CN109632998A - A kind of method of on-line analysis cigarette volatile component in quick-fried bead core material - Google Patents
A kind of method of on-line analysis cigarette volatile component in quick-fried bead core material Download PDFInfo
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- CN109632998A CN109632998A CN201811572401.9A CN201811572401A CN109632998A CN 109632998 A CN109632998 A CN 109632998A CN 201811572401 A CN201811572401 A CN 201811572401A CN 109632998 A CN109632998 A CN 109632998A
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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
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/12—Preparation by evaporation
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/12—Preparation by evaporation
- G01N2030/121—Preparation by evaporation cooling; cold traps
Abstract
The invention discloses a kind of on-line analysis cigarette methods of volatile component in quick-fried bead core material.Method includes the following steps: quick-fried pearl is placed in the syringe of disposable syringe, using isolating core material after the quick-fried pearl of syringe push rod attrition crushing；A small amount of core material is drawn with micro syringe to be injected into purging bottle, is passed through inert gas in 30~60 DEG C of progress dynamic purgings, and trapped using cold hydrazine trapping system, and heating cold hydrazine parsing volatile component enters gas chromatograph-mass spectrometer (GC-MS) and is measured.The cold hydrazine capture method that the present invention is established for cigarette with volatile component in quick-fried bead core material has the advantages that discriminate against without cold and hot point, no cross contamination, no sample, not only overcomes the shortcomings that there are selective absorptions in adsorption trap trapping technique；And trapping analysis is carried out by the way of online, loss of volatile component during purging and trapping can be utmostly reduced, to improve the accuracy of analysis data, sensitivity of analytical method is high, reproducible.
Description
Technical field
The invention belongs to tobacco product physico-chemical examination technique field, more particularly, to a kind of on-line analysis cigarette with quick-fried pearl
The method of volatile component in core material.
Background technique
Quick-fried pearl is a kind of capsule with semi-permeable membrane or sealing for being wrapped in liquid flavor component, including wall material and core material.
Quick-fried pearl cigarette refers to and is implanted into cigarette in cigarette filter with quick-fried pearl by filter stick seed pearl technology that when use pinches brokenly quick-fried pearl, built-in liquid
State flavors and fragrances core material flow to filter stick fiber, to reach cigarette flavouring, adjust the functions such as flavor.Therefore, by cigarette filter
It is middle to add quick-fried pearl to realize that perfuming cigarette is the popular solution route of a comparison.But the side of analysis and detection to filter tip flavoring
Method is all that flue gas trapping analysis is carried out using smoking machine, but up to more than 3000 kinds of chemical substance contained in pipe tobacco, Er Qieyan
Silk specific gravity shared in entire cigarette is very big, and quick-fried pearl only accounts for seldom specific gravity in filter tip, therefore if by pipe tobacco and quick-fried pearl one
Heating evaporation is played, complicated smoke components certainly will make a big impact to the analysis of quick-fried pearl in pipe tobacco.Further, in pipe tobacco
Complicated smoke components very likely mixed with quick-fried pearl, cause when being analyzed using chromatography, chromatographic peak large area be overlapped, nothing
Method tells the fragrance component in quick-fried pearl, this causes very big puzzlement to subsequent chromatography.Therefore, how really and accurately to filter
Perfuming component in the quick-fried pearl of mouth, which is accurately analyzed and detected, becomes the extremely important problem in Tobacco Analysis field.
Analysis of volatile components technology mainly includes direct injected-gas chromatography/mass spectrometry method (DI-GC-MS), static state
HS GC/Mass Spectrometry (HS-GC-MS), purge and trap-gas chromatography/mass spectrometry method (PT-GC-MS) are consolidated
Phase extraction-gas chromatography/mass spectrometry method (HS-SPME-GC-MS), direct injected-gas-chromatography high-resolution flight time matter
Spectrometry (DI-GC-TOF/MS), head space-comprehensive two dimensional gas chromatography/Mass Spectrometry (HS-GC × GC-MS) etc..Quick-fried bead core material
It include mainly solvent and flavor component, solvent is mainly medium chain triglycerides (MCT).It is analyzed to core material volatile component
When, due to the ratio of flavor component and MCT great disparity, according to direct injection analysis, the response of volatile component is greatly done
It disturbs and qualitative, quantitative difficulty is caused to increase, while residual of the MCT in injection port and chromatographic column is more serious, influences GC-MS's
The service life of stability and chromatographic column；HS-GC-MS method, which has, does not use organic solvent, easy to operate, quick, by-product
The advantages that less and can realizing on-line operation, but Static Headspace, without enrichment, sensitivity is relatively low, to low level of voltile
There are certain difficulty when constituent analysis；SPME-GC-MS method is carrying out GC-MS analysis after need to extracting manually, and difference extraction is fine
Tieing up effect of extracting of the head fiber type to volatile component, there is some difference, while testing under the cryogenic conditions lower than 60 DEG C
Repeatability needs to be further increased and improve；PT-GC-MS is excellent with easy to operate, high sensitivity and without using organic solvent etc.
