CN108088946A - A kind of cigarette flavors additive distribution determination method under flue gas different-grain diameter - Google Patents
A kind of cigarette flavors additive distribution determination method under flue gas different-grain diameter Download PDFInfo
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- CN108088946A CN108088946A CN201710988324.4A CN201710988324A CN108088946A CN 108088946 A CN108088946 A CN 108088946A CN 201710988324 A CN201710988324 A CN 201710988324A CN 108088946 A CN108088946 A CN 108088946A
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- cigarette
- flue gas
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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
Abstract
The present invention relates to a kind of cigarette flavors additive under flue gas different-grain diameter distribution determination method, belong to cigarette smoke flavoring and casing technical field, the present invention is to add in essence and flavoring agent in cigarette, with electronics low pressure impactor（ELPI）Trap the particulate matter under cigarette flue gas aerosol different-grain diameter, the analysis of flavoring and casing object is carried out with gas chromatography-mass spectrometry after processing, the particle diameter distribution situation of flavoring and casing object is obtained, basic data support is provided for the flavoring and casing technology of cigarette.
Description
Technical field
The invention belongs to cigarette smoke flavoring and casing technical fields, and a kind of specifically cigarette flavors additive is in flue gas
Distribution determination method and application under different-grain diameter.
Background technology
Perfuming cigarette charging can remove the miscellaneous gas of flue gas, promote flue gas mouthfeel, improve flue gas style, so as to promote cigarette cigarette
Gas aesthetic quality meets the needs of consumption is to cigarette preference.In aspiration procedure, cigarette additive can occur a series of cigarette
Burning, cracking, volatilization, distillation the effects that, it is final some into cigarette flue gas aerosol, influence the object of flue gas aerosol
Reason and chemical property, and then influence the inherent quality of flue gas.Due to the physical chemical differences of tobacco additive agent so that its with
Flue gas causes different-grain diameter distributional difference when entering aerosol, based on oral cavity and nasal cavity to the sensorial differences of different-grain diameter flue gas,
So as to influence the improvement of flue gas, therefore analyze different tobacco additive agents and perfuming cigarette is added in the distributional difference of different-grain diameter
Material is of great significance.Presently relevant researcher is to indoles, nicotine, ethyl phthalate, norphytene, planting in cigarette smoke
The distribution of diene, total granules and copper in different-grain diameter aerosol finds the burst size of these ingredients as grain size increases
In first increasing the trend reduced afterwards, but the burst size on unit mass granule phase substance（Concentration）It is then different, indoles, nicotine, phthalandione two
Concentration of the ethyl ester in medium grain size granule phase substance is higher, the concentration of norphytene, neophytadiene in entire particle size range basic one
It causes, concentration of the copper then in big grain size and small particle granule phase substance is higher, shows that different flue gas compounds are distributed under different-grain diameter
There are larger differences.The position deposited after being entered the respiratory system due to different-grain diameter cigarette flue gas aerosol particle is different, there is mouth
Chamber residual, nasal cavity residual and lung's residual etc., most of aerosol in large grain size particle remains in oral cavity and nasal cavity, and small particle gas is molten
Glue is remained in lung, therefore, is easier to be perceived by oral cavity and nasal cavity in the more tobacco additive agent of big particle diameter distribution.Seldom grind
The person of studying carefully pays close attention to distribution of the perfuming cigarette charging compound under flue gas different-grain diameter aerosol, is fed based on perfuming cigarette to cigarette
Flue gas aesthetic quality influences, it is necessary to perfuming cigarette charging chemical composition distribution situation on cigarette smoke different-grain diameter is studied,
So as to realize accurate perfuming cigarette charging purpose.
The content of the invention
The purpose of the present invention is based on above-mentioned prior art situation and perfuming cigarette feeding technique demand, provides a kind of volume
Cigarette perfume essence spice additive Evaluation on distribution method under flue gas different-grain diameter obtains flavoring and casing object by this method and exists
Cigarette smoke different-grain diameter distribution situation provides technical support for the accurate flavoring and casing of cigarette.
