CN109342629A - Method is determined based on the cigarette style of cigarette cracking ingredient - Google Patents
Method is determined based on the cigarette style of cigarette cracking ingredient Download PDFInfo
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Abstract
The invention discloses a kind of cigarette styles based on cigarette cracking ingredient to determine method, it include: that (1) cracks the pipe tobacco of cigarette sample, and using gas chromatograph-mass spectrometer (GC-MS) to cracking composition detection analysis, gas chromatogram and mass spectrogram are obtained, and pipe tobacco cracking ingredient is carried out qualitative；(2) based on the retention time of gas chromatogram and mass spectrometry as a result, constructing and determining the percentage composition for each sharing peak in finger-print；(3) cigarette style characteristic of cigarette sample is determined using principal component analytical method；(4) sample set is constructed according to the shared cracking ingredient and its percentage composition and cigarette style characteristic of cigarette sample, and discriminant analysis is carried out to sample set, determine that cigarette divides decision model；(5) the cracking ingredient and its percentage composition of the determination of cigarette to be measured cigarette to be measured are calculated using the cigarette segmentation decision model constructed in step (4), determines cigarette style characteristic.The cigarette style determines that method accuracy is high.
Description
Technical field
The invention belongs to Field of Tobacco, and in particular to it is a kind of based on cigarette cracking ingredient cigarette style determine method.
Background technique
Finger-print refers to certain complex materials (such as Chinese medicine), certain organism, certain histiocytic DNA or albumen
After matter is appropriately processed, the chromatogram or spectrogram that can indicate its chemical feature that are obtained using certain analysis means.Refer to
Line graphical spectrum technology is mainly used for characterizing the type and content of chemical component contained in sample, is a kind of quantifying for synthesis
Chromatography identification of means.After obtaining finger-print, using mathematical statistics sides such as principal component analysis (PCA), clusterings (HCA)
Method analyzes finger-print.
Cracking technique can uniformly crack whole samples in moment, and heating time is short, and secondary response is few, is able to reflect original
The composition and feature of beginning sample have many advantages, such as that directly progress, sample volume are few, analysis speed is fast, reproducible.
The difference of raw tobacco material, auxiliary material, tobacco leaf formulation and essence spice for cigarette etc. causes each cigarette brand in chemistry
It is had a certain difference on composition；And due to the difference of brand positioning and chemical composition, each cigarette brand is in long-term development
Unique style and features are formd in journey again.Cigarette style characteristic is the important characterization of kinds of cigarettes brand, is to carry out tobacco leaf product
Matter characteristic divides and the important evidence of production target control.Currently, industry relies primarily on profession to positioning, the evaluation of cigarette style
Evaluation personnel carries out sensory evaluating smoking, but the subjective factor of evaluation personnel may result in evaluation result reproducibility and reliability side
The deficiency in face.
Application publication number is that the patent application of CN106770971A discloses a kind of method of cigarette style characteristic evaluation, first
First construct cigarette style characteristic assessment indicator system；Then according to " GB5606.4-2005 cigarette sense organ technical requirements " to cigarette
It smokes panel test, is evaluated according to each index of the suction impression to characterization cigarette style characteristic；Finally commented according to each index
Valence evaluates cigarette style characteristic as a result, using edge analysis method building cigarette style characteristic profile diagram.This method is still
It is that the subjective consciousness of Utilization assessment personnel goes each index of evaluating cigarette style and features to evaluate, there can be evaluation result again
Deficiency in terms of existing property and reliability.
Application publication number discloses a kind of using index characterization cigarette style characteristic for the patent application of CN108169420A
The method of difference degree, first by being screened to cigarette rags chemical detection index, determine 20 it is representative
Index be characterized chemical index；Then the cigarette sample of different-style feature to be characterized is chosen, and to the 20 of selected sample
Item characteristic chemical index is detected；Then r mode factor analysis is done to the Testing index data of all samples, and calculates each sample
Each factor score of product, factor comprehensive score and each style and features cigarette factor comprehensive score；Finally rolled up with two kinds of style and features
The absolute value of the difference DI of cigarette factor comprehensive score carrys out the difference degree of both cigarette style characteristics of quantization signifying.This method is base
In the difference of pipe tobacco chemical analysis metrics evaluation cigarette style characteristic, there is no the specific cigarette styles for judging product.