Point, but purge the filler in adsorbing and trapping hydrazine and there is absorption discrimination to volatile component；CN107764917A combination GC-TOF/MS
Qualitative and quantitative analysis is carried out using the method for direct injected to volatile component crucial in the quick-fried pearl of cigarette with GC-MS/MS, due to perfume (or spice)
Taste ingredient differs greatly with the solvent in quick-fried bead core material, and the response of volatile component is greatly interfered and causes qualitative, quantitative difficult
Degree increases, while residual of the solvent in injection port and chromatographic column is more serious, influences the stability of GC-MS and making for chromatographic column
Use the service life.
CN107703246A discloses a kind of electronics tobacco tar analysis of components side of dynamic needle trapping gas chromatography combined with mass spectrometry
Method, dynamic trap needle in be filled with adsorbent, at 50 DEG C heat 30min after, will dynamic trapping needle be inserted into GC-MS injection port into
Row desorption, passes through GC-MS qualitative analysis after desorption.CN107328873A discloses a kind of dynamic needle trapping gas chromatography-mass spectrum
Tobacco causes fragrant analysis of components method, and dynamic, which traps, is filled with adsorbent in needle, will dynamic after heating 30min at 90 DEG C
Trapping needle insertion GC-MS injection port is desorbed, and after desorbing 5min, passes through GC-MS qualitative analysis.This adsorption trap trapping technique
There may be selective absorption, in addition adsorbent material can remain some impurity after being used for multiple times, even across repeatedly old
Change is also difficult to clean out, and pollutes to analysis；And above-mentioned two patent document is waved using offline mode
The trapping of hair property ingredient traps after the completion hand sampling again, and this mode increases personnel and operates existing error, while also increasing
Sample composition has been added to there is the risk of loss.
Therefore, currently there is an urgent need to volatilization of the cigarette in quick-fried bead core material is sufficiently obtained using more efficiently capture method
Property ingredient, and prevent loss of volatile component during purging and trapping simultaneously, in conjunction with accurately and effectively detection method,
To improve its detection sensitivity.
Summary of the invention
The technical problem to be solved by the present invention is in view of the deficiencies of the prior art, provide a kind of on-line analysis cigarette quick-fried bead core
The method of volatile component in material.The present invention realize dynamic purging with cold hydrazine trapping and gas chromatography-mass spectrography analysis
Line connection, can utmostly reduce loss of volatile component during purging and trapping, to improve the accuracy of analysis；Its
Sensitivity of analytical method is high, reproducible.
Above-mentioned purpose of the present invention is achieved through the following technical solutions:
A kind of method of on-line analysis cigarette volatile component in quick-fried bead core material, comprising the following steps:
S1. quick-fried pearl is placed in the syringe of disposable syringe, using isolating core after the quick-fried pearl of syringe push rod attrition crushing
Material；
S2. a small amount of core material is drawn with micro syringe to be injected into purging bottle, be passed through inert gas and carry out in 30~60 DEG C
Dynamic purges, and is trapped using cold hydrazine trapping system, and heating cold hydrazine parsing volatile component enters gas chromatography-mass spectrometry
It is measured with instrument；Wherein, the cold hydrazine trapping system are as follows: loaded in deactivation stainless steel tube middle position and be compacted 1~3mg glass
Glass cotton, the size of stainless steel tube are 100~120mm of length, 2~4mm of internal diameter.
The cold hydrazine capture method that the present invention is established for cigarette with volatile component in quick-fried bead core material has without cold and hot point, nothing
The advantages of cross contamination, no sample are discriminated against not only overcomes there are selective absorption in adsorption trap trapping technique, and adsorbent material passes through
It crosses after being used for multiple times, some impurity can be remained, be also difficult to clean out even across multiple aging, lacked to what analysis polluted
Point；And the present invention carries out trapping analysis (i.e. integrated mode) by the way of online, and this mode can utmostly subtract
Few loss of volatile component during purging and trapping, to improve the accuracy of analysis data.
