CN105842378A - Determination method of aroma components in electronic cigarette aerosol - Google Patents
Determination method of aroma components in electronic cigarette aerosol Download PDFInfo
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- CN105842378A CN105842378A CN201610331883.3A CN201610331883A CN105842378A CN 105842378 A CN105842378 A CN 105842378A CN 201610331883 A CN201610331883 A CN 201610331883A CN 105842378 A CN105842378 A CN 105842378A
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- 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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
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Abstract
The invention relates to a determination method of aroma components in an electronic cigarette aerosol, and belongs to the technical field of assay determination. According to the method, a Cambridge filter is used for collecting grain phase compositions in the electronic cigarette aerosol, absorption bottles collect gas phase compositions in the electronic cigarette aerosol in cold trap conditions, then ultrasonic extraction is carried out by using dichloromethane, and deionized water is combined to carry out liquid-liquid back-extraction, the interference of large amounts of alcohol in the aerosol is eliminated, finally, the gas chromatography mass spectrometry is combined to perform qualitative and quantitative analysis. With the adoption of the determination method of the aroma components in the electronic cigarette aerosol disclosed by the invention, loss or decomposition of volatile aroma components in the electronic cigarette aerosol can be effectively avoided, multiple volatile aroma components can be simultaneously analyzed, the repeatability is better, the sensitivity is high and the operation is simple, and the interference of matrix components and solvents can be avoided, so that the determination method of the aroma components in the electronic cigarette aerosol has certain advantages in detection of the volatile aroma components in the electronic cigarette aerosol.
Description
Technical field
The invention belongs to analysis determining technology field, relate to a kind of assay method, especially a kind of to electronic cigarette aerosol
The method that middle flavor component is measured, analyzes.
Background technology
Novel tobacco goods are the strategic products of tobacco industry, are the important directions of tobacco business future development.Electronics
Cigarette is exactly development in recent years a kind of novel tobacco goods, and the tobacco juice in electronic cigarette is atomized into by it by electrical heating
Containing the mixed gas of propane diols/nicotine, suck for smoker.This heating atomization mode of electronic cigarette not only instead of tradition
Cigarette needs burning to aspirate, but also considerably reduces the harmful substance produced because of burning, avoids naked light simultaneously
Light a cigarette, aspirate the potential safety hazard of existence, it also avoid the passive smoking harm that non-smoker is caused by second-hand-cigarette.Electronics both at home and abroad
Cigarette market started explosive growth occur from 2012, and sales volume annual growth is more than 100%.2013, American Electronic cigarette sales volume
Account for the 1% of American Tobacco goods total sales volume.Predicting according to authoritative department, to the year two thousand twenty, electronic cigarette will account for tobacco at the sales volume of the U.S.
The 15% of goods total sales volume.The composition after but electronic cigarette also lacks relevant quality management and control, especially tobacco juice atomization at present, one-tenth
Divide releaser, sensory evolution and security etc., still lack comprehensively understanding, also do not have relevant electronic cigarette Aerosols Evaporation fragrant
Taste composition measurement, the report of analysis method.
Summary of the invention
The invention aims to solve the deficiencies in the prior art, it is provided that flavor component in a kind of electronic cigarette aerosol
Assay method, uses cambridge filter to combine the volatile fragrant one-tenth that absorption bottle traps in electronic cigarette aerosol under the conditions of cold-trap
Point, then use dichloromethane ultrasonic extraction, and combine deionized water and carry out liquid liquid back extraction, finally utilize gaschromatographic mass spectrometry to enter
The method of row qualitative and quantitative analysis aroma volatile, for analyzing electronic cigarette fragrance component accurately and commenting
Valency.
