CN109164187A - A method of distinguishing same type different sources tealeaves - Google Patents
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Abstract
This application discloses use full-automatic headspace solid-phase microextraction (headspace solid-phase microextraction, HS-SPME) method extracts the fragrance component in tealeaves, and combine gas chromatography-mass spectrum (gas chromatography-mass spectrometry, GC-MS) separate and identify the fragrance component of tealeaves, using identify come tea aroma ingredient relative amount, cluster and principal component model are constructed in conjunction with chemometrics method (CA and PCA), so that the tealeaves of same type different sources is distinguished.The present invention evaluates identification (place of production for being based particularly on fragrance component differentiates) for the quality of tealeaves and provides the method for a kind of new effective assessment and control.Operation is simple for the method for the present invention, at low cost, environmentally friendly, can quality evaluation to tealeaves and control a kind of efficient, objective, standardization method is provided.
Description
Technical field
The invention belongs to tea technology fields, are combined in particular to a kind of using full-automatic headspace solid-phase microextraction
Gaschromatographic mass spectrometry and chemometrics method are come the method for distinguishing same type different sources tealeaves.
Background technique
Tea is one of beverage most popular in the world, is consumed by the people in 2/3 or more the whole world.Consumer is to tealeaves
Favor degree depends primarily on the quality and flavour of tealeaves.The quality of tealeaves generally refers to the color, smell, taste, shape and leaf of tealeaves
Bottom.Tealeaves is as a kind of beverage, and for drinking needs, the fragrance and flavour of millet paste are the cores of tea leaf quality, wherein fragrance
It is to feel a critically important factor of tea leaf quality quality, and capture and cultivate the most important factor of customer loyalty,
It is the important factor for determining tealeaves price.In addition, the contribution of chemical component and its multidimensional complicated in tealeaves is to determine tealeaves product
The key factor of matter.
Since ancient times, the quality of tealeaves is evaluated all be by it is some by trained or veteran sensory expert Lai
Assessment.This tealeaves sensory evaluation is that close examination tealeaves shape and leaf are discovered with sense organs such as the smell of people, the sense of taste, vision, tactiles
The thickness at bottom, neat and well spaced degree, tenderness and color, smell the fragrance at the bottom of glass middle period, identify the color of millet paste, taste its taste and aroma
To carry out a kind of method of overall merit.
Have many advantages, such as quick, simple although sensory review's method and it is an experience activity after all being widely used,
Subjective colo(u)r is stronger, and review result is easy to be influenced by experience, external environment and syndic's self-condition, and sensory review
Method has no quantization standard to evaluating also for tea aroma, can not carry out real-time online monitoring, can not accomplish standardization and true
Just objectifying the disadvantages of.
Also, tea aroma ingredient is easy to be affected by many factors, such as: the place of production, tea tree breed, cultivation condition, picking
Season and quality, tea-manufacturing technology and storage condition etc..Therefore, this method of tea leaf quality is evaluated using sensory review's method to be obtained
To inconsistent and inaccurate result.It is badly in need of establishing a kind of more standard and effective method carrys out the quality of objective assessment tealeaves.
HS-SPME be it is a kind of integrate extraction, concentration and sample introduction and be not necessarily to any solvent Sample Pretreatment Technique.And
HS-SPME combination GC-MS has been employed successfully in the fragrance component identification of many tealeaves.However, HS-SPME combination GC-MS method
Analyze and identify tea aroma ingredient and further by chemometrics method (CA and PCA) come quantitatively evaluating tea leaf quality and area
The method of same type different sources tealeaves is divided to be rarely reported.
Chinese Patent Application No. 201510652180.6 discloses a kind of utilization near-infrared spectrum technique identification local tea variety
Method, this method obtains the near-infrared diffusing reflection spectrum of tealeaves sample near infrared spectrometer, and counts to the spectrum
Processing.But this method cannot obtain the specifying information of tea component, especially fragrance, to the fragrance component of different tealeaves
It can not identify.
Chinese Patent Application No. 201710164063.4 discloses a kind of quick, lossless tea-leaf producing area identification method,
Nondestructive analysis is carried out to tealeaves using Proton-Transfer Reactions-time of-flight mass spectrometer, and mass spectrometric data is analyzed, is established
Identification model, to identify tea-leaf producing area.
