Collection method and detection method for content of cyclosiloxane in aerosol and application thereof

Abstract

The invention relates to a collection method, a detection method and application of the content of cyclosiloxane in aerosol. The collection method comprises the following steps: sequentially filtering aerosol by a Cambridge filter and absorbing the aerosol by n-hexane to respectively obtain an enriched filter and n-hexane absorption liquid; the enrichment filter disc is placed in the n-hexane absorption liquid for extraction, and cyclosiloxane collection liquid is obtained. According to the collection method, cyclosiloxane in the aerosol can be effectively collected, then accurate detection of trace cyclosiloxane in the aerosol can be achieved by detecting the cyclosiloxane collection liquid, the detection accuracy is improved, and the method can be used for testing the content of trace cyclosiloxane in the aerosol of the electronic cigarette. The invention further provides a collection device for cyclosiloxane in the aerosol, a detection method for the content of cyclosiloxane in the aerosol and application of the collection method or the collection device or the detection method to detection of the content of cyclosiloxane in the aerosol of an electronic cigarette or quality detection of the electronic cigarette.

Description

Technical Field

[0001] The present application relates to the technical field of analytical chemistry, and in particular to a collection method and a detection method for cyclosiloxane content in an aerosol and applications thereof. Background Art

[0002] Silicone rubber is widely used in electronic cigarette products, and some silicone rubber will be immersed in electronic cigarette aerosol liquid containing a large amount of organic matter for a long time. Cyclosiloxanes, such as octamethylcyclotetrasiloxane (D4), decamethylcyclopentasiloxane (D5), and dodecamethylcyclohexasiloxane (D6), are important intermediates for the preparation of silicone rubber, with high volatility and high diffusion coefficient. When the electronic cigarette is heated, it is easy for the cyclosiloxane to be absorbed by the human body with the aerosol atomization. Studies have found that cyclosiloxanes such as D4, D5, and D6 are toxic to the human nervous, immune, and reproductive systems, and are carcinogenic and mutagenic. These three cyclosiloxanes have been included in the list of substances of very high concern (SVHCs) by the European Chemicals Agency (ECHA). The European Commission (EU) Amendment No. 2018 / 35 stipulates that the content of D4 and D5 in water-washable cosmetics must be less than 0.1%. If cyclosiloxanes enter the human body through electronic cigarette aerosols, it will bring safety hazards.

[0003] Since the content of cyclosiloxane in electronic cigarette aerosol is generally very low, usually far below 1 mg / L, it is difficult for existing methods to fully collect cyclosiloxane in electronic cigarette aerosol, affecting the accuracy of subsequent detection. In addition, the existing methods for detecting the content of cyclosiloxane have low sensitivity and cannot meet the detection requirements of trace cyclosiloxane in electronic cigarette aerosol.

[0004] Therefore, it is of great significance to develop a method to efficiently collect or detect the content of cyclosiloxanes in e-cigarette aerosol. Summary of the invention

[0005] The present invention aims to solve at least one of the above technical problems existing in the prior art. To this end, the present invention provides a method for collecting cyclosiloxane in aerosol, which can effectively enrich the cyclosiloxane in aerosol.

[0006] The invention also provides a device for collecting cyclosiloxane in aerosol.

[0007] The invention also provides a method for detecting the content of cyclosiloxane in the aerosol.

[0008] The present invention also proposes the application of the above-mentioned collection method or collection device or detection method.

[0009] Specifically, the embodiment of the first aspect of the present invention relates to a method for collecting cyclosiloxane in an aerosol, comprising the steps of:

[0010] The aerosol was filtered through Cambridge filter disc and absorbed by n-hexane in turn to obtain enriched filter disc and n-hexane absorption liquid, respectively;

[0011] The enrichment filter disc is placed in the n-hexane absorption liquid for extraction to obtain a cyclosiloxane collection liquid.

