CN102253133A - Method for identifying specificity of Biluochun tea from Tungting Mountains, Soochow - Google Patents
Method for identifying specificity of Biluochun tea from Tungting Mountains, Soochow Download PDFInfo
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Abstract
The invention discloses a method for identifying the specificity of Biluochun tea from Tungting Mountains, Soochow. The method disclosed by the invention comprises the following steps: using tea which is prepared from native populations in a protective range meeting the national standard GB/T 18957-2008F geographical indication tea provision as a standard substance sample and extracting the fingerprint of the tea as a comparison reference group; respectively extracting a specificity liquid chromatogram fingerprint and a specificity gas chromatogram fingerprint of a tea sample to be identified and comparing by utilizing fingerprint computing software; based on the identification reference that the similarity between the liquid chromatogram fingerprint and the standard substance sample fingerprint and the similarity between the gas chromatogram fingerprint and the standard substance sample fingerprint are both higher than 80%, qualitatively and quantitatively identifying the genuineness and quality of the tea sample. By the implementation of the method, the practical restriction that the fake Biluochun tea from Tungting Mountains are hardly identified by the traditional identification method based on perception indexes, rationalization indexes, safety indexes and the like can be broken through, and the genuineness of the Biluochun tea from Tungting Mountains can be effectively and accurately identified, therefore the invention provides a solid guarantee for protecting geographical indication tea.
Description
Technical field
The present invention relates to belong to the discrimination method of special product a kind ofly, relate in particular to the application technology that a kind of chemical fingerprint belongs to special product discriminating aspect with being identified in.
Background technology
Dongting Lake (mountain) Biluochun tea (being title contained " Biluochun tea is produced in mountain region, Dongting Lake, Suzhou ") is one of topmost well-known tea of China.The bud-leaf delicacy of Dongting Lake (mountain) Biluochun tea, profile bar rope is very thin, is curled into spiral shell, fine and soft milli Bi Lu, endoplasm soup look bright-coloured, and the fragrance aquatic foods are dense, and the bright alcohol of flavour is light green bright at the bottom of the leaf, and the title of " tender three delicacies " is arranged.This is by its unique ecological environment and gather and process the technology decision.
Except Dongting Lake (mountain) Biluochun tea in Suzhou, the whole nation has the place, many places also to produce " Pilochun (a green tea) " green tea.Because the outstanding advantage of Dongting Lake (mountain) Biluochun tea on brand, quality is flooded with a large amount of other " Pilochun (a green tea) " counterfeit Dongting Lake (mountain) Biluochun teas on market.Yet standard GB/T 18957-2008F geographical sign product--sense index in the Biluochun tea of Dongting Lake (mountain), physical and chemical index, safety index etc. can not specific differentiation Dongting Lake (mountain) Biluochun tea and other real estates " Pilochun (a green tea) ".
For tealeaves, traditional sensory evaluation, or the method for measuring one or several chemical composition content can't be made holistic approach and evaluation to tea quality.Therefore, study and seek a kind of tea product discriminating method of energy specificity differentiation geographical sign product, for the market sale of protection local Dongting Lake (mountain) Biluochun tea, can provide more practical law evidence.
Summary of the invention
Defective in view of above-mentioned prior art existence; the objective of the invention is to propose the specificity discrimination method that Biluochun tea is produced in mountain region, Dongting Lake, a kind of Suzhou; the means of applied science are excavated the tealeaves finger-print and are come specific differentiation geographical sign product, protect the geographical sign product better to reach.
Purpose of the present invention will be achieved by the following technical programs:
The specificity discrimination method of Biluochun tea is produced in mountain region, Dongting Lake, a kind of Suzhou, it is characterized in that: the tea product that adopt primary population preparation in the protection domain meet standard GB/T 18957-2008F geographical sign tea product regulation are as standard material object sample, and extract its finger-print as the reference group of comparing; Tea sample to required discriminating extracts specificity liquid-phase chromatograph finger print atlas and specificity gas chromatography finger-print respectively, and utilization finger-print software for calculation is compared; Being 80% or more with two finger-print relative standards sample finger-print in kind similarities of liquid and gas serve as the discriminating benchmark, true and false, the quality of qualitative, quantitative ground discriminating tea sample.
Further, the specificity liquid-phase chromatograph finger print atlas of the tea sample of required discriminating is based on specific liquid phase chromatogram condition realizes extracting, described specific liquid phase chromatogram condition is with C8, C18 or connatural reverse chromatograms post, consist of moving phase with organic phase, water, correctives and carry out the program wash-out, and to detect the UV-detector of wavelength 210nm-660nm, record collection of illustrative plates peak area and retention time; Comprise the predetermined substance that component is at least Tea Polyphenols, caffeine, catechin and tannic acid in the described specificity liquid-phase chromatograph finger print atlas.
