CN106501438A - For analyzing analytical equipment and the analysis method of tobacco juice composition - Google Patents
For analyzing analytical equipment and the analysis method of tobacco juice composition Download PDFInfo
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- CN106501438A CN106501438A CN201611258695.9A CN201611258695A CN106501438A CN 106501438 A CN106501438 A CN 106501438A CN 201611258695 A CN201611258695 A CN 201611258695A CN 106501438 A CN106501438 A CN 106501438A
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- tobacco juice
- sample bottle
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- tube
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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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/08—Preparation using an enricher
Abstract
The present invention provides a kind of analytical equipment and analysis method for analyzing tobacco juice composition, and the air pump, sample bottle, the first connecting tube, trap tube and the second connecting tube in analytical equipment connects into the gas flow loop of closed loop；Sample tobacco juice is added in sample bottle, using air pump to sample bottle in tobacco juice purged and volatile ingredient and semi-volatility component in tobacco juice is evaporated and is entered in trap tube, and air-flow is in air pump, sample bottle, first connecting tube, circulate in the gas flow loop of the closed loop that trap tube and the second connecting tube are connected into, so trap tube can fully be enriched with volatile ingredient and semi-volatility component in tobacco juice, and in trap tube, it is filled with activated carbon granule, activated carbon granule high adsorption capacity, the volatile ingredient and semi-volatility component in tobacco juice can substantially more be adsorbed；Thus, a kind of analytical equipment and analysis method for analyzing tobacco juice composition of the invention can improve analysis efficiency.
Description
Technical field
The present invention relates to a kind of analytical equipment and analysis method for analyzing tobacco juice composition, more particularly to one kind is used for
The analytical equipment of analysis electronic cigarette liquid composition and analysis method.
Background technology
Electronic cigarette liquid is typically made up of propane diols, glycerine, nicotine and odor additive.Electronic cigarette is will by electrical heating
Electronic cigarette liquid is atomized into gas, sucks for smoker.In this Smoking regime, the volatile ingredient in electronic cigarette liquid and half volatilizees
Property composition be the important factor in order for determining electronic cigarette sensory evaluating smoking and security.
The flavor component in electronic cigarette liquid is analyzed using solvent extraction method routinely in prior art, it is organic that the method is used
Quantity of solvent is big, concentrates that time-consuming after extraction again, and substantial amounts of glycerine, propane diols can cover the fragrance of some traces during solvent extraction
Composition.Headspace solid-phase microextraction (HS-SPE) method can be prevented effectively from the interference of matrix composition and solvent, but to half volatile into
The absorption for dividing not exclusively, and can lose the volatile fragrance of some low boilings in analyzing.Fragrance matter to some traces, this
Method is also difficult to trap.
Volatilization in electronic cigarette liquid and the analysis of semi-volatility component are present in prior art and are enriched with unstable, enriching quantity
Low, semi-volatility component concentration effect is poor, and the shortcomings of analyze inaccurate and not comprehensive.Especially, adopt in prior art
Typically poor to the adsorption capacity of all kinds of flavor components in tobacco juice using capillary column, the first-class instrument of SPE, adsorption capacity
Relatively low so that bioaccumulation efficiency is relatively low.
Content of the invention
The shortcoming of prior art in view of the above, it is an object of the invention to provide a kind of for analyzing tobacco juice composition
Analytical equipment and analysis method, it is possible to increase analysis efficiency.
For achieving the above object, a kind of analytical equipment for analyzing tobacco juice composition that the present invention is provided adopts following technology
Scheme：A kind of analytical equipment for analyzing tobacco juice composition, including sample bottle, air pump and trap tube, the air pump has air inlet
Mouth and gas outlet, are connected with the first connecting tube, connect between sample bottle and trap tube between the gas outlet of the air pump and sample bottle
Be connected with the 3rd connecting tube between the air inlet for being connected to the second connecting tube, trap tube and air pump, the air pump, sample bottle, first
Connecting tube, trap tube and the second connecting tube connect into the gas flow loop of closed loop；Activated carbon granule is filled with the trap tube.
