CN105842378B - The assay method of flavor component in a kind of electronics smoke sol - Google Patents
The assay method of flavor component in a kind of electronics smoke sol Download PDFInfo
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- CN105842378B CN105842378B CN201610331883.3A CN201610331883A CN105842378B CN 105842378 B CN105842378 B CN 105842378B CN 201610331883 A CN201610331883 A CN 201610331883A CN 105842378 B CN105842378 B CN 105842378B
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- G—PHYSICS
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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 present invention relates to a kind of assay method of flavor component in electronics smoke sol, belong to analysis determining technology field.This method is using the grain phase constituent in cambridge filter trapping electronics smoke sol, gas phase composition of the absorption bottle in trapping electronics smoke sol under the conditions of cold-trap, then dichloromethane ultrasonic extraction is used, and combine deionized water and carry out liquid liquid back extraction, the interference of a large amount of alcohol in aerosol is eliminated, finally carries out qualitative and quantitative analysis with reference to gaschromatographic mass spectrometry.The present invention can effectively avoid the loss or decomposition of aroma volatile in electronics smoke sol, a variety of aroma volatiles can be analyzed at the same time, it is repeated preferable, high sensitivity, it is easy to operate, can be to avoid the interference of matrix composition and solvent, the context of detection of aroma volatile has certain advantage in electronics smoke sol.
Description
Technical field
The invention belongs to analysis determining technology field, is related to a kind of assay method, especially a kind of to electronics smoke sol
The method that middle flavor component is measured, analyzes.
Background technology
Novel tobacco product is the strategic product of tobacco industry, is the important directions of tobacco business future development.Electronics
Cigarette is exactly a kind of novel tobacco product with the fastest developing speed in recent years, and the tobacco juice in electronic cigarette is atomized into by it by electrical heating
Mixed gas containing propane diols/nicotine, sucks for smoker.This heating atomization mode of electronic cigarette not only instead of tradition
Cigarette, which needs to burn, to be aspirated, but also considerably reduces the harmful substance produced by burning, while avoids naked light
Light a cigarette, aspirate existing for security risk, it also avoid secondhand smoke caused by non-smoker passive smoking endanger.Domestic exoelectron
There is explosive growth since 2012 in cigarette market, and sales volume annual growth is more than 100%.2013, American Electronic cigarette sales volume
The 1% of American Tobacco product total sales volume is accounted for.Predicted according to authoritative department, to the year two thousand twenty, sales volume of the electronic cigarette in the U.S. will account for tobacco
The 15% of product total sales volume.But electronic cigarette also lacks relevant quality management and control at present, component especially after tobacco juice atomization, into
Divide releaser, sensory evolution and security etc., still lack comprehensive understanding, also without related electronic cigarette Aerosols Evaporation perfume
Taste composition measurement, the report of analysis method.
The content of the invention
It is an object of the present invention to solve the deficiency of the existing technology and provide flavor component in a kind of electronics smoke sol
Assay method, trapped using cambridge filter combination absorption bottle under the conditions of the cold-trap volatile fragrant in electronics smoke sol into
Point, then with dichloromethane ultrasonic extraction, and combine deionized water and carry out liquid liquid back extraction, finally using gaschromatographic mass spectrometry into
The method of row qualitative and quantitative analysis aroma volatile, for carrying out accurately analysis to electronic cigarette fragrance component with commenting
Valency.
