Nothing Special   »   [go: up one dir, main page]

CN109655532A - A kind of method of pair of cigarette taxonomic history - Google Patents

A kind of method of pair of cigarette taxonomic history Download PDF

Info

Publication number
CN109655532A
CN109655532A CN201710948016.9A CN201710948016A CN109655532A CN 109655532 A CN109655532 A CN 109655532A CN 201710948016 A CN201710948016 A CN 201710948016A CN 109655532 A CN109655532 A CN 109655532A
Authority
CN
China
Prior art keywords
cigarette
sample
dimensional spectrum
cigarette sample
spectrum
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201710948016.9A
Other languages
Chinese (zh)
Inventor
邹西梅
刘剑
谢顺萍
金晶
杨科
赵新海
韩宇
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
China Tobacco Guizhou Industrial Co Ltd
Original Assignee
China Tobacco Guizhou Industrial Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by China Tobacco Guizhou Industrial Co Ltd filed Critical China Tobacco Guizhou Industrial Co Ltd
Priority to CN201710948016.9A priority Critical patent/CN109655532A/en
Publication of CN109655532A publication Critical patent/CN109655532A/en
Pending legal-status Critical Current

Links

Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography

Landscapes

  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)

Abstract

The invention discloses the methods of a kind of pair of cigarette taxonomic history, carry out HS GC-Ion transfer spectrum analysis to cigarette sample, obtain its three-dimensional spectrum;The selected characteristic analyzed area in collected cigarette sample three-dimensional spectrum;The signature analysis region of the three-dimensional spectrum of collected cigarette sample is analyzed, taxonomic history is carried out to cigarette.Head space-gas phase-ion mobility spectrometry joint technology is used to cigarette Fast Classification to identify, method resolution ratio and high sensitivity, analysis time are short, and lossless, no sample pre-treatment, method is environmental-friendly, and it is few to test consumptive material used, testing cost is low, visual result, is suitble to cigarette sample batch taxonomic history.