Chinese Patent Application No. 201711042224.9 discloses a kind of construction method of tealeaves elemental fingerprints map, uses
Tealeaves is cleared up in identification tea-leaf producing area, including with microwave dissolver, and measures Tea Samples with inductivity coupled plasma mass spectrometry
Middle constituent content further converts elemental fingerprints map for tealeaves element composition, to identify tea-leaf producing area.But the party
Method is not related to the identification of tealeaves flavor component yet.
Chinese Patent Application No. 201711321322.6, which is disclosed, establishes essence in tealeaves by GC × GC-TOF/MS technology
High flux examination detection method, and establish in tealeaves fragrance component database in essence rapid screening database and tealeaves.
The patent application is not related to tea-leaf producing area identification method, does not disclose yet and carries out stoichiometry to fragrance component.Head space solid phase is micro-
Extracting (HS-SPME) is a kind of environmental type sample analysis pretreatment technology, and there is sensitive, quick, easy to operate, sample to use
It measures less, have to the advantages of solvent, it can be achieved that selective extraction, the object being enriched to can be at gas chromatograph-mass spectrometer (GC-MS)
On directly analyzed, had been widely used in the research of various food and drug volatile component at present.However, utilizing tealeaves
Fragrance component information, it is fresh come the method for distinguishing same type different sources tealeaves in conjunction with chemometrics method (CA and PCA)
It has been reported that.
For these reasons, the present invention is specifically proposed.
Summary of the invention
For the above-mentioned problems of the prior art and deficiency, the present invention provides a kind of utilization the full-automatic micro- extraction of head space solid phase
The method for distinguishing same type different sources tealeaves, the method for the present invention are taken in conjunction with gaschromatographic mass spectrometry and chemometrics method
Using HS-SPME combination GC-MS method come objective qualitative and quantitative analysis tea aroma ingredient, traditional sensory evaluation can be solved
The shortcoming of tea leaf quality.While it can be by same type not further being analyzed using the combination of tealeaves finger-print CA and PCA
Tealeaves with producing region distinguishes.The tea leaf quality assessment that is established as of this method provides accurate and reliably evaluates foundation,
The foundation of control and criticism is provided for the production, processing and consumer of tealeaves.The present invention is that the quality of tealeaves evaluates identification (spy
It is not that the place of production based on fragrance component differentiates) provide the method for a kind of new effective assessment and control.The method of the present invention behaviour
Make it is simple and easy, at low cost, environmentally friendly, can quality evaluation to tealeaves and control a kind of efficient, objective, standardization side is provided
Method.
In one embodiment, this application involves a kind of methods for distinguishing same type different sources tealeaves, including with
Lower step:
(1) Tea Samples of same type different sources are crushed as tea powder and is further prepared as being used for head space solid phase micro-
The sample of extraction；
(2) with full-automatic Headspace solid phase microextractiom (HS-SPME), tea is extracted using PDMS/DVB/CAR extracting fiber head
Fragrance component in powder；
(3) by the fragrance component desorption in extracting head, and by gas chromatography-mass spectrography (GC-MS) carry out separation and
Identification, obtains mass spectrometric data；
(4) mass spectrometric data is retrieved in standard spectrum library, carries out qualitative and quantitative analysis, obtains fragrance component
The relative amount of each component；
(4) using the relative amount of the fragrance component each component, and CA and the PCA chemistry of fragrance component each component are combined
Metrology method distinguishes the tealeaves of same type different sources.
In another embodiment, extraction 30-90 minutes, preferably 60 minutes in step (2).Another
In embodiment, the PDMS/DVB/CAR extracting fiber head is 65 μm of dimethione/divinylbenzene/carbene extraction
Fiber head, manufacturer are U.S. Supelco company.In one embodiment, desorption 2-4 points in step (3)
Clock, preferably 3.5 minutes.In one embodiment, the standard spectrum library is NIST 08.L standard spectrum library, passes through mass spectrum
RI value progress with degree and each component is qualitative, is quantified using area normalization method.The 08.L standard spectrum library NIST is purchase
It is included when producer's instrument is installed.Software used in CA and PCA chemometrics method is that (Umetrics is public by SIMCA-P15
Department), this method is using the relative amount of the fragrance component of all tealeaves as carrying out in variable import chemo metric software
Analysis.Specific implementation method by based on GC-MS analysis as a result, by analysis Tea Samples fragrance component content matrix table (A
Sample × B kind component) it inputs in multivariate statistics soft sim CA-P15 and is analyzed.Wherein PCA be retain as far as possible it is original
On the basis of variable information, dimension is reduced, it is useful utmostly to extract by the principal component by original variable linear combination
Information.By PCA it can be seen that relationship between sample and sample, the relationship between variable (fragrance component) and variable are being changed
It learns in pattern-recognition for classifying and clustering.Clustering (CA) is the reason according to " things of a kind come together, people of a mind fall into the same group ", to sample or index into
A kind of Multielement statistical analysis method of row classification, the object that it is discussed is a large amount of sample, it is desirable that can reasonably press respective spy
Property is classified, and can for reference or be followed without any mode, is to carry out in the case where no priori knowledge.
