CN105954366B - A kind of essence spice for cigarette character surveillance method - Google Patents
A kind of essence spice for cigarette character surveillance method Download PDFInfo
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- CN105954366B CN105954366B CN201610136714.4A CN201610136714A CN105954366B CN 105954366 B CN105954366 B CN 105954366B CN 201610136714 A CN201610136714 A CN 201610136714A CN 105954366 B CN105954366 B CN 105954366B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas chromatography
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Abstract
The present invention relates to field of tobacco preparation, a kind of essence spice for cigarette character surveillance method is disclosed, conventional fingerprint graphical spectrum technology, two-dimentional color-matter combination are organically combined with sensory evaluating smoking three, advantage mutually merges, disadvantage mutually makes up, and achievees the purpose that effectively to control flavors and fragrances quality.Specific steps are as follows: acquisition flavors and fragrances Gas Chromatography Fingerprint first, the fragrant component information of crucial cause is obtained using GC-MS and is quantitatively weighted in finger-print, finally quantify the experience for teacher of the smokeing panel test, the chemical analysis that analysis instrument can not be detected effectively, it is simulated component and is quantitatively added in finger-print with by way of weighting, form the holographic fingerprint for combining multiple characteristics.On this basis, the fingerprints database for constructing target flavors and fragrances sample, establishes mode standard, finally by the method for statistical analysis, realizes effective identification to the character surveillance or unknown sample of new flavors and fragrances sample.Compared with traditional character surveillance method, the information of the method for the invention is richer, more comprehensively, as a result more acurrate reliable, is with a wide range of applications and market prospects.
Description
Technical field
The present invention relates to field of tobacco preparation, in particular to the character surveillance side of flavors and fragrances in a kind of tobacco preparation process
Method.
Background technique
Tobacco is a kind of complex system, and the place of production, tobacco leaf position, processing technology and flavors and fragrances of addition etc. can be right
Its quality generates certain influence, how to guarantee the quality of tobacco and safety is always flavors and fragrances manufacturing enterprise and tobacco enterprise
The problem of industry is paid high attention to.Essence spice for cigarette is the important factor in order for constituting cigarette brand style, suitable and suitable perfume (or spice)
Smart fragrance is formulated to assign the distinctive fragrance of cigarette product, reduces the stimulation to human body, improves mouthfeel.Therefore, meat flavor formulating technology
It is important one of the core technology of tobacco business.
Essence spice for cigarette refers to the substance used in the tobacco business with certain fragrance or fragrance, including with difference
The natural perfume material that method is extracted and the synthetic perfume obtained by chemical reaction.Flavouring essence for tobacco is the perfume (or spice) by two or more
Material and some auxiliary materials (carrier, solvent, preservative, antioxidant etc.) according to certain proportion and pass through corresponding allocating technology institute
Manufactured spice mixture.Therefore, it carries out analysis and research to essence spice for cigarette ingredient and will be helpful to dissect complicated essence to match
Just and to flavors and fragrances carry out effective quality control.
Finger-print be it is a kind of effectively objectively flavors and fragrances quality control and evaluation means, can qualitatively and quantitatively mark
The feature of flavors and fragrances is known, to distinguish that the quality of flavors and fragrances provides reliable foundation.Currently, most essence spice for cigarette
Method of quality control is all built upon on the basis of finger-print.Flavors and fragrances is such as obtained by gas-chromatography (hereinafter referred to as GC)
Finger-print characterize the composition characteristic of essence spice for cigarette, the advantages of and then effective monitoring its quality, this method is can
With accurate, objective reaction flavors and fragrances quality, the disadvantage is that due to being limited by instrument precision degree, micro flavors and fragrances
It is difficult detected, some information can be omitted.Essence is for another example analyzed using gas chromatography-mass spectrography (hereinafter referred to as GC-MS)
The chemical component of fragrance obtains the finger-print of feature, by comparing the similarity of finger-print between actual measurement sample and sample,
Come the degree of closeness both judged, advantage is that accuracy is good, and can intuitively find out certain flavors and fragrances specifically includes which is changed
It closes object or causes fragrant characteristic, disadvantage is a lack of visual angle of overall importance, cannot effectively be commented the quality of finger-print on the whole
Valence.It is by the sensory evaluating smoking for teacher of the smokeing panel test and physical and chemical index (such as relative density, alcohol number, refractive index) to perfume (or spice) there are also certain methods
Smart quality of flavoring is analyzed, but such method is largely needed by artificial subjective determination, therefore accuracy and can
Control property is poor.
In conclusion needing a kind of scientific and reasonable, objective and accurate quality of flavoring essence for tobacco control method.
