CN105842374A - 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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- CN105842374A CN105842374A CN201610046409.6A CN201610046409A CN105842374A CN 105842374 A CN105842374 A CN 105842374A CN 201610046409 A CN201610046409 A CN 201610046409A CN 105842374 A CN105842374 A CN 105842374A
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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
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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
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
- G01N2030/884—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample organic compounds
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 a kind of method of main Pyrazine fragrance matter in quantitative analysis cigarette mainstream flue gas, specifically come
Say and relate to a kind of measure the side of trace main Pyrazine fragrance matter in cigarette smoke based on gas chromatogram tandem mass spectrometer
Method, belongs to Medicated cigarette physical and chemical index detection technique field.
Background technology
In recent years, being affected with multiple factors such as health, the popular tastes of Medicated cigarette by smoking, the consumption feature of Medicated cigarette is the most gradually
Change to high fragrance, low tar, less harmful direction.For adapting to this requirement, research charging perfuming technology, select various to add perfumery
Matter, to adapt to and to meet the needs of different leaf group structure.Among these, pyrazine compounds plays this in fragrance-enhancing tobacco technology
More and more significant effect.Pyrazine compounds is food flavor material conventional in baked goods, oils and fats perfuming, and it has dense
Strongly fragrant Jiao bakes fragrance, uses as tobacco aromatics using, and product style uniqueness, fragrance abundance, strength not only can be made moderate, and can also
Cover part miscellaneous QI, improve pleasant impression.The 2-methylpyrazine that uses as table perfume (or spice), 2,5-dimethyl pyrazine, 2,6 dimethyl pyrazine,
2-methoxypyrazine, 2,3,5-trimethylpyrazine, 2-ethyl-3-methylpyrazine, 2,3,5,6-tetramethylpyazine and 2-acetyl group
The main pyrazine compounds such as pyrazine, can set off out the distinctive local flavor of Nicotiana tabacum L., makes fragrance harmonious, it is to avoid during cigarette burning its
Its material adverse effect to cigarette smoke.
Research finds, there is multiple pyrazine compounds in Nicotiana tabacum L. and flue gas, the most identified out the nearlyest 60 kinds, its
In two replacements and three replacement pyrazines more, also have some replacements and four replacement pyrazines, substituent group is generally methyl, ethyl, different
Propyl group, vinyl, acetyl group etc..Here, having a class in the fragrance matter of composition cigarette mainstream flue gas feature is alkyl pyrazine,
Such as, 2,5-dimethyl pyrazines, 2, the minor compound such as 6-dimethyl pyrazine, 2，3，5-trimethylpyrazine, 2-acetyl group pyrazine.
Relating its source, beyond outer interpolation, the pyrazine compounds in Nicotiana tabacum L. and flue gas may be from the palm fibre in the course of processing
Color product, additionally, some carbon containing nitrogen substance can be as the source of Pyrazine pyrolysis synthesis when burning and sucking.
Comprehensive consulting literatures, finds that some technological staff (comprise pyrrole to the nitrogen substance in Nicotiana tabacum L. and Medicated cigarette both at home and abroad
Piperazine compounds) carried out qualitative and quantitative analysis, the method for use is mainly the instrument means such as GC, GC/MS.Generally speaking, lack
Weary to the accurate quantification analysis of pyrazine compounds in cigarette smoke.Limit cigarette smoke substrate complicated, and Pyrazine material
Content little, conventional instrument means are difficult to the pyrazine compounds in flue gas is carried out Simultaneous Quantitative Analysis.Gas chromatogram-
Tandem mass spectrum (GC-MS/MS) is a kind of Chromatography/Mass Spectrometry multiple techniques that development in recent years is got up.Owing to having sample pre-treatments
It is simple and convenient to operate, cleans the clear superiorities such as experiment, be 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.To this end, this patent uses the analysis hands of GC-MS/MS
Section, has carried out quantitative analysis to the main Pyrazine material in cigarette smoke first.