In one embodiment, in CA the and PCA chemometrics method, using small echo spectral filtering method to institute
The relative amount for stating fragrance component each component is pre-processed, and to remove invalid data, obtains a series of variables.Further
In embodiment, dimension-reduction treatment is carried out to the variable, to generate new variable for further analyzing.In another embodiment party
In case, in CA the and PCA chemometrics method, using small echo spectral filtering method to the phase of the fragrance component each component
Content is pre-processed, to remove invalid data, a series of variables are obtained, and dimension-reduction treatment is carried out to the variable, to produce
Raw new variable is for further analyzing.In another embodiment, involved in the CA chemometrics method away from
From calculating, the calculating using Euclidean distance algorithm carry out.Data are carried out in CA and PCA chemometrics method above-mentioned
The use of pretreatment, Dimension Reduction Analysis and Euclidean distance algorithm allows the invention to preferably realize method of the invention, phase
Than the default value of each parameter in SIMCA-P15 software, obtains better tealeaves and distinguish result.
In one embodiment, tea powder is crushed using high-speed multifunctional pulverizer, with the sieving of 40 mesh.At another
Embodiment in, the sample for headspace solid-phase microextraction in step (1) is prepared as follows: being weighed the tea powder of each tea sample, is put
Enter in ml headspace bottle, the distilled water boiled is added and brews, immediately closed bottleneck, then brewing time 1-3min places incubating for head space
Change in device, revolving speed 250r/min, in 80 DEG C of balances 5-15min, preferably 10min.In another embodiment, step (3)
Middle GC condition are as follows: HP-5MS fused-silica capillary column (30m × 0.25mm × 0.25 μm)；250 DEG C of injector temperature；Carrier gas is
High-purity helium, purity >=99.999%, column flow 1.0mL/min；Temperature program: 50 DEG C of initial temperature, keep 5min, with 3 DEG C/
Min rises to 210 DEG C, keeps 3min, then rise to 230 DEG C with 15 DEG C/min, Splitless injecting samples；MS condition are as follows: ion source EI, electronics
Energy 70eV, 230 DEG C of ion source temperature, 280 DEG C of converting interface temperature, mass scan range m/z 35~500, the solvent delay time
For 2.8min.
Specifically, utilizing full-automatic headspace solid-phase microextraction combination gaschromatographic mass spectrometry and change this application discloses a kind of
Learn the method that metrology method distinguishes same type different sources tealeaves, the specific steps are as follows:
(1) material prepares: selecting the Tea Samples of representative same type different sources, grade is consistent, production
In 2013.
(2) sample preparation: by PDMS/DVB/CAR extracting fiber head in 250 DEG C of aging 60min of GC injection port.It accurately weighs
The tea powder 2g of each tea sample, is put into 20mL ml headspace bottle, and the distilled water that 5mL is boiled is added and brews, immediately closed bottleneck, brewing time
2min.Then in the incubator for placing head space, revolving speed 250r/min, after 80 DEG C of balance 10min, (G6500 turns autosampler
Disc type autosampler, band headspace solid-phase microextraction device, is produced in CTC company of the U.S.) extracting head is inserted into ml headspace bottle head space
Position extracts 60min, and gas chromatographic sample introduction mouth, desorption 3.5min are immediately inserted into after taking-up, while starting instrument and collecting data；
(3) Components identification: by GC-MS, (7890A-5975C GC-MS combined instrument, manufacturer are U.S. Agilent public
Department) obtained mass spectrometric data is analyzed in NIST 08.L standard spectrum library (the spectrum library is included when installing for purchase producer's instrument) progress
Retrieval, it is qualitative in conjunction with mass spectrum matching degree and the progress of the RI value of each component, while being quantified using using area normalization method, it obtains
To the relative amount of each component；
(4) data are analyzed: GC-MS is analyzed to fragrance component content matrix table (the A sample × B kind of resulting Tea Samples
Component) input multivariate statistics soft sim CA-P15 in carry out PCA and CA analysis, as a result can well same type not
Tealeaves with the place of production distinguishes；
Dimethione/divinylbenzene/carbene that extracting fiber head is 65 μm in the step (2), is purchased from the U.S.