Preferably, first connecting tube, the second connecting tube are detachably connected on sample bottle；The trap tube is removable
It is connected to unloading between the second connecting tube and the 3rd connecting tube.
Preferably, 60-80 mesh activated carbon granules are filled with the trap tube.
Preferably, 20-30mg activated carbon granules are filled with the trap tube.
The present invention also provides a kind of analysis method for analyzing tobacco juice composition, adopts the following technical scheme that：One kind is used for
The analysis method of analysis tobacco juice composition, using described in above-mentioned technical proposal or its arbitrary preferred technical scheme for analyzing cigarette
The analytical equipment of liquid composition carries out operation, comprises the steps：
1) sample：Take tobacco juice sample to be added in sample bottle, rotary sample bottle makes tobacco juice be uniformly distributed in sample bottle, use
Then first connecting tube and the second connecting tube are inserted in sample bottle by bottle cap sealing bottleneck from bottle cap；
2) purge：Tobacco juice during air pump is opened to sample bottle is purged；
3) it is enriched with：The volatile ingredient in tobacco juice and semi-volatility component in sample bottle is evaporated and passes through the second company
Adapter is entered in trap tube, the volatile ingredient in the air-flow that the activated carbon granule enrichment in trap tube is entered in trap tube
And semi-volatility component；
4) elute：After the completion of enrichment, activated carbon trap tube is removed, chromatogram will be eluted to by enriched composition using organic solvent
In bottle, eluent is obtained；
5) analyze：Eluent is carried out gaschromatographic mass spectrometric analysis, you can volatilization and half in Qualitative and quantitative analysis tobacco juice
Volatile ingredient.
Preferably, above-mentioned steps 1) in, taken tobacco juice be 1-2mL.
Preferably, above-mentioned steps 2) in, air pump gas outlet flow velocity be 500-800ml/min.
Preferably, above-mentioned steps 3) in, enrichment time be 1-2 hours.
Preferably, above-mentioned steps 4) in, the organic solvent is dichloromethane or alcohol solvent.
Preferably, above-mentioned steps 4) in, 300-500 μ L.
As described above, a kind of analytical equipment and analysis method for analyzing tobacco juice composition according to the present invention, with
Lower beneficial effect：The present invention a kind of analytical equipment for analyzing tobacco juice composition in air pump, sample bottle, the first connecting tube,
Trap tube and the second connecting tube connect into the gas flow loop of closed loop；Sample tobacco juice is added in sample bottle, using air pump to sample
Tobacco juice in bottle is purged and volatile ingredient and semi-volatility component in tobacco juice is evaporated and is entered into trap tube
In, and air-flow is in the gas flow loop of the closed loop that air pump, sample bottle, the first connecting tube, trap tube and the second connecting tube are connected into
Circulate, so trap tube fully can be enriched with the volatile ingredient and semi-volatility component, and trap tube in tobacco juice
Be filled with activated carbon granule, activated carbon granule high adsorption capacity, substantially more can adsorb volatile ingredient in tobacco juice and
Semi-volatility component；Thus, a kind of analytical equipment for analyzing tobacco juice composition of the invention can improve analysis efficiency.This
Bright a kind of for analyzing a kind of analytical equipment for analyze tobacco juice composition of the analysis method of tobacco juice composition using the present invention
Operation is carried out, there is above-mentioned beneficial effect certainly, here is omitted.
Description of the drawings
Fig. 1 show a kind of structural representation for analyzing the analytical equipment of tobacco juice composition of the present invention；
Fig. 2 is shown as in embodiment 3 certain for utilizing a kind of analysis method for analyzing tobacco juice composition of the present invention to obtain
Brand C electronic cigarette liquid gaschromatographic mass spectrometry TIC.