Further, organic phase is at least acetonitrile, methyl alcohol or ethanol described in the composition of above-mentioned moving phase; Described water is at least water, phosphate buffered solution or citrate buffer solution; Described correctives is at least one or more in alkyl sodium sulfonate, trifluoroacetic acid, acetic acid, the phosphoric acid.
Further, the specificity gas chromatography finger-print of the tea sample of required discriminating is based on specific GC conditions realizes extracting, described specific liquid phase chromatogram condition is with DB-1, DB-5, DB-17 or connatural capillary column, injector temperature 80-300 ℃, make column temperature 40-300 ℃ of intensification by program, the utilization hydrogen flame detector detects sample introduction with 100-350 ℃ detected temperatures, record collection of illustrative plates peak area and retention time; Comprise the predetermined substance that component is at least hexanal, enanthaldehyde, dimethyl pyrazine, aldehyde C-9, acetate, furfural, capraldehyde, fragrant camphor tree alcohol, longifolene, geraniol, phenmethylol, jasmone, trimethyl-15 ketone and indoles in the described specificity gas chromatography finger-print.
Further; described standard sample in kind comprises that primary population different mining is plucked the two or more tea product of preparation in period in the protection domain; in the discrimination process of qualitative, quantitative; the finger-print of the finger-print of sample liquid phase or gas phase and various tea product is compared separately; so that look younger a kind of similarity of tea product wherein is and is discriminating benchmark, true and false, the quality of discriminating tea sample 80% or more.
The enforcement of the above-mentioned specificity discrimination method of the present invention, broken through traditional discrimination method and be difficult to distinguish specifically the practical limit of distinguishing counterfeit Dongting Lake (mountain) Biluochun tea based on sense index, physical and chemical index, safety index etc., by setting up and the cover standard of sharing sample finger-print in kind, only need the sample of required discriminating to be carried out extraction, the comparison of specificity finger-print by simple method, get final product high accuracy ground and differentiate the true and false and quality of tea sample, the effect superiority is remarkable.
Embodiment
The present invention relates to a kind of chemical fingerprint of tea.In recent years people's new method of utilizing the chemical fingerprint analytical technology to be used for comprehensive evaluation natural products quality grows up.The chemical fingerprint analysis is not equal to general instrumental analysis, it is obtained by finger-print usually and finger-print differentiates that calculating two parts is formed, finger-print obtains instrument analytical methods such as being meant employing chromatogram, spectrum and coupling, obtains the component population analysis spectrogram or the image that can characterize the sample chemical composition characteristic; Finger-print differentiates that calculating is that utilization computational analysis technology is handled the spectral data that is obtained, by screening and simplification, obtain exclusive, macroscopical, whole chemical feature integrated information, and the total ripple situation that sample chemical is formed estimated and estimate therefore, after having obtained the sample finger-print, evaluate the global similarity degree between each batch products finger-print, their peculiar quality index of natural products such as the otherness of chemical composition and fluctuation situation separately of quantitative description.Utilize finger-print promptly to estimate its specific material.
Technical solution of the present invention is achieved in that the specificity discrimination method of mountain region, Dongting Lake, a kind of Suzhou product Biluochun tea, comprises following steps:
One, Dongting Lake (mountain) Biluochun tea is differentiated the foundation with reference to the storehouse:
Employing meets the tea product of primary population preparation in the protection domain of standard GB/T 18957-2008F geographical sign tea product regulation as standard sample in kind, and extracts its finger-print as the reference group of comparing.Wherein standard sample in kind comprises that primary population different mining is plucked the two or more tea product of preparation in period in the protection domain, and the finger-print that various tea product are extracted is as indicating in the standard form ground that the discriminating of tea product is with reference to the storehouse.
Two, obtaining of Biluochun tea liquid-phase chromatograph finger print atlas to be checked:
Get the tealeaves sample and in triangular flask, add the water ultrasonic extraction, control temperature simultaneously and be no more than 80 degree, obtain test specimens liquid after the secondary filter.
Liquid phase chromatogram condition: with C8, C18 or with the reverse-phase chromatographic column of its similar performance, moving phase consists of organic phase: water: correctives, the program wash-out, UV-detector detects wavelength 210nm-660nm, sampling liquid is injected in the injector, the record collection of illustrative plates.The composition that records has: Tea Polyphenols, caffeine, catechin, tannic acid etc.
The liquid-phase chromatograph finger print atlas of tealeaves sample and the finger-print utilization finger-print software for calculation of Dongting Lake (mountain) Biluochun tea material standard sample are compared, get its similarity.
Three, obtaining of Biluochun tea gas chromatography finger-print to be checked:
Get the reflux extraction in tool plug triangular flask of tealeaves sample, obtain test specimens liquid after the secondary filter.