Supelco company；
Tea powder is crushed using high-speed multifunctional pulverizer in the step (2), with the sieving of 40 mesh；
GC condition in the step (2) are as follows: HP-5MS fused-silica capillary column (30m × 0.25mm × 0.25 μm)；Into
250 DEG C of sample mouth temperature；Carrier gas is high-purity helium, purity >=99.999%, column flow 1.0mL/min；Temperature program: initial temperature
50 DEG C, 5min is kept, 210 DEG C is risen to 3 DEG C/min, keeps 3min, then rise to 230 DEG C with 15 DEG C/min, Splitless injecting samples.MS
Condition are as follows: ion source EI, electron energy 70eV, 230 DEG C of ion source temperature, 280 DEG C of converting interface temperature, mass scan range m/z
35~500, the solvent delay time is 2.8min.
The present invention its remarkable advantage compared with traditional tea leaf quality sensory review's method is:
(1) to carry out the fragrance component of tealeaves in conjunction with modern times advanced analytical equipment and chemometrics method qualitative
And quantitative analysis；
(2) assessment indicator system of different tealeaves is established and is improved in the methodological study for having expanded tealeaves sensory review；
(3) objectively the fragrance component of tealeaves is analyzed, realizes that operable science digital method, control tealeaves sense organ are examined
Human error that may be present in commenting；
(4) chemometrics method is combined, establishes one reliably for the differentiation of the tealeaves of same type different producing area
Model is distinguished, provides an important criteria for the identification of tea leaf quality feature.
Detailed description of the invention
Fig. 1: the GC-MS map of Yunnan green tea and other province green tea samples used in embodiment 1.
Fig. 2: the classification chart of Yunnan green tea and other province green tea samples used in embodiment 1.The classification chart is based on PCA points
Analysis obtains.
Fig. 3: the dendrogram of Yunnan green tea and other province green tea samples used in embodiment 1.The dendrogram is based on CA points
Analysis obtains.
Fig. 4: the GC-MS map of Hunan Anhua used dark green tea and Guangxi Liu Bao tea sample in embodiment 2.
Fig. 5: the classification chart of Hunan Anhua used dark green tea and Guangxi Liu Bao tea sample in embodiment 2.The classification chart is based on PCA
Analysis obtains.
Fig. 6: the dendrogram of Hunan Anhua used dark green tea and Guangxi Liu Bao tea sample in embodiment 2.The dendrogram is based on CA
Analysis obtains.
Fig. 7: the GC-MS map of yunnan puer tea and Hunan dark green tea sample used in embodiment 3.
Fig. 8: the classification chart of yunnan puer tea and Hunan dark green tea sample used in embodiment 3.The classification chart is analyzed based on PCA
It obtains.
Fig. 9: the dendrogram of yunnan puer tea and Hunan dark green tea sample used in embodiment 3.The dendrogram is analyzed based on CA
It obtains.
Specific embodiment
It further illustrates below by the mode of embodiment and invents herein, but therefore do not limit the present invention to described
Among scope of embodiments.Embodiment in following embodiment can be further combined or replace, professional technique in this field
The various changes and modifications that personnel make the technical solution of this paper, all belong to the scope of protection of the present invention.
Embodiment 1: a kind of to utilize full-automatic headspace solid-phase microextraction combination gaschromatographic mass spectrometry and chemometrics method
Method to distinguish Yunnan green tea He other province green tea, the specific steps are as follows:
(1) material prepares: 19 green tea samples from Yunnan production area different from Yunnan, number are
Y1-1Y19.Other 30 green tea are then Zhejiang, Sichuan, Anhui, Henan, Hubei and Jiangsu etc. respectively from other provinces
Ground, number C1-C30, the productive year of all tealeaves are consistent.