The object of the present invention is achieved like this, and cigarette is after flavoring and casing, by electronics low pressure impactor（ELPI）It catches
Collect the particulate matter under cigarette flue gas aerosol different-grain diameter, use gas chromatograph-mass spectrometer (GC-MS) after processing（GC-MS）Added
The analysis of perfume charging object obtains point of the flavoring and casing object under different suction modes in cigarette smoke different-grain diameter
Cloth situation provides technical support for the accurate flavoring and casing of cigarette.
The method of the present invention includes the following steps：
Step（1）Tobacco additive agent object is made an addition to the 0.005 ~ 2% of pipe tobacco weight in cigarette, in cigarette standard equilibration
Under the conditions of balance 48h, carry out cigarette smoking with one channel smoke sucking machine, suction mode is 10 ~ 150 mL of pumping volume, puff duration
Time is 0.5 ~ 4s, and Puffing interval is 30 ~ 240 s, and puffing profile is bell or square.
Step（2）Flue gas imports ELPI after diluting 10 ~ 5000 times, is trapped with the 12 grades of filter disc aluminium foils equipped in advance on ELPI
Cigarette flue gas aerosol, filter disc trap the flue gas aerosol of 1 ~ 20 cigarette；
Step（3）The aluminium foil filter disc for trapping granule phase substance is placed in 10 mL vials, adds in the methanol solution of 1 ~ 50 mL, ultrasound
5 ~ 50min is extracted, extraction solution filters through 0.22 μm of organic phase mocromembrane, adds in internal standard compound, then use gas chromatography-mass spectrography
Instrument GC-MS is measured；
The gas chromatographic detection condition is as follows：
Chromatographic column：INNOWAX elastic capillary-columns, stationary phase are polyethylene glycol, and specification is 30 m of length × internal diameter, 0.25 mm
0.25 um df of id × film thickness；Injector temperature：280 ℃；Carrier gas：Helium（The % of purity >=99.999）, constant current flow velocity：1.0
mL/min；Sample size：1 μL；Split sampling, split ratio 10:1；Temperature program：35 DEG C of initial temperature keeps 5 min, then
240 DEG C are warming up to the rate of 3 DEG C/min, and keeps 15 min.
The Mass Spectrometer Method condition is as follows：Ionization mode：Electron bombardment ionization source（EI）；Transmission line temperature：240 ℃；Ion
Source temperature：230 ℃；Ionizing energy：70 eV；Solvent delay：5 min；Scanning range：30~350；Scan pattern：Total ion current
Scanning.
Step（4）According to the amount and grain size of object on different-grain diameter, the grain size distribution of object is drawn.
The step（3）Middle internal standard compound can be according to substance similar in the property selection property for adding essence and flavoring agent.
The step（4）Middle grain size distribution can draw 0.1 ~ 10 μm of particle diameter distribution.
The advantages of present invention possesses and effect：This method is easy to operate, as a result accurately, applied widely, the measurement result
Available for the particle diameter distribution for evaluating various types of essence spice for cigarette additives, this method can be effectively used for evaluating different essence
Fragrance influences cigarette smoke aesthetic quality, and provides foundation for the accurate flavoring and casing of cigarette.
Description of the drawings
Fig. 1 is grain size distribution of the glycerine additive in different-grain diameter flue gas.
Fig. 2 is grain size distribution of the vanillic aldehyde additive in different-grain diameter flue gas.
Fig. 3 is grain size distribution of the furanone additive in different-grain diameter flue gas.
Fig. 4 is grain size distribution of the grape sugar additives in different-grain diameter flue gas.
Fig. 5 is grain size distribution of the levulic acid additive in different-grain diameter flue gas.
Fig. 6 is grain size distribution of the isoeugenol additive in different-grain diameter flue gas.