Further, it in preferred embodiments of the present invention, is loaded in deactivation stainless steel tube middle position and is compacted 2mg glass
Glass cotton, the size of stainless steel tube are length 110mm, internal diameter 3mm.
Further, in preferred embodiments of the present invention, the working method of the cold hydrazine trapping system are as follows: cold hydrazine trapping
When system is in cold hydrazine trapping state, inert gas purge volatile component passes through low temperature glass from the arrival end of deactivation stainless steel tube
It traps at glass cotton, then is emptied from outlet end；Cold hydrazine trapping system be in heating parsing when, another way inert gas from deactivation not
The outlet end of rust steel pipe is by parsing at heating mineral wool, then gas chromatograph-mass spectrometer (GC-MS) is flowed into from arrival end.
In preferred embodiments of the present invention, the temperature that the inert gas carries out dynamic purging can be 30 DEG C, 35 DEG C, 40
DEG C, 45 DEG C, 50 DEG C, 55 DEG C or 60 DEG C.
Further, in preferred embodiments of the present invention, the temperature that the inert gas carries out dynamic purging is 60
℃。
Further, in preferred embodiments of the present invention, the inert gas carry out the time of dynamic purging be 10~
60min.Such as the time of the inert gas progress dynamic purging can be 20min, 30min, 40min, 50min or 60min.
Further, in preferred embodiments of the present invention, the time that the inert gas carries out dynamic purging is
50min。
Further, in preferred embodiments of the present invention, the inert gas carry out the flow velocity of dynamic purging be 60~
80mL/min.It is too low to purge flow velocity, purge time extends, and detection efficiency is decreased obviously；It is excessively high to purge flow velocity, then instrument system
Airtightness is unable to get guarantee.
Further, in preferred embodiments of the present invention, the flow velocity that the inert gas carries out dynamic purging is
70mL/min。
Further, in preferred embodiments of the present invention, the purging bottle is that Dynamic headspace purges vial.
Further, in preferred embodiments of the present invention, the inert gas is helium.
Further, in preferred embodiments of the present invention, the trapping operating temperature of the cold hydrazine trapping system is -60 DEG C
(liquid nitrogen refrigerating).
Further, in preferred embodiments of the present invention, the condition of the cold hydrazine heating parsing are as follows: by initial temperature-
60 DEG C are heated to 280 DEG C in 5min.
Further, in preferred embodiments of the present invention, the line temperature for connecting each instrument and equipment is 240~260 DEG C.
Further, in preferred embodiments of the present invention, the line temperature for connecting each instrument and equipment is 250 DEG C.
Further, in preferred embodiments of the present invention, the condition of gas chromatograph-mass spectrometer (GC-MS) includes:
Chromatographic column: the DB-5MS elastic capillary-column of 30m (length) × 0.25mm (internal diameter) × 0.25 μm (film thickness)；
Stationary phase: (5%- phenyl)-methyl polysiloxane；
Temperature program: 40 DEG C of initial temperature, 3min is kept, with the rate of 10 DEG C/min to 240 DEG C, then with 20 DEG C/min's
Rate keeps 20~30min to 280 DEG C；
Injector temperature: 280 DEG C；
Input mode: split sampling, split ratio 10:1~100:1；
Sample volume: inert gas directly purges sample introduction through cold hydrazine system；
Transmission line temperature: 280 DEG C；
Ion source temperature: 230 DEG C；
Level four bars temperature: 150 DEG C；
Ionization mode: electron bombardment ionization source；
Ionizing energy: 70eV；
Mass number range: 35~550amu；
Mensuration mode: full scan；
Solvent delay: do not postpone.
For different quick-fried pearl samples, the present invention can select the micro syringe using different size according to actual needs
Draw the quick-fried bead core material sample of different volumes.
In preferred embodiments of the present invention, qualitative method are as follows: by gained full scan chromatographic peak with NIST library searching into
Row qualitative analysis.
It is quantitative using areas of peak normalization method in preferred embodiments of the present invention, specifically: RTE integral way is used,
Peak area normalization percentage composition is calculated by formula (2):
In formula:
Xi--- the peak area of certain volatile component normalizes percentage composition (%)；
Mi--- the peak area of certain volatile component；
ΣMi--- volatile component total mark area.