Summary of the invention
Based on above-mentioned, the object of the present invention is to provide a kind of cigarette styles based on cigarette cracking ingredient to determine method, has
Body, the correlation cracked between the content and ingredient of ingredient according to cigarette confirms cigarette style characteristic, and this method can be fast
Speed accurately determines cigarette style.
For achieving the above object, the present invention the following technical schemes are provided:
It is a kind of based on cigarette cracking ingredient cigarette style determine method, comprising the following steps:
(1) pipe tobacco of several cigarette samples of different brands is taken out respectively, is placed at 34~45 DEG C dry 3.5~4.5h
Afterwards, it crushes, crosses the offal that 40 meshes obtain each cigarette sample, then, the cigarette offal is cracked using cracking instrument, and use
Gas chromatograph-mass spectrometer (GC-MS) obtains gas chromatogram and mass spectrogram, and use mass spectrum standard spectrum to cracking composition detection analysis
Library carries out pipe tobacco cracking ingredient qualitative；
(2) retention time based on gas chromatogram and mass spectrometry as a result, according to predefined selection standard choose to
Shared peak of the chromatographic peak of few 20 ingredients as finger-print, and finger-print is constructed, and each to share in finger-print
Peak corresponds to the percentage composition for cracking ingredient relative to the percentage of all shared peak areas as each shared peak；
(3) cigarette style characteristic of cigarette sample is determined using principal component analytical method, specifically: it is directed to each cigarette sample
Product carry out principal component analysis based on the shared cracking ingredient and its percentage composition obtained in step (2), obtain 2 main components,
Then, according to the 2 of all cigarette samples main component coordinates, principal component analysis scatter plot is drawn, it is believed that principal component analysis dissipates
Cigarette sample in point diagram in the same area belongs to same cigarette style characteristic；
(4) made with the cigarette style characteristic of the shared cracking ingredient and its percentage composition of each cigarette sample, cigarette sample
For a sample, sample set is constructed, then, discriminant analysis is carried out to the data in sample set, determines optimal discriminant function, with
This optimal discriminant function divides decision model as cigarette；
(5) the cracking ingredient and its percentage composition of cigarette to be measured are obtained using step (1) and step (2), then basis obtains
Cigarette to be measured cracking ingredient and its percentage composition, using the cigarette segmentation decision model constructed in step (4) determine to
Survey the cigarette style characteristic of cigarette.
In the present invention, based on cigarette cracking ingredient and percentage composition, principal component analysis is carried out to cigarette sample and is rolled up
The cigarette style characteristic of cigarette sample constructs modeling sample with this, then discriminant analysis is recycled to handle modeling sample,
The discriminant function that can characterize cracking ingredient and cigarette style characteristic correlation is obtained, finally using the discriminant function to be detected
Cigarette carries out the judgement of cigarette style characteristic, and in this method, cigarette style characteristic is to crack ingredient based on cigarette, avoids and comments
Valence personnel aspirate evaluation bring subjectivity, and this method speed is fast, accuracy is high.
Preferably, in step (1), pipe tobacco is placed at (40 ± 1) DEG C after dry 4h, is crushed, cross 40 meshes obtain it is each
The offal of cigarette sample.
Specifically, in step (3), the cigarette style characteristic of cigarette sample is determined using clustering method, specifically:
Clustering is carried out to the shared cracking ingredient and its percentage composition of all cigarette samples, with Euclidean distance
For module, obtain the cluster dendrogram of cigarette sample, according between class distance determine cigarette sample belonging to cigarette style it is special
Sign.
Clustering method as principal component analytical method, can according to the shared cracking ingredient of cigarette sample and its
Percentage composition realizes the determination to the cigarette style characteristic of cigarette sample.
Wherein, the cracking condition of the cracking instrument are as follows:
Crack atmosphere: He gas；
Cracking temperature: 90~120 DEG C of holding 5s are warming up to 500~700 DEG C with 20 DEG C/ms and keep 10~30s.
