CN109884257A - The discrimination method of cyclocarya paliurus tea - Google Patents
The discrimination method of cyclocarya paliurus tea Download PDFInfo
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Abstract
The present invention provides a kind of discrimination methods of cyclocarya paliurus tea, it is related to tea plant quality identification technical field, this method is impregnated to obtain sample to be tested in boiling water after first crushing cyclocarya paliurus tea, followed by the sample after electronic nose and electronic tongues detection acquisition, and PCA and DFA are carried out to testing result and analyzed, comprehensive identification is carried out to the genuine piece of cyclocarya paliurus tea, adulterant, the place of production for mixing adulterant and cyclocarya paliurus tea in combination with GC-TOFMS mass-spectrometric technique.Above-mentioned discrimination method can quickly identify the genuine piece of cyclocarya paliurus tea, adulterant, the place of production for mixing adulterant and cyclocarya paliurus tea, with resolution height, identify fireballing advantage, effectively alleviates the existing cyclocarya paliurus tea true and false and the quality place of production is not easy the problem of screening.
Description
Technical field
The present invention relates to tea plant quality identification technical fields, more particularly, to a kind of discrimination method of cyclocarya paliurus tea.
Background technique
Blue or green money willow (Cyclocarya paliurus (Batal.) Iljinskaja) is Dicotyledoneae, and Juglandaceae is green
Money sallow is the distinctive Mono-species genus in China, is distributed widely in numerous provinces and cities in Subtropic of China area.Blue or green money willow exists
Some regions of China have very long edible history, and Jiangxi local resident is often with its leaf brewed for drinking, Qingqian Willow leaf bubble
Millet paste sweetness out moistens, promotes the production of body fluid to quench thirst, and is known as " Sweet tea " by local common people.Although Qingqian Willow leaf is taken as tea always to drink
With, but blue or green money willow and it is not belonging to ordinary food scope for a long time, until on October 30th, 2013, planning commission, committee, country was just formally criticized
Quasi- Qingqian Willow leaf is new raw-food material, and it is edible to can be used as ordinary food, and stipulated that its edible way is " brewing ", therefore is worked as
The main utilization form of preceding Qingqian Willow leaf is tea making.
In recent years, blue or green money willow causes domestic and foreign scholars' extensive concern with its distinctive health-care effect and bioactivity.Research
Show containing the multiple compounds such as triterpene, flavones, polysaccharide, phenols in Qingqian Willow leaf, and confirm, Qingqian Willow leaf have it is hypoglycemic,
The active function of lowering blood pressure and blood fat.As this plant resources of Qingqian Willow leaf have been to be concerned by more and more people, cyclocarya paliurus tea
Sales volume and market prospects increased trend year by year is presented.However, as the market share of cyclocarya paliurus tea constantly expands, by blueness
Money willow resource constraint and Qingqian Willow leaf are difficult to the influence distinguished, and cyclocarya paliurus tea adulteration is serious, from cyclocarya paliurus tea form,
Food Inspection person and general public can not directly distinguish cyclocarya paliurus tea the true and false and quality height, and cyclocarya paliurus tea chemistry at
Part, character flavor compound document report are less, the deficiency of basic research, so that the relevant criterion of cyclocarya paliurus tea works out difficult, face
It has no way of judging to very different cyclocarya paliurus tea product.The cyclocarya paliurus tea product that Vehicles Collected from Market is sold is multifarious, price difference
Different great disparity, quality is very different, can not objectively evaluate the quality of cyclocarya paliurus tea, and especially common incorporation shape is similar, cheap
But inactive Chinese Wingmut Leaf, the subsequent development that this status seriously restricts the resource utilize.
How the quality of objective appraisal cyclocarya paliurus tea, be rapidly performed by the identification of the true and false quality of blue or green money willow, and quickly discriminate
Whether other leaves for not having active function do not mix in cyclocarya paliurus tea, are becoming very necessary and urgent at this stage.
In view of this, the present invention is specifically proposed.
Summary of the invention
The first object of the present invention is to provide a kind of discrimination method of cyclocarya paliurus tea, and the discrimination method passes through to electronics
The data obtained after nose and electronic tongues detection carry out PCA and DFA analysis, and combine GC-TOFMS mass spectrogram can be quickly to blueness
The genuine piece of Qian Liucha, adulterant mix adulterant and the place of production of cyclocarya paliurus tea is identified, and have resolution high, identify fireballing
Advantage, effectively alleviates the existing cyclocarya paliurus tea true and false and the quality place of production is not easy the problem of screening.
