CN115616121A - Method for measuring aroma components in cigarette smoke and trapping device - Google Patents

Abstract

The invention provides a method for measuring flavor components in cigarette smoke and a trapping device, wherein the measuring method comprises the following steps: component trapping: smoking the cigarette to respectively obtain a smoke particle phase substance and a smoke gas phase substance; and (3) extraction and collection: collecting the functional segments of the cigarettes after smoking to obtain first extract liquor; extracting the flavor components on the Cambridge filter with an extractant to obtain a granular phase extract; extracting the aroma components in the collected gas to obtain gas phase extract; component determination: obtaining the types and contents of the flavor components in the functional segments, the smoke particle phase substances and the smoke gas phase substances. The determination method can perform qualitative analysis and quantitative determination on the distribution condition of the flavor components in the functional segments, the particle phase substances and the gas phase substances of the cigarettes, has simple and cheap methods for capturing the components and collecting the components by extraction, and simultaneously has unified methods for determining the components and better comparability of determination results in different matrixes.

Description

Method for measuring aroma components in cigarette smoke and trapping device

Technical Field

The invention relates to the technical field of novel tobacco products, in particular to a method for measuring aroma components in cigarette smoke and a trapping device.

Background

The heating cigarette is designed by taking the idea of 'heating without burning', can keep the taste of the tobacco to a certain extent, simultaneously reduces the release of potential harmful substances by igniting the tobacco material, and currently keeps a strong development trend in the overseas market. In the actual product, the requirement of a user on the taste of the smoke cannot be met by only depending on the fact that the tobacco is heated to release the fragrant substances, and the various forms of flavoring and fragrance supplementing play an extremely important role in improving the smoke quality of the heated cigarette.

As the research on heated cigarettes in China starts late, the transfer condition of flavor components to a smoke gas particle phase in the smoking process of the heated cigarettes, particularly the heated cigarettes with filter tips added with flavor (such as bead-blasting heated cigarettes) and the residual condition of the flavor components in the heated cigarette filter tips after smoking are lack of comprehensive understanding at present.

The conventional method for measuring the aroma components in the cigarette smoke gas phase substances reported in the related documents at present is based on a pretreatment mode of cold trap or adsorption tube trapping, and the measuring method has high cost. And the principle of the subsequent instrument analysis method trapped by the adsorption tube is different from the principle of the method for measuring the smoke particle phase substances, so that systematic errors among the methods easily exist, and the method is not beneficial to the comparative analysis of the content of the fragrance components in different matrixes.

Disclosure of Invention

The invention provides a method for measuring flavor components in cigarette smoke, which is used for solving the technical problem.

The invention provides a method for measuring flavor components in cigarette smoke, which comprises the following steps:

component trapping: the method comprises the steps of (1) smoking cigarettes, enabling smoke sucked out to firstly pass through a Cambridge filter disc catcher, and then collecting gas passing through the Cambridge filter disc catcher, so as to respectively obtain smoke particle phase substances and smoke gas phase substances;

extraction and collection: collecting the functional segments of the cigarettes after smoking is finished, and extracting the flavor components in the functional segments by using an extracting agent to obtain first extract liquor; taking out the Cambridge filter disc after trapping the smoke, and extracting the fragrance components on the Cambridge filter disc by using an extracting agent to obtain a granular phase extract; adding an extracting agent into the collected gas, and extracting the fragrant components in the collected gas to obtain gas phase extract liquor;

component determination: and analyzing and detecting the first extraction liquid, the particulate matter extraction liquid and the gas phase matter extraction liquid by using a gas chromatography-mass spectrometer to respectively obtain the types and the contents of the flavor components in the functional section, the smoke particulate matter and the smoke gas phase matter.

By adopting the technical scheme, the distribution conditions of the fragrance components in the functional segments, the particle-phase substances and the gas-phase substances can be qualitatively and quantitatively analyzed, and meanwhile, the determination method is uniform, so that the comparative analysis of data is facilitated. Meanwhile, detection means and data support are provided for future researches on the utilization rate of added spices, environmental pollution, component control in product development and the like.

Optionally, in the component capturing set, a gas sampling bag is communicated with the cambridge filter catcher, so that the flue gas enters the gas sampling bag after passing through the cambridge filter catcher.

Optionally, a flavor component absorber is arranged between the cambridge filter trap and the gas sampling bag and is used for absorbing flavor components in smoke flowing out of the cambridge filter trap, and the smoke passes through the cambridge filter trap and the flavor component absorber and is collected by the gas sampling bag.

Optionally, a suction engine is further disposed between the aroma component absorber and the gas sampling bag, and a smoke circulation loop is formed between the gas sampling bag and the aroma component absorber, so that after suction is finished, smoke in the gas sampling bag is driven by the suction engine to circulate between the aroma component absorber and the gas sampling bag for multiple times.

Optionally, the aroma component absorber is provided with a solid absorbing material for the smoke to pass through, and after the components are captured, an extracting agent is added into the solid absorbing material for extraction to obtain a first gas-phase extract liquid.

Optionally, the flavor component absorber is charged with an extraction agent for passage of the flue gas, and a first gas phase extract is obtained in the component capture.

Optionally, in the extraction collection, an extraction agent is injected into the gas sampling bag, oscillation absorption is performed, a second gas-phase extract is obtained, and the second gas-phase extract is combined with the first gas-phase extract, so as to obtain the gas-phase extract, or the first gas-phase extract is used as the gas-phase extract.