To achieve the above object, the technical solution adopted by the present invention is as follows：
The assay method of flavor component, comprises the following steps in a kind of electronics smoke sol：
Step（1）, electronic cigarette sample is aspirated using electronic cigarette smoking machine, with being placed on smoking machine in trap
Individual layer cambridge filter traps the total granules in electronic cigarette flue gas releaser, 20 ~ 100 mouthfuls of trapping electronic cigarette continuous sucking
The total granules of flue gas releaser, i.e., often aspirate filter disc of 20 ~ 100 mouthfuls of replacements；
Step（2）, the cold trap trapping device trapping between trap and smoking machine suction syringe is through cambridge filter
Gas phase composition；
The cold trap trapping device includes the absorption bottle equipped with 10 ~ 50mL dichloromethane of two series connection and for will absorption
Bottle carries out the insulation barrel of ice salt bath；Cold trap trapping unit temp maintains -5 ~ 0 DEG C；
Step（3）, after to be pumped, cambridge filter is taken out and is placed in container, while two suctions are poured into container
Receiving the trapping in bottle has the dichloromethane solution of gas phase composition, then 20 ~ 60min of ultrasonic extraction together；
Step（4）, after extraction finishes, pipette and isometric deionized water progress liquid liquid added in 10 ~ 30mL extracts
Back extraction, is concentrated into 1mL under the conditions of 40 DEG C, 450 mbar after stratification, then by organic layer, obtains concentrate；
Step（5）, with gas chromatography mass spectrometer to step（4）Concentrate carry out qualitative and quantitative analysis；Condition is：Chromatography
Column：HP-5MS capillary columns, length × internal diameter × thickness are 30m × 0.25mm × 0.25 μm；Carrier gas：He, constant current mode：Stream
Speed： 1.0 mL/min；Temperature programming：50 DEG C holding 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 ℃；2 μ L of sample size, Splitless injecting samples；Transmission line temperature
Degree：280-300℃；Ionization mode：EI；Ionizing energy：70eV；Ion source temperature：230-250℃；Level Four bar temperature：160℃；
Mass range 35-450aum；Solvent delay：4min；Detection pattern：SCAN and SIM is synchronous.
The qualitative analysis of the aroma volatile by chem workstation search criteria mass spectrum picture library, in combination with
Related mass spectrogram document parsing, confirms electronic cigarette volatile ingredient, quantitative analysis is pressed by chem workstation data handling system
Areas of peak normalization method carries out calculating the percentage contents for obtaining each component.
It is further preferred that the electronic cigarette smoking machine is that can aspirate the electricity with jettron and manual switch
The smoking machine of sub- cigarette, meanwhile, the shape of electronic cigarette of the electronic cigarette smoking machine of the present invention to being aspirated does not limit.
It is further preferred that the suction mode of the electronic cigarette is 55.0 mL of pumping volume, puff duration
3s, suction frequencies 30s, puffing profile are square wave.
It is further preferred that each electronic cigarette traps 50 mouthfuls with 44 mm cambridge filters of φ.
It is further preferred that the flavor component include 2,3- dimethyl pyrazines, 2,2,4,6,6- five methylheptanes,
Benzyl carbinol, 1- methyl -4- piperidones, Tetramethylpyrazine, maltol, menthol, 2,6- dimethyl decanes, 2- chloro- 4- (4- first
Phenyl) it is -6- (4- nitrobenzophenones) pyrimidine, nicotine, myosmine, 4- ethylpyridines, 3- methyl-cyclopentanes methyl formate, new
Phytadiene, diisobutyl phthalate, 14 carbamides, western cypress triolefin glycol compound, oleamide, 16 phosphinylidynes
Amine, erucyl amide.
It is further preferred that the flavor component further includes 2- hydroxy-3-methyl -2- cyclopentene-1-ones, sweet basil
Alkene, tea perfume ketone, isopulegol, 2,4- dimethyl -1,3- dioxanes, 3- methyl isophthalic acids-cyclopentene, isomenthol, methyl cyclohexanol,
Vinyl acetate, D-CARVONE, 4- (2,6,6- trimethyl -1- cyclohexenyl groups) -3- butene-2s -one, (1S, 2S, 5S)-(-) -
2- hydroxyl -3- pinanones.
Capturing device structure of the present invention is removed with the capture structure that number of patent application is 201410177530.3 and protected
Outside mixture difference in warm bucket, remaining is all identical.