[0012] The method for collecting cyclosiloxane in aerosol according to the first aspect of the present invention has at least the following beneficial effects:

[0013] The aerosol is first filtered through a Cambridge filter and then absorbed by n-hexane, which can effectively collect the cyclosiloxanes in the aerosol. The cyclosiloxane collection liquid can then be tested to accurately detect the trace cyclosiloxane content in the aerosol.

[0014] The Cambridge filter and n-hexane have a synergistic effect of increasing the amount of cyclosiloxane collected. If the Cambridge filter or n-hexane is used alone for collection, or if the n-hexane in the method is replaced with other solvents, it is difficult to ensure the amount of cyclosiloxane collected.

[0015] According to some embodiments of the first aspect of the present invention, oscillation is performed during the extraction process.

[0016] According to some embodiments of the first aspect of the present invention, the extraction time is 10-60 minutes to take into account both extraction effect and efficiency.

[0017] According to some embodiments of the first aspect of the present invention, the extraction time is 30-60 min.

[0018] According to some embodiments of the first aspect of the present invention, the aerosol is formed by heating the atomized liquid.

[0019] According to some embodiments of the first aspect of the present invention, the atomized liquid is an electronic cigarette atomized liquid.

[0020] According to some embodiments of the first aspect of the present invention, a smoking machine is used to filter the aerosol through a Cambridge filter and absorb it with n-hexane in sequence to obtain an enriched filter and a n-hexane absorption liquid, respectively.

[0021] According to some embodiments of the first aspect of the present invention, the smoking mode of the smoking machine is: single puff duration: (3.0±0.1) s, single puff volume: (55.0±0.6) mL, and puff frequency: (30.0±0.5) s / puff, so as to simulate human smoking.

[0022] According to some embodiments of the first aspect of the present invention, the number of puffs of the smoking machine is 20-500, and / or the volume of the n-hexane is 20-50 ml.

[0023] Furthermore, the smoking machine has 50-150 puffs.

[0024] It is understandable that the number of puffs affects the amount of aerosol tested, which in turn affects the quality of the collected cyclosiloxanes. For electronic cigarette aerosols, the cyclosiloxane content may be lower than 0.02 mg / L. If the number of puffs is too low, the amount of cyclosiloxane collected is low, which may be difficult to meet the test sensitivity requirements of general detection methods.

[0025] According to some embodiments of the first aspect of the present invention, the diameter of the Cambridge filter is 44 mm or 92 mm, which matches most commercially available smoking machines.

[0026] The embodiment of the second aspect of the present invention relates to a device for collecting cyclosiloxane in aerosol, comprising:

[0027] Aerosol generating devices;

[0028] A collector, connected to the aerosol generating device, wherein the collector is provided with a Cambridge filter;

[0029] An absorption device is communicated with the collector, and n-hexane is arranged in the absorption device.

[0030] The device for collecting cyclosiloxane in aerosol according to the second aspect of the present invention has at least the following beneficial effects:

[0031] By using the collecting device to sequentially pass the aerosol through a collector provided with a Cambridge filter and an absorption device provided with n-hexane, the cyclosiloxane in the aerosol can be effectively enriched, and then the cyclosiloxane content in the aerosol can be accurately tested by detecting the collection amount of the cyclosiloxane (the sum of the collection amounts of the Cambridge filter and n-hexane).

[0032] According to some embodiments of the second aspect of the present invention, the aerosol generating device is an electronic cigarette.

[0033] According to some embodiments of the second aspect of the present invention, the collecting device comprises a smoking machine and the aerosol generating device;

[0034] The smoking machine is provided with an interface adapted to the aerosol generating device, and the collector communicated with the interface; or, the smoking machine is provided with an interface adapted to the aerosol generating device, and the collector and the absorption device communicated with the interface in sequence.

[0035] Commercially available smoking machines generally come with a collector (which can be installed with a Cambridge filter). During the test, the electronic cigarette is installed on the interface of the smoking machine, and the electronic cigarette heats the atomized liquid in the cartridge to produce aerosol. The smoking machine is inhaled in a certain suction mode, so that the generated aerosol passes through the collector and is captured by the Cambridge filter to obtain an enriched filter.

