Method for collecting and detecting atomized released substances of electronic cigarette

Abstract

The invention provides a collection and detection method for electronic cigarette atomized released substances, and belongs to the technical field of electronic cigarette detection. The method comprises the following steps: step 1, adsorbing and collecting aerosol release substances generated after atomization of electronic cigarette atomized liquid by using a solid-phase extraction column, wherein the solid-phase extraction column is filled with an adsorbing material polyethylene divinylbenzene; step 2, eluting the solid-phase extraction column after adsorption in the step 1 to obtain an eluent as a to-be-detected sample solution; and 3, detecting the content of a sweetening agent in the to-be-detected sample solution obtained in the step 2 by using a liquid chromatograph, and detecting the content of a cooling agent and a flavor substance in the to-be-detected sample solution by using a gas chromatograph-mass spectrometer. The method provided by the invention has very good trapping efficiency on substances with various phase states and pH values in aerosol release substances of the electronic cigarette, especially has a relatively strong adsorption effect on low-carbon ester and terpene flavor substances, improves the detection accuracy, and is suitable for simultaneous detection of various components in electronic cigarette products.

Description

Technical Field

[0001] The present invention belongs to the technical field of electronic cigarette detection, and particularly relates to a method for collecting and detecting electronic cigarette aerosolized release substances. Background Art

[0002] The commonly used inhaled substance in electronic cigarette products is e-liquid, that is, an electronic atomization liquid used in conjunction with an electronic cigarette. When heated by an electronic cigarette atomizer, it can generate a mist similar to that of a cigarette, becoming a release substance in the form of an aerosol, that is, a gaseous dispersion system composed of solid or liquid particles suspended in a gas medium. The aerosol generated after electronic cigarette atomization is the direct object inhaled by smokers. Therefore, for harmful substances that are not conducive to human health and components that mainly reflect the sensory quality of electronic cigarettes, such as sweeteners, cooling agents, and flavor substances with aromatic odors, accurately detecting the content of the above components plays an important role in the evaluation and improvement of the quality of electronic cigarette products.

[0003] To detect the content of various components in electronic cigarette aerosolized release substances, the first step is to capture the release aerosol. Since the release aerosol contains gaseous, liquid, and solid substances at the same time, and different states of substances contain acidic, alkaline, and neutral compounds at the same time, the components are complex and the properties of different components vary greatly. Therefore, it is difficult to effectively, completely, and non-specifically collect and adsorb components of various forms or properties in the aerosol.

[0004] Currently, the commonly used methods for capturing electronic atomizer aerosol include: 1. Cambridge filter capture; 2. Foaming trap using organic or inorganic solvents; 3. Cold trap capture; 4. Electrostatic capture; 5. Tube-type or box-type adsorption boxes; 6. Activated carbon adsorption, etc. Among them, the Cambridge filter method is applicable to particles with a diameter greater than 0.2 μm and is commonly used for substances with high contents such as nicotine, propylene glycol, and glycerol; the foaming trap method is commonly used for collecting characteristic substances such as nicotine, aldehydes and ketones, and heavy metals; the cold trap capture is commonly used for detecting volatile substances, but the cold trap equipment has a high cost and low stability; the electrostatic capture method is only used for heavy metal detection; there are few existing standards and literatures on the adsorption method, and it is only used for aldehydes and ketones testing at present; the activated carbon adsorption method has good adsorption for various substances in the aerosol, but the desorption is difficult, and even some substances with low contents cannot be desorbed smoothly.

[0005] At the same time, some adsorption methods in electronic cigarettes or other fields are also provided in the prior art. For example, Patent CN217218166U uses activated carbon with different pore volumes for adsorption; Patents CN105842378A and CN118225931A use filters for capture; Patent CN104324521A uses a variety of adsorption materials including activated carbon and silica gel for elution and purification. However, the above methods are similar in principle and effect to the several methods mentioned above, and the improvement effect is not good.

