Sample pretreatment method and GC-MS (Gas Chromatography-Mass Spectrometer) method for simply and rapidly detecting glycidol and monochloropropanol in heated cigarette aerosol

Through the method of ethyl acetate extraction and BSTFA derivatization, the sample pretreatment process of glycidol and monochloropropanol in heating cigarette aerosol is simplified, and the problem of poor detection accuracy in the prior art is solved, and rapid and accurate quantity analysis is achieved.

CN120177683APending Publication Date: 2025-06-20ZHENGZHOU TOBACCO RES INST OF CNTC
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Patent Information

Application Number
CN202510278071.6
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-03-10
Publication Date
2025-06-20

AI Technical Summary

Technical Problem

The existing detection methods are complex in the sample pretreatment process and poor detection accuracy when detecting glycidol and monochloropropanol in heated cigarette aerosols.

Method used

Ethyl acetate was used to extract the particulate phases in the aerosol of the cigarette and perform derivatization reaction through N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA), simplifying the sample pretreatment steps and improving the analytical sensitivity of the target.

Benefits of technology

The rapid and accurate quantity analysis of glycidol and monochloropropanol in the heated cigarette aerosol is achieved, simplifying the sample pretreatment steps and improving the sensitivity and accuracy of the detection.

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Abstract

The invention belongs to the technical field of chemical detection, and particularly relates to a sample pretreatment method and a GC-MS (Gas Chromatography-Mass Spectrometer) method for simply and rapidly detecting glycidol and monochloropropanol in heated cigarette aerosol. The invention provides a sample pretreatment method for simply and rapidly detecting glycidol and monochloropropanol in heated cigarette aerosol. The sample pretreatment method comprises the following steps: capturing particulate matters in the heated cigarette aerosol; mixing the trapping material trapping the particulate matters with ethyl acetate and an internal standard substance, extracting to obtain an extracting solution, and diluting with ethyl acetate; n, O-bis (trimethylsilyl) trifluoroacetamide is added for a derivatization reaction, and a solution to be detected is obtained. According to the present invention, the ethyl acetate is adopted to extract the sample, and the analysis can be performed through the simple dilution and BSTFA derivation, such that the sample pretreatment step is simplified, the volatility and the stability of the glycidyl, the 3-MCPD and the 2-MCPD are increased, and the analysis sensitivity of the target object is improved;
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Description

Technical Field

[0001] The present invention relates to the technical field of chemical detection, and particularly relates to a sample pretreatment method and a GC-MS method for simply and rapidly detecting glycidol and monochloropropanols in heated roll-aerosol. Background Art

[0002] Heat-not-burn (HNB) tobacco cigarettes are an important part of new tobacco products. Due to the smoke release mechanism of only heating (below 400 °C) rather than burning and the special chemical substance basis different from traditional cigarettes (the heated cigarette core contains a large amount of propylene glycol, glycerol, additives, etc.), the aerosol components are not the same as those of traditional cigarette smoke in terms of the number and content of compounds. Comparative analysis and research results of heated aerosol and traditional cigarette smoke show that heated aerosol contains glycidol and chloropropanols, which are derived from the pyrolysis of glycerol and glycerol esters.

[0003] Glycidol, also known as glycidol, has genotoxicity and can affect the kidneys, reproductive system and genetic material. It has a significant impact on gene mutations and unconventional DNA synthesis and is classified by the IARC as a Group 2A (probably carcinogenic to human) carcinogen. Chloropropanol is a chloride of glycerol formed by the nucleophilic substitution of one or two chlorine atoms with the hydroxyl groups of the glycerol molecule, including two monochlorosubstituted compounds, monochloropropanol (MCPD): 3-chloro-1,2-propanediol (3-MCPD) and 2-chloro-1,3-propanediol (2-MCPD); and two dichlorosubstituted compounds (DCP): 1,3-dichloro-2-propanol (1,3-DCP) and 2,3-dichloro-1-propanol (2,3-DCP). In the actual food processing process, although 1,3-DCP and 2,3-DCP are highly toxic, their detection rates in food are extremely low. The production amount of MCPD is usually 100-10,000 times that of DCP, and the highest content among many MCPDs is 3-MCPD. 3-MCPD has attracted much attention due to its strong toxicity, large amount of pollution and wide range, and has mutagenicity and carcinogenic risks. It is classified by the IARC as a Group 2B (possible human carcinogens) carcinogen. The Joint FAO / WHO Expert Committee on Food Additives (JECFA) has set the tolerable daily intake (TDI) of 3-MCPD at 4 μg / kg bw / d. The "GB 2762-2017" promulgated by the state stipulates that it is 0.4 mg / kg in liquid seasonings. In 2018, the European Food Safety Authority (EFSA) further increased the limit standard and recommended its TDI to be 2 μg / kg bw / d.