[0036] By connecting an absorption device (such as an absorption bottle) filled with n-hexane to the air outlet of the smoking machine, secondary collection of cyclosiloxane in the aerosol can be achieved to obtain n-hexane absorption liquid.

[0037] In addition, some smoking machines are equipped with an absorption device trap (connected to the trap and capable of accommodating n-hexane). The aerosol can pass through the trap equipped with a Cambridge filter and the trap filled with n-hexane in the smoking machine in turn to collect cyclosiloxane.

[0038] Since the specific structure of the smoking machine is well known in the art, it will not be described in detail here.

[0039] The third aspect of the present invention relates to a method for detecting the content of cyclosiloxane in an aerosol, comprising the steps of:

[0040] The aerosol passes through the Cambridge filter and n-hexane in sequence to obtain the enrichment filter and n-hexane absorption liquid, respectively;

[0041] The enrichment filter disc is placed in the n-hexane absorption liquid for extraction to obtain a cyclosiloxane collection liquid;

[0042] The cyclosiloxane collected liquid is detected by gas chromatography-mass spectrometry.

[0043] The method for detecting the content of cyclosiloxane in aerosol according to the third aspect of the present invention has at least the following beneficial effects:

[0044] Collecting the aerosol through Cambridge filter and then n-hexane can effectively enrich the cyclosiloxane in the aerosol, realize the accurate detection of trace cyclosiloxane in the aerosol, and improve the detection accuracy.

[0045] It can be understood that in the detection method of this embodiment, the preparation details of the cyclosiloxane collection liquid can refer to the relevant contents of the implementation method of the above-mentioned collection method, and will not be repeated here.

[0046] According to some embodiments of the third aspect of the present invention, the chromatographic column of the gas chromatography is selected from HP-5MS, HP-5, DB-5, DB-5MS, OV-5, BP-5, SE-52, SE-54 or Rtx-5, all of which can achieve good detection effects.

[0047] The present invention does not particularly limit the specifications of the chromatographic column, and commercially available conventional sizes can be selected. For example, the length of the chromatographic column can be 25-35m, such as a column length of 30m; the inner diameter of the chromatographic column can be 300-320μm, such as a column inner diameter of 320μm.

[0048] According to some embodiments of the third aspect of the present invention, the carrier gas of the gas chromatography is helium, which can achieve better separation.

[0049] According to some embodiments of the third aspect of the present invention, the gas chromatograph is a non-split injection; or, the gas chromatograph is a split injection, wherein the split ratio is (10-50):1.

[0050] Choosing splitless injection or a relatively lower split ratio can better ensure the detection accuracy of trace cyclosiloxane content in aerosol. Compared with splitless injection, split injection is more conducive to improving peak shape, but when the split ratio is too high, the cyclosiloxane content entering the chromatographic column may be too low, which may affect the detection.

[0051] According to some embodiments of the third aspect of the present invention, the split ratio of the gas chromatography is (10-30):1.

[0052] According to some embodiments of the third aspect of the present invention, the split ratio of the gas chromatography is (10-20):1.

[0053] According to some embodiments of the first aspect of the present invention, the temperature rising conditions of the gas chromatography are: initial column temperature is 40-80°C, maximum column temperature is 250-300°C, and the temperature rising rate is 5-25°C / min.

[0054] The heating method can be gradient heating or uniform heating. Among them, gradient heating is more conducive to ensuring the separation degree, especially in the separation and detection of multiple components.

[0055] According to some embodiments of the first aspect of the present invention, the initial column temperature of the gas chromatograph is 40-60°C.

[0056] According to some embodiments of the first aspect of the present invention, the temperature rising conditions of the gas chromatography are:

[0057] The initial column temperature was 40-60°C and maintained for 0-5 min;

[0058] Raise the temperature to 150-220°C at a rate of 5-20°C / min and maintain for 0-5min;

[0059] Raise the temperature to 250-300°C at a rate of 10-25°C / min and maintain for 0-5min.

[0060] According to some embodiments of the third aspect of the present invention, the injection port temperature of the gas chromatograph is 200-280°C.

