CN109975467B - Method for measuring epoxypropanol in main stream smoke of cigarette - Google Patents
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Abstract
The invention belongs to the technical field of physicochemical inspection of cigarette smoke, and particularly relates to a method for measuring glycidol in main stream smoke of cigarettes. The invention provides a method for measuring glycidol in main stream smoke of cigarettes, which comprises the following steps: step one, collecting total particulate matters of main stream smoke of cigarettes; step two, pretreatment; step three, balancing; step four, quantitative analysis: and (3) detecting the balance liquid obtained in the step (III) by using a gas chromatography-mass spectrometry method, and detecting the content of the epoxy propanol in the balance liquid. According to the technical scheme provided by the invention, the content of the epoxypropanol in the main stream smoke of the cigarettes can be detected rapidly and accurately, the error in the pretreatment process is reduced, the matrix interference is reduced, and the accuracy of the detection method is further improved by improving the selectivity and the sensitivity of the detection method; solves the technical defect that the prior art lacks a method for accurately detecting the glycidol in the main stream smoke of the cigarettes and can not provide accurate guidance for the safety evaluation of the cigarettes.
Description
Technical Field
The invention belongs to the technical field of physicochemical inspection of cigarette smoke, and particularly relates to a method for measuring glycidol in main stream smoke of cigarettes.
Background
The glycidol is an important fine chemical raw material, can be used as a stabilizer of natural oil, vinyl polymers, demulsifiers and dyeing layering agents, is also used as an intermediate for synthesizing glycerol, glycidyl ether (amine and the like), and can be used as a gel of surface coating, chemical synthesis, medicine, pharmaceutical chemical industry, bactericides and solid fuel. Glycidol can be inhaled into the human body through the skin, causing corrosion of the skin, eyes, respiratory tract, gastrointestinal mucosa, and long-term contact will cause skin necrosis and serious damage to the cornea. The mainstream smoke constituents of cigarettes are very complex, and more than 8000 substances, including glycidol, have been identified.
However, in the prior art, a method capable of accurately detecting the epoxypropanol in the main stream of the cigarette is lacking, and accurate guidance cannot be provided for the safety evaluation of the cigarette.
Disclosure of Invention
In view of the above, the invention provides a method for determining glycidol in main stream smoke of cigarettes, which is used for solving the technical defect that in the prior art, a method for accurately detecting glycidol in main stream smoke of cigarettes is lacking and accurate guidance cannot be provided for safety evaluation of cigarettes.
The invention provides a method for measuring glycidol in main stream smoke of cigarettes, which comprises the following steps:
step one, collecting particulate matters: when the cigarettes are smoked, the total particulate matters of the main stream smoke of the cigarettes are trapped;
step two, pretreatment: dissolving the total particulate matters collected in the first step into an extracting solution for ultrasonic extraction, and collecting supernatant;
step three, balancing: balancing the supernatant fluid obtained in the second step in a static headspace instrument to obtain a balancing solution;
step four, quantitative analysis: and (3) detecting the balance liquid obtained in the step (III) by using a gas chromatography-mass spectrometry method, and detecting the content of the epoxy propanol in the balance liquid.
Preferably, in the first step, the method for collecting the particulate matters comprises the following steps: the total particulate matter in the mainstream smoke was collected using a Cambridge filter.
Preferably, in the first step, the number of cigarettes is 2-5.
Preferably, in the first step, the number of cigarettes is 2.
Preferably, in the second step, the extracting solution includes: a solvent and an internal standard, wherein the solvent is methanol or acetonitrile, and the internal standard is deuterated internal standard.
Preferably, the concentration of the internal standard is 1-5 mg/mL, and the volume of the internal standard is 50-200 mu L.
Preferably, the concentration of the internal standard is 1mg/mL and the volume of the internal standard is 100. Mu.L.
Preferably, the volume of the extracting solution is 10-40 mL.
Preferably, the volume of the extract is 20mL.
Preferably, in the second step, the time of the ultrasonic treatment is 20-60 min.
Preferably, in the second step, the time of the ultrasonic treatment is 20min.
Preferably, in the third step, the temperature of the balancing is 80-120 ℃, and the time of the balancing is 10-40 min.