Optionally, in the extraction collection, an extractant is injected into the gas sampling bag to obtain the gas phase extraction liquid.

Optionally, after injecting an extractant into the gas sampling bag, the whole gas sampling bag is placed in an environment at a temperature lower than-10 ℃ for more than 15 minutes, and then the liquid in the gas sampling bag is taken out to obtain the gas phase extract.

Optionally, in the extraction collection, cutting the functional segments, putting the functional segments into a container, adding the extractant, oscillating, and filtering to obtain the first extract; and (3) putting the Cambridge filter disc into a container, adding the extracting agent, oscillating, and filtering to obtain the granular phase extract.

Optionally, the oscillation time is 10 to 60 minutes respectively.

Optionally, the functional segment is a filter.

Optionally, the extractant is one of methyl tert-butyl ether, ethanol, isopropanol, dichloromethane, acetone, n-hexane, methanol, and acetonitrile.

Optionally, the extractant further comprises an internal standard substance, and the internal standard substance is one or more of methyl valerate, methyl heptanoate, methyl nonanoate, methyl undecanoate, methyl tridecanoate, methyl pentadecanoate, propyl benzoate, phenylethyl phenylacetate and phenylethyl acetate.

Optionally, smoking the plurality of heated cigarettes, and collecting the total first extract, the particulate-phase extract and the gas-phase extract of the plurality of heated cigarettes for flavor component determination.

The invention also provides a trapping device for heating the aroma components in the cigarette smoke, which is used for trapping the components in the method for determining the aroma components in the cigarette smoke, wherein the cigarette has a functional section, the trapping device comprises a Cambridge filter catcher, a suction engine and a gas sampling bag, the Cambridge filter catcher is communicated with the functional section of the cigarette to be determined, the suction engine is respectively communicated with the Cambridge filter catcher and the gas sampling bag, the smoke in the heated cigarette flows out of the functional section of the cigarette through the motive power of the suction engine, passes through the Cambridge filter catcher and then flows into the gas sampling bag to be collected, and therefore, smoke particle phase substances and smoke gas phase substances are respectively obtained in the Cambridge filter catcher and the gas sampling bag.

By adopting the technical scheme, the collection of the fragrance substances in the functional section, the smoke particle phase substances and the smoke gas phase substances can be realized, and then the uniform collection and the measurement of the fragrance components can be completed in an extracting way by the extracting agent.

Optionally, the trapping device further comprises a flavor component absorber, which is positioned between the cambridge filter trap and the gas sampling bag along the flow direction of the smoke and is used for absorbing the flavor components in the smoke flowing out of the cambridge filter trap.

Optionally, a smoke circulation loop is formed between the gas sampling bag and the aroma component absorber, so that after the suction is finished, smoke in the gas sampling bag is driven by the suction engine to circulate between the aroma component absorber and the gas sampling bag for multiple times.

Optionally, the trapping device further comprises a switching valve, a first channel, a second channel and a third channel, the first channel is used for communicating the fragrance component absorber, the suction engine and the gas sampling bag and is connected with the switching valve, the second channel is used for communicating the cambridge filter trap and the switching valve, the third channel is used for communicating the gas sampling bag and the switching valve, and the switching valve is used for controlling the opening and closing of the communication between the first channel and the second channel and the communication between the first channel and the third channel and controlling the closing of the communication between the second channel and the third channel.

Optionally, the trapping device further comprises a first valve disposed on the gas sampling bag and in communication with the third channel.

Optionally, the flavour component absorber contains a solid absorbent material through which the smoke passes.

Optionally, the flavour component absorber contains an extraction agent for passage of the smoke.

Optionally, the aroma component absorber is two or more absorption bottles connected in series, and the extraction agent is contained in the absorption bottles.

Optionally, the gas sampling device further comprises an injector, the injector is used for communicating with the gas sampling bag after the gas sampling bag finishes flue gas collection, and an extracting agent is injected into the gas sampling bag to obtain a gas phase extract.

Optionally, the functional segment is a filter.

Drawings

FIG. 1 shows a schematic view of the connection of a trapping device according to an embodiment of the present invention;

FIG. 2 shows a schematic view of the connection of a trapping device according to another embodiment of the present invention;

FIG. 3 shows a schematic view of the connection of a trapping device according to yet another embodiment of the present invention;

FIG. 4 shows a schematic connection of a trapping device according to yet another embodiment of the present invention;

figure 5 shows a schematic view of a gas sampling bag and syringe connection of the present invention.

Detailed Description

The following description of the embodiments of the present invention is provided for illustrative purposes, and other advantages and effects of the present invention will become apparent to those skilled in the art from the present disclosure. While the invention will be described in conjunction with the preferred embodiments, it is not intended that the features of the invention be limited to that embodiment. On the contrary, the invention is described in connection with the embodiments for the purpose of covering alternatives or modifications that may be extended based on the claims of the present invention. In the following description, numerous specific details are included to provide a thorough understanding of the invention. The invention may be practiced without these particulars. Moreover, some of the specific details have been left out of the description in order to avoid obscuring or obscuring the focus of the present invention. It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.

It should be noted that in this specification, like reference numerals and letters refer to like items in the following drawings, and thus, once an item is defined in one drawing, it need not be further defined and explained in subsequent drawings.