[0004] At present, the analysis and research of glycidol and monochloropropanol are mainly concentrated in the fields of food, medicine and condiments. Since food matrices are usually complex, sample pretreatment (purification and enrichment, etc.) is required before testing food matrices. Glycidol (GLD) and 3-MCPD have no chromophores and are high-polarity, high-boiling-point, low-molecular-weight compounds. The key steps of analysis are the extraction of the target and subsequent derivatization. Sample pretreatment generally uses extraction columns, concentration to dryness and redissolution, and then derivatization. Derivatization generally uses phenylboronic acid (PBA) or heptafluorobutyrylimidazole (HFBI) to derivatize MCPD and then perform GC-MS analysis. For the simultaneous testing and analysis of glycidol and monochloropropanol, the double sample difference subtraction method is generally used. Specifically, two samples of the same amount are taken, one sample is hydrolyzed and ring-opened, the glycidol therein is ring-opened, and the total amount of chloropropanol is analyzed after conversion to chloropropanol. The other sample is not hydrolyzed, and the chloropropanol therein is analyzed. Then, the measured amount of chloropropanol in the two samples is subtracted. At this time, the amount of chloropropanol obtained is the amount obtained by converting the glycidol in the sample, and the conversion can be performed. The pre-processing of the analytical method is complicated, time-consuming and labor-intensive, and the double sample difference subtraction method leads to poor detection accuracy when simultaneously detecting GLD and MCPD.

[0005] The Chinese patent application with application publication number CN118225931A, which was applied for and published on June 21, 2024, discloses a method for detecting the content of chloropropanol in electronic cigarette aerosol. The particle phase of the mainstream smoke generated after the electronic cigarette sample is inhaled is captured by a filter disc, and the filter disc is extracted with an extraction liquid (sodium chloride aqueous solution) and then passed through a solid phase extraction column. After water rinsing, it is eluted with ethyl acetate to obtain an eluent, which is blown dry with nitrogen and re-dissolved with ethyl acetate. A silanization derivatization reagent (N,O-bis(trimethylsilyl)trifluoroacetamide, BSTFA) is added for derivatization reaction, and after filtering, it is measured and analyzed by gas chromatography-tandem mass spectrometry. The patent provides a qualitative and quantitative analysis method for the content of chloropropanol in electronic cigarette aerosol by silanization derivatization GC-MS. The interference of propylene glycol and glycerol in the electronic cigarette aerosol sample can be reduced by purification with a solid phase extraction column, so that the derivatization agent can completely derive the chloropropanol, thereby improving the selectivity and accuracy of the detection.

[0006] However, the above detection method detects compounds such as chloropropanol (1,3-DCP, 3-MCPD) in e-cigarette aerosol, and cannot detect monochloropropanol and glycidol at the same time. In addition, the sample pretreatment method used is still extraction column purification, concentration to dryness and re-dissolution, and derivatization, and the pretreatment method is relatively complicated. Summary of the invention

[0007] The object of the present invention is to provide a sample pretreatment method for simply and rapidly detecting glycidol and monochloropropanols in heated tobacco aerosol, so as to solve the problem of complex sample pretreatment process in existing detection methods.

[0008] The second object of the present invention is to provide a GC-MS method for simply and rapidly detecting glycidol and monochloropropanols in heated tobacco aerosol, so as to solve the problems of complex detection method and poor accuracy existing in existing detection methods.

