Method for analyzing and testing phenolic antioxidants in heated cigarette cores

Abstract

The invention relates to a method for analyzing and testing phenolic antioxidants in a heated cigarette core, and belongs to the technical field of tobacco analysis. The method for analyzing and testing the phenolic antioxidant in the heated cigarette core comprises the following steps: performing grinding extraction and solid-liquid separation on the heated cigarette core by adopting an internal standard substance solution to obtain a to-be-tested solution, and then performing gas chromatography-mass spectrometry analysis on the to-be-tested solution in a selected ion detection mode to obtain the phenolic antioxidant in the heated cigarette core. The ratio of the quantitative ion peak areas of the phenolic antioxidants and the internal standard substance in the to-be-detected liquid is obtained, and finally quantitative analysis is conducted on the phenolic antioxidants in the cigarette core through a standard curve method. When the analysis and test method is used for analyzing and testing 2, 6-di-tert-butyl p-methylphenol, 2, 4-di-tert-butyl phenol and 2, 2 '-methylene bis (4-methyl-6-tert-butyl phenol) in the heated cigarette core, the analysis and test method has the advantages of high sensitivity, stable and reliable detection result and simple operation, and can be used for mass detection of samples.

Description

Technical Field

[0001] The invention relates to an analytical testing method for phenolic antioxidants in heated cigarette cores, belonging to the technical field of tobacco analysis. Background Art

[0002] Heated cigarettes are also called low-temperature cigarettes. Instead of igniting tobacco with an open flame, they heat the tobacco core with an external heat source, causing the atomized medium, flavor components and added fragrance in the tobacco core to volatilize and produce smoke similar to that of traditional cigarettes. At present, there are two main preparation processes for heated cigarette tobacco cores: the thick slurry method and the roller pressing method. When preparing tobacco cores by the thick slurry method and the roller pressing method, the tobacco raw materials are mainly crushed into powder, and then a homogeneous reconstituted tobacco leaf product specially made for heated cigarettes is formed under the action of adhesives and fibers. Therefore, adhesives are the key raw materials for the thick slurry method and the roller pressing method, but a certain amount of antioxidants are usually added to these adhesives to increase the strength and toughness of the adhesives.

[0003] At present, domestic and foreign laws and regulations on food contact materials stipulate the permitted antioxidants and usage requirements, but there is no exact limit on the content of phenolic antioxidants in heated cigarette cores, which pose a safety hazard to smokers' health. Therefore, accurately determining the content of phenolic antioxidants in heated cigarette cores is of great significance for studying the atomization efficiency of heated cigarette additives and the impact of heated cigarettes on smokers' health.

[0004] When analyzing the composition of heated cigarette cores, it is usually necessary to grind the cores into powder before performing sample extraction analysis. Since heated cigarette cores contain a large amount of atomizers, the atomizers will adhere to the surface of the grinding equipment during the grinding process, which will cause sample contamination when grinding batch samples. In addition, the phenolic antioxidants commonly contained in heated cigarette cores are 2,6-di-tert-butyl-p-methylphenol, 2,4-di-tert-butylphenol and 2,2'-methylenebis(4-methyl-6-tert-butylphenol). The current existing technologies for detecting phenolic antioxidants in tobacco products use high performance liquid chromatography and liquid chromatography-mass spectrometry, which have problems such as poor reliability and low sensitivity of the detection results. Summary of the invention

[0005] The purpose of the present invention is to provide an analytical test method for phenolic antioxidants in heated cigarette cores, which can solve the problem of poor reliability of test results when currently testing phenolic antioxidants in tobacco products.

