Method for detecting antioxidant in heated cigarette aerosol

Abstract

The invention relates to a method for detecting an antioxidant in heated cigarette aerosol, and belongs to the technical field of tobacco analysis. The method for detecting the antioxidant in the aerosol of the heated cigarette comprises the following steps: S1, capturing the aerosol of the heated cigarette, and carrying out oscillation extraction on the captured aerosol by adopting an extraction solution to obtain a to-be-detected solution; the extracting solution consists of an extracting solvent and an internal standard substance; and S2, carrying out gas chromatography-mass spectrometry detection analysis on the to-be-detected liquid, determining the quantitative ion peak area ratio of the antioxidant to the internal standard substance in the mass spectrometry data of the to-be-detected liquid, and then calculating the content of the antioxidant in the aerosol based on a standard curve method. According to the method for detecting the antioxidants in the heated cigarette aerosol, the treatment process is simple, and the sensitivity and the precision are high when the antioxidants 2, 6-di-tert-butyl p-methylphenol, 2, 4-di-tert-butyl phenol and 2, 2-methylene bis (4-methyl-6-tert-butyl phenol) are detected.

Description

Technical Field

[0001] The invention relates to a method for detecting antioxidants in heated cigarette aerosols, belonging to the technical field of tobacco analysis. Background Art

[0002] Heated cigarettes are a new type of tobacco product that produces smoke through low-temperature distillation of tobacco core sheets under heating without burning conditions. The various components in heated cigarettes can be converted into aerosols after being atomized by heated cigarette smoking utensils, and enter the human body after being inhaled by smokers. During the preparation process of the reconstructed sheets of heated cigarettes, a certain proportion of adhesives will be added to increase the tensile strength of the sheets. A certain amount of antioxidants are usually added to these adhesives to increase the strength and toughness of the adhesive. At the same time, hot melt adhesive containing antioxidants is used in the molding process of the filter rods of heated cigarettes. Therefore, the aerosol released by the atomization of heated cigarettes contains a certain amount of antioxidants. Therefore, accurately determining the release amount of phenolic antioxidants in the aerosol of heated cigarettes is of great significance for studying the atomization efficiency of heated cigarette additives and the impact of heated cigarettes on the health of smokers.

[0003] The antioxidants commonly used in heated cigarettes are phenolic antioxidants, such as 2,6-di-tert-butyl-p-methylphenol, 2,4-di-tert-butylphenol and 2,2'-methylenebis(4-methyl-6-tert-butylphenol). At present, the analysis methods for 2,6-di-tert-butyl-p-methylphenol, 2,4-di-tert-butylphenol and 2,2'-methylenebis(4-methyl-6-tert-butylphenol) at home and abroad are mainly concentrated in the sample detection of food, chemical industry and other industries. The commonly used methods are mainly high performance liquid chromatography, colorimetry, ultraviolet spectrometry, gas chromatography and gas chromatography-mass spectrometry. Chinese patent documents CN104198605A and CN103115971A both use liquid chromatography to separate phenolic antioxidants in hot melt adhesives or tobacco flavors and fragrances. The liquid chromatography test relies on retention time to conduct qualitative analysis of the sample content. The detection steps are cumbersome, there is a possibility of false positives for complex sample matrices, the detection sensitivity is low, and the detection results have large errors. Summary of the invention

[0004] The object of the present invention is to provide a method for detecting antioxidants in heated cigarette aerosols, which can solve the problem of low sensitivity in the current detection of antioxidants in heated cigarette aerosols.

[0005] In order to achieve the above objectives, the technical solution adopted by the method for detecting antioxidants in heated cigarette aerosols of the present invention is:

[0006] A method for detecting antioxidants in heated cigarette aerosols comprises the following steps:

[0007] S1, using a filter to capture aerosol in heated cigarette smoke, and then using an extraction liquid to oscillate and extract the captured aerosol to obtain a test solution; the extraction solution is composed of an extraction solvent and an internal standard; the antioxidant is 2,6-di-tert-butyl-p-methylphenol, 2,4-di-tert-butylphenol and 2,2-methylenebis(4-methyl-6-tert-butylphenol);

[0008] S2, performing gas chromatography-mass spectrometry detection and analysis on the test liquid to determine the ratio of the quantitative ion peak areas of the antioxidant and the internal standard in the mass spectrum data of the test liquid, and then calculating the content of the antioxidant in the aerosol based on the standard curve method; the gas chromatography uses a 35% phenylmethylpolysiloxane inert chromatographic column, and the mass spectrometry analysis uses a selected ion monitoring mode.