Summary of the invention
It is contemplated that overcome existing technological deficiency, it is provided that a kind of employing gas chromatography tandem mass spectrometry instrument measures Medicated cigarette
The method of trace Pyrazine fragrance matter content in main flume, the method energy accurate quantification analyzes trace in cigarette mainstream flue gas
The content of Pyrazine fragrance matter, measurement result is accurate, highly sensitive, and matrix interference is few.
Technical scheme is as follows:
The method of main Pyrazine fragrance matter, described Pyrazine fragrance matter in a kind of quantitative analysis cigarette mainstream flue gas
Including 2-methylpyrazine, 2,5-dimethyl pyrazine, 2,6 dimethyl pyrazine, 2-methoxypyrazine, 2,3,5-trimethylpyrazine, 2-
Ethyl-3-methylpyrazine, 2，3，5，6-tetramethylpyrazine and 2-acetyl group pyrazine, it is characterised in that described method includes following
Step:
(1) preparation of inner mark solution: with heptadecane as internal standard substance, using ethanol is solvent, prepares inner mark solution；
(2) preparation of standard working solution: with 2-methylpyrazine, 2,5-dimethyl pyrazine, 2,6 dimethyl pyrazine, 2-first
Epoxide pyrazine, 2,3,5-trimethylpyrazine, 2-ethyl-3-methylpyrazine, 2,3,5,6-tetramethylpyazine and 2-acetyl group pyrazine
Being object Deng the standard substance of material, use ethanol is solvent, is prepared as Standard Stock solutions through stepwise dilution, adds the most respectively
Enter a certain amount of inner mark solution, be prepared as 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 kieselguhr and carries out back extraction, then concentrate leacheate,
Obtain sample solution；
(4) gas chromatography tandem mass spectrometry instrument is analyzed: work standard with gas chromatography tandem mass spectrometry instrument (GC-MS/MS)
Solution and sample solution carry out detection and analyze；
(5) drafting of standard working curve and the calculating of sample result.
The wherein preparation of step (1) inner mark solution, specifically includes following steps: (1a) internal standard storing solution: accurately weigh
0.2g heptadecane, is accurate to 0.1mg, in the volumetric flask of 100mL, dissolves with ethanol and is settled to scale；(1b) internal standard
Solution: accurately pipette 0.1mL internal standard storing solution, in the volumetric flask of 100mL, with ethanol dilution and be settled to scale.
Wherein the preparation of step (2) standard working solution specifically includes following steps: (2a) primary standard storing solution: accurately
Weigh 0.2g 2-methylpyrazine, 0.15g 2,5-dimethyl pyrazine, 0.1g 2,6 dimethyl pyrazine, 0.05g 2-methoxyl group pyrrole
Piperazine, 0.1g 2,3,5-trimethylpyrazine, 0.1g 2-ethyl-3-methylpyrazine, 0.05g 2,3,5,6-tetramethylpyazine and
0.05g 2-acetyl group pyrazine, is accurate to 0.1mg, in the volumetric flask of 100mL, dissolves with ethanol and be settled to scale；(2b)
Secondary standard storing solution: accurately pipette 1mL primary standard storing solution, in the volumetric flask of 100mL, with ethanol dilution and be settled to
Scale；(2c) standard working solution: the most accurately pipette secondary standard storing solution 50 μ L, 100 μ L, 300 μ L, 600 μ L, 1mL and
3mL, to the volumetric flask of 10mL, then adds respectively accurately 1mL inner mark solution, with ethanol dilution and be settled to scale, obtains serial
Standard working solution.
