid pipeline and a power device 3;
the flue gas catcher 1 is provided with an inlet and an outlet and is connected through a liquid pipeline to form a closed loop, and the closed loop is used for containing an extraction solution;
the power unit 3 drives the extraction solution to move clockwise or counterclockwise or alternatively clockwise and counterclockwise in the closed loop.
According to the cigarette smoke circulation extraction device provided by the embodiment of the invention, the extraction solution is injected into the closed loop, the power device 3 is started, the power device 3 drives the extraction solution to flow in the closed loop and performs circulation extraction on cigarette smoke particle phase substances in the smoke trap 1, wherein the smoke trap 1 is directly installed in the device without opening the smoke trap 1, so that the loss of a target object in the opening process and the influence of a test result caused by pollution in the operation process are avoided, and the extraction accuracy is improved. In addition, the cigarette smoke circulation extraction method provided by the invention can ensure more sufficient extraction, higher extraction efficiency, shortened extraction time and solvent saving by keeping the fluidity of the extraction solution in the closed loop.
Further, the liquid pipeline comprises a liquid inlet pipeline and a liquid outlet pipeline;
one end of the flue gas catcher 1 is connected with the first end of the power device 3 through a liquid inlet pipeline;
the other end of the smoke catcher 1 is connected with the second end of the power device 3 through a liquid outlet pipeline;
the flue gas catcher 1, the liquid inlet pipeline, the liquid outlet pipeline and the power device 3 form a closed loop;
a liquid inlet valve 4 for injecting an extraction solution is arranged on the liquid inlet pipeline;
a liquid outlet valve 5 for taking out the extraction solution is arranged on the liquid outlet pipeline.
Furthermore, the liquid inlet pipeline and the liquid outlet pipeline are both hoses 2.
Further, the power unit 3 is a peristaltic pump.
The embodiment also provides a cigarette smoke circulation extraction method based on the cigarette smoke circulation extraction device, which comprises the following steps:
step 1: the cigarettes are smoked by adopting a linear smoking machine, wherein the smoking curve is bell-shaped, the smoking capacity is 35 +/-0.3 mL, the smoking duration is 2s, the smoking interval is 30s, glass fiber filter discs with the diameter of 44mm are adopted to collect the particulate matter components of the smoke of the cigarettes, and each filter disc collects 5 cigarettes.
Step 2: taking down the smoke catcher 1 from the linear type smoking machine, enabling the hose 2 to penetrate through the peristaltic pump head, dividing the hose 2 into a liquid inlet pipeline and a liquid outlet pipeline, and connecting one end of the smoke catcher 1 with the first end of the peristaltic pump head through the liquid inlet pipeline; the other end of the smoke catcher 1 is connected with the second end of the peristaltic pump head through a liquid outlet pipeline; the smoke catcher 1, the liquid inlet pipeline, the liquid outlet pipeline and the peristaltic pump head form a closed loop; a liquid inlet valve 4 is arranged on the liquid inlet pipeline, a liquid outlet valve 5 is arranged on the liquid outlet pipeline, 20mL of isopropanol solution (ethanol, quinoline and 1, 4-butanediol, wherein the ethanol is an internal standard of water, the quinoline is an internal standard of nicotine, and the 1, 4-butanediol is an internal standard of 1, 2-propanediol and glycerol) containing internal standards is injected through the liquid inlet valve 4 to fill the whole loop, a peristaltic pump is started for a certain time to realize circulation extraction, the extraction liquid is taken out through the liquid outlet valve 5 after standing, and is filtered through an organic phase filter membrane of 0.45 mu m and then is put into a computer for analysis.
And step 3: performing gas chromatography with double columns and double detectors, wherein the system A is used for determining water content, the chromatographic column is a packed column, and the stationary phase is Porapak Q2(150 μm) as TCD detector, system B for measuring nicotine, 1, 2-propanediol and glycerol, column DB-WAXETR (30m × 0.32mm,1 μm) as FID detector.
Wherein the injection port temperature of the system A is 150 ℃, and the carrier gas is nitrogen (N) with the flow rate of 5mL/min2) The sample injection volume is 0.5 mu L, the sample injection mode is non-split flow sample injection, and the temperature of the detector is 250 ℃.
