CN105784862B - One grow tobacco it is middle volatilization and half volatile ingredient analysis method - Google Patents
One grow tobacco it is middle volatilization and half volatile ingredient analysis method Download PDFInfo
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Abstract
The present invention provide one grow tobacco volatilization and half volatile ingredient analysis method, include the following steps：Balance：Cigarette is removed into filter tip and cigarette paper obtains tobacco sample, sample is fitted into sample bottle and carries out heating balance, the temperature for heating balance is 30 ~ 80 DEG C, and the time for heating balance is 5 ~ 15 minutes；Heating：By sample bottle continuous heating, the temperature of continuous heating is 30 ~ 80 DEG C, and the tobacco sample in sample bottle is purged using air pump；Enrichment, take off and wash and analyze.The component that method enrichment in the present invention obtains is typical case's volatilization, half volatile substance generally contained in cigarette shreds, and each component relative amount is higher, and extraction Product characteristics are clear, and as a result accurately and reliably, the equipment involved by it also assembles simply, of low cost.
Description
Technical field
The present invention relates to chemical composition detection field in tobacco, specifically disclose one and grow tobacco middle volatilization and half volatile ingredient
Analysis method.
Background technology
In the prior art on there is many analysis test methods for tobacco leaf volatile ingredient, as domestic applications number are
The patent of invention of CN201310025742 discloses a kind of analysis method of junior tobacco leaf aroma volatile, Application No.
The patent of invention of CN201210487928 also discloses that the tobacco during beating and double roasting escapes thing analysis method and capturing device,
Domestic applications number are that the quality control that the patent of invention of CN201210431454 is disclosed during a kind of tobacco cutting is intended to diagnose
Analysis method and system.And the constituent analysis for manufactured tobacco finished product, that is, cigarette is actually rare.
Volatility, half volatile chemical composition are being the important factor in order of decision tobacco odor type and style in cigarette.
The solvent extraction method routinely used in the prior art is suitable for separating medium volatile and difficult volatile organises
Compound, the organic solvent amount that this method uses is big, and carrying out concentration after extraction again, time-consuming, and Impurities In Solvents interference is larger.
Simultaneous distillation-extraction extraction (SDE) has good repeated and higher extraction quantity, and easy to operate, qualitative
Quantitative effect is good, but since condition is violent, Maillard reaction and caramelization can be caused to aggravate, accessory substance is more, this
Analysis means add analysis difficulty.
There are flue gas in the flue gas analysis for tobacco smoke product in the prior art to be enriched with unstable not in time, enriching quantity
Low, semi-volatility component concentration effect is poor, and analysis is inaccurate and not comprehensive or introduces other accessory substances and causes analysis result
The defects of deviation.
The content of the invention
The defects of it is an object of the invention to overcome the prior art, there is provided one grow tobacco it is middle volatilization and half volatile ingredient point
Analysis method, the defects of to overcome analysis method in the prior art.
In order to realize object above and other purposes, the present invention including following technical scheme by realizing：
The present invention provide one grow tobacco volatilization and half volatile ingredient analysis method, include the following steps：
1) balance：Cigarette is removed into filter tip and cigarette paper obtains tobacco sample, sample is fitted into sample bottle and is heated
Balance, the temperature for heating balance is 30~80 DEG C, and the time for heating balance is 5~15 minutes；
2) heat：By sample bottle continuous heating, the temperature of continuous heating is 30~80 DEG C, and using air pump in sample bottle
Tobacco sample purged；
3) it is enriched with：Be enriched with purging gained air using open tubular capillary column, and the open tubular capillary column and sample bottle and
Air pump is connected as closed loop；
4) elute：After the completion of enrichment, open tubular capillary column is removed, gas phase will be eluted to by enriched composition using organic solvent
Eluent is obtained in chromatogram bottle；
5) analyze：Eluent is subjected to gas chromatography-mass spectrometry analysis, you can volatilization in Qualitative and quantitative analysis tobacco and
Half volatile ingredient.
Preferably, the temperature of the heating balance in step 1) is 30~45 DEG C.
Preferably, the time of the heating balance in step 1) is 15min.
Preferably, in step 2), purge time is 1~5h.
It is highly preferred that in step 2), purge time 1.5h.
Preferably, in step 3), the internal diameter of the open tubular capillary column is 0.53mm, and length 2m, thickness is 1 μm.
