CN105842374B - Method for quantitative analysis of main pyrazine flavor substances in cigarette mainstream smoke - Google Patents
Method for quantitative analysis of main pyrazine flavor substances in cigarette mainstream smoke Download PDFInfo
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Abstract
The invention discloses a method for quantitative analysis of main pyrazine flavor substances in cigarette mainstream smoke and relates to a method for gas chromatography-tandem mass spectrometer-based determination of eight main pyrazine flavor substances such as 2-methylpyrazine, 2, 5-dimethylpyrazine, 2, 6-dimethylpyrazine, 2-methoxypyrazine, 2, 3, 5-trimethylpyrazine, 2-ethyl-3-methylpyrazine, 2, 3, 5, 6-tetramethylpyrazine and 2-acetylpyrazine in cigarette mainstream smoke. The method comprises internal standard solution, standard work solution and sample solution preparation, gas chromatography-tandem mass spectrometry analysis and determination result calculation. The improved detection method can be operated simply, has response sensitivity and quantitative analysis accuracy, effectively reduces complex sample matrix-caused interference and is suitable for quantitative analysis of a trace quantity of a target object in a complex flue gas matrix.
Description
Technical field
The invention discloses in a kind of quantitative analysis cigarette mainstream flue gas main Pyrazine fragrance matter method, it is concrete come
Say it is to be related to a kind of side that the main Pyrazine fragrance matter of trace in cigarette smoke is determined based on gas-chromatography-tandem mass spectrometer
Method, belongs to cigarette physical and chemical index detection technique field.
Background technology
In recent years, affected by multiple factors such as the popular tastes of smoking and healthy, cigarette, the consumption feature of cigarette is just gradually
To high fragrance, low tar, the transformation of less harmful direction.To adapt to this requirement, research charging perfuming technology selects various plus perfumery
Matter, to adapt to and meet the needs of different leaf group structures.Among these, pyrazine compounds play this in fragrance-enhancing tobacco technology
More and more significant effect.Pyrazine compounds are the food flavor materials commonly used in baked goods, grease perfuming, and it has dense
The roasting fragrance of strongly fragrant Jiao, uses as tobacco aromaticss, can not only make unique product style, fragrance abundance, strength moderate, and can also
The miscellaneous gas in part is covered, improves pleasant impression.The 2- methylpyrazines that use as table perfume (or spice), 2,5-dimethyl pyrazine, 2,6 dimethyl pyrazine,
2- IBMPs, 2,3,5- trimethylpyrazines, 2- ethyl -3- methylpyrazines, 2,3,5,6- Tetramethylpyrazines and 2- acetyl group
The main pyrazine compounds such as pyrazine, can set off out the distinctive local flavor of tobacco, make fragrance harmonious, it is to avoid during cigarette burning its
Adverse effect of its material to cigarette smoke.
Research finds there are various pyrazine compounds in tobacco and flue gas, identified out up to nearly 60 kinds, its
In two replacements and three replacement pyrazines it is more, a more also replacement and four replacement pyrazines, substituent is generally methyl, ethyl, different
Propyl group, vinyl, acetyl group etc..Here, a class is alkyl pyrazine in the fragrance matter for constituting cigarette mainstream flue gas feature,
For example, the minor compound such as 2,5- dimethyl pyrazines, 2,6- dimethyl pyrazines, 2,3,5- trimethylpyrazines, 2- acetyl group pyrazines.
Its source is related, beyond outer addition, the pyrazine compounds in tobacco and flue gas may be from the palm fibre in process
Color product, additionally, some carbon containing nitrogen substances can be used as the source of Pyrazine pyrolysis synthesis when burning and sucking.
Comprehensive consulting literatures, it is found that both at home and abroad some technological staffs (include pyrrole to the nitrogen substance in tobacco and cigarette
Piperazine class compound) qualitative and quantitative analysis were carried out, the method for using is mainly the instrument means such as GC, GC/MS.Generally speaking, lack
The weary accurate quantification analysis to pyrazine compounds in cigarette smoke.Limit cigarette smoke matrix complicated, and Pyrazine material
Content it is little, conventional instrument means are difficult to carry out Simultaneous Quantitative Analysis to the pyrazine compounds in flue gas.Gas-chromatography-
Tandem mass spectrum (GC-MS/MS) is a kind of Chromatography/Mass Spectrometry GC-MS developed in recent years.Due to sample pre-treatments
It is simple and convenient to operate, cleans the clear superiorities such as experiment, is widely used to environmental monitoring, chemical industry, metallurgy, geology, the hydrology, soil
The field of scientific studies such as earth, electronics industry, food and drink, clinical assay.For this purpose, analysis hand of this patent using GC-MS/MS
Section, first to cigarette smoke in main Pyrazine material carried out quantitative analysis.
