CN113341017A - Method for analyzing chemical components in main stream smoke components of cigarettes - Google Patents
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Abstract
The invention provides a method for analyzing chemical components in main stream smoke components of cigarettes, which comprises the following steps: the method comprises the following steps of (1) collecting, extracting, concentrating and carrying out gradient elution on main stream smoke of cigarettes to obtain component samples; firstly, a one-dimensional gas chromatography/olfactory discrimination method is adopted for analysis, and then a center cutting two-dimensional gas chromatography-mass spectrometry/olfactory discrimination method is adopted for qualitative and quantitative analysis so as to determine the required components. The invention further provides an analysis device for chemical components in the main stream smoke components of the cigarette and application of the analysis device. The invention provides an analysis method of chemical components in main stream smoke components of cigarettes, which establishes a two-dimensional gas chromatography-mass spectrometry/olfactory discrimination technology and realizes accurate discrimination of key smell components of cigarette smoke.
Description
Technical Field
The invention belongs to the technical field of chemical odor analysis in cigarette smoke, relates to a method for analyzing chemical components in cigarette mainstream smoke, and particularly relates to a method for analyzing odor components in cigarette mainstream smoke by adopting a two-dimensional gas chromatography-mass spectrometry/olfactory discrimination technology.
Background
The cigarette smoke components are complex, the fragrance components are numerous, and the cigarette smoke components are the result of the synergistic effect of a plurality of aroma substances, particularly the composition of key aroma components in the smoke is one of the most direct factors influencing the cigarette quality and is also a significant factor causing the cigarette quality difference. Therefore, the composition and the odor characteristics of the odor components in the cigarette smoke and the influence on the cigarette smoke are clear, and the cigarette filter has important supporting functions on improving the cigarette quality and in cigarette flavoring.
The aroma components of the cigarette smoke can be divided into acidic, weakly acidic, neutral and alkaline components according to the acid-base properties of substances, and researches show that the acidic odor components in the mainstream smoke can adjust the pH value of the smoke and reduce the irritation in the smoking process of the cigarette; the weak acidic components endow the cigarette with special smell, and most of the neutral flavor components have respective aroma characteristics; the alkaline aroma component has strong burnt aroma and baking aroma.
At present, more researches on cigarette mainstream smoke are focused on qualitative analysis of compounds, less researches on odorous compounds are carried out, the technology commonly used for analyzing the odorous components mainly comprises a one-dimensional gas chromatography-smell identification (GC-O) technology and is widely applied to industries of food, essence, spices and the like.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide an analysis method for chemical components in main stream smoke components of cigarettes, which is based on two-dimensional chromatography, a central cutting two-dimensional gas chromatography-mass spectrometry/olfactory discrimination (MDGC-MS/O) analysis platform is set up, and two nonpolar and polar chromatographic columns are connected in series to separate and analyze complex cigarette smoke samples.
In order to achieve the above objects and other related objects, a first aspect of the present invention provides a method for analyzing chemical components in mainstream smoke of a cigarette, including: the method comprises the following steps of (1) collecting, extracting, concentrating and carrying out gradient elution on main stream smoke of cigarettes to obtain component samples; analyzing by adopting a one-dimensional gas chromatography/sniffing method, separating a sample by a first gas chromatography column, detecting by a hydrogen Flame Ion Detector (FID) and analyzing by sniffing by an sniffing port (ODP) respectively, and determining the cutting time period of the components to be detected; and then, carrying out qualitative and quantitative analysis by adopting a center cutting two-dimensional gas chromatography-mass spectrometry/olfactory discrimination method (MDGC-MS/O), separating the sample by a first gas chromatographic column after the sample is injected, separating by a second gas chromatographic column after a cutting time period is selected, and respectively carrying out detection by a mass spectrometer and olfactory discrimination analysis by an olfactory receptor (ODP) so as to determine the required components.
Preferably, the trapping is to smoke the cigarette after the cigarette is ignited, and the filter disc trapping mode is adopted to trap smoke particulate matters in the mainstream smoke of the cigarette.
More preferably, the suction is performed using a multi-tunnel carousel smoking machine.
More preferably, the filter is a cambridge filter.
Preferably, the extraction is at least one solvent extraction of the captured filter.
The number of solvent extractions may be 2. The solvent was extracted and soaked overnight.
More preferably, the solvent is added in an amount of 350-450mL/15 filter discs.
More preferably, the solvent is selected from one or more of ethyl acetate, methyl tert-butyl ether, n-hexane and diethyl ether.
More preferably, the solvent extraction is selected from one or more of soaking extraction, ultrasonic extraction and shaking extraction.
Further preferably, the time for soaking and extracting is 5-30 min.
Further preferably, the time of the ultrasonic extraction is 5-15min, preferably 10 min.
Further preferably, the shaking extraction time is 10-30 min.
Preferably, the concentration is reduced pressure concentration, the pressure of the reduced pressure concentration is 300-.