Wherein the preparation of step (3) sample solution specifically includes following steps: (3a) cigarette smoking: according to GB/T19609
Requirement 20 Medicated cigarette of suction of standard, wherein with the granule phase substance in cambridge filter trapping cigarette mainstream flue gas；(3b) granule phase substance extraction
Take: the cambridge filter of trapping cigarette mainstream smoke condensate is transferred in 250mL bread bottle, is 10mmol/L by 40mL concentration
Aqueous hydrochloric acid solution carry out oscillation extraction, extraction time is 40min, is extracted liquid；(3c) extract back extraction: in advance to silicon
Diatomaceous earth SPE pillar (filler is 20g) activates, and i.e. moves into 50mL dichloromethane and carries out drip washing activation, drains as far as possible, treat SPE
After pillar is ready to, pipettes the above-mentioned extract of 10mL and enter SPE pillar, concentrate bottle graft with one and receive leacheate；Use 60mL the most again
Dichloromethane repeatedly carries out drip washing to pillar, relies on the feature that dichloromethane density is bigger than water, drips voluntarily, collect all staying
The liquid come, is considered as leacheate；(3d) leacheate concentrates: 50 DEG C, under condition of normal pressure, leacheate is concentrated to 1mL, obtains sample
Product sample introduction solution.
Wherein step (4) GC-MS/MS analyzes, and its instrumental conditions is: using specification is 30m × 0.25mm × 0.25 μ
The HP-INNOWAX capillary chromatographic column 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
Degree is 50 DEG C, is increased to 240 DEG C with the speed of 5 DEG C/min, keeps 5min.Its mass spectral analysis condition is: ionization mode is EI source,
Positive ion mode；Ion source temperature: 230 DEG C；Quadrupole rod temperature: be 150 DEG C；Collision gas: nitrogen, flow velocity 1.5mL/min, carry
Gas (helium) flow velocity is 2.25mL/min；Multiple-reaction monitoring (MRM) pattern, detail parameters is listed in the table below.
The MRM parameter situation 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 in chromatogram, object and the ratio of interior target peak area are as vertical coordinate, carry out linear regression analysis,
Obtain standard working curve.Object and interior target chromatographic peak area ratio in the sample solution that will record under the same terms, substitute into
Standard working curve, tries to achieve the content of object in cigarette sample according to following equation:
In formula:
The content of 8 kinds of main Pyrazine fragrance matters in W cigarette mainstream flue gas, unit is microgram every (μ g/ props up)；
The peak area of the main Pyrazine fragrance matter of A 8 kinds；
Target peak area in As correspondence；
The intercept of b standard working curve；
Ms adds interior target quality, and unit is microgram (μ g)；
The slope of a standard working curve；
The quantity of M cigarette, unit is for propping up.
Beneficial effect: sample treatment and chromatograph mass spectrum analysis condition are optimized really by the detection method of the present invention
Recognize.Compared with prior art, the present invention has a following excellent results:
(1) trace Pyrazine during the inventive method creative use gas chromatography tandem mass spectrometry instrument measures cigarette mainstream flue gas
The content of fragrance matter, solves flue gas pyrazine compounds level low, and the analysis of object is done by flue gas complex matrices
Disturb the impact of the factor such as serious.
(2) the inventive method is easily soluble in water, the most weakly alkaline physicochemical property for pyrazine compounds, uses faintly acid
Aqueous solution object is extracted, then in conjunction with use kieselguhr SPE pillar, from containing object aqueous solution back extraction take out
Trace object, method is novel, strong innovation, compensate for using Simultaneous distillation-extraction to process intensity big, repeated in the past
Not good enough shortcoming.
(3) the inventive method utilizes inner mark method ration, can accurate constant volume, and can reduce by pre-treating method weight
The error that existing property and instrument precision problem are brought.
Accompanying drawing explanation
Fig. 1 is the flow chart of assay method of the present invention；
Fig. 2 is 8 kinds of main Pyrazine fragrance matters and the Ion-pair chromalography of internal standard heptadecane in standard working solution
Figure；
Fig. 3 is 8 kinds of main Pyrazine fragrance matters and the Ion-pair chromalography of internal standard heptadecane in cigarette mainstream flue gas
Figure.
Detailed description of the invention
In conjunction with specific embodiment, the invention will be further described below.