(2) sample preparation: by PDMS/DVB/CAR extracting fiber head in 250 DEG C of aging 60min of GC injection port.It accurately weighs
The tea powder 2g of each tea sample, is put into 20mL ml headspace bottle, and the distilled water that 5mL is boiled is added and brews, immediately closed bottleneck, brewing time
2min.It is then placed in the incubator of head space, revolving speed 250r/min, after 80 DEG C of balance 10min, autosampler will be extracted
Head insertion ml headspace bottle head space position extracts 60min, is immediately inserted into gas chromatographic sample introduction mouth after taking-up, desorption 3.5min, simultaneously
Start instrument and collects data.
(3) Components identification: GC-MS map is shown in Fig. 1.By GC-MS, (7890A-5975C GC-MS combined instrument, manufacturer are
Agilent company of the U.S.) the obtained mass spectrometric data of analysis retrieved in NIST 08.L standard spectrum library, in conjunction with mass spectrum matching degree
It is qualitative with the RI value of each component, while being quantified using using area normalization method, obtain the relative amount of each component.49
In a green tea sample, 103 kinds of volatile components, predominantly alcohols, hydrocarbon and ketone compounds are identified altogether, wherein linalool
Oxide II, linalool, a- terpinol, gaultherolin, geraniol, cis- 3- hexene alcohol benzoic ether, cedrol and hexadecylic acid
Deng in the green tea of Yunnan content it is higher, and geranyl acetone, β-ionone, a- farnesene, dihydroactinidiolide, flores aurantii uncle
Alcohol, caffeine and the phytol content in the green tea in other provinces are higher.
(4) data are analyzed: GC-MS is analyzed to fragrance component content matrix table (49 sample × 103 of resulting Tea Samples
Component) input multivariate statistics soft sim CA-P15 in carry out PCA and CA analysis.Ours as a result, it has been found that Yunnan produce it is green
Preferable differentiation is realized between the green tea that tea and other provinces produce, on the principal component scores figure of PCA, the green tea of the production in Yunnan
Gather on the left side, the green tea that are produced from other provinces gathers on the right (see Fig. 2).On CA dendrogram, Yunnan produce green tea and other
The green tea that is produced from province belongs to Liang great branch, they gather respectively in different classifications (see Fig. 3).Our result indicate that the greatest extent
The green tea of pipe same type different sources belongs to a tealeaves classification, they have embodied similar on fragrance composition and content
Property, but PCA and CA still can preferably be distinguished and respective cluster between them to realizing.
Embodiment 2: a kind of to utilize full-automatic headspace solid-phase microextraction combination gaschromatographic mass spectrometry and chemometrics method
Distinguish the method (belonging to dark green tea classification) of Hunan Anhua dark green tea and Guangxi Liu Bao tea, the specific steps are as follows:
(1) material prepares: 3 Anhua dark green tea samples come from Hunan Province Anhua County, number D1-D3.In addition, 2 six forts
Tea comes from Guangxi, and number E1-E2, all tealeaves are the same productive years.
(2) sample preparation: by PDMS/DVB/CAR extracting fiber head in 250 DEG C of aging 60min of GC injection port.It accurately weighs
The tea powder 2g of each tea sample, is put into 20mL ml headspace bottle, and the distilled water that 5mL is boiled is added and brews, immediately closed bottleneck, brewing time
2min.It is then placed in head space incubator, revolving speed 250r/min, after 80 DEG C of balance 10min, autosampler is by extracting head
It is inserted into ml headspace bottle head space position and extracts 60min, gas chromatographic sample introduction mouth is immediately inserted into after taking-up, desorption 3.5min is opened simultaneously
Dynamic instrument collects data.
(3) Components identification: GC-MS map is shown in Fig. 4.By GC-MS, (7890A-5975C GC-MS combined instrument, manufacturer are
AGILENT company of the U.S.) the obtained mass spectrometric data of analysis retrieved in NIST 08.L standard spectrum library, in conjunction with mass spectrum matching degree
It is qualitative with the RI value progress of each component, while being quantified using using area normalization method, obtain the relative amount of each component.
90 compounds are found altogether in 5 all dark green tea samples, mainly include hydrocarbon, ketone compounds and alcohols chemical combination
Object.