Summary of the invention
The purpose of the present invention is: in order to solve defect and deficiency of the existing technology, it is fragrant that the present invention provides a kind of cigarette
Finger-print, GC-MS analysis and sensory evaluating smoking are organically combined, are mutually drawn excellent by smart fragrance-quality monitoring method, this method
Point, makes up disadvantage, and obtained holographic fingerprint being capable of complete characterization flavors and fragrances chemical composition global information.Pass through comparison
The similarity of sample to be tested and standard fingerprint mode, and assist scheming using principal component analysis shot chart and bi-plot, with judge to
The quality of sample, and the global or local compositional difference between sample is effectively excavated, to precisely be monitored to its quality.
In order to achieve the above objectives, the technical solution adopted by the present invention can by Fig. 1 shows.
Technology segment of the invention mainly includes the content of two aspects, one is the foundation of holographic standard fingerprint mode；
The second is the character surveillance of unknown sample.The former mainly analyzes chromatographic fingerprinting, the GC- of 10 or more target flavors and fragrancess
MS analysis and product inhale teacher's empirical results, by the elimination method of models fitting, the weighting of component experience and singular value, obtain
The standard fingerprint mode of comprehensive each sample Global Information；The latter is then based on same method, obtains the Holographic Fingerprint of unknown sample
Map, using similarity calculation and PCA analysis method, effective evaluation flavors and fragrances quality difference, obtain character surveillance as a result,
And above-mentioned all processes can be completed with the integral form of programme software bundle.
The beneficial effects of the present invention are: the present invention is by conventional fingerprint map, GC-MS analysis and sensory evaluating smoking three
It organically combines, efficiently uses respective advantage, overcome the disadvantage for making up other side, on the basis using tradition GC acquisition finger-print
On, the important qualitative, quantitative information for causing fragrant component is obtained with GC-MS analysis, and find corresponding informance in finger-print, weighted
Important component, finally the component that instrument can't detect is added in finger-print by teacher of the smokeing panel test by way of compositional modeling, with
Three combines to form holographic fingerprint.On the basis of obtaining target essence spice for cigarette sample holographic fingerprint, building
Standard fingerprint mode judges the quality of sample to be tested finally by the statistical methods such as similarity calculation and PCA analysis.Relatively
For conventional fingerprint map, obtained holographic fingerprint information is richer, more comprehensively in the present invention, and verification result is accurate
Reliably, it is with a wide range of applications and market prospects.
Detailed description of the invention
Fig. 1 is the technical solution adopted in the present invention schematic diagram.
Fig. 2 is traditional chromatographic fingerprinting of flavors and fragrances in embodiment 1.
Fig. 3 is to combine conventional fingerprint map, GC-MS and product to inhale the holographic standard fingerprint mode that result obtains in embodiment 1.
Specific embodiment
The present invention is described in detail with reference to the accompanying drawings and examples.
On the basis of conventional fingerprint map of the present invention, GC-MS analysis is based on to the fragrant component of important cause and is weighted processing, it is right
The component not detected in analysis instrument carries out information supplement, forms that information is richer, comprehensively and accurately holographic fingerprint.
First choice collects the flavors and fragrances sample that total 25 numbers of certain cigar mill offer are AB, using following experiment item
Part carries out chromatography, including chromatographic fingerprinting analysis is analyzed with GC-MS.Experiment condition are as follows: analysis instrument Agilent
6890/5973, chromatographic column is DB-1 (30m × 250 μm I.D. × 0.25 μm df), temperature programming condition are as follows: temperature programming item
Part, 30 DEG C of initial temperature, and secondary temperature keep 2.0min, rise to 180 DEG C with 4.0 DEG C/min speed, then again with 5.0 DEG C/
Min rises to 300 DEG C, finally keeps 5.0min, and obtained finger-print is as shown in Figure 2.According to the study found that the essence
Hydroxypropanone-, menthones, geraniol are important cause perfume (or spice) component in fragrance, are analyzed based on GC-MS as a result, carrying out to finger-print
Weighting, and on the basis of artefact inhales teacher, whole synthesis processing is carried out to the finger-print in Fig. 2, also includes the quality of data
It improves, such as shift of retention time correction, background deduction processing, finally all 25 sample standard deviations is similarly analyzed, are obtained
To holographic standard fingerprint mode shown in Fig. 3.Three components being wherein weighted mark in dots, and inhale mould by product
Formal notation of quasi- two compounds being added in finger-print in figure with model is in holographic fingerprint.
Finally in the same way, unknown flavors and fragrances sample is analyzed and processed, its holographic fingerprint is obtained.It is logical
The similarity-rough set with above-mentioned standard fingerprint pattern is crossed, it is found that the unknown sample fully meets the requirement of character surveillance, similarity
Reach 0.97, and by the way that the sample is added to progress PCA analysis in aforementioned 25 samples, from shot chart and bi-plot figure
Also clearly it can be found that the sample and the sample of building standard fingerprint mode do not have conspicuousness difference, thus the standard of verification result
True property.
In particular, it should be pointed out that the present invention relates to including that chromatography component shift of retention time corrects, background deduction, component
The content of identification and simulation, component weighting and similarity calculation and statistical analysis aspect, but whole solve is analyzed by data
Scheme software systems can very quickly, easily obtain the result that every step needs.