Specific embodiment
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 it is carried out according to product description.Reagents or instruments used without specified manufacturer, being can be by buying what is obtained
Conventional products.Below by embodiment, the present invention will be further described,
Embodiment 1
Glycerine is common tobacco additive agent, has good humectation effect to pipe tobacco and improves flue gas aesthetic quality.Cigarette
2% glycerine is added in cigarette, 48h is balanced under 22 DEG C of temperature, 60% humidity, cigarette smoking is carried out with one channel smoke sucking machine, is taken out
60 mL of capacity is inhaled, puff duration 1s, Puffing interval is 100 s, and puffing profile is bell；By flue gas through dilution
（500 times of extension rate）After import ELPI, trap cigarette flue gas aerosol, filter disc with 12 grades of filter disc aluminium foils being equipped in advance on ELPI
Trap 1 cigarette flue gas aerosol；Then every grade of filter disc is respectively placed in 12 10mL vials, sequentially adds 10.0 mL
Methanol solution, ultrasonic extraction 20min, is removed, and extraction solution is filtered through 0.22 μm of organic phase mocromembrane, adds in 1,4-butanediol internal standard
Object solution, then GC-MS be measured, the concentration of propylene glycol is obtained, so as to according to particle size range<0.14 μm、0.26 μm、
0.43 μm, 0.72 μm and>1.17 μm of drafting glycerine distribution maps, as shown in Figure 1.
The gas chromatographic detection condition is as follows.Chromatographic column：INNOWAX elastic capillary-columns, stationary phase are poly- second two
Alcohol, specification are 30 m of length × internal diameter, 0.25 mm id × 0.25 um df of film thickness；Injector temperature：280 ℃；Carrier gas：Helium
（The % of purity >=99.999）, constant current flow velocity：1.0 mL/min；Sample size：1 μL；Split sampling, split ratio 10:1；Heat up journey
Sequence：35 DEG C of initial temperature keeps 5 min, is then warming up to 240 DEG C with the rate of 3 DEG C/min, and keeps 15 min.
The Mass Spectrometer Method condition is as follows.Ionization mode：Electron bombardment ionization source（EI）；Transmission line temperature：240 ℃；Ion
Source temperature：230 ℃；Ionizing energy：70 eV；Solvent delay：5 min；Scanning range：30~350；Scan pattern：Total ion current
Scanning.
Embodiment 2
Vanillic aldehyde is most common cigarette flavors, can improve flue gas style and features well.0.01% is added in Cigarette
Vanillic aldehyde balances 48h under 22 DEG C of temperature, 60% humidity, and cigarette smoking is carried out with one channel smoke sucking machine, 150 mL of pumping volume,
Puff duration is 2 s, and Puffing interval is 60 s, and puffing profile is square；By flue gas through dilution（Extension rate 1000
Times）After import ELPI, trap cigarette flue gas aerosol with 12 grades of filter disc aluminium foils being equipped in advance on ELPI, filter disc traps 10 cigarette
Flue gas aerosol；Then every grade of filter disc is respectively placed in 12 10 mL vials, sequentially adds 2.0 mL methanol solutions, surpassed
Sound extracts 30min, and extraction solution is filtered through 0.22 μm of organic phase mocromembrane, adds in phenethyl acetate internal standard substance solution, then GC-
MS is measured, and obtains the concentration of vanillic aldehyde, so as to according to particle size range<0.1 μm, 0.1~1.0 μm and>1.0 μm of drafting chinese cymbidiums
Plain distribution map, as shown in Figure 2.
The gas chromatographic detection condition is as follows.Chromatographic column：INNOWAX elastic capillary-columns, stationary phase are poly- second two
Alcohol, specification are 30 m of length × internal diameter, 0.25 mm id × 0.25 um df of film thickness；Injector temperature：280 ℃；Carrier gas：Helium
（The % of purity >=99.999）, constant current flow velocity：1.0 mL/min；Sample size：1 μL；Split sampling, split ratio 10:1；Heat up journey
Sequence：35 DEG C of initial temperature keeps 5 min, is then warming up to 240 DEG C with the rate of 3 DEG C/min, and keeps 15 min.