Preferably, the gradient elution is to sequentially perform acid washing, weak alkali washing and strong alkali washing on the concentrated solution obtained after concentration to respectively obtain a smoke alkaline component sample, an acidic component sample, a neutral component sample and a weakly acidic component sample.
More preferably, the gradient elution comprises the steps of:
1) adding a first acid solution into the concentrated solution for extraction, separating to obtain a first organic phase and a first water phase, adding the first water phase into a first alkali liquor, adjusting the pH value, extracting with an organic solvent, and concentrating the organic phase under reduced pressure to obtain a smoke alkaline component sample;
2) adding a second alkali solution into the first organic phase for extraction, separating to obtain a second organic phase and a second water phase, adding a second acid solution into the second water phase, adjusting the pH value, extracting with an organic solvent, and concentrating the organic phase under reduced pressure to obtain a flue gas acidic component sample;
3) adding a third alkali liquor into the second organic phase for extraction, separating to obtain a third organic phase and a third water phase, adding a third acid liquor into the third water phase, adjusting the pH value, extracting with an organic solvent, and concentrating the organic phase under reduced pressure to obtain a flue gas weakly acidic component sample;
4) and (4) decompressing and concentrating the third organic phase to obtain a neutral component sample of the smoke.
Further preferably, in the step 1), the first acid solution is an aqueous solution of sulfuric acid or hydrochloric acid with a mass fraction of 1-10%, preferably 5%.
Further preferably, in the step 2), the second alkali solution is a sodium bicarbonate aqueous solution with a mass fraction of 1-10%, and preferably 5%.
Further preferably, in the step 3), the third alkali solution is a sodium hydroxide aqueous solution with a mass fraction of 1-10%, and preferably 5%.
Further preferably, in the step 1), 2) or 3), the times of the first acid liquid extraction, the second alkaline liquid extraction and the third alkaline liquid extraction are all 2-4 times.
Further preferably, in the step 1), the first alkali solution is a 55-65% sodium hydroxide aqueous solution by mass fraction, and is preferably a 60% sodium hydroxide aqueous solution. Further preferably, in step 2) or 3), the second acid solution and the third acid solution are sulfuric acid aqueous solutions with mass fractions of 55-65%, and preferably 60%.
More preferably, in the step 1), the pH value is adjusted to be 11.5-12.5.
More preferably, in the step 2) or 3), the pH value is adjusted to be 1.5-2.5.
Further preferably, in the step 1), 2) or 3), the organic solvent used in the organic solvent extraction is diethyl ether, and the extraction times are all 2-4 times.
Further preferably, in the step 1), 2), 3) or 4), the pressure of the reduced pressure concentration is 300-.
Preferably, the first gas chromatography column is a non-polar gas chromatography column.
More preferably, the first gas chromatography column is selected from one of an SGE-BPX5 gas chromatography column or an Agilent DB-5ms gas chromatography column.
Preferably, when the first gas chromatography column is used for separation, the temperature rise program of the column oven is as follows: the initial temperature is kept at 40-60 ℃ for 2min, and the temperature is increased to 220 ℃ at the heating rate of 3-6 ℃/min and kept for 10-15 min.
Preferably, the cutting time period is determined as a retention time period in a gas chromatogram obtained by detecting a corresponding component by a hydrogen Flame Ion Detector (FID) corresponding to an odor component to be detected, which is determined by an olfactory mouth (ODP) olfactory discrimination analysis.
And the cutting time period is selected to set a retention time period between peak valleys in the gas chromatogram as a cutting time period, wherein a wider cutting time period is set in a region with fewer chromatographic peaks and lower content, and a narrower cutting time period is set in the opposite direction.
Preferably, the second gas chromatography column is a polar gas chromatography column.
More preferably, the second gas chromatography column is selected from one of a Solgel-Wax gas chromatography column or an Agilent DB-Wax gas chromatography column.
Preferably, when the second gas chromatography column is used for separation, the temperature rise program of the column oven is as follows: keeping the initial temperature at 40-60 ℃ for 2min, heating to the temperature required by the cutting time period at the heating rate of 3-6 ℃/min, cooling to 45-50 ℃ at the cooling rate of 80-120 ℃/min, keeping for 1-5 min, and starting heating to 230 ℃ at 2-5 ℃/min, and keeping for 10-20 min.
Preferably, the flow rate of the first gas chromatographic column or the second gas chromatographic column is 1-2 mL/min.
Preferably, the detection conditions of the mass spectrometer are as follows: the ionization source energy is 70 eV; the ion source temperature is 230 ℃; the transmission line temperature is 235 ℃; the scanning mode is scan; the scanning range is 35-300 m/z; the auxiliary heating transfer line (sniffing ODP) temperature was 240 ℃.
Preferably, the qualitative method for detecting by the mass spectrometry detector is selected from one or two of NIST mass library retrieval compound structural formula qualitative determination and Wiely mass library retrieval compound structural formula qualitative determination.