A kind of discrimination method of cyclocarya paliurus tea provided by the invention, the discrimination method is the following steps are included: first will be green
Qian Liucha is impregnated to obtain sample to be tested in boiling water after crushing, and detects sample to be tested followed by electronic nose and electronic tongues,
And PCA and DFA are carried out to testing result and analyzed, in combination with GC-TOFMS mass spectrum to the genuine piece of cyclocarya paliurus tea, adulterant, mix adulterant
And the place of production of cyclocarya paliurus tea carries out comprehensive identification.
Further, the smashed partial size of the cyclocarya paliurus tea was the powder of 20~100 meshes.
Preferably, described impregnate is that head space impregnates, i.e., cyclocarya paliurus tea is placed in ml headspace bottle and is impregnated.Head space impregnates
Concrete principle are as follows: by solid or fluid sample, i.e., cyclocarya paliurus tea of the present invention is placed in ml headspace bottle, and volatility is to be measured
Substance is then diffused into ml headspace bottle top, once the test substance concentration on ml headspace bottle top reaches flat with the concentration in sample substrate
Weighing apparatus, the gas on ml headspace bottle top are then loaded into the detection devices such as mass spectrum or electronic nose, electronic tongues and are analyzed.Concrete principle can
It hauls, China People's Public Security University Press, publishes within 2015, page 153 referring to " sample in analytical chemistry " (beauty) Mi Te.
Further, the step of head space impregnates are as follows: smashed cyclocarya paliurus tea is put into ml headspace bottle, then with 1:
5~50 solid-liquid ratio injection boiling water and gland sealed soak, obtains sample to be tested；
Preferably, the head space volume that the head space impregnates is the 1/4~2/3 of ml headspace bottle total volume；
Preferably, the soaking time that the head space impregnates is 5~30min, and heating temperature is 50~80 DEG C；
It is furthermore preferred that the boiling water is the distilled water boiled.
Further, flow rate of carrier gas when being detected using electronic nose to sample is 50~150ml/min, sample note
Beam product is 0.5~2ml, and 50~100 DEG C of injector temperature, sample acquisition time is 60~240s, and lag time is 60~300s；
Preferably, the electronic nose is Alpha Fox4000 electronic nose detector.
Further, electronic tongues maximum voltage when being detected using electronic tongues to sample is set as 1~5V, minimum
Voltage is -5~-1V, and Sample injection volume 15-30ml, the pulse spacing is 100~300mV；
Preferably, the electronic tongues are Smart tough electronic tongues detector.
Further, the PCA analysis method is the data that electronic nose and electronic tongues obtain to be inputted pca model, respectively
According to electronic nose and the PCA of electronic tongues analysis as a result, using contributing maximum 2 principal components to respectively obtain two-dimentional shot chart, then
The genuine piece of cyclocarya paliurus tea is determined according to the registration of two-dimentional shot chart and various cyclocarya paliurus tea samples, adulterant, mixes adulterant and blueness
The place of production of Qian Liucha.
Further, the DFA analysis method is the data that electronic nose and electronic tongues obtain to be inputted DFA model, respectively
According to electronic nose and the DFA of electronic tongues analysis as a result, using contributing maximum 2 characterization factors to respectively obtain two-dimentional shot chart,
Further according to two-dimentional shot chart and various cyclocarya paliurus tea samples registration determine the genuine piece of cyclocarya paliurus tea, adulterant, mix adulterant and
The place of production of cyclocarya paliurus tea.
Preferably, the gas-chromatography flight time mass spectrum combined instrument is LECO PEGASUSBT.
Further, the mass spectrographic detection method of the GC-TOFMS is to choose solid phase micro-extracting head to acquire Mass Spectrometer Method sample
Product are inserted into GC-TOFMS injection port after extraction, and injector temperature is 150~250 DEG C.
Preferably, the sample introduction is Splitless injecting samples, carrier gas He gas, flow velocity 1ml/min, temperature programming, 45 DEG C of holdings
2min, 10 DEG C/min rise to 250 DEG C of holding 10min, and 200 DEG C of ion source temperature, scanning range, 33~450amu, sample volume 0.5
~1.5 μ L.
Further, the CAR/PDMS solid phase micro-extracting head that the solid phase micro-extracting head is 65,75,85 μm, it is described to adopt
The collection time is 5~30min.
Further, the true and false of the cyclocarya paliurus tea refers to that cyclocarya paliurus tea and its adulterant, the quality of the cyclocarya paliurus tea are excellent
The bad cyclocarya paliurus tea for referring to different sources and blue or green money willow mix the differentiation of adulterant.