[0009] The method for detecting antioxidants in heated cigarette aerosols of the present invention has the advantages of simple processing process, high sensitivity, good precision and high spike recovery rate when detecting antioxidants 2,6-di-tert-butyl-p-methylphenol, 2,4-di-tert-butylphenol and 2,2-methylenebis(4-methyl-6-tert-butylphenol). The method for detecting antioxidants in heated cigarette aerosols of the present invention adopts internal standard method for quantitative determination, which eliminates the influence of operating conditions on the analysis results compared with external standard method, improves the accuracy of the measurement results, is suitable for the analysis and detection of large batches of samples, and can realize the simultaneous determination of 2,6-di-tert-butyl-p-methylphenol, 2,4-di-tert-butylphenol and 2,2-methylenebis(4-methyl-6-tert-butylphenol) antioxidants in heated cigarette aerosols.

[0010] Preferably, the filter disc is a glass fiber filter disc.

[0011] Preferably, the extraction solvent is methyl tert-butyl ether or dichloromethane, the internal standard is D8-acetophenone, and the concentration of the internal standard in the extract is 3-5 μg / mL.

[0012] Preferably, in the selected ion monitoring mode, two ions are selected for monitoring of the antioxidant and the internal standard respectively; the quantitative ion of 2,6-di-tert-butyl-p-methylphenol is 205, the qualitative ion is 220, the quantitative ion of 2,4-di-tert-butylphenol is 206, the qualitative ion is 191, the quantitative ion of 2,2-methylenebis(4-methyl-6-tert-butylphenol) is 177, and the qualitative ion is 340; the internal standard is D8-acetophenone, the quantitative ion of D8-acetophenone is 110, and the qualitative ion is 128.

[0013] Preferably, the method for calculating the content of antioxidant in aerosol based on the standard curve method is as follows: providing a standard solution composed of an extraction solvent, an antioxidant and an internal standard, the standard solution having different concentration gradients; then performing gas chromatography-mass spectrometry detection and analysis on the standard solution to obtain mass spectrum data of the standard solution, and then performing linear fitting on the concentration ratio of the antioxidant and the internal standard in the standard solution and the ratio of the quantitative ion peak areas of the antioxidant and the internal standard in the mass spectrum data of the standard solution to obtain a concentration solution equation, and then bringing the quantitative ion peak area ratio of the antioxidant and the internal standard in the mass spectrum data of the test solution into the concentration solution equation to calculate the content of antioxidant in the aerosol; the concentration of the internal standard in the standard solution is 3 to 5 μg / mL.

[0014] Preferably, the conditions of gas chromatography are as follows: the chromatographic column is a VF-35MS capillary column, the carrier gas flow rate is 1.2-1.8 mL / min, the injection port temperature is 250-280°C, the injection volume is 1-2 μL, the split ratio is 10:1, and the heating process is: the initial temperature is 60-100°C and maintained for 3-5 min, then heated to 160-200°C at a rate of 2-4°C / min, and then heated to 260-290°C at a rate of 15-20°C / min and maintained for 10-20 min.

[0015] Preferably, the solvent delay time during mass spectrometry analysis is 7 to 9 minutes, the ion source temperature is 230 to 250°C, and the transmission line temperature is 250 to 280°C; the scanning mode is full scan and selected ion monitoring at the same time, and the scanning range of the full scan is 35amu to 350amu.

[0016] Preferably, the oscillation extraction is ultrasonic oscillation or mechanical oscillation.

[0017] Preferably, the ultrasonic frequency during ultrasonic oscillation is 40 to 60 kHz, and the time is 20 to 30 min; the stirring rate during mechanical oscillation is 150 to 200 r / min, and the time is 60 to 120 min. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 It is the mass spectrum of standard solution No. 3 in the embodiment of the present invention. DETAILED DESCRIPTION

[0019] The method for detecting antioxidants in heated cigarette aerosols of the present invention is a pioneering invention. The method for detecting antioxidants in heated cigarette aerosols of the present invention uses gas chromatography to replace conventional liquid chromatography, and by determining the quantitative ion peaks of antioxidants and internal standards and establishing a standard working curve, the content of antioxidants in heated cigarette aerosols can be accurately determined.