For achieving the above object, the technical solution used in the present invention is as follows:
The assay method of flavor component in a kind of electronic cigarette aerosol, comprises the following steps:
Step (1), uses electronic cigarette smoking machine to aspirate electronic cigarette sample, with the individual layer being placed on smoking machine in trap
TPM in electronic cigarette flue gas releaser is trapped by cambridge filter, traps 20 ~ 100 mouthfuls of flue gases of electronic cigarette continuous sucking
The TPM of releaser, the most often aspirates 20 ~ 100 mouthfuls and changes a filter disc；
Step (2), is used in the gas phase through cambridge filter of the cold trap trapping device trapping between trap and smoking machine suction syringe
Composition；
Described cold trap trapping device includes two absorption bottles equipped with 10 ~ 50mL dichloromethane connected and for being entered by absorption bottle
The heat-preserving container of row cryosel bath；Cold trap trapping unit temp maintains-5 ~ 0 DEG C；
Step (3), to be pumped after, cambridge filter is taken out and is placed in container, simultaneously in container, pour two absorption bottles into
In trapping have the dichloromethane solution of gas phase composition, ultrasonic extraction 20 ~ 60min the most together；
Step (4), extract complete after, pipette and 10 ~ 30mL extract adds isopyknic deionized water carry out liquid liquid back extraction
Take, after stratification, then by organic layer 40 DEG C, be concentrated into 1mL under the conditions of 450 mbar, obtain concentrate；
Step (5), carries out qualitative and quantitative analysis with gas chromatography mass spectrometer to the concentrate of step (4)；Condition is: chromatographic column:
HP-5MS capillary column, length × internal diameter × thickness is 30m × 0.25mm × 0.25 m；Carrier gas: He, constant current mode: flow velocity:
1.0 mL/min；Temperature programming: 50 DEG C keep 1min, then rise to 180 DEG C with 5 DEG C/min and keep 1min, then with 10 DEG C/
Min rises to 280 DEG C and keeps 3min；Injector temperature: 280 DEG C；Sample size 2 μ L, Splitless injecting samples；Transmission line temperature:
280-300℃；Ionization mode: EI；Ionizing energy: 70eV；Ion source temperature: 230-250 DEG C；Level Four bar temperature: 160 DEG C；Matter
Weight range 35-450aum；Solvent delay: 4min；Detection pattern: SCAN and SIM synchronizes.
Chem workstation search criteria mass spectrum picture library is passed through in the qualitative analysis of described aroma volatile, in combination with
Relevant mass spectrogram document resolves, and confirms electronic cigarette volatile ingredient, and chem workstation data handling system is passed through in quantitative analysis, presses
Areas of peak normalization method carries out calculating the percentage contents obtaining each component.
It is further preferred that described electronic cigarette smoking machine is to aspirate the electricity with jettron and hand switch
The smoking machine of sub-cigarette, meanwhile, the shape of the electronic cigarette smoking machine of the present invention electronic cigarette to being aspirated does not limits.
It is further preferred that the suction mode of described electronic cigarette is pumping volume 55.0 mL, puff duration
3s, suction frequencies 30s, puffing profile is square wave.
It is further preferred that each electronic cigarette φ 44 mm cambridge filter traps 50 mouthfuls.
It is further preferred that described flavor component includes 2,3-dimethyl pyrazine, 2,2,4,6,6-five methylheptanes,
Benzyl carbinol, 1-methyl-4-piperidones, Tetramethylpyrazine, maltol, menthol, 2,6-dimethyl decane, 2-chloro-4-(4-first
Phenyl)-6-(4-nitrobenzophenone) pyrimidine, nicotine, myosmine, 4-ethylpyridine, 3-methyl-cyclopentane methyl formate, new
Phytadiene, diisobutyl phthalate, 14 phosphoamides, western cypress triolefin glycol compound, oleamide, 16 phosphinylidynes
Amine, erucyl amide.
It is further preferred that described flavor component also includes 2-hydroxy-3-methyl-2-cyclopentene-1-one, sweet basil
Alkene, tea ketone musk, isopulegol, 2,4-dimethyl-1,3-dioxane, 3-methyl isophthalic acid-cyclopentene, isomenthol, methyl cyclohexanol,
Vinyl acetate, D-CARVONE, 4-(2,6,6-trimethyl-1-cyclohexenyl group)-3-butene-2-one, (1S, 2S, 5S)-(-)-
2-hydroxyl-3-pinanone.
Capturing device structure of the present invention and number of patent application are that the capture structure of 201410177530.3 is except protecting
Outside mixture difference in temperature bucket, remaining is the most identical.
