CN109975443B - Method for detecting aldehydes in cigarette filter - Google Patents
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Abstract
The invention belongs to the technical field of physicochemical inspection of cigarette auxiliary materials, and particularly relates to a method for detecting aldehyde substances in a cigarette filter. The invention provides a method for detecting aldehydes in a cigarette filter, which comprises the following steps: step one, collecting cigarette filters: collecting the cigarette filter tips after the smoking; step two, sample pretreatment: longitudinally cutting the collected cigarette filter tip by using a blade, putting the cut cigarette filter tip into a headspace bottle, and adding a deuterated internal standard and an auxiliary agent; step three, analysis and detection: and after the static headspace instrument is balanced for a period of time, detecting the content of aldehyde substances in the filter tip by using a gas chromatography-mass spectrometry method. In the invention, aldehydes do not need to be derivatized, so that side reactions caused in the derivatization process are avoided, the accuracy of an analysis result is improved, and the complexity of detection is reduced; meanwhile, the simultaneous determination of various aldehyde substances can be realized, and the detection efficiency is further improved.
Description
Technical Field
The invention belongs to the technical field of physicochemical inspection of cigarette auxiliary materials, and particularly relates to a method for detecting aldehyde substances in a cigarette filter.
Background
The volatile carbonyl compounds are important harmful substances in cigarette smoke, and based on sufficient animal experimental data and results, the international cancer research organization lists formaldehyde as a 2A carcinogen (human carcinogen), acetaldehyde as a 2B carcinogen (possibly carcinogenic to human), and acrolein and crotonaldehyde as 3 carcinogens. Consumers can intercept partial formaldehyde, acetaldehyde, propionaldehyde, acrolein and crotonaldehyde in the cigarette filter in the cigarette smoking process, and the development of the filter can be guided by accurately measuring the content levels of the formaldehyde, the acetaldehyde, the propionaldehyde, the acrolein and the crotonaldehyde in the smoked cigarette filter, so that the method has important significance for ensuring the smoking quality of cigarettes and reducing the smoking harmfulness.
At present, the reported detection methods of volatile carbonyl compounds in the filter tip are solid phase extraction capillary gas chromatography and liquid chromatography-tandem mass spectrometry. Wherein, the gas chromatography adopts the derivatization reaction of 2, 4-Dinitrophenylhydrazine (DNPH) and carbonyl compounds, and a large amount of side reactions can occur in the process of the derivatization reaction, which seriously influences the detection precision; and purifying the sample by using a C18 solid phase extraction column, and then performing gas chromatography analysis. Secondly, the liquid chromatography-tandem mass spectrometry also needs to adopt 2, 4-Dinitrophenylhydrazine (DNPH) to be derivatized with a carbonyl compound, and analysis is carried out after a filter membrane is carried out, although the sensitivity of the liquid chromatography-tandem mass spectrometry is obviously improved, the pretreatment is complex, and reagents with high toxicity such as pyridine and the like are needed.
Therefore, the development of a method for detecting aldehydes in cigarette filters solves the technical defects of inconvenient inspection and poor accuracy in the detection of aldehydes in cigarette filters in the prior art, and becomes a problem to be solved by technical personnel in the field.
Disclosure of Invention
In view of the above, the invention provides a method for detecting aldehyde substances in a cigarette filter, which is used for solving the technical defects of inconvenience in detection and poor accuracy in detection of the aldehyde substances in the cigarette filter in the prior art.
The invention provides a method for detecting aldehydes in a cigarette filter, which comprises the following steps:
step one, collecting cigarette filters: collecting the cigarette filter tips after the smoking;
step two, pretreatment: cutting the filter tip, putting into a headspace bottle, and adding a certain amount of extractant;
step three, analysis and detection: and (3) balancing the sample by using a static headspace instrument for a period of time, and then detecting the content of aldehyde substances in the sample by using a gas chromatography-mass spectrometry method.
Preferably, in the first step, the number of the cigarette filters is 2 to 5.
Preferably, in the second step, the extraction agent comprises an auxiliary agent and a deuterated internal standard.