[0006] Although there are many existing methods for testing the aerosol of e-cigarettes, during the collection process, the recovery rate of substances is low; and each collection is only used for testing one substance, which brings a relatively large workload to the testing. Therefore, there is an urgent need for a convenient and economical method and device suitable for the simultaneous collection of various substances in the aerosol. Summary of the Invention

[0007] To solve the above problems, the present application aims to provide a method for collecting multiple components in the aerosol generated after the atomization of e-cigarette oil, especially sweeteners, cooling agents, and various flavor substances, and facilitating subsequent elution and reuse for detection and analysis by analytical instruments, for the identification of e-cigarette aerosol components and related research work.

[0008] On the one hand, the present application provides a method for collecting and detecting the atomized release of e-cigarettes, the method comprising:

[0009] Step 1: Adsorb and collect the aerosol release generated after the atomization of the e-cigarette liquid using a solid-phase extraction column, and the adsorption material filled in the solid-phase extraction column is polyvinyl divinylbenzene;

[0010] Step 2: Elute the solid-phase extraction column after the adsorption in Step 1 to obtain an eluate as a sample solution to be tested;

[0011] Step 3: Use a liquid chromatograph to detect the content of sweeteners in the sample solution to be tested obtained in Step 2, and use a gas chromatography-mass spectrometry instrument to detect the content of cooling agents and flavor substances.

[0012] In one embodiment, the e-cigarette liquid can be atomizable e-liquid, e-juice, tobacco flavor, or tobacco additive.

[0013] In one embodiment, the average particle size of the polyvinyl divinylbenzene is 20 - 60 μm, the average pore size is 10 - 80 μm, and the specific surface area is 500 - 700 m 2 / g.

[0014] In one embodiment, the filling amount of the polyvinyl divinylbenzene is (150 mg - 1 g) : (1 ml - 6 ml).

[0015] The "filling amount" in the present application can be understood as how many grams of polyvinyl divinylbenzene particles are filled in a column shell with a certain volume. Among them, the polyvinyl divinylbenzene with the above particle structure can achieve a better trapping and adsorption effect under the above filling amount.

[0016] In one embodiment, in step one, the aerosol release is adsorbed on the adsorbent material of the solid-phase extraction column by suction. The conditions for suction are as follows: the number of suction ports is 20 to 50; the suction frequency is 5 to 60 s; the suction duration is 1 to 10 s; the suction volume is 20 to 80 ml; the suction flow rate is 10 to 30 ml / s.

[0017] In one embodiment, when performing the suction test, the inclination angle α of the e-liquid chamber of the electronic atomizer is -45°, and the nozzle at its top is aligned with the axis of the solid-phase extraction column.

[0018] In one embodiment, in step two, methanol is used as the elution solvent for elution.

[0019] In one embodiment, in step three, the sweeteners include neotame, sucralose, neohesperidin dihydrochalcone, and naringin dihydrochalcone.

[0020] In one embodiment, the cooling agents include N,2,3-trimethyl-2-isopropylbutyramide (WS-23), menthamide (WS-3).

[0021] In one embodiment, the flavor substances include low-carbon esters and terpenoids.

[0022] On the other hand, the present application provides a method for detecting gaseous volatile substances in an e-cigarette aerosol release, the method comprising:

[0023] Step a: Adsorb and collect the aerosol release generated after atomizing the e-cigarette liquid using a solid-phase extraction column, wherein the adsorbent material filled in the solid-phase extraction column is polyvinyl divinylbenzene;

[0024] Step b: Elute the solid-phase extraction column after adsorption in step one to obtain an eluate as a sample solution to be measured;

[0025] Step c: Use a gas chromatography-mass spectrometry instrument to detect the content of gaseous volatile substances in the sample solution to be measured obtained in step two, and the gaseous volatile substances include low-carbon esters and terpene flavor substances.

[0026] In one embodiment, the low-carbon esters include: propyl acetate, isobutyl acetate, ethyl butyrate, ethyl 2-methylbutyrate, and cis-3-hexen-1-yl acetate.

[0027] In one embodiment, the terpene flavor substances include: tricyclene, α-pinene, camphene.

[0028] On the other hand, the present application provides the application of the above method in the quality analysis and detection of e-cigarette products.

[0029] On the other hand, the present application provides the use of polyvinyl divinylbenzene in the preparation of a flue gas collection adsorbent.

[0030] In one embodiment, the average particle size of the polyvinyl divinylbenzene particles is 20 - 60 μm, the average pore size is 10 - 80 μm, and the specific surface area is 500 - 700 m2 / g.