Compared with prior art, it has the beneficial effect that the present invention
The present invention uses cambridge filter to combine the volatile fragrant one-tenth that absorption bottle traps in electronic cigarette aerosol under the conditions of cold-trap
Point, then use dichloromethane ultrasonic extraction, and combine deionized water and carry out liquid liquid back extraction, finally utilize gaschromatographic mass spectrometry
Carry out qualitative and quantitative analysis aroma volatile；
The inventive method can volatile fragrant components in Accurate Determining electronic cigarette aerosol, the group in effective enriched sample
Point, it is to avoid matrix composition and the interference of solvent, have highly sensitive, detection limit is low, the feature such as simple to operate, quick；
The inventive method can make fragrance component be efficiently separated, and can measure the volatilization in electronic cigarette aerosol rapidly and accurately
Property fragrance matter, and measurement result is with a high credibility；
The present invention is simple to operate, reproducible, and sensitivity for analysis is high, it is only necessary to single-time measurement, just can obtain electronic cigarette aerosol
In multiple volatile materials, it is not necessary to complicated pre-treatment, save analysis cost, harmless to environment and health；
The present invention can be prevented effectively from loss or the decomposition of electronic cigarette Aerosols Evaporation fragrance component, can be to multiple volatile aroma
Composition is analyzed simultaneously, simple to operate, and the context of detection at aroma volatile has advantage.
The present invention compares with application for a patent for invention 201510084273.3, and the inventive method can be for electronic cigarette aerosol
In multiple fragrance composition be measured, and the most non-18 kinds of volatile ingredients carry out quantitative and semi-quantitative mensuration, measure object
Matter scope expands significantly, has clear superiority in electronic cigarette aerosol fragrance component context of detection.Pre-treatment of the present invention uses liquid
The method of liquid back extraction, can extract target substance and be analyzed, it is to avoid electronic cigarette tobacco tar solvent glycerin, propane diols
A large amount of interference, measure accurately, and effect is obvious.
Accompanying drawing explanation
Fig. 1 is the capturing device structural representation that the present invention uses；
Fig. 2 is the gas chromatogram of volatile ingredient in the embodiment of the present invention 1；Fig. 3 is the gas phase of volatile ingredient in comparative example 1
Chromatogram；
Wherein, 1 electronic cigarette sample；2 adapters；3 traps；4 smoking machines；5 absorption bottles；6—
Heat-preserving container；7 ice and the mixture of sodium chloride；8 suction syringes.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail.
It will be understood to those of skill in the art that the following example is merely to illustrate the present invention, and should not be regarded as limiting this
Bright scope.Unreceipted concrete technology or condition person in embodiment, according to the technology described by the document in this area or condition
Or carry out according to product description.Agents useful for same or instrument unreceipted production firm person, be and can be obtained by purchase
Conventional products.
The material of all detections of the present invention is the material that gas chromatography mass spectrometer database Auto-matching is given.
Embodiment 1
Capturing device of the present invention is as it is shown in figure 1, put into purpose filter leaf clip holder by the cambridge filter of 44 mm, and filter disc is coarse
One side should towards enter flue gas, purpose filter leaf clip holder of closing, check confirm assembling appropriate.If trap one in aspiration procedure
End can put into electronic cigarette, gas leak phenomenon does not occur, then directly electronic cigarette is inserted trap and aspirate.But it is currently marketed
Electronic cigarette suction nozzle is different, if trap one end is not mated with electronic-cigarette holder, aspiration procedure is leaked gas, then need
The adapter that between trap and electronic cigarette, adjunction seal is good, prevents from leaking gas in aspiration procedure.
Smoking machine trap and suction syringe between be in series with two equipped with 30mL dichloromethane absorption bottle, absorb bottled
Enter heat-preserving container carries out cryosel bath, absorption bottle and heat-preserving container to collectively constitute cold trap trapping device.