The Mass Spectrometer Method condition is as follows.Ionization mode：Electron bombardment ionization source（EI）；Transmission line temperature：240 ℃；Ion
Source temperature：230 ℃；Ionizing energy：70 eV；Solvent delay：5 min；Scanning range：30~350；Scan pattern：Total ion current
Scanning.
Embodiment 3
Furanone is a kind of important fragrance-enhancing tobacco agent, has the strong caramel odour that bakes, characteristic perfume is fruity, burnt odor,
Caramel and pineapple sample fragrance have apparent flavouring modification effect.0.1% furanone is added in Cigarette, 22 DEG C of temperature,
48h is balanced under 60% humidity, carries out cigarette smoking with one channel smoke sucking machine, pumping volume 75mL, puff duration 4s take out
Suction interval time is 30 s, and puffing profile is bell；By flue gas through dilution（2000 times of extension rate）After import ELPI, use ELPI
On equip in advance 12 grades of filter disc aluminium foils trapping cigarette flue gas aerosol, filter disc trap 5 cigarette flue gas aerosols；Then by every grade
Filter disc is respectively placed in 12 10 mL vials, sequentially adds 20.0 mL methanol solutions, and ultrasonic extraction 10min extracts solution
It is filtered through 0.22 μm of organic phase mocromembrane, adds in cyclopentanol internal standard substance solution, then GC-MS is measured, and obtains the dense of furanone
Degree, so as to according to particle size range<0.1 μm, 0.1~0.5 μm, 0.5~1.0 μm and>1.0 μm of drafting furanone distribution maps, such as scheme
Shown in 3.
The gas chromatographic detection condition is as follows.Chromatographic column：INNOWAX elastic capillary-columns, stationary phase are poly- second two
Alcohol, specification are 30 m of length × internal diameter, 0.25 mm id × 0.25 um df of film thickness；Injector temperature：280 ℃；Carrier gas：Helium
（The % of purity >=99.999）, constant current flow velocity：1.0 mL/min；Sample size：1 μL；Split sampling, split ratio 10:1；Heat up journey
Sequence：35 DEG C of initial temperature keeps 5 min, is then warming up to 240 DEG C with the rate of 3 DEG C/min, and keeps 15 min.
The Mass Spectrometer Method condition is as follows.Ionization mode：Electron bombardment ionization source（EI）；Transmission line temperature：240 ℃；Ion
Source temperature：230 ℃；Ionizing energy：70 eV；Solvent delay：5 min；Scanning range：30~350；Scan pattern：Total ion current
Scanning.
Embodiment 4
Glucose is one of main component of tobacco charging, has seasoning and humectation effect, can mitigate flue gas irritation and improvement
Pleasant impression, and the camerlsed of flue gas can be increased etc..1% glucose is added in Cigarette, is balanced under 22 DEG C of temperature, 60% humidity
48h carries out cigarette smoking, 10 mL of pumping volume with one channel smoke sucking machine, and puff duration is 3 s, and Puffing interval is
240 s, puffing profile are square；By flue gas through dilution（50 times of extension rate）After import ELPI, with 12 equipped in advance on ELPI
Grade filter disc aluminium foil trapping cigarette flue gas aerosol, filter disc trap 15 cigarette flue gas aerosols；Then every grade of filter disc is put respectively
In 12 10 mL vials, 30.0 mL methanol solutions, ultrasonic extraction 5min are sequentially added, extraction solution has through 0.22 μm
Machine phase mocromembrane filters, and adds in xylitol internal standard substance solution, and then GC-MS is measured, and obtains the concentration of glucose, thus according to
Different-grain diameter draws glucose profiles, as shown in Figure 4.
