CN105628799B - The analysis method of volatile component in a kind of tealeaves - Google Patents
The analysis method of volatile component in a kind of tealeaves Download PDFInfo
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- CN105628799B CN105628799B CN201410613599.6A CN201410613599A CN105628799B CN 105628799 B CN105628799 B CN 105628799B CN 201410613599 A CN201410613599 A CN 201410613599A CN 105628799 B CN105628799 B CN 105628799B
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Abstract
The present invention provides a kind of analysis method of volatile component in Pu'er tea, for solving the problems, such as that prior art has Pu'er raw tea and ripe tea quality is unmanageable.The analysis method of volatile component in the Pu'er tea of the present invention, due to obtaining the sample of volatile ingredient using distinct methods, then the chemical composition of volatile ingredient is measured using gaschromatographic mass spectrometry work station, carry out obtaining more volatile ingredient, and the relative amount of volatile ingredient is determined, be advantageous to the control of tea leaf quality.
Description
Technical field
The present invention relates to chemical composition detection technique field, in particular it relates in a kind of tealeaves volatile component analysis
Method.
Background technology
Pu'er tea be using the distinctive large leaf sun withering tea in Yunnan as raw material, using specific technique by after fermentation process and
Into.Pu'er tea is prevailing in all over the world because of its remarkable health-care efficacy.The volatility of Pu'er tea (including raw tea and ripe tea)
Component is to weigh one of Pu'er tea quality major criterion, the feedstock grade of Pu'er tea, the place of production, season, processing technology, storage when
Between and mode notable difference is caused to these volatile ingredients and content.But at present on Pu'er tea volatile ingredient composition still
Indefinite, the formulation to Pu'er tea quality standard brings certain difficulty.Thus, establish one kind and enter for Pu'er tea volatile component
The accurate qualitative and quantitative analysis method of row seems extremely important.
The content of the invention
Technical scheme is a kind of analysis method of volatile component in tealeaves used by solving the above problems.
The analysis method of volatile component, comprises the following steps in a kind of tealeaves provided by the invention：
Sample preparation steps：
Aqueous extraction step：By tea-leaf power, ultrasound extraction, suction filtration obtain water extraction solution in water；
Petroleum ether extraction step：Petroleum ether is added in the water extraction solution to be extracted, separation petroleum ether layer obtains oil
Ether extract sample；
Chlorform extraction step：Water layer of the water extraction solution after petroleum ether extraction is extracted with chloroform, obtains chloroform extraction
Thing sample；
Petroleum ether extraction step：By tea-leaf power, ultrasound extraction, suction filtration obtain ligroin extraction sample in petroleum ether；
Sample test step：
Using gas chromatography-mass spectrum work station respectively to the petroleum ether extract sample, chloroform extract sample, oil
Ether extract sample carries out analysis and obtains total ion current figure.
Preferably, the mass volume ratio of tea-leaf power and water described in the aqueous extraction step is：Tea-leaf power (g):Water
(ml)=1:(5-30).
Preferably, in the aqueous extraction step：Water extraction temperature is 80-100 DEG C, and the water extraction time is 30-60min.
Preferably, in the petroleum ether extraction step：Water extraction solution is 1 with petroleum ether volume ratio:(1-3).
In the chlorform extraction step：Chloroform is 1 with water layer volume ratio of the water extraction solution after petroleum ether extraction:3.
Preferably, the mass volume ratio of tea-leaf power and petroleum ether is described in the petroleum ether extraction step：Tealeaves
Powder (g):Water (ml)=1:(5-10).
Preferably, GC conditions are in described sample test step：
Carrier gas：He gas, flow velocity 1.2ml/min；Chromatographic column：Agilent HP-5MS；Sample introduction pattern：Constant current；Mode：No
Shunting；250 DEG C of injector temperature；250 DEG C of connector temperature；Column temperature gradient：45 DEG C of initial temperature, with 15 DEG C/min speed liter
Temperature keeps 1min, then is warming up to 240 DEG C with 5 DEG C/min speed to 210 DEG C, after with 10 DEG C/min speed be warming up to 300
DEG C, keep 6min.
Preferably, Mass Spectrometry Conditions are in described sample test step：
230 DEG C of electron bombardment source temperature, voltage 70eV；Mass scan range:50-2000AMU, 0.3s is scanned every time,
Every 0.2s.
The analysis method of volatile component in the tealeaves of the present invention, due to using petroleum ether extraction again after using water extraction, so
The chemical composition of volatile ingredient is measured using gas chromatography-mass spectrum work station afterwards, carries out obtaining more volatilization
Property composition, and the relative amount of volatile ingredient is determined, be advantageous to the control of tea leaf quality.
