CN108776184B - Method for detecting smoke components of heated non-combustible cigarette - Google Patents
Method for detecting smoke components of heated non-combustible cigarette Download PDFInfo
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- CN108776184B CN108776184B CN201810608156.6A CN201810608156A CN108776184B CN 108776184 B CN108776184 B CN 108776184B CN 201810608156 A CN201810608156 A CN 201810608156A CN 108776184 B CN108776184 B CN 108776184B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G01N30/64—Electrical detectors
- G01N30/66—Thermal conductivity detectors
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N2030/042—Standards
- G01N2030/045—Standards internal
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
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- G01N2030/062—Preparation extracting sample from raw material
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- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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Abstract
The invention provides a method for detecting smoke components of a cigarette which is not combusted when heated, which comprises the following steps: (1) preparing an internal standard solution; (2) preparing a standard working solution; (3) smoking and heating the non-combustible cigarettes, and collecting total particulate matters by using a Cambridge filter disc; (4) extracting total particulate matter; (5) gas chromatography determination; (6) and calculating the measurement result by a double internal standard method. The method established by the invention utilizes the traditional cigarette smoking machine to perform smoking of the heating non-combustion cigarette and capture of the total particulate matter, and does not need to heat a special smoking machine for the non-combustion cigarette; the simultaneous analysis and detection of 6 target components are completed in one experiment; the quantitative determination is carried out by adopting double internal standards, so that the quantitative result is more accurate; the method has the advantages of simple sample suction, total particulate matter trapping and extraction operations, convenient and fast gas chromatography determination, good stability, good linear correlation, good practicability, high sensitivity, good repeatability and the like.
Description
Technical Field
The invention relates to the technical field of tobacco detection, in particular to a method for detecting smoke components of a heated non-combustible cigarette, namely a method for simultaneously detecting the release amount of moisture, nicotine, glycerol, 1, 2-propylene glycol, glyceryl triacetate and menthol in the smoke of the heated non-combustible cigarette.
Background
The low-temperature cigarette, also called a heat-not-burn cigarette (heat-not-burn cigarette), heats the tobacco material by an external heat source, and the atomized medium, the flavor components and the additional flavor in the tobacco material generate smoke similar to the smoke of the traditional cigarette by heating, so that the consumers can obtain physiological satisfaction. The tobacco substances in the low-temperature cigarette are only heated without burning, and the heating temperature (250-350 ℃) is far lower than the burning temperature (800-900 ℃) of the traditional cigarette, so that the harmful components and the biological toxicity of the smoke are greatly reduced, and the side stream smoke and the environmental smoke are also greatly reduced.
The first development of cigarette without burning by heating was carried out by the international companies such as PM (Philip Morris). In recent years, a large number of cigarette products which do not burn with good heat have appeared in the international market, such as iQOS by PM, glo by BAT (British American Tobacco), and Ploom by JT (Japan Tobacco). The existing heating non-combustion cigarette comprises a filter tip and a tobacco section which are connected in sequence, the total length of the existing heating non-combustion cigarette is generally 45-55mm and is obviously shorter than the total length of the traditional cigarette (generally about 84 mm), wherein the length of the tobacco section is generally 15-20mm and is obviously shorter than the length of the tobacco section of the traditional cigarette (generally 50-64 mm). The existing heating non-combustion cigarette tobacco section mainly has two forms: orderly arranged thin slices or tobacco shreds, and disorderly arranged thin slices or tobacco shreds.