Embodiment 1
Following (the described detection of the detection method of the present embodiment Pyrazine main to trace in cigarette mainstream flue gas fragrance matter
The flow chart of method is as shown in Figure 1):
(1) preparation of inner mark solution
1. internal standard storing solution: accurately weigh 0.202g heptadecane, be accurate to 0.1mg, in the volumetric flask of 100mL,
Dissolve with ethanol and be settled to scale.2. inner mark solution: accurately pipette 0.1mL internal standard storing solution, in the volumetric flask of 100mL,
With ethanol dilution and be settled to scale.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-methylpyrazine, 0.1560g 2,5-dimethyl pyrazine,
0.1032g 2,6 dimethyl pyrazine, 0.0523g 2-methoxypyrazine, 0.1005g 2,3,5-trimethylpyrazine, 0.1079g
2-ethyl-3-methylpyrazine, 0.05577g 2，3，5，6-tetramethylpyrazine and 0.0332g 2-acetyl group pyrazine, be accurate to
0.1mg, in the volumetric flask of 100mL, dissolves with ethanol and is settled to scale.2. secondary standard storing solution: accurately pipette 1mL mono-
Grade standard storing solution, in the volumetric flask of 100mL, with ethanol dilution and be settled to scale.3. standard working solution: the most accurately
Pipette secondary standard storing solution 50 μ L, 100 μ L, 300 μ L, 600 μ L, 1mL and 3mL, to the volumetric flask of 10mL, more accurately
Add 1mL inner mark solution, with ethanol dilution and be settled to scale, obtain series standard working solution.Wherein 2-methylpyrazine is dense
Degree scope is 0.1006～6.033 μ g/mL, the concentration range of 2,5-dimethyl pyrazine is 0.078～4.68 μ g/mL, 2,6-bis-
The concentration range of methylpyrazine be the concentration range of 0.0516～3.096 μ g/mL, 2-methoxypyrazine be 0.0261～1.5675
The concentration range of μ g/mL, 2,3,5-trimethylpyrazine is the concentration of 0.0503～3.015 μ g/mL, 2-ethyl-3-methylpyrazines
Scope is 0.054～3.237 μ g/mL, the concentration range of 2，3，5，6-tetramethylpyrazine is 0.029～1.730 μ g/mL, and
2-acetyl group pyrazine concentration range is 0.0166～0.996g/mL.
(3) preparation of sample solution
1. cigarette smoking: Yi Yi city pin Medicated cigarette is object, aspirates 20 Medicated cigarette according to the requirement of GB/T19609 standard, its
Granule phase substance in middle cambridge filter trapping cigarette mainstream flue gas.2. granule phase substance extraction: cigarette mainstream smoke condensate will be trapped
Cambridge filter be transferred in 250mL bread bottle, carry out oscillation extraction with the aqueous hydrochloric acid solution that 40mL concentration is 10mmol/L, extraction
The time of taking is 40min, is extracted liquid.(3) extract back extraction: in advance kieselguhr SPE pillar (filler is 20g) is lived
Change, i.e. move into 50mL dichloromethane and carry out drip washing activation, drain as far as possible.After SPE pillar is ready to, pipette the above-mentioned extraction of 10mL
Liquid enters SPE pillar, concentrates bottle graft with one and receives leacheate；Repeatedly pillar is carried out drip washing with 60mL dichloromethane the most again, depend on
By the feature that dichloromethane density is bigger than water, drip voluntarily, collect all liquid stayed, be considered as leacheate.(4) leacheate
Concentrate: 50 DEG C, under condition of normal pressure, leacheate is concentrated to 1mL, obtains sample feeding solution.
(4) gas chromatography tandem mass spectrometry analysis
The standard working solution and the sample solution to be measured that take 6 variable concentrations respectively carry out gas chromatography tandem mass spectrometry analysis
(in described standard working solution, typical sample solution, the chromatogram of object and internal standard substance is as shown in Figure 2 to 3).