Description

A kind of method of pair of cigarette taxonomic history
Technical field
The present invention relates to quick analysis detection fields, more particularly to the method for a kind of pair of cigarette taxonomic history.
Background technique
Ion mobility spectrometry (IMS) is a kind of trace chemical analysis and detection technology that fast development is got up in recent years, it is Based on the difference of gaseous ion different in gas phase migration velocity in the electric field come characterized to chemical ion substance one Analytical technology.Under normal pressure, test substance passes through charge on ionization source band, substance drift under the action of voltage, due to ion Charge, cross-sectional area, quality etc. are not exactly the same, therefore the drift time in drift pipe is different, thus reach detector Time is different, according to product ion in the drift time of drift pipe, detects to determinand.IMS detection sensitivity is high, responds Speed is fast, and advantage is extremely prominent in the trace detection of volatile organic compounds, and detection limit can be even pg grades down to ng, is suitble to Field quick detection or analysis, detection time are often Millisecond.But IMS also has disadvantage, i.e., only carries out by drift pipe to compound Separation, inferior separating effect, and gas-chromatography and IMS are combined, and GC separation characteristic outstanding and IMS quick response, Gao Ling is utilized The advantage of sensitivity, efficiently solves the low distinguishing ability of GC and when IMS detects mixture existing cross sensitivity is asked Topic, finally obtains the three-dimensional spectrum of retention time, drift time and signal strength, keeps qualitative analysis more accurate.And it is equipped with The fast gas chromatography disengaging time of multiple capillary chromatographic column is substantially reduced compared with conventional chromatogram, can satisfy live quick point The needs of analysis.
For different trade mark cigarette because of tobacco leaf formulation difference, the flavors and fragrances of addition is different, makes it have unique fragrance and waves Hair property ingredient, that is, be different from the chemical composition of other cigarette, and this results in their respective fingerprint characteristics and brand identities.Sense organ Evaluation is the intuitive judgment of cigarette style characteristic, but sensory quality assessment method itself has biggish subjectivity, vulnerable to smokeing panel test The influence of the factors such as person's mood, physical condition.
Therefore it provides different trade mark cigarette can be carried out accurate Fast Classification by the method for a kind of pair of cigarette taxonomic history, It is a technical problem that technical personnel in the field need to solve at present without sample pre-treatments, visual result.
Summary of the invention
The object of the present invention is to provide the methods of a kind of pair of cigarette taxonomic history, and it is accurate to carry out to different trade mark cigarette The identification of Fast Classification, without complicated sample pre-treatments, visual result.
In order to solve the above technical problems, the present invention provides the following technical scheme that
The method of a kind of pair of cigarette taxonomic history, comprising: HS GC-ion mobility spectrometry is carried out to cigarette sample Analysis, obtains its three-dimensional spectrum;The selected characteristic analyzed area in the three-dimensional spectrum of collected cigarette sample;To collected The signature analysis region of the three-dimensional spectrum of cigarette sample is analyzed, and is identified to cigarette.
Preferably, HS GC-Ion transfer spectrum analysis is carried out to cigarette sample, obtains its three-dimensional spectrum, wrapped It includes: in gas-chromatography-Ion mobility spectrometry, using the head space-of the model FlavourSpec of German G.A.S instrument company Gas-chromatography-ion mobility spectrometry equipment;
Set gas-chromatography-Ion mobility spectrometry condition: chromatographic column is multiple capillary splitter, stationary phase OV-5, 32 DEG C of chromatogram column temperature;80 DEG C of injector temperature;Carrier gas is high pure nitrogen, and flow rate of carrier gas rises gas mode, initial flow using program Fast 8ml/min rises to 50ml/min after retaining 40s when 4min, and when 5min rises to 150ml/min, and 150ml/min is protected always It holds to 8min, flow velocity is down to initial flow 8ml/min when 8.5min;Migration spectrum drift gas flow 200ml/min;Migration spectrum drift Move pipe temperature 45 C.
Preferably, HS GC-Ion transfer spectrum analysis is carried out to cigarette sample, obtains its three-dimensional spectrum, wrapped Include: set head space condition: incubation temperature is 80 DEG C;Brooding time is 5min;Sampling volume is 200 μ l;Sample introduction needle temperature is 80 ℃。
Preferably, the three-dimensional spectrum selected characteristic analyzed area of collected cigarette sample is analyzed, to cigarette into Row identifies, comprising: the view in the collected cigarette sample three-dimensional spectrum signature analysis region is generated by Gallery plug-in unit Library, observation compare the appearance situation of each analyzed area signal peak, identify to cigarette;If the appearance phenomenon difference is obvious not Together, then determine the cigarette for different trade mark cigarette samples.
Preferably, the three-dimensional spectrum selected characteristic analyzed area of collected cigarette sample is analyzed, to cigarette into Row identifies, comprising: the knot in the signature analysis region of the three-dimensional spectrum of collected cigarette sample is generated using Gallery plug-in unit Fruit obtains the whole matching angle value of selected analyzed area between each cigarette sample;It will matching angle value and the progress of preset matching degree threshold value Comparison;If matching angle value is less than the matching degree threshold value, determine cigarette for different trade mark cigarette samples;If matching angle value is greater than Preset matching degree threshold value then determines that cigarette is identical trade mark cigarette sample.