(4) data are analyzed: GC-MS is analyzed to fragrance component content matrix table (5 sample × 91 group of resulting Tea Samples
Point) input multivariate statistics soft sim CA-P15 in carry out PCA and CA analysis.Ours as a result, it has been found that the dark green tea that is produced from Guangxi
Preferable differentiation is realized between the dark green tea of Hunan production, on the principal component scores figure of PCA, the dark green tea that is produced from Guangxi gathers on a left side
Side, the dark green tea that is produced from Hunan gather on the right (see Fig. 5).On CA dendrogram, the dark green tea that the dark green tea and Hunan that is produced from Guangxi produce is adhered to separately
In Liang great branch, they gather respectively in different classifications (see Fig. 6).Our result indicate that although same type difference produces
The dark green tea on ground belongs to a tealeaves classification, they have embodied similitude on fragrance composition and content, but PCA and CA are also
It is that can preferably be distinguished and respective cluster between them to realizing.
Embodiment 3: a kind of to utilize full-automatic headspace solid-phase microextraction combination gaschromatographic mass spectrometry and chemometrics method
Method to distinguish two kinds of most typical producing region dark green teas, the specific steps are as follows:
(1) material prepares: 18 yunnan puer teas are from different Pu'er tea producing regions, number A1-A18；14 lakes
Southern dark green tea is purchased from the tea market of Hunan Province Anhua County, number B1-B14, and all tealeaves are all produced in the same time.
(2) sample preparation: by PDMS/DVB/CAR extracting fiber head in 250 DEG C of aging 60min of GC injection port.It accurately weighs
The tea powder 2g of each tea sample, is put into 20mL ml headspace bottle, and the distilled water that 5mL is boiled is added and brews, immediately closed bottleneck, brewing time
2min.It is then placed in head space incubator, revolving speed 250r/min, after 80 DEG C of balance 10min, autosampler is by extracting head
It is inserted into ml headspace bottle head space position and extracts 60min, gas chromatographic sample introduction mouth is immediately inserted into after taking-up, desorption 3.5min is opened simultaneously
Dynamic instrument collects data.
(3) Components identification: GC-MS map is shown in Fig. 7.By GC-MS, (7890A-5975C GC-MS combined instrument, manufacturer are
AGILENT company of the U.S.) the obtained mass spectrometric data of analysis retrieved in NIST 08.L standard spectrum library, in conjunction with mass spectrum matching degree
It is qualitative with the RI value progress of each component, while being quantified using using area normalization method, obtain the relative amount of each component.
In 32 dark green tea samples, 136 kinds of fragrance components are identified altogether, and wherein methoxyl group benzene-like compounds are the spies in yunnan puer tea
Sign property fragrance component, occupies higher ratio, imparts the special Chen Xiang of Pu'er brick tea；Ketone compounds are Hunan dark green tea tea
In Flavoring Components, impart Hunan Fu-brick tea special flowers and fruits perfume (or spice) and wooden fragrance.
(4) data are analyzed: GC-MS is analyzed to fragrance component content matrix table (32 sample × 136 of resulting Tea Samples
Component) input multivariate statistics soft sim CA-P15 in carry out PCA and CA analysis.Ours as a result, it has been found that Yunnan produce it is general
Preferable differentiation is realized between the dark green tea that Pu'er tea tea and Hunan produce, on the principal component scores figure of PCA, the Pu'er tea of Yunnan production
(dark green tea) gathers on the left side, and the dark green tea that is produced from Hunan gathers on the right (see Fig. 8).On CA dendrogram, the Pu'er tea that is produced from Yunnan is (black
Tea) and Hunan produce dark green tea belong to Liang great branch, they gather respectively in different classifications (see Fig. 9).And we also send out
Existing 1,2,3- trimethoxy-benzenes, 1,2,3- trimethoxy -5- methylbenzene, 4- ethyl -1,2- dimethoxy benzene, linalool oxide
The substances such as IV, a- terpinol, 1,2- dimethoxy benzene, hexadecylic acid, geranyl acetone, β-ionone and caffeine are to differentiation model
Contribution it is larger, these substances have significant difference (P < 0.001) in two kinds of dark green teas.Therefore, pass through HS-SPME/GC-MS
In conjunction with chemometrics method, the differentiation of the dark green tea of two same type different sources may be implemented, this is the quality control of dark green tea
System provides a kind of new and standardization standard.
Claims (10)
1. a kind of method for distinguishing same type different sources tealeaves, comprising the following steps:
(1) each place of production Tea Samples are crushed as tea powder and is further prepared as being used for the sample of headspace solid-phase microextraction；
(2) with full-automatic Headspace solid phase microextractiom, using the fragrance in PDMS/DVB/CAR extracting fiber head extraction tea powder at
Point；
(3) it by the fragrance component desorption in extracting head, and is separated and is identified by gas chromatography-mass spectrography (GC-MS),
Obtain mass spectrometric data；
(4) mass spectrometric data is retrieved in standard spectrum library, carries out qualitative and quantitative analysis, obtains fragrance component each group
The relative amount divided；
(5) using the relative amount of the fragrance component each component, and CA the and PCA stoichiometry of fragrance component each component is combined
Method distinguishes the tealeaves of same type different sources.