GC conditions: with DB-1, DB-5, DB-17 or with the capillary column of its similar performance; Injector temperature is greater than 80 degree; The column oven temperature is greater than 40 degree, temperature programme; Detector temperature is greater than 100 degree; Detect with hydrogen flame detector (FID); Sample introduction, the record collection of illustrative plates.The composition that records has: aldehyde, enanthaldehyde, dimethyl pyrazine, aldehyde C-9, acetate, furfural, capraldehyde, fragrant camphor tree alcohol, longifolene, geraniol, phenmethylol, jasmone, trimethyl-15 ketone, indoles etc.
The gas chromatography finger-print of tealeaves sample and the finger-print utilization finger-print software for calculation of Dongting Lake (mountain) Biluochun tea material standard sample are compared, get its similarity.
Have only similarity to be more than 80%, can regard as Dongting Lake (mountain) Biluochun tea when the finger-print of the liquid-phase chromatograph finger print atlas of tealeaves sample and gas phase chromatographic fingerprinting and Dongting Lake (mountain) Biluochun tea material standard sample.Pluck the material standard sample tea product not of the same race in period for difference, the independent comparison mode of above-mentioned comparison for dividing by kind, and so that look younger that a kind of similarity of tea product wherein is 80% or more is the discriminating benchmark, true and false, the quality of discriminating tea sample.
The specificity discrimination method of Dongting Lake of the present invention (mountain) Biluochun tea will represent more intuitively by following two specific embodiments:
Embodiment one
Get tealeaves sample about 2 and restrain to the 50ml triangular flask and add water 20ml ultrasonic extraction 60 minutes, control temperature 60 degree obtain test specimens liquid after the secondary filter.
Liquid phase chromatogram condition: use the ODS chromatographic column, moving phase 50% acetonitrile solution wash-out, UV-detector detects wavelength 260nm, sample size 20 μ l, record collection of illustrative plates peak area and retention time.
The collection of illustrative plates of tealeaves sample and the collection of illustrative plates utilization finger-print software for calculation of Dongting Lake (mountain) Pilochun (a green tea) difference material standard sample are compared, and getting both similarities is 85%.
Other gets tealeaves sample about 3 and restrains the 30ml reflux extraction 60 minutes that adds diethyl ether to the 100ml tool plug triangular flask, obtains test specimens liquid after the secondary filter.
GC conditions: use the DB-5 capillary chromatographic column, injector temperature 220 degree, column temperature is from 60 minutes program to 150 degree of 45 degree, detector temperature 250 degree, hydrogen flame detector, sample size 1 μ l, record collection of illustrative plates peak area and retention time.
The collection of illustrative plates of tealeaves sample and the collection of illustrative plates utilization finger-print software for calculation of Dongting Lake (mountain) Pilochun (a green tea) material standard sample are compared, get two similarities 90%.
Judge conclusion: this tealeaves sample is Dongting Lake (mountain) Biluochun tea.
Embodiment two
Get tealeaves sample about 5 and restrain to the 100ml triangular flask and add water 20ml ultrasonic extraction 90 minutes, control temperature 80 degree obtain test specimens liquid after the secondary filter.
Liquid phase chromatogram condition: use the C8 chromatographic column, moving phase 50% methanol aqueous solution wash-out, UV-detector detects wavelength 254nm, sample size 10 μ l, record collection of illustrative plates peak area and retention time.
The collection of illustrative plates of tealeaves sample and the collection of illustrative plates utilization finger-print software for calculation of Dongting Lake (mountain) Pilochun (a green tea) material standard sample are compared, and getting both similarities is 90%.
Other gets tealeaves sample about 5 and restrains the 50ml reflux extraction 60 minutes that adds diethyl ether to the 100ml tool plug triangular flask, obtains test specimens liquid after the secondary filter.
GC conditions: use the DB-1 capillary chromatographic column, injector temperature 200 degree, column temperature is from 60 minutes program to 180 degree of 45 degree, detector temperature 260 degree, hydrogen flame detector, sample size 1 μ l, record collection of illustrative plates peak area and retention time.
The collection of illustrative plates of tealeaves sample and the collection of illustrative plates utilization finger-print software for calculation of Dongting Lake (mountain) Pilochun (a green tea) material standard sample are compared, get two similarities 60%.
Judge conclusion: this tealeaves sample is not Dongting Lake (mountain) Pilochun (a green tea).
Specificity discrimination method of the present invention can be finished the tealeaves sample at short notice and differentiate detection, and this method accurately and reliably, and high specificity is easy and simple to handle.
The foregoing description only is explanation technical conceive of the present invention and characteristics; its purpose is to allow the personage that is familiar with this technology can understand content of the present invention and is implemented; can not limit protection scope of the present invention with this; all equivalences that spirit is done according to the present invention change or modify, and all should be encompassed in protection scope of the present invention.