Compared with prior art, the present invention its advantage is：
The volatility that the present invention is trapped in electronics smoke sol using cambridge filter combination absorption bottle under the conditions of cold-trap is fragrant
Taste component, then using dichloromethane ultrasonic extraction, and combines deionized water and carries out liquid liquid back extraction, finally utilize gas-chromatography
Mass spectrum carries out qualitative and quantitative analysis aroma volatile；
The method of the present invention can be in Accurate Determining electronics smoke sol volatile fragrant components, in effective enriched sample
Component, avoids the interference of matrix composition and solvent, has the characteristics that high sensitivity, detection limit are low, easy to operate, quick；
The method of the present invention can be efficiently separated fragrance component, and can rapidly and accurately be measured in electronics smoke sol
Volatile flavor compounds, and measurement result is with a high credibility；
The present invention is easy to operate, reproducible, and sensitivity for analysis is high, it is only necessary to single-time measurement, with regard to electronics flue gas can be obtained
A variety of volatile materials in colloidal sol, it is not necessary to which complicated pre-treatment, saves analysis cost, harmless to environment and health；
The present invention can effectively avoid the loss or decomposition of electronic cigarette Aerosols Evaporation fragrance component, can be to a variety of volatility
Fragrance component is analyzed at the same time, easy to operate, has advantage in the context of detection of aroma volatile.
The present invention is compared with application for a patent for invention 201510084273.3, and the method for the present invention can be directed to electronics smoke sol
In multiple fragrance component be measured, and only non-18 kinds of volatile ingredients carry out quantitative and semi-quantitative measure, measure object
Matter scope expands significantly, has a clear superiority in electronics smoke sol fragrance component context of detection.Pre-treatment of the present invention uses liquid
The method of liquid back extraction, target substance can be extracted and analyzed, and avoid electronic cigarette tobacco tar solvent glycerin, propane diols
A large amount of interference, measure is accurate, positive effect.
Brief description of the drawings
Fig. 1 is the capturing device structure diagram 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 volatile ingredient in comparative example 1
Gas chromatogram；
Wherein, 1-electronic cigarette sample；2-adapter；3-trap；4-smoking machine；5-absorption bottle；6—
Insulation barrel；The mixture of 7-ice and sodium chloride；8-suction syringe.
Embodiment
With reference to 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 it should not be regarded as limiting this hair
Bright scope.In the examples where no specific technique or condition is specified, according to the described technology of document in the art or condition
Or carried out according to product description.Reagents or instruments used without specified manufacturer, is that can be obtained by buying
Conventional products.
The material of all detections of the present invention is the material that gas chromatography mass spectrometer database Auto-matching provides.
Embodiment 1
Capturing device of the present invention by the cambridge filter of 44 mm as shown in Figure 1, be put into filter disc clamper, filter disc
Coarse one side should close filter disc clamper towards the flue gas of entrance, check and confirm that assembling is appropriate.If trapping in aspiration procedure
Device one end can be put into electronic cigarette, and gas leak phenomenon does not occur, then directly aspirated electronic cigarette insertion trap.But now
Commercially available electronic cigarette suction nozzle is different, if trap one end is mismatched with electronic-cigarette holder, gas leakage occurs for aspiration procedure, then needs
Will between trap and electronic cigarette the good adapter of adjunction seal, prevent that gas leakage occurs in aspiration procedure.
Two are in series between smoking machine trap and suction syringe 30mL dichloromethane absorption bottles are housed, absorbed bottled
Enter and ice salt bath is carried out in insulation barrel, absorption bottle and insulation barrel collectively constitute cold trap trapping device.
Fume collector is removed from smoking machine, is opened, filter disc ultrasonic extraction is taken out with tweezers.Flue gas grain will have been collected
The cambridge filter of phase thing is placed in conical flask, and 20min is extracted at room temperature with 100W power ultrasonics with corresponding extractant, quiet
5min is put, draws appropriate upper layer of extraction liquid, extract is obtained with 0.45 μm of filtering with microporous membrane, loads chromatography bottle and carries out gas phase
Chromatography, measures the content of the target analytes in extract.
Flavor component in certain brand electronics smoke sol is measured, is comprised the following steps that：
Step（1）, electronic cigarette sample is aspirated using electronic cigarette smoking machine, with being placed on smoking machine in trap
Individual layer cambridge filter traps the total granules in electronic cigarette flue gas releaser, traps electronic cigarette 50 mouthfuls of flue gases of continuous sucking
The total granules of releaser；
Suction mode is 55.0 mL of pumping volume, and puff duration 3s, suction frequencies 30s, puffing profile is square wave.