[0006] In order to achieve the above objectives, the technical scheme adopted by the analytical test method of the phenolic antioxidant in the heated cigarette core of the present invention is:

[0007] A method for analyzing and testing phenolic antioxidants in heated cigarette cores comprises the following steps: grinding and extracting the heated cigarette cores with an internal standard solution, separating the solid and the liquid to obtain a test liquid, then analyzing the test liquid with gas chromatography-mass spectrometry in a selected ion detection mode to obtain the ratio of the quantitative ion peak area of ​​the phenolic antioxidants in the test liquid and the internal standard, and finally quantitatively analyzing the phenolic antioxidants in the cores with a standard curve method; the gas chromatography uses a 35% phenylmethylpolysiloxane inert chromatographic column.

[0008] The analytical testing method for phenolic antioxidants in heated cigarette cores of the present invention grinds and extracts the heated cigarette cores, which can complete the synchronous operations of sample grinding and extraction in a short time and efficiently; gas chromatography-mass spectrometry analysis is performed on the test liquid in a selected ion detection mode, which can reduce reagent consumption and avoid environmental pollution; compared with the external standard method, the present invention adopts the internal standard method for quantification, eliminates the influence of operating conditions on the analysis results, and improves the accuracy and reliability of the measurement results. The analytical testing method for phenolic antioxidants in heated cigarette cores of the present invention is used for analyzing and testing 2,6-di-tert-butyl-p-methylphenol, 2,4-di-tert-butylphenol and 2,2'-methylenebis(4-methyl-6-tert-butylphenol) in heated cigarette cores, and has high sensitivity and spike recovery rate, and can realize simultaneous detection of 2,6-di-tert-butyl-p-methylphenol, 2,4-di-tert-butylphenol and 2,2'-methylenebis(4-methyl-6-tert-butylphenol) in heated cigarette cores, and the detection results are stable and reliable, with high precision and simple operation, and can be used for large-scale detection of samples.

[0009] Preferably, the phenolic antioxidant is selected from one, two or three of 2,6-di-tert-butyl-p-methylphenol, 2,4-di-tert-butylphenol and 2,2-methylenebis(4-methyl-6-tert-butylphenol).

[0010] Preferably, the method for quantitatively analyzing phenolic antioxidants in cigarette cores using the standard curve method is as follows:

[0011] S1, preparing standard solutions with different concentration gradients, the standard solutions consist of internal standard substances, phenolic antioxidants and solvents;

[0012] S2, performing gas chromatography-mass spectrometry analysis on each standard solution to obtain mass spectrum data of each standard solution, then determining the ratio of the quantitative ion peak area of ​​the phenolic antioxidant and the internal standard in each standard solution, and then performing linear fitting on the ratio of the concentration of the phenolic antioxidant and the internal standard in the standard solution and the ratio of the quantitative ion peak area of ​​the phenolic antioxidant and the internal standard in the mass spectrum data of the standard solution to obtain a standard curve equation;

[0013] S3, substituting the ratio into the standard curve equation to calculate the content of the phenolic antioxidant in the cigarette core.

[0014] Preferably, the internal standard in the internal standard solution and the standard solution is D8-acetophenone, the solvent in the internal standard solution and the standard solution is dichloromethane or methyl tert-butyl ether, and the concentration of the internal standard in the internal standard solution and the standard solution is 3-5 μg / mL.

[0015] Preferably, the chromatographic column for gas chromatography analysis 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 minutes, 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 minutes.

[0016] Preferably, the solvent delay time during mass spectrometry analysis is 7 to 9 minutes, the ion source temperature is 230 to 250° C., the transmission line temperature is 250 to 280° C., and the mass spectrometry analysis is performed in a simultaneous full scan and selected ion monitoring mode.

[0017] Preferably, the scanning range of the full scan is 35 amu to 350 amu.

[0018] Preferably, in the selected ion monitoring mode, two ions are selected for monitoring of the phenolic antioxidant and the internal standard respectively; 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 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.

[0019] Preferably, the grinding extraction is ball milling extraction. During ball milling extraction, 10 to 20 mL of the internal standard solution is used for every 0.8 g of heated cigarette core, and stainless steel grinding balls with a diameter of 12 mm are used during ball milling; when the mass of the heated cigarette core is less than 0.5 g, the amount of grinding balls added is 2, and when the mass of the heated cigarette core is 0.5 to 1.0 g, the amount of grinding balls added is 4.