[0009] In order to solve the above technical problems, the technical solution of the sample pretreatment method for simply and rapidly detecting glycidol and monochloropropanols in heated tobacco aerosol of the present invention is as follows:

[0010] A sample pretreatment method for simply and rapidly detecting glycidol and monochloropropanols in heated tobacco aerosol comprises the following steps:

[0011] (1) Trapping the particulate matter in the heated tobacco aerosol;

[0012] (2) Mixing the trapping material trapped with the particulate matter with ethyl acetate and an internal standard for extraction to obtain an extract, and diluting with ethyl acetate;

[0013] (3) Adding N,O-bis(trimethylsilyl)trifluoroacetamide to the diluted extract obtained in step (2) for derivatization reaction to obtain a test solution.

[0014] The present invention pioneerly provides a sample pretreatment method for simply and rapidly detecting glycidol and monochloropropanols in heated tobacco aerosol. By using N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) to derivatize glycidol, 3-MCPD, 2-MCPD and their internal standards, the mass spectrometry characteristics and chromatographic retention indices of glycidol, 3-MCPD, 2-MCPD and the corresponding internal standards can be confirmed, providing a new way for the identification of glycidol, and increasing the volatility and stability of glycidol, 3-MCPD and 2-MCPD, improving the analysis sensitivity of the target substances, which is beneficial to realizing the rapid and accurate quantitative analysis of glycidol and chloropropanols in heated tobacco aerosol; Using ethyl acetate to extract the sample, and it can be analyzed after simple dilution and derivatization, without the need for sample pretreatment steps such as purification with a diatomaceous earth column and concentration and reconstitution, and the method is simple.

[0015] In order to further improve the derivatization efficiency, preferably, pyridine is added during the derivatization reaction, and the volume ratio of pyridine to N,O-bis(trimethylsilyl)trifluoroacetamide is (1-1.2):1. Adding the catalytic reagent pyridine during the derivatization process can enable the derivatives of 3-MCPD and 2-MCPD to be rapidly and completely dimethylsilylated, and can realize the accurate quantitative analysis of 3-MCPD and 2-MCPD.

[0016] In order to further completely extract the target object in the capture material, preferably, the capture is to use a filter to capture the particulate matter in the aerosol of the heated cigarette, and the mixing is to mix the filter that captures the particulate matter in the aerosol when every 3 to 5 heated cigarettes are smoked with 125 to 150 μL of internal standard solution and 10 to 15 mL of ethyl acetate.

[0017] In order to further improve the detection accuracy, preferably, the internal standard solution includes D5-glycidol, D5-2-MCPD and D5-3-MCPD, the concentrations of D5-glycidol and D5-2-MCPD are both 250-300 ng / mL, and the concentration of D5-3-MCPD is 500-550 ng / mL.

[0018] In order to further improve the extraction efficiency, preferably, the extraction is carried out at room temperature under ultrasonic conditions for 5 to 10 minutes, and the power of the ultrasound is 40 to 50W.

[0019] In order to further improve the derivatization efficiency, preferably, the temperature of the derivatization reaction is 70-80° C., and the time of the derivatization reaction is 5-8 min.

[0020] In order to further completely derivatize the target compound in the extract, preferably, ethyl acetate is added to every 200 μL of the extract to make the volume 1-2 mL to obtain a diluted extract, and 50-80 μL of N,O-bis(trimethylsilyl)trifluoroacetamide is added to every 1-2 mL of the diluted extract.

[0021] The technical scheme of the GC-MS method for simply and quickly detecting glycidol and monochloropropanol in heated cigarette aerosol of the present invention is:

[0022] A GC-MS method for simply and quickly detecting glycidol and monochloropropanol in heated cigarette aerosols is disclosed. The sample pretreatment method is used to obtain a test solution, and GC-MS detection and analysis are performed.

[0023] The detection method provided by the present invention adopts the sample pretreatment steps described above. Without the need for extraction column purification and concentration reconstitution, the pretreatment method is simple and efficient. N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) is used to derivatize glycidol, 3-MCPD, 2-MCPD and their internal standards, which increases the volatility and stability of glycidol, 3-MCPD and 2-MCPD, improves the analysis sensitivity of the target substances. Combined with gas chromatography-mass spectrometry (GC-MS), a simple and rapid analysis method for glycidol in heated aerosol is established. Glycidol, 3-MCPD and 2-MCPD are all present in the particulate phase, and rapid and accurate quantitative analysis of glycidol and chloropropanol in heated aerosol can be achieved. The detection method of the present invention has good sensitivity and accuracy. In the linear concentration range, the linear relationships of each standard curve are good, and the correlation coefficient r 2 is 0.9969 - 0.9995. The detection limits of glycidol, 3-MCPD and 2-MCPD are 1 - 20 ng / mL, and the quantification limits are 3 - 70 ng / mL, which fully meet the quantitative analysis requirements of glycidol and monochloropropanol in heated cigarette aerosol. This method has high sensitivity, is simple, accurate and easy to operate, providing technical support for the safety research of heated cigarettes.