[0031] On the other hand, the present application provides a collection device for electronic cigarette aerosolized releases, the device comprising:

[0032] A release collection unit for collecting the aerosol releases generated after the atomization of the electronic cigarette atomization liquid;

[0033] The release collection unit includes a solid phase extraction column filled with polyvinyl divinylbenzene;

[0034] And

[0035] A suction unit for sucking the electronic cigarette; the suction unit is connected to the release collection unit so that the aerosol releases generated by sucking the electronic cigarette flow through the solid phase extraction column and are adsorbed and collected by the polyvinyl divinylbenzene material.

[0036] On the other hand, the present application provides an analysis system for electronic cigarette aerosolized releases, the analysis system comprising:

[0037] A collection module for collecting electronic cigarette aerosolized releases;

[0038] An elution module for eluting the electronic cigarette aerosolized releases collected by the collection module and obtaining an eluate; and

[0039] An analysis module for detecting the components of the eluate obtained by the elution module;

[0040] Wherein, the collection module includes the above-mentioned collection device for electronic cigarette aerosolized releases.

[0041] In one embodiment, the elution solvent used for elution in the elution module is methanol.

[0042] In one embodiment, the analysis module includes detection and analysis equipment using mass spectrometry, chromatography, spectroscopy or any combination thereof, such as a mass spectrometer, a gas chromatograph, a liquid chromatograph, a gas - mass spectrometer, a liquid - mass spectrometer, an infrared spectrometer, a ultraviolet spectrometer, a Raman spectrometer, etc.

[0043] The present application has at least the following beneficial effects:

[0044] The collection and detection method of the aerosol release of the electronic cigarette provided by the present application uses a solid-phase extraction column as the adsorption and collection device for the smoke aerosol. Different from the traditional separation and purification using a solid-phase extraction column, the present application uses polyvinyl divinylbenzene as the adsorption material of the solid-phase extraction column. Utilizing the pyrrolidone-bonded trace urea functional groups on the surface of polyvinyl divinylbenzene and under the conditions of specific pore characteristics and adsorption capacity, it can simultaneously and efficiently adsorb gaseous, liquid, and solid substances as well as acidic, alkaline, and neutral substances in the aerosol release, especially having a significant adsorption effect on volatile gaseous substances such as low-carbon esters and terpenoids in flavor substances, and having a high elution efficiency in subsequent elution steps, which is beneficial for the analysis and detection of various components. The experimental results show that the overall capture efficiency of the collection device of the present application for the aerosol can reach more than 99%, and the recovery rate is 94.7% - 110.6%. The operation is simple and efficient, and the result accuracy and repeatability are high, which has a positive effect on the quality detection and improvement of e-cigarette products. Brief Description of the Drawings

[0045] The drawings here are incorporated into the description and form a part of this description, showing the embodiments in line with the present invention and used together with the description to explain the principles of the present invention.

[0046] In order to more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the following will briefly introduce the drawings required for use in the description of the embodiments or the prior art. For those of ordinary skill in the art, without creative efforts, other drawings can also be obtained based on these drawings. In the drawings:

[0047] Figure 1 is the structural schematic diagram of the aerosol release collection device in Embodiment 1;

[0048] Figure 2 is Figure 1 the structural schematic diagram of the solid-phase extraction column in;

[0049] In the figure: 1, smoking machine; 2, solid-phase extraction column; 3, e-cigarette; 4, suction joint; 5, connecting piece; 201, outer tube; 202, packing; 203, first sieve plate; 204, second sieve plate. Detailed Embodiments

[0050] In order to more clearly explain the overall concept of the present application, the following will be described in detail by way of embodiments. In the following description, a large number of specific details are given to provide a more thorough understanding of the present application. However, it is obvious to those skilled in the art that the present application can be implemented without one or more of these details. In other examples, in order to avoid confusion with the present application, some well-known technical features in the art are not described.

[0051] Unless otherwise specified, in the following embodiments, the reagents or instruments used without indicating the manufacturer are all conventional products that can be obtained by purchasing in the market.

[0052] For those not specifying the specific conditions in the embodiments, they are carried out according to the conventional conditions or the conditions recommended by the manufacturer.