[0020] The technical solution of the present invention is further described below in conjunction with specific embodiments.

[0021] Example

[0022] The method for detecting antioxidants in heated cigarette aerosol of this embodiment specifically comprises the following steps:

[0023] (1) Smoking heated cigarettes

[0024] A linear smoking machine was used for smoking according to the smoking parameters of 55 mL per puff, 2 s per puff, and 30 s per puff frequency. Eight puffs were taken from each heated cigarette, and the total particulate matter of the heated cigarette aerosol was captured by a collector equipped with a glass fiber filter. Each glass fiber filter collected the aerosol released by 4 heated cigarettes. After the smoking was completed, the glass fiber filter capturing the heated cigarette aerosol was taken out from the collector.

[0025] (2) Obtain the test solution

[0026] Each glass fiber filter that captures the heated cigarette aerosol is placed in a 50mL centrifuge tube, and then 10mL of an extraction solution consisting of an extraction solvent and an internal standard is added (the extraction solvent in the extraction solution is methyl tert-butyl ether, the internal standard is D8-acetophenone, and the concentration of the internal standard in the extraction solution is 3μg / mL), and ultrasonic oscillation extraction is performed. The frequency of the ultrasonic oscillation extraction is 40kHz, and the time is 30min. After the ultrasonic oscillation extraction is completed, the centrifuge tube is allowed to stand for 10min, and the supernatant is the test solution.

[0027] (3) Determination of concentration solution equation

[0028] Methyl tert-butyl ether, internal standard D8-acetophenone, 2,6-di-tert-butyl-p-methylphenol, 2,4-di-tert-butylphenol and 2,2-methylenebis(4-methyl-6-tert-butylphenol) were fully stirred and mixed to prepare standard solutions containing different concentrations of antioxidants. The prepared standard solutions were named standard solution No. 1, standard solution No. 2, standard solution No. 3, standard solution No. 4, standard solution No. 5, standard solution No. 6 and standard solution No. 7, respectively; the concentration of the internal standard in standard solution No. 1 was 3 μg / mL, the concentration of 2,6-di-tert-butyl-p-methylphenol was 0.21 μg / mL, the concentration of 2,4-di-tert-butylphenol was 0.20 μg / mL, and the concentration of 2, The concentration of 2-methylenebis(4-methyl-6-tert-butylphenol) was 0.20 μg / mL; the concentration of the internal standard in standard solution No. 2 was 3 μg / mL, the concentration of 2,6-di-tert-butyl-p-methylphenol was 0.51 μg / mL, the concentration of 2,4-di-tert-butylphenol was 0.49 μg / mL, and the concentration of 2,2-methylenebis(4-methyl-6-tert-butylphenol) was 0.50 μg / mL; the concentration of the internal standard in standard solution No. 3 was 3 μg / mL, the concentration of 2,6-di-tert-butyl-p-methylphenol was 1.03 μg / mL, the concentration of 2,4-di-tert-butylphenol was 0.98 μg / mL, and the concentration of 2,2-methylenebis(4-methyl- The concentration of the internal standard in standard solution No. 4 was 3 μg / mL, the concentration of 2,6-di-tert-butyl-p-methylphenol was 2.05 μg / mL, the concentration of 2,4-di-tert-butylphenol was 1.96 μg / mL, and the concentration of 2,2-methylenebis(4-methyl-6-tert-butylphenol) was 2.00 μg / mL; the concentration of the internal standard in standard solution No. 5 was 3 μg / mL, the concentration of 2,6-di-tert-butyl-p-methylphenol was 5.13 μg / mL, the concentration of 2,4-di-tert-butylphenol was 4.90 μg / mL, and the concentration of 2,2-methylenebis(4-methyl-6-tert-butylphenol) was The concentration of the internal standard in standard solution No. 6 was 3 μg / mL, that of 2,6-di-tert-butyl-p-methylphenol was 7.18 μg / mL, that of 2,4-di-tert-butylphenol was 6.86 μg / mL, and that of 2,2-methylenebis(4-methyl-6-tert-butylphenol) was 7.00 μg / mL; the concentration of the internal standard in standard solution No. 7 was 3 μg / mL, that of 2,6-di-tert-butyl-p-methylphenol was 10.25 μg / mL, that of 2,4-di-tert-butylphenol was 9.80 μg / mL, and that of 2,2-methylenebis(4-methyl-6-tert-butylphenol) was 10.00 μg / mL.

