CN106442590A - Method for identifying tea leaf quality by adopting energy dispersion X-fluorescence light spectrum fingerprint identification technology - Google Patents
Method for identifying tea leaf quality by adopting energy dispersion X-fluorescence light spectrum fingerprint identification technology Download PDFInfo
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- CN106442590A CN106442590A CN201610528731.2A CN201610528731A CN106442590A CN 106442590 A CN106442590 A CN 106442590A CN 201610528731 A CN201610528731 A CN 201610528731A CN 106442590 A CN106442590 A CN 106442590A
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- camelliae sinensis
- folium camelliae
- tea
- tea leaf
- fingerprint
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/223—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/05—Investigating materials by wave or particle radiation by diffraction, scatter or reflection
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/60—Specific applications or type of materials
- G01N2223/612—Specific applications or type of materials biological material
Abstract
The invention provides a method for identifying tea leaf quality by adopting an energy dispersion X-fluorescence light spectrum fingerprint identification technology. The method comprises the following steps: (1) taking tea leaf genuine products or authentic tea leaves to prepare a sample; carrying out Omnian none-standard quantitative full-spectrum analysis on tea leaves to obtain types and semi-quantitative contents of elements in the tea leaves; (2) establishing a tea leaf fingerprint identification method according to data obtained by the step (1); (3) carrying out energy dispersion X-fluorescence spectrometry measurement on a plurality of tea leaf genuine products or authentic tea leaf products, and establishing a standard fingerprint spectrum base of the tea leaf genuine products or the authentic tea leaves; (4) preparing a tea leaf sample to be detected into a sample, and carrying out the energy dispersion X-fluorescence spectrometry measurement to obtain a fingerprint spectrum; carrying out similarity threshold judgment on the fingerprint spectrum and the standard fingerprint spectrum base, so as to obtain an identifying result of the tea leaves. The method provided by the invention provides convenience for work including on-site rapid screening of the tea leaves, port market supervision and control, quality control on products of tea leaf enterprises and the like.
Description
Technical field
The present invention relates to a kind of method that employing fingerprint pattern technology differentiates tea leaf quality, especially relates to one kind and adopts energy
The method that chromatic dispersion quantity X fluorescence spectrum fingerprint identification technology differentiates tea leaf quality.
Background technology
China is the native place of tea, in Folium Camelliae sinensis containing multiple antioxidant, antioxidants and multivitamin and
Aminoacid, greasy to edible vegetable oil solution, strengthen neural excitation and the diuresis tool that helps digestion has certain effect, with health-care effect, because
This, it is the traditional dining culture of China to drink tea.Chinese tea is divided into green tea, black tea, oolong tea, scented tea, a small bay in a river according to manufacture method
A few big class such as tea, brick tea, include many kinds again in all kinds of tea.For its processing method, tea can be divided into three major types：Green tea,
Or claim unfermentable tea；Black tea, or claim the tea of fermentation；The tea of half-fermented, has two kinds of properties of green tea and black tea concurrently.
In China in 2015（Guangzhou）In tea theme auction, Ramulus et Folium Mussaendae Pubescentis price such as gold, old tea price crosses gold.By
Ordering about in interests, in recent years domestic tea market spread out of the message of fake and forged Folium Camelliae sinensis, such as " many tea art houses in frequent succession
Doubt and use fake and inferior Folium Camelliae sinensis ", " selecting white sand green tea dining room Shanghai south green tea ", " Biluochun tea of CCTV's exposure ", " reporter's real name is lifted
Fake and forged Folium Camelliae sinensis problem of report " etc..Tea business knows perfectly well in violation of rules and regulations, falsely uses his Moral quality card still with loose tea inferior, is packaged into
Brand tea flows to market.Some coffee-houses, tea art house, teahouse, restaurant, hotel etc. are then using these are cheap, be accused of vacation
The Folium Camelliae sinensis for emitting poor quality are sold goods at a high figure again to customer, and this has formed the interests chain of a Lycoperdon polymorphum Vitt, and has been accused of violating China《Product
Mass method》《Law on Protection of the Rights and Interests of Consumers》And《The Law of the People's Republic of China Against Competition by Inappropriate Means》.In the face of true and false Folium Camelliae sinensis, ordinary consumer almost distinguish by difficulty
The true and false.