[0020] Preferably, the rotation speed of ball mill extraction is 900-1500 rpm, and the time is 5-10 min. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1 It is the mass spectrum of the standard solution in the embodiment of the present invention. DETAILED DESCRIPTION

[0022] The analytical testing method for phenolic antioxidants in heated cigarette cores of the present invention is a pioneering invention. The analytical testing method for phenolic antioxidants in heated cigarette cores of the present invention extracts phenolic antioxidants from heated cigarette cores by grinding and extraction, and then performs gas chromatography-mass spectrometry analysis and utilizes a standard curve to achieve quantitative detection of phenolic antioxidants in the extracted test solution.

[0023] The technical solution of the present invention is further described below in conjunction with specific embodiments.

[0024] Example

[0025] The analytical test method for phenolic antioxidants in the heated cigarette core of this embodiment specifically comprises the following steps:

[0026] (1) Take 4 heated cigarettes, take out the core segments of the heated cigarettes, accurately weigh them (the weighing result is 0.8 g), and put them into a ball mill. Then, add 10 mL of extraction reagent into the ball mill (the extraction reagent consists of an internal standard substance and an organic solvent. The organic solvent is dichloromethane, the internal standard substance is D8-acetophenone, and the concentration of the internal standard substance in the extraction reagent is 3 μg / mL). Then, add 4 stainless steel grinding balls with a diameter of 12 mm into the ball mill. Then, place the ball mill in a ball mill for ball milling. The ball milling speed is 1500 rpm and the ball milling time is 10 min. After the ball milling is completed, transfer the centrifuge tube to a centrifuge for centrifugation for 5 min. The supernatant after centrifugation is the test solution.

[0027] (2) Prepare a series of standard solutions, which consist of dichloromethane, internal standard substances and phenolic antioxidants. The phenolic antioxidants are 2,6-di-tert-butyl-p-methylphenol, 2,4-di-tert-butylphenol and 2,2-methylenebis(4-methyl-6-tert-butylphenol). The internal standard substance is D8-acetophenone. The concentration of the internal standard substance in the series of standard solutions is 3 μg / mL. The concentration of 2,6-di-tert-butyl-p-methylphenol, 2,4-di-tert-butylphenol and 2,2-methylenebis(4-methyl-6-tert-butylphenol) in each series of standard solutions is 3 μg / mL. The concentrations of 2,6-di-tert-butyl-p-methylphenol, 2,4-di-tert-butylphenol and 2,2-methylenebis(4-methyl-6-tert-butylphenol) were the same, which were 0.2, 0.5, 1.0, 2.0, 5.0, 7.5 and 10.0 μg / mL respectively; each standard solution was then analyzed and detected by gas chromatography-mass spectrometry to obtain the mass spectrum peak spectra of each standard solution. The mass spectrum peak spectra of the standard solutions when the concentrations of 2,6-di-tert-butyl-p-methylphenol, 2,4-di-tert-butylphenol and 2,2-methylenebis(4-methyl-6-tert-butylphenol) were all 5.0 μg / mL were as follows: Figure 1 As shown, Figure 1Here, 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 (30m×0.25mm×1.0μm); the carrier gas was helium, and the carrier gas flow rate was 1.8mL / min; the injection port temperature was 280°C; the injection volume was 1μL, split injection, and the split ratio was 10:1; the temperature was increased using a programmed temperature rise mode, and the heating process was as follows: the initial temperature was maintained at 100°C for 3min, 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 10min, with a total operating time of 42.5min; the mass spectrum was detected using a mass spectrometer detector (MSD), and the solvent delay time was 7min; the ionization voltage was 70ev; the ion source The temperature was 230°C; the transfer line temperature was 280°C; the scanning mode was full scan and selected ion monitoring simultaneously. 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.

