CN110441423A - A kind of method and its system measuring grain fragrance component - Google Patents
A kind of method and its system measuring grain fragrance component Download PDFInfo
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- CN110441423A CN110441423A CN201910728491.4A CN201910728491A CN110441423A CN 110441423 A CN110441423 A CN 110441423A CN 201910728491 A CN201910728491 A CN 201910728491A CN 110441423 A CN110441423 A CN 110441423A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- 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
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- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
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Abstract
The present invention provides a kind of methods for measuring grain fragrance component, for to grain affiliated region and the affiliated time identify, include: that the grain samples of different geographical and different year are detected using gas-chromatography-ion mobility spectrometry combination, obtains sample data；Statistic of classification analysis is carried out to sample data, obtains the signature object for characterizing the grain in some region or some time, and corresponding sample database is established based on analysis result；Grain samples to be measured are detected using gas-chromatography-ion mobility spectrometry combination, obtain the analysis data of the grain samples to be measured；The analysis data of obtained grain samples to be measured are compared with the signature object in corresponding sample database, so that it is determined that the affiliated region of grain samples to be measured and/or affiliated time.The present invention can quickly and easily be measured the place of production of grain and time, without being chemically treated to grain samples.
Description
Technical field
The present invention relates to a kind of methods and its system for measuring grain fragrance component, belong to technical field of analysis and detection.
Background technique
China is agricultural production big country, vast in territory, and the grain of same kind is planted in different geographical, the wind contained by itself
How taste substance identifies the grain place of production, how the difference of different geographical grain flavor identifies there are difference, is always Grain Trade
Problems faced.
The method of current test flavor substance includes the naked eyes evaluation (trial test) of someone, the electronic nose for copying people's sense organ
Method, instrument aspect have been reported that using gas phase, gas phase-mass spectrometry detection method.However, naked eyes evaluation and copying people's sense organ
Electronic nose be measured, inefficiency and can have error in judgement, all be needed using gas phase, gas phase-mass spectrometry method
A series of more complex pretreatment process are carried out to sample.
It would therefore be highly desirable to need to provide it is a kind of being capable of simple and quick and comprehensive and accurate measurement grain fragrance technical side
Case.
Summary of the invention
In view of the above technical problems, the embodiment of the present invention provides a kind of method for measuring grain fragrance component, this method energy
Comprehensively and accurately measure fragrance component (volatile organic matter) ingredient of grain.In addition, the embodiment of the present invention also provides a kind of survey
Determine the system of grain fragrance component.
The technical solution adopted by the present invention are as follows:
The embodiment of the present invention provides a kind of method for measuring grain fragrance component, for affiliated region to grain and affiliated
Time is identified, which comprises
The grain samples of different geographical and different year are detected using gas-chromatography-ion mobility spectrometry combination, are obtained
To GC-IMS sample data, the sample data includes the type and content of the volatile materials in grain samples；
Statistic of classification analysis is carried out to the GC-IMS sample data, characterization is obtained and belongs to some region or some time
The signature object of grain, and corresponding GC-IMS sample database, including grain zone data library are established based on analysis result
With grain time database；
Grain samples to be measured are detected using the gas-chromatography-ion mobility spectrometry combination, obtain the grain to be measured
The GC-IMS for eating sample analyzes data, the type and content including the volatile materials in grain samples to be measured；
By the GC-IMS analysis data of obtained grain samples to be measured and the feature in corresponding GC-IMS sample database
Marker is compared, so that it is determined that the affiliated region of the grain samples to be measured and/or affiliated time.
Optionally, detecting step associated with the gas-chromatography-ion mobility spectrometry includes:
The sample to be tested for weighing predetermined amount is placed in headspace sampling bottle, wherein the quality and headspace sampling bottle of sample to be tested
Volume between relationship be 5g:20ml；
By the headspace sampling bottle under 70 DEG C~90 DEG C of incubation temperature, with the mixing speed of 500rpm hatching 10~
30min；
Using sample introduction needle the sample to be tested of 0.1~1ml is extracted in treated headspace sampling bottle be put into gas phase from being hatched
In chromatography-ion mobility spectrometry combined instrument, the detection of volatile materials is realized, wherein sample introduction needle temperature is 5 DEG C higher than incubation temperature；
The gas-chromatography-ion mobility spectrometry combined instrument setting parameter are as follows: injector temperature is 65-85 DEG C；Chromatographic column uses capillary
Pipe chromatographic column；Carrier gas is nitrogen；Drift tube temperature is 40-50 DEG C；Gas-chromatography column temperature is 50-70 DEG C；Injection port chromatographic column
Converter temperature is 60-80 DEG C；Chromatographic column migration tube converter temperature is 40-60 DEG C；Ion mode uses positive ion mode.