In order to ensure that the amount of smoke generated during smoking is similar to that of the traditional cigarette, a great amount of atomizing agents of glycerin and propylene glycol are loaded in the tobacco shreds of the cigarette which is not heated to burn. Because the tobacco shreds of the traditional cigarette are difficult to load a large amount of atomizing agents, the tobacco shreds of the cigarette which are not heated are generally all thin shreds obtained by a rolling method (or a thick paste method), or the main body of the cigarette is thin shreds obtained by the rolling method (or the thick paste method) and is supplemented with a small amount of tobacco shreds of the traditional cigarette for taste adjustment, so that the composition of the tobacco shreds of the cigarette which are not heated is greatly different from that of the tobacco shreds of the traditional cigarette; in order to achieve the effect of rapid cooling, the filter rod of the cigarette which is not heated and combusted is compounded with cooling materials which are not used in the traditional cigarette, so that the structure and the materials of the filter rod of the cigarette which is not heated and combusted are greatly different from those of the filter rod of the traditional cigarette; in addition, the heating temperature (250-350 ℃) is far lower than the combustion temperature (800-900 ℃) of the traditional cigarette, so the smoke composition of the cigarette which is not combusted is obviously different from the smoke of the traditional cigarette, the main components of the aerosol of the smoke of the cigarette which is not combusted comprise water, glycerol, 1, 2-propylene glycol, nicotine and the like, wherein the content ratio of the water, the glycerol and the 1, 2-propylene glycol is greatly changed compared with the smoke of the traditional cigarette, and the content of carbon monoxide, polycyclic aromatic hydrocarbon, tobacco-specific nitrosamine and the like is greatly reduced. The cigarette is heated and does not burn as a new thing which is just appeared, at present, no detection method aiming at smoke components of the heated and non-burned cigarette exists at home and abroad, and no special smoking machine for the heated and non-burned cigarette is generally verified and approved. The existing traditional cigarette smoke component analysis method generally classifies and detects components such as nicotine, moisture, polyols and the like, and is relatively time-consuming and labor-consuming, and the detection cost is high. The method of the invention fully utilizes the traditional cigarette smoking machine to perform smoking of the heating non-combustion cigarette and capture of total particulate matters, and simultaneously detects the moisture, nicotine, glycerol, 1, 2-propylene glycol, glyceryl triacetate and menthol in the smoke of the heating non-combustion cigarette.
The inventor of the invention researches and discovers that: the moisture in the aerosol of the smoke of the non-burning cigarette is heated, so that the smoking feelings of irritation, dryness, wetness and the like of a consumer during smoking are influenced; nicotine in the aerosol of the smoke of the cigarette is not combusted by heating, so that the physiological satisfaction of a consumer during smoking is directly influenced; the glycerol and the 1, 2-propylene glycol in the cigarette smoke aerosol are heated without being combusted, so that the smoke amount of a consumer during smoking is directly influenced; for a mint-flavored heating non-combustible cigarette, menthol in smoke aerosol directly influences the cool feeling of a consumer when smoking; the glyceryl triacetate is a colorless oily liquid, has a faint fruity and fleshy sweet taste, is also an important fragrance fixing agent in a main plasticizer and a fragrance perfume used in the production of cigarette filter sticks, and can influence the smoking taste of a consumer when the glyceryl triacetate in cigarette smoke aerosol is heated and is not combusted to a certain extent when the content is too high. Therefore, the method has important significance for detecting moisture, nicotine, glycerol, 1, 2-propylene glycol, glyceryl triacetate and menthol in the aerosol of the smoke of the heated non-combustible cigarette.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for detecting smoke components of a non-burning heated cigarette aiming at the non-burning heated cigarette, namely simultaneously detecting moisture, nicotine, glycerol, 1, 2-propylene glycol, glyceryl triacetate and menthol in the aerosol of the non-burning heated cigarette.