Claims (6)
1. a kind of essence spice for cigarette character surveillance method, which is characterized in that by conventional fingerprint map, based on GC-MS analysis
Key causes fragrant composition weighting and sense organ product suction three to organically combine, and reaches more accurately quantization quality monitoring purpose, specific to wrap
Include following steps:
Step 1: establish essence spice for cigarette holography standard fingerprint mode, including following sub-step:
Step 1.1: selection or the accumulative essence spice for cigarette sample for obtaining 10 or more；
Step 1.2: fingerprint map analyzing being carried out to the sample by conventional gas-phase chromatography and data acquire；
Step 1.3: the characteristic flavor matter information of sample is obtained by GC-MS, i.e., the known qualitative, quantitative letter for causing fragrant component
Breath finds corresponding component chromatographic peak according to mass spectrum and retention time in conventional fingerprint map, and carries out to these specific components
Weighting processing, weighted factor empirically determine；
Step 1.4: professional product inhale teacher and carry out the suction of sense organ product to above-mentioned flavors and fragrances sample, not by finger-print or GC-MS instrument
It can detect, and inhale teacher by product and inhale the chemical composition found by product, be inhaled according to quantitative product as a result, passing through what multi-component model was simulated
These components are added into above-mentioned finger-print by mode, and rule of thumb carry out component weighting processing, and it is fragrant to obtain new cigarette
Smart fragrance holographic fingerprint；
Step 1.5: by shift of retention time correction, background deduction step, optimization finger-print sample data is obtained, using phase
Like the method that degree calculating or PCA are analyzed, unusual sample is rejected, and then constructs flavors and fragrances holography standard fingerprint mode, and calculate
Similarity between each sample, with average similarity SimstdStandard of comparison as unknown sample；
Step 2: in above-mentioned identical method, obtaining the holographic fingerprint of essence spice for cigarette sample to be analyzed, specific method
Referring to step 1.2-1.5；
Step 3: the holographic fingerprint for being analysed to essence spice for cigarette sample is compared with standard fingerprint mode, passes through phase
Like the method that degree calculates, compare similarity between the two, and with SimstdThe threshold value mark qualified or not as flavors and fragrances quality
Standard, the quality of comparative evaluation sample to be analysed.
2. essence spice for cigarette character surveillance method according to claim 1, which is characterized in that special in the step 1.3
Sign flavor matter is determined by prior information first, then accurately finds correspondingization in GC-MS data according to corresponding Information in Mass Spectra
Object is closed, and based on the chromatogram under same experimental conditions, in addition shift of retention time alignment technique, in traditional chromatographic fingerprinting
Find corresponding cause aroma compounds information.
3. essence spice for cigarette character surveillance method according to claim 1, which is characterized in that in the step 1.3, look for
To after feature flavor matter, using the method for chromatographic peak identification, the outflow information of feature flavor matter is found, and be based on the substance
Cause perfume (or spice) characteristic be weighted processing.
4. essence spice for cigarette character surveillance method according to claim 1, which is characterized in that in the step 1.4, product
The obtained compound information of teacher is inhaled, is simulated using EMG model, model parameter is inhaled the obtained result of teacher by product and determined.
5. essence spice for cigarette character surveillance method according to claim 1, which is characterized in that in the step 3,
To after corresponding finger-print, need to carry out it pretreatment operation of shift of retention time correction, background deduction.
6. essence spice for cigarette character surveillance method according to claim 1, which is characterized in that passing through comparison similarity
Method judge outside essence spice for cigarette sample quality, need to assist analyzing obtained shot chart and bi- using PCA
Plot figure carries out singular values standard form, and assists similarity evaluation.
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106568882B (en) * | 2017-02-21 | 2019-02-12 | 广东铭康香精香料有限公司 | A method of analysis shampoo fragrance component |
| CN107941978B (en) * | 2017-11-23 | 2020-07-31 | 陕西中烟工业有限责任公司 | Method for evaluating internal quality stability of bead blasting for cigarettes |
| CN109932436B (en) * | 2017-12-19 | 2022-04-12 | 湖南中烟工业有限责任公司 | Digital fragrance distinguishing method based on characteristic mass spectrum |
| CN109061017B (en) * | 2018-08-10 | 2021-06-15 | 上海烟草集团有限责任公司 | Method for evaluating cigarette perfuming uniformity |
| CN110954604A (en) * | 2018-09-27 | 2020-04-03 | 上海烟草集团有限责任公司 | GC-MS/MS-based tobacco essence quality monitoring method |
| CN114324716B (en) * | 2021-08-30 | 2023-06-30 | 华南农业大学 | Method for measuring oxidation rancidity degree of infant formula rice flour and application thereof |
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| CN102680627A (en) * | 2012-05-15 | 2012-09-19 | 上海烟草集团有限责任公司 | Method for analyzing and identifying key aromatic substances in tobacco leaf |
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