Each electronic cigarette traps 50 mouthfuls with a diameter of 44 mm cambridge filters；Often aspirate filter disc of 50 mouthfuls of replacements；
Step（2）, the cold trap trapping device trapping between trap and smoking machine suction syringe is through cambridge filter
Gas phase composition；
The cold trap trapping device includes the absorption bottle equipped with 30mL dichloromethane of two series connection and for by absorption bottle
Carry out the insulation barrel of ice salt bath；Cold trap trapping unit temp maintains 0 DEG C；
Step（3）, after to be pumped, Fume collector is removed from smoking machine, opens, is taken cambridge filter with tweezers
Go out to be placed in 100 mL conical flasks, while the trapping poured into conical flask in two absorption bottles has the dichloromethane of gas phase composition
Solution, then ultrasonic extraction 30min together, to extract the grain phase part of cambridge filter trapping；
Step（4）, after extraction finishes, pipette 20 mL extracts and added in the separatory funnel of 100 mL in equal volume
Deionized water carries out not good liquor liquid back extraction, is poured into completely in 50 mL concentrate bottles after stratification, then by organic layer, 40
DEG C, be concentrated into 1mL under the conditions of 450 mbar, obtain concentrate；
Step（5）, with gas chromatography mass spectrometer to step（4）Concentrate carry out qualitative and quantitative analysis；Condition is：Chromatography
Column：HP-5MS capillary columns, length × internal diameter × thickness are 30m × 0.25mm × 0.25 μm；Carrier gas：He, constant current mode：Stream
Speed： 1.0 mL/min；Temperature programming：50 DEG C holding 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 ℃；2 μ L of sample size, Splitless injecting samples；Transmission line temperature
Degree：280-300℃；Ionization mode：EI；Ionizing energy：70eV；Ion source temperature：230-250℃；Level Four bar temperature：160℃；
Mass range 35-450aum；Solvent delay：4min；Detection pattern：SCAN and SIM is synchronous.
Wherein：The qualitative analysis of aroma volatile by chem workstation search criteria mass spectrum picture library, in combination with
Related mass spectrogram document parsing, confirms electronic cigarette volatile ingredient, quantitative analysis is pressed by chem workstation data handling system
Areas of peak normalization method carries out calculating the percentage contents for obtaining each component.
The result chromatogram measured is as shown in Fig. 2, volatile ingredient and its relative amount are shown in Table 1：
Certain the brand electronic cigarette volatile ingredient table of table 1
Note：Relative amount is the percentage contents of chromatographic peak area, i.e., the peak area ratio total peak area of each material.
From table 1 and Fig. 2：Present invention determine that 21 components in electronics smoke sol, predominantly aldehydes, phenols, alcohol
Class, esters, ketone etc..This method has the characteristics that easy to operate, analyze 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 by the cambridge filter of 44 mm as shown in Figure 1, be put into filter disc clamper, filter disc
Coarse one side should close filter disc clamper towards the flue gas of entrance, check and confirm that assembling is appropriate.If trapping in aspiration procedure
Device one end can be put into electronic cigarette, and gas leak phenomenon does not occur, then directly aspirated electronic cigarette insertion trap.But now
Commercially available electronic cigarette suction nozzle is different, if trap one end is mismatched with electronic-cigarette holder, gas leakage occurs for aspiration procedure, then needs
Will between trap and electronic cigarette the good adapter of adjunction seal, prevent that gas leakage occurs in aspiration procedure.
Two are in series between smoking machine trap and suction syringe 40mL dichloromethane absorption bottles are housed, absorbed bottled
Enter and ice salt bath is carried out in insulation barrel, absorption bottle and insulation barrel collectively constitute cold trap trapping device.
Fume collector is removed from smoking machine, is opened, filter disc ultrasonic extraction is taken out with tweezers.Flue gas grain will have been collected
The cambridge filter of phase thing is placed in conical flask, and 30min is extracted at room temperature with 100W power ultrasonics with corresponding extractant, quiet
5min is put, draws appropriate upper layer of extraction liquid, extract is obtained with 0.45 μm of filtering with microporous membrane, loads chromatography bottle and carries out gas phase
Chromatography, measures the content of the target analytes in extract.