Component label instructions
1 sample bottle, 6 gas outlet
2 air pump, 7 first connecting tube
3 trap tube, 8 second connecting tube
The 3rd connecting tube of 4 activated carbon granule 9
5 air inlets
Specific embodiment
Embodiments of the present invention are illustrated by particular specific embodiment below, those skilled in the art can be by this explanation
Content disclosed by book understands other advantages and effect of the present invention easily.
It should be clear that structure, ratio, size depicted in this specification institute accompanying drawings etc., only in order to coordinating specification to be taken off
The content that shows, so that those skilled in the art understands and reads, is not limited to enforceable qualifications of the invention, therefore
Do not have technical essential meaning, the modification of any structure, the change of proportionate relationship or the adjustment of size are not affecting the present invention
Under the effect that can be generated and the purpose that can be reached, all should still fall and the model that can cover is obtained in disclosed technology contents
In enclosing.Meanwhile, in this specification cited such as " on ", D score, "left", "right", the term of " centre " and " " etc., be also only
It is easy to described to understand, and is not used to limit enforceable scope of the invention, its relativeness is altered or modified, without essence
Under change technology contents, when being also considered as enforceable category of the invention.
As shown in figure 1, the present invention provides a kind of analytical equipment for analyzing tobacco juice composition, including sample bottle 1, air pump 2
With trap tube 3, the air pump 2 has air inlet 5 and gas outlet 6, is connected between the gas outlet 6 of the air pump 2 and sample bottle 1
First connecting tube 7, is connected between sample bottle 1 and trap tube 3 between the air inlet 5 of the second connecting tube 8, trap tube 3 and air pump 2
The 3rd connecting tube 9 is connected with, the air pump 2, sample bottle 1, the first connecting tube 7, trap tube 3 and the second connecting tube 8 are connected into and closed
The gas flow loop of ring；Activated carbon granule 4 is filled with the trap tube 3.Utilize the present invention one kind be used for analyze tobacco juice into
During the analytical equipment for dividing, sample tobacco juice is added in sample bottle 1, the tobacco juice in sample bottle 1 is purged using air pump 2 and made
Volatile ingredient and semi-volatility component in tobacco juice is evaporated and is entered in trap tube 3, and air-flow is in air pump 2, sample
Circulate in the gas flow loop of the closed loop that the 1, first connecting tube 7 of bottle, trap tube 3 and the second connecting tube 8 are connected into, so trapping
Pipe 3 can fully be enriched with volatile ingredient and semi-volatility component in tobacco juice, and be filled with activated carbon granule in trap tube 3
4,4 high adsorption capacity of activated carbon granule can substantially more adsorb the volatile ingredient and semi-volatility component in tobacco juice；By
This, a kind of analytical equipment for analyzing tobacco juice composition of the present invention can improve analysis efficiency.
The present invention a kind of analytical equipment for analyzing tobacco juice composition in air pump 2, sample bottle 1, the first connecting tube 7,
The closed loop gas flow loop that trap tube 3 and the second connecting tube 8 are connected into, is detachably connected with bottle cap, bottle on the bottleneck of sample bottle 1
The bottleneck in order to sealed sample bottle 1 is covered, the first connecting tube 7 and the second connecting tube 8 are inserted in sample bottle 1 from bottle cap, the first connection
Bottom of 7 to the second connecting tube 8 of pipe closer to sample bottle 1, is so more beneficial for purging the tobacco juice in sample bottle 1, in air pump 2
To in sample bottle 1 sample tobacco juice purging effect under, volatile ingredient and semi-volatility component in sample tobacco juice are evaporated into
In air-flow, the air-flow containing volatile ingredient and semi-volatility component is circulated between sample bottle 1 and trap tube 3, air-flow
In volatile ingredient and semi-volatility component be component to be detected, the activity in the adsorbed trap tube 3 of these components to be detected
On charcoal particle 4；Compare at present compared with frequently with open open gas flow loop pipe method of trapping, the gas flow tube method of trapping of closed loop has more