Preferably, in the third step, the temperature of the balancing is 90 ℃, and the time of the balancing is 10min.
Preferably, in step four, the column is PerkinElmer Elite-624 (60 m. Times.0.32 mm. Times.1.8 μm) for gas chromatography detection.
Preferably, in the fourth step, in the gas chromatography detection, the temperature raising program of the chromatographic column is: the initial temperature is 30-50 ℃, and the temperature is kept for 1-3 min; then heating to 80-100 ℃ at a heating rate of 2-4 ℃/min; then heating to 180-220 ℃ at 15-20 ℃/min, and keeping for 5-8 min.
Preferably, in the fourth step, in mass spectrometry detection, the ion source is an electron bombardment source, the ion source temperature is 200-280 ℃, and the ion transmission line temperature is 200-280 ℃.
In summary, the invention provides a method for determining glycidol in main stream smoke of cigarettes, which comprises the following steps: step one, collecting total particulate matters of cigarette smoke: when the cigarettes are smoked, the total particulate matters of the main stream smoke of the cigarettes are trapped; step two, pretreatment: dissolving the total particulate matters collected in the first step into an extracting solution, and collecting a supernatant; step three, balancing: balancing the supernatant obtained in the second step by adopting a static headspace instrument to obtain a balancing solution; step four, quantitative analysis: and (3) detecting the balance liquid obtained in the step (III) by using a gas chromatography-mass spectrometry method, and detecting the content of the epoxy propanol in the balance liquid. According to the technical scheme provided by the invention, the content of glycidol in main stream smoke can be detected rapidly and accurately, errors in the pretreatment process are reduced, matrix interference is reduced, and the accuracy of the detection method is further improved by improving the selectivity and sensitivity of the detection method. The method for measuring the glycidol in the main stream smoke of the cigarette provided by the invention solves the technical defect that the method for accurately detecting the glycidol in the main stream smoke of the cigarette is lacking in the prior art and cannot provide accurate guidance for the safety evaluation of the cigarette.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required to be used in the embodiments or the description of the prior art will be briefly described below, and it is obvious that the drawings in the following description are only embodiments of the present invention, and that other drawings can be obtained according to the provided drawings without inventive effort for a person skilled in the art.
Fig. 1 is a schematic flow chart of a method for measuring glycidol in main stream smoke of cigarettes provided by the embodiment of the invention;
fig. 2 is an ion extraction flow chart of epoxypropanol when the measurement method provided by the embodiment of the invention is applied to flue gas detection.
Detailed Description
The method for measuring the glycidol in the main stream smoke of the cigarettes provided by the embodiment of the invention solves the technical defect that in the prior art, a method capable of accurately detecting the glycidol in the main stream smoke of the cigarettes is lacking and accurate guidance cannot be provided for safety evaluation of the cigarettes.
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In order to more specifically explain the invention, the method for measuring the glycidol in the main stream smoke of the cigarette provided by the invention is specifically described below by combining the examples.
Example 1
Collecting total particulate matters of cigarette smoke: and 2 cigarettes are smoked according to standard conditions, and the Cambridge filter disc is adopted to collect total particulate matters of main stream smoke of the cigarettes.
Pretreatment: placing the Cambridge filter disc obtained in the last step in a 50mL triangular flask, adding an extracting solution 1 composed of deuterated internal standard solution and 20mL of solvent 1, dissolving the total particle phase in the Cambridge filter disc in the extracting solution 1, and collecting the supernatant 1 after ultrasonic treatment for 20min. Wherein the solvent 1 is methanol, the concentration of the deuterated internal standard solution is 1mg/mL, and the volume of the deuterated internal standard solution is 100 mu L.
Balance: balancing supernatant 1 with static headspace instrument at 90deg.C for 10min to obtain balanced solution 1
Quantitative analysis: detecting the balance liquid 1 by gas chromatography-mass spectrometry, and detecting the content of the epoxy propanol in the balance liquid. Wherein, headspace bottle 20mL, sample ring 3.0mL, sample equilibrium temperature 90 ℃, sample ring temperature 160 ℃, transmission line temperature 180 ℃, sample equilibrium time 10min, sample bottle pressurization pressure 130kPa, pressurization time 0.2min, aeration time 0.2min, sample ring equilibrium time 0.05min, sample introduction time: 0.5min.