Flavor component in another brand electronics smoke sol is measured, is comprised the following steps that：
Step（1）, electronic cigarette sample is aspirated using electronic cigarette smoking machine, with being placed on smoking machine in trap
Individual layer cambridge filter traps the total granules in electronic cigarette flue gas releaser, traps electronic cigarette 100 mouthfuls of cigarettes of continuous sucking
The total granules of gas releaser；
Suction mode is 55.0 mL of pumping volume, and puff duration 3s, suction frequencies 30s, puffing profile is square wave.
Each electronic cigarette traps 100 mouthfuls with a diameter of 44 mm cambridge filters；Often aspirate filter disc of 100 mouthfuls of replacements；
Step（2）, the cold trap trapping device trapping between trap and smoking machine suction syringe is through cambridge filter
Gas phase composition；
The cold trap trapping device includes the absorption bottle equipped with 50mL dichloromethane of two series connection and for by absorption bottle
Carry out the insulation barrel of ice salt bath；Cold trap trapping unit temp maintains -1 DEG C；
Step（3）, after to be pumped, Fume collector is removed from smoking machine, opens, is taken cambridge filter with tweezers
Go out to be placed in 100 mL conical flasks, while the trapping poured into conical flask in two absorption bottles has the dichloromethane of gas phase composition
Solution, then ultrasonic extraction 30min together, to extract the grain phase part of cambridge filter trapping；
Step（4）, after extraction finishes, pipette 30 mL extracts and added in the separatory funnel of 100 mL in equal volume
Deionized water carries out not good liquor liquid back extraction, is poured into completely in 50 mL concentrate bottles after stratification, then by organic layer, 40
DEG C, be concentrated into 1mL under the conditions of 450 mbar, obtain concentrate；
Step（5）, with gas chromatography mass spectrometer to step（4）Concentrate carry out qualitative and quantitative analysis；Condition is：Chromatography
Column：HP-5MS capillary columns, length × internal diameter × thickness are 30m × 0.25mm × 0.25 μm；Carrier gas：He, constant current mode：Stream
Speed： 1.0 mL/min；Temperature programming：50 DEG C holding 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 ℃；2 μ L of sample size, Splitless injecting samples；Transmission line temperature
Degree：280-300℃；Ionization mode：EI；Ionizing energy：70eV；Ion source temperature：230-250℃；Level Four bar temperature：160℃；
Mass range 35-450aum；Solvent delay：4min；Detection pattern：SCAN and SIM is synchronous.
Wherein：The qualitative analysis of aroma volatile by chem workstation search criteria mass spectrum picture library, in combination with
Related mass spectrogram document parsing, confirms electronic cigarette volatile ingredient, quantitative analysis is pressed by chem workstation data handling system
Areas of peak normalization method carries out calculating the percentage contents for obtaining each component.
Volatile ingredient and its relative amount are shown in Table 2：
Embodiment 3
Capturing device of the present invention by the cambridge filter of 44 mm as shown in Figure 1, be put into filter disc clamper, filter disc
Coarse one side should close filter disc clamper towards the flue gas of entrance, check and confirm that assembling is appropriate.If trapping in aspiration procedure
Device one end can be put into electronic cigarette, and gas leak phenomenon does not occur, then directly aspirated electronic cigarette insertion trap.But now
Commercially available electronic cigarette suction nozzle is different, if trap one end is mismatched with electronic-cigarette holder, gas leakage occurs for aspiration procedure, then needs
Will between trap and electronic cigarette the good adapter of adjunction seal, prevent that gas leakage occurs in aspiration procedure.
Two are in series between smoking machine trap and suction syringe 40mL dichloromethane absorption bottles are housed, absorbed bottled
Enter and ice salt bath is carried out in insulation barrel, absorption bottle and insulation barrel collectively constitute cold trap trapping device.