Optionally, the grain includes wheat, corn, flour and paddy.
The embodiment of the present invention also provides a kind of system for measuring grain fragrance component, which is characterized in that for grain
Affiliated region and affiliated time are identified, the system comprises:
Detection module, for the grain sample using gas-chromatography-ion mobility spectrometry combination to different geographical and different year
Product are detected, and obtain GC-IMS sample data, the sample data include the volatile materials in grain samples type and
Content；And
For being detected using the combination of the gas-chromatography-ion mobility spectrometry to grain samples to be measured, obtain it is described to
The GC-IMS for surveying grain samples analyzes data, the type and content including the volatile materials in grain samples to be measured；
Analysis module obtains characterization and belongs to some area for carrying out statistic of classification analysis to the GC-IMS sample data
The signature object of the grain in domain or some time, and corresponding GC-IMS sample database is established based on analysis result, including
Grain zone data library and grain time database；
Identification module, for the GC-IMS of obtained grain samples to be measured to be analyzed data and corresponding GC-IMS sample number
It is compared according to the signature object in library, so that it is determined that the affiliated region of the grain samples to be measured and/or affiliated time.
Optionally, detecting step associated with the gas-chromatography-ion mobility spectrometry includes:
The sample to be tested for weighing predetermined amount is placed in headspace sampling bottle, wherein the quality and headspace sampling bottle of sample to be tested
Volume between relationship be 5g:20ml；
By the headspace sampling bottle under 70 DEG C~90 DEG C of incubation temperature, with the mixing speed of 500rpm hatching 10~
30min；
Using sample introduction needle the sample to be tested of 0.1~1ml is extracted in treated headspace sampling bottle be put into gas phase from being hatched
In chromatography-ion mobility spectrometry combined instrument, the detection of volatile materials is realized, wherein sample introduction needle temperature is 5 DEG C higher than incubation temperature；
The gas-chromatography-ion mobility spectrometry combined instrument setting parameter are as follows: injector temperature is 65-85 DEG C；Chromatographic column uses capillary
Pipe chromatographic column；Carrier gas is nitrogen；Drift tube temperature is 40-50 DEG C；Gas-chromatography column temperature is 50-70 DEG C；Injection port chromatographic column
Converter temperature is 60-80 DEG C；Chromatographic column migration tube converter temperature is 40-60 DEG C；Ion mode uses positive ion mode.
Optionally, the grain includes wheat, corn, flour and paddy.
The embodiment of the present invention also provides a kind of computer storage medium, is stored thereon with computer program, the computer
When program is executed by processor, the measuring method of grain fragrance component above-mentioned is realized.
The embodiment of the present invention also provides a kind of computer storage medium, is stored thereon with computer journey described in computer program
When sequence is executed by processor, the measurement system of grain fragrance component above-mentioned is realized.
It is provided in an embodiment of the present invention measurement grain fragrance component method and its system, due to using gas-chromatography-from
Sub- migration spectrum combination detects sample to be tested, and sample needs not move through complicated pre-treatment (solvent extraction, solid phase microextraction
Deng), direct headspace sampling analysis can save a large amount of labours, and can be improved detection efficiency and improve the accurate of detection
Degree.