GC conditions when using gas chromatograph-mass spectrometer (GC-MS) to cracking composition detection analysis are as follows:
Chromatographic column: DB-5MS chromatographic column (30m × 0.25mm × 0.25 μm)；
Injector temperature: 280~300 DEG C；
Split ratio: 50:1；
Carrier gas: He；
Flow: 1.0~1.2mL/min；
Temperature program: 50 DEG C of initial temperature, and with the speed of 5 DEG C/min be warming up to 280~300 DEG C and keep 10~
20min。
Mass Spectrometry Conditions when using gas chromatograph-mass spectrometer (GC-MS) to cracking composition detection analysis are as follows:
Transmission line temperature: 280~300 DEG C；
Ion source temperature: 230 DEG C；
Ionization mode: EI；
Ionizing energy: 70eV；
Level four bars temperature: 150 DEG C；
Mass scan range: 35~650amu.
The control of above-mentioned cracking condition, GC conditions and Mass Spectrometry Conditions can obtain accurate cracking ingredient
And corresponding percentage composition, stable accurate data basis is provided, determines that the accuracy of cigarette style characteristic mentions to improve
It has supplied to ensure.
Preferably, the cracking condition of the cracking instrument are as follows: cracking atmosphere: He gas；Cracking temperature: 100 DEG C of holding 5s, with 20
DEG C/ms is warming up to 600 DEG C and keeps 10s；Cracking furnace temperature: 280 DEG C；
GC conditions when using gas chromatograph-mass spectrometer (GC-MS) to cracking composition detection analysis are as follows: chromatographic column:
DB-5MS chromatographic column (30m × 0.25mm × 0.25 μm)；Injector temperature: 280 DEG C；Split ratio: 50:1；Carrier gas: He；Flow:
1.0mL/min；Temperature program: 50 DEG C of initial temperature, and be warming up to 280 DEG C with the speed of 5 DEG C/min and keep 10min；
Mass Spectrometry Conditions when using gas chromatograph-mass spectrometer (GC-MS) to cracking composition detection analysis are as follows: transmission line temperature:
280℃；Ion source temperature: 230 DEG C；Ionization mode: EI；Ionizing energy: 70eV；Level four bars temperature: 150 DEG C；Mass scanning model
It encloses: 35~650amu.
Wherein, pipe tobacco cracking ingredient is carried out using the library Nist11 qualitative.
Compared with prior art, the device have the advantages that are as follows:
(1) solid sample direct injected is used when cracking, and is handled without solvent, it is environmentally friendly, easy；Using pyrolysis gas chromatograph
Mass spectrography carries out qualitative and quantitative detection to cigarette sample, can effectively save the operating time, simplify experimental procedure, in conjunction with fingerprint image
Spectral model identification can quickly identify different-style cigarette brand, and the model sample successively established is accurate, determine mould for cigarette style
The foundation of type provides Data safeguard；
(2) cigarette style decision model is established based on determining sample and provides the objectivity of cigarette style decision model,
And it can guarantee accuracy.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to do simply to introduce, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art, can be with root under the premise of not making the creative labor
Other accompanying drawings are obtained according to these attached drawings.
Fig. 1 is modeling cigarette sample total ion chromatogram at a temperature of different Py；Wherein, a~e be respectively 200 DEG C,
Total ion chromatogram at 400 DEG C, 600 DEG C, 800 DEG C, 1000 DEG C；
Fig. 2 is modeling cigarette sample pyrolysis product and nicotine content figure at a temperature of different Py；
Fig. 3 is the total ion current figure for modeling the cracking ingredient of cigarette sample；
Fig. 4 is the Hierarchical Clustering dendrogram for modeling cigarette sample；
Fig. 5 is the perspective view for modeling the principal component analysis result of cigarette sample.
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention more comprehensible, with reference to the accompanying drawings and embodiments to this
Invention is described in further detail.It should be appreciated that the specific embodiments described herein are only used to explain the present invention,
And the scope of protection of the present invention is not limited.
The material and instrument of embodiment application:
Model cigarette sample: A1, A2, A3, A4, A5, A6 and A7 are company A difference trade mark cigarette；B1, B2 and B3 are B public
Take charge of different trade mark cigarette；C1, C2 and C3 are C company difference trade mark cigarette；D1 and D2 is D company difference trade mark cigarette.
