CN105628780B - A kind of Production area recognition method of flat tea - Google Patents
A kind of Production area recognition method of flat tea Download PDFInfo
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Abstract
A kind of Production area recognition method of flat tea, it is characterised in that：The recognition methods establishes discrimination model respectively by measuring the tealeaves rare earth element content of different sources, and the rare earth element content discrimination model then measured in the Tea Samples in the unknown place of production judges its place of production.The Production area recognition technology model, by back substitution inspection and cross validation, it is 84.8% that back substitution inspection correct decision rate, which is 92.93% cross validation differentiation rate, can preferably distinguish the place of production of different flat teas.
Description
Technical field
The invention belongs to rapid test paper identification technologies, and in particular to a kind of tea Production area recognition side based on rare earth element
Method.
Background technology
Longjing tea is the trizonal famous local distinguishing products in Zhejiang, is divided into Xihu Longjing Tea, money pool Dragon Well tea and more state is imperial
Well, by the protection of place of origin, since the benefit of Longjing tea especially West Lake Dragon Well tea is preferable always, there is hair in when event being counterfeited
Raw, but the shape of many flat teas and processing technology are almost the same with Longjing tea, people can not with the naked eye its place of production of Direct Recognition
Source, there is an urgent need for research and development the place of production trace to the source with mirror method for distinguishing to protect place of production brand.In recent years, more and more researchs, which use, refers to
Line collection of illustrative plates carries out the place of production to tealeaves and traces to the source, and common technology has HPLC near infrared spectrums, ICP-MS etc..Have researcher and uses ICP-
Multiple element content in the means analysis such as MS/AES tealeaves, with principal component analysis（PCA）, linear discriminant analysis（FLD）, it is poly-
Alanysis（CA）, Stepwise Discriminatory Analysis, artificial neural network（ANN）The methods of tealeaves differently is differentiated, but at present
The Production area recognition detection method research of tealeaves is still in the starting stage, currently identifies inspection still without a kind of relatively good tea-leaf producing area
Survey method.
Rare earth element（Rare Earth Element, REE）Refer to atomic number be 57（La）To 71（Lu）Group of the lanthanides member
Element（Including La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu）, in addition also include
No. 39 Y.The smaller REE of atomic number (La~Eu) is usually called light rare earth elements（LREE）, and atomic number is larger
REE（Gd~Lu）Referred to as heavy rare earth element（HREE）.Rare Earth Elements in Tea content difference due to type and producing region are different,
Open report is had not yet to see using rare earth element as discriminant criterion.
Invention content
The problem of for background technology, the object of the present invention is to provide a kind of Production area recognition method of flat tea,
Distinguish model in the place of production that different sources flat tea is established by using the method for different sources content of rare earth difference（Differentiate mould
Type）, to distinguish the provenance of different flat teas.
Realize that the used technical solution of the present invention is as follows：
A kind of Production area recognition method of flat tea, it is characterised in that：The tea that the recognition methods passes through measurement different sources
Leaf rare earth element content establishes discrimination model respectively, then measures rare earth element content in the Tea Samples in the unknown place of production with sentencing
Other model judges its place of production.
A kind of Production area recognition method of the flat tea, it is characterised in that：Steps are as follows for the recognition methods：
1）Select the tealeaves representative sample from different sources：Work is distributed and processed according to the main place of production of flat tea
Skill, the Shandong Rizhao for selecting processing technology almost the same（SD）, Sichuan Qing Chuan (SC), Guizhou Liping (GZ) and Zhejiang (ZJ) totally four
The Tea Samples of a tealeaves main producing region, standard of plucking are one leaf of a bud, select the representative sample of early, middle and late different times.
2）Rare-earth Element Dy：The tealeaves representative sample of different sources is measured after micro-wave digestion pre-processes with ICP-MS
Rare earth element content, the rare earth element be La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm,
The running parameter of Yb, Lu, Y, ICP-MS is：1400 W of radio-frequency power, 18 L/min of cooling air flow velocity, secondary air speed 1.65
L/min, 0.95 L/min of atomizer flow rate, 0.25 L/min of sheath gas, 6.5 mm of height of sampling pump 30 s of stabilization time.