Preferably, the auxiliary agent is glyceryl triacetate, and the deuterated internal standard is benzene-D6 or acetone-D3.
Preferably, the concentration of the deuterated internal standard is 1-5 mg/mL;
the volume of the auxiliary agent is 1-3 mL.
Preferably, in the third step, the temperature of the equilibrium is 80 to 120 ℃, and the time of the equilibrium is 10 to 40min.
Preferably, in the third step, the temperature of the equilibrium is 90 ℃, and the time of the equilibrium is 10min.
Preferably, in step three, the column is PerkinElmer Elite-624 (60 m.times.0.32 mm. Times.1.8 μm) as detected by gas chromatography.
Preferably, in the third step, during the detection of the gas chromatography, the temperature-raising program of the chromatographic column is: the initial temperature is 30-40 ℃, and the temperature is kept for 1-3 min; then heating to 80-100 ℃ at a heating rate of 2-4 ℃/min; then the temperature is increased to 180-220 ℃ at the speed of 15-20 ℃/min and then is kept for 5-8 min.
Preferably, in the third step, during mass spectrometry, the ion source is an electron bombardment source, the temperature of the ion source is 200-280 ℃, and the temperature of the ion transmission line is 200-280 ℃.
Preferably, the aldehydes are selected from: any one or more of formaldehyde, acetaldehyde, propionaldehyde, acrolein, and crotonaldehyde.
In summary, the invention provides a method for detecting aldehydes in a cigarette filter, which comprises the following steps: step one, collecting cigarette filters: collecting the cigarette filter tips after the smoking; step two, pretreatment: cutting the filter tip, putting into a headspace bottle, and adding an auxiliary agent and a deuterated internal standard; step three, quantitative analysis: and (3) balancing the sample for a period of time by using a static headspace instrument, and detecting the content of aldehyde substances in the sample by using a gas chromatography-mass spectrometry method. In the technical scheme provided by the invention, aldehydes do not need to be derivatized, so that side reactions caused in the derivatization process are avoided, the accuracy of an analysis result is improved, and the complexity of detection is reduced; meanwhile, the simultaneous determination of various aldehyde substances can be realized, and the detection efficiency is further improved; the technical defects of inconvenience in inspection and poor accuracy in the detection of the aldehyde substances in the cigarette filter in the prior art are overcome.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
Fig. 1 is a schematic flow chart of a method for detecting aldehyde substances in a cigarette filter according to an embodiment of the present invention;
fig. 2 is an ion flow diagram of extraction of aldehyde substances when the detection method provided by the embodiment of the invention is applied to cigarette filter detection.
Detailed Description
The method for detecting the aldehyde substances in the cigarette filter provided by the embodiment of the invention solves the technical defects of inconvenience in detection and poor accuracy in the detection of the aldehyde substances in the cigarette filter in the prior art.
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In order to explain the present invention in more detail, the following will specifically describe a method for detecting aldehydes in a cigarette filter according to the present invention with reference to the following examples.
Example 1
This example is a specific example of detecting the content of aldehyde substances in a filter 1 which has been smoked in a commercially available cigarette 1.
Pretreatment: after the filter tip 1 which is sucked is longitudinally cut by a blade, putting the filter tip into a headspace bottle, and adding 1mL of an extracting agent 1; wherein the number of filters 1 is 2. The extractant 1 comprises an auxiliary agent 1 and an internal standard 1, wherein the auxiliary agent 1 is glyceryl triacetate, and the internal standard 1 is benzene-D6; wherein the concentration of the internal standard 1 is 3mg/mL.
Static headspace device balancing: the auxiliary agent 1 dissolved with the filter tip 1 is balanced for 10min at the temperature of 90 ℃, so that aldehyde substances in the filter tip 1 are uniformly distributed in the headspace bottle.