The gas chromatographic detection condition is as follows.Chromatographic column：INNOWAX elastic capillary-columns, stationary phase are poly- second two
Alcohol, specification are 30 m of length × internal diameter, 0.25 mm id × 0.25 um df of film thickness；Injector temperature：280 ℃；Carrier gas：Helium
（The % of purity >=99.999）, constant current flow velocity：1.0 mL/min；Sample size：1 μL；Split sampling, split ratio 10:1；Heat up journey
Sequence：35 DEG C of initial temperature keeps 5 min, is then warming up to 240 DEG C with the rate of 3 DEG C/min, and keeps 15 min.
The Mass Spectrometer Method condition is as follows.Ionization mode：Electron bombardment ionization source（EI）；Transmission line temperature：240 ℃；Ion
Source temperature：230 ℃；Ionizing energy：70 eV；Solvent delay：5 min；Scanning range：30~350；Scan pattern：Total ion current
Scanning.
Embodiment 5
Levulic acid can assign flue gas tart flavour, and neutralize alkaline matter and mitigate thorn as a kind of important fragrance in tobacco
Swash and improve pleasant impression.0.5% levulic acid is added in Cigarette, 48h is balanced under 22 DEG C of temperature, 60% humidity, uses one channel
Smoking machine carries out cigarette smoking, and 100 mL of pumping volume, puff duration 2s, Puffing interval is 150 s, and suction is bent
Line is bell；By flue gas through dilution（5000 times of extension rate）After import ELPI, with the 12 grades of filter disc aluminium foils equipped in advance on ELPI
Cigarette flue gas aerosol is trapped, filter disc traps 3 cigarette flue gas aerosols；Then every grade of filter disc is respectively placed in 12 10 mL
In vial, 15.0 mL methanol solutions are sequentially added, ultrasonic extraction 45min, extraction solution is through 0.22 μm of organic phase mocromembrane mistake
Filter, adds in deuterated valeric acid-d9 internal standard substance solutions, and then GC-MS is measured, and obtains the concentration of levulic acid, so as to according to not
Levulic acid distribution map is drawn with grain size, as shown in Figure 5.
The gas chromatographic detection condition is as follows.Chromatographic column：INNOWAX elastic capillary-columns, stationary phase are poly- second two
Alcohol, specification are 30 m of length × internal diameter, 0.25 mm id × 0.25 um df of film thickness；Injector temperature：280 ℃；Carrier gas：Helium
（The % of purity >=99.999）, constant current flow velocity：1.0 mL/min；Sample size：1 μL；Split sampling, split ratio 10:1；Heat up journey
Sequence：35 DEG C of initial temperature keeps 5 min, is then warming up to 240 DEG C with the rate of 3 DEG C/min, and keeps 15 min.
The Mass Spectrometer Method condition is as follows.Ionization mode：Electron bombardment ionization source（EI）；Transmission line temperature：240 ℃；Ion
Source temperature：230 ℃；Ionizing energy：70 eV；Solvent delay：5 min；Scanning range：30~350；Scan pattern：Total ion current
Scanning.
Embodiment 6
Isoeugenol has eugenol fragrance, pleasantly sweet, has elegant, the soft pungent fragrance of caramel, is widely used as tobacco essence.
1.5% isoeugenol is added in Cigarette, 48h is balanced under 22 DEG C of temperature, 60% humidity, cigarette is carried out with one channel smoke sucking machine
Suction, 30 mL of pumping volume, puff duration are 0.5 s, and Puffing interval is 120 s, and puffing profile is square；It will
Flue gas is through dilution（3000 times of extension rate）After import ELPI, trap cigarette smoke with 12 grades of filter disc aluminium foils being equipped in advance on ELPI
Aerosol, filter disc trap 20 cigarette flue gas aerosols；Then every grade of filter disc is respectively placed in 12 10 mL vials, according to
40.0 mL methanol solutions of secondary addition, 15 min of ultrasonic extraction, extraction solution are filtered through 0.22 μm of organic phase mocromembrane, add in 2,4-
Xylenol-d10 internal standard substance solutions, then GC-MS be measured, the concentration of isoeugenol is obtained, so as to according to different grains
Isoeugenol distribution map is drawn in footpath, as shown in Figure 3.