Micro-wave digestion preprocess method is：Sample that 0.3 g is ground through ball mill is weighed in counteracting tank, 5 ml are added
70% HNO3, capping stand 1 h；Sample after standing is put into microwave dissolver to clear up, resolution program parameter is 5 min
Rise to 120 DEG C of holding 5 min, 5 min rise to 140 DEG C of holding 10 min, and 5 min rise to 180 DEG C of 10 min of holding, taken after cooling
Go out, slowly opens cover exhaust, counteracting tank is placed on control-temperature electric heating plate and catches up with acid for 140 DEG C, digestive juice is transferred to 25 ml capacity
In bottle, ultra-pure water is settled to scale, and mixing is spare.
3) the Production area recognition technology model of tealeaves is built：It is multiple using one-way analysis of variance and least significant difference
Comparative approach compares difference of the rare earth element content between different sources, and the Production area recognition of tealeaves is established based on rare earth element content
Technology model；The Production area recognition technology model is linear discriminant model, and the model is as follows：
U(SD)=-7.76+4.18La-8.92Ce+24.85Pr-10.09Nd-5.23Sm-5.71Eu+1.73Gd+1.04Tb
+5.9Dy-7.89Ho-2.67Er+4.6Tm-10.85Yb+12.12Y
U(SC)=-5.21+3.64La-3.36Ce-6.13Pr+4.1Nd+5.65Sm+8.44Eu-10.62Gd+1.41Tb-
4.26Dy+13.37Ho-13.89Er-11.07Tm+25.82Yb-14.22Y
U(ZJ)=-0.76-0.71La+0.87Ce+0.82Pr-0.95Nd-0.19Sm-0.27Eu-2.97Gd+0.36Tb+
2.54Dy-1.42Ho+5.12Er+6.73Tm-11.55Yb+1.53Y
U(GZ)=-8.07-7.13La+11.91Ce-26.13Pr+11.15Nd-0.59Sm-3.56Eu+26.48Gd-
4.95Tb-12.99Dy-2.57Ho-0.46Er-20.9Tm+29.9Yb-2.01Y。
4) it by the Tea Samples of unknown place of production information, is pre-processed through resolution, after rare earth element assay, inputs tealeaves
Production area recognition technology model differentiates tea-leaf producing area information；When carrying out place of production differentiation, by the tealeaves sample of unknown place of production information
Each element content in product is inputted respectively in aforementioned four model, compares U value sizes, takes the corresponding production of the maximum model of U values
Ground is determined as the unknown sample place of production.
Above-mentioned Production area recognition technology model, by back substitution inspection and cross validation, back substitution inspection correct decision rate is
92.93% cross validation differentiation rate is 84.8%, can preferably distinguish the place of production of different flat teas.
Description of the drawings
Fig. 1 is first three principal component scores figure of PLS-DA；
Fig. 2 is first three discriminant function shot chart of LDA.
Specific implementation mode
The present invention is further described in detail With reference to embodiment.
A kind of Production area recognition technical method of West Lake Dragon Well tea, mainly includes the following steps that：
1) the tealeaves representative sample from different sources is selected：Work is distributed and processed according to the main place of production of flat tea
Skill, this research is from the almost the same Shandong Rizhao of processing technology（SD）, Sichuan Qing Chuan（SC）, Guizhou Liping（GZ）, Longjing tea west
Lake (XH), more state (YZ, Shaoxing Yuecheng District, Shengzhou, Xinchang), the money pool（QT, Fuyang City, Yuhang District, Chunan County）Producing region
99 Tea Samples are selected.Wherein Longjing tea producing region sample has 55, Sichuan Qing Chuan 17,12, Guizhou Liping, Shandong day
According to 15.Tea Samples take spot sampling mode to obtain, and process time is different because of local phenological period difference in various regions,
Standard of plucking is one leaf of a bud, but the sample of the early, middle and late different times of each regional attentional selection；It has chosen and works as when sampling
Ground representativeness tea tree breed：Dragon Well tea 43 and endemic species.