Detailed description of the invention
Fig. 1 is the flow diagram of the measuring method of grain fragrance component provided in an embodiment of the present invention；
Fig. 2 to Fig. 4 is the volatile organic matter contrast difference figure in different wheats and flour in the embodiment of the present invention；
Fig. 5 and Fig. 6 is respectively the partial enlargement diagram of Fig. 3 and Fig. 4；
Fig. 7 is to carry out the schematic diagram that clustering obtains using wheat and flour sample of the PCA to the present embodiment；
Fig. 8 is to carry out the schematic diagram that clustering obtains using wheat samples of the PCA to the different sources of the present embodiment；
Fig. 9 is to be shown using what wheat and flour sample progress clustering of the PCA to the identical place of production of the present embodiment obtained
It is intended to；
Figure 10 is to carry out the schematic diagram that clustering obtains using wheat of the PCA to the different sources of the present embodiment；
Figure 11 is the structural block diagram of the measurement system of grain fragrance component provided in an embodiment of the present invention.
Specific embodiment
To keep the technical problem to be solved in the present invention, technical solution and advantage clearer, below in conjunction with attached drawing and tool
Body embodiment is described in detail.
Technical idea of the invention is to provide a kind of method for measuring grain fragrance component, and this method passes through gas phase color
Spectrum-ion mobility spectrometry combination is measured, and more can comprehensively and accurately measure fragrance (volatile organic matter) ingredient of grain,
For to grain affiliated region and the affiliated time identify, feature is without can be quick under conditions of sample pre-treatments
The volatile organic matter in grain samples is detected, the source area of grain can be quickly judged by the analysis of software, without destruction sample
The physical form of product itself provides the test method and analysis foundation of a kind of feasibility for the identification in grain source area.One
In a illustrative examples, method provided in an embodiment of the present invention can be used for measuring wheat, corn, flour and paddy etc..
As shown in Figure 1, it is provided in an embodiment of the present invention measurement grain fragrance component method the following steps are included:
S101, the grain samples of different geographical and different year are examined using gas-chromatography-ion mobility spectrometry combination
It surveys, obtains GC-IMS sample data, the sample data includes the type and content of the volatile materials in grain samples.
In this step, the region of grain samples, storage time and quantity can be selected as needed, as long as can protect
It is sufficient, authentic and valid to demonstrate,prove sample.Detecting step associated with gas-chromatography-ion mobility spectrometry of use can include:
(1) sample to be tested for weighing predetermined amount is placed in headspace sampling bottle, wherein the quality and headspace sampling of sample to be tested
Relationship between the volume of bottle is 5g:20ml；In one example, take grain samples to be measured, sample to be tested can for 5.00 ±
0.01g, headspace sampling bottle are 20mL.
(2) by the headspace sampling bottle under 70 DEG C~90 DEG C of incubation temperature, hatch 10 with the mixing speed of 500rpm
~30min.In an optimum condition, incubation temperature is 80 DEG C；Brooding time is 20min.
(3) sample to be tested of 0.1~1ml is extracted in treated headspace sampling bottle be put into gas using sample introduction needle from being hatched
In phase chromatography-ion mobility spectrometry combined instrument, the detection of volatile materials is realized, wherein sample introduction needle temperature is higher than incubation temperature by 5
℃；The gas-chromatography-ion mobility spectrometry combined instrument setting parameter are as follows: injector temperature is 65-85 DEG C；Chromatographic column uses hair
Capillary chromatographic column；Carrier gas is nitrogen；Drift tube temperature is 40-50 DEG C；Gas-chromatography column temperature is 50-70 DEG C；Injection port chromatography
Column converter temperature is 60-80 DEG C；Chromatographic column migration tube converter temperature is 40-60 DEG C；Ion mode uses positive ion mode.
In a preferable example, sample introduction needle temperature is 85 DEG C；Sampling volume is 0.1mL；Gas-chromatography-ion mobility spectrometry combined instrument is set
Set parameter are as follows: injector temperature is 80 DEG C；Chromatographic column uses capillary chromatographic column；Carrier gas is nitrogen；Drift tube temperature is 45 DEG C；
Gas-chromatography column temperature is 60 DEG C；Injection port chromatographic column converter temperature is 70 DEG C；Chromatographic column migration tube converter temperature is 50
℃；Ion mode uses positive ion mode.In this way, storage can be collected according to actual needs by the way that such testing conditions are arranged
Different types of sample information, such as: the grain fragrance for being 5 years with kind different geographical, different productive lifes such as time span
Compositional data.Region, age can be distinguished according to statistical analysis, whether can also be had according to the identification of sample database data and artificially be added
Add, such as uses essence class flavouring additive.,
In this step, sample introduction can be carried out automatically and also carries out sample introduction manually.Automatic sampling can be used full-automatic head space into
Sample device carries out sample introduction.The sample pretreatment process that redundant and complicated can be exempted using head-space sampler, avoid organic solvent to point
The pollution of interference, reduction to chromatographic column and injection port, can adapt to batch samples sample introduction, compensates for artificial sample introduction caused by analysis
Trouble.Using hand sampling, water-bath can be used or hatching is completed in air bath, then utilize syringe sampling inserting needle.