The gas chromatography conditions were: the chromatographic column adopts Elite-624 (60 m multiplied by 0.32mm multiplied by 1.8 mu m), the carrier gas is high-purity helium (purity is 99.999%), the flow speed is 1.0mL/min, the sample inlet temperature is 300 ℃, the sample inlet mode is split sample inlet, and the split ratio is 10:1. The room temperature is carried out by adopting a temperature programming mode, and the method specifically comprises the following steps: the initial temperature is 35 ℃, and the temperature is kept for 2min; then heating to 80 ℃ at a heating rate of 2 ℃/min; then heating to 200 ℃ at 20 ℃ per minute, and keeping for 6 minutes.
The mass spectrum conditions are as follows: the ion source is an electron bombardment source, the electron energy is 70eV, the ion source temperature is 230 ℃, and the ion transmission line temperature is 220 ℃; and a mass fraction scanning mode, wherein a Selective Ion (SIM) monitoring mode is used for detecting the content of the epoxypropanol by using quantitative ions of 44 respectively.
Example 2
Collecting total particulate matters of cigarette smoke: and (5) smoking the cigarettes according to standard conditions, and capturing total particulate matters of main stream smoke of the cigarettes by adopting a Cambridge filter disc.
Dissolving: placing the Cambridge filter disc obtained in the last step in a 50mL triangular flask, adding an extracting solution 2 composed of deuterated internal standard solution and 25mL solvent 2, dissolving the total particle phase in the Cambridge filter disc in the extracting solution 2, and collecting the supernatant 2 after ultrasonic treatment for 60min. Wherein the solvent 2 is methanol, the concentration of the deuterated internal standard solution is 2mg/mL, and the volume of the deuterated internal standard solution is 50 mu L.
Balance: and (3) balancing the supernatant liquid 2 in a static headspace instrument at 100 ℃ for 40min to obtain a balanced liquid 2.
Quantitative analysis: the balance liquid 2 was detected by gas chromatography-mass spectrometry to detect the content of the epoxypropanol in the balance liquid. Wherein, headspace bottle 20mL, sample ring 3.0mL, sample equilibrium temperature 90 ℃, sample ring temperature 160 ℃, transmission line temperature 180 ℃, sample equilibrium time 10min, sample bottle pressurization pressure 130kPa, pressurization time 0.2min, aeration time 0.2min, sample ring equilibrium time 0.05min, sample introduction time: 0.5min.
The gas chromatography conditions were: the chromatographic column adopts Elite-624 (60 m multiplied by 0.32mm multiplied by 1.8 mu m), the carrier gas is high-purity helium (purity is 99.999%), the flow speed is 1.0mL/min, the sample inlet temperature is 300 ℃, the sample inlet mode is split sample inlet, and the split ratio is 10:1. The room temperature is carried out by adopting a temperature programming mode, and the method specifically comprises the following steps: the initial temperature is 40 ℃, and the temperature is kept for 3min; then heating to 100 ℃ at a heating rate of 3 ℃/min; then heating to 180 ℃ at 15 ℃ per minute, and keeping for 5 minutes.
The mass spectrum conditions are as follows: the ion source is an electron bombardment source, the electron energy is 70eV, the ion source temperature is 280 ℃, and the ion transmission line temperature is 200 ℃; and a mass fraction scanning mode, wherein a Selective Ion (SIM) monitoring mode is used for detecting the content of the epoxypropanol by using quantitative ions of 44 respectively.
Example 3
Collecting total particulate matters of main stream smoke of cigarettes: 3 cigarettes are smoked according to standard conditions, and the Cambridge filter disc is adopted to collect total particulate matters of main stream smoke of the cigarettes.
Dissolving: placing the Cambridge filter disc obtained in the last step in a 50mL triangular flask, adding an extracting solution 3 composed of xx mu L of deuterated internal standard solution and 30mL of solvent 3, dissolving the total particulate matters in the Cambridge filter disc in the extracting solution 3, and collecting supernatant 3 after ultrasonic treatment for 40min. Wherein the solvent 3 is acetonitrile, the concentration of the deuterated internal standard solution is 5mg/mL, and the volume of the deuterated internal standard solution is 200 mu L.