[0029] Then, each standard solution was analyzed by gas chromatography-mass spectrometry to obtain the mass spectrum of each standard solution. The mass spectrum of standard solution No. 3 is as follows: Figure 1As shown, Figure 1 Here, 1 represents the internal standard D8-acetophenone, 2 represents the antioxidant 2,6-di-tert-butyl-p-methylphenol, 3 represents the antioxidant 2,4-di-tert-butylphenol, and 4 represents the antioxidant 2,2-methylenebis(4-methyl-6-tert-butylphenol). When gas chromatography-mass spectrometry was used for detection and analysis, gas chromatography was performed using a gas chromatograph (GC), and the chromatographic column used was a VF-35MS capillary column; the carrier gas was helium, and the carrier gas flow rate was 1.8 mL / min; the injection port temperature was 280°C; the injection volume was 1 μL, split injection, and the split ratio was 10:1; the temperature was increased in a programmed temperature rise mode, and the heating process was as follows: the initial temperature was maintained at 100°C for 3 minutes, then increased to 200°C at a rate of 4°C / min, and then increased to 290°C at a rate of 20°C / min and maintained for 10 minutes, with a total operating time of 42.5 minutes; the mass spectrum was detected by a mass spectrometer detector (MSD), and the solvent delay time was 7 minutes; the ionization voltage was 70 ev; the ion source temperature was 230°C; the transmission The transmission line temperature was 280°C; the scanning mode was full scan and selected ion monitoring at the same time. In the full scan monitoring mode, the scanning range was 35amu to 350amu; in the selected ion monitoring mode (SIM), the quantitative ion of 2,6-di-tert-butyl-p-methylphenol was 205, the qualitative ion was 220, and the retention time was 23.8min, the quantitative ion of 2,4-di-tert-butylphenol was 206, the qualitative ion was 191, and the retention time was 24.1min, the quantitative ion of 2,2-methylenebis(4-methyl-6-tert-butylphenol) was 177, the qualitative ion was 340, and the retention time was 37.3min, and the quantitative ion of D8-acetophenone was 110, the qualitative ion was 128, and the retention time was 11.4min.

[0030] Then, according to the mass spectrum obtained by the detection, the ratio of the quantitative ion peak area of ​​the target compound and the internal standard in the mass spectrum of each standard solution is calculated. The target compound refers to 2,6-di-tert-butyl-p-methylphenol, 2,4-di-tert-butylphenol or 2,2-methylenebis(4-methyl-6-tert-butylphenol), and then the ratio of the concentration of the target compound and the internal standard in each standard solution is calculated. Finally, the ratio of the quantitative ion peak area of ​​the target compound and the internal standard in the mass spectrum of the calculated standard solution and the ratio of the concentration of the target compound and the internal standard in the standard solution are used as the ordinate and the abscissa, respectively. The linear fitting equation is obtained, which is the concentration solution equation of the antioxidant. The linear fitting equation, concentration linear range, standard deviation of the linear fitting equation, detection limit and quantification limit of different target compounds are shown in Table 1.

[0031] Table 1 Linear fitting equations, standard deviations of linear fitting equations, detection limits and quantification limits of different target compounds

[0032]

[0033] As shown in Table 1, within the linear concentration range, the concentration equations of the three target compounds have good linearity. The detection limits of 2,6-di-tert-butyl-p-methylphenol, 2,4-di-tert-butylphenol and 2,2-methylenebis(4-methyl-6-tert-butylphenol) are 0.01, 0.02 and 0.03 μg / vial, respectively.