Compared with prior art, the invention has the benefit that
The discrimination method of cyclocarya paliurus tea provided by the invention is to impregnate in boiling water after first crushing cyclocarya paliurus tea
Sample to be tested is obtained, detects sample to be tested followed by electronic nose and electronic tongues, and PCA and DFA is carried out to testing result and is analyzed,
Comprehensive mirror is carried out to the genuine piece of cyclocarya paliurus tea, adulterant, the place of production for mixing adulterant and cyclocarya paliurus tea in combination with GC-TOFMS mass spectrum
Not.The present invention is analyzed by carrying out PCA and DFA to the data obtained after electronic nose and electronic tongues detection, and combines GC-TOFMS
Mass spectrogram can quickly identify the genuine piece of cyclocarya paliurus tea, adulterant, the place of production for mixing adulterant and cyclocarya paliurus tea, have and know
Bie Dugao, identifies fireballing advantage, effectively alleviates the existing cyclocarya paliurus tea true and false and what the quality place of production was not easy to screen asks
Topic.
Detailed description of the invention
It, below will be to specific in order to illustrate more clearly of the specific embodiment of the invention or technical solution in the prior art
Embodiment or attached drawing needed to be used in the description of the prior art be briefly described, it should be apparent that, it is described below
Attached drawing is some embodiments of the present invention, for those of ordinary skill in the art, before not making the creative labor
It puts, is also possible to obtain other drawings based on these drawings.
Fig. 1 is the cyclocarya paliurus tea e-nose signal response diagram for the common process that the embodiment of the present invention 1 provides；
Fig. 2 is the cyclocarya paliurus tea e-nose signal response diagram that the embodiment of the present invention 1 provides；
Fig. 3 is the cyclocarya paliurus tea GC-TOFMS total ion current figure for 9 kinds of separate sources that the embodiment of the present invention 2 provides；
Fig. 4 is the GC-TOFMS total ion current figure for the adulterant Chinese ash that the embodiment of the present invention 2 provides；
Fig. 5 is cyclocarya paliurus tea, the blue or green money willow prophyll, adulterant that the electronic nose that the embodiment of the present invention 5 provides detects different sources
Chinese ash is analyzed with pseudo- cyclocarya paliurus tea PCA is mixed；
Fig. 6 is that the electronic tongues that the embodiment of the present invention 5 provides detect cyclocarya paliurus tea, adulterant Chinese ash and mix pseudo- cyclocarya paliurus tea PCA
Analysis；
Fig. 7 is that the electronic nose that the embodiment of the present invention 6 provides detects cyclocarya paliurus tea, adulterant Chinese ash and mixes pseudo- cyclocarya paliurus tea DFA
Analysis.
Specific embodiment
Technical solution of the present invention is clearly and completely described below in conjunction with embodiment, it is clear that described reality
Applying example is a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field
Art personnel every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
According to an aspect of the present invention, a kind of discrimination method of cyclocarya paliurus tea, the discrimination method the following steps are included:
Impregnated to obtain sample to be tested in boiling water after cyclocarya paliurus tea is crushed first, followed by electronic nose and electronic tongues detection to
Sample, and PCA and DFA is carried out to testing result and is analyzed, genuine piece, puppet in combination with GC-TOFMS mass spectrum to cyclocarya paliurus tea
Product mix adulterant and the place of production carries out comprehensive identification.
The present invention uses GC-TOFMS mass spectrum to detect cyclocarya paliurus tea first, is tentatively judged by the comparison of mass spectra peak
The true and false of cyclocarya paliurus tea obtains the total ion current figure of cyclocarya paliurus tea according to Mass Spectrometer Method it is found that there are cyclocarya paliurus tea 19 kinds to share
Peak substance (specifically sees below embodiment 2), if 19 kinds of shared peaks of mass spectrogram and this of the cyclocarya paliurus tea of detection are with uniformity,
And without obvious miscellaneous peak be then genuine piece, it is adulterant if not having.
But for partially mixing pseudo- cyclocarya paliurus tea (mixing adulterant), the mass spectra peak in total ion current figure is complex, only
It can not be distinguished well by the map analysis of GC-TOFMS total ion current.Therefore, inventor examines further through electronic nose and electronic tongues
It surveys device to be collected the voltage change pulse data that cyclocarya paliurus tea brews using carrier gas detection method, and to the number obtained after detection
According to carrying out PCA and DFA analysis, it is distributed in by what PCA and DFA analysis can intuitively obtain that cyclocarya paliurus tea sample more concentrates
It analyzes a concentrated area of map, and adulterant and mixes adulterant and differed farther out with the region of cyclocarya paliurus tea, and then to cyclocarya paliurus tea
Genuine piece, adulterant and mix adulterant and intuitively distinguished.Meanwhile it can also be to the green money of different sources by PCA and DFA analysis
Willow tea is further distinguished.It follows that the discrimination method of the application cyclocarya paliurus tea has resolution high, it is fast to identify speed
The advantages of, it effectively alleviates the existing cyclocarya paliurus tea true and false and the quality place of production is not easy the problem of screening.