Brief description of the drawings
Fig. 1 is the volatilization for obtaining the tealeaves of Pu'er raw tea in sample in the embodiment of the present invention 1 using different extracting methods
The mass spectrogram of property component.
Fig. 2 is the volatilization for obtaining the tealeaves of Pu'er cooked tea in sample in the embodiment of the present invention 2 using different extracting methods
The mass spectrogram of property component.
Embodiment
To make those skilled in the art more fully understand technical scheme, below in conjunction with the accompanying drawings and specific embodiment party
Formula is described in further detail to the present invention.
Embodiment 1：
The present embodiment provides a kind of analysis method of volatile component in tealeaves, comprises the following steps：
Sample preparation steps：
Aqueous extraction step：The tea-leaf power 15g of the Pu'er raw tea of 50 mesh is weighed, adds 150ml water, it is ultrasonic at 100 DEG C
30min, 30min is then shaken, filter, take 50ml filtrates；
Petroleum ether extraction step：With the petroleum ether extraction of 150ml volumes, it is evaporated, is obtained using revolving instrument concentration at 25 DEG C
To the petroleum ether extract sample of light green color solid-state.
Chlorform extraction step：The aqueous solution crossed with the above-mentioned petroleum ether extraction of chloroform extraction of 3 times of volumes, extracts 3 times, merges
Chloroform extract, it is evaporated at 25 DEG C using revolving instrument concentration, obtains the chloroform extract of light green color powdery.
Petroleum ether extraction step：The tea-leaf power 15g of the Pu'er raw tea of 50 mesh is weighed, adds 150ml petroleum ethers, ultrasound
30min, 30min is then shaken, filter, take 50ml filtrates；It is evaporated at 25 DEG C using revolving instrument concentration, obtains bottle green oily
Ligroin extraction sample.
Sample test step：
Using gas chromatography-mass spectrum work station respectively to the petroleum ether extract sample, chloroform extract sample, oil
Ether extract sample carries out analysis and obtains total ion current figure.
Specifically, above-mentioned acquisition petroleum ether extract sample, chloroform extract sample, petroleum ether is dissolved respectively with methanol to carry
Thing sample is taken, then filters acquisition test sample respectively with 0.45 μm of filter membrane, three kinds of test samples distinguish sample introduction to Agilent
7200GC/Q-TOF type gas chromatography-mass spectrum work stations are tested；
Wherein, GC conditions are：
Carrier gas：He gas, flow velocity 1.2ml/min；Chromatographic column：Agilent HP-5MS(30m×0.25mm×0.25μm)；
Sample introduction pattern：Constant current；Input mode：Do not shunt；250 DEG C of injector temperature；250 DEG C of connector temperature；Column temperature gradient：Initial temperature
45 DEG C of degree, be warming up to 210 DEG C with 15 DEG C/min speed, keep 1min, then 240 DEG C are warming up to 5 DEG C/min speed, after with
10 DEG C/min speed is warming up to 300 DEG C, keeps 6min.
Mass Spectrometry Conditions are：
230 DEG C of electron bombardment source temperature, voltage 70eV；Mass scan range:50-2000AMU, 0.3s is scanned every time,
Every 0.2s.
The present embodiment tests the total ion current figure that three samples obtain and sees Fig. 1 respectively, wherein, a parts are petroleum ether extraction
The total ion current figure of thing sample, b parts are the total ion current figure of ligroin extraction sample, c parts are chloroform extract sample
Total ion current figure.
Preferably, in addition to each total ion current figure the step of processing obtains relative peak area is carried out.Specifically, using gas
The data handling system (MassHunter) that phase chromatography-mass spectroscopy work station carries will obtain maximum peak area and be defined as 100%, its
Its peak area uses to be represented relative to the relative value of the maximum peak area, is specifically shown in Table 1, wherein, for petroleum ether extract sample
Product and chloroform extract sample its maximum peak area tie element are caffeine, for its maximum peak face of ligroin extraction sample
Product tie element is desmosterol.
Using the mass spectrometric data storehouse of gas chromatography-mass spectrum work station retrieval matching and artificial solution are carried out to obtaining mass spectrogram
Analysis.Associated mass spectrometry data is checked, retention time, mass-to-charge ratio and relative peak area of quasi-molecular ions etc. are analyzed, with reference to
Fragment ion peak confirms to mass spectra peak respectively, composition corresponding to preliminary obtaining portion sub-prime spectral peak, is specifically shown in Table 1；Further
The relative amount that each composition can be obtained according to the relative area of each mass spectra peak.