Cigarette sample to be measured: X1 and X2 is company A trade mark cigarette；X3 and X4 is the cigarette of the different month productions of the B1 trade mark.
5250 type thermal cracking instrument of Pyroprobe (CDS company of the U.S.)；
7890/5977A type Gc/ms Analyser (Agilent company of the U.S.)；
XP205 type electronic analytical balance (sensibility reciprocal 0.1mg, Mettler Toledo company of Switzerland)；
1093 cyclone type sample mill of Cyclotec ((Beijing) scientific & trading Co., Ltd. of Fox China).
Cigarette style provided in this embodiment based on cigarette cracking ingredient determines that method includes cigarette segmentation and classification model
Determination and using determining cigarette genre classification model to judgement two parts of the cigarette style characteristic of cigarette sample to be measured, tool
Body process are as follows:
First part: cigarette genre classification model is determined:
Firstly, respectively taking out the pipe tobacco that 15 kinds model cigarette samples, at (40 ± 1) DEG C after dry 4h, crushes, cross 40
Mesh obtains using offal sample for cracking experiment；
Then, 15 offal sample (1.0 ± 0.1) mg are weighed respectively be placed in and be laid in cracking silica tube, use silica wool
The both ends of pipe are blocked, quartz ampoule is then packed into 5250 type thermal cracking instrument of Pyroprobe and carries out thermal cracking, cracking condition are as follows:
Crack atmosphere: He gas；Cracking temperature: 100 DEG C of holding 5s are warming up to 600 DEG C (keeping 10s) with 20 DEG C/ms.
In order to guarantee the reproducibility of testing result, sample should crack in the shortest possible time, to avoid two as far as possible
The generation of secondary response.A possibility that sample size is bigger, and heat transfer speed is slower, and secondary response occurs is bigger, therefore sample size should be use up
It may be small.According to the needs of the form of cigarette shreds offal and actual experiment, when cracking, the sample volume of cigarette sample be (1.0 ±
0.1)mg。
Cracking of the cigarette shreds in He atmosphere is shown in Fig. 1 under different temperatures, while measuring nicotine and pyrolysis product
The relationship of absolute peak area and temperature is shown in Fig. 2.It can be found that: 1. cracking temperature has significant shadow to the variation of pyrolysis product
It rings, at 600 DEG C or less, as the temperature rises, the cracking of pipe tobacco occupies leading role, and pyrolysis product is continuously increased.Temperature
When reaching 600 DEG C or more, cracking terminates substantially, and product no longer increased significantly.2. the burst size of nicotine reaches at 400 DEG C
Maximum, then as the raising of cracking temperature decreases, but the range of decrease is little.Comprehensively consider the burst size of sample nicotine and splits
The number of product is solved, this experiment cracking temperature selects 600 DEG C.
Pyrolysis product is passed directly into GC/MS injection port and is analyzed, and obtains total ion chromatogram.Analysis condition are as follows:
Chromatographic column: DB-5MS chromatographic column (30m × 0.25mm × 0.25 μm)；Injector temperature: 280 DEG C；Split ratio: 50:
1；Carrier gas: He；Flow: 1.0mL/min；Temperature program: 50 DEG C of initial temperature, and 280 DEG C are warming up to simultaneously with the speed of 5 DEG C/min
Keep 10min；Transmission line temperature: 280 DEG C；Ion source temperature: 230 DEG C；Ionization mode: EI；Ionizing energy: 70eV；Level four bars
Temperature: 150 DEG C；Mass scan range: 35~650amu.Retrieve using NIST11 spectrum library qualitative.
Fig. 3 is the total ion chromatogram of 15 modeling cigarette samples.As seen from Figure 3, the pyrogram of different samples
Similarity is higher, still can not intuitively distinguish different brands sample.
Through mass spectrometric data library searching and artificial spectrum elucidation, cigarette shreds pyrolysis product be mainly nicotine, alkene, alcohol, ketone,
Aldehyde, benzene substituent and heterocyclic compound.There are hundreds of chromatographic peaks in the total ion current figure of each cigarette sample pyrolysis product, but
It is wherein to have part chromatography overlap of peaks serious, it, will certainly impact analysis result if all carrying out data analysis using these peaks.