Preferably, in step 3), the air pump exit velocity is 500~1000ml/min.
It is highly preferred that in step 3), the air pump exit velocity is 500~800ml/min.
It is highly preferred that in step 3), the air pump exit velocity is 800ml/min.
Preferably, one or more of combinations of the organic solvent in dichloromethane, ethanol or ether in step 4).
It is highly preferred that organic solvent is dichloromethane in step 4).
Preferably, in step 4), the usage amount of organic solvent is 0.5~2ml.
Preferably, in step 4), the usage amount of organic solvent is 1ml.
Preferably, in step 4), the washing steps of the organic solvent are 1~3 time.
Preferably, in step 4), the washing steps of the organic solvent are 3 times.
Preferably, in step 5), gas-chromatography uses DB-WAX capillary columns, and injector temperature is 240~260 DEG C, into
Sample amount is 1~5 μ l；Carrier gas uses high-purity helium, and flow rate of carrier gas is 1~5ml/min.
It is highly preferred that in step 5), gas-chromatography uses DB-WAX capillary columns, and injector temperature is 250 DEG C, sample size
For 3 μ l；Carrier gas uses high-purity helium, flow rate of carrier gas 2ml/min.Carrier gas uses high-purity helium, helium purity in gas-chromatography
>=99.999%.
Preferably, in step 5), initial temperature for 30~40 DEG C and is kept for 2~5 minutes in gas-chromatography heating schedule, is risen
Warm speed is 2~5 DEG C/min, is warming up to 220~240 DEG C and is kept for 10~20 minutes.
Preferably, in step 5), Mass Spectrometry Conditions are：Transmission line temperature is 230~250 DEG C, ion source temperature for 220~
240 DEG C, level Four bar temperature is 140~160 DEG C.
Preferably, Mass Spectrometry Conditions are：Transmission line temperature：240℃；Ion source temperature：230℃；Level Four bar temperature：150℃；
Solvent delay：11min；Ionization mode：EI sources；Ionizing energy：70eV；Scan mode：Full scan and Salbutamol Selected Ion Monitoring.
The one of the present invention grows tobacco volatilization, the enrichment of half volatile ingredient and washing device and analysis method, by using closing
Volatilization, half volatile ingredient in loop back path gas enrichment cigarette shreds, in closed loop system, the gas of certain volume passes through gas
Pump and pipe-line system circulate between sample bottle, enrichment pipe, and volatility component to be measured continuously extracts absorption by air-flow and exists in sample
In open tubular capillary column.Therefore, first, compared at present compared with frequently with open open pipe trap system, closed loop formula open pipe
Method of trapping has cycles of concentration, the stronger adsorption efficiency of higher, particularly suitable for the analysis of semi-volatile compounds.Secondly, originally
It is used for enrichment volatilization, semi-volatility component using longer open tubular capillary column (length is up to tens of rice) in invention, compared to
The adsorption tube of other short sizes, longer enriching column can effectively realize classification absorption, substantially reduce by adsorption component in richness
Penetrance in collector.Furthermore using the open tubular capillary column that thickness of liquid film is higher in the present invention, relatively thin compared to liquid film opens
Pipe capillary, thicker liquid film can be improved effectively by the enriching quantity of adsorption component so that bioaccumulation efficiency improves.In the present invention
The component that obtains of method enrichment be typical case's volatilization, half volatile substance generally contained in cigarette shreds, and each component is opposite
Content is higher, and extraction Product characteristics are clear, and as a result accurately and reliably, the equipment involved by it also assembles simply, of low cost.
Tobacco volatilization and the enrichment of half volatile ingredient and washing device and analysis method disclosed in the present invention overcome existing
There are many disadvantages in technology and creative.
Brief description of the drawings
Fig. 1 is the schematic diagram of CLSA enriching apparatus figures；
Fig. 2 is the washing device schematic diagram of tobacco volatilization and half volatile ingredient.
Fig. 3 is that method carries out analysis acquisition result using Gas chromatographyMass spectrometry in embodiment 1.
Wherein, the reference numeral in Fig. 1~3 is as follows：
1 is switch capillary column；
2 be air pump；
21 be the first air inlet；
22 be the first gas outlet；
3 be temperature controlled water bath heating kettle；
4 be sample bottle；
41 be the second air inlet；
42 be the second gas outlet；
5 be air inlet pipe；
6 be air outlet pipe.