High cycles of concentration, higher adsorption efficiency, are particularly suited for the analysis of semi-volatile compounds.Secondly, compared to adopting capillary
Pipe adsorption column, SPE are first-class as enrichment tool, make in a kind of analytical equipment for analyzing tobacco juice composition of the present invention
Volatile ingredient and semi-volatility component are enriched with the trap tube 3 filled with activated carbon granule 4, are significantly increased
Adsorption capacity to all kinds of flavor components so that bioaccumulation efficiency is improved；Additionally, 4 adsorption capacity of activated carbon granule from filling is big,
The big sample of this kind of solvent of electronic cigarette liquid is particularly well-suited to, in order to reach preferable adsorption effect, is filled in trap tube 3
There is 60-80 mesh activated carbon granule 4, can fill 20-30mg (mg represents milligram) activated carbon granule 4 in the trap tube 3, one
As for, filling 25mg activated carbon granules 4.So, filled using a kind of analysis for analyzing tobacco juice composition of the present invention
Put and can be enriched with volatile ingredient and semi-volatility component in acquisition electronic cigarette liquid, and fully can extract in electronic cigarette liquid
Each middle volatile ingredient and semi-volatility component, sensitivity for analysis are high, and as a result accurately and reliably, one kind of the present invention is used for analyzing cigarette
The analytical equipment assembling of liquid composition is simple, with low cost.In a kind of device pair for tobacco juice constituent analysis using the present invention
When tobacco juice composition is analyzed, need to pull down sample bottle 1 to load sample tobacco juice in sample bottle 1, for the ease of removing or
The sample bottle 1 is installed, first connecting tube 7, the second connecting tube 8 are detachably connected on sample bottle 1；Complete to be enriched with
After operation, in addition it is also necessary to remove trap tube 3 to carry out wash-out operation, for the ease of removing or installing trap tube 3, the trapping
Pipe 3 is removably attachable between the second connecting tube 8 and the 3rd connecting tube 9.The air pump 2 is used for preparing air to produce gas
Stream, it is preferable that the air pump 2 is electronic diaphragm air pump 2.
The present invention also provides a kind of analysis method for analyzing tobacco juice composition, adopts the following technical scheme that, of the invention
A kind of analysis method for analyzing tobacco juice composition, using the sheet described in above-mentioned technical proposal or its arbitrary preferred technical scheme
A kind of analytical equipment for analyzing tobacco juice composition of invention carries out operation, comprises the steps：
1) sample：Take tobacco juice sample to be added in sample bottle 1, rotary sample bottle 1 makes tobacco juice uniformly divide in sample bottle 1
Cloth, uses bottle cap sealing bottleneck, is then inserted in sample bottle 1 first connecting tube 7 and the second connecting tube 8 from bottle cap；
2) purge：Open air pump 2 to purge the tobacco juice in sample bottle 1；
3) it is enriched with：The volatile ingredient in tobacco juice and semi-volatility component in sample bottle 1 is evaporated and passes through second
Connecting tube 8 is entered in trap tube 3, waving in the air-flow that the enrichment of activated carbon granule 4 in trap tube 3 is entered in trap tube 3
The property sent out composition and semi-volatility component；
4) elute：After the completion of enrichment, activated carbon trap tube 3 is removed, color will be eluted to by enriched composition using organic solvent
In spectrum bottle, eluent is obtained；
5) analyze：Eluent is carried out gaschromatographic mass spectrometric analysis, you can volatilization and half in Qualitative and quantitative analysis tobacco juice
Volatile ingredient.
Preferably, above-mentioned steps 1) in, taken tobacco juice be 1-2mL (mL represents milliliter).
It is further preferable that above-mentioned steps 1) in, taken tobacco juice be 2mL.
Preferably, above-mentioned steps 1) in, the volume of the sample bottle 1 is 30-50mL.
It is further preferable that preferably, above-mentioned steps 1) in, the volume of the sample bottle 1 is 40mL.
Preferably, above-mentioned steps 2) in, 2 gas outlet of air pump, 6 flow velocity be 500-800ml/min (1mL/min represent per point
The flow of clock is 1 milliliter).