[0028] Then, according to the mass spectrometry peak spectrum, the ratio of the quantitative ion peak area of ​​the phenolic antioxidant to the quantitative ion peak area of ​​the internal standard, and the ratio of the concentration of the phenolic antioxidant to the concentration of the internal standard were subjected to linear regression analysis to obtain the standard curve equation (with the ratio of the quantitative ion peak area of ​​the antioxidant to the quantitative ion peak area of ​​the internal standard as the ordinate, and the ratio of the concentration of the antioxidant to the concentration of the internal standard as the abscissa). The standard curve equation of each phenolic antioxidant, the linear concentration range of the standard curve equation, and the standard deviation R of the standard curve equation 2 The detection limits and quantification limits of various phenolic antioxidants are shown in Table 1.

[0029] Table 1 Standard curve equations, linear concentration ranges, and R values ​​of the standard curve equations for each phenolic antioxidant 2 And the detection limit and quantification limit of each phenolic antioxidant

[0030]

[0031] It can be seen from Table 1 that within the linear concentration range, the standard curve equations of the three phenolic antioxidants have good linearity, and 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 μg / g, 0.01 μg / g and 0.02 μg / g, respectively.

[0032] (3) Add 1 mL of the test solution obtained in step (1) into a 2 mL chromatographic bottle, perform gas chromatography-mass spectrometry detection and analysis, and obtain a mass spectrum of the test solution. 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 (specifications: 30m×0.25mm×1.0μm); the carrier gas was helium, and the carrier gas flow rate was 1.8mL / min; the injection port temperature was 280°C; the injection volume was 1μL, 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 3min, the temperature was increased to 200°C at a rate of 4°C / min, and then the temperature was increased to 290°C at a rate of 20°C / min and maintained for 10min, with a total operating time of 42.5min; the mass spectrum was detected by a mass spectrometer detector (MSD), and the solvent delay time was 7min; the ionization voltage was 70ev; the ion The source temperature was 230°C; the transfer line temperature was 280°C; the scanning mode was full scan and selected ion monitoring simultaneously. 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.

[0033] Then, according to the mass spectrum of the test liquid, the ratio of the quantitative ion peak area of ​​the phenolic antioxidant and the internal standard in the mass spectrum is obtained, and then the obtained ratio is substituted into the standard curve equation in step (2) to calculate the ratio of the concentration of the phenolic antioxidant and the internal standard in the test liquid, and then according to the concentration of the internal standard in the test liquid, the concentration of the phenolic antioxidant in the test liquid is calculated, and then according to the volume of the test liquid and the concentration of the phenolic antioxidant, the content of the phenolic antioxidant in the core segment of the heated cigarette 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 core segments of the four heated cigarettes are 0.68, 7.41 and 1.95 μg / g, respectively.

[0034] In other embodiments, the dichloromethane in step (1) and step (2) is replaced with methyl tert-butyl ether; or the concentration of the internal standard in the extraction reagent is adjusted from 3 μg / mL to 5 μg / mL; or the volume of the extraction reagent is adjusted from 10 mL to 20 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 adjusted to 100 °C; the injection volume is adjusted to 2 μL; Maintain at 60℃ for 5min, increase the temperature to 160℃ at a rate of 2℃ / min, then increase the temperature to 260℃ at a rate of 15℃ / min and maintain for 20min; or adjust the solvent delay time during mass spectrometry analysis to 9min, the ion source temperature to 250℃, and the transmission line temperature to 250℃; or replace ultrasonic oscillation with mechanical stirring at a stirring rate of 150-200r / min and a time of 60-120min; or adjust the ball mill speed to 900 rpm and the ball mill time to 5min.