Embodiment
With reference to embodiment, the present invention is further explained.It is to be understood that embodiment is merely to illustrate the present invention, and it is unrestricted
The scope of the present invention.
Embodiment 1
Volatilization, half volatile ingredient in cigarette shreds are enriched with and are analyzed using following preparation method, step is as follows：
1) after cigarette being removed filter tip and cigarette paper, obtain tobacco sample, weigh 4.5g tobacco sample load band sealing every
In the head space glass sample bottle of pad, sample bottle is put into temperature controlled water bath heating kettle and carries out at 45 DEG C heating balance 15 minutes；
2) after balancing, sample bottle is continued through into temperature controlled water bath heating kettle and is heated, heating-up temperature is 50 DEG C, and is made
Prepare air with electronic diaphragm air pump, electronic diaphragm air pump exit velocity is 800ml/min, to the tobacco sample in sample bottle into
When row purging 1.5 is small；
3) it is using open tubular capillary column enrichment purging gained air, the parameter of the open tubular capillary column：Internal diameter：
0.53mm；Length：2m；Thickness：1μm；
4) after the completion of being enriched with, remove open tubular capillary column and be eluted to gas-chromatography bottle 3 times using 1ml dichloromethane point
In, up to tobacco volatilization, half volatile ingredient.
5) dichloromethane solution obtained for above-mentioned enrichment, is analyzed using Gas chromatographyMass spectrometry, knot
Fruit is such as
Shown in Fig. 3.
Wherein, gas chromatography-mass spectrometry (GC-MS) testing conditions are：
GC conditions are：Chromatographic column：DB-WAX capillary columns (60m × 0.25mm, 0.25 μm)；Injector temperature：
250℃；Sample size：3μl；Carrier gas：High-purity helium, carrier gas purity >=99.999%；Flow rate of carrier gas：2ml/min, constant current mode；
Split ratio：Do not shunt；Heating schedule：40 DEG C of holding 2min of initial temperature, rise to 230 DEG C with the speed of 4 DEG C/min, keep
15min。
Mass Spectrometry Conditions are：Transmission line temperature：240℃；Ion source temperature：230℃；Level Four bar temperature：150℃；Solvent prolongs
Late：11min；Ionization mode：EI sources；Ionizing energy：70eV；Scan mode：Full scan (Scan) and Salbutamol Selected Ion Monitoring
(SIM)。
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 is carried out, the spectrum data storehouse is WILEY07 databases, and component basis for estimation selects matching degree >=90.
After Gas chromatographyMass spectrometry is analyzed, tobacco volatilization, half volatile ingredient are as shown in table 1, these components are all
Be tobacco and typical case's volatilization that tobacco product contains, half volatile ingredient, the component of extraction comprehensively, typical case, each component relative amount
Higher, extraction Product characteristics are clear.
Table 1
As shown in Figure 1, in CLSA enriching apparatus in the method for the present invention, for volatilizing and half enrichment for volatilizing tobacco component
Device mainly includes open tubular capillary column 1, air pump 2, temperature controlled water bath heating kettle 3, sample bottle 4, air inlet pipe 5 and air outlet pipe 6.Its
In, the sample bottle 4 heats in the temperature controlled water bath heating kettle 3.The air pump 2 goes out equipped with the first air inlet 21 and first
Gas port 22.The sample bottle 4 is equipped with the second air inlet 41 and the second gas outlet 42.Described 5 one end of air inlet pipe and the first outlet
Mouth 22 connects, and the other end is connected with the second air inlet.The intermediate connection of the air outlet pipe 6 has the open tubular capillary column 1, and institute
State one end of air outlet pipe 6 to be connected with the first air inlet 21 of the air pump 2, the other end of the air outlet pipe 6 and the sample bottle 4
The second gas outlet 42 connect.
It is in sample box trap by the gas stripping gas of certain volume by pump and pipe-line system that formulation CLSA is blown in closed cycle
Between circulate, in sample volatility component to be measured by air-flow continuously extract absorption on trap, there is cycles of concentration higher, can
The characteristics of compound range is wide is surveyed, the higher volatile organic matter of boiling point can be analyzed.A kind of works of the CLSA as Dynamic headspace
Skill means, can be enriched with volatilization, half volatile chemical composition, easy to operate, reproducible, and are used directly for sense organ and comment
Valency.