In the preferred embodiment of the present invention, the smashed partial size of the cyclocarya paliurus tea was 20~100 meshes
Powder.
As a preferred embodiment, the above-mentioned smashed partial size of cyclocarya paliurus tea was the powder of 20~100 meshes,
The powder of 20~100 meshes can more effectively be such that the effective component of cyclocarya paliurus tea is dissolved among sample to be tested.
In the preferred embodiment of the present invention, the step of head space impregnates are as follows: by smashed cyclocarya paliurus tea
It is put into ml headspace bottle, then with the solid-liquid ratio injection boiling water and gland sealed soak of 1:5~50, obtains sample to be tested；
As a preferred embodiment, cyclocarya paliurus tea can be made by carrying out head space immersion with the solid-liquid ratio of 1:5~50
Property material is adequately dissolved in sample to be tested, and then the sample to be tested after making the application carry out head space immersion is when detecting
Data response signal is more strong, in favor of the detection of later period mass spectrum and electronic nose, electronic tongues.
Preferably, the soaking time that the head space impregnates is 5~30min, and heating temperature is 50~80 DEG C；
It is furthermore preferred that the boiling water is the distilled water boiled.
In the preferred embodiment of the present invention, flow rate of carrier gas when being detected using electronic nose to sample is
50~150ml/min, Sample injection volume be 0.5~2ml, 50~100 DEG C of injector temperature, sample acquisition time be 60~
240s, lag time are 60~300s.
As a preferred embodiment, above-mentioned flow rate of carrier gas when being detected using electronic nose to sample be 50~
150ml/min, Sample injection volume are 0.5~2ml, and 50~100 DEG C of injector temperature, sample acquisition time is 60~240s, is prolonged
The stagnant time is that the design parameter of 60~300s can make electronic nose detector is more accurate to cyclocarya paliurus tea to detect.
Preferably, the electronic nose is Alpha Fox4000 electronic nose detector.
It is furthermore preferred that 18 sensors that the electronic nose uses are respectively T30/1, T40/2, T40/1, TA/2, T70/
2, P10/1, P10/2, P40/1, PA/2, P30/1, P40/2, P30/2, LY2/LG, LY2/G, LY2/AA, LY2/GH, LY2/
gCTL、LY2/gCT。
In the preferred embodiment of the present invention, electronic tongues when being detected using electronic tongues to sample are maximum
Voltage is set as 1~5V, and minimum voltage is -5~-1 V, and Sample injection volume is 15~30ml, and the pulse spacing is 100~
300mV。
As a preferred embodiment, above-mentioned electronic tongues maximum voltage when being detected using electronic tongues to sample is set
It is set to 1~5V, minimum voltage is -5~-1 V, and Sample injection volume is 15~30ml, and the pulse spacing is 100~300mV, upper
Electronic tongues can carry out accurate detection analysis to sample to be tested in the range of stating detection parameters, and then be the PCA of next step points
Analysis and DFA analysis are prepared.
Preferably, the electronic tongues are Smart tough electronic tongues detector.
It is furthermore preferred that the sensor that the electronic tongues use is respectively ZZ, AB, GA, BB, CA, DA, JE.
In the preferred embodiment of the present invention, the PCA analysis method are as follows: obtain electronic nose and electronic tongues
Data carry out PCA analysis, are substituted into computer PCA analysis software obtain according to electronic nose and the PCA of electronic tongues analysis result respectively
To two-dimentional shot chart, further according to two-dimentional shot chart and various cyclocarya paliurus tea samples registration determine cyclocarya paliurus tea the true and false and
Mix the place of production of adulterant and cyclocarya paliurus tea.It is genuine piece if the two-dimentional shot chart of cyclocarya paliurus tea to be measured is in same concentration section, such as
Then for adulterant or adulterant is mixed not in above-mentioned section.
In the preferred embodiment of the present invention, the DFA analysis method are as follows: obtain electronic nose and electronic tongues
Data carry out DFA analysis, are substituted into computer DFA analysis software obtain according to electronic nose and the DFA of electronic tongues analysis result respectively
To two-dimentional shot chart, further according to two-dimentional shot chart and various cyclocarya paliurus tea samples registration determine cyclocarya paliurus tea the true and false and
Mix the place of production of adulterant and cyclocarya paliurus tea.It is genuine piece if the two-dimentional shot chart of cyclocarya paliurus tea to be measured is in same concentration section, such as
Then for adulterant or adulterant is mixed not in above-mentioned section.