Preferably, the sniff-port (ODP) sniff analysis is used for recording smell information and sniff time.
More preferably, the scent information includes scent characteristics and scent intensity.
The olfactory discrimination method (Odor) is conventionally used in the tobacco field, and is characterized in that an olfactory discrimination group consisting of sniffers trained by a system carries out olfactory discrimination analysis on chemical components in main stream smoke components of cigarettes through artificial sensory olfactory discrimination.
The odor is characterized by a direct descriptive perception of the senses of the sniffing person. The odor intensity is the strength degree of the odor which is sensed by the sniffing person in the sense, and is generally a value system comprising 0: no smell; 1: weak; 2: performing the following steps; 3: is strong.
Preferably, in the olfactory analysis by sniffing (ODP), the component sample is diluted with a solvent selected from one or more of methanol, ethanol, methyl tert-butyl ether or diethyl ether.
More preferably, the dilution factor of the component sample is 2n、3nOr 4nStepwise dilution was performed for the gradient.
The component samples can be diluted by a solvent and then subjected to subsequent analysis, and when the sample is diluted until a person smelling the compound cannot perceive the odor, the dilution factor of the sample is the dilution factor of the compound. The larger the dilution factor, the more the odor contribution of the odor substance to the sample, the key odor compound of the sample.
The second aspect of the invention provides an analysis device for chemical components in mainstream smoke components of cigarettes, as shown in fig. 1, comprising a column incubator, a hydrogen Flame Ion Detector (FID) and a mass spectrometer, wherein the column incubator is internally provided with a first gas chromatography column and a second gas chromatography column, and the column incubator is provided with a sample inlet and a sniffing port; the sample inlet end of the first gas chromatographic column is communicated with the sample inlet, and the sample outlet end of the first gas chromatographic column is respectively communicated with the sample inlet end of the second gas chromatographic column, a hydrogen Flame Ion Detector (FID) and a smell identification port; and the sample outlet end of the second gas chromatographic column is respectively communicated with the sniffing port and the mass spectrum detector.
Preferably, a first three-way connector is arranged at the sample outlet end of the first gas chromatographic column, the first three-way connector is connected with a second three-way connector, and a four-way connector is arranged at the sample outlet end of the second gas chromatographic column; the first interface of first three way connection ware is linked together with the appearance end of appearing of first gas chromatography column, the second interface of first three way connection ware and the appearance end of second gas chromatography column communicate, the third interface of first three way connection ware through the pipeline with the first interface of second three way connection ware is linked together, the second interface of second three way connection ware through the pipeline and is linked together with hydrogen Flame Ion Detector (FID), the third interface of second three way connection ware through the pipeline with the first interface of four way connection ware is linked together, the second interface of four way connection ware through the pipeline with smell distinguish the mouth and be linked together, the third interface of four way connection ware is linked together with the appearance end of second gas chromatography column, the fourth interface of four way connection ware through the pipeline and mass spectrum detector are linked together.
More preferably, a pipeline between the first three-way connector and the sample injection end of the second gas chromatography column is provided with carbon dioxide (CO)2) And a central cutting valve is arranged on a pipeline between the first three-way connector and the second three-way connector.
Further preferably, the carbon dioxide (CO)2) The opening time of the valve is 2-5 min before the central cutting valve is opened.
More preferably, a wet gas valve is arranged on a pipeline between the four-way connector and the sniffing port.
The third aspect of the invention provides application of the analysis device for the chemical components in the mainstream smoke components of the cigarettes in the analysis of the chemical components in the mainstream smoke components of the cigarettes.
As mentioned above, the method for analyzing chemical components in mainstream smoke components of cigarettes provided by the invention has the following beneficial effects:
(1) the invention provides an analysis method of chemical components in main stream smoke components of cigarettes, which comprises the steps of firstly adopting a one-dimensional gas chromatography/olfactory discrimination method to carry out analysis, then adopting a center cutting two-dimensional gas chromatography-mass spectrometry/olfactory discrimination method (MDGC-MS/O) to carry out qualitative and quantitative analysis for analyzing the smell components of the main stream smoke, improving the separation capability and detection sensitivity of a complex system by connecting two columns with different polarities in series, shortening the olfactory time by setting segmented cutting olfactory discrimination, improving the accuracy and realizing accurate discrimination of the smell components of the cigarette smoke.
(2) According to the method for analyzing the chemical components in the mainstream smoke components of the cigarettes, provided by the invention, the analysis conditions of the second chromatographic column are determined through the odor characteristics and the peak-appearing time of the first chromatographic column, so that the method is more selective and can be used for efficiently analyzing the compounds.
(3) Compared with one-dimensional chromatographic analysis, the method for analyzing the chemical components in the mainstream smoke components of the cigarettes has the advantages that the complex samples are well separated, the separation degree is improved, and the method is suitable for analyzing the odor of the complex samples.