The technical scheme provided by the invention is as follows: a method for detecting smoke components of a heated non-combustible cigarette comprises the following steps:
(1) preparing an internal standard solution: weighing an internal standard sample n-butyl alcohol and 1, 3-butanediol, and fixing the volume by taking chromatographically pure isopropanol as a solvent to obtain an internal standard solution;
(2) preparation of standard working solution: weighing a certain amount of water, nicotine, glycerol, 1, 2-propylene glycol, glyceryl triacetate and menthol standard substance, and fixing the volume by taking chromatographic pure isopropanol as a solvent to obtain a standard stock solution; taking 5 or more extraction bottles, respectively adding standard stock solutions according to gradients, and then adding internal standard solutions with the same volume to prepare standard working solutions of grade 5 or more;
(3) smoking and heating the non-combustible cigarettes, and collecting total particulate matters by using a Cambridge filter disc;
(4) extracting the total particulate matters collected by the Cambridge filter in the step (3) by using the internal standard solution in the step (1) to obtain extract liquid of the total particulate matters;
(5) performing gas chromatography determination on the extract of the total particulate matter obtained in the step (4);
(6) and (3) calculating a measurement result by an internal standard method: and (3) carrying out quantitative determination by adopting double internal standards, wherein n-butyl alcohol is used as the internal standard for quantifying water, and 1, 3-butanediol is used as the internal standard for quantitatively determining nicotine, 1, 2-propylene glycol, glycerol, glyceryl triacetate and menthol.
Further, the step (3) of smoking and heating the non-burning cigarettes and collecting the total particulate matters comprises the following specific steps: after a smoking machine is prepared according to the traditional cigarette smoking method, the cigarette branch end of the cigarette which is not combusted by heating is inserted into a heating appliance, the mouth rod end is inserted into a holder of the smoking machine, a switch of the heating appliance is turned on for preheating, the smoking machine starts to smoke after the preheating time is reached, and total particulate matters are collected. The smoking machine may employ any one of a canadian deep smoking mode and an ISO standard smoking mode. The number of the suction ports is determined according to the suction mode and the heating time set by the heating appliance, and after the number of the suction ports is reached, the suction is completed.
Further, the specific steps of extracting the total particulate matters in the step (4) are as follows: and (3) placing the Cambridge filter disc trapping the total particulate matters in the step (3) into an extraction flask, adding 20-50mL of the internal standard solution in the step (1), fully oscillating for 0.5-2h, and filtering to obtain an extraction liquid of the total particulate matters.
Further, the gas chromatography detector in step (5) is a Thermal Conductivity Detector (TCD).
Further, the conditions of the gas chromatography in the step (5) are as follows: DB-1701 fused silica capillary chromatography column, size of 30m × 0.32mm × 1.0 μm; the temperature of a sample inlet is 260 ℃; temperature programming: maintaining the initial temperature at 80 deg.C for 2.5min, increasing to 250 deg.C at 40 deg.C/min, and maintaining for 3 min; helium is taken as carrier gas, the flow rate of the carrier gas is 1.5mL/min, and the constant flow mode is adopted; tail gas blowing helium gas 30 mL/min; the sample introduction volume is 1 mu L, and the split flow sample introduction is carried out, wherein the split flow ratio is 5: 1; the TCD detector temperature was 260 ℃.
Because no special smoking machine for heating non-burning cigarettes which is generally verified and approved exists at present, the invention performs smoking of the heating non-burning cigarettes and collection of total particulate matters on the traditional cigarette smoking machine. After a smoking machine is prepared according to the traditional cigarette smoking method, the cigarette branch end of the cigarette which is not combusted by heating is inserted into a heating appliance, the mouth rod end is inserted into a holder of the smoking machine, a switch of the heating appliance is turned on for preheating, the smoking machine starts to smoke after the preheating time is reached, and total particulate matters are collected. Wherein, in order to avoid the bending or breaking of the cigarette which is not burnt when being heated in the smoking process, the heating device can be manually supported or an object is placed under the heating device for supporting. The condition that the smoking machine adopts a Canadian deep suction mode is as follows: the suction capacity of each suction port is 55mL, the suction time of each suction port is 2 seconds, and the interval time between different suction ports is 28 seconds; the smoking machine adopts the conditions of an ISO standard smoking mode as follows: the volume of each suction port is 35mL, the suction time is 2 seconds, and the interval time between different suction ports is 58 seconds. Thus, the canadian deep draw mode may draw 2 puffs per minute and the ISO standard draw mode may draw 1 puff per minute. The heating device is set to be capable of continuously heating for 3-6 minutes, so that the Canadian deep suction mode can suck 6-12 mouths, the ISO standard suction mode can suck 3-6 mouths, and after the number of suction mouths is reached, the suction is finished.