Quantitative analysis: and detecting the content of aldehyde substances in the balanced headspace bottle by using a headspace-gas chromatography-mass spectrometry combined detection method. 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 aeration time is 0.2min, the sample ring balance time is 0.05min, and the sample introduction time is as follows: 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 99.999%), the flow rate is 1.0mL/min, the injection port temperature is 300 ℃, the injection mode is split injection, and the split ratio is 10. The room temperature is carried out by adopting a temperature programming mode, which specifically comprises the following steps: the initial temperature is 35 ℃, and the temperature is kept for 2min; then heating to 80 ℃ at the heating rate of 2 ℃/min; then the temperature is raised to 200 ℃ at a rate of 20 ℃/min and then kept for 6min.
The mass spectrum conditions are as follows: the ion source is an electron bombardment source, the electron energy is 70eV, the temperature of the ion source is 230 ℃, and the temperature of an ion transmission line is 220 ℃; and in a mass spectrometry scanning mode and a Selective Ion (SIM) monitoring mode, quantitative ions of 29, 44, 58, 56, 70 and 84 respectively are selected to detect the contents of formaldehyde, acetaldehyde, propionaldehyde, acrolein, crotonaldehyde and deuterated internal standard in the sample to be detected.
Example 2
This example is a specific example of detecting the content of aldehyde substances in a filter 2 of a commercially available cigarette 2 after smoking.
Pretreatment: after the filter tip 2 which is sucked is longitudinally cut by a blade, the filter tip is placed into a headspace bottle, and 1mL of extractant 2 is added; wherein the number of the filter tips 2 is 4. The extractant 2 comprises an auxiliary agent 2 and an internal standard 2, wherein the auxiliary agent 2 is glyceryl triacetate, and the internal standard 2 is benzene-D6; wherein the concentration of the internal standard 2 is 5mg/mL.
Balancing a static headspace device: the auxiliary agent 2 dissolved with the filter tip 2 is balanced for 30min at the temperature of 80 ℃, so that the aldehyde substances in the filter tip 2 are uniformly distributed in the headspace bottle.
Quantitative analysis: and detecting the content of aldehyde substances in the balanced headspace bottle by using a headspace-gas chromatography-mass spectrometry combined detection method. 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 aeration time is 0.2min, the sample ring balance time is 0.05min, and the sample introduction time is as follows: 0.5min.
The gas chromatography conditions were: the chromatographic column adopts Elite-624 (60 m × 0.32mm × 1.8 μm), the carrier gas is high-purity helium (purity 99.999%), the flow rate is 1.0mL/min, the injection port temperature is 300 ℃, the injection mode is split injection, and the split ratio is 10. The room temperature is carried out by adopting a temperature programming mode, which specifically comprises the following steps: the initial temperature is 35 ℃, and the temperature is kept for 2min; then heating to 80 ℃ at the heating rate of 2 ℃/min; then the temperature is raised to 220 ℃ at a speed of 25 ℃/min and then kept for 6min.
The mass spectrum conditions are as follows: the ion source is an electron bombardment source, the electron energy is 70eV, the temperature of the ion source is 230 ℃, and the temperature of an ion transmission line is 220 ℃; and in a mass spectrometry scanning mode and a Selective Ion (SIM) monitoring mode, quantitative ions of 29, 44, 58, 56, 70 and 84 respectively are selected to detect the contents of formaldehyde, acetaldehyde, propionaldehyde, acrolein, crotonaldehyde and deuterated internal standard in the sample to be detected.
Example 3
This example is a specific example of the detection of the content of aldehyde substances in a filter 3 of a commercially available cigarette 3 after smoking.
Pretreatment: after the filter tip 3 which is sucked is longitudinally cut by a blade, putting the filter tip into a headspace bottle, and adding 1mL of an extracting agent 3; wherein the number of filters 3 is 5. The extractant 3 comprises an auxiliary agent 3 and an internal standard 3, wherein the auxiliary agent 3 is triacetin, and the internal standard 3 is acetone-D3; wherein the concentration of the internal standard 3 is 5mg/mL.
Static headspace device balancing: the auxiliary agent 3 dissolved with the filter tip 3 is balanced for 40min at 120 ℃, so that the aldehyde substances in the filter tip 3 are uniformly distributed in the headspace bottle.