2) Rare-earth Element Dy：Blank is arranged through pretreatments such as micro-wave digestion, dilutions in Rare-earth Element Dy sample
Control sample；0.3 g is weighed through ball mill（MM301, Germany, Retsch）5 ml are added in high-pressure digestion tank in the sample ground
70% HNO3（Top pure grade, the U.S., Thermo Fisher Scientific）Capping stands 1 h.High-pressure digestion tank uses preceding warp
20% nitric acid dousing is stayed overnight, and ultra-pure water cleaning is dried.Sample after standing is put into microwave dissolver to clear up, clears up program
Parameter be 5 min rise to 120 DEG C holding 5 min, 5 min rise to 140 DEG C holding 10 min, 5 min rise to 180 DEG C keep 10
Min takes out after cooling, slowly opens cover exhaust, high-pressure digestion tank is placed on control-temperature electric heating plate and catches up with acid for 140 DEG C, will be digested
Liquid is transferred in 25 ml volumetric flasks, and ultra-pure water is settled to scale, and mixing is spare.
Rare earth element content is by ICP-MS（AURORA M90, Germany, BRUKER companies）It measures, the running parameter of ICP-MS
For：1400 W of radio-frequency power, 18 L/min of cooling air flow velocity, secondary air speed 1.65 L/min, 0.95 L/ of atomizer flow rate
Min, 0.25 L/min of sheath gas, 6.5 mm of height of sampling pump 30 s of stabilization time.
Inner mark solution：1000 μ g/ml Rh, In, Re mixed standard solutions of certain volume（Chinese metering scientific research
Institute）, use 1%HNO31 μ g/ml are diluted to, mass spectrograph is introduced by internal standard pipe online.
Instrument tunes stock solution：10 μ g/ml Be, Mg, Co, In, Ce, Tl tune 1% HNO of stock solution3It is diluted to 1
Ng/ml, it is spare.
Specification Curve of Increasing：With 1% dust technology by rare earth element hybrid standard stock solution（100 μ g/ml contain 15 kinds of rare earths
Element La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Y) it is diluted to 0.5 step by step,
The mixed standard solution of 1,2,4,6 μ g/L.Blank solution is acquired under the operating condition of ICP-MS（1% HNO3）It is molten with standard
Liquid series, standard curve is drawn by instrument automatically.
3) the Production area recognition technology model of tealeaves is built：Using one-way analysis of variance and least significant difference（LSD）
Multiple range test method compares difference of the rare earth element content between different sources.Using Principal Component Analysis（PCA）, partially minimum two
Multiplication discriminant analysis（PLS-DA）And Fisher face（FLD）Differentiate with to different sources tealeaves.
Above-mentioned statistical analysis is completed using SPSS 19.0 and SIMCA 13.0.3.The effective mass information in sample is extracted,
Build the Production area recognition technology model of tealeaves；
4) it by the Tea Samples of unknown place of production information, is pre-processed through resolution, rare earth element assay, data prediction
Afterwards, the Production area recognition technology model for inputting tealeaves, predicts tea-leaf producing area information.
Rare earth element content characteristics between different sources flat tea：99 parts of Tea Samples rare earth element contents exist in total
Between 0.11~2.48 mg/kg, each department total amount of rare earth mean value is 0.26~0.95 mg/kg.In the sample of areas in Rizhao
Rare earth element total amount is significantly higher than Zhejiang, Sichuan Qing Chuan, three area of Guizhou Liping, Zhejiang, Guizhou Liping sample rare earth elements
Total amount is significantly higher than Sichuan Qing Chuan, and Zhejiang and Guizhou Liping tealeaves rare earth element total amount are close.
15 kinds of rare earth element contents of tealeaves and the ratio for accounting for rare earth element total amount are as shown in table 1.6 kinds of light rare earth elements
（LREE, La,Ce,Pr,Nd,Sm,Eu）0.21~0.76 mg/kg of content range, accounts for 80% of total amount of rare earth or so.Heavy rare earth
Element (HREE) content range is 0.058~0.19 mg/kg, accounts for 20% of total amount of rare earth or so.LREE/HREE values 3.5~
Between 4.3, hence it is evident that ratio 2.3 ~ 3.5 corresponding higher than in rock illustrates Rare Earth Elements in Tea based on light rare earth, light rare earth point
Enrichment is evaporated, and heavy rare earth is fractionated dilution.