Preferably, the signature analysis region of the three-dimensional spectrum of collected cigarette sample is analyzed, cigarette is carried out Identify, comprising: can by chemometrics method progress to the signature analysis region of the three-dimensional spectrum of collected cigarette sample It is analyzed depending on changing, cigarette is identified.
Preferably, chemometrics method carries out visual analyzing, comprising: principal component analysis, factorial analysis differentiate and divide Analysis, partial least squares discriminant analysis.
Preferably, chromatographic column further include: using the multi-capillary column or single long capillary column of other stationary phases.
Compared with prior art, above-mentioned technical proposal has the advantage that
The method of a kind of pair of cigarette taxonomic history provided by the present invention, to cigarette sample carry out HS GC-from Son migration spectrum analysis, obtains its three-dimensional spectrum;The selected characteristic analyzed area in the three-dimensional spectrum of collected cigarette sample;It is right The signature analysis region of the three-dimensional spectrum of collected cigarette sample is analyzed, and is identified to cigarette.By head space-gas phase- Ion mobility spectrometry joint technology identifies for cigarette Fast Classification, and method resolution ratio and high sensitivity, analysis time is short, and nothing Damage, no sample pre-treatment, method is environmental-friendly, tests that consumptive material used is few, and testing cost is low, visual result, is suitble to cigarette sample Product batch taxonomic history.
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 be briefly described, it should be apparent that, the accompanying drawings in the following description is the present invention Some embodiments for those of ordinary skill in the art without creative efforts, can also basis These attached drawings obtain other attached drawings.
Fig. 1 is the method flow diagram of a kind of pair of cigarette taxonomic history provided by a kind of specific embodiment of the present invention;
Fig. 2 is headspace gas chromatography-ion mobility spectrometry (GC-IMS) structural schematic diagram;
Fig. 3 is tri- trade mark cigarette GC-IMS three-dimensional spectrums of A, B, C;
Fig. 4 is that the selected signature analysis region of the trade mark cigarette 21 of A, B, C tri- regards library figure;
Fig. 5 is that A, B cigarette different batches select analyzed area matching degree comparison histogram;
Fig. 6 is that B, C cigarette sample select analyzed area matching degree comparison histogram;
Fig. 7 is OPLS-DA model the 1st, the 2 principal component scores figures in D, E cigarette sample signature analysis region;
Fig. 8 is the S-Plot figure that cigarette OPLS-DA analyzes 18 variables.
Specific embodiment
Core of the invention is to provide the method for a kind of pair of cigarette taxonomic history, and it is accurate to carry out to different trade mark cigarette Fast Classification, without complicated sample pre-treatments, visual result.
It is understandable in order to enable the above objects, features and advantages of the present invention to become apparent, with reference to the accompanying drawing to this hair Bright specific embodiment is described in detail.
Detail is elaborated in the following description to fully understand the present invention.But the present invention can with it is a variety of not Other way described herein is same as to implement, those skilled in the art can do class without violating the connotation of the present invention Like popularization.Therefore the present invention is not limited to the specific embodiments disclosed below.
Referring to FIG. 1, Fig. 1 is the method for a kind of pair of cigarette taxonomic history provided by a kind of specific embodiment of the present invention Flow chart.
A kind of specific embodiment of the invention provides the method for a kind of pair of cigarette taxonomic history, comprising steps of
S11: HS GC-Ion transfer spectrum analysis is carried out to cigarette sample, obtains its three-dimensional spectrum.
According to Headspace-Gas Chromatography Analysis-ion mobility spectrometry (HS-GC-IMS) method, different cigarette samples is divided Analysis, finally obtains the spectrogram of analysis.
S12: in the three-dimensional spectrum selected characteristic analyzed area of collected cigarette sample.
According to the three of the collected cigarette sample generated by HS GC-Ion mobility spectrometry of step S11 Spectrogram is tieed up, the signature analysis region that can characterize each cigarette sample volatility and semi-volatility component is chosen on the three-dimensional spectrum.
S13: the signature analysis region of the three-dimensional spectrum of collected cigarette sample is analyzed, is reflected to cigarette Not.
In step s 12, signature analysis region is had chosen to the three-dimensional spectrum of collected cigarette sample, according to right Signature analysis region is analyzed, and is identified to cigarette.
Can fast and accurately it be classified to different trade mark cigarette using this method, by directly acquiring cigarette sample to be sorted HS-GC-IMS spectrogram compares the signature analysis region of cigarette sample by software, the data processing software carried using instrument Gallery generate view library figure, or to analyzed area carry out whole matching degree compare, or by statistics software such as spss, The softwares such as simca-p, matlab to signature analysis region carry out chemometrics application for example principal component analysis, discriminant analysis, partially Least square method discriminant analysis etc., which is realized, carries out accurate Fast Classification identification to different trade mark finished cigarettes.
In a kind of embodiment provided by the present invention, HS GC-ion step S11: is carried out to cigarette sample Spectrum analysis is migrated, its three-dimensional spectrum is obtained, may include:
In gas-chromatography-Ion mobility spectrometry, using the model FlavourSpec of German G.A.S instrument company HS GC-ion mobility spectrometry equipment;
Set gas-chromatography-Ion mobility spectrometry condition: chromatographic column is multiple capillary splitter, stationary phase OV-5, 32 DEG C of chromatogram column temperature;80 DEG C of injector temperature;Carrier gas is high pure nitrogen, and flow rate of carrier gas rises gas mode, initial flow using program Fast 8ml/min rises to 50ml/min after retaining 40s when 4min, and when 5min rises to 150ml/min, and 150ml/min is protected always It holds to 8min, flow velocity is down to initial flow 8ml/min when 8.5min;Migration spectrum drift gas flow 200ml/min;Migration spectrum drift Move pipe temperature 45 C.