Embodiment 2
Volatilization, half volatile ingredient in cigarette shreds are enriched with and are analyzed using following preparation method, step is as follows：
1) after cigarette being removed filter tip and cigarette paper, obtain tobacco sample, weigh 4.5g tobacco sample load band sealing every
In the head space glass sample bottle of pad, sample bottle is put into temperature controlled water bath heating kettle and carries out at 30 DEG C heating balance 15 minutes；
2) after balancing, sample bottle is continued through into temperature controlled water bath heating kettle and is heated, heating-up temperature is 80 DEG C, and is used
Electronic diaphragm air pump prepares air, and electronic diaphragm air pump exit velocity is 500ml/min, and the tobacco sample in sample bottle is carried out
Purge 1 it is small when；
3) it is using open tubular capillary column enrichment purging gained air, the parameter of the open tubular capillary column：Internal diameter：
0.53mm；Length：2m；Thickness：1μm；
4) after the completion of being enriched with, remove open tubular capillary column and be eluted to gas-chromatography bottle 3 times using 1ml dichloromethane point
In, up to tobacco volatilization, half volatile ingredient.
5) dichloromethane solution obtained for above-mentioned enrichment, is analyzed using Gas chromatographyMass spectrometry, its
In, gas chromatography-mass spectrometry (GC-MS) testing conditions are：
GC conditions are：Chromatographic column：DB-WAX capillary columns (60m × 0.25mm, 0.25 μm)；Injector temperature：
240℃；Sample size：1μl；Carrier gas：High-purity helium, carrier gas purity >=99.999%；Flow rate of carrier gas：5ml/min, constant current mode；
Split ratio：Do not shunt；Heating schedule：30 DEG C of holding 2min of initial temperature, rise to 240 DEG C with the speed of 5 DEG C/min, keep
10min。
Mass Spectrometry Conditions are：Transmission line temperature：230℃；Ion source temperature：240℃；Level Four bar temperature：160℃；Solvent prolongs
Late：12min；Ionization mode：EI sources；Ionizing energy：70eV；Scan mode：Full scan and Salbutamol Selected Ion Monitoring.
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 is carried out, the spectrum data storehouse is WILEY07 databases, and component basis for estimation selects matching degree >=90.
Embodiment 3
Volatilization, half volatile ingredient in cigarette shreds are enriched with and are analyzed using following preparation method, step is as follows：
1) after cigarette being removed filter tip and cigarette paper, obtain tobacco sample, weigh 4.5g tobacco sample load band sealing every
In the head space glass sample bottle of pad, sample bottle is put into temperature controlled water bath heating kettle and carries out at 80 DEG C heating balance 5 minutes；
2) after balancing, sample bottle is continued through into temperature controlled water bath heating kettle and is heated, heating-up temperature is 40 DEG C, and is used
Electronic diaphragm air pump prepares air, and electronic diaphragm air pump exit velocity is 500ml/min, and the tobacco sample in sample bottle is carried out
Purge 5 it is small when；
3) it is using open tubular capillary column enrichment purging gained air, the parameter of the open tubular capillary column：Internal diameter：
0.53mm；Length：2m；Thickness：1μm；
4) after the completion of being enriched with, remove open tubular capillary column and be eluted to gas-chromatography bottle 1 time using 1ml dichloromethane point
In, up to tobacco volatilization, half volatile ingredient.
5) dichloromethane solution obtained for above-mentioned enrichment, is analyzed using Gas chromatographyMass spectrometry, knot
Fruit is as shown in Figure 3.
Wherein, gas chromatography-mass spectrometry (GC-MS) testing conditions are：
GC conditions are：Chromatographic column：DB-WAX capillary columns (60m × 0.25mm, 0.25 μm)；Injector temperature：
260℃；Sample size：5μl；Carrier gas：High-purity helium, carrier gas purity >=99.999%；Flow rate of carrier gas：5ml/min, constant current mode；
Split ratio：Do not shunt；Heating schedule：50 DEG C of holding 5min of initial temperature, rise to 240 DEG C with the speed of 2 DEG C/min, keep
20min。
Mass Spectrometry Conditions are：Transmission line temperature：250℃；Ion source temperature：220℃；Level Four bar temperature：140℃；Solvent prolongs
Late：10min；Ionization mode：EI sources；Ionizing energy：70eV；Scan mode：Full scan (Scan) and Salbutamol Selected Ion Monitoring
(SIM)。
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 is carried out, the spectrum data storehouse is WILEY07 databases, and component basis for estimation selects matching degree >=90.