Balance: the supernatant 3 is balanced in a static headspace analyzer at 80 ℃ for 15min to obtain a balanced solution 3.
Quantitative analysis: the balance liquid 3 was examined by gas chromatography-mass spectrometry to examine the content of the epoxypropanol in the balance liquid. Wherein, headspace bottle 20mL, sample ring 3.0mL, sample equilibrium temperature 90 ℃, sample ring temperature 160 ℃, transmission line temperature 180 ℃, sample equilibrium time 10min, sample bottle pressurization pressure 130kPa, pressurization time 0.2min, aeration time 0.2min, sample ring equilibrium time 0.05min, sample introduction time: 0.5min.
The gas chromatography conditions were: the chromatographic column adopts Elite-624 (60 m multiplied by 0.32mm multiplied by 1.8 mu m), the carrier gas is high-purity helium (purity is 99.999%), the flow speed is 1.0mL/min, the sample inlet temperature is 300 ℃, the sample inlet mode is split sample inlet, and the split ratio is 10:1. The room temperature is carried out by adopting a temperature programming mode, and the method specifically comprises the following steps: the initial temperature is 40 ℃, and the temperature is kept for 3min; then heating to 100 ℃ at a heating rate of 3 ℃/min; then heating to 180 ℃ at 15 ℃ per minute, and keeping for 8 minutes.
The mass spectrum conditions are as follows: the ion source is an electron bombardment source, the electron energy is 70eV, the ion source temperature is 280 ℃, and the ion transmission line temperature is 200 ℃; and a mass fraction scanning mode, wherein a Selective Ion (SIM) monitoring mode is used for detecting the content of the epoxypropanol by using quantitative ions of 44 respectively.
Example 4
This example shows the results of the tests of examples 1 to 3.
In the mainstream smoke of cigarettes, the extraction ion graph of the epoxypropanol is shown in fig. 2, and the measurement result of the epoxypropanol is shown in table 1.
TABLE 1
| Example 1 | Example 2 | Example 3 | |
| Glycidol (mug/cigarette) | 7.03 | 3.33 | 2.09 |
Example 5
This example is a specific example of a working curve, detection limit and quantitative limit.
Serial standard solutions of glycidol with different concentrations were prepared with methanol as solvent, and headspace-gas chromatography-mass spectrometry was performed using the instrument conditions described in example 1 above, respectively.
Then, quantitative determination is carried out by adopting an internal standard method, regression analysis is carried out by taking the peak area ratio of each target object and the internal standard as an ordinate (Y) and the concentration of each target object as an abscissa (X, ng/mL), and a regression equation Y=0.00486884x+0.00180935 of the epoxypropanol is obtained, and the correlation coefficient R is obtained 2 0.9992.
The lowest concentration standard solution was diluted and subjected to headspace-gas chromatography-mass spectrometry analysis with a 3-fold signal to noise ratio (snr) as the detection Limit (LOD) and a 10-fold snr as the quantification Limit (LOQ), and the LOD and LOQ of glycidol were 0.014 μg/cigarette and 0.045 μg/cigarette, respectively. The method has higher sensitivity and is suitable for quantitative analysis of the epoxy propanol in the main stream smoke of the cigarettes.
The headspace-gas chromatography-mass spectrometry analysis was performed using the conditions in example 2 and example 3, respectively, to obtain experimental results similar to the measurement conditions in example 1, and will not be described in detail here.
Example 6
This example is a specific example of recovery and precision.
Two cigarettes were extracted according to standard smoking conditions, total particulate matter of 2 cigarettes was trapped with a Cambridge filter, standard solutions were added at 3 addition levels of low, medium and high on the collected Cambridge filter, then samples were treated according to the described sample pretreatment method, each addition level was measured in parallel 6 times, and recovery and precision were measured, and experimental results are shown in table 3.
Table 2 recovery of epoxypropanol in mainstream smoke of cigarettes and precision (n=6)
As can be seen from Table 2, the average standard recovery rate of the glycidol is between 83.9% and 95.3%, and the relative standard deviation is less than 10%, so that the quantitative requirement can be met.