Above-mentioned gas-chromatography-Ion transfer spectral condition is a kind of optimum condition of specific embodiment of the present invention, using it His condition may also obtain preferable analysis as a result, can specifically set according to the actual situation, and the application is for the condition Setting without limitation.
Different batches flavors and fragrances sample is analyzed using the equipment, it, can also be first to this before obtaining analysis of spectra Gas-chromatography-ion mobility spectrometry equipment is cleaned, in case other remaining substances of the equipment have an impact analysis result.
In a kind of embodiment provided by the present invention, HS GC-ion step S11: is carried out to cigarette sample Spectrum analysis is migrated, its three-dimensional spectrum is obtained, may include:
Setting head space condition: 80 DEG C of incubation temperature;Brooding time 5min;200 μ l of sampling volume;80 DEG C of sample introduction needle temperature.
Above-mentioned head space condition is a kind of optimum condition of specific embodiment of the present invention, may also be obtained using other conditions Preferably analysis as a result, can specifically be set according to the actual situation, the application for the condition setting without limitation.
In a kind of embodiment provided by the present invention, step S13: the three-dimensional spectrum of collected cigarette sample is chosen Signature analysis region is analyzed, and is identified to cigarette, may include: described collected by the generation of Gallery plug-in unit The view library in cigarette sample three-dimensional spectrum signature analysis region, observation compares the appearance situation of each analyzed area signal peak, to volume Cigarette is identified;If the appearance phenomenon difference is significantly different, determine the cigarette for different trade mark cigarette samples.
In a kind of embodiment provided by the present invention, step S13: the three-dimensional spectrum of collected cigarette sample is chosen Signature analysis region is analyzed, and is identified to cigarette, may include:
Using Gallery plug-in unit generate the signature analysis region of the three-dimensional spectrum of collected cigarette sample as a result, Whole matching angle value to analyzed area selected between each cigarette sample matches angle value;Will matching angle value and preset matching degree threshold value into Row comparison;If matching angle value is less than the matching degree threshold value, determine cigarette for different trade mark cigarette samples;If it is big to match angle value In preset matching degree threshold value, then determine that cigarette is identical trade mark cigarette sample.
G.A.S company provides a series of integrated software analysis tools, it can be achieved that automatic data acquisition, data visualization, Assessment, calibration, the quantitative and functions such as qualitative, the LAV software and Gallery plug-in unit provided using G.A.S company in the present embodiment The signature analysis region of the three-dimensional spectrum of collected cigarette sample is analyzed, and is carried out pair with preset matching degree threshold value Than being classified with this to cigarette sample.
In a kind of embodiment provided by the present invention, step S13: the three-dimensional spectrum of collected cigarette sample is chosen Signature analysis region is analyzed, and is identified to cigarette, may include: the spy to the three-dimensional spectrum of collected cigarette sample It levies analyzed area and visual analyzing is carried out by chemometrics method, cigarette is identified.Chemometrics method carries out Visual analyzing, comprising: principal component analysis, factorial analysis, discriminant analysis, partial least squares discriminant analysis.
In a kind of embodiment provided by the present invention, HS GC-ion step S11: is carried out to cigarette sample Spectrum analysis is migrated, its three-dimensional spectrum is obtained, can also include:
Using the multi-capillary column or single long capillary column of other stationary phases;
Preferable separating effect such as can be obtained using 60m long DB-5 capillary column, but on analysis time, compared with MCC Capillary column is slow;It according to the actual situation and can need to select suitable chromatographic column.
Preferably to help to understand, citing is illustrated above method below:
Headspace gas chromatography-ion mobility spectrometry (GC-IMS) structural schematic diagram is as shown in Figure 2;
In figure, Drift gas is drift gas, and Carrier gas is gas of carrier gas, and T1 is migration spectrum drift tube temperature, T2 is chromatogram column temperature, and T3 is injector temperature, and IMS is ionic migration spectrometer, and EPC1 is migration spectrum drift gas flow, EPC2 For flow rate of carrier gas, sample is sample.
Embodiment one:
1) preparation of cigarette sample
The cigarette sample for choosing the different trades mark to be analyzed, taking 3 cigarette at random from each cigarette sample, (nominal cigarette is not Choosing) it is fitted into the ml headspace bottle of 20ml, a cigarette is packed into each ml headspace bottle, gland sealing is to be measured.
2) cigarette sample is analyzed using HS-GC-IMS
Analysis condition is as follows:
Head space condition: 80 DEG C of incubation temperature;Brooding time 5min;200 μ l of sampling volume;80 DEG C of sample introduction needle temperature;
GC-IMS condition: chromatographic column be multiple capillary splitter (MCC), stationary phase OV-5,32 DEG C of chromatographic column temperature;Injection port 80 DEG C of temperature;Carrier gas is high pure nitrogen;Flow rate of carrier gas: using program rise gas mode, initial flow rate 8ml/min, retain 40s after, Rise to 50ml/min when 4min, when 5min rises to 150ml/min, and 150ml/min is always maintained to 8min, flow velocity when 8.5min It is down to initial flow 8ml/min.
Migration spectrum drift gas flow 200ml/min;45 DEG C of migration spectrum drift tube temperature.
3) sample analysis and spectrogram are evaluated