Sample inlet temperature of system B: n at 250 ℃ and a carrier gas flow rate of 0.7mL/min2The sample introduction volume is 1 mu L, the sample introduction mode adopts split sample introduction, the split ratio is 30:1, and the tail gas blowing is N with the flow rate of 30mL/min2The detector temperature was 275 deg.C, the flow rate of hydrogen was 30mL/min, and the flow rate of air was 400 mL/min.
Different electric heating devices are adopted to respectively heat the adaptive non-burning cigarette rods, the glass fiber filter disc is used for trapping aerosol particulate matters, the total weight of the smoke trap 1 (the trap and the glass fiber filter disc) before and after smoking is respectively measured, and the difference value is calculated to obtain the Total Particulate Matter (TPM). After smoking the cigarettes, extracting water, nicotine, 1, 2-propylene glycol and glycerol in the glass fiber filter disc by using an extraction solution containing an internal standard (circulation extraction), then analyzing by using a GC-TCD (gas chromatography thermal conductivity detector) and a GC-FID (gas chromatography hydrogen flame ionization detector), and quantifying by using an internal standard method, wherein the internal standard of the water is ethanol, the internal standard of the nicotine is quinoline, the internal standard of the 1, 2-propylene glycol and the glycerol is 1, 4-butanediol, and the measurement results are shown in Table 1.
TABLE 1 measurement results of total particulate matter, moisture, nicotine, 1, 2-propanediol and glycerol of cigarette aerosol not combusted by different heating in example 1
Note: other ═ TPM-moisture-nicotine-1, 2-propanediol-glycerol
Example 2
Referring to fig. 3 and 4, the cigarette smoke circulating extraction device provided in this embodiment further includes a closed container 6, and the smoke catcher 1 is disposed in the closed container 6;
the closed containers 6 are connected through a liquid pipeline to form a closed loop.
Further, one end of the closed container 6 is connected with the first end of the power device 3 through a liquid inlet pipeline;
the other end of the closed container 6 is connected with the second end of the power device 3 through a liquid outlet pipeline;
the closed container 6, the liquid inlet pipeline, the liquid outlet pipeline and the power device 3 form a closed loop.
The embodiment also provides a cigarette smoke circulation extraction method based on the cigarette smoke circulation extraction device, wherein the difference between the embodiment 2 and the embodiment 1 is that the step 2: the method comprises the following steps of taking down a smoke catcher 1 from a linear type smoking machine, arranging the smoke catcher 1 in a closed container 6, enabling a hose 2 to penetrate through a peristaltic pump head, dividing the hose 2 into a liquid inlet pipeline and a liquid outlet pipeline, and connecting one end of the closed container 6 with a first end of the peristaltic pump head through the liquid inlet pipeline; the other end of the closed container 6 is connected with the second end of the peristaltic pump head through a liquid outlet pipeline; the smoke catcher 1, the liquid inlet pipeline, the liquid outlet pipeline and the peristaltic pump head form a closed loop; a liquid inlet valve 4 is arranged on the liquid inlet pipeline, a liquid outlet valve 5 is arranged on the liquid outlet pipeline, 20mL of isopropanol solution (ethanol, quinoline and 1, 4-butanediol, wherein the ethanol is an internal standard of water, the quinoline is an internal standard of nicotine, and the 1, 4-butanediol is an internal standard of 1, 2-propanediol and glycerol) containing internal standards is injected through the liquid inlet valve 4 to fill the whole loop, a peristaltic pump is started for a certain time to realize circulation extraction, the extraction liquid is taken out through the liquid outlet valve 5 after standing, and is filtered through an organic phase filter membrane of 0.45 mu m and then is put into a computer for analysis.
Different electric heating devices are adopted to respectively heat the adaptive non-burning cigarette rods, the glass fiber filter disc is used for trapping aerosol particulate matters, the total weight of the smoke trap 1 and the glass fiber filter disc before and after smoking is respectively measured, and the difference value is calculated to obtain the Total Particulate Matter (TPM). After smoking the cigarettes, extracting water, nicotine, 1, 2-propylene glycol and glycerol in the glass fiber filter disc by using an extraction solution containing an internal standard (circulation extraction), then analyzing by using a GC-TCD (gas chromatography thermal conductivity detector) and a GC-FID (gas chromatography hydrogen flame ionization detector), and quantifying by using an internal standard method, wherein the internal standard of the water is ethanol, the internal standard of the nicotine is quinoline, the internal standard of the 1, 2-propylene glycol and the glycerol is 1, 4-butanediol, and the measurement results are shown in Table 2.