Therefore shared peak of the chromatographic peak as finger-print of several ingredients is chosen from total ion chromatogram.It is predetermined
The selection standard of justice: the retention time and relative peak area of gas chromatogram are stablized, be separated clearly, mass spectrum can be accurate qualitative,
And chromatographic peak has detectable content in all samples.
29 shared peaks have been determined by the analysis to 15 cigarette sample spectrograms, it is shared relative to 29 with each shared peak
Percentage composition of the percentage of peak area as each shared corresponding cracking ingredient in peak, qualitative and quantitative result are shown in Table 1 and table
2.The reproducibility of PY-GC/MS spectrogram is investigated, the relative standard deviation of 29 shared Component peak area relative amounts
RSD (n=5) is respectively less than 5%, shows that this method has good reproducibility.
The similitude for modeling cigarette sample to above-mentioned 15 based on shared cracking ingredient judges, specifically, with A1 sample
Product as a control group, calculate the similarity of each sample and its using Cosin method, and as a result respectively 0.9994,0.9989,
0.9995,0.9986,0.9999,0.9992,0.9874,0.9724,0.9810,0.9979,0.9977,0.9981,0.9911,
0.9935.Similarity result shows that 15 cigarette shreds pyrolysis product similarities are higher, it is difficult to directly distinguish.
1 10 cigarette sample pipe tobaccos of table share identification and the percentage contents at peak
After obtaining shared cracking ingredient and its percentage composition, cigarette sample is modeled to 15 and carries out cigarette style characteristic
It determines, specifically, shared is cracked into a point percentage contents application to 29 of 15 in Tables 1 and 2 modeling cigarette samples
16 software of Minitab carries out clustering.Using Euclidean distance as module, Fig. 4 is as a result seen.
Fig. 4 is the cluster dendrogram for modeling cigarette sample, and abscissa is sample number, distance of the ordinate between class, between class
Distance it is smaller, show that map is more similar.As shown in Figure 4, when distance about 3,15 cigarette samples can be divided into four classes, and every
One kind comes under the same brand.
29 cigarette sample pipe tobaccos of table share identification and the percentage contents at peak
29 shared cracking ingredients for also modeling cigarette sample to 15 carry out principal component analysis, specifically, with table 1 and table
29 common constituent percentage contents of 15 modeling cigarette samples in 2 establish matrix, using 16 software pair of Minitab
Sample carries out principal component analysis, acquires characteristic value corresponding to 29 components respectively, the results are shown in Table 3.It is generally acknowledged that characteristic value is big
It can be used as principal component in 1 or several components of accumulation contribution degree greater than 85% or more, the first two component characterization value is big in table 3
In 1, and its corresponding accumulation contribution degree reaches 93.9%, shows that the two components crack ingredient essentially comprising 29 kinds
All information.Therefore selecting the two components as principal component, perspective view is as shown in Figure 5.As shown in Figure 5, with the knot of clustering
Seemingly, by the first component and second component, the cigarette sample of different brands can be separated preferably fruit, same brand difference board
Number cigarette sample can preferably assemble, this shows in the cigarette style of different brands there are larger difference, and same brand
Cigarette style it is then more similar.In addition, by the discovery of the loading matrix of the first component and second component, 1,12,16,17,20
There is high load on the first component with No. 28 peaks, shows that the first component mainly reflects the information of above-mentioned several cracking ingredients.Together
Manage visible second component reflection is 1,14,15,17,20,24,28 and No. 29 peak.
Table 3 forms dtex value indicative and contribution rate
The cigarette style of the shared cracking ingredient and its percentage composition, cigarette sample that model cigarette sample with above-mentioned 15 is special
Sign is used as a sample, constructs sample set, carries out discriminant analysis to the data in sample set, determines optimal linear function conduct
Cigarette genre classification model.