Various regions section rare earth element changes of contents shows certain similitude.Each element content shows Shandong most substantially
Height, Zhejiang are taken second place, Sichuan and the lower trend in Guizhou.By least significant difference（LSD）After multiple comparative test, each element
Content shows as Shandong and is significantly higher than Sichuan, Zhejiang, Guizhou San Sheng, consistent with total amount of rare earth performance（p<0.05）, but Eu contents
It is slightly different, Shandong is significantly higher than other three provinces, and there is also significant differences for Zhejiang and two province's sample room of Guizhou（p<0.05）.
2. the place of production based on rare earth element fingerprint differentiates
2.1 Partial Least Squares discriminant analyses (PLS-DA)
PLS-DA models are established based on 15 kinds of rare earth element contents, using seven cycle cross verifications intersect and test
Card, extracts three main compositions, and it is 97% to add up variance contribution ratio.Partial Least Squares discriminant analysis PLS-DA first three it is main at
Get component and see that Fig. 1, Shandong Rizhao and Sichuan Qing Chuan sample can be separated substantially, Guizhou Liping, Zhejiang sample and various regions have not
Intersect with degree.It is 60.63% that correct decision rate is verified in model back substitution, and cross validation correct decision rate is 61.61%（It is shown in Table 2）.
It is relatively low to be applied to the right judging rate that the flat tea place of production is traced to the source based on the PLS-DA models that rare earth element content is established.
2.2 linear discriminant analysis（FLD）
By variance analysis, distribution pattern variance analysis and the principal component analysis of different province tealeaves sample rare earth element contents
As a result can be seen that differentiate it being feasible to tea-leaf producing area using rare earth element fingerprint.Based on 15 kinds of rare earth element contents, build
The FLD discrimination models in the vertical place of production.Discrimination model is as follows
U(SD)=-7.76+4.18La-8.92Ce+24.85Pr-10.09Nd-5.23Sm-5.71Eu+1.73Gd+1.04Tb
+5.9Dy-
7.89Ho-2.67Er+4.6Tm-10.85Yb+12.12Y
U(SC)=-5.21+3.64La-3.36Ce-6.13Pr+4.1Nd+5.65Sm+8.44Eu-10.62Gd+1.41Tb-
4.26Dy+
13.37Ho-13.89Er-11.07Tm+25.82Yb-14.22Y
U(ZJ)=-0.76-0.71La+0.87Ce+0.82Pr-0.95Nd-0.19Sm-0.27Eu-2.97Gd+0.36Tb+
2.54Dy-1.42Ho+5.12Er+6.73Tm-11.55Yb+1.53Y
U(GZ)=-8.07-7.13La+11.91Ce-26.13Pr+11.15Nd-0.59Sm-3.56Eu+26.48Gd-
4.95Tb-12.99Dy-2.57Ho-0.46Er-20.9Tm+29.9Yb-2.01Y
First three typical discriminant function of extraction model（DF, Discriminant function）DF1, DF2, DF3, variance
Contribution rate is respectively 66.73%, 25.12%, 8.14%.
First three discriminant function shot chart of linear discriminant analysis is shown in that Fig. 2, various regions sample distribution are more concentrated, Shandong Rizhao,
Sichuan Qing Chuan, Guizhou Liping sample can distinguish completely, although three ground samples have with Zhejiang sample intersects, but still can be with Zhejiang
Sample substantially distinguishes.By back substitution inspection and cross validation, the results are shown in Table 3 for discriminant analysis, and back substitution inspection is correctly sentenced
It is 84.8% that rate, which is not 92.93% cross validation differentiation rate,.