In the preferred embodiment of the present invention, the mass spectrographic detection method of the GC-TOFMS is that it is micro- to choose solid phase
Extracting head acquires Mass Spectrometer Method sample, is inserted into GC-TOFMS injection port after extraction, and injector temperature is 150~250 DEG C.
In above-mentioned preferred embodiment, the solid phase micro-extracting head is 65,75,85 μm of CAR/PDMS solid phase microextraction
Head, the acquisition time are 5~30min.
Embodiment 1 pre-processes cyclocarya paliurus tea to be measured
Choose the cyclocarya paliurus tea of 9 kinds of different sources, specific producing region is respectively as follows: Hunan cyclocarya paliurus tea, Jiangxi cyclocarya paliurus tea,
Hubei cyclocarya paliurus tea, Guangxi cyclocarya paliurus tea, Sichuan cyclocarya paliurus tea, Guizhou cyclocarya paliurus tea, Anhui cyclocarya paliurus tea, Zhejiang blue or green money willow
Tea, Jiangsu cyclocarya paliurus tea.
Above-mentioned cyclocarya paliurus tea is crushed respectively, smashed partial size was the powder of 40 meshes, then by smashed blueness
Qian Liucha 0.25g is put into ml headspace bottle, is then sealed in 10ml ml headspace bottle with the solid-liquid ratio injection boiling water and gland of 1:15, in advance
Stay head space volume of the total volume 1/2, as 5ml, and 80 DEG C at a temperature of impregnate 30min, sample to be tested is obtained, after progress
Continuous detection；
Fig. 1 is the cyclocarya paliurus tea e-nose signal response diagram of common process that the embodiment of the present invention 1 provides, the figure be without
Above-mentioned process of refinement directly acquires the resulting e-nose signal figure of 0.25g cyclocarya paliurus tea in a manner of commonly making tea；
Fig. 2 is the cyclocarya paliurus tea e-nose signal response diagram that the embodiment of the present invention 1 provides.Blueness money used in Fig. 1 and Fig. 2
Willow tea sample is identical, compares the signal graph of above-mentioned same sample Different front processing method, and electronic nose sensor difference signal is opposite
Obviously.
By above-mentioned Fig. 1 and Fig. 2 it is found that the sample to be tested pre-processed by the application, in 0~30S, electronic nose is rung
Induction signal positive peak has reached 0.6 (Fig. 2), and electronic nose response signal positive peak obtained by common sample processing method only reaches
0.3 (Fig. 1), signal value, which responds bigger electronic nose, more to have an opportunity to obtain preferable differentiation effect.
Wherein, the electronic nose sensor specifically: LY2/LG, LY2/G, LY2/AA, LY2/GH, LY2/ECTL, LY2/
CT、T30/1、P10/1、P10/2、P40/1、T70/2、PA/2。
2 GC-TOFMS Mass Spectrometer Method of embodiment
The cyclocarya paliurus tea of the 9 kinds of different sources provided in embodiment 1 and 2 kinds of adulterated adulterants are subjected to GC-TOFMS matter
Spectrum detection, specific Mass Spectrometry detection method are as follows:
1, acquire sample: the partial size that cyclocarya paliurus tea is ground into crosses the powder of 40 meshes, weighs 0.2g, by the feed liquid of 1:20
Than the distilled water that boils of 4ml is added in sample bottle, gland is sealed immediately after being watered, to prevent fragrance evolution.To blue or green money willow powder
End moves into preheating cabinet after impregnating 30min, adjusts the temperature to 70 DEG C, head space preheats 20min.Choose 75 μ of solid phase microextraction column
MCAR/PDMS carries out head space and acquires sample, acquisition time 20min.
2, it will acquire in sample extracted insertion GC-TOFMS injection port, 0.5 μ L injector temperature of sample volume is 150~
250 DEG C, Splitless injecting samples, carrier gas He gas, flow velocity 1ml/min, temperature programming, 45 DEG C of holdings 2min, 10 DEG C/min rise to 250 DEG C
Keep 10min, 200 DEG C of ion source temperature, scanning range, 33~450amu, shown in specific testing result Fig. 3.