It is reported that, Folium Camelliae sinensis subdivision kind in the market has thousands of kinds, and is applied to all Folium Camelliae sinensis qualities of discriminating
Universal method.Because tea-leaf producing area, processing technology, kind are different with personal taste, high Folium Camelliae sinensis of price and low-cost
Folium Camelliae sinensis can not simply contrast quality.Relevant departments are sent to after typical tea leaves sampling to check, emphasis inspection Pesticide Residues in Tea,
The indexs such as content of beary metal.The laboratory inspection means of Folium Camelliae sinensis real and fake discrimination or method are not reported so far, and lack corresponding
Monitoring specification, does not more list national standard detection method in, is not formally applied in inspection.
Finger printing refers to sample after proper treatment, and using certain analysis method and means, obtained can mark
Show the total peak figure spectrum of its feature, in order to control sample quality and cultivar identification.The foundation of finger printing should be with the correlation of system
Chemical constitution study embodies systematicness, characteristic and three basic principles of stability for relying on, it is ensured that the standardization of finger printing,
Standardize, objectify consequently facilitating promotion and application.
The fingerprint pattern technology of similar research, predominantly obtains component colony using the technology such as spectrum and chromatograph both at home and abroad
Characteristic spectrum or image, and with reference to computer technology, the data for being obtained is analyzed, by appropriate data processing method
" filtration " being carried out to collection of illustrative plates and is simplified, obtains exclusive, stable, practical characteristic, so as to differentiate to the true and false of product
And product quality is controlled.Finger printing can be divided into product chemistry (composition) finger printing and product by mensuration means classification
Product biofingerprint, and chemical（Composition）Finger printing apply in terms of product formulation analysis and research particularly extensive, according to
Concrete grammar used in research is different from technology, mainly has thin layer chromatography (TLC), high performance liquid chromatography
(HPLC), gas chromatography (GC), high-performance capillary electrophoresis method (HPCE), high performance countercurrent chromatography method (HSCCC), X-ray
Diffraction approach (XRD), X-ray fluorescence spectroscopy (XRF) etc..Meanwhile, multiple techniques is current most valued means, HPLC/MS,
The multiple techniques such as HPLC/UV, HPLC/NMC, HPLC/MS/MS bring brand-new prospect to product analyses, and finger printing also reaches
To multidimensional, multi information stage.
The digitized of the processing method product fingerprint collection of illustrative plates of finger printing information can scientifically carry out the comparison of collection of illustrative plates, real
By means of Chemical Measurement and computer technology, the numeral of digitized battlefield environment is compiled into software for using in the application of border.
At present the computer analyzing method of finger printing have artificial neural network method, Euclidean distance, absolute distance, Minkowsky distance,
Correlation coefficient process, peak match degree and Cosin method etc..
Energy translation spectrum（EDXRF）Technology, is to carry out sample irradiation by using X-ray and realize exciting, sample
Various elements present in product discharge fluorescent X-ray after illuminated, present the different-energy feature of existing element, right
Analysis object X-ray is identified and counts.The development of more than 60 year is experienced, X-ray fluorescence spectra analytical technology is in various sections
Grind and be widely used with industrial circle, and develop to deeper field.Dutch PANalytical instrument company head in 2011
Secondary by finger printing software engineering introduce energy color dispersing X fluorescent spectrometer (EDXRF), be currently the only with fingerprint identification technology
EDXRF, predominantly rely on the various software modules such as quick fingerprint identification technology, the analysis of advanced no mark to strengthen its function.Mesh
Before, the country has no that the fingerprint pattern technology of application EDXRF is traced to the source and carry out quick finger printing to the true and false of tea products or the place of production
Differentiate.
Content of the invention
The present invention provides a kind of method that employing energy translation spectral fingerprint technology of identification differentiates tea leaf quality, should
Method can be used to differentiate that the true and false of Folium Camelliae sinensis and the place of production are traced to the source discriminating.
The purpose of the present invention is realized by following technical measures：One kind adopts energy translation spectral fingerprint
The method that technology of identification differentiates tea leaf quality, which comprises the following steps：
(1) Folium Camelliae sinensis genuine piece or genuine Folium Camelliae sinensis sample preparation are taken, Omnian no scalar quantity analysis Folium Camelliae sinensis, obtain chemical element class in Folium Camelliae sinensis
Other and sxemiquantitative content；
(2) according to the data of step (1) gained, characteristic chemical element in Folium Camelliae sinensis is selected, sets up Folium Camelliae sinensis fingerprint identification method；
(3) taking multiple Folium Camelliae sinensis genuine pieces or genuine Tea Samples carries out energy translation spectroscopy measurements, obtains Folium Camelliae sinensis genuine piece
Or the element data of genuine Folium Camelliae sinensis set up the standard fingerprint map library of Folium Camelliae sinensis genuine piece or genuine Folium Camelliae sinensis；
(4) Tea Samples sample preparation to be measured is taken, and finger printing is obtained using energy translation spectroscopy measurements, with standard fingerprint
Spectrum library carries out similarity threshold judgement, and the true and false and the place of production so as to obtain Folium Camelliae sinensis is traced to the source identification result.