Because the content difference of the water in the total particle phase substances is larger than that of nicotine, 1, 2-propylene glycol, glycerol, glyceryl triacetate and menthol, the method disclosed by the invention adopts double internal standards to carry out quantitative determination, and can ensure the quantitative accuracy of all target components, namely, the water is quantified by adopting n-butyl alcohol as the internal standard, and the nicotine, 1, 2-propylene glycol, glycerol, glyceryl triacetate and menthol are quantitatively determined by adopting 1, 3-butanediol as the internal standard. The retention time of the n-butanol and the 1, 3-butanediol are respectively 3.67min and 5.73min, no overlapping with other components of the sample, and good peak shape symmetry, and the method is suitable for being used as an internal standard.
The inventors examined the separation effect of four different polarity columns DB-1, DB-5, DB-1701 and DB-INNOWAX. 1, 2-propylene glycol and glycerol have short and fat peak types in DB-5 and DB-1 chromatographic columns, and a chromatographic peak tailing phenomenon occurs; nicotine and 1, 2-propanediol did not peak in the strongly polar DB-INNOWAX column. The DB-1701 chromatographic column can be adopted to better separate 6 target substances, the chromatographic peak types of all the target substances are sharp and symmetrical, no tailing exists, the analysis time is short, the target substances can be completely separated in only 10min, the detection sensitivity of low-concentration nicotine in the extract liquid can be met, the sample injection detection amount of high-concentration 1, 2-propylene glycol and glycerol is not overloaded, the extract liquid does not need to be further diluted, and therefore the DB-1701 chromatographic column is selected for sample analysis.
The chromatographic peak of 6 targets is characterized by retention time and peak height increase. Determining the target object by comparing the retention time of the standard sample in the gas chromatogram of glycerol, 1, 2-propylene glycol, glyceryl triacetate, nicotine, menthol and water and the retention time of the components in the gas chromatogram in the smoke extraction liquid; and simultaneously, confirming the target object by using a peak height increasing method, adding the standard sample into the extraction liquid, comparing with a sample chromatogram map without the standard sample, and if the peak height is increased, considering that the added standard sample and the component to be detected in the sample are the same compound.
Compared with the prior art, the method has the following excellent effects:
1. the invention provides a method for simultaneously detecting the release amounts of moisture, nicotine, glycerol, 1, 2-propylene glycol, glyceryl triacetate and menthol in smoke of a heated non-combustible cigarette.
2. The invention realizes simultaneous determination of 6 target components in the smoke of the cigarette without burning in one experiment, and saves the detection cost.
3. The method can fully utilize the traditional cigarette smoking machine to perform smoking of the heating non-combustion cigarette and capture the total particulate matter, and does not need to heat a special smoking machine for the non-combustion cigarette.
4. The method adopts double internal standards for quantitative determination, namely, the normal butanol is used as the internal standard for quantitative determination of water, and the 1, 3-butanediol is used as the internal standard for quantitative determination of nicotine, 1, 2-propylene glycol, glycerol, glyceryl triacetate and menthol, so that the quantitative result is more accurate.
5. The method has the advantages of simple sample suction, total particulate matter trapping and extraction operation, convenient and fast gas chromatography determination, good stability, better linear correlation and good practicability.
6. The method has high sensitivity and good repeatability. The detection limits of water, nicotine, glycerol, 1, 2-propylene glycol, glyceryl triacetate and menthol are respectively 0.63 mg/count, 0.035 mg/count, 0.059 mg/count, 0.048 mg/count, 0.046 mg/count and 0.031 mg/count, the standard recovery rate is 95.1-109.2%, and the relative standard deviation is 1.77-4.28%.
Drawings
FIG. 1 is a chromatogram of a standard sample;
FIG. 2 is a chromatogram of a sample of example 1 of the present invention.