From smoking machine, take off Fume collector, open, take out filter disc ultrasonic extraction with tweezers.Flue gas grain will have been collected
The cambridge filter of phase thing is placed in conical flask, extracts 20min with 100W power ultrasonic at room temperature with corresponding extractant, quiet
Put 5min, draw appropriate upper layer of extraction liquid, obtain extract with 0.45 μm filtering with microporous membrane, load chromatogram bottle and carry out gas phase
Chromatography, the content of the target analytes in mensuration extract.
Flavor component in certain brand electronic cigarette aerosol is measured, specifically comprises the following steps that
Step (1), uses electronic cigarette smoking machine to aspirate electronic cigarette sample, with the individual layer being placed on smoking machine in trap
TPM in electronic cigarette flue gas releaser is trapped by cambridge filter, the 50 mouthfuls of flue gas releases of trapping electronic cigarette continuous sucking
The TPM of thing；
Suction mode is pumping volume 55.0 mL, puff duration 3s, suction frequencies 30s, and puffing profile is square wave.Each
Electronic cigarette traps 50 mouthfuls with a diameter of 44 mm cambridge filters；Often a filter disc is changed in suction 50 mouthfuls；
Step (2), is used in the gas phase through cambridge filter of the cold trap trapping device trapping between trap and smoking machine suction syringe
Composition；
Described cold trap trapping device includes two absorption bottles equipped with 30mL dichloromethane connected and for being carried out by absorption bottle
The heat-preserving container of cryosel bath；Cold trap trapping unit temp maintains 0 DEG C；
Step (3), to be pumped after, from smoking machine, take off Fume collector, open, with tweezers by cambridge filter take out put
In 100 mL conical flasks, pour the trapping in two absorption bottles in conical flask into has the dichloromethane of gas phase composition molten simultaneously
Liquid, the most together ultrasonic extraction 30min, in order to extract the grain phase part of cambridge filter trapping；
Step (4), extract complete after, pipette 20 mL extracts add in the separatory funnel of 100 mL isopyknic go from
Sub-water carries out a not good liquor liquid back extraction, after stratification, then organic layer is poured into 50 mL completely concentrates in bottles, 40 DEG C,
It is concentrated into 1mL under the conditions of 450 mbar, obtains concentrate；
Step (5), carries out qualitative and quantitative analysis with gas chromatography mass spectrometer to the concentrate of step (4)；Condition is: chromatographic column:
HP-5MS capillary column, length × internal diameter × thickness is 30m × 0.25mm × 0.25 m；Carrier gas: He, constant current mode: flow velocity:
1.0 mL/min；Temperature programming: 50 DEG C keep 1min, then rise to 180 DEG C with 5 DEG C/min and keep 1min, then with 10 DEG C/
Min rises to 280 DEG C and keeps 3min；Injector temperature: 280 DEG C；Sample size 2 μ L, Splitless injecting samples；Transmission line temperature:
280-300℃；Ionization mode: EI；Ionizing energy: 70eV；Ion source temperature: 230-250 DEG C；Level Four bar temperature: 160 DEG C；Matter
Weight range 35-450aum；Solvent delay: 4min；Detection pattern: SCAN and SIM synchronizes.
Wherein: the qualitative analysis of aroma volatile pass through chem workstation search criteria mass spectrum picture library, in combination with
Relevant mass spectrogram document resolves, and confirms electronic cigarette volatile ingredient, and chem workstation data handling system is passed through in quantitative analysis, presses
Areas of peak normalization method carries out calculating the percentage contents obtaining each component.
The result chromatogram that records is as in figure 2 it is shown, volatile ingredient and relative amount thereof are shown in Table 1:
Certain brand electronic cigarette volatile ingredient table of table 1
Note: relative amount is the percentage contents of chromatographic peak area, the peak area ratio total peak area of the most each material.
From table 1 and Fig. 2: present invention determine that 21 components in electronic cigarette aerosol, predominantly aldehydes, phenols, alcohol
Class, esters, ketone etc..This method has simple to operate, the analysis feature that speed is fast, amount of samples is few, can effectively analyze electronics
Volatile fragrant components in smoke sol.