The gas chromatographic detection condition is as follows.Chromatographic column：INNOWAX elastic capillary-columns, stationary phase are poly- second two
Alcohol, specification are 30 m of length × internal diameter, 0.25 mm id × 0.25 um df of film thickness；Injector temperature：280 ℃；Carrier gas：Helium
（The % of purity >=99.999）, constant current flow velocity：1.0 mL/min；Sample size：1 μL；Split sampling, split ratio 10:1；Heat up journey
Sequence：35 DEG C of initial temperature keeps 5 min, is then warming up to 240 DEG C with the rate of 3 DEG C/min, and keeps 15 min.
The Mass Spectrometer Method condition is as follows.Ionization mode：Electron bombardment ionization source（EI）；Transmission line temperature：240 ℃；Ion
Source temperature：230 ℃；Ionizing energy：70 eV；Solvent delay：5 min；Scanning range：30~350；Scan pattern：Total ion current
Scanning.
Basic principle, main feature and the advantages of the present invention of the present invention has been shown and described above.The present invention is from upper
The limitation of embodiment is stated, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, this
A little changes and improvements all fall within the protetion scope of the claimed invention.The claimed scope of the invention is by appended claims
And its equivalent thereof.
Claims (3)
1. the assay method that a kind of cigarette flavors additive is distributed under flue gas different-grain diameter, it is characterised in that including following
Step：
Step（1）Tobacco additive agent object is made an addition to the 0.005 ~ 2% of pipe tobacco weight in cigarette, in cigarette standard equilibration
Under the conditions of balance 48h, aspirated with one channel smoke sucking machine, suction mode be 10 ~ 150 mL of pumping volume, puff duration
For 0.5 ~ 4 s, Puffing interval is 30 ~ 240 s, and puffing profile is bell or square；
Step（2）Flue gas imports ELPI after diluting 10 ~ 5000 times, and cigarette is trapped with the 12 grades of filter disc aluminium foils equipped in advance on ELPI
Flue gas aerosol, filter disc trap the flue gas aerosol of 1 ~ 20 cigarette；
Step（3）The aluminium foil filter disc for trapping granule phase substance is placed in 10 mL vials, adds in the methanol solution of 1 ~ 50 mL, ultrasound
5 ~ 50min is extracted, extraction solution filters through 0.22 μm of organic phase mocromembrane, adds in internal standard compound, then use gas chromatography-mass spectrography
Instrument GC-MS is measured；
The gas chromatographic detection condition is as follows：
Chromatographic column：INNOWAX elastic capillary-columns, stationary phase are polyethylene glycol, and specification is 30 m of length × internal diameter, 0.25 mm
0.25 um df of id × film thickness；Injector temperature：280 ℃；Carrier gas：Helium（The % of purity >=99.999）, constant current flow velocity：1.0
mL/min；Sample size：1 μL；Split sampling, split ratio 10:1；Temperature program：35 DEG C of initial temperature keeps 5 min, then
240 DEG C are warming up to the rate of 3 DEG C/min, and keeps 15 min；
The Mass Spectrometer Method condition is as follows：Ionization mode：Electron bombardment ionization source（EI）；Transmission line temperature：240 ℃；Ion source temperature
Degree：230 ℃；Ionizing energy：70 eV；Solvent delay：5 min；Scanning range：30~350；Scan pattern：Total ion current is swept
It retouches；
Step（4）According to the amount and grain size of object on different-grain diameter, the grain size distribution of object is drawn.
2. cigarette flavors additive according to claim 1 Evaluation on distribution method under flue gas different-grain diameter, special
Sign is：The step（3）Middle internal standard compound substance according to similar in the property selection property of addition essence and flavoring agent.
3. cigarette flavors additive according to claim 1 Evaluation on distribution method under flue gas different-grain diameter, special
Sign is：The step（4）Middle grain size distribution draws 0.1 ~ 10 μm of particle diameter distribution.
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