[0024] To further improve the separation effect of the target substances, preferably, the chromatographic conditions for GC-MS detection and analysis are as follows: chromatographic column: elastic quartz capillary chromatographic column, the stationary phase is 5% phenyl-methyl polysiloxane; inlet temperature: 280 - 290 °C; injection volume: 1.0 - 2.0 μL; injection mode: split injection, split ratio: 10:1; carrier gas: helium, constant flow mode, flow rate 1.0 - 2.0 mL / min; programmed temperature rise: initial temperature 40 - 50 °C, then rising to 80 - 90 °C at a heating rate of 10 - 15 °C / min, holding for 2 - 3 min, and then rising to 280 - 290 °C at a heating rate of 40 - 50 °C / min, holding for 10 - 12 min.

[0025] To further improve the detection accuracy, preferably, the mass spectrometry conditions for GC-MS detection and analysis are as follows: ionization mode: electron impact ionization, ionization energy 70 eV; ion source temperature: 290 - 300 °C; transfer line temperature: 290 - 300 °C; mass spectrometry scanning mode: selected ion monitoring SIM mode. By optimizing the chromatographic conditions and mass spectrometry conditions, the baseline separation of glycidol, 3-MCPD and 2-MCPD in the smoke of heated cigarettes is ensured, the corresponding quantitative ions and qualitative ions are selected, and the qualitative analysis of the compounds is more accurate. Standard working curves are established for glycidol, 3-MCPD and 2-MCPD by the internal standard method, and the contents of the corresponding components are calculated according to the areas of each target substance and the standard curves of each target substance. The method has higher sensitivity, better precision and repeatability. Description of the Drawings

[0026] Figure 1 Selective ion chromatograms of glycidol standard (200 ng / mL) and glycidol in a typical heated tobacco product sample (Sample 5);

[0027] Figure 2 Selective ion chromatograms of D5-glycidol standard (250 ng / mL) and D5-glycidol in a typical heated tobacco product sample (Sample 5);

[0028] Figure 3 Selective ion chromatograms of 3-MCPD (200 ng / mL), 2-MCPD (200 ng / mL) standards and 3-MCPD, 2-MCPD in a typical heated tobacco product sample (Sample 5);

[0029] Figure 4 Selective ion chromatograms of D5-3-MCPD (500 ng / mL), D5-2-MCPD (250 ng / mL) standards and D5-3-MCPD, D5-2-MCPD in a typical heated tobacco product sample (Sample 5). Detailed implementation mode

[0030] The technical concept of the sample pretreatment method for the simple and rapid detection of glycidol and monochloropropanols in heated tobacco aerosol of the present invention is as follows:

[0031] At present, the simultaneous detection of glycidol and monochloropropanols mainly focuses on the fields of food, medicine and condiments. However, complex pretreatment steps such as extraction column extraction, concentration to dryness and reconstitution, and derivatization are required during detection, and the dual-sample subtraction method needs to be used for quantification, resulting in cumbersome and complex pretreatment steps and low detection accuracy. For the detection of mainstream smoke of tobacco samples, the current focus is only on the separate detection of chloropropanols, and still requires complex pretreatment processes such as extraction column extraction, concentration to dryness and reconstitution, and BSTFA derivatization.

[0032] The present invention simultaneously detects glycidol, 3-MCPD, and 2-MCPD in the aerosol generated by puffing on a heated tobacco product. After the filter for collecting particulate matter is extracted with ethyl acetate, diluted, and derivatized with BSTFA, it can be used for detection and analysis, without the need for extraction column extraction, concentration and reconstitution, nor the dual-sample subtraction method for quantification, greatly simplifying the sample pretreatment steps and improving the sensitivity and accuracy of detection.