S102, statistic of classification analysis is carried out to the GC-IMS sample data, is characterizedBelong toSome region or some The signature object of the grain in time, and corresponding GC-IMS sample database, including grain region are established based on analysis result Database and grain time database。
In this step, statistic of classification analysis can be by establishing regression model or using analyses sides such as least square methods
Method calculates correlation, the coefficient of variation of test data (content of volatile materials), finds out significant factors and difference sexual factor
Deng then obtaining signature object, signature object is the volatility object that can be come with other regions or time significant difference
The type and content of matter, can be used clustering method, dynamic principal component analytical method, Gallery Plot analysis method and
Reporter analysis method etc..In specific implementation, statistic of classification analysis can be matched by gas-chromatography-ion mobility spectrometry combined instrument
The software of set carries out statistic of classification analysis, such as: passing through spectrogram difference (two-dimensional top-down view and the Three Dimensional Spectrum between direct contrast sample
Figure) Reporter plug-in unit realize Reporter analysis；Compared by finger-print, intuitively and quantitatively more different samples it
Between volatile organic matter difference Gallery Plot plug-in unit realize Gallery Plot analysis；For sample clustering to be divided
Analysis, and quickly determine that the Dynamic PCA plug-in unit of the type of unknown sample realizes dynamic principal component analysis etc..
S103, grain samples to be measured are detected using the combination of the gas-chromatography-ion mobility spectrometry, obtain it is described to
The GC-IMS for surveying grain samples analyzes data, the type and content including the volatile materials in grain samples to be measured.
In the step as the detecting step in abovementioned steps S101 to grain samples, omitted herein to its specific Jie
It continues.
S104, by the GC-IMS of obtained grain samples to be measured analysis data in corresponding GC-IMS sample database
Signature object is compared, so that it is determined that the affiliated region of the grain samples to be measured and/or affiliated time.
In this step, can according to analysis purpose by the type and content of the volatile materials of grain samples to be measured with it is corresponding
Grain sample database in signature object be compared, can will for example, it is desired to when determining the place of production of grain samples to be measured
The type and content of the volatile materials of the grain samples to be measured withWhat the signature object in grain zone data library was characterized The type and content of volatile materials are compared, to obtain the place of production of the grain samples to be measured, dynamic principal component can be used
Analysis method and Gallery Plot analysis method etc. carry out.It in actual operation, can be by comparing grain samples to be measured Volatile materials map in volatile materials map and grain samples database compares.
The method of measurement grain fragrance provided in an embodiment of the present invention, can be by collecting different zones, various years even
The grain samples of country variant test the constituent of its flavor substance, find out signature object, more particularly to passing through big data
Judge that the place of production of a collection of sample, harvest time (the storage time limit) are of great significance in current Grain Trade, can be used to integrate
Determine storage situation (new-old degree), the production region characteristic etc. of grain, can also be routinely made up of flavor substance map come pair
The flavors and fragrances artificially added determines, and provides reference frame for the place of production of grain and time identification.
[Application Example]
Hereinafter, providing for wheat and flour volatile materials to distinguish different regions using the embodiment of the present invention
Method concrete application illustrate.
Sample message
Sample description: 30 wheats and 15 flour
Preserving type: it is stored at room temperature
Sample number into spectrum: it is detailed in the following table 1
1 sample message table of table
Experiment information
Experiment purpose: the wheat and flour volatile materials of different sources are distinguished.
Sample treatment: taking sample 5g, is placed in 20mL headspace sampling bottle, and 80 DEG C are incubated for sample introduction after twenty minutes.
Analysis condition
Analysis instrument:Flavor analyzer
System condition: as shown in the following table 2 and 3.