Compared with prior art, the invention has the following advantages:
The cold hydrazine capture method that the present invention is established for cigarette with volatile component in quick-fried bead core material has without cold and hot point, nothing
The advantages of cross contamination, no sample are discriminated against not only overcomes there are selective absorption in adsorption trap trapping technique, and adsorbent material passes through
It crosses after being used for multiple times, some impurity can be remained, be also difficult to clean out even across multiple aging, lacked to what analysis polluted
Point；And the present invention carries out trapping analysis (i.e. integrated mode) by the way of online, can utmostly reduce volatility
Loss of ingredient during purging and trapping, to improve the accuracy of analysis data.The present invention realizes dynamic purging and cold hydrazine
The on-line joining process of trapping and gas chromatography-mass spectrography analysis, can utmostly reduce volatile component and purge and trapping
Loss in journey, to improve the accuracy of analysis；Its sensitivity of analytical method is high, reproducible.
Detailed description of the invention
Fig. 1 is the analytical procedure figure of quick-fried bead core material volatile component.
Fig. 2 is that Dynamic headspace purges vial master drawing.
Fig. 3 is quick-fried pearl sample A core material volatile component GC-MS spectrogram.
Fig. 4 is quick-fried pearl sample B core material volatile component GC-MS spectrogram.
Fig. 5 is quick-fried pearl sample C core material volatile component GC-MS spectrogram.
Specific embodiment
Following embodiment is the preferable embodiment of the present invention, but is not done to protection scope of the present invention any type of
It limits.The present invention mainly illustrates the cigarette analysis application thought of volatile component in quick-fried bead core material, simple in embodiment
The replacement of parameter cannot repeat in embodiment one by one, but be not intended to limit the present invention, other any without departing from the present invention
Spiritual essence and principle under made changes, modifications, substitutions, combinations, simplifications, equivalent substitute mode should be considered as, all answered
Comprising within the scope of the present invention.
Unless otherwise stated, agents useful for same of the present invention is that analysis is pure.
Following embodiment material therefor and reagent are as follows:
Cigarette quick-fried pearl sample A, B, C；
Helium: purity 99.999%；
Ethyl alcohol: chromatographically pure；
Ultrapure water: resistivity reaches 18M Ω cm.
Following embodiment instrument equipment:
Gas chromatograph-mass spectrometer (GC-MS)；
Vortex mixer: digital display multitube；
Cyclotron oscillation device；
Ultrasonic extraction instrument；
Electronic balance；
Bottleneck dispenser；
Syringe injector: 5mL.
The analysis of 1 cigarette of embodiment volatile component in quick-fried pearl sample A core material
1 sample pre-treatments
Cigarette is placed in 5mL syringe with quick-fried pearl sample A more, using core material after the quick-fried pearl of syringe push rod attrition crushing from syringe needle
Place flows into 2mL chromatogram bottle.
2 dynamics purge
5 μ L core materials are drawn with 10 μ L micro syringes to be injected into purging bottle (see Fig. 2), are passed through inert gas helium progress
Dynamic purges, and purging flow velocity is 70mL/min, and purging temperature is 60 DEG C, purge time 50min.
The trapping of 3 cold hydrazines
- 60 DEG C of cold hydrazines of purge gas process are trapped, and cold hydrazine trapping system is to fill in deactivation stainless steel tube middle position
2mg mineral wool is filled out and is compacted, the size of stainless steel tube is length 110mm, internal diameter 3mm.After the completion of trapping, cold hydrazine system is carried out
Heating parsing, heat temperature raising program are as follows: 280 DEG C are heated in 5min by -60 DEG C of initial temperature.Ingredient is parsed with another road-load
Gas helium enters gas chromatograph-mass spectrometer (GC-MS) analysis measurement.Wherein, cold hydrazine system is when being trapped and parsing two states
Working method are as follows: cold hydrazine trapping system be in cold hydrazine trapping state when, helium purge volatile component from deactivation stainless steel tube
Arrival end by trapping at low temperature glass cotton, then emptied from outlet end；It is another when cold hydrazine trapping system is in heating parsing
Road helium is from the outlet end of deactivation stainless steel tube by parsing from heating mineral wool, then inflow gas-chromatography-matter from arrival end
Compose combined instrument.