[0061] According to some embodiments of the first aspect of the present invention, the injection port temperature of the gas chromatograph is 220-250°C.

[0062] According to some embodiments of the third aspect of the present invention, the ion source of the mass spectrometer is an electron impact ionization source (EI).

[0063] According to some embodiments of the third aspect of the present invention, the interface temperature of the mass spectrometer is 250-280°C.

[0064] According to some embodiments of the third aspect of the present invention, the interface temperature of the mass spectrometer is 270-280°C.

[0065] It should be noted that the present invention has no special requirements on parameters such as the gas chromatography inlet temperature, carrier gas flow rate, sampling needle temperature (which may be 5-15°C higher than the equilibrium temperature), and mass spectrometry detection conditions, which can be reasonably determined based on actual experience and detection requirements.

[0066] During the detection process, in order to eliminate the influence of the solvent on the mass spectrometer, a solvent delay time is usually set, that is, after the gas chromatograph flows out for a period of time (mainly the solvent comes out at the beginning), the mass spectrometer is turned on to measure the mass spectrum. The solvent delay time can be controlled at about 2 minutes.

[0067] According to some embodiments of the third aspect of the present invention, the scanning mode of the mass spectrometer is an ion scanning mode (SIM).

[0068] According to some embodiments of the third aspect of the present invention, the mass spectrometer selects the SIM scanning mode, and the charge-to-mass ratios of the monitored ions are: 73, 147, 207, 221, 267, 271, 295, 341, 255, and 429, which can well meet the detection requirements for D4, D5, and D6.

[0069] According to some embodiments of the third aspect of the present invention, the quantitative analysis is performed using an external standard method.

[0070] It can be understood that the external standard method is to first prepare standard solutions of target compounds (test components, such as D4, D5, D6) of different concentrations, inject the standard solutions for testing, and draw a standard curve based on the corresponding relationship between the peak area (or peak height) and concentration of the target compound. Then, inject the sample to be tested under the same test conditions, and obtain the concentration of the target compound in the sample to be tested based on the peak area (or peak height) of the target compound in the sample to be tested and the corresponding standard curve.

[0071] Among them, in the standard solution, the solvent is selected as a good solvent that does not interfere with the peak of the target compound. In this article, the cyclosiloxane collection solution uses n-hexane as the solvent, so the standard solution also uses n-hexane as the solvent.

[0072] The implementation of the fourth aspect of the present invention relates to the application of the collection method or the collection device or the detection method in detecting the content of cyclosiloxane in electronic cigarette aerosol.

[0073] The collection method or collection device can effectively enrich the cyclosiloxane in the aerosol, and can be used to detect the cyclosiloxane content in the electronic cigarette aerosol, thereby improving the detection accuracy.

[0074] The use of gas chromatography-mass spectrometry for detection can efficiently and accurately detect cyclosiloxanes in aerosols, and can be used for precise testing of trace amounts of cyclosiloxanes in e-cigarette aerosols, filling the technical gap in the e-cigarette industry in detecting the content of cyclosiloxanes in aerosols.

[0075] The implementation of the fifth aspect of the present invention relates to the application of the collection method or the collection device or the detection method in the quality detection of electronic cigarettes.

[0076] The collection method or collection device can effectively enrich the cyclosiloxanes in the aerosol, facilitate the accurate detection of trace cyclosiloxanes in the aerosol, and can be used for the quality detection of electronic cigarettes to better ensure the safety of electronic cigarette products.

[0077] Herein, the term "trace amount" means a content not exceeding 1 mg / L.

[0078] Atomizer liquid refers to the electronic atomizer liquid used with an atomizer device, specifically, electronic cigarette atomizer liquid (commonly known as electronic cigarette oil or electronic cigarette liquid). The main ingredients of electronic cigarette oil on the market are: glycerin, 1,2-propylene glycol, nicotine, tobacco flavors, etc., and may also contain ethanol.