[0033] The sample pretreatment method for the simple and rapid detection of glycidol and monochloropropanols in heated tobacco aerosol of the present invention comprises the following steps:

[0034] (1) Use a smoking machine to puff on 3-5 heated tobacco products, and collect particulate matter with a Cambridge filter;

[0035] (2) After the suction is completed, mix the Cambridge filter, 10 - 15 mL of ethyl acetate, and 125 - 150 μL of the internal standard solution, and perform ultrasonic extraction for 5 - 10 min at room temperature with an ultrasonic power of 40 - 50 W to obtain an extract. Dilute every 200 μL of the extract with n - ethyl acetate to a volume of 1 - 2 mL. The internal standard solution includes D5 - glycidol, D5 - 2 - MCPD, and D5 - 3 - MCPD. The concentrations of D5 - glycidol and D5 - 2 - MCPD are both 250 - 300 ng / mL, and the concentration of D5 - 3 - MCPD is 500 - 550 ng / mL;

[0036] (3) Add 50 - 80 μL of BSTFA and pyridine to the 1 - 2 mL of diluted extract obtained in step (2). The volume ratio of pyridine to BSTFA is (1 - 1.2):1, and perform a derivatization reaction at 70 - 80 °C for 5 - 8 min. Let it cool to room temperature to obtain a test solution.

[0037] In a specific embodiment, the smoking machine is a linear smoking machine, and the suction is performed in the HCI suction mode. The suction volume, frequency, and duration are 55 - 60 mL, 30 - 50 s, and 2 - 5 s respectively.

[0038] In a specific embodiment, after extraction, let it stand for 2 - 5 min, and take the supernatant to pass through a 0.2 - 0.5 μm filter membrane to obtain an extract.

[0039] In a specific embodiment, the derivatization reaction is carried out under a water - bath condition.

[0040] The following further illustrates the embodiments of the present invention in conjunction with specific examples. The chemical reagents involved in the following examples are all commercially available conventional products unless otherwise specified.

[0041] I. Specific examples of the sample pretreatment method for simply and rapidly detecting glycidol and monochloropropanols in heated - tobacco aerosol of the present invention

[0042] Example 1

[0043] The sample pretreatment method for simply and rapidly detecting glycidol and monochloropropanols in heated - tobacco aerosol in this example is as follows:

[0044] (1) Use a linear smoking machine to suction 3 heated - tobacco cigarettes in the HCI suction mode (suction volume / frequency / duration: 55 mL / 30 s / 2 s), and collect the particulate matter with a Cambridge filter.

[0045] (2) After the suction is completed, place the Cambridge filter in a triangular flask (25 mL), add 10 mL of extraction solvent (ethyl acetate) and 125 μL of internal standard working solution (D5-glycidol, D5-2-MCPD, D5-3-MCPD, with concentrations of 250 ng / mL, 250 ng / mL, and 500 ng / mL respectively), sonicate at a power of 40 W for 10 min at room temperature, let it stand for 2 min, take the supernatant and filter it through a 0.2 μm filter membrane to obtain the filtrate (i.e., the extract). Take 200 μL of the filtrate and place it in a derivatization vial, and make up the volume to 1 mL with ethyl acetate.

[0046] (3) Add 80 μL of derivatization reagent BSTFA and 80 μL of pyridine to the filtrate with a volume of 1 mL obtained in step (2), derivatize at 80 °C in a water bath for 5 min, and let it cool to room temperature to obtain the solution to be measured.

[0047] II. Specific examples of the simple and rapid GC-MS method for detecting glycidol and monochloropropanols in heated tobacco aerosol of the present invention

[0048] Example 2

[0049] The simple and rapid GC-MS method for detecting glycidol and monochloropropanols in heated tobacco aerosol in this example is as follows:

[0050] Use the sample pretreatment method of Example 1 to obtain the solution to be measured, and perform GC-MS detection and analysis.

[0051] The chromatographic conditions for GC-MS detection and analysis are as follows: Chromatographic column: elastic quartz capillary chromatographic column, the stationary phase is 5% phenyl-methyl polysiloxane, specification 30 m × 0.25 mm × 0.25 μm; injection port temperature: 280 °C; injection volume: 2.0 μL; injection mode: split injection, split ratio: 10:1; carrier gas: helium, constant flow mode, flow rate 1.0 mL / min; programmed temperature rise: initial temperature 50 °C, then rise to 90 °C at a heating rate of 10 °C / min, hold for 2 min, and then rise to 280 °C at a heating rate of 40 °C / min, hold for 10 min.