Its instrumental conditions is: use 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, split sampling, split ratio is 10:1；Injection port
Temperature is 240 DEG C；Transmission line temperature is 260 DEG C；Heating schedule be initial temperature be 50 DEG C, be increased to the speed of 5 DEG C/min
240 DEG C, keep 5min.Its mass spectral analysis condition is: ionization mode is EI source, positive ion mode；Ion source temperature: 230 DEG C；Four
Pole bar temperature: be 150 DEG C；Collision gas: nitrogen, flow velocity 1.5mL/min, carrier gas (helium) flow velocity is 2.25mL/min；The most anti-
Should monitor (MRM) pattern, detail parameters is listed in the table below.
The MRM parameter situation of object
(5) Specification Curve of Increasing and result calculate
First, in standard working solution, object and the ratio of interior target concentration are as abscissa, with object in chromatogram
It is vertical coordinate with the ratio of interior target peak area, carries out linear regression analysis, obtain standard working curve.Take the standard of least concentration
Working solution, does 9 Parallel testing analyses, calculates its standard deviation, and with the concentration that the standard deviations of 3 times are corresponding, conversion draws
The detection limit of method.The data such as the regression equation corresponding with standard working curve, correlation coefficient, detection limit see table.
The working curve of analysis method and detection limit
Object and interior target chromatographic peak area ratio in the sample solution that will record under the same terms, substitute into standard work song
Line, tries to achieve the content of object in cigarette sample according to following equation.
In formula:
The content of 8 kinds of main Pyrazine fragrance matters in W cigarette mainstream flue gas, unit is microgram every (μ g/ props up)；
The peak area of the main Pyrazine fragrance matter of A 8 kinds；
Target peak area in As correspondence；
The intercept of b standard working curve；
Ms adds interior target quality, and unit is microgram (μ g)；
The slope of a standard working curve；
The quantity of M cigarette, unit is for propping up.
In the present embodiment, in cigarette sample main flume, 8 kinds of main Pyrazine fragrance matter testing results see table:
| Material title | Content (μ g/ props up) |
| 2-methylpyrazine | 15.95 |
| 2,5-dimethyl pyrazine | 2.31 |
| 2,6 dimethyl pyrazine | 9.01 |
| 2-methoxypyrazine | 0.11 |
| 2,3,5-trimethylpyrazine | 2.33 |
| 2-ethyl-3-methylpyrazine | 0.70 |
| 2,3,5,6-tetramethylpyazine | 0.29 |
| 2-acetyl group pyrazine | 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 in embodiment 1, for analyzing object, has carried out withinday precision experiment respectively, in a few days accurate
Degree experiment is same sample parallel assay 6 times (same batch processed) under identical conditions, calculates 6 parallel determinations respectively
Relative standard deviation (RSD), measurement result see table.In table, result shows, this experimental technique in a few days repeatability RSD <
10%, for the quantitative analysis of trace materials, show that method has good precision.
| Material title | RSD (%) |
| 2-methylpyrazine | 5.20 |
| 2,5-dimethyl pyrazine | 5.17 |
| 2,6 dimethyl pyrazine | 8.78 |
| 2-methoxypyrazine | 8.13 |
| 2,3,5-trimethylpyrazine | 9.97 |
| 2-ethyl-3-methylpyrazine | 3.18 |
| 2,3,5,6-tetramethylpyazine | 5.31 |
| 2-acetyl group pyrazine | 9.76 |
With yoghurt example used by replica test for analyzing object, process according to above-mentioned sample-pretreating method, add
Entering the standard specimen of the suitable content of its burst size, carry out substrate mark-on test, result see table.As can be seen from the table, sample
Recovery of standard addition is between 84.50%～118.88%, and illustration method has preferable accuracy.