The content of the invention
It is contemplated that overcoming existing technological deficiency, there is provided one kind determines cigarette using gas chromatography tandem mass spectrometry instrument
The method of trace Pyrazine fragrance matter content in main flume, trace in the method energy accurate quantification analysis cigarette mainstream flue gas
The content of Pyrazine fragrance matter, measurement result is accurate, sensitivity is high, and matrix interference is few.
Technical scheme is as follows：
The method of main Pyrazine fragrance matter, the Pyrazine fragrance matter in a kind of quantitative analysis cigarette mainstream flue gas
Including 2- methylpyrazines, 2,5-dimethyl pyrazine, 2,6 dimethyl pyrazine, 2- IBMPs, 2,3,5- trimethylpyrazines, 2-
Ethyl -3- methylpyrazines, Tetramethylpyradine and 2- acetyl group pyrazines, it is characterised in that methods described includes following
Step：
(1) preparation of inner mark solution：The use of ethanol is solvent with heptadecane as internal standard compound, prepares inner mark solution；
(2) preparation of standard working solution：With 2- methylpyrazines, 2,5-dimethyl pyrazine, 2,6 dimethyl pyrazine, 2- first
Epoxide pyrazine, 2,3,5- trimethylpyrazines, 2- ethyl -3- methylpyrazines, 2,3,5,6- Tetramethylpyrazines and 2- acetyl group pyrazines
Standard items Deng material are object, the use of ethanol are solvent, and Jing stepwise dilutions are prepared into Standard Stock solutions, are then added respectively
Enter a certain amount of inner mark solution, be prepared into standard working solution；
(3) preparation of sample solution：Gather the object in cigarette smoke, accurately add a certain amount of inner mark solution with
And the extraction solution of certain volume, mechanical shaking extraction, extract crosses diatomite and carries out back extraction, then leacheate is concentrated,
Obtain sample solution；
(4) gas chromatography tandem mass spectrometry instrument analysis：Standard is worked with gas chromatography tandem mass spectrometry instrument (GC-MS/MS)
Solution and sample solution are tested and analyzed；
(5) drafting of standard working curve and the calculating of sample result.
Wherein the preparation of step (1) inner mark solution, specifically includes following steps：(1a) internal standard storing solution：Accurately weigh
0.2g heptadecanes, are accurate to 0.1mg, in the volumetric flask of 100mL, scale are dissolved and be settled to ethanol；(1b) internal standard
Solution：0.1mL internal standard storing solutions are accurately pipetted, in the volumetric flask of 100mL, scale is diluted and be settled to ethanol.
The preparation of wherein step (2) standard working solution specifically includes following steps：(2a) primary standard storing solution：Accurately
Weigh 0.2g 2- methylpyrazines, 0.15g 2,5-dimethyl pyrazines, 0.1g 2,6 dimethyl pyrazines, 0.05g 2- methoxyl group pyrroles
Piperazine, 0.1g 2,3,5- trimethylpyrazines, 0.1g 2- ethyl -3- methylpyrazines, 0.05g 2,3,5,6- Tetramethylpyrazines and
0.05g 2- acetyl group pyrazines, are accurate to 0.1mg, in the volumetric flask of 100mL, scale are dissolved and be settled to ethanol；(2b)
Secondary standard storing solution：1mL primary standard storing solutions are accurately pipetted, in the volumetric flask of 100mL, is diluted with ethanol and is settled to
Scale；(2c) standard working solution：Accurately pipette respectively the μ L of secondary standard storing solution 50,100 μ L, 300 μ L, 600 μ L, 1mL and
3mL, into the volumetric flask of 10mL, then accurately adds respectively 1mL inner mark solutions, and scale is diluted and be settled to ethanol, obtains serial
Standard working solution.