[0079] Electronic cigarette aerosol refers to the smoke formed by heating the electronic cigarette aerosol liquid. BRIEF DESCRIPTION OF THE DRAWINGS

[0080] Figure 1 is a schematic structural diagram of a collecting device according to an embodiment;

[0081] Among them, there are an aerosol generating device 100; a smoking machine 200, an interface 210, a collector 220, a Cambridge filter 221; an air outlet 230; and an absorption bottle 300.

[0082] Figure 2 It is the chromatogram of the mixed standard series solution in Example 1.

[0083] Figure 3 This is the standard curve of D4 in Example 1.

[0084] Figure 4 It is the standard curve of D5 in Example 1.

[0085] Figure 5 It is the standard curve of D6 in Example 1.

[0086] Figure 6It is the chromatogram of the test solution in Example 1.

[0087] Figure 7 It is the chromatogram of the blank solution in Example 1. DETAILED DESCRIPTION

[0088] In order to make the purpose, technical solution and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with the embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention.

[0089] Unless otherwise specified, all reagents used in this example were chromatographically pure and the weighing accuracy of the sample was 0.1 mg.

[0090] Electronic cigarettes (cartridge sealing plug: silicone material) and atomizing liquid (electronic cigarette oil) are both common types on the market.

[0091] 1. Related experimental equipment and materials

[0092] Gas chromatograph: Agilent 7890B; Chromatographic column: HP-5MS, column length 30m, column inner diameter 320μm;

[0093] Mass spectrometer: Agilent 5977B.

[0094] Smoking machine: British Cerulean CETI8.

[0095] Collection device: Figure 1 As shown, the smoking machine 200 is provided with an interface 210 for connecting the aerosol generating device 100 (i.e., the electronic cigarette of this embodiment), and a collector 220 and an air outlet 230 which are sequentially connected to the aerosol generating device 100. A Cambridge filter 221 with a diameter of 44 mm (with a loading capacity of 300 mg) is installed in the collector 220. An absorption bottle 300 (with a volume of 50 mL) filled with n-hexane is connected to the air outlet 230, and the volume of n-hexane is 20 mL.

[0096] 2. Solution Preparation

[0097] Stock solution: Accurately weigh 0.500g of D4, D5, and D6 standards respectively into a beaker, dilute with n-hexane, transfer to a 100mL volumetric flask, and make up to the mark with n-hexane to prepare 5.00mg / mL stock solutions.

[0098] Mixed standard intermediate solution: Take 1.00 mL of stock solution into 10 mL volumetric flasks respectively, make up to volume with n-hexane, and prepare a mixed standard intermediate solution with a single standard (D4 / D5 / D6) concentration of 500 mg / L.

[0099] Example 1

[0100] This embodiment provides a method for detecting the content of cyclosiloxane in an aerosol, which uses a gas chromatography-mass spectrometer for detection.

[0101] 1.1 Test conditions

[0102] Gas chromatography conditions: injection port temperature of 250°C; split ratio of 20:1; injection volume of 1 μL; programmed temperature: initial column temperature of 60°C, maintained for 2 min, then heated to 150°C at a rate of 10°C / min, maintained for 2 min, then heated to 300°C at a rate of 25°C / min, maintained for 2 min; carrier gas was helium at a flow rate of 3 mL / min.

[0103] Mass spectrometry conditions: interface temperature 280°C; ion source temperature 230°C; solvent delay 2 min; scan mode SIM was selected, and the monitored ions m / z were: 73, 147, 207, 221, 267, 271, 295, 341, 255, 429.

[0104] 1.2 Sample pretreatment

[0105] Use the collection device in Section 1 to collect the test solution and blank solution.

