CN108169376A - A kind of method of Rapid identification Wuyi cliff tea and its tea perfume fine work matter - Google Patents
A kind of method of Rapid identification Wuyi cliff tea and its tea perfume fine work matter Download PDFInfo
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- CN108169376A CN108169376A CN201711476690.8A CN201711476690A CN108169376A CN 108169376 A CN108169376 A CN 108169376A CN 201711476690 A CN201711476690 A CN 201711476690A CN 108169376 A CN108169376 A CN 108169376A
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- wuyi cliff
- wuyi
- cliff tea
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas chromatography
Abstract
The invention discloses a kind of Rapid identification Wuyi cliff tea and its methods of essence quality.This method prepares the Chinese cassia tree millet paste sample, using Headspace solid-phase microextraction GC/MS by Different Extraction Method first using a kind of Wuyi Chinese cassia tree as raw material（HS‑SPME/GC‑MS）Detect aroma volatile in sample.Secondly, it designs and prepares subjective appreciation standard sample, subjective appreciation is carried out according to subjective appreciation standard sample.Finally, it is that X matrix carries out successive Regression by Y matrixes, volatile component content of results of sensory evaluation（SR）Analysis obtains regression model, and the model prediction ability is verified, the results showed that the model can carry out Accurate Prediction to Wuyi Chinese cassia tree tealeaves and essence aroma strength.The present invention can realize the fast and accurately evaluation to Wuyi cliff tea and tea perfume fine work matter, use easy to spread.
Description
Technical field
The invention belongs to tealeaves and essence quality identification fields, and subjective appreciation is carried out especially by established standards, with reference to
GC-MS by the way of successive Regression, establishes the recurrence of Wuyi cliff tea and essence quality prediction to volatile ingredient testing result
Model.
Background technology
In China, tea making is had tea as long as having had thousand, and is had tea and had become a kind of custom, to tea leaf quality requirement
Also it is higher and higher.One of an important factor for fragrance is influence tea leaf quality, the research temperature of tea perfume gas is growing on and on.Wuyi cliff tea
It gives off a strong fragrance fresh sharp, fragrant benefit long is clear, is one of national well-known tea, the top grade of oolong tea.Relative amount is higher in Wuyi cliff tea
Volatile ingredient have dihydroactinidiolide, benzyl alcohol, benzyl carbinol, nerolidol, indoles etc..
With the rise of tea beverage, research hotspot is also become with preparing to the research of tea perfume essence.Tea beverage processing technology mistake
Cheng Zhonghui makes the loss of tea perfume gas, leads to the reduction of tea beverage quality.Therefore it needs to add tea perfume essence in tea beverage process
It is allocated.The quality of tea perfume essence has great influence to tea beverage quality.
The present invention carries out subjective appreciation by established standards, with reference to GC-MS to volatile ingredient testing result, using gradually
The mode of recurrence establishes regression model, can realize the quick and precisely identification to Wuyi cliff tea and tea perfume fine work matter.
Invention content
The purpose of the invention is to provide a kind of method of Rapid identification Wuyi cliff tea and its essence quality.
To achieve these goals, the present invention provides technical solution：
（1）90 groups of Wuyi Chinese cassia tree millet paste samples, headspace solid-phase microextraction are prepared by different extracting modes（HS-SPME）It is enriched with tea
Volatile ingredient in soup, gas chromatography-mass spectrography（GC-MS）Volatile ingredient is detected, detects 89 peaks altogether.
（2）Subjective appreciation is carried out to prepared millet paste sample.
（3）Using results of sensory evaluation as Y matrixes, 89 shared peak contents are X matrix, carry out regression analysis, obtain Wuyi
The regression model of rock tea and essence quality identification.
（4）The verification of prediction model.
90 Wuyi cliff tea millet paste sample GC-MS detections, include the following steps：
（1）The enrichment of Wuyi cliff tea volatile ingredient：
2g NaCl are weighed in 15ml sample bottles, sequentially add magnetic rotor, 5.9ml millet paste sample, 100 μ L 0.0625mL/
L sec-n-octyl alcohol internal standards.Then extracting head is inserted into sample bottle, water-bath balance 10min, is then released in 50 DEG C of magnetic stirring apparatus
The good fiber head headspace extraction 40min of aging.Finally parsed at 250 DEG C in gas chromatograph-mass spectrometer (GC-MS) injection port
5min starts simultaneously at operation program and carries out data acquisition.
（2）The GC-MS testing conditions of Wuyi cliff tea volatile ingredient：
Chromatographic condition：Chromatographic column HP-5MS capillary columns (30 m × 0.25 μm × 0.25 mm)；Temperature program：Starting
Temperature 50 C keeps 6 min, 90 DEG C is warming up to, then be warming up to 180 DEG C with 3 DEG C/min with 2 DEG C/min；Injector temperature 250
℃；Manual split sampling, split ratio 20:1；The solvent delay time：5 min；Carrier gas is high-purity He purity 99.999%.