In the present invention, in step (1) and (4), Folium Camelliae sinensis sample making course is：Folium Camelliae sinensis are size-reduced, mixing, take 5-7 gram of tea-leaf power
The print of a diameter of 40mm is pressed under 4 tons of pressure.
The Folium Camelliae sinensis fingerprint identification method of step (2) is：
In step (3) of the present invention or (4), the measuring condition of energy translation spectrographic method is：
In step (5), Folium Camelliae sinensis atlas analysis adopt artificial spectrum unscrambling, comprising unit have Mg, Al, Si, P, S, Cl, Ar, K,
Ca, Mn, Fe, Cu, Zn, Br, Rb, Sr, Rh, Ag etc.；Folium Camelliae sinensis similarity threshold is using the Chi2 system of the X 2 test in statistics
Meter regression Calculation method, 0<chi2<2 is equivalent or similar；2<chi2<3 be with similarity；chi2>3 for not being equal to.
The present invention has following remarkable result compared with prior art：
(1) present invention is provided employing energy translation spectrum fingerprint identification quick discriminating Folium Camelliae sinensis real and fake discrimination or product
The method traced to the source, realize instrument work station and Folium Camelliae sinensis differentiated automatically, compared with prior art, the technology of the present invention has letter
Just quick, detection cycle is short, environmental protection and energy saving, nondestructive measurement, the superiority such as single-minded, exclusive, be Folium Camelliae sinensis on-site quick screening, port
The work such as market surpervision, tea-enterprise product Quality Control provide convenient method.
(2) chemical element of the present invention is the distinguishing indexes technology of finger printing, have full spectrogram Fitting Analysis identification function and
Chi2 automatic identification statistical method, can be different from the organic compound fingerprint image of prior art without the need for spectrum unscrambling or artificial spectrum unscrambling
Spectral technology, can quick and precisely recognize different brands and the close similar Folium Camelliae sinensis of generic outward appearance, fill up domestic and international correlation technique
Blank.
(3) present invention is realized complete using an equipment using the characteristic chemical element of product as single-minded, specificity index
Become finger printing technology of identification, with existing multiple devices, multiple detection meanss, multiclass statistical software conjoint analysis technology phase
Than with superioritys such as on-site quick screening, simple and efficient, nondestructive measurement, environmental protection and energy saving.
(4) the quick finger printing differential method of EDXRF of the present invention, detection cycle is short, high working efficiency.Sample preparation and survey
Measure simple, quick, safe, lossless and low power consuming, it is not necessary to loaded down with trivial details sample pre-treatments, it is not necessary to expensive standard substance and use
Chemical reagent, sample preparation is simple, strong applicability, be easy to grasp.Application.
Description of the drawings
Fig. 1 is the Folium Camelliae sinensis finger printing of the present invention；
Fig. 2 is the Folium Camelliae sinensis fingerprint databases of the present invention；
Fig. 3 is the same Folium Camelliae sinensis genuine piece of the present invention and sample finger printing comparison diagram.
Specific embodiment
Following examples are used merely to explain the present invention, and protection scope of the present invention is not intended to be limited to following enforcement
Example.The those of ordinary skill of the technical field all can achieve the purpose of the present invention according to disclosure above.