In the description of the present embodiment, it should be noted that the terms "upper", "lower", "high", "low", and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings or orientations or positional relationships that are conventionally placed when the products of the present invention are used, and are only used for convenience in describing the present invention and simplifying the description, but do not indicate or imply that the devices or elements indicated must have specific orientations, be configured in specific orientations, and operate, and thus, should not be construed as limiting the present invention.

The terms "first," "second," and the like are used solely to distinguish one from another and are not to be construed as indicating or implying relative importance.

In the description of the present embodiment, it should be further noted that, unless explicitly stated or limited otherwise, the terms "disposed," "connected" and "connected" should be interpreted broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present embodiment can be understood in specific cases by those of ordinary skill in the art.

In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be described in detail with reference to the accompanying drawings.

Referring to fig. 1, the invention provides a method for measuring flavor components in cigarette smoke, comprising the following steps:

component trapping: smoking the cigarette, so that the smoked smoke firstly passes through the Cambridge filter disc catcher, and then the gas passing through the Cambridge filter disc catcher is collected, thereby respectively obtaining smoke particle phase substances and smoke gas phase substances;

extraction and collection: collecting the functional segments of the cigarettes after smoking is finished, and extracting the flavor components in the functional segments by using an extracting agent to obtain first extract liquor; taking out the Cambridge filter disc after trapping the smoke, and extracting the fragrance components on the Cambridge filter disc by using an extracting agent to obtain a granular phase extract; adding an extracting agent into the collected gas, and extracting the fragrant components in the collected gas to obtain gas phase extract liquor;

component determination: and analyzing and detecting the first extraction liquid, the particulate matter extraction liquid and the gas phase extraction liquid by using a gas chromatography-mass spectrometer to respectively obtain the types and the contents of the flavor components in the functional section, the smoke particulate matter and the smoke gas phase matter.

The determination method can be used for determining the flavor components in the smoke of the traditional combustion type cigarette, and can also be used for determining the flavor components in the smoke of the heating non-combustion type cigarette. Alternatively, the aroma component in the electronic smoke sol can also be measured. In the case of the component trapping, the smoking type cigarette may be ignited and smoked, and the smoking type cigarette may be electrically heated and smoked without burning. Smoking may employ a powered device to drive the release of smoke from a cigarette from a filter. The functional section refers to a component through which smoke flows in the cigarette or a component in which spices are placed. For example, a tobacco smoking segment, a cooling segment, or a filter. The smoke can remain flavor components when passing through the smoking segment, the cooling segment or the filter tip, and the invention can collect and measure the flavor components remained in the functional segment. Or to measure the residual flavour content in the flavour storage site after the smoke has passed through the entrained flavour. At present, the filter tip of a cigarette is added with spice, so that the filter tip of the cigarette after being sucked can be taken out, the flavor components in the filter tip are extracted to obtain filter tip extract, and then the type and the content of the flavor components in the filter tip are measured.

The invention can measure the heated cigarette containing the exploded beads so as to detect the component types and distribution conditions of the flavor components flowing out of the exploded beads in the filter tip, the smoke particle phase substances and the smoke gas phase substances respectively. In addition, other heated cigarettes with spices are also applicable to the determination method of the invention.

The determination method provided by the invention is used for performing qualitative and quantitative analysis on the flavor components in the filter tip, the smoke particle phase matter and the smoke gas phase matter respectively, and is beneficial to performing comprehensive and complete analysis on the transfer trend of the flavor components. In addition, the conventional methods for detecting a flavor component are different, and different measurement methods are different in error. If the components and the contents of the filter tip, the smoke particulate matter and the smoke gaseous matter are respectively measured by different methods, the comparison of the content values of the three parts is lack of reliability due to the existence of significant differences among the methods.

The determination method of the invention adopts the same solution to extract the flavor components in the functional segment (such as a filter tip), the smoke particle phase matter and the smoke gas phase matter, and then uses a gas chromatography mass spectrometer to respectively analyze and detect the three kinds of extraction liquid, and has the same pretreatment method and instrument analysis method.

The measuring method can carry out qualitative and quantitative analysis on the distribution condition of the flavor components in the filter tip, the particulate matter and the gas phase matter, and meanwhile, the detection mode is unified, so that the comparative analysis of data is facilitated. Meanwhile, detection means and data support are provided for future researches on the utilization rate of added spices, environmental pollution, component control in product development and the like.

Furthermore, the components are collected and concentrated, and the gas sampling bag is communicated with the Cambridge filter catcher, so that the flue gas enters the gas sampling bag after passing through the Cambridge filter catcher. The invention collects the smoke passing through the Cambridge filter catcher through the gas sampling bag, can perform solvent extraction on the collected smoke, and collects the fragrance components in the smoke gas phase substances. In addition, the smoke in the cigarette can be sucked out by adopting a power device, the embodiment can adopt a suction engine which is connected with the cigarette and the gas sampling bag, and the smoke is driven by the suction engine to flow out of the cigarette, pass through the Cambridge filter catcher and then reach the gas sampling bag.