Quantitative analysis: and detecting the content of aldehyde substances in the balanced headspace bottle by using a headspace-gas chromatography-mass spectrometry combined detection method. 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 aeration time is 0.2min, the sample ring balance time is 0.05min, and the sample introduction time is as follows: 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 99.999%), the flow rate is 1.0mL/min, the injection port temperature is 300 ℃, the injection mode is split injection, and the split ratio is 10. The room temperature is carried out by adopting a temperature programming mode, which specifically comprises the following steps: the initial temperature is 30 ℃, and the temperature is kept for 1min; then heating to 86 ℃ at the heating rate of 4 ℃/min; then the temperature is raised to 220 ℃ at a rate of 18 ℃/min and then kept for 8min.
The mass spectrum conditions are as follows: the ion source is an electron bombardment source, the electron energy is 70eV, the temperature of the ion source is 230 ℃, and the temperature of an ion transmission line is 220 ℃; and in a mass spectrometry scanning mode and a Selective Ion (SIM) monitoring mode, quantitative ions of 29, 44, 58, 56, 70 and 84 respectively are selected to detect the contents of formaldehyde, acetaldehyde, propionaldehyde, acrolein, crotonaldehyde and deuterated internal standard in the sample to be detected.
Example 4
This example shows the results of the tests of examples 1 to 3.
For the extraction of formaldehyde, acetaldehyde, propionaldehyde, acrolein and crotonaldehyde in the filter of cigarette, refer to fig. 2, and for the measurement results of aldehydes, refer to table 1.
TABLE 1
Example 5
This example is a specific example of working curve, detection limit and quantitation limit determination.
A series of standard solutions of formaldehyde, acetaldehyde, propionaldehyde, acrolein and crotonaldehyde at different concentrations were prepared, respectively, using triacetin as a solvent, and headspace-gas chromatography-mass spectrometry was performed, respectively, using the conditions in example 1.
Then, the (deuterated benzene) is quantified by an internal standard method, and regression analysis is performed by taking the peak area ratio of each target to the internal standard thereof as the ordinate (Y) and the concentration of each target as the abscissa (X, mu g/mL), so as to obtain the regression equation and the correlation coefficient of formaldehyde, acetaldehyde, propionaldehyde, acrolein and crotonaldehyde, which are shown in Table 2.
TABLE 2 working curves and correlation coefficients, detection limits and quantification limits of the method
As can be seen from Table 2, the standard curves for formaldehyde, acetaldehyde, propionaldehyde, acrolein and crotonaldehyde are in good linearity, R is 2 Between 0.9974 and 0.9992.
Diluting the standard solution with the lowest concentration, and performing headspace-gas chromatography-mass spectrometry, wherein the detection Limit (LOD) is 3 times of signal-to-noise ratio, and the quantification Limit (LOQ) is 10 times of signal-to-noise ratio, so as to obtain: LOD and LOQ of formaldehyde, acetaldehyde, propionaldehyde, acrolein and crotonaldehyde are 0.003 to 0.024 mu g/filter tip and 0.01 to 0.08 mu g/filter tip respectively. The method has higher sensitivity and is suitable for quantitative analysis of formaldehyde, acetaldehyde, propionaldehyde, acrolein and crotonaldehyde in the cigarette filter.
Headspace-gas chromatography-mass spectrometry was performed under the conditions of example 2 and example 3, respectively, to obtain experimental results similar to the measurement conditions of example 1, and further description thereof is omitted.
Example 5
This example is a specific example of recovery and precision.
Taking a blank cigarette filter sample, adding standard solution on the collected filter according to 3 addition levels of low, medium and high, then processing the sample according to the described sample pretreatment method, parallelly measuring each addition level for 6 times, and measuring the recovery rate and the precision, wherein the experimental result is shown in Table 3.
TABLE 3 recovery and precision of aldehydes in cigarette filters (n = 6)
As can be seen from Table 3, the average normalized recovery rates of formaldehyde, acetaldehyde, propionaldehyde, acrolein and crotonaldehyde are 88.1% -107%, and the relative standard deviation is less than 10%, so that the quantitative requirement can be met.