Fume collector is removed from smoking machine, is opened, filter disc ultrasonic extraction is taken out with tweezers.Flue gas grain will have been collected
The cambridge filter of phase thing is placed in conical flask, and 60min is extracted at room temperature with 100W power ultrasonics with corresponding extractant, quiet
5min is put, draws appropriate upper layer of extraction liquid, extract is obtained with 0.45 μm of filtering with microporous membrane, loads chromatography bottle and carries out gas phase
Chromatography, measures the content of the target analytes in extract.
Flavor component in brand electronics smoke sol same as Example 1 is measured, is comprised the following steps that：
Step（1）, electronic cigarette sample is aspirated using electronic cigarette smoking machine, with being placed on smoking machine in trap
Individual layer cambridge filter traps the total granules in electronic cigarette flue gas releaser, traps electronic cigarette 20 mouthfuls of flue gases of continuous sucking
The total granules of releaser；
Suction mode is 55.0 mL of pumping volume, and puff duration 3s, suction frequencies 30s, puffing profile is square wave.
Each electronic cigarette traps 20 mouthfuls with a diameter of 44 mm cambridge filters；Often aspirate filter disc of 20 mouthfuls of replacements；
Step（2）, the cold trap trapping device trapping between trap and smoking machine suction syringe is through cambridge filter
Gas phase composition；
The cold trap trapping device includes the absorption bottle equipped with 10mL dichloromethane of two series connection and for by absorption bottle
Carry out the insulation barrel of ice salt bath；Cold trap trapping unit temp maintains -5 DEG C；
Step（3）, after to be pumped, Fume collector is removed from smoking machine, opens, is taken cambridge filter with tweezers
Go out to be placed in 100 mL conical flasks, while the trapping poured into conical flask in two absorption bottles has the dichloromethane of gas phase composition
Solution, then ultrasonic extraction 60min together, to extract the grain phase part of cambridge filter trapping；
Step（4）, after extraction finishes, pipette 10 mL extracts and added in the separatory funnel of 100 mL in equal volume
Deionized water carries out not good liquor liquid back extraction, is poured into completely in 50 mL concentrate bottles after stratification, then by organic layer, 40
DEG C, be concentrated into 1mL under the conditions of 450 mbar, obtain concentrate；
Step（5）, with gas chromatography mass spectrometer to step（4）Concentrate carry out qualitative and quantitative analysis；Condition is：Chromatography
Column：HP-5MS capillary columns, length × internal diameter × thickness are 30m × 0.25mm × 0.25 μm；Carrier gas：He, constant current mode：Stream
Speed： 1.0 mL/min；Temperature programming：50 DEG C holding 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 ℃；2 μ L of sample size, Splitless injecting samples；Transmission line temperature
Degree：280-300℃；Ionization mode：EI；Ionizing energy：70eV；Ion source temperature：230-250℃；Level Four bar temperature：160℃；
Mass range 35-450aum；Solvent delay：4min；Detection pattern：SCAN and SIM is synchronous.
Wherein：The qualitative analysis of aroma volatile by chem workstation search criteria mass spectrum picture library, in combination with
Related mass spectrogram document parsing, confirms electronic cigarette volatile ingredient, quantitative analysis is pressed by chem workstation data handling system
Areas of peak normalization method carries out calculating the percentage contents for obtaining each component.
Its testing result and table 1 are basically identical.
Comparative example 1
Other steps of this comparative example and embodiment 1 are identical, but are not stripped using liquid liquid, after directly being extracted with dichloromethane
Extract carry out gaschromatographic mass spectrometric analysis, the material detected is only 4 kinds, be respectively propane diols, glycerine, nicotine and wheat
This is bright.Chromatogram is as shown in Figure 3.As a result if explanation does not use liquid liquid to be stripped, electronic cigarette tobacco tar solvent glycerin, propane diols meeting
A large amount of interference are produced, largely effect on the accuracy of measurement result.