Energy translation spectrum（EDXRF）Technology, carries out sample irradiation by using X-ray and realizes exciting, sample
Present in various elements discharge fluorescent X-ray after illuminated, present the different-energy feature of existing element, to point
Analysis object X-ray is identified and counts.Finger printing software engineering is introduced by Dutch PANalytical instrument company first within 2011
Energy color dispersing X fluorescent spectrometer（EDXRF）, it is the currently the only EDXRF with fingerprint identification technology, predominantly relies on quick
The various software modules such as fingerprint identification technology, advanced no mark analysis strengthen its function.The finger printing of instrument configuration of the present invention
Technology is mainly Chi2 statistical regression calculating method, i.e. X 2 test technology (Chi-square test/Chi-Square
Goodness-of-Fit Test).X 2 test is a kind of very wide hypothesis testing method of purposes, and it counts in group data
Application in deduction, including two rates or two X 2 tests for constituting frequently relatively；Multiple rates or multiple compositions compare card relatively
Correlation analysiss of side's inspection and group data etc..X 2 test is between the actual observed value of statistical sample and theoretical implications value
Departure degree, departure degree between actual observed value and theoretical implications value determines the size of chi-square value, and chi-square value is bigger, more
Do not meet, deviation is less；Chi-square value is less, more tends to meeting；If value is essentially equal, chi-square value is zero, shows theory
Value is complied fully with.Application EDXRF carries out Unmarked word to lightweight secondary element, intermediate mass element and heavy secondary element in Folium Camelliae sinensis standard
Quantitative full spectral element analysis, under multiple different measuring conditions, finds the general character of the content distribution of elements, difference during Folium Camelliae sinensis are composed entirely
Property, characteristic, single-minded, specificity etc.；In application instrument, quick fingerprint identification software module, sets up all kinds of Folium Camelliae sinensis genuine pieces（Standard
Product）Master pattern EDXRF fingerprint databases Folium Camelliae sinensis spectrum storehouse；By the judgement to characteristic spectrum similarity threshold Chi2, right
The result of Sample Scan measurement is compared, and so as to carry out differentiating to the true and false of tea products, the place of production is traced to the source or to product quality
It is monitored.
Embodiment one
(1) Folium Camelliae sinensis genuine piece（Standard substance）Sample preparation
Take appropriate genuine piece（Standard substance）Tea Samples crush, mix, weigh 6 grams of samples be pressed under 2 tons of pressure a diameter of
The print of 40mm.The sample preparation time of each sample is below 5min.
（2）Omnian quantitative analysis of non-sampler Folium Camelliae sinensis
The instrument condition of Omnian quantitative analysis of non-sampler is shown in Tables 1 and 2, and the time of measuring of each sample is 13min.Choose tool
Representational Tea Samples, application no scalar quantity analysis software, full spectrogram scanning, one-point measurement, thickness school is carried out to sample
Just, the correction of fluorescence geometric effect, automatically selects calibration trace etc., obtains genuine piece（Standard substance）Element species and contain in Tea Samples
Amount scope（Table 3-1 ~ table 3-3）.
(3）Set up Folium Camelliae sinensis fingerprint identification method
In above-mentioned steps（2）Omnian Unmarked word quantitative result in, select sample in distinctive element, set up Folium Camelliae sinensis
The method of fingerprint recognition（Table 4）, the time of measuring of each sample is 3min.
（4）Set up Folium Camelliae sinensis fingerprint recognition parameter
Genuine piece (standard substance) Tea Samples are taken, using the method repeated measure three times of fingerprint recognition table 4, application EDXRF optimizes choosing
Measurement parameter is selected, sets up the measuring condition of Folium Camelliae sinensis fingerprint recognition（Table 5）.And it is being measured as under non-measured parameter to work as measuring condition
Abnormal prompt, such as measuring condition：Conditional name<5KVnone >, when voltage is 5KV, electric current is 480uA；Conditional name<
Cl-V >, when voltage is 12KV, electric current is 48uA；Conditional name<Mo-Sb>, when voltage is 50KV, electric current is 7uA, to measure
There is abnormal prompt.
（5）Measurement Folium Camelliae sinensis genuine piece（Standard substance）, set up Folium Camelliae sinensis standard substance fingerprint databases
From totally 57 Tea Samples of multiple brands both at home and abroad, the Folium Camelliae sinensis standard finger-print under 3D state is established（Fig. 1）With
Folium Camelliae sinensis standard diagram storehouse（Fig. 2）.
（6）Method according to step (1) prepares Tea Samples to be measured.
（7）The identification measurement of energy translation spectral fingerprint is carried out using the condition of step (5) to Tea Samples to be measured,
Obtain the finger printing of Tea Samples to be measured.
（8）Folium Camelliae sinensis atlas analysis and determination similarity threshold
Folium Camelliae sinensis atlas analysis adopt artificial spectrum unscrambling, comprising unit have Mg, Al, Si, P, S, Cl, Ar, K, Ca, Mn, Fe, Cu, Zn,
Br, Rb, Sr, Rh, Ag etc..Application chi2 comparison standard diagram and sample collection of illustrative plates（Fig. 3）, Folium Camelliae sinensis similarity threshold is using system
The Chi2 statistical regression calculating method of the X 2 test in meter, similarity threshold is set as 3.0<chi2<2 is equivalent or similar；2
<chi2<3 be with similarity；chi2>3 for not being equal to.