This research selects flat tea as discriminant analysis object, and Partial Least Squares discriminant analysis is respectively adopted and linearly sentences
The tealeaves to four is not analyzed and carries out place of production discriminating, and Fisher face correct decision rate is higher, and Partial Least Squares differentiates
It is unsatisfactory to analyze correct decision rate.
Claims (2)
1. a kind of Production area recognition method of flat tea, it is characterised in that：The tealeaves that the recognition methods passes through measurement different sources
Rare earth element content establishes discrimination model respectively, and the rare earth element content then measured in the Tea Samples in the unknown place of production differentiates
Model judges its place of production；
Steps are as follows for the recognition methods：
1）Select the tealeaves representative sample from different sources：According to the distribution of the main place of production of flat tea and processing technology, choosing
Select the almost the same Shandong Rizhao of processing technology（SD）, Sichuan Qing Chuan (SC), Guizhou Liping (GZ) and Zhejiang (ZJ) totally four tea
The Tea Samples of leaf main producing region, standard of plucking are one leaf of a bud, select the representative sample of early, middle and late different times；
2）Rare-earth Element Dy：The tealeaves representative sample of different sources measures rare earth after micro-wave digestion pre-processes with ICP-MS
Constituent content, the rare earth element be La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb,
The running parameter of Lu, Y, ICP-MS is：1400 W of radio-frequency power, 18 L/min of cooling air flow velocity, 1.65 L/ of secondary air speed
Min, 0.95 L/min of atomizer flow rate, 0.25 L/min of sheath gas, 6.5 mm of height of sampling pump 30 s of stabilization time；
3) the Production area recognition technology model of tealeaves is built：Using one-way analysis of variance and least significant difference Multiple range test
Method compares difference of the rare earth element content between different sources, and the Production area recognition technology of tealeaves is established based on rare earth element content
Model；
4) it by the Tea Samples of unknown place of production information, is pre-processed through resolution, after rare earth element assay, inputs the place of production of tealeaves
Identification technology model differentiates tea-leaf producing area information；
The Production area recognition technology model is linear discriminant model, and the model is as follows：
U(SD)=-7.76+4.18La-8.92Ce+24.85Pr-10.09Nd-5.23Sm-5.71Eu+1.73Gd+1.04Tb+
5.9Dy-7.89Ho-2.67Er+4.6Tm-10.85Yb+12.12Y
U(SC)=-5.21+3.64La-3.36Ce-6.13Pr+4.1Nd+5.65Sm+8.44Eu-10.62Gd+1.41Tb-
4.26Dy+13.37Ho-13.89Er-11.07Tm+25.82Yb-14.22Y
U(ZJ)=-0.76-0.71La+0.87Ce+0.82Pr-0.95Nd-0.19Sm-0.27Eu-2.97Gd+0.36Tb+
2.54Dy-1.42Ho+5.12Er+6.73Tm-11.55Yb+1.53Y
U(GZ)=-8.07-7.13La+11.91Ce-26.13Pr+11.15Nd-0.59Sm-3.56Eu+26.48Gd-4.95Tb-
12.99Dy-2.57Ho-0.46Er-20.9Tm+29.9Yb-2.01Y
When carrying out place of production differentiation, each element content in the Tea Samples of unknown place of production information is inputted into aforementioned four model respectively
In, compare U value sizes, the corresponding place of production of the maximum model of U values is taken to be determined as the unknown sample place of production.
2. a kind of Production area recognition method of flat tea according to claim 1, it is characterised in that：The step 2）Middle microwave
Clearing up preprocess method is：Sample that 0.3 g is ground through ball mill is weighed in counteracting tank, 5 ml, 70% HNO3, capping is added
Stand 1 h；Sample after standing is put into microwave dissolver to clear up, resolution program parameter is that 5 min rise to 120 DEG C of holdings
5 min, 5 min rise to 140 DEG C and 10 min, 5 min are kept to rise to 180 DEG C of 10 min of holding, are taken out after cooling, slowly open tank
Lid exhaust, counteracting tank is placed on control-temperature electric heating plate and catches up with acid for 140 DEG C, digestive juice is transferred in 25 ml volumetric flasks, ultra-pure water is fixed
Hold to scale, mixing is spare.
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