Embodiment 2
Capturing device of the present invention is as it is shown in figure 1, put into purpose filter leaf clip holder by the cambridge filter of 44 mm, and filter disc is coarse
One side should towards enter flue gas, purpose filter leaf clip holder of closing, check confirm assembling appropriate.If trap one in aspiration procedure
End can put into electronic cigarette, gas leak phenomenon does not occur, then directly electronic cigarette is inserted trap and aspirate.But it is currently marketed
Electronic cigarette suction nozzle is different, if trap one end is not mated with electronic-cigarette holder, aspiration procedure is leaked gas, then need
The adapter that between trap and electronic cigarette, adjunction seal is good, prevents from leaking gas in aspiration procedure.
Smoking machine trap and suction syringe between be in series with two equipped with 40mL dichloromethane absorption bottle, absorb bottled
Enter heat-preserving container carries out cryosel bath, absorption bottle and heat-preserving container to collectively constitute cold trap trapping device.
From smoking machine, take off Fume collector, open, take out filter disc ultrasonic extraction with tweezers.Flue gas grain will have been collected
The cambridge filter of phase thing is placed in conical flask, extracts 30min with 100W power ultrasonic at room temperature with corresponding extractant, quiet
Put 5min, draw appropriate upper layer of extraction liquid, obtain extract with 0.45 μm filtering with microporous membrane, load chromatogram bottle and carry out gas phase
Chromatography, the content of the target analytes in mensuration extract.
Flavor component in another brand electronic cigarette aerosol is measured, specifically comprises the following steps that
Step (1), uses electronic cigarette smoking machine to aspirate electronic cigarette sample, with the individual layer being placed on smoking machine in trap
TPM in electronic cigarette flue gas releaser is trapped by cambridge filter, and trapping 100 mouthfuls of flue gases of electronic cigarette continuous sucking are released
Put the TPM of thing；
Suction mode is pumping volume 55.0 mL, puff duration 3s, suction frequencies 30s, and puffing profile is square wave.Each
Electronic cigarette traps 100 mouthfuls with a diameter of 44 mm cambridge filters；Often a filter disc is changed in suction 100 mouthfuls；
Step (2), is used in the gas phase through cambridge filter of the cold trap trapping device trapping between trap and smoking machine suction syringe
Composition；
Described cold trap trapping device includes two absorption bottles equipped with 50mL dichloromethane connected and for being carried out by absorption bottle
The heat-preserving container of cryosel bath；Cold trap trapping unit temp maintains-1 DEG C；
Step (3), to be pumped after, from smoking machine, take off Fume collector, open, with tweezers by cambridge filter take out put
In 100 mL conical flasks, pour the trapping in two absorption bottles in conical flask into has the dichloromethane of gas phase composition molten simultaneously
Liquid, the most together ultrasonic extraction 30min, in order to extract the grain phase part of cambridge filter trapping；
Step (4), extract complete after, pipette 30 mL extracts add in the separatory funnel of 100 mL isopyknic go from
Sub-water carries out a not good liquor liquid back extraction, after stratification, then organic layer is poured into 50 mL completely concentrates in bottles, 40 DEG C,
It is concentrated into 1mL under the conditions of 450 mbar, obtains concentrate；
Step (5), carries out qualitative and quantitative analysis with gas chromatography mass spectrometer to the concentrate of step (4)；Condition is: chromatographic column:
HP-5MS capillary column, length × internal diameter × thickness is 30m × 0.25mm × 0.25 m；Carrier gas: He, constant current mode: flow velocity:
1.0 mL/min；Temperature programming: 50 DEG C keep 1min, then rise to 180 DEG C with 5 DEG C/min and keep 1min, then with 10 DEG C/
Min rises to 280 DEG C and keeps 3min；Injector temperature: 280 DEG C；Sample size 2 μ L, Splitless injecting samples；Transmission line temperature:
280-300℃；Ionization mode: EI；Ionizing energy: 70eV；Ion source temperature: 230-250 DEG C；Level Four bar temperature: 160 DEG C；Matter
Weight range 35-450aum；Solvent delay: 4min；Detection pattern: SCAN and SIM synchronizes.