In addition, the invention can arrange a fragrance component absorber between the Cambridge filter sheet catcher and the gas sampling bag, and on the path of the smoke flowing out from the Cambridge filter sheet catcher to the gas sampling bag, the smoke passes through the fragrance component absorber, thereby absorbing the fragrance component in the smoke flowing out from the Cambridge filter sheet catcher, namely the fragrance component in the smoke gas phase object, and then the smoke reaches the gas sampling bag to be collected. Thus, the flavor component in the smoke gas phase is collected on the path of the smoke gas. Furthermore, after the aroma components in the smoke gas phase object are collected, the aroma components in the smoke gas in the gas sampling bag can be collected, for example, an extracting agent can be injected into the gas sampling bag, so that the aroma components in the smoke gas phase object can be collected to the maximum extent.

Furthermore, a suction engine is arranged between the aroma component absorber and the gas sampling bag, a smoke circulation loop is formed between the gas sampling bag and the aroma component absorber, and after suction is finished, smoke in the gas sampling bag is driven by the suction engine to circulate between the aroma component absorber and the gas sampling bag for multiple times. That is, the invention forms a circulating path among the aroma component absorber, the gas sampling bag and the suction engine, the suction engine provides power to make the smoke in the gas sampling bag circulate for many times, and the smoke can pass through the aroma component absorber for many times through the circulation for many times, thereby achieving the purpose that the aroma component in the smoke gas phase object is fully absorbed by the aroma component absorber.

Specifically, as shown in fig. 1, the invention provides a device for trapping aroma components in cigarette smoke, which can trap aroma components in heated cigarettes. The trapping device comprises a cambridge filter trap 2, a suction engine 3 and a gas sampling bag 4. The cambridge filter catcher 2 is communicated with the filter of the heated cigarette 1 to be measured, for example, the heated cigarette 1 can be directly inserted into the cambridge filter catcher 2 with a cigarette holder, or the catching device of the invention is provided with a fixer for fixing the heated cigarette, the heated cigarette is fixed on the fixer, and then the filter of the heated cigarette is communicated with the inlet of the cambridge filter catcher. The suction engine 3 is respectively communicated with the Cambridge filter catcher 2 and the gas sampling bag 4, when the suction engine 3 sucks, smoke in the heated cigarette 1 flows into the suction engine 3 from the filter tip through the Cambridge filter catcher 2, when the suction engine 3 exhausts, the smoke flows into the gas sampling bag 4 to be collected, and therefore smoke particle phase objects and smoke gas phase objects are respectively obtained in the Cambridge filter catcher 2 and the gas sampling bag 4.

Referring to fig. 2-4, the trapping device further comprises a flavor component absorber 5, which is located between the cambridge filter catcher 2 and the gas sampling bag 4 along the smoke flowing direction and is used for absorbing flavor components in the smoke flowing out of the cambridge filter catcher 2. While the flavor component absorber 5 is shown in fig. 2 and 3 as being located between the cambridge filter trap 2 and the suction engine 3, in other embodiments, the flavor component absorber may be located between the suction engine and the gas sampling bag in the direction of flow of the flue gas, with the suction engine located between the cambridge filter trap and the flavor component absorber.

The method for measuring the aroma components in the cigarette smoke can adopt the trapping device to collect the smoke particle phase substances and the smoke gas phase substances, and can also adopt a mode of circulating the smoke between the aroma component absorber and the gas sampling bag for many times to collect the aroma components in the smoke gas phase substances.

Specifically, referring to fig. 4, the trapping device further includes a switching valve 6, a first passage 61, a second passage 62, and a third passage 63. The first passage 61 is for communicating the aroma component absorber 5, the suction engine 3, and the gas sampling bag 4, and is connected to the switching valve 6. I.e. the first channel 61 is connected at one end to the switching valve 6 and at the other end to the gas sampling bag 4, and in series with the aroma component absorber 5 and the suction engine 3. The positions of the suction engine and the aroma composition absorber in fig. 4 can also be reversed. The second channel 62 is used for connecting the cambridge filter trap 2 and the switching valve 6, the third channel 63 is used for connecting the gas sampling bag 4 and the switching valve 6, and the switching valve 6 is used for controlling the first channel 61 and the second channel 62, opening and closing of communication between the first channel 61 and the third channel 63, and closing of communication between the second channel 62 and the third channel 63. Thus, at the start of suction, the first passage 61 and the second passage 62 are communicated, the third passage 63 is closed from the first passage 61, and the third passage and the second passage 62 are closed by the control of the switching valve 6. During the smoking test, smoke is collected in a gas sampling bag 4 after passing from cambridge filter trap 2 through a fragrance composition absorber 5 and a smoking engine 3. After the smoking of the heated cigarette is finished, the switching valve 6 is controlled to enable the first channel 61 to be communicated with the third channel 63, and the second channel 62 is closed, so that the second channel 62 is not communicated with the first channel 61 and the third channel 63 respectively. At this time, the suction engine 3 provides power to circulate the smoke collected in the gas sampling bag 4 between the aroma component absorber 5 and the gas sampling bag 4 for a plurality of times. Wherein the number of cycles can be determined according to the measurement requirement and the absorption effect of the aroma component absorber 5.

Further, with continued reference to fig. 4, with regard to the trapping device described above, there is also included a first valve 8, the first valve 8 being disposed on the third channel 63 between the switching valve 6 and the gas sampling bag 4. The first valve 8 may be closed when the cigarette is heated for smoking. The first valve 8 may be disposed near the connection of the third channel 63 to the gas sampling bag 4, i.e., the first valve 8 is near the connection port of the gas sampling bag 4, or the first valve is disposed on the connection port of the gas sampling bag 4, such that gas is primarily collected in the gas sampling bag 4.