The above, be only presently preferred embodiments of the present invention, not to the present invention in any form with substantial limitation,
It should be pointed out that for those skilled in the art, on the premise of the method for the present invention is not departed from, can also make
Some improvement and supplement, these are improved and supplement also should be regarded as protection scope of the present invention.All those skilled in the art,
Without departing from the spirit and scope of the present invention, when made using disclosed above technology contents it is a little more
Dynamic, modification and the equivalent variations developed, are the equivalent embodiment of the present invention；Meanwhile all substantial technologicals pair according to the present invention
The variation, modification and evolution for any equivalent variations that above-described embodiment is made, still fall within the scope of technical scheme
It is interior.
Claims (8)
1. one grow tobacco volatilization and half volatile ingredient analysis method, include the following steps：
1) balance：Cigarette is removed into filter tip and cigarette paper obtains tobacco sample, sample is fitted into sample bottle and carries out heating balance,
The temperature of heating balance is 30~80 DEG C, and the time for heating balance is 5~15 minutes；
2) heat：By sample bottle continuous heating, the temperature of continuous heating is 30~80 DEG C, and using air pump to the cigarette in sample bottle
Silk sample is purged；
3) it is enriched with：Purging gained air, and the open tubular capillary column and sample bottle and air pump are enriched with using open tubular capillary column
It is connected as closed loop；The internal diameter of the open tubular capillary column is 0.53mm, and length 2m, thickness is 1 μm；The air pump outlet
Flow velocity is 500~1000ml/min；
4) elute：After the completion of enrichment, open tubular capillary column is removed, gas-chromatography will be eluted to by enriched composition using organic solvent
Eluent is obtained in bottle；
5) analyze：Eluent is subjected to gas chromatography-mass spectrometry analysis, you can volatilization in Qualitative and quantitative analysis tobacco and partly wave
Send out component.
2. method as claimed in claim 1, it is characterised in that：In step 2), purge time is 1~5h.
3. method as claimed in claim 1, it is characterised in that：Organic solvent is selected from dichloromethane, ethanol or ether in step 4)
In one or more of combinations.
4. method as claimed in claim 1, it is characterised in that：In step 4), the usage amount of organic solvent is 0.5~2ml.
5. method as claimed in claim 1, it is characterised in that：In step 4), the washing steps of the organic solvent are 1~3 time.
6. method as claimed in claim 1, it is characterised in that：In step 5), gas-chromatography uses DB-WAX capillary columns, sample introduction
Mouth temperature is 240~260 DEG C, and sample size is 1~5 μ l；Carrier gas uses high-purity helium, and flow rate of carrier gas is 1~5ml/min；.
7. method as claimed in claim 1, it is characterised in that：In step 5), initial temperature is 30 in gas-chromatography heating schedule
~50 DEG C and keep 2~5 minutes, programming rate be 2~5 DEG C/min, be warming up to 220~240 DEG C and holding 10~20 minutes.
8. method as claimed in claim 1, it is characterised in that：In step 5), Mass Spectrometry Conditions are：Transmission line temperature is 230~250
DEG C, ion source temperature is 220~240 DEG C, and level Four bar temperature is 140~160 DEG C.
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| CN106501438A (en) * | 2016-12-30 | 2017-03-15 | 上海烟草集团有限责任公司 | For analyzing analytical equipment and the analysis method of tobacco juice composition |
| CN107328873A (en) * | 2017-06-22 | 2017-11-07 | 河北中烟工业有限责任公司 | A kind of tobacco of dynamic pin trapping gas chromatography combined with mass spectrometry causes fragrant analysis of components method |
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| CN109781908B (en) * | 2019-03-19 | 2022-02-01 | 上海烟草集团有限责任公司 | Method for analyzing odor substances in tobacco material |
| CN110554130A (en) * | 2019-09-20 | 2019-12-10 | 云南中烟工业有限责任公司 | Material management and control list construction method based on LSE-GC-MS/MS detection result |
| 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 |
| CN112782324B (en) * | 2021-03-02 | 2023-08-22 | 云南中烟工业有限责任公司 | Volatile organic compound acquisition device and application method thereof |
| CN115326991B (en) * | 2022-09-02 | 2024-07-02 | 上海烟草集团有限责任公司 | Method for analyzing open-pack smell of cigarettes |
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