The volatile and semi-volatile compounds for analyzing tri- trade mark cigarette samples of A, B, C under the above conditions, obtain its HS- GC-IMS three-dimensional spectrum.The spectrogram marker of analyzed cigarette, i.e. the signature analysis region of cigarette sample are selected, passes through what is selected Analyzed area generates view library using the Gallery plug-in unit that software carries, and is compared, reaches pair to analyzed area appearance situation The purpose of cigarette Fast Classification.
Fig. 3 is tri- trade mark cigarette GC-IMS three-dimensional spectrums of A, B, C.Most of peak concentrates on preceding 5min, and all peaks are basic It is complete out in 7min.
21 analyzed areas with obvious characteristic for choosing three trade mark cigarette three-dimensional spectrums, are handled by instrument data The included Gallery plug-in unit of software generates view library figure, as shown in figure 4, Fig. 4 is 18 batch A cigarette, 17 batch B cigarette, 15 A batch C cigarette selectes the view library of analyzed area, and different trade mark cigarette have strong response, same board in different analyzed areas The Ion transfer spectral peak of cigarette is extremely similar between number different batches, and peak shape is not much different with peak intensity, the peak shape between the trade mark with Peak intensity has significant difference.Analyzed area whole matching degree is 80% or more between same trade mark cigarette batch, and between the different trades mark Analyzed area matching degree 65% hereinafter, as shown in figure 5, by the basis of A4 cigarette sample, remaining cigarette sample and its into Row comparison, A1-A18 sample match degree is higher, matching degree > 80%, and B1-B17 cigarette sample and A1-A18 cigarette sample Matching degree < 65% of product, similitude is poor, illustrate No. A1-A18 from No. B1-B17 be the different trades mark cigarette sample.With No. B1 On the basis of cigarette sample, remaining cigarette sample is compared with it, matching degree > 80% between B1-B17 cigarette sample, and B1- Matching degree < 65% of B17 cigarette sample and C1-C15 cigarette sample, similitude is poor, illustrates No. B1-B17 and C1-C15 It number is the cigarette sample of the different trades mark.The method is carried out classification prediction for the blind sample of A, B, C cigarette, accuracy rate is up to 100%.
Embodiment two:
1) preparation of cigarette sample
Collecting D, E trade mark cigarette, closely different batches cigarette sample, each batch choose 3 cigarette (bear in parallel in two years Cigarette does not select) be fitted into the ml headspace bottle of 20ml seal it is to be measured.
2) cigarette sample is analyzed using HS-GC-IMS
Analysis condition is the same as example 1.
3) sample analysis and spectrogram are evaluated
18 signature analysis regions for choosing D, E cigarette sample GC-IMS three-dimensional spectrum, using 13 software pair of simca-p It carries out data analysis.D cigarette acquires 98 batches, and E cigarette acquires 34 batches, first carries out principal component point respectively to D and E Analysis checks that whether there is or not abnormal points in sample, reject after having abnormal point then to search reason;Then D and E sample is carried out orthogonal partially minimum Two multiply diagnostic method (OPLS-DA) analysis, and each analyzed area peak height is independent variable X, classified variable Y, and it is special to establish cigarette GC-IMS The disaggregated model for levying analyzed area, the classification for be used for after inside and outside verifying to sample to model are predicted.With 90 D and OPLS-DA disaggregated model is established as training set in the signature analysis region of E cigarette sample, and 3 principal components of extraction are to original number According to the accumulation interpretability [R of matrix2X (CUM)] up to 86.1%, cross validation obtains total explained variance [R of classified variable2 It (CUM)] is 98.8%, the predictive ability [Q of model2(CUM)] up to 98.5%, R2(CUM) and Q2(CUM) difference is much smaller than 0.3, illustrate that this model is an outstanding classification prediction model.The OPLS-DA model score figure of Fig. 7 can intuitively show model Classifying quality, two groups of sample separation degrees are big in figure, illustrate that the category of model effect is good.It can be found from the S-PLOTL figure of Fig. 8 The difference marker of 2 groups of sample variables, as shown in frame red in figure.Using the signature analysis region of 32 D, E cigarette samples as testing Card collection carries out external certificate to OPLS-DA disaggregated model, determines by decision rule prediction result, as a result, it has been found that 31 samples This obtains correct judgement.The method is suitble to identify cigarette high-volume Fast Classification.
In conclusion the method for a kind of pair of cigarette taxonomic history provided by the present invention, carries out head space-gas to cigarette sample Phase chromatography-Ion transfer spectrum analysis, obtains its three-dimensional spectrum;The selected characteristic point in the three-dimensional spectrum of collected cigarette sample Analyse region;The signature analysis region of the three-dimensional spectrum of collected cigarette sample is analyzed, taxonomic history is carried out to cigarette. HS GC-ion mobility spectrometry joint technology is used to cigarette Fast Classification to identify, method resolution ratio and high sensitivity, Analysis time is short, and lossless, no sample pre-treatment, and method is environmental-friendly, tests that consumptive material used is few, and testing cost is low, as a result Intuitively, it is suitble to cigarette sample batch taxonomic history.
The method of a kind of pair of cigarette taxonomic history provided by the present invention is described in detail above.It is used herein A specific example illustrates the principle and implementation of the invention, and the above embodiments are only used to help understand Method and its core concept of the invention.It should be pointed out that for those skilled in the art, not departing from this , can be with several improvements and modifications are made to the present invention under the premise of inventive principle, these improvement and modification also fall into the present invention In scope of protection of the claims.