Wherein: the qualitative analysis of aroma volatile pass through chem workstation search criteria mass spectrum picture library, in combination with
Relevant mass spectrogram document resolves, and confirms electronic cigarette volatile ingredient, and chem workstation data handling system is passed through in quantitative analysis, presses
Areas of peak normalization method carries out calculating the percentage contents obtaining each component.
Volatile ingredient and relative amount thereof are shown in Table 2:
Embodiment 3
Capturing device of the present invention is as it is shown in figure 1, put into purpose filter leaf clip holder by the cambridge filter of 44 mm, and filter disc is coarse
One side should towards enter flue gas, purpose filter leaf clip holder of closing, check confirm assembling appropriate.If trap one in aspiration procedure
End can put into electronic cigarette, gas leak phenomenon does not occur, then directly electronic cigarette is inserted trap and aspirate.But it is currently marketed
Electronic cigarette suction nozzle is different, if trap one end is not mated with electronic-cigarette holder, aspiration procedure is leaked gas, then need
The adapter that between trap and electronic cigarette, adjunction seal is good, prevents from leaking gas in aspiration procedure.
Smoking machine trap and suction syringe between be in series with two equipped with 40mL dichloromethane absorption bottle, absorb bottled
Enter heat-preserving container carries out cryosel bath, absorption bottle and heat-preserving container to collectively constitute cold trap trapping device.
From smoking machine, take off Fume collector, open, take out filter disc ultrasonic extraction with tweezers.Flue gas grain will have been collected
The cambridge filter of phase thing is placed in conical flask, extracts 60min with 100W power ultrasonic at room temperature with corresponding extractant, quiet
Put 5min, draw appropriate upper layer of extraction liquid, obtain extract with 0.45 μm filtering with microporous membrane, load chromatogram bottle and carry out gas phase
Chromatography, the content of the target analytes in mensuration extract.
Flavor component in brand electronic cigarette aerosol same as in Example 1 is measured, specifically comprises the following steps that
Step (1), uses electronic cigarette smoking machine to aspirate electronic cigarette sample, with the individual layer being placed on smoking machine in trap
TPM in electronic cigarette flue gas releaser is trapped by cambridge filter, the 20 mouthfuls of flue gas releases of trapping electronic cigarette continuous sucking
The TPM of thing；
Suction mode is pumping volume 55.0 mL, puff duration 3s, suction frequencies 30s, and puffing profile is square wave.Each
Electronic cigarette traps 20 mouthfuls with a diameter of 44 mm cambridge filters；Often a filter disc is changed in suction 20 mouthfuls；
Step (2), is used in the gas phase through cambridge filter of the cold trap trapping device trapping between trap and smoking machine suction syringe
Composition；
Described cold trap trapping device includes two absorption bottles equipped with 10mL dichloromethane connected and for being carried out by absorption bottle
The heat-preserving container of cryosel bath；Cold trap trapping unit temp maintains-5 DEG C；
Step (3), to be pumped after, from smoking machine, take off Fume collector, open, with tweezers by cambridge filter take out put
In 100 mL conical flasks, pour the trapping in two absorption bottles in conical flask into has the dichloromethane of gas phase composition molten simultaneously
Liquid, the most together ultrasonic extraction 60min, in order to extract the grain phase part of cambridge filter trapping；
Step (4), extract complete after, pipette 10 mL extracts add in the separatory funnel of 100 mL isopyknic go from
Sub-water carries out a not good liquor liquid back extraction, after stratification, then organic layer is poured into 50 mL completely concentrates in bottles, 40 DEG C,
It is concentrated into 1mL under the conditions of 450 mbar, obtains concentrate；
Step (5), carries out qualitative and quantitative analysis with gas chromatography mass spectrometer to the concentrate of step (4)；Condition is: chromatographic column:
HP-5MS capillary column, length × internal diameter × thickness is 30m × 0.25mm × 0.25 m；Carrier gas: He, constant current mode: flow velocity:
1.0 mL/min；Temperature programming: 50 DEG C keep 1min, then rise to 180 DEG C with 5 DEG C/min and keep 1min, then with 10 DEG C/
Min rises to 280 DEG C and keeps 3min；Injector temperature: 280 DEG C；Sample size 2 μ L, Splitless injecting samples；Transmission line temperature:
280-300℃；Ionization mode: EI；Ionizing energy: 70eV；Ion source temperature: 230-250 DEG C；Level Four bar temperature: 160 DEG C；Matter
Weight range 35-450aum；Solvent delay: 4min；Detection pattern: SCAN and SIM synchronizes.