The preparation of wherein step (3) sample solution specifically includes following steps：(3a) cigarette smoking：According to GB/T19609
20 cigarette are aspirated in the requirement of standard, wherein trapping the granule phase substance in cigarette mainstream flue gas with cambridge filter；(3b) granule phase substance extraction
Take：The cambridge filter of trapping cigarette mainstream smoke condensate is transferred in 250mL bread bottles, is 10mmol/L with 40mL concentration
Aqueous hydrochloric acid solution carry out oscillation extraction, extraction time is 40min, obtains extract；(3c) extract back extraction：In advance to silicon
Diatomaceous earth SPE pillar (filler is 20g) is activated, that is, moving into 50mL dichloromethane carries out drip washing activation, drains as far as possible, treats SPE
After pillar is ready to, the above-mentioned extracts of 10mL are pipetted into SPE pillars, with a concentrate bottle leacheate is received；Then 60mL is used again
Dichloromethane repeatedly carries out drip washing to pillar, by the big feature of dichloromethane density ratio water, voluntarily drips, and collects all staying
The liquid for coming, is considered as leacheate；(3d) leacheate concentration：Under 50 DEG C, condition of normal pressure, 1mL is concentrated to leacheate, obtains sample
Product sample introduction solution.
Wherein step (4) GC-MS/MS is analyzed, and its instrumental conditions is：Specification is adopted for 30m × 0.25mm × 0.25 μ
The HP-INNOWAX capillary chromatographic columns of m；Carrier gas is helium, and constant current speed is 1.0mL/min；Input mode：Sample size is 1 μ
L, split sampling, split ratio is 10：1；Injector temperature is 240 DEG C；Transmission line temperature is 260 DEG C；Heating schedule is initial temperature
Spend for 50 DEG C, with the speed of 5 DEG C/min 240 DEG C are increased to, keep 5min.Its mass spectral analysis condition is：Ionization mode is EI sources,
Positive ion mode；Ion source temperature：230℃；Quadrupole rod temperature：It is 150 DEG C；Collision gas：Nitrogen, flow velocity 1.5mL/min is carried
Gas (helium) flow velocity is 2.25mL/min；Multiple-reaction monitoring (MRM) pattern, detail parameters are listed in the table below.
The MRM parameter situations of object
Wherein step (5) Specification Curve of Increasing and result are calculated as follows：With object in standard working solution and interior target
The ratio of concentration is abscissa, and object carries out linear regression analysis with the ratio of interior target peak area as ordinate with chromatogram,
Obtain standard working curve.By object in the sample solution measured under the same terms and interior target chromatographic peak area ratio, substitute into
Standard working curve, according to following equation the content of object in cigarette sample is tried to achieve：
In formula：
W --- the content of 8 kinds of main Pyrazine fragrance matters in cigarette mainstream flue gas, unit is microgram per (μ g/)；
A --- the peak area of 8 kinds of main Pyrazine fragrance matters；
As --- target peak area in correspondence；
The intercept of b --- standard working curve；
Ms --- target quality in addition, unit is microgram (μ g)；
The slope of a --- standard working curve；
The quantity of M --- cigarette, unit is to prop up.
Beneficial effect：The detection method of the present invention is optimized really to sample treatment and chromatograph mass spectrum analysis condition
Recognize.Compared with prior art, the present invention has following excellent results：
(1) the inventive method creative use gas chromatography tandem mass spectrometry instrument determines trace Pyrazine in cigarette mainstream flue gas
The content of fragrance matter, solves that flue gas pyrazine compounds level is low, and analysis of the flue gas complex matrices to object is done
Disturb the impact of the factor such as serious.
(2) the inventive method is easily soluble in water, partially weakly alkaline physicochemical property for pyrazine compounds, using faintly acid
The aqueous solution object is extracted, then in conjunction with using diatomite SPE pillars, take out from the aqueous solution back extraction containing object
Trace object, method is novel, strong innovation, compensate in the past big, repeated using Simultaneous distillation-extraction process intensity
Not good enough shortcoming.
(3) the inventive method utilizes inner mark method ration, without accurate constant volume, and be able to can reduce by pre-treating method weight
The error that existing property and instrument precision problem are brought.