Claims (8)

1. the method for a kind of pair of cigarette taxonomic history characterized by comprising
HS GC-Ion transfer spectrum analysis is carried out to cigarette sample, obtains corresponding three-dimensional spectrum;
The selected characteristic analyzed area in collected cigarette sample three-dimensional spectrum;
The signature analysis region of the collected cigarette sample three-dimensional spectrum is analyzed, taxonomic history is carried out to cigarette.
2. the method according to claim 1, wherein carrying out HS GC-Ion transfer to cigarette sample Spectrum analysis obtains corresponding three-dimensional spectrum, comprising:
In the HS GC-Ion mobility spectrometry, using the HS GC-of model FlavourSpec Ion mobility spectrometry equipment;
Set gas-chromatography-Ion mobility spectrometry condition: chromatographic column is multiple capillary splitter, stationary phase OV-5, chromatography 32 DEG C of column temperature;80 DEG C of injector temperature;Carrier gas is high pure nitrogen, and flow rate of carrier gas rises gas mode, initial flow rate using program 8ml/min rises to 50ml/min after retaining 40s when 4min, and when 5min rises to 150ml/min, and 150ml/min is always maintained at To 8min, flow velocity is down to initial flow 8ml/min when 8.5min;Migration spectrum drift gas flow 200ml/min;Migrate Frequency bias Pipe temperature 45 C.
3. the method according to claim 1, wherein carrying out HS GC-Ion transfer to cigarette sample Spectrum analysis obtains corresponding three-dimensional spectrum, comprising:
Setting head space condition: 80 DEG C of incubation temperature;Brooding time 5min;200 μ l of sampling volume;80 DEG C of sample introduction needle temperature.
4. method according to any one of claims 1 to 3, which is characterized in that collected cigarette sample three-dimensional spectrum Middle selected characteristic analyzed area is analyzed, and is identified to cigarette, comprising:
The view library in the collected cigarette sample three-dimensional spectrum signature analysis region is generated by Gallery plug-in unit, is observed The appearance situation for comparing each analyzed area signal peak, identifies cigarette;If the appearance phenomenon difference is significantly different, sentence The fixed cigarette is different trade mark cigarette samples.
5. method according to any one of claims 1 to 3, which is characterized in that collected cigarette sample three-dimensional spectrum Middle selected characteristic analyzed area is analyzed, and is identified to cigarette, comprising:
Using Gallery plug-in unit generate the signature analysis region of the three-dimensional spectrum of collected cigarette sample as a result, obtaining each The whole matching angle value of selected analyzed area between cigarette sample;
The matching angle value and preset matching degree threshold value are compared;If the matching angle value is less than the preset matching degree threshold Value, then determine the cigarette for different trade mark cigarette samples;If the matching angle value is greater than the preset matching degree threshold value, sentence The fixed cigarette is identical trade mark cigarette sample.
6. method according to any one of claims 1 to 3, which is characterized in that three-dimensional to the collected cigarette sample The signature analysis region of spectrogram is analyzed, and is identified to cigarette, comprising:
The signature analysis region of the three-dimensional spectrum of the collected cigarette sample is carried out visually by chemometrics method Change analysis, cigarette is identified.
7. according to the method described in claim 6, it is characterized in that, the three-dimensional spectrum to the collected cigarette sample Signature analysis region by chemometrics method carry out visual analyzing include:
Using principal component analysis, and/or factorial analysis, and/or discriminant analysis, and/or partial least squares discriminant analysis to described The signature analysis region of the three-dimensional spectrum of collected cigarette sample carries out visual analyzing.
8. according to the method described in claim 2, it is characterized in that, the chromatographic column further include:
Using the multi-capillary column or single long capillary column of stationary phase.
CN201710948016.9A 2017-10-12 2017-10-12 A kind of method of pair of cigarette taxonomic history Pending CN109655532A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710948016.9A CN109655532A (en) 2017-10-12 2017-10-12 A kind of method of pair of cigarette taxonomic history