Mass Spectrometry Conditions：230 DEG C of ion source temperature；Level four bars temperature：150℃；Scan pattern：Full scan；Mass scanning model
It encloses：m/z 30-550.
（3）GC-MS analysis methods：
The GC-MS testing results of all millet paste samples are composed library with NIST.11L to retrieve, library searching result is according to reservation
Time and No. CAS, which merge, to summarize, and finds out 89 peaks altogether.Volatile ingredient in each sample is calculated with internal standard semiquantitative method
Content.
The present invention remarkable result be：The present invention detects 89 kinds of volatile ingredients of Wuyi cliff tea and its content, with 90
The volatile component content of sample is X matrix, and results of sensory evaluation is Y matrixes, establish Wuyi cliff tea and essence quality by
Walk regression model.The related coefficient of model（R2）It is 0.880.Show model-fitting degree height.Model prediction proficiency testing result
It shows the ＜ F crit 0.05=5.317655 of F=0.015157, illustrates that model has good predictive ability, can realize pair
The quick and precisely judgement of Wuyi cliff tea and essence quality.
Description of the drawings
Fig. 1 is the scatter plot of regression result and results of sensory evaluation based on 90 samples, 89 components.
Specific embodiment
Embodiment 1
1. sample and instrument
1.1 sample：Wuyi cliff tea（Chinese cassia tree）, provided by Fujian Gong Tai Tea Industry Co., Ltd.
1.2 instrument：BL150 electronic balances, Sartorius AG；SPME solid phase microextraction handles, the U.S.
Supelco companies；50/30umDVB/CAR/PDMS extracting heads, Supelco companies of the U.S.；DF-1 heat-collecting magnetic stirring devices, gold
Altar city Xin Nuo laboratory apparatus factory；7890B gas-chromatographies and 5977A mass spectrums, Anjelen Sci. ＆ Tech. Inc of the U.S..
2. experimental method
The enrichment of 2.1 Wuyi cliff tea volatile ingredients：
2g Nacl are weighed in 15ml sample bottles, sequentially add magnetic rotor, the millet paste sample that 5.9ml has been prepared, 100 μ L
0.0625mL/L sec-n-octyl alcohol internal standards.Then extracting head is inserted into sample bottle, the water-bath balance 10min in 50 DEG C of magnetic stirring apparatus,
Then the good fiber head headspace extraction 40min of aging is released.Finally in gas chromatograph-mass spectrometer (GC-MS) injection port in 250 DEG C
Lower parsing 5min starts simultaneously at operation program and carries out data acquisition.
The GC-MS testing conditions of 2.2 Wuyi cliff tea volatile ingredients：
Chromatographic condition：Chromatographic column HP-5MS capillary columns (30 m × 0.25 μm × 0.25 mm)；Temperature program：Starting
Temperature 50 C keeps 6 min, 90 DEG C is warming up to, then be warming up to 180 DEG C with 3 DEG C/min with 2 DEG C/min；Injector temperature 250
℃；Manual split sampling, split ratio 20:1；The solvent delay time：5 min；Carrier gas is high-purity He purity 99.999%.
Mass Spectrometry Conditions：230 DEG C of ion source temperature；Level four bars temperature：150℃；Scan pattern：Full scan；Mass scanning model
It encloses：m/z 30-550.
2.3 GC-MS analysis methods：
The GC-MS testing results of all millet paste samples are composed library with NIST.11L to retrieve, library searching result is according to reservation
Time and No. CAS, which merge, to summarize, and finds out 89 peaks altogether.Volatile ingredient in each sample is calculated with internal standard semiquantitative method
Content.
2.4 GC-MS precision tests：
The highest preceding 3 kinds of volatile ingredients of content and sec-n-octyl alcohol in the Wuyi cliff tea millet paste obtained to the extraction of continuous 15 boiling water
（Internal standard）Retention time analyzed, the precision of this method is verified.When as a result showing that 4 kinds of volatile ingredients retain
Between coefficient of variation CV values in 0.003%-0.115%, illustrate that this method has higher precision.
2.5 subjective appreciation
（1）It is as former state 10 points to define millet paste, with water in mass ratio 9:1、8:2、7:3、6:4、5:5、4:6、3:7、2:8、1:9 is mixed
The sample of conjunction is respectively defined as the standard that 9,8,7,6,5,4,3,2,1 points are subjective appreciation, and 8ml standard samples is taken to be centrifuged in 10ml
It is spare in pipe.
（2）Health, noninductive official's planar defect are picked out, there are 5 personnel of interest for being engaged in organoleptic analysis to be felt
Official evaluates.
（3）Keep neat and tidy, drying in subjective appreciation room；Bright light；Air is fresh, free from extraneous odour.
（4）Indoor temperature is made to maintain 20 DEG C ~ 25 DEG C using air-conditioning equipment, subjective appreciation personnel is kept to be in the most comfortable
State；The interference of external environment is reduced, noise is avoided to cause to divert one's attention and interfere to subjective appreciation personnel.