(4) The method for analyzing the chemical components in the mainstream smoke components of the cigarettes effectively removes substance interference of odorless high-content compounds, and can realize detection of trace but odorous compounds.
(5) The method for analyzing the chemical components in the main stream smoke components of the cigarettes provided by the invention is simple and strong in operability, and can effectively avoid long-time smell and improve accuracy by segmented cutting.
Drawings
FIG. 1 is a schematic structural diagram of an analysis device for chemical components in mainstream smoke components of cigarettes in the invention.
FIG. 2 shows the mass spectrum of the smoke acid component sample in the cutting time period of 1.9-13.25min in the embodiment 2 of the invention.
FIG. 3 shows a mass spectrum of a smoke acid component sample obtained by conventional GC-MS detection in comparative example 1 of the present invention.
FIG. 4 is a mass spectrum of a weakly acidic component sample of flue gas in the cutting time period of 9-17.4min in example 6 of the present invention.
Reference numerals
1 column incubator
2 hydrogen flame ion detector
3 mass spectrum detector
4 sample inlet
5 Bixie Biao
6 first three-way connector
61 first interface of first three-way connector
62 second interface of first three-way connector
63 third interface of the first three-way connector
7 second three-way connector
71 first interface of second three-way connector
72 second interface of second three-way connector
73 third interface of second three-way connector
8 four-way connector
First interface of 81 four-way connector
Second interface of 82 four-way connector
Third interface of 83 four-way connector
Fourth interface of 84 four-way connector
9 carbon dioxide valve
10 center cutting valve
11 first gas chromatography column
12 second gas chromatography column
13 humid gas valve
Detailed Description
The present invention is further illustrated below with reference to specific examples, which are intended to be illustrative only and not to limit the scope of the invention.
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
The invention provides an analysis device for chemical components in mainstream smoke components of cigarettes, which comprises a column incubator, a hydrogen Flame Ion Detector (FID) and a mass spectrum detector, wherein the column incubator is internally provided with a first gas chromatographic column and a second gas chromatographic column and is provided with a sample inlet and a smell identification port; the sample inlet end of the first gas chromatographic column is communicated with the sample inlet, and the sample outlet end of the first gas chromatographic column is respectively communicated with the sample inlet end of the second gas chromatographic column, a hydrogen Flame Ion Detector (FID) and a smell identification port; and the sample outlet end of the second gas chromatographic column is respectively communicated with the sniffing port and the mass spectrum detector.
In the device for analyzing chemical components in the mainstream smoke components of the cigarettes, the column temperature box, the hydrogen Flame Ion Detector (FID) and the mass spectrometer are all components of a gas chromatography-mass spectrometer which is used conventionally. Specifically, the gas chromatography-mass spectrometer is a 7890B/5977AGC-MS spectrometer.
In the device for analyzing chemical components in mainstream smoke components of cigarettes, as shown in fig. 1, a first three-way connector is arranged at a sample outlet end of a first gas chromatography column, the first three-way connector is connected with a second three-way connector, and a four-way connector is arranged at a sample outlet end of a second gas chromatography column; the first interface of first three way connection ware is linked together with the appearance end of appearing of first gas chromatography column, the second interface of first three way connection ware and the appearance end of second gas chromatography column communicate, the third interface of first three way connection ware through the pipeline with the first interface of second three way connection ware is linked together, the second interface of second three way connection ware through the pipeline and is linked together with hydrogen Flame Ion Detector (FID), the third interface of second three way connection ware through the pipeline with the first interface of four way connection ware is linked together, the second interface of four way connection ware through the pipeline with smell distinguish the mouth and be linked together, the third interface of four way connection ware is linked together with the appearance end of second gas chromatography column, the fourth interface of four way connection ware through the pipeline and mass spectrum detector are linked together.
The first three-way connector and the second three-way connector are both conventional three-way switching valves, and the four-way connector is a conventional four-way switching valve.
In a specific embodiment, as shown in fig. 1, a pipeline between the first three-way connector and the sample inlet end of the second gas chromatography column is provided with carbon dioxide (CO)2) A valve, the first three-way connector and the secondAnd a central cutting valve is arranged on a pipeline between the three-way connectors. Said carbon dioxide (CO)2) The valve sleeve is sleeved on a pipeline between the first three-way connector and the sample introduction end of the second gas chromatographic column and used for cooling the pipeline.
The central cutting valve can be used for adjusting the first three-way connector, when the central cutting valve is opened, the set pressure is high, and the analytical components enter the second gas chromatographic column through the first interface and the second interface of the first three-way connector; when the central cutting valve is closed, the set pressure is small, and the analysis component enters the second three-way connector through the first interface and the third interface of the first three-way connector.
Carbon dioxide (CO) as described above2) The valve is a conventionally used pressure valve. The above-described center-cut valve is a conventionally used gas valve.
In a further preferred embodiment, the carbon dioxide (CO)2) The opening time of the valve is 2-5 min before the central cutting valve is opened.