2 analysis condition of table
3 GC conditions of table
| Time | E1 | E2 | R |
| 00:00,000 | 150mL/min | 2ml/min | Rec |
| 02:00,000 | 150mL/min | 2ml/min | - |
| 20:00,000 | 150mL/min | 150ml/min | - |
| 25:00,000 | 150mL/min | 150mL/min | Stop |
| 55:00,020 | 150mL/min | 150mL/min | --- |
Analyze software
The matched analysis software package of instrument include LAV (Laboratory Analytical Viewer) and three sections of plug-in units and
GC × IMS Library Search can carry out sample analysis from different perspectives respectively.
LAV: for checking analysis of spectra, each point represents a kind of volatile organic matter in figure；Standard song is established to it
Quantitative analysis can be carried out after line.
Reporter plug-in unit: the spectrogram difference (two-dimensional top-down view and three-dimensional spectrum) between direct contrast sample.
Gallery Plot plug-in unit: finger-print comparison, intuitively and quantitatively the volatility between more different samples has
Machine object difference.
Dynamic PCA plug-in unit: dynamic principal component analysis for analyzing sample clustering, and quickly determines unknown sample
The type of product.
GC × IMS Library Search: NIST database and ims database built in application software can to substance into
Row qualitative analysis, user can utilize standard items voluntarily expanding data library according to demand.
Analyze result
1. selected part sample directly compares the volatile organic matter difference in different wheats and flour, comparing result is as schemed
Shown in 2.Wherein, in Fig. 2:
(1) ordinate represents the retention time of gas-chromatography, and abscissa represents the Ion transfer time；
(2) entire figure background is black, and light tone vertical line is the peak RIP (reactant ion peak, at normalization at abscissa 1.0
Reason)；
(3) each point of the peak RIP two sides represents a kind of volatile organic matter.The concentration of shade representative species, it is white
Color table shows that concentration is lower, and high bright limb black table shows that concentration is higher, and color shows that concentration is bigger more deeply feeling.
From figure 2 it can be seen that the volatile materials between different samples has differences.Less for more obvious ratio
With the difference of sample room, contrast difference's mode can be used: the spectrogram (SD40-2) for choosing one of sample is used as reference, other
The spectrogram of sample reduces reference.If the two volatile organic matter is consistent, the background after reducing is white, and black is represented and is somebody's turn to do
The concentration of substance is higher than reference, and grey represents the concentration of the substance lower than reference.As can be seen from Figure 3 the part in HB08-2
Volatile matter content increases, and part volatile matter content is reduced；Most of volatile matter content in SDF40-2 is bright
It is aobvious to reduce.
In order to preferably compare the situation of change of volatile organic matter, frame selects the peak of these volatile organic matters, forms sample
Product finger-print compares.
2. volatile organic matter finger-print compares in wheat and flour sample
Volatile organic matter finger-print comparing result is as shown in Figure 4 in wheat and flour sample.Wherein:
(1) every a line represents the whole signal peaks chosen in a sample in figure.
(2) each column represent signal peak of the same volatile organic matter in different samples in figure.
(3) as can be seen from Figure 4 volatile organic matter between the complete volatile matter information and sample of every kind of sample
Difference.
In entire fingerprint image, the finger-print of Hebei wheat, Shandong wheat, Shandong wheat flour is marked in figure with black wire
Region.It is followed successively by Hebei wheat, Shandong wheat and Shandong flour from top to bottom.Wherein it can be seen that the volatility in the flour of Shandong
Substance is relatively minimal；And the volatile materials in the wheat of Hebei is more relatively fewer than the volatile materials in Shandong；In order to better
Each component volatile materials the change of divergence is compared, partial enlargement is carried out, amplified local fingerprint figure is as shown in Figure 5 and Figure 6.In
In local fingerprint Fig. 5, in which:
(1) substance that number is 11,16,55,58,28,44,34,64 and 57 content in the wheat of Hebei is apparently higher than mountain
Eastern wheat and flour；
(2) substance that number is 1,24,4,10,25,26,18,43,41,88,30,36,50 and 61 is on Hebei wheat and mountain
Exist in eastern wheat, and content is then seldom in the flour of Shandong；
(3) number be 27,22,35,47,75,33,5,36,9,17,2,12,45,86,53,42,81,29,66,60,77,
63, then the content in the wheat of Shandong is higher than the content in the wheat of Hebei for 65,37 and 3 substance, and content is then in the flour of Shandong
Seldom.