In addition, the trapping device further includes a second valve 7, the second valve 7 being provided on the first passage 61 between the switching valve 6 and the gas sampling bag 4 for opening and closing the first passage 61. Further, when the suction engine 3 is adjacent to the gas sampling bag 4 in the smoke flowing direction, the second valve 7 may be provided between the suction engine 3 and the gas sampling bag 4. Or the second valve 7 is disposed between the aroma component absorber 5 and the gas sampling bag 4 when the aroma component absorber 5 is adjacent to the gas sampling bag 4 in the smoke flow direction. Preferably, second valve 7 is disposed near the connection of first channel 61 with gas sampling bag 4, second valve 7 is near the connection port of gas sampling bag 4, or second valve is disposed at the connection port of gas sampling bag 4, such that gas is primarily collected in gas sampling bag 4.

The trapping device is used for trapping the aroma components in the smoke gas phase, wherein the aroma component absorber 5 can be provided with a solid absorbing material for smoke to pass through, as shown in figure 3, after the trapping is carried out, the aroma components are extracted from the solid absorbing material by using an extracting agent, and a first gas phase extract liquid is obtained. If the trapping device in FIG. 4 is adopted, after the flue gas circulates for multiple times, the extracting agent is added into the solid absorbing material to obtain the first gas-phase extract liquid. The effect that different flavor components in the smoke gas phase can be absorbed is different, and the solid absorbing material can be used for absorbing the flavor components in a targeted manner. Then extracting by an extracting agent to obtain the smoke gas phase substance extract. In addition, after the fragrance component absorber finishes collection, an extracting agent is injected into the gas sampling bag, oscillation absorption is carried out, and second gas phase extract liquid is obtained, so that all fragrances which are easy to absorb by solid absorption materials and liquid are collected, then the first gas phase extract liquid and the second gas phase extract liquid are combined, total gas phase extract liquid is obtained, and then the total gas phase extract liquid is separated and detected by a gas chromatography mass spectrometer. Alternatively, when the solid absorbent material can sufficiently absorb the flavor component in the smoke gas phase, the first gas phase extract may be directly used as the gas phase extract to perform the chromatography-mass spectrometry.

In other embodiments, as shown in FIG. 2, the aroma constituent absorber 5 contains an extraction agent through which the flue gas passes. In the process of component capture, the flue gas passes through the flavor component absorber 5 to be absorbed by the extracting agent, so that in the step of component capture, the extraction of the flavor components in the gas phase is completed, and a first gas phase extract liquid is obtained. If the first gas-phase extract is collected by the collecting device in FIG. 4, the first gas-phase extract is obtained after circulating for many times. That is, in the embodiment, the flavor component in the smoke gas phase is collected and extracted (absorbed by the solution) in the process of collecting the smoke from the filter tip to the gas sampling bag. Specifically, the fragrance component absorber 5 is two or more serially connected absorption bottles, and the extraction agent is contained in the absorption bottles. In this embodiment, the first gas-phase extract obtained after absorption may be used as a gas-phase extract to perform chromatography-mass spectrometry, or after the extraction is completed by the fragrance component absorber 5, an extractant is injected into the gas sampling bag 4, oscillation absorption is performed to obtain a second gas-phase extract, and then the first gas-phase extract and the second gas-phase extract are combined to obtain a total gas-phase extract, so that the gas-phase mass spectrometer is used to perform separation detection on the extracts.

In other embodiments, the gas phase aroma components may be collected in gas sampling pouch 4 and the extraction collection completed in gas sampling pouch 4. The gas phase extract is obtained by injecting an extractant into the gas sampling bag 4. Specifically, referring to fig. 5, the trapping device of the present invention further includes an injector 9, after the gas sampling bag 4 completes the component collection step, the gas sampling bag 4 is communicated with the injector 9, and the injector injects an extractant into the gas sampling bag 4 to obtain a gas-phase extract. A through valve 91 can be arranged between the injector and the gas sampling bag 4, the through valve is opened, so that the extract liquid in the injector can be injected into the gas sampling bag 4, then the through valve 91 is closed, and the gas sampling bag 4 is oscillated, so that the smoke in the gas sampling bag 4 is fully contacted with the extractant.

In the above embodiment, after the extractant is injected into the gas sampling bag 4, the whole gas sampling bag 4 is placed in an environment at a temperature lower than-10 ℃ and kept for more than 15 minutes, thereby reducing experimental errors caused by evaporation of the extractant. And then taking out the liquid in the gas sampling bag to obtain the gas phase extract. Further, the gas sampling bag may be placed in a-20 ℃ refrigerator for cooling for 20 minutes.

The gas sampling bag in each embodiment can be provided with one opening, and simultaneously used as a gas inlet, a liquid inlet and a liquid taking opening, and can be respectively provided with a gas inlet and a larger liquid taking opening, so that liquid taking and cleaning are facilitated. The gas sampling bag may be a Tedlar gas sampling bag or an FEP gas sampling bag.