[0053] Example 1

[0054] The first embodiment of the present application provides a collection device for the aerosolized release of an electronic cigarette. This collection device can simultaneously collect various components in the aerosol generated after the atomization of e-liquid, especially sweeteners, cooling agents, and various flavor substances, and is convenient for subsequent elution and reuse for detection and analysis by analytical instruments, and is used for the identification of e-cigarette aerosol components and related research work.

[0055] As Figure 1 shown, the collection device includes: a release capture unit for capturing the aerosolized release generated after the atomization of the e-cigarette liquid.

[0056] Among them, the release capture unit includes a solid-phase extraction column 2, referring to Figure 1 and Figure 2 , the solid-phase extraction column 2 includes a hollow and through columnar outer shell, such as a syringe-shaped outer tube 201, which has two opposite and open ends, namely an air inlet end for receiving the smoke and an air outlet end for allowing the smoke to flow towards the suction unit. When collecting the smoke, the air flow release end of the e-cigarette 3 is connected to the air inlet end of the solid-phase extraction column 2.

[0057] Continue to refer to Figure 1 and Figure 2 , the solid-phase extraction column 2 is filled with a polymer adsorption material 202 for adsorbing and collecting the aerosolized release. Among them, the polymer adsorption material 202 is tightly filled inside the columnar outer tube 201. When performing the adsorption capture operation, the air flow generated by sucking the e-cigarette can enter from the air inlet end of the solid-phase extraction column 2, and after being adsorbed by the densely packed polymer adsorption material, it flows out of the solid-phase extraction column 2 from the air outlet end. Optionally, to avoid the interference of the outer shell on the air flow components during adsorption, the material of the outer tube 201 can be polyethylene or polypropylene.

[0058] In this embodiment, the polymer adsorbent 2 is polyvinyl divinylbenzene. Preferably, the average particle size of the polyvinyl divinylbenzene is 20 - 60 μm, such as 20 μm, 30 μm, 40 μm, 50 μm, 60 μm; the average pore size is 10 - 80 μm, such as 10 μm, 20 μm, 30 μm, 40 μm, 50 μm, 60 μm, 70 μm, 80 μm; the specific surface area is 500 - 700 m2 / g, such as 500 m2 / g, 600 m2 / g, 700 m2 / g; the filling amount is (150 mg - 1 g):(1 ml - 6 ml).

[0059] Among them, the "filling amount" can be understood as how many grams of polyvinyl divinylbenzene particles are filled in a column shell with a certain volume. Among them, the polyvinyl divinylbenzene with the above particle structure can achieve a better trapping and adsorption effect under the above filling amount. Optionally, in this embodiment, the filling amount of polyvinyl divinylbenzene in the outer tube 201 can be 150 mg / 1 ml, 200 mg / 3 ml, 300 mg / 4 ml, 400 mg / 5 ml, 500 mg / 6 ml, 600 mg / 6 ml, 700 mg / 3 ml, 800 mg / 5 ml, 900 mg / 6 ml, 1 g / 6 ml.

[0060] Among them, the solid-phase extraction column 2 with the above pore characteristics and filling amount can be made by oneself or can use commercially available products. For example, the solid-phase extraction cartridge with the brand model of Agela Cleanert PEP-2, and the specification can be 500 mg / 6 ml.

[0061] Continue to refer to Figure 1 and Figure 2 , in order to clamp and fix the polymer adsorbent 202, a porous first sieve plate 203 and a second sieve plate 204 are also arranged in the solid-phase extraction column 2. Among them, when the first sieve plate 203 and the second sieve plate 204 clamp the polymer adsorbent 202, they can be placed at any position inside the outer tube 201. For better adsorption of the air flow, it is preferably at the position near the air inlet end as shown in Figure 2 . Among them, the materials of the porous sieve plates 203 and 204 are preferably polyethylene.

[0062] As shown in Figure 1 , a connector 5 for receiving aerosol releases is arranged at the air inlet end of the solid-phase extraction column 2. In this embodiment, the connector 5 is a tubular connecting pipe, and the material of the connector is preferably polyethylene.

[0063] Among them, the porous sieve plates and connectors made of polyethylene have almost no adsorption effect on the flue gas, which is beneficial to reducing the loss of substances in the flue gas.