Claims (5)
1. a kind of method that employing energy translation spectral fingerprint technology of identification differentiates tea leaf quality, is characterized in that, including with
Lower step：
(1) Folium Camelliae sinensis genuine piece or genuine Folium Camelliae sinensis sample preparation are taken, Omnian no scalar quantity analysis Folium Camelliae sinensis, obtain chemical element class in Folium Camelliae sinensis
Other and sxemiquantitative content；
(2) according to the data of step (1) gained, characteristic chemical element in Folium Camelliae sinensis is selected, sets up Folium Camelliae sinensis fingerprint identification method；
(3) taking multiple Folium Camelliae sinensis genuine pieces or genuine Tea Samples carries out energy translation spectroscopy measurements, obtains Folium Camelliae sinensis genuine piece
Or the element data of genuine Folium Camelliae sinensis set up the standard fingerprint map library of Folium Camelliae sinensis genuine piece or genuine Folium Camelliae sinensis；
(4) Tea Samples sample preparation to be measured is taken, and finger printing is obtained using energy translation spectroscopy measurements, with standard fingerprint
Spectrum library carries out atlas analysis, judges to obtain the true and false of Folium Camelliae sinensis by similarity threshold and the place of production is traced to the source identification result.
2. the method that employing energy translation spectral fingerprint technology of identification according to claim 1 differentiates tea leaf quality,
It is characterized in that, in the present invention, in step (1) and (4), Folium Camelliae sinensis sample making course is：Folium Camelliae sinensis are size-reduced, mix, take 5-7 gram of tea-leaf power
It is pressed into the print of a diameter of 40mm.
3. the method that employing energy translation spectral fingerprint technology of identification according to claim 1 differentiates tea leaf quality,
It is characterized in that, the Folium Camelliae sinensis fingerprint identification method of step (2) is：
(1) passage/title K, measuring sequence 3, spectral line title KA, conditional name Cl-V, time of measuring 60s；
(2) passage/title Rh, measuring sequence 1, spectral line title KAC, conditional name Mo-Sb, time of measuring 60s；
(3) passage/title Rh, measuring sequence 2, spectral line title LA, conditional name 5KVnone, time of measuring 60s.
4. the method that employing energy translation spectral fingerprint technology of identification according to claim 1 differentiates tea leaf quality,
It is characterized in that, in step (3) or (4), the measuring condition of energy translation spectrographic method is：
(1) conditional name：5KVnone, voltage：5.000 KV, electric current：1020uA, filter：None, gas：Helium, inspection
Survey pattern：High-resolution, application type：Normality；
(2) conditional name：Cl-V, voltage：12.000 KV, electric current：570uA, filter：Al-50, gas：Air, detection
Pattern：Normally, application type：Normality；
(3) conditional name：Mo-Sb, voltage：50.000 KV, electric current：65uA, filter：Ag, gas：Air, detects mould
Formula：Normally, application type：Normality.
5. the method that employing energy translation spectral fingerprint technology of identification according to claim 1 differentiates tea leaf quality,
It is characterized in that, in step (5), Folium Camelliae sinensis atlas analysis adopt artificial spectrum unscrambling；Folium Camelliae sinensis similarity threshold is using in statistics
The Chi2 statistical regression calculating method of X 2 test, 0<chi2<2 is equivalent or similar；2<chi2<3 be with similarity；chi2>3
For not being equal to.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106951458A (en) * | 2017-02-24 | 2017-07-14 | 陈智锋 | A kind of product ontology is traced to the source Jianzhen's method for anti-counterfeit and system |
| CN115684316A (en) * | 2022-11-08 | 2023-02-03 | 广州市中耕信息技术有限公司 | Odor identification method of bionic electronic nose based on MOS gas sensor array |
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2016
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| CN101158657A (en) * | 2007-11-12 | 2008-04-09 | 浙江大学 | Tea-leaf producing area identification method based on x-ray fluorescence technology |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106951458A (en) * | 2017-02-24 | 2017-07-14 | 陈智锋 | A kind of product ontology is traced to the source Jianzhen's method for anti-counterfeit and system |
| CN115684316A (en) * | 2022-11-08 | 2023-02-03 | 广州市中耕信息技术有限公司 | Odor identification method of bionic electronic nose based on MOS gas sensor array |
| CN115684316B (en) * | 2022-11-08 | 2023-12-22 | 中耕生态环境科技(广州)有限公司 | Smell recognition method of bionic electronic nose based on MOS gas sensor array |
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Application publication date: 20170222 |