In a specific embodiment, as shown in fig. 1, a humid gas valve is arranged on the pipeline between the four-way connector and the sniffing port. The moist air valve is always in an open state and is used as compensation air to avoid nose drying of people.
The above-mentioned wet gas valve is a conventionally used gas valve.
In the device for analyzing chemical components in mainstream smoke components of cigarettes, as shown in fig. 1, a sample is firstly input into a first gas chromatographic column through an injection port to separate the obtained components, and carbon dioxide (CO) is turned off2) The pressure of the valve and the center cutting valve enables the components to sequentially flow into the hydrogen flame ion detector through the first interface of the first three-way connector, the third interface of the first three-way connector, the first interface of the second three-way connector and the second interface of the second three-way connector, and simultaneously enables the components to sequentially flow into the sniffing port through the first interface of the first three-way connector, the third interface of the first three-way connector, the first interface of the second three-way connector, the third interface of the second three-way connector, the first interface of the four-way connector and the second interface of the four-way connector; then the sample is input into the first gas phase color through the sample inletSeparating the obtained components by opening carbon dioxide (CO) when the desired cutting time is reached2) And opening the pressure of the central cutting valve to enable the components in the cutting time period to sequentially flow into a second gas chromatographic column through a first interface of a first three-way connector and a second interface of the first three-way connector for separation, then flow into a mass spectrum detector through a third interface of a four-way connector and a fourth interface of the four-way connector, and simultaneously flow into an olfactory discrimination port through the third interface of the four-way connector and the second interface of the four-way connector.
Example 1
On a multi-channel rotary disc type smoking machine, smoking is carried out after the cigarette is ignited, and smoke particle phase substances in mainstream smoke of the Cambridge filter sheet cigarette are adopted to obtain the Cambridge filter sheet captured substances. Adding 400mL of diethyl ether into the captured substance of 15 Cambridge filter sheets, soaking and extracting for 10min, performing ultrasonic extraction for 10min, performing shake extraction for 20min, and standing for one day to obtain an extract. The extraction was repeated again and combined to give 800mL of extract. Concentrating the extractive solution under reduced pressure to 100mL to obtain concentrated solution, wherein the concentration under reduced pressure is 800mbar, and the water bath temperature is 30 deg.C.
Adding 150mL of H with the mass fraction of 6% into 100mL of concentrated solution2SO4And extracting the aqueous solution serving as a first acid solution for 3 times, and separating to obtain a first organic phase and a first water phase. The first organic phase was added to 150mL of 5% NaHCO3And extracting the aqueous solution serving as a second alkali solution for 3 times, and separating to obtain a second organic phase and a second water phase. And (3) combining the second water phases, adding a 60% sulfuric acid aqueous solution by mass fraction to adjust the pH value to 2, adding 200mL of diethyl ether to extract for 3 times, and then concentrating the organic phase under reduced pressure to 20mL to obtain a flue gas acidic component sample.
Example 2
The acidic components in the flue gas obtained in example 1 are analyzed by the analyzer shown in fig. 1, and first, a one-dimensional gas chromatography/sniffing method is used for analysis, 3mL of the acidic components in the flue gas are separated by a first gas chromatography column to obtain chemical components, which are respectively detected by a Flame Ionization Detector (FID) and sniffed by an sniffing port (ODP), and then, the odor information and the sniffing time are recorded, and the cutting time period (i.e., retention time) of the acidic components in the flue gas to be detected is determined. Wherein the first gas chromatographic column is SGE-BPX5 gas chromatographic column (30m × 0.53mm id × 0.5 μm). When the first gas chromatographic column is separated, the temperature rise program of the column temperature box is as follows: the initial temperature is kept at 40 ℃ for 2min, and the temperature is increased to 220 ℃ at the heating rate of 4 ℃/min and kept for 10 min. The results of the one-dimensional gas chromatography/sniffing analysis and sniffing are shown in table 1.
TABLE 1
Then, the flue gas acid component sample is qualitatively and quantitatively analyzed by adopting a center cutting two-dimensional gas chromatography-mass spectrometry/olfactory discrimination method (MDGC-MS/O), namely, the flue gas acid component sample is re-injected and is separated by a first gas chromatographic column, and then the compound separated by the first gas chromatographic column in a certain time period is selectively cut into a second gas chromatographic column for analysis by controlling the opening and closing of a center cutting valve. According to the cutting principle, the selected cutting time period is as follows: 1.9-13.25min, 13.25-19.75min, 19.75-32.5min, and opening the carbon dioxide valve 2min before cutting time. And separating by a second gas chromatographic column after selecting the cutting time period, and carrying out olfactory analysis on the separated sample by an olfactory receptor (ODP) to record odor information and olfactory time. And detecting by a mass spectrum detector to determine the required components. Wherein, the separation conditions of the first gas chromatographic column are the same as those of a gas chromatography/olfactory discrimination method. The second gas chromatography column was a Solgel-WAX column (30 m.times.0.53 mm id. times.0.5 μm). During the separation of the second gas chromatographic column, the temperature rise program of the column oven is shown in table 2 and is as follows: keeping the initial temperature at 40 ℃ for 2min, heating to the temperatures of 85, 111 and 162 ℃ required by the cutting time period at the heating rate of 4 ℃/min, cooling to 45 ℃ at the cooling rate of 120 ℃/min for 2min, and starting heating to 230 ℃ at the temperatures of 2, 2 and 3 ℃/min for 10, 10 and 15 min. The detection conditions of the mass spectrum detector are as follows: the ionization source energy is 70 eV; the ion source temperature is 230 ℃; the transmission line temperature is 235 ℃; the scanning mode is scan; the scanning range is 35-300 m/z, and the temperature of the auxiliary heating transmission line (sniffing ODP) is 240 ℃.