Embodiment 2：
The present embodiment provides a kind of analysis method of volatile component in tealeaves, comprises the following steps：
Sample preparation steps：
Aqueous extraction step：The tea-leaf power 15g of the Pu'er cooked tea of 50 mesh is weighed, adds 150ml water, it is ultrasonic at 100 DEG C
30min, 30min is then shaken, filter, take 50ml filtrates；
Petroleum ether extraction step：With the petroleum ether extraction of 150ml volumes, it is evaporated, is obtained using revolving instrument concentration at 25 DEG C
To the petroleum ether extract sample of light green color solid-state.
Chlorform extraction step：The aqueous solution crossed with the above-mentioned petroleum ether extraction of chloroform extraction of 3 times of volumes, extracts 3 times, merges
Chloroform extract, it is evaporated at 25 DEG C using revolving instrument concentration, obtains the chloroform extract of light green color powdery.
Petroleum ether extraction step：The tea-leaf power 15g of the Pu'er cooked tea of 50 mesh is weighed, adds 150ml petroleum ethers, ultrasound
30min, 30min is then shaken, filter, take 50ml filtrates；It is evaporated at 25 DEG C using revolving instrument concentration, obtains bottle green oily
Ligroin extraction sample.
Sample test step：
Using gas chromatography-mass spectrum work station respectively to the petroleum ether extract sample, chloroform extract sample, oil
Ether extract sample carries out analysis and obtains total ion current figure.
Specifically, specifically, dissolved respectively with methanol above-mentioned acquisition petroleum ether extract sample, chloroform extract sample,
Ligroin extraction sample, acquisition test sample is then filtered respectively with 0.45 μm of filter membrane, three kinds of test sample difference sample introductions are extremely
Agilent7200GC/Q-TOF type gas chromatography-mass spectrum work stations are tested；
Wherein, GC conditions are：
Carrier gas：He gas, flow velocity 1.2ml/min；Chromatographic column：Agilent HP-5MS(30m×0.25mm×0.25μm)；
Sample introduction pattern：Constant current；Input mode：Do not shunt；250 DEG C of injector temperature；250 DEG C of connector temperature；Column temperature gradient：Initial temperature
45 DEG C of degree, be warming up to 210 DEG C with 15 DEG C/min speed, keep 1min, then 240 DEG C are warming up to 5 DEG C/min speed, after with
10 DEG C/min speed is warming up to 300 DEG C, keeps 6min.
Mass Spectrometry Conditions are：
230 DEG C of electron bombardment source temperature, voltage 70eV；Mass scan range:50-2000AMU, 0.3s is scanned every time,
Every 0.2s.
The present embodiment tests the total ion current figure that three samples obtain and sees Fig. 2 respectively, wherein, a parts are petroleum ether extraction
The total ion current figure of thing sample, b parts are the total ion current figure of ligroin extraction sample, c parts are chloroform extract sample
Total ion current figure.
Preferably, in addition to each total ion current figure the step of processing obtains relative peak area is carried out.Specifically, using gas
The data handling system (MassHunter) that phase chromatography-mass spectroscopy work station carries will obtain maximum peak area and be defined as 100%, its
Its peak area uses to be represented relative to the relative value of the maximum peak area, is specifically shown in Table 1, wherein, for petroleum ether extract sample
Product and chloroform extract sample its maximum peak area tie element are caffeine, for its maximum peak face of ligroin extraction sample
Product tie element is 9,12,15- octatecatrienoic acids.
Using the mass spectrometric data storehouse of gas chromatography-mass spectrum work station retrieval matching and artificial solution are carried out to obtaining mass spectrogram
Analysis.Associated mass spectrometry data is checked, retention time, mass-to-charge ratio and relative peak area of quasi-molecular ions etc. are analyzed, with reference to
Fragment ion peak confirms to mass spectra peak respectively, composition corresponding to preliminary obtaining portion sub-prime spectral peak, is specifically shown in Table 2；Further
The relative amount that each composition can be obtained according to the relative area of each mass spectra peak.
The present invention is by the measurement (embodiment 1) to volatile ingredient under Pu'er raw tea progress Different Extraction Method and to general
The measurement (embodiment 2) that the ripe tea of Pu'er tea carries out volatile ingredient under Different Extraction Method finds to extract using by above-mentioned water extraction-petroleum ether
Take-chloroform extraction method and petroleum ether extracting method be combined the sample for obtaining three kinds of volatile ingredients, it can detect to obtain more
Pu'er tea volatile ingredient, it is suitable for controlling the quality of Pu'er tea (including raw tea and ripe tea)；And pass through gas chromatography-mass spectrum
Work station obtains corresponding mass spectrogram, and the convenient quality to Pu'er tea carries out qualitative and quantitative control.