The technical scheme provided by the invention has the following advantages:
(1) The detection method can realize the simultaneous determination of formaldehyde, acetaldehyde, propionaldehyde, acrolein and crotonaldehyde in the cigarette filter tip without carrying out sample pretreatment and derivatization on aldehydes, thereby avoiding a large amount of side reactions in the derivatization reaction process, improving the accuracy of an analysis result and simultaneously improving the detection efficiency;
(2) And deuterated benzene or deuterated acetone is selected as an internal standard to quantify each compound, so that the experimental error is effectively reduced, and the accuracy of the analysis result is improved.
According to the method, the content levels of formaldehyde, acetaldehyde, propionaldehyde, acrolein and crotonaldehyde in the cigarette filter can be rapidly and accurately detected, the deuterated benzene is used as an internal standard quantitative analyte, errors caused in the sample pretreatment process can be reduced, the matrix interference is reduced, and the selectivity and the sensitivity of the method are better improved by a mass spectrometry method, so that the accuracy of the method is improved.
In summary, the invention provides a method for detecting aldehydes in a cigarette filter, which comprises the following steps: step one, collecting cigarette filters: collecting the cigarette filter tips after the smoking; step two, sample pretreatment: longitudinally cutting the collected cigarette filter tip by using a blade, putting the cut cigarette filter tip into a headspace bottle, and adding a deuterated internal standard and an auxiliary agent; step three, analysis and detection: and after the static headspace instrument is balanced for a period of time, detecting the content of aldehyde substances in the filter tip by using a gas chromatography-mass spectrometry method. In the technical scheme provided by the invention, aldehydes do not need to be derivatized, so that side reactions caused in the derivatization process are avoided, the accuracy of an analysis result is improved, and the complexity of detection is reduced; meanwhile, the simultaneous determination of various aldehyde substances can be realized, and the detection efficiency is further improved; the technical defects of inconvenience in inspection and poor accuracy in the detection of the aldehyde substances in the cigarette filter in the prior art are overcome.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (5)
1. A method for detecting aldehydes in a cigarette filter is characterized by comprising the following steps:
step one, collecting cigarette filters: collecting the cigarette filter tips after the smoking;
step two, pretreatment: cutting the filter tip, putting the cut filter tip into a headspace bottle, and adding a certain amount of extractant;
step three, analysis and detection: balancing the sample for a period of time by using a static headspace instrument, and detecting the content of aldehyde substances in the sample by using a gas chromatography-mass spectrometry;
the extraction agent comprises an auxiliary agent and a deuterated internal standard, the concentration of the deuterated internal standard is 1-5 mg/mL, and the volume of a deuterated internal standard solution is 5-50 mu L;
during gas chromatography detection, the temperature rise program of the chromatographic column is as follows: the initial temperature is 30 to 40 ℃, and the temperature is kept for 1 to 3min; then heating to 80 to 100 ℃ at a heating speed of 2 to 4 ℃/min; heating to 180 to 220 ℃ at a speed of 15 to 20 ℃/min, and keeping for 5 to 8 min;
the aldehyde substances are formaldehyde, acetaldehyde, propionaldehyde, acrolein and crotonaldehyde;
the auxiliary agent is glyceryl triacetate;
in step three, the gas chromatography was performed using a Perkin Elmer Elite-624 column, 60 m.times.0.32 mm.times.1.8. Mu.m.
2. The detection method according to claim 1, wherein in the first step, the number of the cigarette filters is 2 to 5.
3. The detection method according to claim 1, wherein the deuterated internal standard is benzene-D6 or acetone-D3.
4. The detection method according to claim 1, wherein in step three, the headspace condition is: the equilibrium temperature is 80 to 120 ℃, and the equilibrium time is 10 to 40min.
5. The detection method according to claim 1, wherein in the third step, the ion source is an electron bombardment source, the ion source temperature is 200 to 280 ℃, and the ion transport line temperature is 200 to 280 ℃ during mass spectrometry.
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