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710948016.9A CN109655532A (en) 2017-10-12 2017-10-12 A kind of method of pair of cigarette taxonomic history

Publications (1)

Publication Number Publication Date
CN109655532A true CN109655532A (en) 2019-04-19

Family

ID=66109876

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201710948016.9A Pending CN109655532A (en) 2017-10-12 2017-10-12 A kind of method of pair of cigarette taxonomic history

Country Status (1)

Country Link
CN (1) CN109655532A (en)

Cited By (19)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110907556A (en) * 2019-12-10 2020-03-24 湖北中烟工业有限责任公司 GC-IMS-based evaluation method for tobacco aroma of different producing areas
CN111044638A (en) * 2019-12-31 2020-04-21 贵州中烟工业有限责任公司 Method for classifying and identifying different varieties of flue-cured tobacco leaves
CN111060642A (en) * 2019-12-31 2020-04-24 贵州中烟工业有限责任公司 Method for classifying and identifying tobacco leaves of same variety and different producing areas
CN111443161A (en) * 2020-01-23 2020-07-24 华东理工大学 Electronic nose gas-sensitive-chromatographic information fusion and flavor substance on-site detection and analysis method
CN111505174A (en) * 2020-06-12 2020-08-07 上海烟草集团有限责任公司 Method for identifying true and false cigarettes
CN111624265A (en) * 2020-04-22 2020-09-04 南京农业大学 Method for identifying egg species
CN111830184A (en) * 2020-08-07 2020-10-27 中国农业科学院农业质量标准与检测技术研究所 Method for identifying difference of quality of thin-skinned sweet fruits after forchlorfenuron application
CN112179870A (en) * 2020-10-15 2021-01-05 湖北中烟工业有限责任公司 Cigarette classification recognition model construction method based on near infrared spectrum and OPLS-DA
CN113138248A (en) * 2021-04-25 2021-07-20 贵州中烟工业有限责任公司 Characteristic spectrum extraction method and detection method for feed liquid preparation quality stability
CN113655110A (en) * 2021-07-28 2021-11-16 中国科学院合肥物质科学研究院 Mass spectrum detection method and device for rapidly discriminating different brands of cigarettes on line
CN114720611A (en) * 2022-04-02 2022-07-08 云南中烟工业有限责任公司 Method for analyzing shelf life attenuation characteristics of aroma compounds of finished cigarette paper
CN114720599A (en) * 2022-04-02 2022-07-08 云南中烟工业有限责任公司 Chemometrics and organoleptic analysis method of finished cigarette paper
CN114755333A (en) * 2022-04-02 2022-07-15 云南中烟工业有限责任公司 Attenuation characteristic analysis method for stability acceleration experiment sample of finished cigarette paper
CN114755330A (en) * 2022-04-02 2022-07-15 云南中烟工业有限责任公司 Chemometrics and organoleptic analysis method of finished cigarette paper after combustion
CN114755353A (en) * 2022-04-02 2022-07-15 云南中烟工业有限责任公司 Chemometrics and sensory omics analysis method of aromatized cigarette paper
CN114814052A (en) * 2022-04-02 2022-07-29 云南中烟工业有限责任公司 GC-IMS-based method for analyzing similarity of essence and spice complex system
CN114965815A (en) * 2022-05-24 2022-08-30 云南中烟工业有限责任公司 Aromatized cigarette paper classification and identification method based on chemometrics-sensory omics
CN115047098A (en) * 2022-05-24 2022-09-13 云南中烟工业有限责任公司 Fingerprint spectrum analysis method for aroma components of different aromatized cigarette paper
CN114720611B (en) * 2022-04-02 2024-11-08 云南中烟工业有限责任公司 Method for analyzing shelf life decay characteristics of aroma compound of finished cigarette paper

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6495823B1 (en) * 1999-07-21 2002-12-17 The Charles Stark Draper Laboratory, Inc. Micromachined field asymmetric ion mobility filter and detection system
CN104833700A (en) * 2015-03-20 2015-08-12 红云红河烟草(集团)有限责任公司 Online mildew detection method for cigarette production line
CN106770862A (en) * 2017-01-17 2017-05-31 江苏大学 A kind of Classification of Tea method

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6495823B1 (en) * 1999-07-21 2002-12-17 The Charles Stark Draper Laboratory, Inc. Micromachined field asymmetric ion mobility filter and detection system
CN104833700A (en) * 2015-03-20 2015-08-12 红云红河烟草(集团)有限责任公司 Online mildew detection method for cigarette production line
CN106770862A (en) * 2017-01-17 2017-05-31 江苏大学 A kind of Classification of Tea method

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
北京格林德国际科技有限公司: "FlavourSpec®风味仪离子迁移谱技术及其在烟草行业的应用", 《HTTPS://WWW.ANTPEDIA.COM/IBOOK4520/DISTDL.PHP?ID=8490》 *
周沅桢等: "芯片级非对称场离子迁移谱技术快速识别不同霉变烟草", 《中国烟草学报》 *
霍羽佳 等: "气相离子迁移谱(GC-IMS):基于挥发性化合物指纹信息的茶叶质量评估新技术", 《第八届食品质量安全技术论坛论文集》 *