In the extraction and collection step, the method for measuring the flavor components in the cigarette smoke specifically comprises the following steps of: cutting a filter tip, putting the cut filter tip into a container, adding an extracting agent, carrying out vortex oscillation, and filtering to obtain the filter tip extract liquid; taking out the Cambridge filter disc, putting the Cambridge filter disc into a container, adding an extracting agent, carrying out vortex oscillation, and filtering to obtain a particle-phase extract liquid. Wherein the container can be a centrifuge tube or a conical flask, and the vortex oscillation time can be 10-60 minutes. The volume of the extractant added into the filter tip or the cambridge filter sheet catcher is 10-50 mL.

Further, in the above embodiments, the selected extractant is one of methyl tert-butyl ether, ethanol, isopropanol, dichloromethane, acetone, n-hexane, methanol and acetonitrile. The preferred extractant is methyl tert-butyl ether, which has better extraction effect.

Further, in each of the above embodiments, the extraction agent further includes an internal standard substance, and the internal standard substance is one or more of methyl valerate, methyl heptanoate, methyl nonanoate, methyl undecanoate, methyl tridecanoate, methyl pentadecanoate, propyl benzoate, phenethyl phenylacetate, and phenethyl acetate. The method adopts an internal standard method to analyze and detect the fragrance components, and has higher accuracy.

Furthermore, the determination method of the invention can smoke a plurality of heated cigarettes, and collect the total filter extract, the grain-phase extract and the gas-phase extract of the plurality of heated cigarettes to perform the determination of the flavor components. Sometimes, the content of the aroma components released by smoking of one heated cigarette is low, so that the detection result has large error, the aroma components of a plurality of heated cigarettes can be collected at one time, and after the components and the content are detected, the average value is obtained to obtain the distribution condition of the aroma components of each heated cigarette in the filter tip, the smoke particle phase matter and the smoke gas phase matter respectively. Wherein the upper limit of the number of the cigarettes sucked can be determined according to the bearing capacity of the Cambridge filter.

In addition, the pumping mode can be set by setting the operation mode of the pumping engine 3, and the specific pumping mode is set according to the experimental needs.

In the above embodiments, regarding the component measurement step, the chromatographic conditions and mass spectrometry conditions are set as appropriate for the measurement of the flavor component in the cigarette, and specifically as follows:

and (3) chromatographic column: DB-HeavyWAX capillary column (60 m × 320 μm × 0.25 μm); sample inlet temperature: 280 ℃; carrier gas: helium (more than or equal to 99.999%); constant flow mode flow rate: 1.5mL/min; sample injection amount: 1 mu L of the solution; the split ratio is as follows: 10; temperature rising procedure: 60 deg.C (keeping for 5 min), 5 deg.C/min to 160 deg.C (keeping for 2 min), 10 deg.C/min to 250 deg.C (keeping for 8 min), and 30 deg.C/min to 280 deg.C (keeping for 33 min).

Mass spectrum conditions: the GC/MS interface temperature is 280 ℃; an ionization mode: an electron impact source (EI); transmission line temperature: 280 ℃; ion source temperature: 230 ℃; temperature of the quadrupole rods: 150 ℃; ionization energy: 70eV; solvent retardation: 4min; scanning mode: SCAN and SIM. And for SIM scanning, determining the grouping time of each target substance in the SIM parameters and quantifying ions according to the retention time of each target substance and the corresponding mass spectrogram.

In addition, since the boiling point of flavor components that may remain in the filter is high, the temperature at which the chromatographic conditions of the present invention are finally raised is high. For the smoke particle phase matter and the smoke gas phase matter, the gas chromatography condition can properly reduce the temperature rise temperature, and specifically comprises the following steps:

and (3) chromatographic column: DB-HeavyWAX capillary column (60 m 320 μm 0.25 μm); sample inlet temperature: 280 ℃; carrier gas: helium (more than or equal to 99.999%); constant flow mode flow rate: 1.5mL/min; sample introduction amount: 1 mu L of the solution; the split ratio is as follows: 10, a step of; temperature rising procedure: 60 deg.C (5 min hold), 5 deg.C/min to 160 deg.C (2 min hold), and then 10 deg.C/min to 250 deg.C (8 min hold).

Taking a heated cigarette containing exploded beads in a filter as an example, the contents of the aroma components of the exploded beads in the filter, a filter disc (smoke particulate matter) and a smoke gaseous matter after smoking are measured. The beads used in this example contained the target compositions of Table 1.

TABLE 1 Targeted aroma Retention time and qualitative, quantitative ion selection

The specific operation method comprises the following steps:

taking 5 cigarettes heated by bead blasting, inserting the cigarettes into a heated cigarette smoking set, pinching bead blasting in the filter, triggering a heating device for 3s, starting heating, preheating for 30s, and then starting smoking a first smoke, and smoking 9 cigarettes by referring to the smoking parameters of the HCI smoking mode, namely the smoking capacity of 55mL, the smoking duration of 2s, the smoking interval of 30s and a bell-shaped smoking curve, but not closing the air vent of the filter for smoking. Trapping smoke particulate matters of 5 cigarettes by using a Cambridge filter sheet with the diameter of 44mm, taking out the filter sheet, placing the filter sheet in a 50mL centrifuge tube, simultaneously taking off the corresponding 5 heated cigarette filters, cutting the filter sheet, placing the cut filter sheet in another 50mL centrifuge tube, respectively adding 20mL of methyl tert-butyl ether with the concentration of 2ppm as an internal standard (methyl tridecanoate), oscillating for 60min at 2000 rpm, filtering the obtained extract by a 0.45-micron nylon microporous filter membrane, and then injecting a sample.