[0064] Continue to refer to Figure 1, the device further includes a suction unit for sucking the electronic cigarette, and the suction unit is connected to the above-mentioned release capture unit so that the aerosol release flow generated by sucking the electronic cigarette flows through the solid-phase extraction column 2 and is adsorbed and captured by the polymer adsorption material 202.

[0065] In one embodiment, the suction unit includes a smoking machine 1, which can provide power for the suction action of the electronic cigarette and can set suction parameters including but not limited to suction frequency, suction flow rate, suction duration, number of suction puffs, etc. according to experimental requirements.

[0066] Continue to refer to Figure 1 , the smoking machine 1 has an open suction joint 4, which can be used to block the outlet end of the solid-phase extraction column 2 so that the airflow after adsorption flows from the solid-phase extraction column 2 into the smoking machine 1.

[0067] In one embodiment, the smoking machine 1 can be a commercially available automatic smoking machine for electronic cigarettes, such as a smoking machine with the manufacturer and model Jingyao JY-JM08.

[0068] In one embodiment, when performing a suction test, the e-liquid cartridge of the electronic cigarette is placed with a downward inclination in the horizontal direction, the inclination angle is preferably 45°, and the mouthpiece at its top is axially aligned with the solid-phase extraction column 2. Optionally, to achieve the above-mentioned inclination angle of the electronic cigarette, the collection device may further be provided with a clamping assembly for fixing the electronic cigarette 3, and the clamping assembly can adopt conventional clamping tools, such as a clamping table base with a clip in chemical experimental instruments, which are not shown in the figure.

[0069] Among them, the collection device of this embodiment uses a solid-phase extraction column 2 filled with polyvinyl divinylbenzene as the polymer adsorption material 202 to adsorb and collect the aerosol release of the electronic cigarette 3. The surface of the polyvinyl divinylbenzene is bonded with pyrrolidone with a trace amount of ureido functional groups, and under the conditions of specific pore characteristics and dosage, it can simultaneously and efficiently adsorb gaseous, liquid and solid substances as well as acidic, alkaline and neutral substances in the aerosol release, especially volatile gaseous substances such as low-carbon esters and terpenoids in flavor substances, and has a significant adsorption effect, and has a high elution efficiency in subsequent elution steps, which is beneficial to the analysis and detection of various components.

[0070] Example 2

[0071] The second embodiment of the present application provides an electronic cigarette atomization release analysis system, wherein the analysis system includes:

[0072] A collection module for collecting electronic cigarette atomization releases;

[0073] An elution module for eluting the electronic cigarette atomization releases collected by the collection module and obtaining an eluate; and

[0074] An analysis module, used for detecting the components of the eluate obtained by the elution module;

[0075] The collection module in this embodiment adopts the device for collecting electronic cigarette aerosolized substances provided in Embodiment 1.

[0076] In one embodiment, the elution module may use conventional laboratory elution instruments, such as a separatory funnel for extraction, a rotary evaporator for concentrating the elution solvent, etc. Preferably, the elution solvent used for elution in the elution module is methanol.

[0077] In one embodiment, the analysis module includes detection and analysis equipment using mass spectrometry, chromatography, spectroscopy or any combination of these, such as a mass spectrometer, gas chromatograph, liquid chromatograph, gas-mass spectrometer, liquid-mass spectrometer, infrared spectrometer, ultraviolet spectrometer, Raman spectrometer, etc.

[0078] Optionally, the above-mentioned analytical instruments can be commercially available chemical analytical instruments, such as Agilent 8860-5977B gas chromatograph-mass spectrometer (GCMS), Waters E2695 high performance liquid chromatograph (with 2998 photodiode array (PDA) detector), Aotai 6100 evaporative light detector (ELSD), etc.

[0079] Optionally, the electronic cigarette atomizing liquid may be atomizable cigarette oil, cigarette flavoring or cigarette additive.