TABLE 2 measurement results of aerosol total particulate matter, moisture, nicotine, 1, 2-propanediol and glycerol of cigarette not combusted by different heating in example 2
The results of comparing the conventional method with the extraction method provided in the examples of the present invention are shown in Table 3
TABLE 3 results of determination of water, nicotine, propylene glycol and glycerol in total particulate matter of cigarette without combustion by different extraction methods
In summary, as can be seen from the data in tables 1,2 and 3, the method provided in the embodiment of the present invention can achieve accurate determination of moisture in the total particulate matter of the cigarette without burning, and avoid the low determination result and the low moisture value caused by water dispersion and residue on the smoke trap 1, which result in the calculated NFPDM value and other (TPM-moisture-propylene glycol-glycerol-nicotine) values being higher.
The above-mentioned embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the same; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. A cigarette smoke circumfluence extraction device is characterized by comprising a smoke catcher, a liquid pipeline and a power device;
the flue gas catcher is provided with an inlet and an outlet and is connected through the liquid pipeline to form a closed loop, and the closed loop is used for containing an extraction solution;
the power device drives the extraction solution to move clockwise or anticlockwise in the closed loop or alternatively move clockwise and anticlockwise.
2. The cigarette smoke circulating extraction device of claim 1, further comprising a closed container, wherein the smoke catcher is arranged in the closed container;
the closed containers are connected through the liquid pipeline to form the closed loop.
3. The cigarette smoke circulating extraction device of claim 1, wherein the liquid pipeline comprises a liquid inlet pipeline and a liquid outlet pipeline;
one end of the flue gas catcher is connected with the first end of the power device through the liquid inlet pipeline;
the other end of the flue gas catcher is connected with the second end of the power device through the liquid outlet pipeline;
the flue gas catcher, the liquid inlet pipeline, the liquid outlet pipeline and the power device form the closed loop;
a liquid inlet valve for injecting an extraction solution is arranged on the liquid inlet pipeline;
and a liquid outlet valve for taking out the extraction solution is arranged on the liquid outlet pipeline.
4. A cigarette smoke circulation extraction method is characterized by comprising the following steps:
step 1: smoking cigarettes by using a smoking machine, and trapping smoke particulate matters of the cigarettes by using a smoke catcher;
step 2: taking down the smoke catcher from the smoking machine, wherein an inlet and an outlet of the smoke catcher are connected through a liquid pipeline to form a closed loop for containing an extraction solution;
the power device drives the extraction solution to do clockwise motion or anticlockwise motion or alternating motion of the clockwise motion and the anticlockwise motion in the closed loop, so that the extraction solution performs circulation extraction on the cigarette smoke particle phase substances in the smoke catcher to obtain extraction liquid;
and step 3: the extract was taken out and subjected to gas chromatography.
5. The cigarette smoke circulating extraction method according to claim 4, wherein the step 2 further comprises a closed container, the smoke catcher is arranged in the closed container;
the closed containers are connected through the liquid pipeline to form the closed loop.
6. The cigarette smoke circular flow extraction method of claim 4, wherein the extraction solution is an internal standard solution;
the solvent of the internal standard solution comprises one or more of methanol, ethanol, isopropanol, dichloromethane, ethyl acetate and acetonitrile.
7. The cigarette smoke circular flow extraction method of claim 4, wherein the smoke catcher comprises a catcher and a glass fiber filter disc arranged in the catcher;
the diameter of the glass fiber filter disc is 1-150 mm.
8. The cigarette smoke recirculation extraction method of claim 7, wherein each glass fiber filter traps 2-20 cigarettes.
9. The cigarette smoke circulation extraction method according to claim 4, wherein the circulation extraction time is 1-180 min.
10. The cigarette smoke circular flow extraction method of claim 4, wherein the volume of the extraction solution is 2-100 mL.
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