[0052] The mass spectrometric conditions for GC-MS detection and analysis are as follows: Ionization mode: electron impact ionization, ionization energy 70 eV; filament current: 35 μA; ion source temperature: 290 °C; transfer line temperature: 290 °C; mass spectrometry scanning mode: selected ion monitoring (SIM) mode, and the SIM parameters are shown in Table 1.

[0053] Table 1 Monitoring ions of BSTFA derivatives of glycidol, 3-MCPD, 2-MCPD and their deuterated compounds

[0054]

[0055]

[0056] III. Experimental Examples

[0057] (1) Determination of working curve and detection limit

[0058] According to the content of the target substance in the sample, the 7-level calibration line concentrations of glycidol and 2-MCPD are: 5, 25, 50, 100, 200, 400, 800 ng / mL, and the corresponding internal standard concentration is: 250 ng / mL. The 7-level calibration line concentrations of 3-MCPD are 50, 100, 200, 400, 800, 1600, 3200 ng / mL respectively, and the internal standard concentration is: 500 ng / mL. Linear regression analysis was performed on the ratio of the peak area of each target substance to the peak area of the internal standard and the ratio of the concentration of each target substance to the internal standard concentration to obtain the standard working curve. The experimental results show that within the linear concentration range, the linear relationships of the standard curves are good and suitable for quantitative analysis. The method detection limit (LOD) and quantification limit (LOQ) were calculated based on 3 times the signal-to-noise ratio and 10 times the signal-to-noise ratio. The detection limits of glycidol, 3-MCPD, and 2-MCPD are 1 - 20 ng / mL, and the quantification limits are 3 - 70 ng / mL, which fully meet the quantitative analysis requirements of glycidol in heated tobacco aerosol. The test results of the standard working curves, correlation coefficients, detection limits, and quantification limits of the 3 target substances are shown in Table 2.

[0059] Table 2 Standard working curves, correlation coefficients, detection limits, and quantification limits of 3 target substances

[0060]

[0061] (2) Recovery and precision

[0062] A typical heated cigarette was selected and tested and analyzed with reference to Example 2. Five parallel experiments were carried out intra-day and five parallel experiments were carried out inter-day to investigate the precision of the method, and the determination of sample spiked recovery was carried out at three content levels of high, medium, and low (the added amounts were based on the content in the sample, 0.5 times, 1 times, and 2 times the added content). The test results of precision and recovery are shown in Table 3. It can be seen from Table 3 that the intra-day RSD% of the determination results of glycidol, 3-MCPD, and 2-MCPD are between 4% and 10%, and the inter-day RSD% are between 2% and 8%; the results of the three-level method recovery are between 98% and 110%. The results show that this method has good precision, accuracy, and stability, and can meet the needs of analysis and detection.

[0063] Table 3 Test results of recovery and precision of 3 compounds

[0064]

[0065] (3) Determination of the content of the target substance in the sample

[0066] Referring to the detection method of Example 2, the contents of glycidol and monochloropropanols in the aerosol of 6 domestic and foreign heated tobacco products were detected, and the test results are shown in Table 4. Among them, the selected ion chromatograms of the glycidol standard sample and glycidol in Sample 5 are as shown in Figure 1 shown, where the abscissa is time (min) and the ordinate is relative abundance. The selected ion chromatograms of the D5-glycidol standard sample and D5-glycidol in Sample 5 are as shown in Figure 2 shown, the selected ion chromatograms of the 3-MCPD, 2-MCPD standard samples and 3-MCPD, 2-MCPD in Sample 5 are as shown in Figure 3 shown, and the selected ion chromatograms of the D5-3-MCPD, D5-2-MCPD standard samples and 3-MCPD, 2-MCPD in Sample 5 are as shown in Figure 4 shown.