Wherein: the qualitative analysis of aroma volatile pass through chem workstation search criteria mass spectrum picture library, in combination with
Relevant mass spectrogram document resolves, and confirms electronic cigarette volatile ingredient, and chem workstation data handling system is passed through in quantitative analysis, presses
Areas of peak normalization method carries out calculating the percentage contents obtaining each component.
Its testing result is basically identical with table 1.
Comparative example 1
Other steps of this comparative example are identical with embodiment 1, but are provided without liquid liquid back extraction, the extraction after directly extracting with dichloromethane
Taking liquid and carry out gaschromatographic mass spectrometric analysis, the material detected is only 4 kinds, respectively propane diols, glycerine, nicotine and Mace
Bright.Chromatogram is as shown in Figure 3.If result explanation does not use liquid liquid back extraction, electronic cigarette tobacco tar solvent glycerin, propane diols can produce
Raw a large amount of interference, largely effects on the accuracy of measurement result.
The general principle of the present invention, principal character and advantages of the present invention have more than been shown and described.The technology of the industry
Personnel, it should be appreciated that the present invention is not restricted to the described embodiments, simply illustrating this described in above-described embodiment and specification
The principle of invention, without departing from the spirit and scope of the present invention, the present invention also has various changes and modifications, and these become
Change and improvement both falls within scope of the claimed invention.Claimed scope by appending claims and
Equivalent defines.
Claims (6)
1. the assay method of flavor component in an electronic cigarette aerosol, it is characterised in that comprise the following steps:
Step (1), uses electronic cigarette smoking machine to aspirate electronic cigarette sample, with the individual layer being placed on smoking machine in trap
TPM in electronic cigarette flue gas releaser is trapped by cambridge filter, traps 20 ~ 100 mouthfuls of flue gases of electronic cigarette continuous sucking
The TPM of releaser；
Step (2), is used in the gas phase through cambridge filter of the cold trap trapping device trapping between trap and smoking machine suction syringe
Composition；
Described cold trap trapping device includes two absorption bottles equipped with 10 ~ 50mL dichloromethane connected and for being entered by absorption bottle
The heat-preserving container of row cryosel bath；Cold trap trapping unit temp maintains-5 ~ 0 DEG C；
Step (3), to be pumped after, cambridge filter is taken out and is placed in container, simultaneously in container, pour two absorption bottles into
In trapping have the dichloromethane solution of gas phase composition, ultrasonic extraction 20 ~ 60min the most together；
Step (4), extract complete after, pipette and 10 ~ 30 mL extracts add isopyknic deionized water carry out liquid liquid back extraction
Take, after stratification, then by organic layer 40 DEG C, be concentrated into 1mL under the conditions of 450 mbar, obtain concentrate；
Step (5), carries out qualitative and quantitative analysis with gas chromatography mass spectrometer to the concentrate of step (4)；Condition is: chromatographic column:
HP-5MS capillary column, length × internal diameter × thickness is 30m × 0.25mm × 0.25 m；Carrier gas: He, constant current mode: flow velocity:
1.0 mL/min；Temperature programming: 50 DEG C keep 1min, then rise to 180 DEG C with 5 DEG C/min and keep 1min, then with 10 DEG C/
Min rises to 280 DEG C and keeps 3min；Injector temperature: 280 DEG C；Sample size 2 μ L, Splitless injecting samples；Transmission line temperature:
280-300℃；Ionization mode: EI；Ionizing energy: 70eV；Ion source temperature: 230-250 DEG C；Level Four bar temperature: 160 DEG C；Matter
Weight range 35-450aum；Solvent delay: 4min；Detection pattern: SCAN and SIM synchronizes.