Description of the drawings
Fig. 1 is the flow chart of assay method of the present invention；
Fig. 2 is the Ion-pair chromalography of 8 kinds of main Pyrazine fragrance matters and internal standard heptadecane in standard working solution
Figure；
Fig. 3 is the Ion-pair chromalography of 8 kinds of main Pyrazine fragrance matters and internal standard heptadecane in cigarette mainstream flue gas
Figure.
Specific embodiment
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1
Detection method following (the detection of the present embodiment to the main Pyrazine fragrance matter of trace in cigarette mainstream flue gas
The flow chart of method is as shown in Figure 1)：
(1) preparation of inner mark solution
1. internal standard storing solution：0.202g heptadecanes are accurately weighed, 0.1mg is accurate to, in the volumetric flask of 100mL,
Scale is dissolved and is settled to ethanol.2. inner mark solution：0.1mL internal standard storing solutions are accurately pipetted, in the volumetric flask of 100mL,
Scale is diluted and is settled to ethanol.Wherein the concentration of heptadecane is 2.02 μ g/mL.
(2) preparation of standard working solution
1. primary standard storing solution：Accurately weigh 0.2011g 2- methylpyrazines, 0.1560g 2,5-dimethyl pyrazines,
0.1032g 2,6 dimethyl pyrazines, 0.0523g 2- IBMPs, 0.1005g 2,3,5- trimethylpyrazines, 0.1079g
2- ethyl -3- methylpyrazines, 0.05577g Tetramethylpyradines and 0.0332g 2- acetyl group pyrazines, are accurate to
0.1mg, in the volumetric flask of 100mL, dissolves and is settled to scale with ethanol.2. secondary standard storing solution：Accurately pipette 1mL mono-
Level standard reserving solution, in the volumetric flask of 100mL, dilutes and is settled to scale with ethanol.3. standard working solution：It is accurate respectively
The μ L of secondary standard storing solution 50,100 μ L, 300 μ L, 600 μ L, 1mL and 3mL are pipetted, it is into the volumetric flask of 10mL then accurate respectively
1mL inner mark solutions are added, scale is diluted and be settled to ethanol, obtain series standard working solution.Wherein 2- methylpyrazines is dense
Degree scope be 0.1006～6.033 μ g/mL, 2,5-dimethyl pyrazine concentration range be 0.078～4.68 μ g/mL, 2,6- bis-
It is 0.0261～1.5675 that the concentration range of methylpyrazine is the concentration range of 0.0516～3.096 μ g/mL, 2- IBMPs
The concentration range of μ g/mL, 2,3,5- trimethylpyrazines is the concentration of 0.0503～3.015 μ g/mL, 2- ethyl -3- methylpyrazines
Scope be 0.054～3.237 μ g/mL, Tetramethylpyradine concentration range be 0.029～1.730 μ g/mL, and
2- acetyl group pyrazines concentration range is 0.0166～0.996g/mL.
(3) preparation of sample solution
1. cigarette smoking：Yi Yi cities pin cigarette is object, and according to the requirement of GB/T19609 standards 20 cigarette are aspirated, its
The middle granule phase substance trapped with cambridge filter in cigarette mainstream flue gas.2. granule phase substance extraction：Cigarette mainstream smoke condensate will be trapped
Cambridge filter be transferred in 250mL bread bottles, oscillation extraction is carried out with the aqueous hydrochloric acid solution that 40mL concentration is 10mmol/L, extract
The time is taken for 40min, extract is obtained.(3) extract back extraction：Diatomite SPE pillars (filler is 20g) are lived in advance
Change, that is, moving into 50mL dichloromethane carries out drip washing activation, drains as far as possible.After SPE pillars are ready to, the above-mentioned extractions of 10mL are pipetted
Liquid enters SPE pillars, and with a concentrate bottle leacheate is received；Then with 60mL dichloromethane repeatedly drip washing is carried out to pillar again, according to
By the big feature of dichloromethane density ratio water, voluntarily drip, collect all liquid for staying, be considered as leacheate.(4) leacheate
Concentration：Under 50 DEG C, condition of normal pressure, 1mL is concentrated to leacheate, obtains sample feeding solution.
(4) gas chromatography tandem mass spectrometry analysis
Taking the standard working solution and sample solution to be measured of 6 variable concentrations respectively carries out gas chromatography tandem mass spectrometry analysis
(in the standard working solution, typical sample solution the chromatogram of object and internal standard compound as shown in Figure 2 to 3).