[0035] Experimental Example 1

[0036] The core segments of the heated cigarettes of the same brand and specification were selected to detect the content of the phenolic antioxidant in the core according to the method of the embodiment, and the intra-day precision of the analysis and testing method was investigated by parallel smoking and experiment 5 times a day, and the inter-day precision of the analysis and testing method was investigated by parallel smoking and experiment once a day for 5 consecutive days. The experimental results of intra-day precision are shown in Table 2, and the experimental results of inter-day precision are shown in Table 3.

[0037] Table 2 Experimental results of intra-day precision

[0038]

[0039] Table 3 Experimental results of inter-day precision

[0040]

[0041]

[0042] It can be seen from Table 2-3 that when the analytical test 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 the heated cigarette core, the intra-day precision is 6.4%, 4.6% and 5.2% respectively, and the inter-day precision is 7.7%, 5.8% and 6.5% respectively.

[0043] Experimental Example 2

[0044] On the basis of the precision experiment of the test results of the same heated cigarette sample, the recovery experiment was carried out by matrix addition. The recovery experiment method is as follows: take 6 commercially available heated cigarettes, then take out the core segments of each heated cigarette, add the same amount of high-concentration standard solution to the core segments of 2 heated cigarettes, add the same amount of medium-concentration standard solution to the core segments of 2 heated cigarettes, and add the same amount of low-concentration standard solution to the core segments of 2 heated cigarettes. After the high-concentration standard solution is added to the core segments, the content of antioxidants in the core segments is 3 times the content of antioxidants before the addition of the standard solution, after the medium-concentration standard solution is added to the core segments, the content of antioxidants in the core segments is 2 times the content of antioxidants before the addition of the standard solution, and after the low-concentration standard solution is added to the core segments, the content of antioxidants in the core segments is 1.5 times the content of antioxidants before the addition of the standard solution. Then, the antioxidant content of the cigarette core after adding the standard solution was tested according to the method of the embodiment, and the antioxidant content contained in the cigarette core before adding the standard solution was subtracted from the test result to obtain the test value of adding the antioxidant, and then the recovery rate was calculated using the test value and the actual value of adding the antioxidant. The results are shown in Table 4.

[0045] Table 4 Recovery of phenolic antioxidants in heated cigarette cores

[0046]

[0047] As can be seen from Table 4, when the method of the present invention is used to detect the antioxidant content in the heated cigarette core, 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 91.7% and 97.9%, 93.6% and 99.2%, and 92.8% and 96.3%, respectively.

[0048] Experimental Example 3

[0049] According to the determination method of the embodiment, three kinds of antioxidants were determined in the cigarette cores of 10 domestic heated cigarettes and 5 foreign brand heated cigarettes. The results showed that the three kinds of antioxidants were detected in all heated cigarettes, and the content range of the antioxidants is shown in Table 5.

[0050] Table 5 Antioxidant content range in different heated cigarettes

[0051] Antioxidants Content range (μg / g) 2,6-Di-tert-butyl-p-methylphenol 0.36～10.75 2,4-Di-tert-butylphenol 3.58～40.67 2,2-Methylenebis(4-methyl-6-tert-butylphenol) 0.37～31.41

[0052] As shown in Table 5, the three phenolic antioxidants were detected in the heated cigarette cores, among which 2,4-di-tert-butylphenol was detected in the heated cigarette cores at the highest level, ranging from 3.58 to 40.67 μg / g, and 2,6-di-tert-butyl-p-methylphenol was detected in a relatively small amount, ranging from 0.36 to 10.75 μg / g.

Claims

1. A method for analyzing and testing phenolic antioxidants in heated cigarette cores, characterized in that: The following steps are involved: The heated cigarette core is ground and extracted with an internal standard solution, and the solid-liquid separation is performed to obtain a test liquid, and then the test liquid is analyzed by gas chromatography-mass spectrometry in a selected ion detection mode to obtain the ratio of the quantitative ion peak area of ​​the phenolic antioxidant and the internal standard in the test liquid. Finally, the standard curve method is used to quantitatively analyze the phenolic antioxidant in the cigarette core; the gas chromatography uses a 35% phenylmethylpolysiloxane inert chromatographic column.