Second part: the judgement of the cigarette style characteristic of cigarette sample to be measured:
Select cigarette genre classification model (namely linear function) and cross validation method to four known class to
The cracking analysis result (being shown in Table X1, X2, X3 and X4 data in 2) for surveying cigarette sample is judged that the results are shown in Table 4.By table 4
The probability of miscarriage of justice for knowing 15 training samples is 0, while the established cigarette genre classification model of application is to sample X1, X2, X3
Differentiated with X4, accuracy rate reaches 100%.Wherein, X1 and X2 determines that result is the company A difference trade mark, with exact brand name one
It causes, shows that the model can be applied to identify the cigarette brand of different-style, also can be used as the supplementary means that true and false cigarette identifies.
X3, X4 and the B1 trade mark are the B1 sample in different months in the same season, determine that result is consistent with the practical trade mark, show model warp
It, can be with assistance application in the cigarette product quality stability monitoring of the identical trade mark different production times after crossing certain expansion.When
So, carrying out discriminant analysis to cigarette sample using this method requires modeling sample to have fully representativeness, simultaneously because cigarette
Manufacturing enterprise can be adjusted formula, and periodically carrying out maintenance to model could correctly predicted result.
4 cross validation of table and discriminant analysis result
Method pre-treatment provided in this embodiment uses solid sample direct injected, handles without solvent, environmental protection, simplicity；
It develops pyrolysis gas chromatography mass spectrometry method and qualitative and quantitative detection is carried out to cigarette sample, can effectively save the operating time, simplify in fact
Step is tested, can quickly identify different-style cigarette brand in conjunction with finger-print pattern-recognition；The detection technique can be generalized to very
False identification of cigarettes and cigarette product stability monitoring field can dissect the production that homogenizes with cigarette for the style and features of cigarette
Differentiate and auxiliary reference means are provided.
Technical solution of the present invention and beneficial effect is described in detail in above-described specific embodiment, Ying Li
Solution is not intended to restrict the invention the foregoing is merely presently most preferred embodiment of the invention, all in principle model of the invention
Interior done any modification, supplementary, and equivalent replacement etc. are enclosed, should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of cigarette style based on cigarette cracking ingredient determines method, comprising the following steps:
(1) pipe tobacco of several cigarette samples of different brands is taken out respectively, after being placed at 34~45 DEG C dry 3.5~4.5h,
It crushes, crosses the offal that 40 meshes obtain each cigarette sample, then, the cigarette offal is cracked using cracking instrument, and use gas
Phase chromatograph-mas spectrometer obtains gas chromatogram and mass spectrogram, and use mass spectrum standard spectrum library to cracking composition detection analysis
Pipe tobacco cracking ingredient is carried out qualitative；
(2) retention time based on gas chromatogram and mass spectrometry are as a result, choose at least 20 according to predefined selection standard
Shared peak of the chromatographic peak of a ingredient as finger-print, and finger-print is constructed, and each to share peak phase in finger-print
The percentage composition for cracking ingredient is corresponded to as each shared peak for the percentage of all shared peak areas；
(3) cigarette style characteristic of cigarette sample is determined using principal component analytical method, specifically: it is directed to each cigarette sample,
Principal component analysis is carried out based on the shared cracking ingredient and its percentage composition obtained in step (2), obtains 2 main components, so
Afterwards, according to the 2 of all cigarette samples main component coordinates, principal component analysis scatter plot is drawn, it is believed that principal component analysis scatterplot
Cigarette sample in figure in the same area belongs to same cigarette style characteristic；
(4) using the shared cracking ingredient and its percentage composition of each cigarette sample, cigarette sample cigarette style characteristic as one
A sample constructs sample set, then, carries out discriminant analysis to the data in sample set, determines optimal discriminant function, most with this
Excellent discriminant function divides decision model as cigarette；
(5) the cracking ingredient and its percentage composition that cigarette to be measured is obtained using step (1) and step (2), then according to acquisition
The cracking ingredient and its percentage composition of cigarette to be measured determine volume to be measured using the cigarette segmentation decision model constructed in step (4)
The cigarette style characteristic of cigarette.