Cited By (25)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110907556A (en) * 2019-12-10 2020-03-24 湖北中烟工业有限责任公司 GC-IMS-based evaluation method for tobacco aroma of different producing areas
CN111044638A (en) * 2019-12-31 2020-04-21 贵州中烟工业有限责任公司 Method for classifying and identifying different varieties of flue-cured tobacco leaves
CN111060642A (en) * 2019-12-31 2020-04-24 贵州中烟工业有限责任公司 Method for classifying and identifying tobacco leaves of same variety and different producing areas
CN111443161A (en) * 2020-01-23 2020-07-24 华东理工大学 Electronic nose gas-sensitive-chromatographic information fusion and flavor substance on-site detection and analysis method
CN111443161B (en) * 2020-01-23 2021-01-05 华东理工大学 Electronic nose gas-sensitive-chromatographic information fusion and flavor substance on-site detection and analysis method
CN111624265A (en) * 2020-04-22 2020-09-04 南京农业大学 Method for identifying egg species
CN111505174A (en) * 2020-06-12 2020-08-07 上海烟草集团有限责任公司 Method for identifying true and false cigarettes
CN111830184A (en) * 2020-08-07 2020-10-27 中国农业科学院农业质量标准与检测技术研究所 Method for identifying difference of quality of thin-skinned sweet fruits after forchlorfenuron application
CN111830184B (en) * 2020-08-07 2021-06-22 中国农业科学院农业质量标准与检测技术研究所 Method for identifying difference of quality of thin-skinned sweet fruits after forchlorfenuron application
CN112179870A (en) * 2020-10-15 2021-01-05 湖北中烟工业有限责任公司 Cigarette classification recognition model construction method based on near infrared spectrum and OPLS-DA
CN113138248A (en) * 2021-04-25 2021-07-20 贵州中烟工业有限责任公司 Characteristic spectrum extraction method and detection method for feed liquid preparation quality stability
CN113655110A (en) * 2021-07-28 2021-11-16 中国科学院合肥物质科学研究院 Mass spectrum detection method and device for rapidly discriminating different brands of cigarettes on line
CN114720611A (en) * 2022-04-02 2022-07-08 云南中烟工业有限责任公司 Method for analyzing shelf life attenuation characteristics of aroma compounds of finished cigarette paper
CN114720599A (en) * 2022-04-02 2022-07-08 云南中烟工业有限责任公司 Chemometrics and organoleptic analysis method of finished cigarette paper
CN114755333A (en) * 2022-04-02 2022-07-15 云南中烟工业有限责任公司 Attenuation characteristic analysis method for stability acceleration experiment sample of finished cigarette paper
CN114755330A (en) * 2022-04-02 2022-07-15 云南中烟工业有限责任公司 Chemometrics and organoleptic analysis method of finished cigarette paper after combustion
CN114755353A (en) * 2022-04-02 2022-07-15 云南中烟工业有限责任公司 Chemometrics and sensory omics analysis method of aromatized cigarette paper
CN114814052A (en) * 2022-04-02 2022-07-29 云南中烟工业有限责任公司 GC-IMS-based method for analyzing similarity of essence and spice complex system
CN114814052B (en) * 2022-04-02 2024-07-26 云南中烟工业有限责任公司 Similarity analysis method of essence and spice complex system based on GC-IMS
CN114720611B (en) * 2022-04-02 2024-11-08 云南中烟工业有限责任公司 Method for analyzing shelf life decay characteristics of aroma compound of finished cigarette paper
CN114755333B (en) * 2022-04-02 2024-11-08 云南中烟工业有限责任公司 Attenuation characteristic analysis method of stability acceleration experiment sample of finished cigarette paper
CN114965815A (en) * 2022-05-24 2022-08-30 云南中烟工业有限责任公司 Aromatized cigarette paper classification and identification method based on chemometrics-sensory omics
CN115047098A (en) * 2022-05-24 2022-09-13 云南中烟工业有限责任公司 Fingerprint spectrum analysis method for aroma components of different aromatized cigarette paper
CN115047098B (en) * 2022-05-24 2024-03-19 云南中烟工业有限责任公司 Fingerprint analysis method for aroma components of different aroma-imparting cigarette paper
CN114965815B (en) * 2022-05-24 2024-04-19 云南中烟工业有限责任公司 Method for classifying and identifying aroma-added cigarette paper based on chemometrics-sensory group

Similar Documents

Publication Publication Date Title
CN109655532A (en) A kind of method of pair of cigarette taxonomic history
CN109655529A (en) A method of identifying genuine-fake cigarette
US20190302069A1 (en) Apparatus and method for classifying a tobacco sample into one of a predefined set of taste categories
JP4594154B2 (en) Analysis of at least one sample based on two or more techniques for characterizing the sample in terms of at least one component and the product produced and providing characterization data; method, system and instruction program
CN110441423A (en) A kind of method and its system measuring grain fragrance component
CN106770862A (en) A kind of Classification of Tea method
CN103134850A (en) Tea quality rapid detection apparatus and detection method based on characteristic fragrance
Klemenc In common batch searching of illicit heroin samples—evaluation of data by chemometrics methods
CN109655533A (en) A method of identifying flavors and fragrances type
CN109655566A (en) A method of identifying Volatile Components in Cigarette stability
CN111044638A (en) Method for classifying and identifying different varieties of flue-cured tobacco leaves
US20220229040A1 (en) Method for authentication of animal species origin of leather products
CN109738569B (en) High-imitation cigarette identification method based on SPME-GC-MS
Pereira et al. Direct classification of new psychoactive substances in seized blotter papers by ATR-FTIR and multivariate discriminant analysis
CN112578039B (en) Method for analyzing and identifying adulterants in bird&#39;s nest
CN105917221A (en) Tandem mass spectrometry data processing device
CN111060642A (en) Method for classifying and identifying tobacco leaves of same variety and different producing areas
CN106932510A (en) The sorting technique of one vegetable oil
CN104713845A (en) Mixture component identification method based on terahertz absorption spectrum processing
CN109655530A (en) A method of identifying flavors and fragrances quality difference
CN106770607B (en) A method of identifying genuine-fake cigarette using HS-IMR-MS
CN105928899A (en) Method and system for detecting color spot contamination of cigarettes
CN106404884A (en) Method for quickly evaluating quality consistency of flavors and fragrances of volatile cigarettes by HS-IMR-MS
CN111505174A (en) Method for identifying true and false cigarettes
CN112116964A (en) Detection method for rapidly judging fruit producing area

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20190419

RJ01 Rejection of invention patent application after publication