4 GC-MS analysis conditions are as follows:
Chromatographic column: DB-5MS chromatographic column, column length 30m, internal diameter 0.25mm, 0.25 μm of film thickness；
Temperature program: 40 DEG C of initial temperature, with the rate of 10 DEG C/min to 240 DEG C, then with the rate of 20 DEG C/min to 280
DEG C, keep 25min；
Injector temperature: 280 DEG C；
Input mode: split sampling, split ratio 100:1；
Sample volume: helium directly purges sample introduction through cold hydrazine system；
Transmission line temperature: 280 DEG C；
Ion source temperature: 230 DEG C；
Level four bars temperature: 150 DEG C；
Ionization mode: electron bombardment ionization source；
Ionizing energy: 70eV；
Mass number range: 35~550amu；
Mensuration mode: full scan；
Solvent delay: do not postpone.
5 qualitative, quantitative results
It is tested by above-mentioned steps (see Fig. 1), the qualitative, quantitative of cigarette major volatile constituents in quick-fried pearl sample A core material
As a result (chromatogram is shown in Fig. 3) as shown in table 1 below.
1 cigarette of table volatile component qualitative, quantitative result in quick-fried pearl sample A core material
The influence of the purging temperature of embodiment 2
Filter end temperature has the tendency that gradually increasing with the increase of pump orifice sequence when cigarette smoking, from light cigarette aspirate
To subsequent mouth second from the bottom, filter end temperature increases slowly first, and temperature range is room temperature between 40 DEG C, it is last flatly
There is a peak value in filter end temperature.Therefore, the detection being similar in embodiment 1 is carried out, in addition to will step 2 in embodiment 1
In purging temperature be respectively set to 30 DEG C, 40 DEG C, 50 DEG C, 60 DEG C it is outer, other conditional synchronizations rapid 1,3 and 4 are tested, to examine
Examine the influence that purging temperature discharges quick-fried bead core material volatile component.The results are shown in Table 2.
The influence of the purging temperature of table 2
As shown in Table 2, with the increase of purging temperature, the response peak area of 5 kinds of major volatile constituents is also gradually increased,
Amplitude of variation when especially increasing to 50 DEG C by 40 DEG C is maximum, reaches maximum value when to 60 DEG C.And discovery is tested, purge temperature
After reaching 60 DEG C, if the similar side reaction such as Maillard reaction can be occurred by continuing raising purging temperature, so as to cause
The generation of many side reaction products, result destroy the authenticity of sample.
The influence of 3 purge time of embodiment
Purge time is also an important parameter for influencing ingredient response peak area change, and purge time is too short, volatility
Ingredient can not trap completely, and purge time is too long, since in cryogenic trapping state, helium is blown to cold hydrazine system to cold hydrazine system
It is emptying mode behind place, the arresting efficiency of cold hydrazine will decline.Therefore, the detection being similar in embodiment 1 is carried out, in addition to will be in reality
It applies the purge time in example 1 in step 2 to be respectively set to outside 20min, 30min, 40min, 50min and 60min, other conditions are same
Step 1,3 and 4 are tested, to investigate influence of the purge time to quick-fried bead core material volatile component response peak area.As a result such as
Shown in table 3.
The influence of 3 purge time of table
As shown in Table 3, with the increase of purge time, the response peak area of 5 kinds of major volatile constituents is also gradually increased,
It is to reach stable state at 50~60min in purge time.
The evaluation of 4 test repeatability of embodiment
5 repetitive tests are carried out with quick-fried pearl sample A to cigarette by the detection and analysis step of embodiment 1, with evaluation method
Repeatability.
4 reproducibility of table
As shown in Table 4, the RSD value range of 5 kinds of main volatile components of selection is 3.85%~7.67%, shows this
The repeatability of invention detection method preferably, can meet the cigarette analysis of quick-fried bead core material volatile component.
The analysis of 5 cigarette of embodiment volatile component in quick-fried pearl sample B core material
Step tests cigarette with quick-fried pearl sample B as described in Example 1, and volatile component is qualitative fixed in core material
It is (chromatogram is shown in Fig. 4) as shown in table 5 below to measure result.
5 cigarette of table volatile component qualitative, quantitative result in quick-fried pearl sample B core material
The analysis of 3 cigarette of embodiment volatile component in quick-fried pearl sample C core material
Step tests cigarette with quick-fried pearl sample C as described in Example 1, and volatile component is qualitative fixed in core material
It is (chromatogram is shown in Fig. 5) as shown in table 5 below to measure result.