Claims (5)
1. the specificity discrimination method of Biluochun tea is produced in mountain region, Dongting Lake, a Suzhou, it is characterized in that: the tea product that adopt primary population preparation in the protection domain meet standard GB/T 18957-2008F geographical sign tea product regulation are as standard material object sample, and extract its finger-print as the reference group of comparing; Tea sample to required discriminating extracts specificity liquid-phase chromatograph finger print atlas and specificity gas chromatography finger-print respectively, and utilization finger-print software for calculation is compared; Being 80% or more with two finger-print relative standards sample finger-print in kind similarities of liquid and gas serve as the discriminating benchmark, true and false, the quality of qualitative, quantitative ground discriminating tea sample.
2. the specificity discrimination method of Biluochun tea is produced in mountain region, Dongting Lake, a kind of Suzhou according to claim 1, it is characterized in that: the specificity liquid-phase chromatograph finger print atlas of the tea sample of required discriminating is based on specific liquid phase chromatogram condition realizes extracting, described specific liquid phase chromatogram condition is with C8, C18 or connatural reverse-phase chromatographic column, consist of moving phase with organic phase, water, correctives and carry out the program wash-out, and to detect the UV-detector of wavelength 210nm-660nm, record collection of illustrative plates peak area and retention time; Comprise the predetermined substance that component is at least Tea Polyphenols, caffeine, catechin and tannic acid in the described specificity liquid-phase chromatograph finger print atlas.
3. the specificity discrimination method of Biluochun tea is produced in mountain region, Dongting Lake, a kind of Suzhou according to claim 2, and it is characterized in that: in the composition of moving phase, described organic phase is at least acetonitrile, methyl alcohol or ethanol; Described water is at least water, phosphate buffered solution or citrate buffer solution; Described correctives is at least one or more in alkyl sodium sulfonate, trifluoroacetic acid, acetic acid, the phosphoric acid.
4. the specificity discrimination method of Biluochun tea is produced in mountain region, Dongting Lake, a kind of Suzhou according to claim 1, it is characterized in that.The specificity gas chromatography finger-print of the tea sample of required discriminating is based on specific GC conditions realizes extracting, described specific liquid phase chromatogram condition is with DB-1, DB-5, DB-17 or connatural capillary column, injector temperature 80-300 ℃, make column temperature 40-300 ℃ of intensification by program, the utilization hydrogen flame detector detects sample introduction with 100-350 ℃ detected temperatures, record collection of illustrative plates peak area and retention time; Comprise the predetermined substance that component is at least hexanal, enanthaldehyde, dimethyl pyrazine, aldehyde C-9, acetate, furfural, capraldehyde, fragrant camphor tree alcohol, longifolene, geraniol, phenmethylol, jasmone, trimethyl-15 ketone and indoles in the described specificity gas chromatography finger-print.
5. the specificity discrimination method of Biluochun tea is produced in mountain region, Dongting Lake, a kind of Suzhou according to claim 1; it is characterized in that: described standard sample in kind comprises that primary population different mining is plucked the two or more tea product of preparation in period in the protection domain; in the discrimination process of qualitative, quantitative; the finger-print of the finger-print of sample liquid phase or gas phase and various tea product is compared separately; so that look younger a kind of similarity of tea product wherein is and is discriminating benchmark, true and false, the quality of discriminating tea sample 80% or more.
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| CN105738505A (en) * | 2016-02-03 | 2016-07-06 | 长沙理工大学 | Detection method for volatile spice ingredients in coriander |
| CN108152386A (en) * | 2017-11-13 | 2018-06-12 | 信阳农林学院 | Miniature region tea-leaf producing area recognition methods and application based on fingerprint pattern technology |
| CN113834886A (en) * | 2021-09-06 | 2021-12-24 | 中国农业科学院茶叶研究所 | Detection method for rapidly and accurately quantifying nitrogen-oxygen heterocyclic compounds in green tea and evaluation method for dryness degree of green tea |
| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105738505A (en) * | 2016-02-03 | 2016-07-06 | 长沙理工大学 | Detection method for volatile spice ingredients in coriander |
| CN108152386A (en) * | 2017-11-13 | 2018-06-12 | 信阳农林学院 | Miniature region tea-leaf producing area recognition methods and application based on fingerprint pattern technology |
| CN113834886A (en) * | 2021-09-06 | 2021-12-24 | 中国农业科学院茶叶研究所 | Detection method for rapidly and accurately quantifying nitrogen-oxygen heterocyclic compounds in green tea and evaluation method for dryness degree of green tea |
| CN113834886B (en) * | 2021-09-06 | 2022-12-20 | 中国农业科学院茶叶研究所 | Detection method for rapidly and accurately quantifying nitrogen-oxygen heterocyclic compounds in green tea and evaluation method for dryness degree of green tea |
| 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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Application publication date: 20111123 |