2. determining method based on the cigarette style of cigarette cracking ingredient as described in claim 1, which is characterized in that step (3)
In, the cigarette style characteristic of cigarette sample is determined using clustering method, specifically:
Clustering is carried out to the shared cracking ingredient and its percentage composition of all cigarette samples, is degree with Euclidean distance
Amount standard obtains the cluster dendrogram of cigarette sample, according between class distance determine cigarette sample belonging to cigarette style characteristic.
3. determining method based on the cigarette style of cigarette cracking ingredient as claimed in claim 1 or 2, which is characterized in that described
Crack the cracking condition of instrument are as follows:
Crack atmosphere: He gas；
Cracking temperature: 90~120 DEG C of holding 5s are warming up to 500~700 DEG C with 20 DEG C/ms and keep 10~30s.
4. determining method based on the cigarette style of cigarette cracking ingredient as claimed in claim 1 or 2, which is characterized in that use
GC conditions when gas chromatograph-mass spectrometer (GC-MS) is to cracking composition detection analysis are as follows:
Chromatographic column: DB-5MS chromatographic column (30m × 0.25mm × 0.25 μm)；
Injector temperature: 280~300 DEG C；
Split ratio: 50:1；
Carrier gas: He；
Flow: 1.0~1.2mL/min；
Temperature program: 50 DEG C of initial temperature, and be warming up to 280~300 DEG C with the speed of 5 DEG C/min and keep 10~20min.
5. determining method based on the cigarette style of cigarette cracking ingredient as claimed in claim 1 or 2, which is characterized in that use
Mass Spectrometry Conditions when gas chromatograph-mass spectrometer (GC-MS) is to cracking composition detection analysis are as follows:
Transmission line temperature: 280~300 DEG C；
Ion source temperature: 230 DEG C；
Ionization mode: EI；
Ionizing energy: 70eV；
Level four bars temperature: 150 DEG C；
Mass scan range: 35~650amu.
6. determining method based on the cigarette style of cigarette cracking ingredient as claimed in claim 1 or 2, which is characterized in that described
Crack the cracking condition of instrument are as follows:
Crack atmosphere: He gas；
Cracking temperature: 100 DEG C of holding 5s are warming up to 600 DEG C with 20 DEG C/ms and keep 10s；
GC conditions when using gas chromatograph-mass spectrometer (GC-MS) to cracking composition detection analysis are as follows:
Chromatographic column: DB-5MS chromatographic column (30m × 0.25mm × 0.25 μm)；
Injector temperature: 280 DEG C；
Split ratio: 50:1；
Carrier gas: He；
Flow: 1.0mL/min；
Temperature program: 50 DEG C of initial temperature, and be warming up to 280 DEG C with the speed of 5 DEG C/min and keep 10min；
Mass Spectrometry Conditions when using gas chromatograph-mass spectrometer (GC-MS) to cracking composition detection analysis are as follows:
Transmission line temperature: 280 DEG C；
Ion source temperature: 230 DEG C；
Ionization mode: EI；
Ionizing energy: 70eV；
Level four bars temperature: 150 DEG C；
Mass scan range: 35~650amu.
7. determining method based on the cigarette style of cigarette cracking ingredient as claimed in claim 1 or 2, which is characterized in that use
The library Nist11 carries out pipe tobacco cracking ingredient qualitative.
8. determining method based on the cigarette style of cigarette cracking ingredient as claimed in claim 1 or 2, which is characterized in that step
(1) in, pipe tobacco is placed at (40 ± 1) DEG C after dry 4h, is crushed, the offal that 40 meshes obtain each cigarette sample is crossed.
9. determining method based on the cigarette style of cigarette cracking ingredient as claimed in claim 1 or 2, which is characterized in that cracking
When, the sample volume of cigarette sample is (1.0 ± 0.1) mg.
10. determining method based on the cigarette style of cigarette cracking ingredient as claimed in claim 1 or 2, which is characterized in that predetermined
The selection standard of justice: the retention time and relative peak area of gas chromatogram are stablized, be separated clearly, mass spectrum can be accurate qualitative,
And chromatographic peak has detectable content in all samples.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN112345654A (en) * | 2019-08-06 | 2021-02-09 | 红塔烟草(集团)有限责任公司 | Method for identifying oil stain smoke pollution source based on chromatographic fingerprint spectrum |
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