Basic principle, main feature and the advantages of the present invention of the present invention has been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (4)
1. the assay method of flavor component in a kind of electronics smoke sol, it is characterised in that comprise the following steps：
Step（1）, electronic cigarette sample is aspirated using electronic cigarette smoking machine, with the individual layer being placed on smoking machine in trap
Cambridge filter traps the total granules in electronic cigarette flue gas releaser, traps electronic cigarette 20 ~ 100 mouthfuls of flue gases of continuous sucking
The total granules of releaser；
Step（2）, the cold trap trapping device trapping between syringe is aspirated through the gas phase of cambridge filter used in trap and smoking machine
Component；
The cold trap trapping device include two series connection absorption bottle equipped with 10 ~ 50mL dichloromethane and for by absorption bottle into
The insulation barrel of row ice salt bath；Cold trap trapping unit temp maintains -5 ~ 0 DEG C；
Step（3）, after to be pumped, cambridge filter is taken out and is placed in container, while two absorption bottles are poured into container
In trapping have the dichloromethane solution of gas phase composition, then 20 ~ 60min of ultrasonic extraction together；
Step（4）, after extraction finishes, pipette and isometric deionized water progress liquid liquid back extraction added in 10 ~ 30 mL extracts
Take, be concentrated into 1mL under the conditions of 40 DEG C, 450 mbar after stratification, then by organic layer, obtain concentrate；
Step（5）, with gas chromatography mass spectrometer to step（4）Concentrate carry out qualitative and quantitative analysis；Condition is：Chromatographic column：
HP-5MS capillary columns, length × internal diameter × thickness are 30m × 0.25mm × 0.25 μm；Carrier gas：He, constant current mode：Flow velocity：
1.0 mL/min；Temperature programming：50 DEG C holding 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 ℃；2 μ L of sample size, Splitless injecting samples；Transmission line temperature：
280-300℃；Ionization mode：EI；Ionizing energy：70eV；Ion source temperature：230-250℃；Level Four bar temperature：160℃；Matter
Measure scope 35-450aum；Solvent delay：4min；Detection pattern：SCAN and SIM is synchronous；
The flavor component includes 2,3- dimethyl pyrazines, 2,2,4,6,6- five methylheptanes, benzyl carbinol, 1- methyl -4-
Piperidones, Tetramethylpyrazine, maltol, menthol, 2,6- dimethyl decanes, the chloro- 4- of 2- (4- methoxyphenyls) -6- (4- nitre
Base phenyl) pyrimidine, nicotine, myosmine, 4- ethylpyridines, 3- methyl-cyclopentanes methyl formate, neophytadiene, phthalic acid
Diisobutyl ester, 14 carbamides, western cypress triolefin glycol compound, oleamide, 16 carbamides, erucyl amide；
The flavor component further includes 2- hydroxy-3-methyl -2- cyclopentene-1-ones, ocimenum, tea perfume ketone, isopulegol, 2,
4- dimethyl -1,3- dioxanes, 3- methyl isophthalic acids-cyclopentene, isomenthol, methyl cyclohexanol, vinyl acetate, dextrorotation Sheep's-parsley
Ketone, 4- (2,6,6- trimethyl -1- cyclohexenyl groups) -3- butene-2s -one, (1S, 2S, 5S)-(-) -2- hydroxyl -3- pinanones.
2. the assay method of flavor component in electronics smoke sol according to claim 1, it is characterised in that the electricity
Sub- cigarette smoking machine is the smoking machine that can aspirate the electronic cigarette with jettron and manual switch.
3. the assay method of flavor component in electronics smoke sol according to claim 1, it is characterised in that the electricity
The suction mode of sub- cigarette is 55.0 mL of pumping volume, and puff duration 3s, suction frequencies 30s, puffing profile is square wave.