[0034] (4) Detection of antioxidants in the test solution

[0035] 1 mL of the test solution obtained in step (2) was added to a 2 mL chromatographic bottle, and a gas chromatography-mass spectrometry was performed to obtain a mass spectrum of the test solution. When the gas chromatography-mass spectrometry was performed, the gas chromatography was performed using a gas chromatograph (GC), and the chromatographic column used was a VF-35MS capillary column. The carrier gas was helium, and the carrier gas flow rate was 1.8 mL / min. The injection port temperature was 280°C. The injection volume was 1 μL, and the split injection was performed with a split ratio of 10:1. The temperature was raised in a programmed temperature rise mode, and the heating process was as follows: the initial temperature was maintained at 100°C for 3 min, the temperature was raised to 200°C at a rate of 4°C / min, and then the temperature was raised to 290°C at a rate of 20°C / min and then maintained for 10 min, with a total operating time of 42.5 min. The mass spectrum was detected using a mass spectrometer detector (MSD), and the solvent delay time was 7 min; ionization voltage was 70ev; ion source temperature was 230℃; transfer line temperature was 280℃; scanning mode was full scan and selected ion monitoring simultaneously, in full scan monitoring mode, the scanning range was 35amu~350amu; in selected ion monitoring mode (SIM), the quantitative ion of 2,6-di-tert-butyl-p-methylphenol was 205, the qualitative ion was 220, and the retention time was 23.8min, the quantitative ion of 2,4-di-tert-butylphenol was 206, the qualitative ion was 191, and the retention time was 24.1min, the quantitative ion of 2,2-methylenebis(4-methyl-6-tert-butylphenol) was 177, the qualitative ion was 340, and the retention time was 37.3min, and the quantitative ion of D8-acetophenone was 110, the qualitative ion was 128, and the retention time was 11.4min.

[0036] Then, according to the mass spectrum of the test liquid, the ratio of the quantitative ion peak area of ​​the antioxidant and the internal standard in the mass spectrum is obtained, and then the obtained ratio is substituted into the concentration solution equation in step (3) to calculate the ratio of the concentration of the antioxidant and the internal standard in the test liquid. Then, according to the concentration of the internal standard in the test liquid, the concentration of the antioxidant in the test liquid is calculated. Then, according to the volume of the test liquid and the concentration of the antioxidant, the content of the antioxidant in the captured heated cigarette aerosol is calculated. The contents of 2,6-di-tert-butyl-p-methylphenol, 2,4-di-tert-butylphenol and 2,2-methylenebis(4-methyl-6-tert-butylphenol) in the aerosol of the heated cigarette captured by each glass fiber filter are 0.57, 4.32 and 1.15 μg / cigarette, respectively.

[0037] In other embodiments, the methyl tert-butyl ether in step (2) and step (3) is replaced by dichloromethane; or the concentration of the internal standard in the extraction solution is adjusted from 3 μg / mL to 5 μg / mL; or the concentration of the internal standard in the standard solution is adjusted from 3 μg / mL to 5 μg / mL; or the carrier gas flow rate during gas chromatography analysis is adjusted to 1.2 mL / min, the injection port temperature is adjusted to 250°C, the injection volume is adjusted to 2 μL, and the heating process is adjusted to: the initial temperature is 60°C and maintained for 5 min, the temperature is increased to 160°C at a rate of 2°C / min, and then the temperature is increased to 260°C at a rate of 15°C / min and maintained for 20 min; or the solvent delay time during mass spectrometry analysis is adjusted to 9 min, the ion source temperature is adjusted to 250°C, and the transmission line temperature is adjusted to 250°C; or ultrasonic oscillation is replaced by mechanical stirring, the stirring rate is 150-200 r / min, and the time is 60-120 min.

[0038] Experimental Example 1

[0039] This experimental example is used to evaluate the stability of the detection method of the present invention. First, the same brand and specification of heated cigarettes are smoked using the same heated cigarette smoking device in a deep smoking mode, and the total particulate matter of the heated cigarette aerosol is captured using a glass fiber filter. Each glass fiber filter collects the aerosol of 4 heated cigarettes. After the puffing, the antioxidant content in the aerosol of the heated cigarette captured by the glass fiber filter is determined according to the method of the embodiment. Five parallel puffs and experiments are carried out in one day to examine the intra-day precision of the detection method, and one parallel puff and experiment is carried out every day for 5 consecutive days to examine the inter-day precision of the detection method. The experimental results of intra-day precision and inter-day precision are shown in Table 2 and Table 3.