Qualitative substance out is as shown in table 4 below in local fingerprint Fig. 5:
The qualitative substance out in local fingerprint Fig. 5 of table 4
In local fingerprint Fig. 6, in which:
(1) content of material that number is 7,52,31,69 compares Hebei wheat sample in Shandong wheat and Shandong flour content
Content in product is high；
(2) substance that number is 84,54,87,56,59,83 and 82 is then that content is with respect to highest in flour, in wheat sample
Content is then almost seldom in product；
(3) substance that number is 20,40,67,15,39,23,21 and 85 is then in Hebei wheat and Shandong flour content phase
To higher, and content is then relatively lower in the wheat of Shandong；
(4) substance that number is 46,14,70,32,48,13,49 and 62 is all contained substantially in wheat and flour sample
Have, only there is little bit different in content.
Qualitative substance out is as shown in table 5 below in local fingerprint Fig. 6:
The qualitative substance out in local fingerprint Fig. 5 of table 5
3, wheat and flour sample clustering (dynamic principal component analysis PCA)
Clustering, obtained analysis result such as Fig. 7 are carried out to wheat and flour sample using dynamic principal component analysis PCA
It is shown.
In Fig. 7, the dark dot of upper right side is Shandong wheat flour sample, and the dot in left side is Hebei wheat samples,
The light dot of lower right side is Shandong wheat samples.From fig. 6 it can be seen that the differentiation of wheat and wheat flour is clearly,
And the wheat of different sources is distinguished also clearly, is intersected between sample without existing.
4, the wheat samples clustering (dynamic principal component analysis PCA) of different sources
Clustering, obtained analysis result are carried out using wheat samples of the dynamic principal component analysis PCA to different sources
As shown in Figure 8.
In fig. 8, dark dot is Hebei wheat samples, and light dot is Shandong wheat samples.It can from Fig. 8
Out, the wheat of different sources is distinguished also clearly, is intersected between sample without existing.The wheat samples in Hebei comparatively collect
In it is some, and Shandong wheat samples relative distribution is some.
5, the clustering (dynamic principal component analysis PCA) of identical place of production wheat and flour
Clustering is carried out using wheat and flour sample of the dynamic principal component analysis PCA to the identical place of production, obtained point
It is as shown in Figure 9 to analyse result.
In Fig. 9, left side dark color dot is Shandong wheat flour sample, and lower right side light color dot is Shandong wheat sample
Product.It can be seen in figure 9 that differentiation of the wheat samples between flour sample is clearly, this is consistent with fingerprint chromatogram information.
6, the wheat samples clustering (dynamic principal component analysis PCA) of different sources
Clustering, obtained analysis result are carried out using wheat samples of the dynamic principal component analysis PCA to different sources
As shown in Figure 10, the compound obtained is listed as follows shown in table 6:
6 compound list of table
Conclusion:
By FlavourSpec flavor analyzer, wheat can be quickly detected under conditions of without sample pre-treatments
And the volatile organic matter in flour, the source area of wheat can be quickly judged by the analysis of software, clustering is obviously by river
Northern wheat and Shandong wheat separate, and the wheat in Shandong and flour are clearly separated and are individually separated, and analysis time is short, easy to operate,
A kind of analysis foundation of feasibility is provided for the identification in wheat source area.
Based on the same inventive concept, the embodiment of the invention also provides a kind of systems for measuring grain fragrance, since this is
The principle for solved problem of uniting is similar to the aforementioned measurement method of grain fragrance, therefore the implementation of the system may refer to aforementioned side
The implementation of method, overlaps will not be repeated.