[0106] Liquid to be tested: The atomized liquid is placed in the cartridge of the electronic cigarette and placed at room temperature and pressure for 30 days. Then the electronic cigarette is connected to the interface 210 of the smoking machine 200, and the atomized liquid is heated by the electronic cigarette to generate an aerosol. The smoking machine 200 is operated in the set suction mode to collect the aerosol of the specified number of puffs, wherein the aerosol is successively captured by the Cambridge filter 221 in the collector 220 and the n-hexane in the absorption bottle 300 to obtain the enriched filter and the n-hexane absorption liquid. After the collection is completed, the n-hexane absorption liquid in the absorption bottle 300 is transferred to a 50mL centrifuge tube, and the inner wall of the absorption bottle 300 is washed three times with 2-4mL n-hexane, and the washed liquid is transferred to the centrifuge tube, and then the enriched filter is divided into four equal parts and placed in the centrifuge tube, and the extraction is oscillated for 30 minutes. After the extraction is completed, the liquid in the centrifuge tube is transferred to a 25ml volumetric flask, and the volume is fixed to 25mL with n-hexane to obtain the liquid to be tested.

[0107] Blank liquid: The interface 210 of the smoking machine 200 is not connected to the electronic cigarette, and the smoking machine 200 is operated in the set suction mode, so that the air passes through the trap 220 and the absorption bottle 300 in sequence through the interface 210. After the suction is completed, the n-hexane in the absorption bottle 300 is transferred to a 50mL centrifuge tube, and the inner wall of the gas outlet 230 is washed three times with 2-4mL n-hexane, and the washed liquid is transferred to the centrifuge tube, and then the enriched Cambridge filter 221 is cut into four uniform pieces and placed in the centrifuge tube, and the extraction is shaken for 30 minutes. After the extraction is completed, the liquid in the centrifuge tube is transferred to a 25ml volumetric flask, and the volume is fixed to 25mL with n-hexane to obtain a blank liquid.

[0108] Among them, the smoking mode of the smoking machine 200 is as follows: single-puff duration: (3.0±0.1) s, single-puff capacity: (55.0±0.6) mL, puff frequency: (30.0±0.5) s / puff, and the number of puffs is 100; when a certain number of puffs (for example, 20-30 puffs) are taken, the weight gain of the Cambridge filter is weighed and calculated. When the weight gain is close to the load capacity, the Cambridge filter needs to be replaced. In subsequent extractions, all Cambridge filters of the same sample are extracted.

[0109] 1.3 Standard curve drawing

[0110] 10 μL, 20 μL, 50 μL, 100 μL, and 200 μL of the mixed standard intermediate solution were respectively measured and placed in a 100 mL volumetric flask, and the volume was fixed with n-hexane to obtain a mixed standard series solution with single standard products (D4 / D5 / D6) of concentrations of 50 ng / mL, 100 ng / mL, 250 ng / L, 400 ng / L, and 500 ng / L, respectively. According to the set detection conditions, the mixed standard series solutions of different concentrations were sampled and analyzed in sequence to obtain the chromatogram of the mixed standard series solution, see Figure 2 ( Figure 2 The upper figure is in full ion scanning mode, and the lower figure is in SIM scanning mode). Plot a standard curve of peak area versus concentration of the target compound. The standard curves of D4, D5, and D6 are shown in Figure 1. Figure 3-Figure 5 It can be seen that D4, D5, and D6 have a good linear relationship in the range of 50.0ng / ml-500ng / ml, and the linear correlation coefficient is greater than 0.999.

[0111] 1.4 Determination of cyclosiloxane content in the test solution

[0112] The test solution was sampled and analyzed under the same detection conditions as the mixed standard series solution to obtain the chromatogram of the test solution. Figure 6 ( Figure 6 In the figure, the upper figure is the full ion scanning mode, and the lower figure is the SIM scanning mode). According to the peak area of ​​each target compound in the test solution and the corresponding standard curve, the concentration C1 of the corresponding target compound in the test solution is obtained.

[0113] The blank solution was injected and analyzed under the same detection conditions as the mixed standard series solution to obtain the blank solution chromatogram, see Figure 7 ( Figure 7In the figure, the upper figure is the full ion scan mode, and the lower figure is the SIM scan mode). It can be seen that the blank aerosol has no interference with the chromatographic peak of the target compound. According to the peak area of ​​each target compound in the blank solution and the corresponding standard curve, the concentration C0 of the corresponding target compound in the blank solution is obtained. By calculating the concentration C0 of the target compound in the blank solution, the influence of the pollution of related substances in the air on the test results can be excluded.