Fig. 3 is the cyclocarya paliurus tea GC-TOFMS total ion current figure of 9 kinds of separate sources.As shown in figure 3, result is established with 19
Shared peak is characterized gas-chromatography-flight time mass spectrum finger-print of finger print information.Referring to NIST spectrum library to being measured
The gas phase map of cyclocarya paliurus tea sample carries out the determination of shared peak substance, obtains wherein 19 kinds of shared peak substances, is cyclocarya paliurus tea
Property material component, it is specific as follows:
The Chinese Wingmut Leaf that adulterant is shape function similar but inactive to Qingqian Willow leaf is mixed in artificial setting, and specific sample is adulterated
50% Chinese ash and 100% Chinese ash.
The GC-TOFMS total ion current figure for the adulterated adulterant Chinese ash that Fig. 4 embodiment of the present invention 2 provides.Map solution is carried out to it
Analysis, does not find the property material same substance with cyclocarya paliurus tea.
By the Contrast analysis to Fig. 3 and Fig. 4, what can be will be apparent that distinguishes blue or green money willow and adulterated adulterant Chinese ash,
This result shows that the cyclocarya paliurus tea property material that the present invention chooses can represent the characteristic attribute of cyclocarya paliurus tea well, by its with mix
False object distinguishes well.But the cyclocarya paliurus tea adulterated for part only passes through GC-TOFMS total ion current map analysis can not
Obtain specific adulterated content and mix adulterant type, it is also necessary to by PCA analysis (principal component analysis) and DFA analysis (differentiation because
Son analysis) carry out comprehensive descision.
The detection of 3 electronic nose of embodiment
The cyclocarya paliurus tea of different sources and the Chinese ash of Bu Tong adulterated ratio are crushed respectively, smashed partial size was 20 mesh
Smashed cyclocarya paliurus tea 0.4g is then put into ml headspace bottle by the powder of sieve, then simultaneously with the solid-liquid ratio injection boiling water of 1:15
Gland is sealed in 10ml sample bottle, reserve head space volume of the total volume 1/3, and 80 DEG C at a temperature of impregnate 20min, obtain
To sample to be tested.Then it is measured with Alpha Fox4000 electronic nose, in Alpha Fox4000 electric nasus system software
Set detection parameters are as follows: flow rate of carrier gas: 150ml/min, injection needle temperature: 60 DEG C, volume injected: 1ml, 80 DEG C of injector temperature.
Sample acquisition time: 120s, lag time: 200s.
The electronic nose is Alpha Fox4000 electronic nose detector.18 sensors difference that the electronic nose uses
For T30/1, T40/2, T40/1, TA/2, T70/2, P10/1, P10/2, P40/1, PA/2, P30/1, P40/2, P30/2, LY2/
LG、LY2/G、LY2/AA、LY2/GH、LY2/gCTL、LY2/gCT。
The detection of 4 electronic tongues of embodiment
Cyclocarya paliurus tea and adulterated Chinese ash are crushed respectively, smashed partial size was the powder of 20 meshes, will then be crushed
Cyclocarya paliurus tea 1g afterwards is put into ml headspace bottle, is then sealed in sample bottle with the solid-liquid ratio injection boiling water and gland of 1:20, in advance
Stay head space volume of the total volume 1/2, and 70 DEG C at a temperature of impregnate 20min, obtain sample to be tested.Then it uses
Smarttough electronic tongues are measured, and set detection parameters in electronic tongue system software are as follows: sampling volume 15ml, maximum voltage
1V, minimum voltage -1V, pulse spacing 100MV, sensitivity 10- 4~-6。
The electronic tongues are Smart tough electronic tongues detector.Electricity when being detected using electronic tongues to sample
Sub- tongue maximum voltage is set as 1~5V, and minimum voltage is -5~-1V, and Sample injection volume is 15~30ml, and the pulse spacing is
100~300mV.
5 PCA of embodiment analysis
Different sources blue or green money willow sample and the electronic nose of adulterated Chinese ash, electronic tongues detection data are subjected to PCA analysis, PCA
Analyzing (principal component analysis) is that one kind is usually used in Data Dimensionality Reduction, and solves the Multivariable Statistical Methods of linear problem.This method is logical
Generation new variables is crossed instead of original incoherent variable, and carry out dimensionality reduction by linear combination data, simplifies acquisition data set
In all variable informations task.Under normal conditions, some new variables, referred to as principal component (PCs), can explain former variable
Therefore data information only considers multiple principal components, high dimensional data can be reduced to a lower dimension, and data information
It loses small.Current this technology is widely used in data processing.The present invention is applied to the analysis of cyclocarya paliurus tea, can
Intuitively to show that the cyclocarya paliurus tea of different sources more concentrates on a region, thus mixing cyclocarya paliurus tea and different content
Adulterant distinguishes, and concrete analysis result is as shown in Figure 5, Figure 6:
Fig. 5 is PCA of the electronic nose to the detection data of blue or green money willow prophyll, different sources cyclocarya paliurus tea sample and adulterated Chinese ash
Analysis chart, PCA is analyzed on result X-Y scheme as can be seen that electronic nose can carry out different sources cyclocarya paliurus tea with pseudo- Chinese ash tea is mixed
It is effective to distinguish, the above-mentioned non-overlapping phenomenon of sample.Visual result shows that the cyclocarya paliurus tea of different sources more concentrates on an area
Domain, energy is obvious and mixes pseudo- 50% Chinese ash, 100% Chinese ash tea distinguishes, and the contribution rate of accumulative total of bidimensional principal component reaches before PCA
97.352%.