The reference numerals in the figures are as follows: 1. water; 2. n-butanol; 1, 2-propanediol; 4.1, 3-butanediol; 5. glycerol; 6. menthol; 7. glyceryl triacetate; 8. nicotine.
Detailed Description
The invention is further illustrated with reference to specific embodiments and figures.
Example 1
(1) Preparing an internal standard solution: accurately weighing 2.000g of normal butanol (the purity is more than or equal to 99%) and 0.2000g of 1, 3-butanediol (the purity is more than or equal to 99%) of an internal standard sample, and taking chromatographic pure isopropanol as a solvent to fix the volume in a 1000mL volumetric flask to obtain an internal standard solution; the concentration of the n-butanol serving as an internal standard substance in the internal standard solution is 2mg/mL, and the concentration of the 1, 3-butanediol is 0.2 mg/mL.
(2) Preparation of standard working solution: accurately weighing 6.000g of pure water, 3.000g of a glycerol standard substance (the purity is more than or equal to 99%), 0.6000g of a nicotine standard substance (the purity is more than or equal to 99%), 0.6000g of a 1, 2-propylene glycol standard substance (the purity is more than or equal to 99%), 0.6000g of a glyceryl triacetate standard substance (the purity is more than or equal to 99%), and 0.6000g of a menthol standard substance (the purity is more than or equal to 99%), and taking chromatographic pure isopropanol as a solvent to be fixedly contained in a 100mL volumetric flask to obtain a standard stock solution, wherein the concentration of water is 60mg/mL, the concentration of glycerol is 30mg/mL, and the concentration of other substances is 6 mg/mL; and (3) taking 5 extraction bottles, adding 0.1mL, 0.2mL, 0.5mL, 1mL and 2mL of standard stock solutions respectively, and adding 20mL of internal standard solution to prepare a 5-grade standard working solution.
(3) The series of standard working solutions were subjected to gas chromatography, TCD detector detection. The conditions of the gas chromatography were: DB-1701 fused silica capillary chromatography column, size of 30m × 0.32mm × 1.0 μm; the temperature of a sample inlet is 260 ℃; temperature programming: maintaining the initial temperature at 80 deg.C for 2.5min, increasing to 250 deg.C at 40 deg.C/min, and maintaining for 3 min; helium is taken as carrier gas, the flow rate of the carrier gas is 1.5mL/min, and the constant flow mode is adopted; tail gas blowing helium gas 30 mL/min; the sample introduction volume is 1 mu L, and the split flow sample introduction is carried out, wherein the split flow ratio is 5: 1; the TCD detector temperature was 260 ℃. The method is characterized in that double internal standards are adopted for quantitative determination, n-butyl alcohol is used as the internal standard for quantitative determination of water, and 1, 3-butanediol is used as the internal standard for quantitative determination of nicotine, 1, 2-propylene glycol, glycerol, glyceryl triacetate and menthol.
(4) Standard working curve and detection limit: performing linear regression analysis by using the ratio of the peak area of each target to the peak area of the corresponding internal standard and the ratio of the concentration of each target to the concentration of the internal standard to obtain a standard working curve and a correlation coefficient of each target compound; the standard solution of the minimum concentration was injected 8 times, the standard deviation of the measurement results was calculated, the detection limit and the quantification limit were determined by 3 times and 10 times the standard deviation, respectively, and the calculation results are shown in table 1. The results show that the working curves of 6 targets are good in linearity, and the correlation coefficients are all higher than 0.999; the quantitative limit of each target object is far lower than the content of the target object in the extraction liquid, and the method is suitable for quantitative analysis.
TABLE 1 Standard working curves and detection limits
(5) After a smoking machine is prepared according to the traditional cigarette smoking method, inserting the cigarette end of the non-combustible heating cigarette sample A into a heating appliance, inserting the cigarette holder end of the non-combustible heating cigarette holder into a smoking machine holder, starting a switch of the heating appliance to preheat for 2min, starting smoking by the smoking machine, and collecting total particulate matters by a Cambridge filter disc. The smoking machine adopts a Canadian deep smoking mode, the heating time set by the heating appliance is 4min, and after 8 mouths of smoking are smoked, the smoking is finished.