The Pu'er tea of table 1 life tea Different Extraction Method obtains volatile component and its retention time, peak area relative percentage
The puerh tea Different Extraction Method of table 2 obtains volatile component and its retention time, peak area relative percentage
It is understood that the principle that embodiment of above is intended to be merely illustrative of the present and the exemplary implementation that uses
Mode, but the invention is not limited in this.For those skilled in the art, the essence of the present invention is not being departed from
In the case of refreshing and essence, various changes and modifications can be made therein, and these variations and modifications are also considered as protection scope of the present invention.
Claims (6)
1. the analysis method of volatile component in a kind of Pu'er tea, it is characterised in that comprise the following steps：
Sample preparation steps：
Aqueous extraction step：By tea-leaf power, ultrasound extraction, suction filtration obtain water extraction solution in water；
Petroleum ether extraction step：Petroleum ether is added in the water extraction solution to be extracted, separation petroleum ether layer obtains petroleum ether extraction
Take thing sample；
Chlorform extraction step：Water layer of the water extraction solution after petroleum ether extraction is extracted with chloroform, obtains chloroform extract sample
Product；
Petroleum ether extraction step：By tea-leaf power, ultrasound extraction, suction filtration obtain ligroin extraction sample in petroleum ether；
Sample test step：
The petroleum ether extract sample, chloroform extract sample, petroleum ether are carried respectively using gas chromatography-mass spectrum work station
Take thing sample to carry out analysis and obtain total ion current figure；
GC conditions are in described sample test step：
Carrier gas：He gas, flow velocity 1.2ml/min；Chromatographic column：Agilent HP-5MS；Sample introduction pattern：Constant current；Input mode：No
Shunting；250 DEG C of injector temperature；250 DEG C of connector temperature；Column temperature gradient：45 DEG C of initial temperature, with 15 DEG C/min speed liter
Temperature keeps 1min, then is warming up to 240 DEG C with 5 DEG C/min speed to 210 DEG C, after with 10 DEG C/min speed be warming up to 300
DEG C, keep 6min；
Mass Spectrometry Conditions are in described sample test step：
230 DEG C of electron bombardment source temperature, voltage 70eV；Mass scan range:50-2000AMU, 0.3s is scanned every time, be spaced
0.2s。
2. the analysis method of volatile component in Pu'er tea as claimed in claim 1, it is characterised in that in the aqueous extraction step
The mass volume ratio of the tea-leaf power and water is：Tea-leaf power/g：Water/ml=1:(5-30).
3. the analysis method of volatile component in Pu'er tea as claimed in claim 1, it is characterised in that the aqueous extraction step
In：Water extraction temperature is 80-100 DEG C, and the water extraction time is 30-60min.
4. the analysis method of volatile component in Pu'er tea as claimed in claim 1, it is characterised in that the petroleum ether extraction
In step：Water extraction solution is 1 with petroleum ether volume ratio:(1-3).
5. the analysis method of volatile component in Pu'er tea as claimed in claim 1, it is characterised in that the chloroform extraction step
In rapid：Chloroform is 1 with water layer volume ratio of the water extraction solution after petroleum ether extraction:3.
6. the analysis method of volatile component in Pu'er tea as claimed in claim 1, it is characterised in that the petroleum ether extraction
The mass volume ratio of tea-leaf power described in step and petroleum ether is：Tea-leaf power/g:Water/ml=1:(5-10).
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1557841A (en) * | 2004-01-14 | 2004-12-29 | 中国农业科学院茶叶研究所 | Process for synthetic extraction of polysaccharides, tea-polyphenol, theanine, caffeine from tea |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1557841A (en) * | 2004-01-14 | 2004-12-29 | 中国农业科学院茶叶研究所 | Process for synthetic extraction of polysaccharides, tea-polyphenol, theanine, caffeine from tea |
Non-Patent Citations (4)
| Title |
|---|
| SDE-GC-MS法测定茶叶中的挥发成分;丁林芳等;《中国酿造》;20090831(第4期);第147-150页 * |
| SPME—GC—MS分析普洱茶的挥发性成分;罗发美等;《林产化学与工业》;20101031;第30卷(第5期);全文 * |
| 普洱茶抗氧化特性的初步研究;揭国良等;《茶叶》;20050331(第3期);全文 * |
| 普洱茶挥发性成分指纹图谱研究;吕海鹏等;《茶叶科学》;20140131;第34卷(第1期);全文 * |
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