Wherein, it 1~9 is embodied as in described Fig. 5: 1 Jiangxi cyclocarya paliurus tea, 2 Hubei cyclocarya paliurus teas, 3 Guangxi blueness money
Willow tea, 4 Sichuan cyclocarya paliurus teas, 5 Guizhou cyclocarya paliurus teas, 6 Anhui cyclocarya paliurus teas, 7 blue or green money willow prophylls, 8 adulterant Chinese ash 100%, 9 are mixed
False 50% Chinese ash.
It, can be with as shown in fig. 6, Fig. 6 is electronic tongues to the PCA analysis chart of the detection data of blue or green money willow sample and adulterated Chinese ash
Find out that electronic tongues to cyclocarya paliurus tea and can mix pseudo- Chinese ash tea and effectively be distinguished, the above-mentioned non-overlapping phenomenon of sample.Visual result
Show that cyclocarya paliurus tea more concentrates on a region, energy is obvious and mixes pseudo- 50% Chinese ash, 100% Chinese ash tea distinguishes, PCA
The contribution rate of accumulative total of preceding bidimensional principal component has reached 90.24%.
6 DFA of embodiment analysis
The electronic nose detection data of different sources blue or green money willow sample and adulterated Chinese ash is subjected to DFA analysis, DFA analysis (is sentenced
Other factorial analysis) it is to calculate on the basis of based on priori data classification the boundary between inhomogeneity, so that side between class
Poor maximum and each variance within clusters are minimum.So maximise being capable of maximum difference between Display Group for this linear combination mode
Dimension contribution rate.In this way, the data under same data set with heterogeneity meaning can effectively be distinguished.Mesh
Before, this technology is widely used in complicated data analysis.The present invention is applied to the analysis of cyclocarya paliurus tea, can intuitively see
Adulterated cyclocarya paliurus tea differs farther out with the region of known cyclocarya paliurus tea out, thus to mixing adulterant and mixing the ratio progress area of adulterant
Point, concrete analysis result is as shown in Figure 7:
Fig. 7 be electronic nose to cyclocarya paliurus tea, adulterated 50% Chinese ash and 100% Chinese ash detection data DFA analysis chart,
It can be seen that electronic nose distinguishes three kinds of difference tea sample DFA, effect is also preferable, adulterated cyclocarya paliurus tea and known cyclocarya paliurus tea
Region differs farther out.The contribution rate of accumulative total of bidimensional principal component has reached 99.993% before DFA, can understand and intuitively distinguish
True and false cyclocarya paliurus tea.
In conclusion the present invention uses GC-TOFMS mass spectrum to detect cyclocarya paliurus tea first, pass through pair of mass spectra peak
Than the true and false for tentatively judging cyclocarya paliurus tea, the total ion current figure of cyclocarya paliurus tea is obtained it is found that blue or green money willow tea set according to Mass Spectrometer Method
There are 19 kinds of shared peak substances (referring specifically to embodiment 2), if the mass spectrogram of the cyclocarya paliurus tea of detection has with this 19 kinds shared peaks
There is consistency, and be then genuine piece without obvious miscellaneous peak, is adulterant if not having.But it (is mixed for partially mixing pseudo- cyclocarya paliurus tea
Adulterant), the mass spectra peak in total ion current figure is complex, only can not be good by the map analysis of GC-TOFMS total ion current
It distinguishes.Therefore, the voltage that inventor brews cyclocarya paliurus tea using carrier gas detection method further through electronic nose and electronic tongues detector
Change pulse data are collected, and are carried out PCA and DFA to the data obtained after detection and analyzed, can by PCA and DFA analysis
Intuitively to obtain the concentrated area for being distributed in analysis map that cyclocarya paliurus tea sample more concentrates, and adulterant and mix adulterant
It is differed farther out with the region of cyclocarya paliurus tea, and then the genuine piece to cyclocarya paliurus tea, adulterant and mixes adulterant and intuitively distinguished.Together
When, by PCA and DFA analysis can also the cyclocarya paliurus tea to different sources further distinguished.It follows that the application
The discrimination method of cyclocarya paliurus tea has resolution high, identifies fireballing advantage, effectively alleviates the existing cyclocarya paliurus tea true and false
And the quality place of production is not easy the problem of screening.
Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations；To the greatest extent
Pipe present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: its according to
So be possible to modify the technical solutions described in the foregoing embodiments, or to some or all of the technical features into
Row equivalent replacement；And these are modified or replaceed, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution
The range of scheme.
Claims (10)
1. a kind of discrimination method of cyclocarya paliurus tea, which is characterized in that the discrimination method is the following steps are included: first by blue or green money willow
It is impregnated to obtain sample to be tested in boiling water after tea powder is broken, detects sample to be tested followed by electronic nose and electronic tongues, and right
Testing result carry out PCA and DFA analysis, in combination with GC-TOFMS mass spectrum to the genuine piece of cyclocarya paliurus tea, adulterant, mix adulterant and
The place of production of cyclocarya paliurus tea carries out comprehensive identification.
2. the discrimination method of cyclocarya paliurus tea according to claim 1, which is characterized in that the smashed grain of cyclocarya paliurus tea
Diameter was the powder of 20~100 meshes.
3. the discrimination method of cyclocarya paliurus tea according to claim 1, which is characterized in that the step of the immersion are as follows: by powder
Cyclocarya paliurus tea after broken is put into ml headspace bottle, then with the solid-liquid ratios of 1:5~50 injection boiling water and gland sealed soak, obtain to
Sample；
Preferably, the soaking time of the immersion is 5~30min, and heating temperature is 50~80 DEG C；
Preferably, the boiling water is the distilled water boiled.
4. the discrimination method of cyclocarya paliurus tea according to claim 1, which is characterized in that it is described using electronic nose to sample into
Row detection when flow rate of carrier gas be 50~150ml/min, Sample injection volume be 0.5~2ml, 50~100 DEG C of injector temperature, sample
Acquisition time is 60~240s, and lag time is 60~300s；
Preferably, the electronic nose is Alpha Fox4000 electronic nose detector.
5. the discrimination method of cyclocarya paliurus tea according to claim 1, which is characterized in that it is described using electronic tongues to sample into
Electronic tongues maximum voltage is set as 1~5V when row detection, and minimum voltage is -5~-1V, and Sample injection volume is 15~30ml, arteries and veins
100~300mV is divided between punching；
Preferably, the electronic tongues are Smart tough electronic tongues detector.
6. the discrimination method of cyclocarya paliurus tea according to claim 1, which is characterized in that the PCA analysis method are as follows: will be electric
The data that sub- nose and electronic tongues obtain input pca model, respectively according to electronic nose and the PCA of electronic tongues analysis as a result, using tribute
It offers maximum 2 principal components and respectively obtains two-dimentional shot chart, further according to being overlapped for two-dimentional shot chart and various cyclocarya paliurus tea samples
Spend the genuine piece for determining cyclocarya paliurus tea, adulterant, the place of production for mixing adulterant and cyclocarya paliurus tea.
7. the discrimination method of cyclocarya paliurus tea according to claim 1, which is characterized in that the DFA analysis method are as follows: will be electric
The data that sub- nose and electronic tongues obtain input DFA model, respectively according to electronic nose and the DFA of electronic tongues analysis as a result, using tribute
It offers maximum 2 characterization factors and respectively obtains two-dimentional shot chart, further according to the weight of two-dimentional shot chart and various cyclocarya paliurus tea samples
The genuine piece of right determining cyclocarya paliurus tea, adulterant, the place of production for mixing adulterant and cyclocarya paliurus tea.
8. the discrimination method of cyclocarya paliurus tea according to claim 1, which is characterized in that the mass spectrographic detection of GC-TOFMS
Method are as follows: choose solid phase micro-extracting head and acquire Mass Spectrometer Method sample, be inserted into GC-TOFMS injection port after extraction, injector temperature is
150~250 DEG C.
9. the discrimination method of cyclocarya paliurus tea according to claim 8, which is characterized in that the GC-TOFMS mass spectrometer
For LECO PEGASUSBT.
10. the discrimination method of cyclocarya paliurus tea according to claim 8, which is characterized in that the solid phase micro-extracting head is
CAR/PDMS solid phase micro-extracting head, the acquisition time are 5~30min.
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Application publication date: 20190614 |