Measuring the content of the bead-blasting aroma components in the gas sampling bag (smoke gas phase material) after suction:

the smoking process was as above, and 5L volume Tedlar gas sampling bags were used to collect the smoke vapour phase of 5 cigarettes, the connection being as shown in figure 5. Closing a straight-through valve of the gas sampling bag, taking down the gas sampling bag, injecting 40mL of methyl tert-butyl ether with the concentration of 2ppm of internal standard (methyl tridecanoate) by using an injector, oscillating the sampling bag for 10min to ensure that the absorption solvent fully washes the inner wall of the sampling bag, standing for 30min to obtain a flue gas phase substance absorption liquid in the sampling bag, taking out the absorption liquid for sample injection (in order to reduce the experimental error caused by evaporation of the absorption solvent, placing the absorption liquid in a refrigerator at the temperature of-20 ℃ for 20min before taking out the gas phase substance absorption liquid).

Gas chromatography conditions: a chromatographic column: DB-HeavyWAX capillary column (60 m 320 μm 0.25 μm); sample inlet temperature: 280 ℃; carrier gas: helium (more than or equal to 99.999%); constant flow mode flow rate: 1.5mL/min; sample introduction amount: 1. mu L; the split ratio is as follows: 10, a step of; temperature rising procedure: 60 deg.C (5 min), 5 deg.C/min to 160 deg.C (2 min), 10 deg.C/min to 250 deg.C (8 min), and 30 deg.C/min to 280 deg.C (33 min).

Mass spectrum conditions: the GC/MS interface temperature is 280 ℃; an ionization mode: an electron impact source (EI); transmission line temperature: 280 ℃; ion source temperature: 230 ℃; quadrupole rod temperature: 150 ℃; ionization energy: 70eV; solvent retardation: 4min; scanning mode: SIM mode. The grouping time, the quantitative ions and the auxiliary qualitative ions of each target substance in the SIM scanning parameters are determined according to the retention time and the corresponding mass spectrogram of the fragrance component standard substance in the table 1.

The contents of the target flavor components in the filter tip, the smoke particulate matter and the smoke gaseous matter are shown in table 2.

TABLE 2 test results

Wherein n.d. represents no detection.

As can be seen from Table 2, the distribution of different flavor components in the filter, the particulate matter and the gas phase can be greatly different, and the method of the invention has an important role in researching the distribution of the flavor components in the filter, the particulate matter and the gas phase.

While the invention has been shown and described with reference to certain preferred embodiments thereof, it will be understood by those skilled in the art that the foregoing is a more detailed description of the invention, taken in conjunction with the specific embodiments thereof, and that no limitation of the invention is intended thereby. Various changes in form and detail, including simple deductions or substitutions, may be made by those skilled in the art without departing from the spirit and scope of the invention.

Claims (25)

1. A method for measuring flavor components in cigarette smoke is characterized by comprising the following steps:

component trapping: the method comprises the steps of (1) smoking cigarettes, enabling smoke sucked out to firstly pass through a Cambridge filter disc catcher, and then collecting gas passing through the Cambridge filter disc catcher, so as to respectively obtain smoke particle phase substances and smoke gas phase substances;

and (3) extraction and collection: collecting the functional segments of the cigarettes after smoking is finished, and extracting the flavor components in the functional segments by using an extracting agent to obtain first extract liquor; taking out the Cambridge filter after trapping the smoke, and extracting the fragrance components on the Cambridge filter by using an extracting agent to obtain a particle-phase substance extract liquid; adding an extracting agent into the collected gas, and extracting the fragrant components in the collected gas to obtain gas phase extract liquor;

component determination: and analyzing and detecting the first extraction liquid, the particulate matter extraction liquid and the gas phase matter extraction liquid by using a gas chromatography-mass spectrometer to respectively obtain the types and the contents of the flavor components in the functional section, the smoke particulate matter and the smoke gas phase matter.

2. The method of claim 1, wherein in the component capture set, a gas sampling bag is in communication with the cambridge filter trap such that the smoke passes through the cambridge filter trap and into the gas sampling bag.

3. The method for determining flavor components in cigarette smoke according to claim 2, wherein a flavor component absorber is arranged between the cambridge filter catcher and the gas sampling bag and used for absorbing flavor components in the smoke flowing out of the cambridge filter catcher, and the smoke passes through the cambridge filter catcher and the flavor component absorber and then is collected by the gas sampling bag.

4. The method for determining flavor components in cigarette smoke according to claim 3, wherein a smoking engine is further arranged between the flavor component absorber and the gas sampling bag, and a smoke circulation loop is formed between the gas sampling bag and the flavor component absorber, so that after smoking is finished, smoke in the gas sampling bag is driven by the smoking engine to circulate between the flavor component absorber and the gas sampling bag for a plurality of times.

5. The method for measuring the aroma components in the smoke of the cigarette according to claim 3 or 4, wherein the aroma component absorber is provided with a solid absorbing material for the smoke to pass through, and after the components are captured, an extracting agent is added into the solid absorbing material for extraction to obtain a first gas-phase extract.