Its instrumental conditions is：Using HP-INNOWAX (30m × 0.25mm × 0.25 μm) capillary chromatographic column；Carrier gas
For helium, constant current speed is 1.0mL/min；Input mode：Sample size is 1 μ L, and split sampling, split ratio is 10：1；Injection port
Temperature is 240 DEG C；Transmission line temperature is 260 DEG C；It is 50 DEG C that heating schedule is initial temperature, is increased to the speed of 5 DEG C/min
240 DEG C, keep 5min.Its mass spectral analysis condition is：Ionization mode be EI sources, positive ion mode；Ion source temperature：230℃；Four
Pole bar temperature：It is 150 DEG C；Collision gas：Nitrogen, flow velocity 1.5mL/min, carrier gas (helium) flow velocity is 2.25mL/min；It is more anti-
(MRM) pattern should be monitored, detail parameters are listed in the table below.
The MRM parameter situations of object
(5) Specification Curve of Increasing and result are calculated
First, the ratio with object in standard working solution and interior target concentration is as abscissa, with object in chromatogram
Ratio with interior target peak area is ordinate, carries out linear regression analysis, obtains standard working curve.Take the standard of least concentration
Working solution, does 9 Parallel testing analyses, calculates its standard deviation, and with the corresponding concentration of 3 times of standard deviation, conversion draws
The detection limit of method.The data such as regression equation, coefficient correlation, the detection limit corresponding with standard working curve see the table below.
The working curve and detection limit of analysis method
By object in the sample solution measured under the same terms and interior target chromatographic peak area ratio, standard work is substituted into bent
Line, according to following equation the content of object in cigarette sample is tried to achieve.
In formula：
W --- the content of 8 kinds of main Pyrazine fragrance matters in cigarette mainstream flue gas, unit is microgram per (μ g/)；
A --- the peak area of 8 kinds of main Pyrazine fragrance matters；
As --- target peak area in correspondence；
The intercept of b --- standard working curve；
Ms --- target quality in addition, unit is microgram (μ g)；
The slope of a --- standard working curve；
The quantity of M --- cigarette, unit is to prop up.
8 kinds of main Pyrazine fragrance matter testing results see the table below in cigarette sample main flume in the present embodiment：
| Material title | Content (μ g/) |
| 2- methylpyrazines | 15.95 |
| 2,5-dimethyl pyrazine | 2.31 |
| 2,6 dimethyl pyrazine | 9.01 |
| 2- IBMPs | 0.11 |
| 2,3,5- trimethylpyrazines | 2.33 |
| 2- ethyl -3- methylpyrazines | 0.70 |
| 2,3,5,6- Tetramethylpyrazines | 0.29 |
| 2- acetyl group pyrazines | 0.32 |
Embodiment 2
The present embodiment is as follows to the precision of the present invention and the detection method of recovery of standard addition：
Cigarette sample used has carried out respectively withinday precision experiment to analyze object with embodiment 1, in a few days accurate
Degree experiment is same sample parallel determination 6 times (same batch processed) under identical conditions, and 6 parallel determinations are calculated respectively
Relative standard deviation (RSD), measurement result see the table below.Result shows in table, the in a few days repeated RSD of this experimental technique<
10%, for the quantitative analysis of trace materials, show that method has good precision.
| Material title | RSD (%) |
| 2- methylpyrazines | 5.20 |
| 2,5-dimethyl pyrazine | 5.17 |
| 2,6 dimethyl pyrazine | 8.78 |
| 2- IBMPs | 8.13 |
| 2,3,5- trimethylpyrazines | 9.97 |
| 2- ethyl -3- methylpyrazines | 3.18 |
| 2,3,5,6- Tetramethylpyrazines | 5.31 |
| 2- acetyl group pyrazines | 9.76 |
With yoghurt example used by replica test to analyze object, processed according to above-mentioned sample-pretreating method, plus
Enter the standard specimen of the suitable content of its burst size, carry out matrix mark-on test, as a result see the table below.As can be seen from the table, sample
Between 84.50%～118.88%, illustration method has preferable accuracy to recovery of standard addition.