[0080] In one embodiment, the collecting device is used to collect sweeteners, cooling agents and flavoring substances in the electronic cigarette aerosol release. Optionally, the sweeteners include neotame, sucralose, neomethyl hesperidin dihydrochalcone, and naringin dihydrochalcone. Cooling agents include N,2,3-trimethyl-2-isopropylbutyramide (WS-23) and menthyl amide (WS-3). Flavoring substances include low-carbon esters and terpenes, wherein low-carbon esters include: propyl acetate, isobutyl acetate, ethyl butyrate, ethyl 2-methylbutyrate, and leaf acetate; terpene flavoring substances include: tricyclic alkenes, α-pinene, and camphene.

[0081] Example 3

[0082] This embodiment provides a method for collecting and detecting electronic cigarette aerosol release, comprising the following steps:

[0083] Step 1: using a solid phase extraction column to adsorb and collect aerosol release generated after the electronic cigarette atomization liquid is atomized;

[0084] Step 2, eluting the solid phase extraction column after adsorption in step 1, and obtaining the eluate as the sample solution to be tested;

[0085] Step 3. Use a liquid chromatograph to detect the content of sweeteners in the sample solution to be tested obtained in Step 2, and use a gas chromatography-mass spectrometry (GC-MS) instrument to detect the content of cooling agents and flavor substances in it.

[0086] Preferably, this method uses the collection device shown in Example 1 to achieve the collection and adsorption in Step 1.

[0087] Among them, the suction conditions of the smoking machine in Step 1 are shown in Table 1:

[0088] Table 1 Suction test parameters of the electronic atomizer

[0089]

[0090] Among them, the number of puffs of the electronic atomizer is 20, the tilt angle α of the oil chamber of the electronic atomizer during the suction test is -45°, and the top nozzle is aligned with the equipment axis.

[0091] Specifically, the component elution in Step 2 is carried out as follows: After the suction is completed, remove the adsorption column and fix it on the extraction device, and elute it 4 times with 20 ml of methanol, that is, each elution uses 5 ml of methanol and is eluted 4 times. After the elution is completed, collect all the eluates, filter them through a 0.22 μm filter membrane, transfer the filtered solution into a 1.5 ml chromatographic vial and test it on the machine.

[0092] Specifically, the detection method in Step 3 is carried out as follows:

[0093] (1) Sweetener test: Test the content of various sweeteners in the collected eluate with a liquid chromatograph. Among them, neotame, neohesperidin dihydrochalcone (NHDC), and naringin dihydrochalcone are detected with a PDA detector, and sucralose is detected with an ELSD detector. The content of sweeteners in the aerosol is finally determined by calculation.

[0094] (2) Cooling agent test: Detect the collected eluate with a gas chromatography-mass spectrometry (GC-MS) instrument, and quantify various cooling agents in the collected liquid. The content of cooling agents in the aerosol is finally determined by calculation.

[0095] (3) Flavor substance test: Detect the collected eluate with a gas chromatography-mass spectrometry (GC-MS) instrument, and qualitatively and semi-quantitatively analyze the flavor substances in the collected liquid by semi-quantitative method. The content of each flavor substance in the aerosol is finally confirmed by calculation.

[0096] The equipment information involved in this embodiment and the following embodiments is as follows: Brand model of the smoking machine: JY-JM08 Jingyao; Brand model of the gas chromatography-mass spectrometry (GCMS): Agilent8860-5977B; Brand model of the high performance liquid chromatography: Waters E2695 with 2998 photodiode array (PDA) detector; Brand model of the evaporative light scattering detector (ELSD): Aotai 6100.

[0097] Example 4

[0098] In this embodiment, the adsorption material used in step one of the detection method provided in Example 3 is optimized and selected. The specific method is as follows:

[0099] Select 5 portions of the same batch of e-cigarette aerosol (1#), and select 5 different types of solid phase extraction columns with the same specifications. The packing types are: polyvinyl divinylbenzene, silica gel, Florisil, C18, and neutral alumina. As Figure 1 shown, connect the e-cigarette in series with the solid phase extraction column and the smoking machine at the same time, and carry out puffing according to the puffing parameters shown in Table 1. At the same time, collect 20 breaths of aerosol for 5 groups of samples. After the puffing is completed, elute each solid phase extraction with 20 mL of methanol in 4 times, and finally combine and constant volume the eluate to 20 mL. After mixing, filter through a 0.22 μm filter membrane and then test by HPLC and GC-MS. The test results of the sweeteners, cooling agents and flavor substances obtained by the instrument are shown in Table 2:

[0100] Table 2 Test results of each component in the aerosol

[0101]

[0102]

[0103]

[0104] It can be seen from the data in Table 2 that the collection efficiency of each component of the aerosol varies for different types of packings. Comparing the 5 different types of packings, the polyvinyl divinylbenzene packing has a better collection effect on various components than the other 4 packings, especially for terpene substances such as tricyclene, α-pinene, camphene, etc. Therefore, the packing of the solid phase extraction column selected in this method is polyvinyl divinylbenzene.