The assay method of flavor component in electronic cigarette aerosol the most according to claim 1, it is characterised in that described electricity
Sub-cigarette smoking machine is can to aspirate with jettron and the smoking machine of the electronic cigarette of hand switch.
The assay method of flavor component in electronic cigarette aerosol the most according to claim 1, it is characterised in that described electricity
The suction mode of sub-cigarette is pumping volume 55.0 mL, puff duration 3s, suction frequencies 30s, and puffing profile is square wave.
The assay method of flavor component in electronic cigarette aerosol the most according to claim 1, it is characterised in that each electronics
Cigarette φ 44 mm cambridge filter traps 50 mouthfuls.
The assay method of flavor component in electronic cigarette aerosol the most according to claim 1, it is characterised in that described perfume (or spice)
Taste composition includes 2,3-dimethyl pyrazine, 2,2,4,6,6-five methylheptane, benzyl carbinol, 1-methyl-4-piperidones, tetramethyl
Pyrazine, maltol, menthol, 2,6-dimethyl decane, the chloro-4-of 2-(4-methoxyphenyl)-6-(4-nitrobenzophenone) pyrimidine, cigarette
Alkali, myosmine, 4-ethylpyridine, 3-methyl-cyclopentane methyl formate, neophytadiene, diisobutyl phthalate, 14 carbon
Acid amides, western cypress triolefin glycol compound, oleamide, 16 phosphoamides, erucyl amide.
The assay method of flavor component in electronic cigarette aerosol the most according to claim 1, it is characterised in that described perfume (or spice)
Taste composition also includes 2-hydroxy-3-methyl-2-cyclopentene-1-one, ocimenum, tea ketone musk, isopulegol, 2,4-dimethyl-1,
3-dioxane, 3-methyl isophthalic acid-cyclopentene, isomenthol, methyl cyclohexanol, vinyl acetate, D-CARVONE, 4-(2,6,6-
Trimethyl-1-cyclohexenyl group)-3-butene-2-one, (1S, 2S, 5S)-(-)-2-hydroxyl-3-pinanone.
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| CN106290639A (en) * | 2016-08-11 | 2017-01-04 | 云南中烟工业有限责任公司 | A kind of quantitative forecasting technique of Medicated cigarette milk flavoured type |
| CN107189857A (en) * | 2017-07-07 | 2017-09-22 | 重庆中烟工业有限责任公司 | A kind of apparatus and method for preparing smoke spices |
| CN107817195A (en) * | 2017-10-21 | 2018-03-20 | 云南中烟工业有限责任公司 | Particle size distribution measuring method of the electronic cigarette solution additive in flue gas aerosol |
| CN108037045A (en) * | 2017-10-21 | 2018-05-15 | 云南中烟工业有限责任公司 | Heat the assay method that cigarette flavors are distributed in different-grain diameter flue gas aerosol that do not burn |
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| CN113720937A (en) * | 2021-08-30 | 2021-11-30 | 深圳市真味生物科技有限公司 | Method for measuring content of cooling agent in electronic smoke sol |
| CN113720934A (en) * | 2021-08-20 | 2021-11-30 | 中国烟草总公司郑州烟草研究院 | Method for detecting aroma components in cigarette mainstream smoke |
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| CN108872416B (en) * | 2018-06-25 | 2021-07-02 | 上海市食品药品包装材料测试所 | Method for simultaneously and quantitatively detecting erucamide and ethylene bis-stearamide |
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| CN109557202A (en) * | 2018-11-27 | 2019-04-02 | 湖北稻花香酒业股份有限公司 | The detection method of 16 carbamides in food contact plastics |
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| CN110320292A (en) * | 2019-06-28 | 2019-10-11 | 河南中烟工业有限责任公司 | The measuring method of volatile component in a kind of full flue gas of electronic cigarette |
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| CN113720934A (en) * | 2021-08-20 | 2021-11-30 | 中国烟草总公司郑州烟草研究院 | Method for detecting aroma components in cigarette mainstream smoke |
| CN113720937A (en) * | 2021-08-30 | 2021-11-30 | 深圳市真味生物科技有限公司 | Method for measuring content of cooling agent in electronic smoke sol |
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