| Material title | Recovery of standard addition (%) |
| 2- methylpyrazines | 84.50 |
| 2,5-dimethyl pyrazine | 101.75 |
| 2,6 dimethyl pyrazine | 92.30 |
| 2- IBMPs | 89.49 |
| 2,3,5- trimethylpyrazines | 114.81 |
| 2- ethyl -3- methylpyrazines | 101.65 |
| 2,3,5,6- Tetramethylpyrazines | 118.88 |
| 2- acetyl group pyrazines | 114.35 |
What the standard liquid used in the present embodiment was only illustrated by taking one of concentration as an example, other concentration value institutes
The standard liquid Jing gas chromatography tandem mass spectrometries instrument of preparation analyzes obtained calibration curve and regression equation and above-described embodiment
Identical, here is not being enumerated.Illustrated embodiment is intended merely to be better understood from the inventive method, not with any restriction
The method of effect, i.e. said method or the above-mentioned situation of equivalent is all contained in the protection domain of technical scheme.
Embodiments of the present invention are described in detail above in conjunction with the drawings and specific embodiments, but the present invention is not
Be limited to above-mentioned embodiment, in the ken that art those of ordinary skill possesses, can with without departing from
Make a variety of changes on the premise of present inventive concept.
Claims (6)
1. in a kind of quantitative analysis cigarette mainstream flue gas main Pyrazine fragrance matter method, the Pyrazine fragrance matter bag
Include 2- methylpyrazines, 2,5-dimethyl pyrazine, 2,6 dimethyl pyrazine, 2- IBMPs, 2,3,5- trimethylpyrazines, 2- second
Base -3- methylpyrazines, Tetramethylpyradine and 2- acetyl group pyrazines, it is characterised in that methods described includes following step
Suddenly：
(1) preparation of inner mark solution：The use of ethanol is solvent with heptadecane as internal standard compound, prepares inner mark solution；
(2) preparation of standard working solution：With 2- methylpyrazines, 2,5-dimethyl pyrazine, 2,6 dimethyl pyrazine, 2- methoxyl groups
The mark of pyrazine, 2,3,5- trimethylpyrazines, 2- ethyl -3- methylpyrazines, 2,3,5,6- Tetramethylpyrazines and 2- acetyl group pyrazines
Quasi- product are object, the use of ethanol are solvent, and Jing stepwise dilutions are prepared into Standard Stock solutions, are then respectively adding a certain amount of
Inner mark solution, is prepared into standard working solution；
(3) preparation of sample solution：Aqueous hydrochloric acid solution using concentration as 10mmol/L is as extraction solution and with dichloromethane work
For back extraction eluent solution, the object in cigarette smoke is gathered, accurately add a certain amount of inner mark solution and certain body
Long-pending extraction solution, mechanical shaking extraction, extract crosses diatomite and carries out back extraction, then leacheate is concentrated, and obtains sample molten
Liquid；
(4) gas chromatography tandem mass spectrometry instrument analysis：With gas chromatography tandem mass spectrometry instrument to standard working solution and sample solution
Tested and analyzed；
(5) drafting of standard working curve and the calculating of sample result.
2. in quantitative analysis cigarette mainstream flue gas according to claim 1 main Pyrazine fragrance matter method, it is special
Levy and be, the preparation of step (1) inner mark solution includes：
(1a) internal standard storing solution：0.2g heptadecanes are accurately weighed, 0.1mg is accurate to, in the volumetric flask of 100mL, second is used
Alcohol dissolves and is settled to scale；
(1b) inner mark solution：0.1mL internal standard storing solutions are accurately pipetted, in the volumetric flask of 100mL, is diluted with ethanol and is settled to
Scale.