2. The method for analyzing and testing phenolic antioxidants in heated cigarette cores according to claim 1, characterized in that: The phenolic antioxidant is selected from one, two or three of 2,6-di-tert-butyl-p-methylphenol, 2,4-di-tert-butylphenol and 2,2-methylenebis(4-methyl-6-tert-butylphenol).

3. The method for analyzing and testing phenolic antioxidants in heated cigarette cores according to claim 1, characterized in that: The method for quantitative analysis of phenolic antioxidants in cigarette cores using the standard curve method is as follows: S1, preparing standard solutions with different concentration gradients, the standard solutions consist of internal standard substances, phenolic antioxidants and solvents; S2, performing gas chromatography-mass spectrometry analysis on each standard solution to obtain mass spectrum data of each standard solution, then determining the ratio of the quantitative ion peak area of ​​the phenolic antioxidant and the internal standard in each standard solution, and then performing linear fitting on the ratio of the concentration of the phenolic antioxidant and the internal standard in the standard solution and the ratio of the quantitative ion peak area of ​​the phenolic antioxidant and the internal standard in the mass spectrum data of the standard solution to obtain a standard curve equation; S3, substituting the ratio into the standard curve equation to calculate the content of the phenolic antioxidant in the cigarette core.

4. The method for analyzing and testing phenolic antioxidants in heated cigarette cores according to claim 3, characterized in that: The internal standard in the internal standard solution and the standard solution is D8-acetophenone, the solvent in the internal standard solution and the standard solution is dichloromethane or methyl tert-butyl ether, and the concentration of the internal standard in the internal standard solution and the standard solution is 3-5 μg / mL.

5. The method for analyzing and testing phenolic antioxidants in heated cigarette cores according to any one of claims 1 to 4, characterized in that: The chromatographic column used in gas chromatography analysis 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 as follows: 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.

6. The method for analyzing and testing phenolic antioxidants in heated cigarette cores 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, the transfer line temperature was 250 to 280°C, and the mass spectrometry analysis was performed in a simultaneous full scan and selected ion monitoring mode.

7. The method for analyzing and testing phenolic antioxidants in heated cigarette cores according to claim 6, characterized in that: The scanning range of the full scan is 35amu to 350amu.

8. The method for analyzing and testing phenolic antioxidants in heated cigarette cores according to any one of claims 1 to 4, characterized in that: In the selected ion monitoring mode, two ions were selected for monitoring for phenolic antioxidants and internal standards respectively; the antioxidants were 2,6-di-tert-butyl-p-methylphenol, 2,4-di-tert-butylphenol and 2,2-methylenebis(4-methyl-6-tert-butylphenol), the quantification ion of 2,6-di-tert-butyl-p-methylphenol was 205 and the qualifier ion was 220, the quantification ion of 2,4-di-tert-butylphenol was 206 and the qualifier ion was 191, the quantification ion of 2,2-methylenebis(4-methyl-6-tert-butylphenol) was 177 and the qualifier ion was 340; the internal standard was D8-acetophenone, the quantification ion of D8-acetophenone was 110 and the qualifier ion was 128.

9. The method for analyzing and testing phenolic antioxidants in heated cigarette cores according to any one of claims 1 to 4, characterized in that: The grinding extraction is ball milling extraction. During ball milling extraction, 10 to 20 mL of the internal standard solution is used for every 0.8 g of heated cigarette core, and a stainless steel grinding ball with a diameter of 12 mm is used for ball milling. When the mass of the heated cigarette core is less than 0.5 g, the amount of grinding balls added is 2, and when the mass of the heated cigarette core is 0.5 to 1.0 g, the amount of grinding balls added is 4.

10. The method for analyzing and testing phenolic antioxidants in heated cigarette cores according to claim 9, characterized in that: The rotation speed of ball mill extraction is 900-1500 rpm, and the time is 5-10 min.

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