(6) Placing the Cambridge filter plate with the total particulate matter trapped therein into an extraction flask, adding 20mL of internal standard solution, fully oscillating for 40min, and filtering with 0.45 μm microporous membrane to obtain the total particulate matter extraction liquid.
(7) And (4) carrying out gas chromatography analysis on the extract of the total particulate matter according to the conditions of the step (3) and detecting by a TCD detector. The content of each target in the smoke aerosol of the sample A is obtained by respectively substituting the peak area of each target and the peak area of the corresponding internal standard into the standard working curve, and the result is shown in Table 2.
TABLE 26 analysis results (mg/cigarette) of heated non-burning cigarette samples of examples
(8) Precision and recovery rate experiments. Dividing the smoke extraction liquid into four parts, wherein 1 part is used as a reference, adding water with high, medium and low concentration levels, 1, 2-propylene glycol, glycerol, menthol, glyceryl triacetate and nicotine standard solution into the other 3 parts, and repeatedly measuring 2 samples at each addition level. The samples were pre-treated and chromatographed under selected conditions and the recovery calculated from the original content of the extract, the amount of spiked and the amount of spiked assay (table 3). The results show that the standard recovery rates of water, 1, 2-propylene glycol, glycerol, menthol, glyceryl triacetate and nicotine are respectively 95.1-107.7%, 96.1-104.2%, 98.5-109.2%, 101.4-103.9%, 96.3-104.3% and 96.0-108.0%. The samples of the extracts added with the medium concentration standard solution were repeatedly analyzed 6 times, and the Relative Standard Deviation (RSD) of water, 1, 2-propanediol, glycerol, menthol, triacetin and nicotine was calculated to be 1.77%, 4.13%, 3.37%, 2.26%, 4.28% and 2.87%, respectively. . Therefore, the method has the advantages of high precision and high recovery rate, and is suitable for quantitative analysis of water, 1, 2-propylene glycol, glycerol, menthol, glyceryl triacetate and nicotine in the smoke extract of the non-burning cigarette.
TABLE 3 recovery of spiked analytical methods
Example 2
The cigarette sample B was tested as described in example 1, all the procedures were the same as in example 1, and the results of the contents of the respective target substances in the aerosol of the smoke of the sample B are shown in Table 2.
Example 3
The cigarette sample C was tested as described in example 1, all the procedures were the same as in example 1, and the content of each target in the aerosol of smoke of sample C is shown in Table 2.
Example 4
The cigarette sample D was tested as described in example 1, with all steps being the same as in example 1, and the results of the contents of each target in the smoke aerosol of sample D are shown in Table 2.
Example 5
The cigarette sample E was tested as described in example 1, with all steps being the same as in example 1, and the results of the contents of the target substances in the aerosol of smoke of sample E are shown in Table 2.
Example 6
The heated non-burning cigarette sample F was tested as described in example 1, wherein the smoking machine used an ISO standard smoking mode, the heating time set for the heating appliance was 4min, and smoking was completed after 4 puffs. The other steps are the same as example 1, and the content of each target in the smoke aerosol of sample F is shown in table 2.
The above description is only a detailed description of specific embodiments of the present invention, and should not be taken as limiting the invention, and any modifications, equivalents, improvements, etc. made on the design concept of the present invention should be included in the protection scope of the present invention.