[0040] Table 2 Experimental results of intra-day precision

[0041]

[0042] Table 3 Experimental results of inter-day precision

[0043]

[0044] It can be seen from Table 2-3 that when the detection method of the present invention is used to detect 2,6-di-tert-butyl-p-methylphenol, 2,4-di-tert-butylphenol and 2,2-methylenebis(4-methyl-6-tert-butylphenol) in heated cigarette aerosol, the intra-day precision is 5.7%, 4.8% and 5.3% respectively, and the inter-day precision is 7.4%, 6.2% and 6.3% respectively.

[0045] Experimental Example 2

[0046] In this experimental example, a recovery experiment was conducted by matrix spike addition. The same heated cigarette sample was puffed 11 times in parallel according to the puffing scheme, and glass fiber filters were collected. Five glass fiber filters were taken as sample matrices for analysis to determine the release of three antioxidants in the captured aerosols. Standard solutions with high, medium and low content levels were added to the other six glass fiber filters for spiked recovery experiments. Two parallel experiments were conducted at each concentration level. In this experimental example, the standard solutions are composed of methyl tert-butyl ether, internal standard D8-acetophenone and antioxidants. The antioxidants are 2,6-di-tert-butyl-p-methylphenol, 2,4-di-tert-butylphenol and 2,2-methylenebis(4-methyl-6-tert-butylphenol). The standard solutions are divided into three levels: high, medium and low according to the concentration of the antioxidants. After the high-level standard solution is added to the glass fiber filter, the content of the antioxidant is 3 times that before the addition of the standard solution. After the medium-level standard solution is added to the glass fiber filter, the content of the antioxidant is 2 times that before the addition of the standard solution. After the low-level standard solution is added to the glass fiber filter, the content of the antioxidant is 1.5 times that before the addition of the standard solution. The spiked recovery experiment is to determine the antioxidant content of the glass fiber filter after adding the standard solution according to the method of the embodiment, and then subtract the antioxidant content in the glass fiber filter before adding the standard solution from the measured value to obtain the test value, and then use the test value and the antioxidant content added to the glass fiber filter to calculate the recovery rate. The results are shown in Table 4.

[0047] Table 4 Recovery rate experimental results

[0048]

[0049] As can be seen from Table 4, when the detection method of the present invention is used to detect the antioxidant content in the heated cigarette aerosol, the spiked recoveries of 2,6-di-tert-butyl-p-methylphenol, 2,4-di-tert-butylphenol and 2,2-methylenebis(4-methyl-6-tert-butylphenol) are between 93.6% and 97.9%, 95.5% and 98.4%, and 95.1% and 99.3%, respectively.

[0050] Experimental Example 3

[0051] Ten domestic heated cigarettes and five foreign brand heated cigarettes were selected respectively, and then the contents of three antioxidants in the aerosol of the heated cigarettes were detected according to the detection method of the embodiment. The results showed that 2,6-di-tert-butyl-p-methylphenol, 2,4-di-tert-butylphenol and 2,2-methylenebis(4-methyl-6-tert-butylphenol) were detected in the aerosol released by the selected heated cigarettes. The release ranges of the three antioxidants are shown in Table 5.

[0052] Table 5 Release range of antioxidants in different heated cigarettes

[0053] Antioxidants Release range (μg / vial) 2,6-Di-tert-butyl-p-methylphenol 0.14～0.57 2,4-Di-tert-butylphenol 1.63～10.49 2,2-Methylenebis(4-methyl-6-tert-butylphenol) 0.90～16.70

[0054] As shown in Table 5, the three phenolic antioxidants were detected in the aerosol of heated cigarette smoke. Among them, the detection amount of 2,4-di-tert-butylphenol in the aerosol was the largest, ranging from 1.63 to 10.49 μg / cigarette, and the detection amount of 2,6-di-tert-butyl-p-methylphenol was relatively small, ranging from 0.14 to 0.57 μg / cigarette.