It is provided in an embodiment of the present invention measurement grain fibre fragrance system, for grain affiliated region and the affiliated time
Identified, as shown in figure 11, the system comprises:
Detection module 201, for the grain using gas-chromatography-ion mobility spectrometry combination to different geographical and different year
Sample is detected, and GC-IMS sample data is obtained, and the sample data includes the type of the volatile materials in grain samples
And content；And
For being detected using the combination of the gas-chromatography-ion mobility spectrometry to grain samples to be measured, obtain it is described to
The GC-IMS for surveying grain samples analyzes data, the type and content including the volatile materials in grain samples to be measured；
Analysis module 202 obtains characterization and belongs to some for carrying out statistic of classification analysis to the GC-IMS sample data
The signature object of the grain in region or some time, and corresponding GC-IMS sample database is established based on analysis result, it wraps
Include grain zone data library and grain time database；
Identification module 203, for the GC-IMS of obtained grain samples to be measured to be analyzed data and corresponding GC-IMS sample
Signature object in database is compared, so that it is determined that the affiliated region of the grain samples to be measured and/or affiliated year
Part.
Further, detecting step associated with the gas-chromatography-ion mobility spectrometry includes:
The sample to be tested for weighing predetermined amount is placed in headspace sampling bottle, wherein the quality and headspace sampling bottle of sample to be tested
Volume between relationship be 5g:20ml；
By the headspace sampling bottle under 70 DEG C~90 DEG C of incubation temperature, with the mixing speed of 500rpm hatching 10~
30min；
Using sample introduction needle the sample to be tested of 0.1~1ml is extracted in treated headspace sampling bottle be put into gas phase from being hatched
In chromatography-ion mobility spectrometry combined instrument, the detection of volatile materials is realized, wherein sample introduction needle temperature is 5 DEG C higher than incubation temperature；
The gas-chromatography-ion mobility spectrometry combined instrument setting parameter are as follows: injector temperature is 65-85 DEG C；Chromatographic column uses capillary
Pipe chromatographic column；Carrier gas is nitrogen；Drift tube temperature is 40-50 DEG C；Gas-chromatography column temperature is 50-70 DEG C；Injection port chromatographic column
Converter temperature is 60-80 DEG C；Chromatographic column migration tube converter temperature is 40-60 DEG C；Ion mode uses positive ion mode.
Further, the grain includes wheat, corn, flour and paddy.
The embodiment of the invention also provides a kind of computer readable storage medium, stored on the computer readable storage medium
There is computer program, which executes the measuring method of above-mentioned grain fragrance component when being run by processor the step of.
The embodiment of the invention also provides a kind of computer readable storage medium, stored on the computer readable storage medium
There is computer program, which executes the function of the measurement system of above-mentioned grain fragrance component when being run by processor.
Specifically, which can be general storage medium, such as mobile disk, hard disk, on the storage medium
Computer program when being run, be able to carry out above-mentioned sample data classification and determine method, to solve in the related technology to height
The problem that it is not objective enough and low accuracy that dimension data is classified.
Embodiment described above, only a specific embodiment of the invention, to illustrate technical solution of the present invention, rather than
It is limited, scope of protection of the present invention is not limited thereto, although having carried out with reference to the foregoing embodiments to the present invention detailed
Illustrate, those skilled in the art should understand that: anyone skilled in the art the invention discloses
In technical scope, it can still modify to technical solution documented by previous embodiment or variation can be readily occurred in, or
Person's equivalent replacement of some of the technical features；And these modifications, variation or replacement, do not make corresponding technical solution
Essence is detached from the spirit and scope of technical solution of the embodiment of the present invention, should be covered by the protection scope of the present invention.Therefore,
The protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (8)
1. it is a kind of measure grain fragrance component method, which is characterized in that for grain affiliated region and the affiliated time into
Row identifies, which comprises
The grain samples of different geographical and different year are detected using gas-chromatography-ion mobility spectrometry combination, obtain GC-
IMS sample data, the sample data include the type and content of the volatile materials in grain samples；
Statistic of classification analysis is carried out to the GC-IMS sample data, characterization is obtained and belongs to some region or the grain in some time
Signature object, and based on analysis result establish corresponding GC-IMS sample database, including grain zone data library and grain
Eclipse year database；
Grain samples to be measured are detected using the gas-chromatography-ion mobility spectrometry combination, obtain the grain sample to be measured
The GC-IMS of product analyzes data, the type and content including the volatile materials in grain samples to be measured；
By the GC-IMS analysis data of obtained grain samples to be measured and the signature in corresponding GC-IMS sample database
Object is compared, so that it is determined that the affiliated region of the grain samples to be measured and/or affiliated time.