[0067] Table 4 Test results of the contents of glycidol and monochloropropanols in the aerosol of 6 heated tobacco products

[0068]

[0069] Finally, it should be noted that the above are only the preferred embodiments of the present invention and are not intended to limit the present invention. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments, or perform equivalent replacements for some of the technical features. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims

1. A simple and rapid sample pretreatment method for detecting glycidol and monochloropropanol in heated cigarette aerosol, characterized in that: The following steps are involved: (1) Capture the particulate matter in the heated cigarette aerosol; (2) extracting the captured particulate matter by mixing the capture material with ethyl acetate and the internal standard to obtain an extract, which is then diluted with ethyl acetate; (3) Add N,O-bis(trimethylsilyl)trifluoroacetamide to the diluted extract obtained in step (2) to carry out a derivatization reaction to obtain a test solution.

2. The sample pretreatment method for simply and quickly detecting glycidol and monochloropropanol in heated cigarette aerosol according to claim 1, characterized in that: Pyridine is added during the derivatization reaction, and the volume ratio of pyridine to N,O-bis(trimethylsilyl)trifluoroacetamide is (1-1.2):

1.

3. The sample pretreatment method for simply and quickly detecting glycidol and monochloropropanol in heated cigarette aerosol according to claim 1, characterized in that: The capturing is to capture the particulate matter in the heated cigarette aerosol using a filter, and the mixing is to mix the filter that captures the particulate matter in the aerosol when every 3 to 5 heated cigarettes are smoked with 125 to 150 μL of internal standard solution and 10 to 15 mL of ethyl acetate.

4. The sample pretreatment method for simply and quickly detecting glycidol and monochloropropanol in heated cigarette aerosol according to claim 3, characterized in that: The internal standard solution includes D5-glycidol, D5-2-MCPD and D5-3-MCPD. The concentrations of D5-glycidol and D5-2-MCPD are both 250-300 ng / mL, and the concentration of D5-3-MCPD is 500-550 ng / mL.

5. The sample pretreatment method for simply and quickly detecting glycidol and monochloropropanol in heated cigarette aerosol according to claim 1, characterized in that: The extraction is carried out at room temperature under ultrasonic conditions for 5 to 10 minutes, and the power of the ultrasonic is 40 to 50W.

6. The sample pretreatment method for simply and quickly detecting glycidol and monochloropropanol in heated cigarette aerosol according to claim 1, characterized in that: The temperature of the derivatization reaction is 70-80° C., and the time of the derivatization reaction is 5-8 minutes.

7. The sample pretreatment method for simply and quickly detecting glycidol and monochloropropanol in heated cigarette aerosol according to claim 1, characterized in that: Ethyl acetate was added to every 200 μL of the extract to make the volume 1-2 mL to obtain a diluted extract, and 50-80 μL of N,O-bis(trimethylsilyl)trifluoroacetamide was added to every 1-2 mL of the diluted extract.

8. A GC-MS method for simple and rapid detection of glycidol and monochloropropanol in heated cigarette aerosol, characterized in that: The sample pretreatment method according to any one of claims 1 to 7 is used to obtain a test solution, which is then subjected to GC-MS detection and analysis.

9. The GC-MS method for simple and rapid detection of glycidol and monochloropropanol in heated cigarette aerosol according to claim 8, characterized in that: The chromatographic conditions for GC-MS detection and analysis were as follows: chromatographic column: elastic quartz capillary column, the stationary phase was 5% phenyl-methylpolysiloxane; injection port temperature: 280~290℃; injection volume: 1.0~2.0μL; injection mode: split injection, split ratio: 10:1; carrier gas: helium, constant flow mode, flow rate 1.0~2.0mL / min; programmed temperature rise: initial temperature 40~50℃, then increase to 80~90℃ at a heating rate of 10~15℃ / min, maintain for 2~3min, and then increase to 280~290℃ at a heating rate of 40~50℃ / min, and maintain for 10~12min.

10. The GC-MS method for simple and rapid detection of glycidol and monochloropropanol in heated cigarette aerosol according to claim 8, characterized in that: The mass spectrometry conditions during GC-MS detection and analysis were as follows: ionization mode: electron impact ionization, ionization energy 70 eV; ion source temperature: 290~300°C; transfer line temperature: 290~300°C; mass spectrometry scanning mode: selected ion monitoring SIM mode.

Citation Information

Patent Citations

  • Method for detecting content of chloropropanol in electronic cigarette aerosol

    CN118225931A