It is further preferable that above-mentioned steps 2) in, 2 gas outlet of air pump, 6 flow velocity be 600ml/min.
Preferably, above-mentioned steps 3) in, enrichment time be 1-2 hours.
It is further preferable that above-mentioned steps 3) in, enrichment time be 2 hours.
Preferably, above-mentioned steps 4) in, the organic solvent is one or more in dichloromethane or alcohol solvent
Combination.
It is further preferable that above-mentioned steps 4) in, the organic solvent be dichloromethane.
Preferably, above-mentioned steps 4) in, 300-500 μ L (μ L represent microlitre).
It is further preferable that preferably, above-mentioned steps 4) in, 400 μ L.
Preferably, in above-mentioned steps are rapid 4), the washing steps of the organic solvent are 1～3 time.
It is further preferable that in above-mentioned steps are rapid 4), the washing steps of the organic solvent are 2 times.
Preferably, above-mentioned steps 5) in, when eluent is carried out gaschromatographic mass spectrometric analysis, GC conditions are：
Chromatographic column：DB-WAX capillary columns (60m × 0.25mm × 0.25 μm)；Injector temperature：250℃；Sample size：1μl；Carrier gas：
High-purity helium, carrier gas purity >=99.999%；Flow rate of carrier gas：1.5ml/min, constant current mode；Split ratio：Do not shunt；Intensification journey
Sequence：35 DEG C of holding 1min of initial temperature, rise to 230 DEG C with the speed of 5 DEG C/min, keep 15min.Mass Spectrometry Conditions are：Transmission line
Temperature：250℃；Ion source temperature：230℃；Level Four bar temperature：150℃；Solvent delay：9min；Ionization mode：EI sources；Ionization
Energy：70eV；Scan mode：Full scan (Scan).
With reference to embodiments a kind of analysis method for analyzing tobacco juice composition of the present invention is further illustrated.
Embodiment 1
Utilize the present invention's is a kind of for the analysis method of tobacco juice composition being analyzed to the volatility in certain brand A electronic cigarette liquid
Composition and semi-volatility component are enriched with and are analyzed, and step is as follows：
1) sample：Take certain brand A electronic cigarette liquid 2mL to be placed in 40mL sample bottles 1, rotary sample bottle 1 makes tobacco juice in sample
It is uniformly distributed in bottle 1, with bottle cap sealing sample bottle 1, the first connecting tube 7 and the second connecting tube 8 is inserted sample from bottle cap then
In bottle 1；
2) purge：Air is prepared using electronic diaphragm air pump 2, the air-flow velocity of 2 gas outlet 6 of air pump is 500mL/min, right
Electronic cigarette liquid in sample bottle 1 is purged；
3) it is enriched with：The volatile ingredient in tobacco juice and semi-volatility component in sample bottle 1 is evaporated and passes through second
Connecting tube 8 is entered in trap tube 3, the volatilization in trap tube 3 filled with activated carbon granule 4 to be enriched with the air of purging gained
Property composition and semi-volatility component, enrichment time 2 hours is filled with 25mg60-80 mesh activated carbon granule 4 in trap tube used 3；
4) elute：After the completion of enrichment, remove trap tube 3 and add 400 μ L dichloromethane to be eluted to gas-chromatography in two times
In bottle, that is, obtain the eluent of volatile ingredient and semi-volatility component containing electronic cigarette liquid；
5) analyze：For above-mentioned eluent, it is analyzed using Gas chromatographyMass spectrometry, with qualitative and quantitative
Volatilization and semi-volatility component in analysis tobacco juice, as a result as shown in table 1.