（5）Influencing each other between evaluating member is avoided, evaluating member is respectively independently evaluated.
（6）8ml samples are taken in 10ml centrifuge tubes, and are encoded at random, subjective appreciation personnel carry out smelling for the first time
Afterwards, it is compared with similar standard sample, final score retains a decimal.
（7）To avoid evaluating member tired, each subjective appreciation time control is within 20min.
Results of sensory evaluation and GC-MS testing results are carried out stepwise regression analysis by 2.6, with the volatility of 90 samples
Component content is X matrix, and results of sensory evaluation is Y matrixes, establishes Wuyi cliff tea and the Gradual regression analysis model of essence quality.Mould
The related coefficient of type（R2）It is 0.880.Show model-fitting degree height.
The verification of 2.7 forecast of regression model abilities：Method according to 2.1-2.4 prepares millet paste, and carries out GC-MS detections
And subjective appreciation, GC-MS testing results are brought into 2.6 obtained regression models, score value is obtained and is carried out with results of sensory evaluation
One-way analysis of variance as a result, it has been found that simultaneously there was no significant difference for the two, illustrates that the model has good predictive ability, Ke Yishi
Now to the Accurate Prediction of Wuyi cliff tea and essence quality.
1 forecast of regression model proficiency testing experimental result of table
2 forecast of regression model ability one-way analysis of variance result of table
Claims (4)
1. a kind of method of Rapid identification Wuyi cliff tea and its essence quality, which is characterized in that include the following steps：
（1）Changing Extracting temperature, time, solid-liquid ratio and macroreticular resin are inhaled in millet paste and prepare 90 by way of volatile ingredient
Group Wuyi Chinese cassia tree millet paste sample, headspace solid-phase microextraction HS-SPME are enriched with volatile ingredient in millet paste, gas chromatography-mass spectrometry
Volatile ingredient is detected with GC-MS, detects 89 peaks altogether；
（2）Subjective appreciation is carried out to prepared millet paste sample；
（3）Using results of sensory evaluation as Y matrixes, 89 peak contents are X matrix, carry out regression analysis, obtain Wuyi cliff tea and perfume (or spice)
The regression model of smart quality identification；
（4）The verification of prediction model.
2. according to a kind of Rapid identification Wuyi cliff tea and its method of essence quality described in claim 1, which is characterized in that
The step（2）In subjective appreciation method be：It is as former state 10 points to define millet paste, with water in mass ratio 9:1、8:2、7:3、
6:4、5:5、4:6、3:7、2:8、1:The sample of 9 mixing is respectively defined as 9,8,7,6,5,4,3,2,1 points；As standard, by 5
Reviewer of the position by screening is to step（1）The millet paste of middle preparation scores.
3. according to a kind of Rapid identification Wuyi cliff tea and its method of essence quality described in claim 1, which is characterized in that
The step（3）In regression analysis using Stepwise Regression Method SR, establish Wuyi cliff tea and tea perfume fine work matter by
Regression model is walked, realizes the fast and accurately judgement to Wuyi cliff tea and tea perfume fine work matter.
4. according to a kind of Rapid identification Wuyi cliff tea and its method of essence quality described in claim 1, which is characterized in that
The step（4）In prediction model verification, the specific steps are：Using different brewing times, temperature and solid-liquid ratio system
Standby 5 groups of Wuyi cliff tea millet paste samples, by step（2）Subjective appreciation method carries out subjective appreciation, by results of sensory evaluation with returning
Model prediction result carries out one-way analysis of variance, determines the accuracy of prediction model.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109781893A (en) * | 2019-02-22 | 2019-05-21 | 中华全国供销合作总社济南果品研究院 | A kind of method of Rapid identification red date slices quality and processing method |
| CN110564507A (en) * | 2019-09-24 | 2019-12-13 | 福州大学 | Method for enriching aroma of black tea through dynamic adsorption of resin |
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| CN103076411A (en) * | 2013-01-07 | 2013-05-01 | 中国农业科学院茶叶研究所 | Analytical method for determining aromatic constituents in tea |
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| CN105572283A (en) * | 2015-12-21 | 2016-05-11 | 南京财经大学 | Analysis method for judging unpolished rice tea aroma quality |
| CN106053628A (en) * | 2016-05-16 | 2016-10-26 | 湖北省农业科学院农业质量标准与检测技术研究所 | Method for rapidly determining fragrance components of tea quantitatively and qualitatively |
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| US20070028935A1 (en) * | 2005-08-02 | 2007-02-08 | Wm. Wrigley Jr. Company | Screening method for the identification of compositions suitable for the treatment of oral cavity malodor associated with smoking a tobacco product |
| CN103076411A (en) * | 2013-01-07 | 2013-05-01 | 中国农业科学院茶叶研究所 | Analytical method for determining aromatic constituents in tea |
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| CN105572283A (en) * | 2015-12-21 | 2016-05-11 | 南京财经大学 | Analysis method for judging unpolished rice tea aroma quality |
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