[0105] Example 5

[0106] In this embodiment, the elution solvent used in step two of the detection method provided in Example 3 is optimized and selected. The specific method is as follows:

[0107] Weigh 4 portions of 0.2 g each of the same e-cigarette aerosol (2#). Place one portion in a 20 mL volumetric flask and make up the volume with methanol (this solution is used for testing the theoretical values of each analyte to be measured). Place the other 3 portions in solid-phase extraction columns, and elute the solid-phase extraction with 20 mL of methanol, ethanol, and isopropanol respectively in 4 times. Combine the eluates and make up the volume to 20 mL. Then, pass the samples in the volumetric flask and the collected liquid passing through the extraction column through a 0.22 μm filter membrane and load them onto the machine, and test the contents of sweeteners, cooling agents, and flavor substances using HPLC and GC-MS respectively. The final test results are shown in Table 3:

[0108] Table 3 Differences in recovery rates of elution with different solvents

[0109]

[0110]

[0111]

[0112] As shown in the data in Table 3, when eluting with methanol, the recovery rates of each substance are all in the range of 94.7% - 102.6%. When eluting with ethanol, the recovery rates of each substance (except ethanol) are all in the range of 91.4% - 101.4%. When eluting with isopropanol, the recovery rates of each substance are all in the range of 48.5% - 99.9%. Generally speaking, the recovery rates of elution with methanol and ethanol are both better. However, considering that most e-cigarette aerosols may contain ethanol, methanol is finally selected as the optimal eluting solvent. At the same time, this example proves that this adsorption column can elute sweeteners, cooling agents, and flavor substances in e-cigarette aerosols well, and there is no specific adsorption situation.

[0113] Example 6

[0114] In this example, an experiment was carried out on the stability of the detection method provided in Example 3 under optimal conditions. The specific method is as follows:

[0115] Select 3 portions of the same batch of e-cigarette aerosol (3#), and connect the e-cigarette in series with the solid-phase extraction column and the smoking machine as shown in Figure 1 , and carry out puffing according to the puffing parameters shown in Table 1. At the same time, collect 20 breaths of aerosol for 3 groups of samples. After the puffing is completed, elute the solid-phase extraction with 20 mL of methanol in 4 times. Finally, combine the eluates and make up the volume to 20 mL. After mixing, pass through a 0.22 μm filter membrane and load it onto the machine, and then test it using HPLC and GC-MS respectively. Weigh the e-cigarette atomizer and the solid-phase extraction column accurately before and after puffing, and calculate the loss amount of the e-cigarette atomizer and the collection amount of the adsorption device by the difference method. The overall absorption and collection situation of the aerosol is shown in Table 4, and the results of the contents of sweeteners, cooling agents, and flavor substances obtained by instrument testing are shown in Table 5:

[0116] Table 4 Aerosol collection effect

[0117]

[0118]

[0119] Table 5 Test results of each component of the aerosol

[0120]

[0121]

[0122] It can be seen from the data in Table 4 that according to the experimental procedure described in Example 3, the overall capture efficiency of this method for the aerosol can reach more than 99%; the data in Table 5 shows that this method has good adsorption and elution effects on each component of the aerosol and has high stability at the same time.