Above-mentioned steps 5) in, GC-MS testing conditions are：
GC conditions：Chromatographic column：DB-WAX capillary columns (60m × 0.25mm × 0.25 μm)；Injector temperature：
250℃；Sample size：1μl；Carrier gas：High-purity helium, carrier gas purity >=99.999%；Flow rate of carrier gas：1.5ml/min, constant current mould
Formula；Split ratio：Do not shunt；Heating schedule：35 DEG C of holding 1min of initial temperature, rise to 230 DEG C with the speed of 5 DEG C/min, keep
15min；
Mass Spectrometry Conditions：Transmission line temperature：250℃；Ion source temperature：230℃；Level Four bar temperature：150℃；Solvent delay：
9min；Ionization mode：EI sources；Ionizing energy：70eV；Scan mode：Full scan (Scan)；
Also, quantitative analysis is carried out to testing result using peak area normalization method, using spectrum data library searching to detection
As a result qualitative analysis carried out, the spectrum data storehouse is WILEY07 databases, composition basis for estimation selects matching degree>90.
After through gas chromatography combined with mass spectrometry technical Analysis, in electronic cigarette liquid, volatilization, semi-volatility component are as shown in table 1, this
A little is all the volatile ingredient and semi-volatility component that can be measured in electronic cigarette liquid, and comprehensively, each component sensitivity is high for extract component.
Table 1
Embodiment 2：
Utilize the present invention's is a kind of for the analysis method of tobacco juice composition being analyzed to the volatility in certain brand B electronic cigarette liquid
Composition and semi-volatility component are enriched with and are analyzed, and step is as follows：
1) sample：Certain brand B electronic cigarette is taken, after cigarette bullet is disassembled, wherein tobacco juice 2mL is taken out and is placed in 40mL sample bottles 1,
Rotary sample bottle 1 makes tobacco juice be uniformly distributed in sample bottle 1, uses bottle cap sealing bottleneck, then connects the first connecting tube 7 and second
Adapter 8 is inserted in sample bottle 1 from bottle cap；
2) purge：Air is prepared using electronic diaphragm air pump 2,2 gas outlet of air pump, 6 flow velocity is 600mL/min, to sample bottle
Electronic cigarette liquid in 1 is purged；
3) it is enriched with：The volatile ingredient in tobacco juice and semi-volatility component in sample bottle 1 is evaporated and passes through second
Connecting tube 8 is entered in trap tube 3, waving in the air-flow that the enrichment of activated carbon granule 4 in trap tube 3 is entered in trap tube 3
The property sent out composition and semi-volatility component；Enrichment time 2 hours, is filled with 25mg60-80 mesh activated carbon granules in the trap tube 3
4；
4) elute：After the completion of enrichment, remove trap tube 3 and add 400 μ L dichloromethane to be eluted to gas-chromatography in two times
In bottle, the eluent containing electronic cigarette liquid volatile ingredient and semi-volatility component is obtained final product；
5) analyze：For above-mentioned eluent, it is analyzed using Gas chromatographyMass spectrometry.
Above-mentioned steps 5) in, GC-MS testing conditions are：
GC conditions：Chromatographic column：DB-WAX capillary columns (60m × 0.25mm × 0.25 μm)；Injector temperature：
250℃；Sample size：1μl；Carrier gas：High-purity helium, carrier gas purity >=99.999%；Flow rate of carrier gas：1.5ml/min, constant current mould
Formula；Split ratio：Do not shunt；Heating schedule：35 DEG C of holding 1min of initial temperature, rise to 230 DEG C with the speed of 5 DEG C/min, keep
15min；
Mass Spectrometry Conditions：Transmission line temperature：250℃；Ion source temperature：230℃；Level Four bar temperature：150℃；Solvent delay：
9min；Ionization mode：EI sources；Ionizing energy：70eV；Scan mode：Full scan (Scan).
After through gas chromatography combined with mass spectrometry technical Analysis, in electronic cigarette liquid, volatilization, semi-volatility component are as shown in table 2, this
A little is all the volatile ingredient and semi-volatility component that can be measured in electronic cigarette liquid, and comprehensively, each component sensitivity is high for extract component.