4. the assay method of flavor component in electronics smoke sol according to claim 1, it is characterised in that each electronics
Cigarette traps 50 mouthfuls with 44 mm cambridge filters of φ.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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Families Citing this family (14)
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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 |
| CN107189857B (en) * | 2017-07-07 | 2023-10-27 | 重庆中烟工业有限责任公司 | Device and method for preparing smoke flavor |
| 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 |
| CN108088946A (en) * | 2017-10-21 | 2018-05-29 | 云南中烟工业有限责任公司 | A kind of cigarette flavors additive distribution determination method under flue gas different-grain diameter |
| 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 |
| CN108125277B (en) * | 2018-03-21 | 2021-03-05 | 福建中烟工业有限责任公司 | Electronic cigarette and manufacturing method thereof |
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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 |
| CN110823649A (en) * | 2019-10-21 | 2020-02-21 | 河南中烟工业有限责任公司 | Method for collecting and detecting organic acid in cigarette mainstream smoke |
| CN113720934B (en) * | 2021-08-20 | 2023-06-30 | 中国烟草总公司郑州烟草研究院 | Method for detecting aroma components in main stream smoke of cigarettes |
| CN113720937B (en) * | 2021-08-30 | 2023-06-27 | 深圳市真味生物科技有限公司 | Method for measuring content of cooling agent in electronic smoke sol |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6440223B1 (en) * | 2000-02-15 | 2002-08-27 | R. J. Reynolds Tobacco Co. | Smoking article containing heat activatable flavorant-generating material |
| BG65650B1 (en) * | 2004-09-01 | 2009-04-30 | Солея ДАНЬО | Method for the evaluation of the aroma of tobacco smoke and classification by aroma of types and varieties of tobaccos |
| CN101566535A (en) * | 2009-06-03 | 2009-10-28 | 湖南中烟工业有限责任公司 | Smoking machine-mainstream flue gas cold trap integrated device and using method thereof |
| CN103940639A (en) * | 2014-04-29 | 2014-07-23 | 云南中烟工业有限责任公司 | Method for capturing main components in smoke releasing substances of electronic cigarette |
| CN104316634A (en) * | 2014-10-24 | 2015-01-28 | 贵州中烟工业有限责任公司 | Determination method of volatile organic acids in cigarette mainstream smoke |
| CN104655778A (en) * | 2015-02-16 | 2015-05-27 | 国家烟草质量监督检验中心 | Method for determining contents of 18 kinds of volatile and semi-volatile organic compounds in electronic cigarette smoke liquid and aerosol |
-
2016
- 2016-05-18 CN CN201610331883.3A patent/CN105842378B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6440223B1 (en) * | 2000-02-15 | 2002-08-27 | R. J. Reynolds Tobacco Co. | Smoking article containing heat activatable flavorant-generating material |
| BG65650B1 (en) * | 2004-09-01 | 2009-04-30 | Солея ДАНЬО | Method for the evaluation of the aroma of tobacco smoke and classification by aroma of types and varieties of tobaccos |
| CN101566535A (en) * | 2009-06-03 | 2009-10-28 | 湖南中烟工业有限责任公司 | Smoking machine-mainstream flue gas cold trap integrated device and using method thereof |
| CN103940639A (en) * | 2014-04-29 | 2014-07-23 | 云南中烟工业有限责任公司 | Method for capturing main components in smoke releasing substances of electronic cigarette |
| CN104316634A (en) * | 2014-10-24 | 2015-01-28 | 贵州中烟工业有限责任公司 | Determination method of volatile organic acids in cigarette mainstream smoke |
| CN104655778A (en) * | 2015-02-16 | 2015-05-27 | 国家烟草质量监督检验中心 | Method for determining contents of 18 kinds of volatile and semi-volatile organic compounds in electronic cigarette smoke liquid and aerosol |
Non-Patent Citations (4)
| Title |
|---|
| An inventory of methods suitable to assess additive-induced characterising flavours of tobacco products;Reinskje Talhout et al;《Drug and Alcohol Dependence》;20151230;第161卷;9-14 * |
| Headspace solid-phase microextraction and on-fibre derivatization of primary aromatic amines for their determination by pyrolysis to aryl isothiocyanates and gas chromatography-mass spectrometry;Nisha Sharma et al;《Analytical Methods》;20110307;第3卷;970-976 * |
| 制丝关键工序对细支卷烟燃烧温度及主流烟气成分的影响;田忠 等;《中国烟草学报》;20151231;第21卷(第6期);19-26 * |
| 电子烟气溶胶的研究进展;蔡君兰 等;《中国烟草学报》;20160229;第22卷(第1期);138-146 * |
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