Claims (3)
1. A method for detecting smoke components of a heated non-combustible cigarette is characterized by comprising the following steps:
(1) preparing an internal standard solution: weighing an internal standard sample n-butyl alcohol and 1, 3-butanediol, and fixing the volume by taking chromatographically pure isopropanol as a solvent to obtain an internal standard solution;
(2) preparation of standard working solution: weighing a certain amount of water, nicotine, glycerol, 1, 2-propylene glycol, glyceryl triacetate and menthol standard substance, and fixing the volume by taking chromatographic pure isopropanol as a solvent to obtain a standard stock solution; taking 5 or more extraction bottles, respectively adding standard stock solutions according to gradients, and then adding internal standard solutions with the same volume to prepare standard working solutions of grade 5 or more;
(3) smoking and heating the non-combustible cigarettes, and collecting total particulate matters by using a Cambridge filter disc;
(4) extracting the total particulate matters collected by the Cambridge filter in the step (3) by using the internal standard solution in the step (1) to obtain extract liquid of the total particulate matters;
(5) performing gas chromatography determination on the extract of the total particulate matter obtained in the step (4);
(6) and (3) calculating a measurement result by an internal standard method: performing quantitative determination by using double internal standards, wherein n-butyl alcohol is used as the internal standard for quantifying water, and 1, 3-butanediol is used as the internal standard for performing quantitative determination on nicotine, 1, 2-propylene glycol, glycerol, glyceryl triacetate and menthol;
the conditions of the gas chromatography in the step (5) are as follows: DB-1701 fused silica capillary chromatography column, size of 30m × 0.32mm × 1.0 μm; the temperature of a sample inlet is 260 ℃; temperature programming: maintaining the initial temperature at 80 deg.C for 2.5min, increasing to 250 deg.C at 40 deg.C/min, and maintaining for 3 min; helium is taken as carrier gas, the flow rate of the carrier gas is 1.5mL/min, and the constant flow mode is adopted; tail gas blowing helium gas 30 mL/min; the sample introduction volume is 1 mu L, and the split flow sample introduction is carried out, wherein the split flow ratio is 5: 1; the TCD detector temperature was 260 ℃.
2. The method for detecting smoke components of a heated non-combustible cigarette according to claim 1, wherein the step (3) of smoking the heated non-combustible cigarette and collecting total particulate matters comprises the following specific steps: after a smoking machine is prepared according to the traditional cigarette smoking method, the branch end of the cigarette which is not combusted by heating is inserted into a heating appliance, the tip end of the cigarette is inserted into a holder of the smoking machine, a switch of the heating appliance is turned on for preheating, the smoking machine starts to smoke after the preheating time is reached, a Cambridge filter disc collects total particulate matters, the smoking machine can use any one of a Canada deep smoking mode and an ISO standard smoking mode for smoking, the number of smoking openings is determined according to the smoking mode and the heating time set by the heating appliance, and the smoking is finished after the number of the smoking openings is reached.
3. The method for detecting smoke components of a heated non-combustible cigarette according to claim 1, wherein the step (4) comprises the following steps: and (3) placing the Cambridge filter disc trapping the total particulate matters in the step (3) into an extraction flask, adding 20-50mL of the internal standard solution in the step (1), fully oscillating for 0.5-2h, and filtering to obtain an extraction liquid of the total particulate matters.
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| CN111366665A (en) * | 2018-12-26 | 2020-07-03 | 贵州中烟工业有限责任公司 | In-situ extraction method for cigarette smoke |
| CN109975452A (en) * | 2019-02-15 | 2019-07-05 | 云南中烟工业有限责任公司 | Heat the measuring method of menthol in the cigarette core substrate that do not burn |
| CN112114023A (en) * | 2019-06-19 | 2020-12-22 | 湖北中烟工业有限责任公司 | Method for detecting aluminum release amount in smoke of cigarette heated without burning |
| CN111337603A (en) * | 2020-05-07 | 2020-06-26 | 贵州中烟工业有限责任公司 | Method for measuring nicotine content in tobacco product and method for simultaneously measuring water, 1, 2-propylene glycol, glycerol and nicotine content |
| CN114062579A (en) * | 2021-11-13 | 2022-02-18 | 红云红河烟草(集团)有限责任公司 | Parallel detection device for gas chromatograph and cigarette total particulate matter determination method |
| CN114740126B (en) * | 2022-05-14 | 2024-02-20 | 河南中烟工业有限责任公司 | Method for determining quality of explosive-containing bead heating cigarette product by utilizing HPLC-IR-MS |
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