6. The method for measuring a flavor component in cigarette smoke according to claim 3 or 4, wherein said flavor component absorber contains an extracting agent for passing said smoke, and a first gas phase extract is obtained in said component trap.

7. The method for determining the flavor components in the cigarette smoke according to claim 5 or 6, wherein the extracting and collecting further comprises injecting an extracting agent into the gas sampling bag, oscillating and absorbing to obtain a second gas-phase extract, and combining the second gas-phase extract with the first gas-phase extract to obtain the gas-phase extract, or using the first gas-phase extract as the gas-phase extract.

8. The method for determining flavor components in cigarette smoke according to claim 2, wherein in the extraction collection, an extractant is injected into the gas sampling bag to obtain the gas phase extract.

9. The method for measuring flavor components in cigarette smoke according to claim 8, wherein after the extracting agent is injected into the gas sampling bag, the whole gas sampling bag is placed in an environment at a temperature lower than-10 ℃ for more than 15 minutes, and then the liquid in the gas sampling bag is taken out to obtain the gas phase extract.

10. The method for determining the flavor components in the cigarette smoke according to claim 1, wherein in the extraction collection, the functional segments are cut and then placed into a container, the extracting agent is added, the oscillation is carried out, and the first extraction liquid is obtained after the filtration; and (3) putting the Cambridge filter into a container, adding the extracting agent, oscillating and filtering to obtain the particle-phase extract liquid.

11. The method for measuring flavor components in cigarette smoke according to claim 10, wherein the oscillation time is 10 to 60 minutes, respectively.

12. The method for measuring a flavor component in cigarette smoke according to any one of claims 1 to 11, wherein the functional segment is a filter.

13. The method for measuring the flavor components in cigarette smoke according to any one of claims 1 to 11, wherein the extractant is one of methyl t-butyl ether, ethanol, isopropanol, dichloromethane, acetone, n-hexane, methanol and acetonitrile.

14. The method for measuring flavor components in cigarette smoke according to any one of claims 1 to 11, wherein the extraction agent further comprises an internal standard substance, and the internal standard substance is one or more of methyl valerate, methyl heptanoate, methyl nonanoate, methyl undecanoate, methyl tridecanoate, methyl pentadecanoate, propyl benzoate, phenylethyl phenylacetate and phenylethyl acetate.

15. The method for measuring the flavor components in the cigarette smoke according to claim 1, wherein a plurality of cigarettes are smoked, and the total first extract, particulate-phase extract and gaseous-phase extract of the plurality of cigarettes are collected to measure the flavor components.

16. A device for trapping aroma components in cigarette smoke, which is used for trapping the components in the method for determining the aroma components in the cigarette smoke according to any one of claims 1 to 14, wherein the cigarette has a functional section, the trapping device comprises a cambridge filter trap, a suction engine and a gas sampling bag, the cambridge filter trap is communicated with the functional section of the cigarette to be determined, the suction engine is respectively communicated with the cambridge filter trap and the gas sampling bag, smoke in the heated cigarette flows out from the functional section of the cigarette through the motive power of the suction engine, passes through the cambridge filter trap and then flows into the gas sampling bag to be collected, and therefore smoke particle phase substances and smoke gas phase substances are respectively obtained in the cambridge filter trap and the gas sampling bag.

17. The cigarette smoke aroma component capturing device of claim 16, further comprising an aroma component absorber positioned between said cambridge filter trap and said gas sampling bag in the direction of smoke flow for absorbing aroma components in smoke exiting said cambridge filter trap.

18. The cigarette smoke aroma component trapping device of claim 17, wherein a smoke circulation loop is formed between the gas sampling bag and the aroma component absorber, so that after the smoking is finished, the smoke in the gas sampling bag is driven by the smoking engine to circulate between the aroma component absorber and the gas sampling bag for a plurality of times.

19. The apparatus for trapping flavor components in cigarette smoke according to claim 18, further comprising a switching valve, a first channel, a second channel and a third channel, wherein the first channel is used for communicating the flavor component absorber, the suction engine and the gas sampling bag and is connected with the switching valve, the second channel is used for communicating the cambridge filter trap and the switching valve, the third channel is used for communicating the gas sampling bag and the switching valve, and the switching valve is used for controlling the opening and closing of the first channel and the second channel and the communication between the first channel and the third channel and controlling the closing of the communication between the second channel and the third channel.

20. The apparatus for trapping a flavor component in cigarette smoke of claim 19, further comprising a first valve disposed on the gas sampling bag and in communication with the third passageway.

21. The device for trapping a flavor component in cigarette smoke according to any one of claims 17 to 20, wherein said flavor component absorber contains a solid absorbing material through which said smoke passes.

22. The apparatus for trapping aroma components in cigarette smoke according to any one of claims 17 to 20, wherein said aroma component absorber contains an extracting agent for passing said smoke.

23. The apparatus for trapping aroma components in cigarette smoke according to claim 22, wherein said aroma component absorber is two or more serially connected absorption bottles, and said extraction agent is contained in said absorption bottles.

24. The apparatus according to any one of claims 16 to 20, further comprising an injector for communicating with the gas sampling bag after the gas sampling bag has finished collecting the smoke, and injecting an extraction agent into the gas sampling bag to obtain a gas phase extract.

25. The apparatus for trapping flavor components in cigarette smoke according to any one of claims 16 to 20, wherein said functional segment is a filter.

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