Table 2
Embodiment 3：
Utilize the present invention's is a kind of for the analysis method of tobacco juice composition being analyzed to the volatility in certain brand C electronic cigarette liquid
Composition and semi-volatility component are enriched with and are analyzed, and step is as follows：
1) sample：Take certain brand C electronic cigarette liquid 2mL to be placed in 40mL sample bottles 1, rotary sample bottle 1 makes tobacco juice in sample
It is uniformly distributed in bottle 1, uses bottle cap sealing bottleneck, the first connecting tube 7 and the second connecting tube 8 are inserted into sample bottle from bottle cap then
In 1；
2) purge：Air is prepared using electronic diaphragm air pump 2,2 gas outlet of air pump, 6 flow velocity is 600mL/min, to sample bottle
Electronic cigarette liquid in 1 is purged；
3) it is enriched with：The volatile ingredient in tobacco juice and semi-volatility component in sample bottle 1 is evaporated and passes through second
Connecting tube 8 is entered in trap tube 3, volatile ingredient in activated carbon granule 4 in trap tube 3 enrichment purging gained air and
Semi-volatility component, enrichment time 2 hours are filled with 25mg60-80 mesh activated carbon granule 4 in the trap tube 3；
4) elute：After the completion of enrichment, remove trap tube 3 and add 400 μ L dichloromethane to be eluted to gas-chromatography in two times
In bottle, the eluent containing electronic cigarette liquid volatile ingredient and semi-volatility component is obtained final product；
5) analyze：For above-mentioned eluent, it is analyzed using Gas chromatographyMass spectrometry.
Above-mentioned steps 5) in, GC-MS testing conditions are：
GC conditions：Chromatographic column：DB-WAX capillary columns (60m × 0.25mm × 0.25 μm)；Injector temperature：
250℃；Sample size：1μl；Carrier gas：High-purity helium, carrier gas purity >=99.999%；Flow rate of carrier gas：1.5ml/min, constant current mould
Formula；Split ratio：Do not shunt；Heating schedule：35 DEG C of holding 1min of initial temperature, rise to 230 DEG C with the speed of 5 DEG C/min, keep
15min；
Mass Spectrometry Conditions：Transmission line temperature：250℃；Ion source temperature：230℃；Level Four bar temperature：150℃；Solvent delay：
9min；Ionization mode：EI sources；Ionizing energy：70eV；Scan mode：Full scan (Scan).
Analyze through GC-MS, volatile ingredient and semi-volatility component result such as Fig. 2 in electronic cigarette liquid
Shown, each composition is separated clearly, and chromatogram response is sensitive.
In sum, the present invention effectively overcomes various shortcoming of the prior art and has high industrial utilization.
The principle and its effect of above-described embodiment only illustrative present invention, of the invention not for limiting.Any ripe
The personage for knowing this technology all can carry out modifications and changes to above-described embodiment under the spirit and the scope without prejudice to the present invention.Cause
This, those of ordinary skill in the art is complete with institute under technological thought without departing from disclosed spirit such as
Into all equivalent modifications or change, should by the present invention claim be covered.
Claims (10)
1. a kind of analytical equipment for analyzing tobacco juice composition, including sample bottle (1), air pump (2) and trap tube (3), the gas
Pump (2) has air inlet (5) and gas outlet (6), it is characterized in that：
The first connecting tube (7), sample bottle (1) and trapping is connected between the gas outlet (6) of air pump (2) and sample bottle (1)
The second connecting tube (8) is connected between pipe (3), the 3rd is connected between trap tube (3) and the air inlet (5) of air pump (2) and is connected
Pipe (9), air pump (2), sample bottle (1), the first connecting tube (7), trap tube (3) and the second connecting tube (8) connect into closed loop
Gas flow loop；Activated carbon granule (4) is filled with trap tube (3).
2. the analytical equipment for analyzing tobacco juice composition according to claim 1, it is characterised in that：First connecting tube
(7), the second connecting tube (8) is detachably connected on sample bottle (1)；Trap tube (3) are removably attachable to the second company
Between adapter (8) and the 3rd connecting tube (9).
3. the analytical equipment for analyzing tobacco juice composition according to claim 1, it is characterised in that：Trap tube (3)
In be filled with 60-80 mesh activated carbon granules (4).