Claims

1. A method for detecting antioxidants in heated cigarette aerosol, characterized in that: The following steps are involved: S1, using a filter to capture aerosol in heated cigarette smoke, and then using an extraction liquid to oscillate and extract the captured aerosol to obtain a test solution; the extraction solution is composed of an extraction solvent and an internal standard; the antioxidant is 2,6-di-tert-butyl-p-methylphenol, 2,4-di-tert-butylphenol and 2,2-methylenebis(4-methyl-6-tert-butylphenol); S2, performing gas chromatography-mass spectrometry detection and analysis on the test liquid to determine the ratio of the quantitative ion peak areas of the antioxidant and the internal standard in the mass spectrum data of the test liquid, and then calculating the content of the antioxidant in the aerosol based on the standard curve method; the gas chromatography uses a 35% phenylmethylpolysiloxane inert chromatographic column, and the mass spectrometry analysis uses a selected ion monitoring mode.

2. The method for detecting antioxidants in heated cigarette aerosol according to claim 1, characterized in that: The filter disc is a glass fiber filter disc.

3. The method for detecting antioxidants in heated cigarette aerosol according to claim 1, characterized in that: The extraction solvent is methyl tert-butyl ether or dichloromethane, the internal standard is D8-acetophenone, and the concentration of the internal standard in the extract is 3-5 μg / mL.

4. The method for detecting antioxidants in heated cigarette aerosol according to claim 1, characterized in that: In the selected ion monitoring mode, two ions were selected for monitoring of antioxidants and internal standards respectively; the quantitative ion of 2,6-di-tert-butyl-p-methylphenol was 205 and the qualitative ion was 220, the quantitative ion of 2,4-di-tert-butylphenol was 206 and the qualitative ion was 191, the quantitative ion of 2,2-methylenebis(4-methyl-6-tert-butylphenol) was 177 and the qualitative ion was 340; the internal standard was D8-acetophenone, the quantitative ion of D8-acetophenone was 110 and the qualitative ion was 128.

5. The method for detecting antioxidants in heated cigarette aerosol according to any one of claims 1 to 4, characterized in that: The method for calculating the content of antioxidants in aerosols based on the standard curve method is as follows: providing a standard solution composed of an extraction solvent, an antioxidant and an internal standard, wherein the standard solution has different concentration gradients; then performing gas chromatography-mass spectrometry detection and analysis on the standard solution to obtain mass spectrum data of the standard solution, then performing linear fitting on the concentration ratio of the antioxidant and the internal standard in the standard solution and the ratio of the quantitative ion peak areas of the antioxidant and the internal standard in the mass spectrum data of the standard solution to obtain a concentration solution equation, then substituting the ratio of the quantitative ion peak areas of the antioxidant and the internal standard in the mass spectrum data of the test solution into the concentration solution equation to calculate the content of the antioxidant in the aerosol; the concentration of the internal standard in the standard solution is 3 to 5 μg / mL.

6. The method for detecting antioxidants in heated cigarette aerosol according to any one of claims 1 to 4, characterized in that: The gas chromatography conditions are as follows: the chromatographic column is a VF-35MS capillary column, the carrier gas flow rate is 1.2-1.8 mL / min, the injection port temperature is 250-280 °C, the injection volume is 1-2 μL, the split ratio is 10:1, and the heating process is: the initial temperature is 60-100 °C and maintained for 3-5 min, then the temperature is increased to 160-200 °C at a rate of 2-4 °C / min, and then the temperature is increased to 260-290 °C at a rate of 15-20 °C / min and maintained for 10-20 min.

7. The method for detecting antioxidants in heated cigarette aerosol according to any one of claims 1 to 4, characterized in that: The solvent delay time during mass spectrometry analysis was 7 to 9 minutes, the ion source temperature was 230 to 250°C, and the transfer line temperature was 250 to 280°C; the scanning mode was full scan and selected ion monitoring at the same time, and the scanning range of the full scan was 35 amu to 350 amu.

8. The method for detecting antioxidants in heated cigarette aerosol according to any one of claims 1 to 4, characterized in that: Oscillation extraction is ultrasonic oscillation or mechanical oscillation.

9. The method for detecting antioxidants in heated cigarette aerosol according to claim 8, characterized in that: The ultrasonic frequency during ultrasonic oscillation is 40-60kHz, and the time is 20-30min; the stirring rate during mechanical oscillation is 150-200r / min, and the time is 60-120min.

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