3. in quantitative analysis cigarette mainstream flue gas according to claim 1 main Pyrazine fragrance matter method, it is special
Levy and be, the preparation of step (2) standard working solution includes：
(2a) primary standard storing solution：Accurately weigh 0.2g 2- methylpyrazines, 0.15g 2,5-dimethyl pyrazines, 0.1g 2,6-
Dimethyl pyrazine, 0.05g 2- IBMPs, 0.1g 2,3,5- trimethylpyrazines, 0.1g 2- ethyl -3- methylpyrazines,
0.05g Tetramethylpyradines and 0.05g 2- acetyl group pyrazines, are accurate to 0.1mg, in the volumetric flask of 100mL, use
Ethanol dissolves and is settled to scale；
(2b) secondary standard storing solution：1mL primary standard storing solutions are accurately pipetted, in the volumetric flask of 100mL, is diluted with ethanol
And it is settled to scale；
(2c) standard working solution：Accurately pipette respectively the μ L of secondary standard storing solution 50,100 μ L, 300 μ L, 600 μ L, 1mL and
3mL, into the volumetric flask of 10mL, then accurately adds respectively 1mL inner mark solutions, and scale is diluted and be settled to ethanol, obtains serial
Standard working solution.
4. in quantitative analysis cigarette mainstream flue gas according to claim 1 main Pyrazine fragrance matter method, it is special
Levy and be, the preparation of step (3) sample solution includes：
(3a) cigarette smoking：20 cigarette are aspirated in requirement according to GB/T19609 standards, wherein trapping cigarette master with cambridge filter
Granule phase substance in stream flue gas；
(3b) granule phase substance extraction：The cambridge filter of trapping cigarette mainstream smoke condensate is transferred in 250mL bread bottles, is used
40mL concentration carries out oscillation extraction for the aqueous hydrochloric acid solution of 10mmol/L, and extraction time is 40min, obtains extract；
(3c) extract back extraction：The diatomite SPE pillars of filler 20g are activated in advance, that is, moves into 50mL dichloromethane
Drip washing activation is carried out, is drained as far as possible, after SPE pillars are ready to, pipette the above-mentioned extracts of 10mL into SPE pillars；Then again
Repeatedly drip washing is carried out to pillar with 60mL dichloromethane, by the big feature of dichloromethane density ratio water, voluntarily dripped, collect institute
There is the liquid for staying, be considered as leacheate, with a concentrate bottle leacheate is received；
(3d) leacheate concentration：Under 50 DEG C, condition of normal pressure, 1mL is concentrated to leacheate, obtains sample feeding solution.
5. in quantitative analysis cigarette mainstream flue gas according to claim 1 main Pyrazine fragrance matter method, it is special
Levy and be, the instrumental conditions of step (4) GC-MS/MS analyses are：Adopt specification for 30m × 0.25mm × 0.25 μm HP-
INNOWAX capillary chromatographic columns；Carrier gas is helium, and constant current speed is 1.0mL/min；Input mode：Sample size is 1 μ L, is shunted
Sample introduction, split ratio is 10：1；Injector temperature is 240 DEG C；Transmission line temperature is 260 DEG C；It is 50 that heating schedule is initial temperature
DEG C, 240 DEG C are increased to the speed of 5 DEG C/min, keep 5min；Its mass spectral analysis condition is：Ionization mode be EI sources, cation
Pattern；Ion source temperature：230℃；Quadrupole rod temperature：It is 150 DEG C；Collision gas：Nitrogen, flow velocity 1.5mL/min, carrier gas helium
Flow velocity is 2.25mL/min；Multiple-reaction monitoring MRM patterns, detail parameters are listed in the table below：
The MRM parameter situations of object
6. in quantitative analysis cigarette mainstream flue gas according to claim 1 main Pyrazine fragrance matter method, it is special
Levy and be, step (5) Specification Curve of Increasing and result are calculated as follows：With object in standard working solution and interior target concentration it
Than for abscissa, object carries out linear regression analysis with the ratio of interior target peak area as ordinate with chromatogram, is marked
Quasi- working curve；By object in the sample solution measured under the same terms and interior target chromatographic peak area ratio, standard work is substituted into
Make curve, the content of object in cigarette sample is tried to achieve according to following equation：
In formula：
W --- the content of 8 kinds of main Pyrazine fragrance matters in cigarette mainstream flue gas, unit is μ g/；
A --- the peak area of 8 kinds of main Pyrazine fragrance matters；
As --- target peak area in correspondence；
The intercept of b --- standard working curve；
Ms --- target quality in addition, unit is μ g；
The slope of a --- standard working curve；
The quantity of M --- cigarette, unit is to prop up.
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| CN110031571B (en) * | 2019-05-23 | 2021-09-07 | 上海烟草集团有限责任公司 | Method for measuring content of vanillin and ethyl vanillin in cigarette mainstream smoke |
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