[0114] The content of cyclosiloxane in the aerosol is calculated according to the following formula:

[0115] X=(C-C0)*V / N / 1000

[0116] Where: X represents the content of cyclosiloxane in the aerosol, in μg / mouth;

[0117] C1, C0, both in μg / L;

[0118] V represents the volume of n-hexane, in mL;

[0119] N represents the number of puffs.

[0120] The test results are as follows: the contents of three cyclosiloxanes D4, D5 and D6 in the aerosol are 0.073 μg / mouth, 0.098 μg / mouth and 0.91 μg / mouth respectively.

[0121] Example 2

[0122] This embodiment provides a method for detecting the content of cyclosiloxane in an aerosol. Compared with Embodiment 1, the difference is that:

[0123] In Section 1.2, the number of puffs is 150.

[0124] The test results are as follows: the contents of three cyclosiloxanes D4, D5 and D6 in the aerosol are 0.074 μg / mouth, 0.099 μg / mouth and 0.93 μg / mouth respectively.

[0125] Example 3

[0126] This embodiment provides a method for detecting the content of cyclosiloxane in an aerosol. Compared with Embodiment 1, the difference is that:

[0127] In the test conditions in Section 1.1, the split ratio is 10:1.

[0128] The test results are as follows: the contents of three cyclosiloxanes D4, D5 and D6 in the aerosol are 0.072 μg / mouth, 0.096 μg / mouth and 0.92 μg / mouth respectively.

[0129] Comparative Example 1

[0130] This comparative example provides a method for detecting the content of cyclosiloxane in an aerosol. Compared with Example 1, the difference is that:

[0131] Replace hexane with an equal amount of methanol in all steps.

[0132] The test results are as follows: the contents of three cyclosiloxanes D4, D5 and D6 in the aerosol are 0.059 μg / mouth, 0.088 μg / mouth and 0.75 μg / mouth respectively.

[0133] Comparative Example 2

[0134] This comparative example provides a method for detecting the content of cyclosiloxane in an aerosol. Compared with Example 1, the difference is that:

[0135] The n-hexane in all steps was replaced with an equal amount of ethyl acetate.

[0136] The test results are as follows: the contents of three cyclosiloxanes D4, D5 and D6 in the aerosol are 0.055 μg / mouth, 0.085 μg / mouth and 0.72 μg / mouth respectively.

[0137] Comparative Example 3

[0138] This comparative example provides a method for detecting the content of cyclosiloxane in an aerosol. Compared with Example 1, the difference is that:

[0139] Replace n-hexane with an equal amount of dichloromethane in all steps.

[0140] The test results are as follows: the contents of three cyclosiloxanes D4, D5 and D6 in the aerosol are 0.066 μg / mouth, 0.083 μg / mouth and 0.85 μg / mouth respectively.

[0141] Comparative Example 4

[0142] This comparative example provides a method for detecting the content of cyclosiloxane in an aerosol. Compared with Example 1, the difference is that:

[0143] The n-hexane in all steps was replaced with an equal amount of methanol; and the Cambridge filter 221 was not installed in the trap 220. Accordingly, the sample pretreatment in Section 1.2 did not include the operation of trapping with the Cambridge filter 221 and extracting the enrichment filter.

[0144] The test results are as follows: the contents of three cyclosiloxanes D4, D5 and D6 in the aerosol are 0.048 μg / mouth, 0.083 μg / mouth and 0.65 μg / mouth respectively.

[0145] Comparative Example 5

[0146] This comparative example provides a method for detecting the content of cyclosiloxane in an aerosol. Compared with Example 1, the difference is that:

[0147] The Cambridge filter 221 is not installed in the trap 220. Accordingly, the sample pretreatment in Section 1.2 does not include the operations of trapping with the Cambridge filter 221 and extracting the enrichment filter.

[0148] The test results are as follows: the contents of three cyclosiloxanes D4, D5 and D6 in the aerosol are 0.053 μg / mouth, 0.088 μg / mouth and 0.76 μg / mouth respectively.