TABLE 2
Determining the structure of the three-section cutting compound of the smoke acid component sample, specifically referring to the mass spectrogram of the first section 1.9-13.25min cutting section shown in figure 2. After determining the structure and the characteristic odor of the three-section cutting compound of the smoke acidic component sample, diluting the acidic sample with ether step by step, respectively carrying out sniffing and Olving (ODP) analysis on the acidic sample with different concentrations in three cutting sections, and recording the change condition of odor substances in the sample under different concentration gradients. Dilution factor is 2nAnd (3) diluting until the sample is diluted to the extent that the smell of the compound cannot be perceived by a sniffer, wherein n is the dilution factor of the compound, and compounds with larger dilution factors n are key smell components of acidic samples. Wherein, the analysis results of the key odor components of the second section 13.25-19.75min cutting section are shown in Table 3.
TABLE 3
As can be seen from Table 3, 17 acidic components in the 13.25-19.75min cut segment of the smoke acidic component sample are detected and smelled by mass spectrometry, the largest dilution factor in Table 2 is caproic acid, and the dilution factors such as 64, 3-methylvaleric acid, 4-methylvaleric acid, heptanoic acid, nonanoic acid and the like are 16, so that caproic acid can represent key odor components of the cut segment and is expressed as slightly acidic and fatty gas.
Comparative example 1
A sample of acidic components in flue gas obtained in example 1 was subjected to measurement by conventional GC-MS/O, and the chemical components obtained after separation by a gas chromatographic column were detected by GC-MS and analyzed by sniffing (ODP). Wherein the gas chromatography column is DB-wax gas chromatography column (60m × 0.32mm id × 0.25 μm). When the gas chromatographic column is used for separation, the temperature rising procedure of the column temperature box is as follows: the initial temperature is 60 ℃, the temperature is increased to 240 ℃ at the heating rate of 3 ℃/min and is kept for 20 min. The detection conditions of the mass spectrum detector are as follows: the ionization source energy is 70 eV; the ion source temperature is 230 ℃; the transmission line temperature is 235 ℃; the scanning mode is scan; the scanning range is 35-300 m/z, and the temperature of the auxiliary heating transmission line (sniffing ODP) is 240 ℃. The mass spectrogram of the specific component detection of the smoke acid component sample is shown in figure 3.
Comparing fig. 3 with fig. 2 in example 2, the time for analyzing the flue gas acidic component sample by the conventional method in comparative example 1 is longer, which results in too long smell time, not high enough sensitivity, and poor separation degree, co-effluent exists, which affects smell identification, and the operability and accuracy for the flue gas acidic component sample are far lower than those of the determination method in example 2.
Example 3
The first water phase obtained in the separation in the example 1 is added with a sodium hydroxide aqueous solution with the mass fraction of 60% as a first alkali liquor, the pH value is adjusted to 12, 200mL of diethyl ether is added for extraction for 3 times, the organic phase is concentrated to 20mL under the reduced pressure, the reduced pressure concentration condition is 800mbar, the water bath temperature is 30 ℃, and a smoke alkaline component sample is obtained.
Example 4
And (3) separating to obtain a second organic phase in the example 1, adding a 5% sodium hydroxide aqueous solution serving as a third alkali liquor for extraction, extracting for 3 times, and separating to obtain a third organic phase and a third water phase. And combining the third water phases, adding a 60% sulfuric acid aqueous solution by mass fraction to adjust the pH value to 2, adding 200mL of diethyl ether to extract for 3 times, concentrating the organic phase to 20mL under reduced pressure under the condition of 800mbar and 30 ℃ of water bath, and obtaining a weakly acidic component sample of the flue gas.
Example 5
And (3) concentrating the third organic phase obtained in the separation in the example 4 to 20mL under the reduced pressure of 800mbar and at the water bath temperature of 30 ℃ to obtain a neutral component sample in the smoke.