5 cigarette of table volatile component qualitative, quantitative result in quick-fried pearl sample C core material
In summary, the cold hydrazine capture method that the present invention is established for cigarette with volatile component in quick-fried bead core material has nothing
The advantages of cold and hot point, no cross contamination, no sample are discriminated against not only overcomes in adsorption trap trapping technique there are selective absorption,
It is also difficult to the shortcomings that cleaning out, polluting to analysis even across multiple aging, and the present invention is by the way of online
It carries out trapping analysis (i.e. integrated mode), can utmostly reduce damage of volatile component during purging and trapping
It loses, to improve the accuracy of analysis data.The present invention realizes that dynamic purging is analyzed with cold hydrazine trapping and gas chromatography-mass spectrography
On-line joining process, can utmostly reduce loss of volatile component during purging and trapping, with improve analysis it is accurate
Property；Its sensitivity of analytical method is high, reproducible.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of on-line analysis cigarette method of volatile component in quick-fried bead core material, which comprises the following steps:
S1. quick-fried pearl is placed in the syringe of disposable syringe, using isolating core material after the quick-fried pearl of syringe push rod attrition crushing；
S2. a small amount of core material is drawn with micro syringe to be injected into purging bottle, be passed through inert gas in 30~60 DEG C of progress dynamics
Purging, and trapped using cold hydrazine trapping system, heating cold hydrazine parsing volatile component enters gas chromatograph-mass spectrometer (GC-MS)
It is measured；Wherein, the cold hydrazine trapping system are as follows: loaded in deactivation stainless steel tube middle position and be compacted 1~3 mg glass
Cotton, the size of stainless steel tube are 100~120 mm of length, 2~4 mm of internal diameter.
2. the method according to claim 1, wherein the working method of the cold hydrazine trapping system are as follows: cold hydrazine is caught
When collecting system is in cold hydrazine trapping state, inert gas purge volatile component passes through low temperature from the arrival end of deactivation stainless steel tube
It traps at mineral wool, then is emptied from outlet end；When cold hydrazine trapping system is in heating parsing, another way inert gas is from deactivation
The outlet end of stainless steel tube is by parsing at heating mineral wool, then gas chromatograph-mass spectrometer (GC-MS) is flowed into from arrival end.
3. the method according to claim 1, wherein the inert gas carry out dynamic purging time be 10~
60 min。
4. the method according to claim 1, wherein the inert gas carry out dynamic purging flow velocity be 60~
80 mL/min。
5. the method according to claim 1, wherein the purging bottle is that Dynamic headspace purges vial.
6. the method according to claim 1, wherein the inert gas is helium.
7. the method according to claim 1, wherein the trapping operating temperature of the cold hydrazine trapping system is -60
℃。
8. the method according to claim 1, wherein the condition of cold hydrazine heating parsing are as follows: by initial temperature-
60 DEG C are heated to 280 DEG C in 5 min.
9. the method according to claim 1, wherein the line temperature for connecting each instrument and equipment is 240~260
℃。
10. any method according to claim 1~9, which is characterized in that the condition packet of gas chromatograph-mass spectrometer (GC-MS)
It includes:
Chromatographic column: the DB-5MS elastic capillary-column of mm × 0.25 μm 30 m × 0.25；
Stationary phase: (5%- phenyl)-methyl polysiloxane；
Temperature program: 40 DEG C of initial temperature, 3 min are kept, with the rate of 10 DEG C/min to 240 DEG C, then with the speed of 20 DEG C/min
Rate keeps 20~30 min to 280 DEG C；
Injector temperature: 280 DEG C；
Input mode: split sampling, split ratio 10:1~100:1；
Sample volume: inert gas directly purges sample introduction through cold hydrazine system；
Transmission line temperature: 280 DEG C；
Ion source temperature: 230 DEG C；
Level four bars temperature: 150 DEG C；
Ionization mode: electron bombardment ionization source；
Ionizing energy: 70 eV；
Mass number range: 35~550 amu；
Mensuration mode: full scan；
Solvent delay: do not postpone.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112763633A (en) * | 2021-01-19 | 2021-05-07 | 云南中烟工业有限责任公司 | Device and method for determining heated migration components of filter stick additive by dynamic headspace method |
| CN115326946A (en) * | 2022-06-27 | 2022-11-11 | 红塔烟草(集团)有限责任公司 | Pretreatment method for flavoring glyceryl triacetate for cigarettes |
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