2. method described in claim 1, wherein extraction 30-90 minutes, preferably 60 minutes in step (2).
3. method as claimed in claim 2, wherein the PDMS/DVB/CAR extracting fiber head be 65 μm dimethione/
Divinylbenzene/carbene extracting fiber head.
4. method described in claim 1, wherein desorption 2-4 minutes, preferably 3.5 minutes in step (3).
5. method described in claim 1 passes through mass spectrum matching degree wherein the standard spectrum library is NIST 08.L standard spectrum library
The qualitative analysis is carried out with the RI value of each component, the quantitative analysis is carried out using area normalization method.
6. method described in claim 1, wherein tea powder is crushed using high-speed multifunctional pulverizer, with the sieving of 40 mesh.
7. method described in claim 1, wherein the sample for headspace solid-phase microextraction in step (1) is prepared as follows: claiming
The tea powder for taking each tea sample, is put into ml headspace bottle, and the distilled water boiled is added and brews, immediately closed bottleneck, brewing time 1-3min,
It is preferred that 2 minutes, then in the incubator of placement head space, revolving speed 250r/min, in 80 DEG C of balances 5-15min, preferably 10min.
8. the described in any item methods of claim 1-7, wherein GC condition in step (3) are as follows: HP-5MS elastic quartz capillary tube
Column (30m × 0.25mm × 0.25 μm)；250 DEG C of injector temperature；Carrier gas is high-purity helium, purity >=99.999%, column flow
1.0mL/min；Temperature program:, keeping 5min by 50 DEG C of initial temperature, rises to 210 DEG C with 3 DEG C/min, keeps 3min, then with 15
DEG C/min rises to 230 DEG C, Splitless injecting samples；MS condition are as follows: ion source EI, electron energy 70eV, turn by 230 DEG C of ion source temperature
280 DEG C of interface temperature, mass scan range m/z 35~500, the solvent delay time is 2.8min.
9. method described in claim 1, wherein in CA the and PCA chemometrics method, using small echo spectral filtering
Method pre-processes the relative amount of the fragrance component each component, to remove invalid data, obtains a series of variables, and right
The variable carries out dimension-reduction treatment, to generate new variable for further analyzing.
10. method described in claim 1, wherein the calculating of the distance involved in the CA chemometrics method, the calculating
It is carried out using Euclidean distance algorithm.
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| CN201811204570.7A CN109164187A (en) | 2018-10-16 | 2018-10-16 | A method of distinguishing same type different sources tealeaves |
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| CN109884257A (en) * | 2019-03-28 | 2019-06-14 | 南京林业大学 | The discrimination method of cyclocarya paliurus tea |
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| CN111208251A (en) * | 2020-01-16 | 2020-05-29 | 中国农业科学院茶叶研究所 | Method for judging year of white tea by taking S-linalool and R/S-dihydroactinidiolide as markers |
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| CN111738548A (en) * | 2020-05-21 | 2020-10-02 | 福建省农业科学院农业生物资源研究所 | Jasmine tea aroma quality evaluation method and application thereof |
| CN111738548B (en) * | 2020-05-21 | 2023-04-07 | 福建省农业科学院农业生物资源研究所 | Jasmine tea aroma quality evaluation method and application thereof |
| CN115326944A (en) * | 2022-06-09 | 2022-11-11 | 华南农业大学 | Method for distinguishing black-leaf simple plexus in different producing areas |
| CN115326944B (en) * | 2022-06-09 | 2023-09-26 | 华南农业大学 | Method for distinguishing different producing areas of radix aconiti kusnezoffii She Shancong |
| CN115219620A (en) * | 2022-07-14 | 2022-10-21 | 西北大学 | Jingyang Fuzhuan tea specific identification volatile component combination, preparation method and application thereof, and Jingyang Fuzhuan tea identification method |
| CN115219620B (en) * | 2022-07-14 | 2024-01-26 | 西北大学 | Jingyang Fu tea specific identification volatile component combination, preparation method and application thereof, and Jingyang Fu tea identification method |
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