Example 6
The weakly acidic components in flue gas obtained in example 4 are analyzed by the analyzer shown in fig. 1, a one-dimensional gas chromatography/sniffing method is firstly used for analysis, 3mL of the weakly acidic components in flue gas are separated by a first gas chromatography column to obtain chemical components, the chemical components are respectively detected by a hydrogen Flame Ion Detector (FID) and analyzed by sniffing through an sniffing port (ODP), odor information and sniffing time are recorded, and the cutting time period (namely retention time) of the acidic components in flue gas to be detected is determined. Wherein the first gas chromatographic column is SGE-BPX5 gas chromatographic column (30m × 0.53mm id × 0.5 μm). When the first gas chromatographic column is separated, the temperature rise program of the column temperature box is as follows: the initial temperature is kept at 45 ℃ for 2min, and the temperature is increased to 220 ℃ at the temperature rising speed of 5 ℃/min and kept for 15 min.
Then, the flue gas acidic component sample is qualitatively and quantitatively analyzed by adopting a center-cut two-dimensional gas chromatography-mass spectrometry/olfactory discrimination method (MDGC-MS/O), namely, the flue gas acidic component sample is re-injected and is separated by a first gas chromatographic column, and the compound separated by the first gas chromatographic column in a certain time period is selectively cut into a second gas chromatographic column for analysis by controlling the opening and closing of a center cutting valve. According to the cutting principle, the selected cutting time period is as follows: 9-17.4min, 17.4-20.2min, 20.2-25.2min, 25.2-30.4min, and opening the carbon dioxide valve 2min before cutting time. And separating by a second gas chromatographic column after selecting the cutting time period, and carrying out olfactory analysis on the separated sample by an olfactory receptor (ODP) to record odor information and olfactory time. And detecting by a mass spectrum detector to determine the required components. Wherein, the separation conditions of the first gas chromatographic column are the same as those of a gas chromatography/olfactory discrimination method. The second gas chromatography column was a Solgel-WAX column (30 m.times.0.53 mm id. times.0.5 μm). When the second gas chromatographic column is used for separation, the temperature rise program of the column temperature box is as follows: keeping the initial temperature at 45 ℃ for 2min, respectively heating to the temperatures 122, 136, 161 and 187 required by the cutting time period at the heating rate of 5 ℃/min, then cooling to 80 ℃ at the cooling rate of 120 ℃/min for 2min, and then respectively starting to heat to 230 ℃ at the temperatures of 3, 3 and 4 ℃/min for 20, 25 and 25 min. The detection conditions of the mass spectrum detector are as follows: the ionization source energy is 70 eV; the ion source temperature is 230 ℃; the transmission line temperature is 235 ℃; the scanning mode is scan; the scanning range is 35-300 m/z, and the temperature of the auxiliary heating transmission line (sniffing ODP) is 240 ℃.
Determining the structure of the three-section cutting compound of the smoke weakly acidic component sample, specifically referring to a mass spectrogram of a first section 9-17.4min cutting section as shown in figure 4. After determining the structure and the characteristic odor of the three-section cut compound of the flue gas weakly acidic component sample, diluting the flue gas weakly acidic component sample with ether step by step, respectively carrying out sniffing and olfactive analysis of three cutting sections on the flue gas weakly acidic component samples with different concentrations, and recording the change condition of odor substances in the samples under different concentration gradients. Dilution factor is 2nAnd (3) diluting until the sample is diluted to the extent that a smell of the compound cannot be perceived by a sniffer, wherein n is a dilution factor of the compound, and the compound with the larger dilution factor n is a key smell component of the sample of the weakly acidic components in the smoke. Wherein, the analysis results of the key odor components of the first 9-17.4min cut segment are shown in Table 4.
TABLE 4
As can be seen from Table 4, the weakly acidic components in the smoke have higher contents of guaiacol, 2-methoxy-4-methylphenol, p-methylphenol and m-methylphenol, which are more representative of the key odor of the cut segment and are represented by sweet, fragrant, incense and phenolic odor.
In conclusion, the method for analyzing chemical components in main stream smoke components of cigarettes provided by the invention establishes a two-dimensional gas chromatography-mass spectrometry/sniffing technology, and realizes accurate identification of key smell components of cigarette smoke. Therefore, the invention effectively overcomes various defects in the prior art and has high industrial utilization value.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (10)
1. A method for analyzing chemical components in mainstream smoke components of cigarettes comprises the following steps: the method comprises the following steps of (1) collecting, extracting, concentrating and carrying out gradient elution on main stream smoke of cigarettes to obtain component samples; firstly, analyzing by adopting a one-dimensional gas chromatography/sniffing method, separating a sample by a first gas chromatography column, and respectively detecting by a hydrogen flame ion detector and carrying out sniffing analysis to determine the cutting time period of the components to be detected; and then, carrying out qualitative and quantitative analysis by adopting a center cutting two-dimensional gas chromatography-mass spectrometry/sniffing method, separating the sample by a first gas chromatographic column, selecting a cutting time period, separating by a second gas chromatographic column, and respectively carrying out detection by a mass spectrometer and sniffing mouth sniffing analysis to determine the required components.