In summary, the invention provides a method for determining glycidol in main stream smoke of cigarettes, which comprises the following steps: step one, collecting total particulate matters of main stream smoke of cigarettes: when the cigarettes are smoked, the total particulate matters of the main stream smoke of the cigarettes are trapped; step two, pretreatment: dissolving the total particulate matters collected in the first step into an extracting solution, carrying out ultrasonic extraction, and collecting supernatant; step three, balancing: balancing the supernatant obtained in the second step through a static headspace meter to obtain a balancing solution; step four, quantitative analysis: and (3) detecting the balance liquid obtained in the step (III) by using a gas chromatography-mass spectrometry method, and detecting the content of the epoxy propanol in the balance liquid. According to the technical scheme provided by the invention, the content of the epoxypropanol in the main stream smoke of the cigarettes can be detected rapidly and accurately, the error in the pretreatment process is reduced, the matrix interference is reduced, and the accuracy of the detection method is further improved by improving the selectivity and the sensitivity of the detection method. The method for measuring the glycidol in the main stream smoke of the cigarette provided by the invention solves the technical defect that the method for accurately detecting the glycidol in the main stream smoke of the cigarette is lacking in the prior art and cannot provide accurate guidance for the safety evaluation of the cigarette.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (7)
1. The method for measuring the glycidol in the main stream smoke of the cigarettes is characterized by comprising the following steps of:
step one, collecting total particulate matters of main stream smoke of cigarettes: when the cigarettes are smoked, the total particulate matters of the main stream smoke of the cigarettes are trapped;
step two, sample pretreatment: dissolving the total particulate matters collected in the first step into an extracting solution for ultrasonic extraction, and collecting supernatant;
step three, balancing: balancing the supernatant obtained in the second step by adopting a static headspace analyzer, wherein the balancing temperature is 80-120 ℃, and the balancing time is 10-40 min, so as to obtain a balancing solution;
step four, quantitative analysis: detecting the balance liquid obtained in the step three by using a gas chromatography-mass spectrometry method, and detecting the content of the epoxy propanol in the balance liquid, wherein the headspace bottle is 20mL, the sample ring is 3.0mL, the sample balance temperature is 90 ℃, the sample ring temperature is 160 ℃, the transmission line temperature is 180 ℃, the sample balance time is 10min, the sample bottle pressurization pressure is 130kPa, the pressurization time is 0.2min, the inflation time is 0.2min, the sample ring balance time is 0.05min, and the sample injection time is: 0.5min;
in the fourth step, the gas chromatography conditions are as follows: the chromatographic column adopts Elite-624 with the specification of 60m multiplied by 0.32mm multiplied by 1.8 mu m, the carrier gas is high-purity helium with the purity of 99.999 percent, the flow rate of 1.0mL/min, the sample inlet temperature of 300 ℃ and the sample inlet mode of split sample injection, and the split ratio of 10:1; the temperature is raised by adopting a temperature programming mode, and the method specifically comprises the following steps: the initial temperature is 35 ℃, and the temperature is kept for 2min; then heating to 80 ℃ at a heating rate of 2 ℃/min; heating to 200 ℃ at 20 ℃/min, and then keeping for 6min;
the mass spectrum conditions are as follows: the ion source is an electron bombardment source, the electron energy is 70eV, the ion source temperature is 230 ℃, and the ion transmission line temperature is 220 ℃; and a mass scanning mode, a selective ion monitoring mode and a quantitative ion detection mode of 44 are adopted to detect the content of the epoxypropanol.
2. The method according to claim 1, wherein in the first step, the method for collecting the particulate matter comprises: and collecting total particulate matters in the main stream smoke of the cigarettes by using a Cambridge filter.
3. The method according to claim 1, wherein in the first step, the number of cigarettes is 2 to 5.
4. The method according to claim 1, wherein in the second step, the extract solution comprises: a solvent and an internal standard, wherein the solvent is methanol or acetonitrile, and the internal standard is deuterated internal standard.
5. The method according to claim 4, wherein the concentration of the internal standard is 1 to 5mg/mL and the volume of the internal standard is 50 to 200. Mu.L.
6. The method according to claim 3, wherein the volume of the extract is 10 to 40mL.
7. The method according to claim 1, wherein in the second step, the ultrasonic wave is performed for 20 to 60 minutes.
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