2. the method according to claim 1, wherein detecting step associated with the gas-chromatography-ion mobility spectrometry
Suddenly include:
The sample to be tested for weighing predetermined amount is placed in headspace sampling bottle, wherein the quality of sample to be tested and the body of headspace sampling bottle
Relationship between product is 5g:20ml；
By the headspace sampling bottle under 70 DEG C~90 DEG C of incubation temperature, 10~30min is hatched with the mixing speed of 500rpm；
Using sample introduction needle the sample to be tested of 0.1~1ml is extracted in treated headspace sampling bottle be put into gas-chromatography-from being hatched
In ion mobility spectrometry combined instrument, the detection of volatile materials is realized, wherein sample introduction needle temperature is 5 DEG C higher than incubation temperature；The gas
Phase chromatography-ion mobility spectrometry combined instrument setting parameter are as follows: injector temperature is 65-85 DEG C；Chromatographic column uses capillary chromatography
Column；Carrier gas is nitrogen；Drift tube temperature is 40-50 DEG C；Gas-chromatography column temperature is 50-70 DEG C；Injection port chromatographic column converter
Temperature is 60-80 DEG C；Chromatographic column migration tube converter temperature is 40-60 DEG C；Ion mode uses positive ion mode.
3. the method according to claim 1, wherein the grain includes wheat, corn, flour and paddy.
4. it is a kind of measure grain fragrance component system, which is characterized in that for grain affiliated region and the affiliated time into
Row identifies, the system comprises:
Detection module, for using the combination of gas-chromatography-ion mobility spectrometry to the grain samples of different geographical and different year into
Row detection, obtains GC-IMS sample data, the sample data includes the type and content of the volatile materials in grain samples；
And
For detecting using the gas-chromatography-ion mobility spectrometry combination to grain samples to be measured, the grain to be measured is obtained
The GC-IMS for eating sample analyzes data, the type and content including the volatile materials in grain samples to be measured；
Analysis module, for the GC-IMS sample data carry out statistic of classification analysis, obtain characterization belong to some region or
The signature object of the grain in some time, and corresponding GC-IMS sample database, including grain are established based on analysis result
Zone data library and grain time database；
Identification module, for the GC-IMS of obtained grain samples to be measured to be analyzed data and corresponding GC-IMS sample database
In signature object be compared, so that it is determined that the affiliated region of the grain samples to be measured and/or affiliated time.
5. system according to claim 4, which is characterized in that detect step associated with the gas-chromatography-ion mobility spectrometry
Suddenly include:
The sample to be tested for weighing predetermined amount is placed in headspace sampling bottle, wherein the quality of sample to be tested and the body of headspace sampling bottle
Relationship between product is 5g:20ml；
By the headspace sampling bottle under 70 DEG C~90 DEG C of incubation temperature, 10~30min is hatched with the mixing speed of 500rpm；
Using sample introduction needle the sample to be tested of 0.1~1ml is extracted in treated headspace sampling bottle be put into gas-chromatography-from being hatched
In ion mobility spectrometry combined instrument, the detection of volatile materials is realized, wherein sample introduction needle temperature is 5 DEG C higher than incubation temperature；The gas
Phase chromatography-ion mobility spectrometry combined instrument setting parameter are as follows: injector temperature is 65-85 DEG C；Chromatographic column uses capillary chromatography
Column；Carrier gas is nitrogen；Drift tube temperature is 40-50 DEG C；Gas-chromatography column temperature is 50-70 DEG C；Injection port chromatographic column converter
Temperature is 60-80 DEG C；Chromatographic column migration tube converter temperature is 40-60 DEG C；Ion mode uses positive ion mode.
6. system according to claim 1, which is characterized in that the grain includes wheat, corn, flour and paddy.
7. a kind of computer storage medium, is stored thereon with computer program, which is characterized in that the computer program is processed
When device executes, the measuring method of grain fragrance component as described in any one of claims 1-3 is realized.
8. a kind of computer storage medium, is stored thereon with computer program, which is characterized in that the computer program is processed
When device executes, the measurement system such as the described in any item grain fragrance components of claim 4-6 is realized.
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