2. The method of claim 1, wherein the obtaining of the component sample comprises any one or more of the following conditions:
1) the trapping is to smoke the cigarette after the cigarette is ignited, and trap smoke particulate matters in the mainstream smoke of the cigarette in a filter disc trapping mode;
2) the extraction is to carry out at least one time of solvent extraction on the trapped filter disc;
3) the concentration is reduced pressure concentration, the pressure of the reduced pressure concentration is 300-;
4) the gradient elution is to carry out acid washing, weak alkali washing and strong alkali washing on concentrated solution obtained after concentration in sequence to respectively obtain a smoke alkaline component sample, an acidic component sample, a neutral component sample and a weak acidic component sample.
3. The method of claim 1, wherein the first gas chromatography column is a non-polar gas chromatography column; when the first gas chromatographic column is separated, the temperature rise program of the column temperature box is as follows: the initial temperature is kept at 40-60 ℃ for 2min, and the temperature is increased to 220 ℃ at the heating rate of 3-6 ℃/min and kept for 10-15 min.
4. The method of claim 1, wherein the second gas chromatography column is a polar gas chromatography column; when the second gas chromatographic column is used for separation, the temperature rise program of the column temperature box is as follows: keeping the initial temperature at 40-60 ℃ for 2min, heating to the temperature required by the cutting time period at the heating rate of 3-6 ℃/min, cooling to 45-50 ℃ at the cooling rate of 80-120 ℃/min, keeping for 1-5 min, and starting heating to 230 ℃ at 2-5 ℃/min, and keeping for 10-20 min.
5. The method for analyzing chemical components in mainstream smoke components of cigarettes according to claim 1, wherein the detection conditions of the mass spectrometer are as follows: the ionization source energy is 70 eV; the ion source temperature is 230 ℃; the transmission line temperature is 235 ℃; the scanning mode is scan; the scanning range is 35-300 m/z; auxiliary heating transmission line, smelling ODP temperature of 240 ℃.
6. The method of claim 1, wherein the breath-sniff analysis is performed by diluting the component sample with a solvent selected from one or more of methanol, ethanol, methyl tert-butyl ether and diethyl ether.
7. The device for analyzing the chemical components in the mainstream smoke components of the cigarettes is characterized by comprising a column incubator (1), a hydrogen flame ion detector (2) and a mass spectrum detector (3), wherein a first gas chromatographic column (11) and a second gas chromatographic column (12) are arranged in the column incubator (1), and a sample inlet (4) and an olfactory discrimination port (5) are arranged on the column incubator (1); the sample inlet end of the first gas chromatographic column (11) is communicated with the sample inlet (4), and the sample outlet end of the first gas chromatographic column (11) is respectively communicated with the sample inlet end of the second gas chromatographic column (12), the hydrogen flame ion detector (2) and the sniffing port (5); the sample outlet end of the second gas chromatographic column (12) is respectively communicated with the sniffing port (5) and the mass spectrum detector (3).
8. The device for analyzing the chemical components in the mainstream smoke components of the cigarettes according to claim 7, wherein a first three-way connector (6) is arranged at the sample outlet end of the first gas chromatography column (11), the first three-way connector (6) is connected with a second three-way connector (7), and a four-way connector (8) is arranged at the sample outlet end of the second gas chromatography column (7); the first interface (61) of the first three-way connector (6) is communicated with the sample outlet end of the first gas chromatographic column (11), the second interface (62) of the first three-way connector (6) is communicated with the sample inlet end of the second gas chromatographic column (12), the third interface (63) of the first three-way connector (6) is communicated with the first interface (71) of the second three-way connector (7) through a pipeline, the second interface (72) of the second three-way connector (7) is communicated with the hydrogen flame ion detector (2) through a pipeline, the third interface (73) of the second three-way connector (7) is communicated with the first interface (81) of the four-way connector (8) through a pipeline, the second interface (82) of the four-way connector (8) is communicated with the sniffing port (5) through a pipeline, the third interface (83) of the four-way connector (8) is communicated with the sample outlet end of the second gas chromatographic column (12), and a fourth interface (84) of the four-way connector (8) is communicated with the mass spectrum detector (3) through a pipeline.
9. The device for analyzing the chemical components in the mainstream smoke components of the cigarettes according to claim 8, wherein a carbon dioxide valve (9) is arranged on a pipeline between the first three-way connector (6) and the sample introduction end of the second gas chromatography column (12), and a central cutting valve (10) is arranged on a pipeline between the first three-way connector (6) and the second three-way connector (7); a wet gas valve (13) is arranged on a pipeline between the four-way connector (8) and the sniffing port (5).
10. Use of the device for analyzing chemical components in mainstream smoke of cigarettes according to any one of claims 7 to 9 in the analysis of chemical components in mainstream smoke of cigarettes.
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