[0149] From the results of the above examples and comparative examples, it can be seen that the contents of D4, D5, and D6 in the aerosol measured with methanol, ethyl acetate or dichloromethane as the absorption liquid are significantly lower than those with n-hexane as the absorption liquid, indicating that the collection effects of solvents such as methanol, ethyl acetate or dichloromethane on cyclosiloxane are not as good as n-hexane, which will affect the detection accuracy. At the same time, filtering the aerosol through a Cambridge filter first and then absorbing it through n-hexane can effectively collect cyclosiloxane in the aerosol, further improving the detection accuracy.

Claims

1. A method for collecting cyclosiloxane in an aerosol, characterized in that: Includes steps: The aerosol was filtered through Cambridge filter disc and absorbed by n-hexane in turn to obtain enriched filter disc and n-hexane absorption liquid, respectively; The enrichment filter disc is placed in the n-hexane absorption liquid for extraction to obtain a cyclosiloxane collection liquid.

2. The method for collecting cyclosiloxane in aerosol according to claim 1, characterized in that: Oscillation is performed during the extraction process, and / or the extraction time is 10-60 min.

3. The method for collecting cyclosiloxane in aerosol according to claim 1, characterized in that: The aerosol is formed by heating an atomizing liquid, and the atomizing liquid is an electronic cigarette atomizing liquid.

4. The method for collecting cyclosiloxane in aerosol according to claim 3, characterized in that: The aerosol was filtered through a Cambridge filter disc and absorbed by n-hexane in sequence using a smoking machine to obtain an enriched filter disc and n-hexane absorption liquid, respectively.

5. The method for collecting cyclosiloxane in aerosol according to claim 4, characterized in that: The number of puffs of the smoking machine is 20-500, and / or the volume of the n-hexane is 20-50 ml.

6. A device for collecting cyclosiloxane in aerosol, characterized in that: include: Aerosol generating devices; A collector, connected to the aerosol generating device, wherein the collector is provided with a Cambridge filter; An absorption device is communicated with the collector, and n-hexane is arranged in the absorption device.

7. The collecting device according to claim 6, characterized in that: The collecting device comprises a smoking machine and the aerosol generating device; The smoking machine is provided with an interface adapted to the aerosol generating device, and the collector communicated with the interface; or, the smoking machine is provided with an interface adapted to the aerosol generating device, and the collector and the absorption device communicated with the interface in sequence.

8. A method for detecting the content of cyclosiloxane in an aerosol, characterized in that: Includes steps: Collecting the cyclosiloxane in the aerosol by the collection method according to any one of claims 1 to 5 to obtain a cyclosiloxane collection liquid; The cyclosiloxane collected liquid is detected by gas chromatography-mass spectrometry.

9. The method for detecting the content of cyclosiloxane in aerosol according to claim 8, characterized in that: The chromatographic column of the gas chromatography is selected from HP-5MS, HP-5, DB-5, DB-5MS, OV-5, BP-5, SE-52, SE-54 or Rtx-5.

10. The method for detecting the content of cyclosiloxane in aerosol according to claim 8, characterized in that: The carrier gas of the gas chromatography is helium.

11. The method for detecting the content of cyclosiloxane in aerosol according to claim 8, characterized in that: The split ratio of the gas chromatograph is (10-50):

1.

12. The method for detecting the content of cyclosiloxane in aerosol according to claim 8, characterized in that: The heating conditions of the gas chromatography are: The initial column temperature was 40-60°C and maintained for 0-5 min; Raise the temperature to 150-220°C at a rate of 5-20°C / min and maintain for 0-5min; Raise the temperature to 280-300°C at a rate of 10-25°C / min and maintain for 0-5min.

13. Use of the collection method according to any one of claims 1 to 5, or the collection device according to claim 6 or 7, or the detection method according to any one of claims 8 to 12 in detecting the content of cyclosiloxane in electronic cigarette aerosol or in the quality detection of electronic cigarettes.

Images