4. the analytical equipment for analyzing tobacco juice composition according to claim 2, it is characterised in that：Trap tube (3)
In be filled with 20-30mg activated carbon granules (4).
5. a kind of analysis method for analyzing tobacco juice composition, using described in claim 1 for analyze tobacco juice composition point
Analysis apparatus carry out operation, it is characterized in that, comprise the steps：
1) sample：Take tobacco juice sample to be added in sample bottle (1), rotary sample bottle (1) makes tobacco juice uniformly divide in sample bottle (1)
Cloth, uses bottle cap sealing bottleneck, is then inserted in sample bottle (1) the first connecting tube (7) and the second connecting tube (8) from bottle cap；
2) purge：Open air pump (2) to purge the tobacco juice in sample bottle (1)；
3) it is enriched with：The volatile ingredient in tobacco juice and semi-volatility component in sample bottle (1) is evaporated and passes through the second company
Adapter (8) is entered in trap tube (3), the gas that activated carbon granule (4) enrichment in trap tube (3) is entered in trap tube (3)
Volatile ingredient and semi-volatility component in stream；
4) elute：After the completion of enrichment, activated carbon trap tube (3) is removed, chromatogram will be eluted to by enriched composition using organic solvent
In bottle, eluent is obtained；
5) analyze：Eluent is carried out gaschromatographic mass spectrometric analysis, you can volatilization and half is volatilized in Qualitative and quantitative analysis tobacco juice
Property composition.
6. the analysis method for analyzing tobacco juice composition according to claim 5, it is characterised in that：Above-mentioned steps 1) in,
Taken tobacco juice is 1-2mL.
7. the analysis method for analyzing tobacco juice composition according to claim 5, it is characterised in that：Above-mentioned steps 2) in,
Air pump (2) gas outlet (6) flow velocity is 500-800ml/min.
8. the analysis method for analyzing tobacco juice composition according to claim 5, it is characterised in that：Above-mentioned steps 3) in,
Enrichment time is 1-2 hours.
9. the analysis method for analyzing tobacco juice composition according to claim 5, it is characterised in that：Above-mentioned steps 4) in,
The organic solvent is dichloromethane or alcohol solvent.
10. the analysis method for analyzing tobacco juice composition according to claim 5, it is characterised in that：Above-mentioned steps 4) in,
300-500μL.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611258695.9A CN106501438A (en) | 2016-12-30 | 2016-12-30 | For analyzing analytical equipment and the analysis method of tobacco juice composition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611258695.9A CN106501438A (en) | 2016-12-30 | 2016-12-30 | For analyzing analytical equipment and the analysis method of tobacco juice composition |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106501438A true CN106501438A (en) | 2017-03-15 |
Family
ID=58333419
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| CN201611258695.9A Pending CN106501438A (en) | 2016-12-30 | 2016-12-30 | For analyzing analytical equipment and the analysis method of tobacco juice composition |
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| CN108444778A (en) * | 2018-06-08 | 2018-08-24 | 云南中烟工业有限责任公司 | The capturing device of volatile ingredient in a kind of air |
| CN108593816A (en) * | 2018-04-28 | 2018-09-28 | 江苏中烟工业有限责任公司 | A kind of method and device improving volatile ingredient purging efficiency in tobacco |
| CN111411022A (en) * | 2020-03-30 | 2020-07-14 | 上海烟草集团有限责任公司 | Preparation method and device of volatile aroma components in natural product |
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| CN108593816B (en) * | 2018-04-28 | 2021-08-24 | 江苏中烟工业有限责任公司 | Method for improving purging efficiency of volatile components in tobacco |
| CN108444778A (en) * | 2018-06-08 | 2018-08-24 | 云南中烟工业有限责任公司 | The capturing device of volatile ingredient in a kind of air |
| CN111411022A (en) * | 2020-03-30 | 2020-07-14 | 上海烟草集团有限责任公司 | Preparation method and device of volatile aroma components in natural product |
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