[0123] Comparative Example 1

[0124] This comparative example is the comparative example of Example 6. Compared with Example 3, in this example, the capture solid-phase extraction column of the sol is replaced with a Cambridge filter. The specific steps include: selecting 1 part of the e-cigarette aerosol (3#), connecting the e-cigarette in series with the Cambridge filter collection box and the smoking machine. There are two Cambridge filters placed in the Cambridge filter collection box, and the suction is carried out according to the suction parameters shown in Table 1, and 20 breaths of aerosol are collected at the same time. After the suction is completed, the Cambridge filter is extracted with 20 mL of methanol in portions. After sufficient extraction, it is filtered through a 0.22 μm filter membrane and then tested by HPLC and GC-MS. The e-cigarette atomizer and the solid-phase extraction column are accurately weighed before and after suction. The test results of the contents of sweeteners, cooling agents and flavor substances obtained by the instrument are shown in Table 6:

[0125] Table 6 Test results of each component of the aerosol captured by the Cambridge filter

[0126]

[0127]

[0128] Comparing the data in Table 5 and Table 6, it can be seen that using the adsorption device and detection method provided in this application, various flavor substances in the aerosol can be better captured, especially for low-carbon esters and terpenes and other volatile substances in the gaseous part of the aerosol. Therefore, it can be shown that the aerosol components obtained by using this e-cigarette collection and analysis technology have the advantages of being more comprehensive and accurate, and can provide reliable data support for subsequent related aerosol research.

[0129] The above is only an embodiment of the present application and is not intended to limit the present application. For those skilled in the art, the present application may have various changes and variations. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the scope of the claims of the present application.

Claims

1. A method for collecting and detecting electronic cigarette aerosol release, characterized in that: The method comprises: Step 1: using a solid phase extraction column to adsorb and collect aerosol release generated after the electronic cigarette atomization liquid is atomized, wherein the adsorption material filled in the solid phase extraction column is polyethylene divinylbenzene; Step 2, eluting the solid phase extraction column after adsorption in step 1, and obtaining the eluate as the sample solution to be tested; Step 3: The sample liquid obtained in step 2 is used to detect the sweetener content thereof by liquid chromatography, and the cooling agent and flavor substance content thereof by gas chromatography-mass spectrometry.

2. The method according to claim 1, characterized in that The average particle size of the polyethylene divinylbenzene is 20-60 μm, the average pore size is 10-80 μm, and the specific surface area is 500-700 m 2 / g; And / or, the filling amount of the polyethylene divinylbenzene is (150mg-1g): (1ml-6ml).

3. The method according to claim 1, characterized in that In the step 1, the aerosol release is adsorbed on the adsorption material of the solid phase extraction column by suction, and the suction conditions are: the number of suction puffs is 20 to 50 puffs; the suction frequency is 5 to 60 seconds; the suction duration is 1 to 10 seconds; the suction volume is 20 to 80 ml; and the suction flow rate is 10 to 30 ml / s.

4. The method according to claim 1, characterized in that The elution in step 2 uses methanol as the elution solvent.

5. The method according to claim 1, characterized in that In the step 3, the sweetener includes neotame, sucralose, neomethyl hesperidin dihydrochalcone, and naringin dihydrochalcone; and / or, the cooling agent includes WS-23, WS-3; And / or, the flavor substances include low-carbon esters and terpenes.

6. A method for collecting and detecting gaseous volatile substances in electronic cigarette aerosol release, characterized in that: The method comprises: Step a, using a solid phase extraction column to adsorb and collect aerosol release generated after the electronic cigarette atomization liquid is atomized, wherein the adsorption material filled in the solid phase extraction column is polyethylene divinylbenzene; Step b, eluting the solid phase extraction column after adsorption in step 1, and obtaining an eluate as a sample solution to be tested; Step c, using a gas chromatography-mass spectrometer to detect the content of gaseous volatile substances in the sample liquid obtained in step 2; The gaseous volatile substances include low-carbon esters and terpene flavor substances.

7. The method according to claim 6, characterized in that The low carbon esters include: propyl acetate, isobutyl acetate, ethyl butyrate, ethyl 2-methylbutyrate, and leaf acetate; And / or, the terpene flavor substances include: tricycloene, α-pinene, and camphene.

8. Application of the method according to any one of claims 1 to 5, or the method according to claim 6 or 7, in the quality analysis and detection of electronic cigarette products.

9. Application of polyethylene divinylbenzene in the preparation of flue gas collection adsorbent.

10. The use according to claim 9, characterized in that: The average particle size of the polyethylene divinylbenzene is 20-60 μm, the average pore size is 10-80 μm, and the specific surface area is 500-700 m 2 / g.

Images