| Material title | Recovery of standard addition (%) |
| 2-methylpyrazine | 84.50 |
| 2,5-dimethyl pyrazine | 101.75 |
| 2,6 dimethyl pyrazine | 92.30 |
| 2-methoxypyrazine | 89.49 |
| 2,3,5-trimethylpyrazine | 114.81 |
| 2-ethyl-3-methylpyrazine | 101.65 |
| 2,3,5,6-tetramethylpyazine | 118.88 |
| 2-acetyl group pyrazine | 114.35 |
Standard solution used in the present embodiment only illustrates as a example by one of them concentration, other concentration value institute
Standard curve that the standard solution of preparation is obtained through gas chromatography tandem mass spectrometry instrument analysis and regression equation and above-described embodiment
Identical, do not enumerating at this.Illustrated embodiment is intended merely to be better understood from the inventive method, does not have any restriction
Effect, i.e. said method or be equal to the method for above-mentioned situation and be all contained in the protection domain of technical scheme.
Above in conjunction with the drawings and specific embodiments, embodiments of the present invention are described in detail, but the present invention is not
Be limited to above-mentioned embodiment, in the ken that art those of ordinary skill is possessed, it is also possible to without departing from
Make a variety of changes on the premise of present inventive concept.
Claims (6)
1. a method for main Pyrazine fragrance matter, described Pyrazine fragrance matter bag in quantitative analysis cigarette mainstream flue gas
Include 2-methylpyrazine, 2,5-dimethyl pyrazine, 2,6 dimethyl pyrazine, 2-methoxypyrazine, 2,3,5-trimethylpyrazine, 2-second
Base-3-methylpyrazine, 2，3，5，6-tetramethylpyrazine and 2-acetyl group pyrazine, it is characterised in that described method includes following step
Rapid:
(1) preparation of inner mark solution: with heptadecane as internal standard substance, using ethanol is solvent, prepares inner mark solution；
(2) preparation of standard working solution: with 2-methylpyrazine, 2,5-dimethyl pyrazine, 2,6 dimethyl pyrazine, 2-methoxyl group
Pyrazine, 2,3,5-trimethylpyrazine, 2-ethyl-3-methylpyrazine, 2,3,5,6-tetramethylpyazine and the mark of 2-acetyl group pyrazine
Quasi-product are object, and use ethanol is solvent, is prepared as Standard Stock solutions through stepwise dilution, is then respectively adding a certain amount of
Inner mark solution, is prepared as standard working solution；
(3) preparation of sample solution: gather the object in cigarette smoke, accurately adds a certain amount of inner mark solution and
Determining the extraction solution of volume, mechanical shaking extraction, extract is crossed kieselguhr and is carried out back extraction, then concentrates leacheate, obtain sample
Product solution；
(4) gas chromatography tandem mass spectrometry instrument is analyzed: with gas chromatography tandem mass spectrometry instrument to standard working solution and sample solution
Carry out detection to analyze；
(5) drafting of standard working curve and the calculating of sample result.
The method of main Pyrazine fragrance matter in quantitative analysis cigarette mainstream flue gas the most according to claim 1, it is special
Levying and be, the preparation of step (1) inner mark solution includes:
(1a) internal standard storing solution: accurately weigh 0.2g heptadecane, be accurate to 0.1mg, in the volumetric flask of 100mL, uses second
Alcohol dissolves and is settled to scale；
(1b) inner mark solution: accurately pipette 0.1mL internal standard storing solution, in the volumetric flask of 100mL, with ethanol dilution and be settled to
Scale.
The method of main Pyrazine fragrance matter in quantitative analysis cigarette mainstream flue gas the most according to claim 1, it is special
Levying and be, the preparation of step (2) standard working solution includes:
(2a) primary standard storing solution: accurately weigh 0.2g 2-methylpyrazine, 0.15g 2,5-dimethyl pyrazine, 0.1g 2,6-
Dimethyl pyrazine, 0.05g 2-methoxypyrazine, 0.1g 2,3,5-trimethylpyrazine, 0.1g 2-ethyl-3-methylpyrazine,
0.05g 2，3，5，6-tetramethylpyrazine and 0.05g 2-acetyl group pyrazine, be accurate to 0.1mg, in the volumetric flask of 100mL, uses
Ethanol dissolves and is settled to scale；
(2b) secondary standard storing solution: accurately pipette 1mL primary standard storing solution, in the volumetric flask of 100mL, use ethanol dilution
And it is settled to scale；
(2c) standard working solution: the most accurately pipette secondary standard storing solution 50 μ L, 100 μ L, 300 μ L, 600 μ L, 1mL and
3mL, to the volumetric flask of 10mL, then adds respectively accurately 1mL inner mark solution, with ethanol dilution and be settled to scale, obtains serial
Standard working solution.
The method of main Pyrazine fragrance matter in quantitative analysis cigarette mainstream flue gas the most according to claim 1, it is special
Levying and be, the preparation of step (3) sample solution includes:
(3a) cigarette smoking: aspirate 20 Medicated cigarette according to the requirement of GB/T19609 standard, wherein trap Medicated 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 bottle, uses
40mL concentration is that the aqueous hydrochloric acid solution of 10mmol/L carries out oscillation extraction, and extraction time is 40min, is extracted liquid；
(3c) extract back extraction: activate the kieselguhr SPE pillar of filler 20g in advance, i.e. moves into 50mL dichloromethane
Carry out drip washing activation, drain as far as possible, after SPE pillar is ready to, pipettes the above-mentioned extract of 10mL and enter SPE pillar, dense with one
Contracting bottle graft receives leacheate；Repeatedly pillar is carried out with 60mL dichloromethane drip washing the most again, relies on dichloromethane density bigger than water
Feature, drip voluntarily, collect all liquid stayed, be considered as leacheate；
(3d) leacheate concentrates: 50 DEG C, under condition of normal pressure, leacheate is concentrated to 1mL, obtains sample feeding solution.
The method of main Pyrazine fragrance matter in quantitative analysis cigarette mainstream flue gas the most according to claim 1, it is special
Levying and be, the instrumental conditions that step (4) GC-MS/MS analyzes is: the HP-using specification to be 30m × 0.25mm × 0.25 μm
INNOWAX capillary chromatographic column；Carrier gas is helium, and constant current speed is 1.0mL/min；Input mode: sample size is 1 μ L, shunting
Sample introduction, split ratio is 10:1；Injector temperature is 240 DEG C；Transmission line temperature is 260 DEG C；Heating schedule be initial temperature be 50
DEG C, it is increased to 240 DEG C with the speed of 5 DEG C/min, keeps 5min；Its mass spectral analysis condition is: ionization mode is EI source, cation
Pattern；Ion source temperature: 230 DEG C；Quadrupole rod temperature: be 150 DEG C；Collision gas: nitrogen, flow velocity 1.5mL/min, carrier gas helium
Flow velocity is 2.25mL/min；Multiple-reaction monitoring MRM pattern, detail parameters is listed in the table below:
The MRM parameter situation of object
The method of main Pyrazine fragrance matter in quantitative analysis cigarette mainstream flue gas the most according to claim 1, it is special
Levying 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
Ratio is abscissa, and in chromatogram, object and the ratio of interior target peak area are as vertical coordinate, carry out linear regression analysis, are marked
Quasi-working curve；Object and interior target chromatographic peak area ratio in the sample solution that will record under the same terms, substitute into standard work
Make curve, try to achieve the content of object in cigarette sample according to following equation:
In formula:
The content of 8 kinds of main Pyrazine fragrance matters in W cigarette mainstream flue gas, unit is that μ g/ props up；
The peak area of the main Pyrazine fragrance matter of A 8 kinds；
Target peak area in As correspondence；
The intercept of b standard working curve；
Ms adds interior target quality, and unit is μ g；
The slope of a standard working curve；
The quantity of M cigarette, unit is for propping up.
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| CN110749679A (en) * | 2019-11-08 | 2020-02-04 | 华熙生物科技股份有限公司 | Detection method of trimethyl pyrazine residues |
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| CN115047095B (en) * | 2022-04-27 | 2023-12-22 | 国家烟草质量监督检验中心 | Method for simultaneously detecting 8 heterocyclic compounds |
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