CN105628799A - Method for analysis of volatile components in tea - Google Patents
Method for analysis of volatile components in tea Download PDFInfo
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- CN105628799A CN105628799A CN201410613599.6A CN201410613599A CN105628799A CN 105628799 A CN105628799 A CN 105628799A CN 201410613599 A CN201410613599 A CN 201410613599A CN 105628799 A CN105628799 A CN 105628799A
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Abstract
The present invention provides a method for analysis of volatile components in tea, and the method is used to solve the problems that the quality of raw Pu'er tea and cooked Pu'er tea is difficult to control in the prior art. According to the method for analysis of volatile components in Pu'er tea, samples of volatile components can be obtained by different methods, then a gas chromatography-mass spectrometry workstation is used for determination of chemical composition of the volatile components, many volatile components are obtained, the relative contents of the volatile components can be obtained, and the method is conducive to tea quality control.
Description
Technical field
The present invention relates to chemical composition detection technique field, in particular it relates to a kind of analysis method of volatile component in Folium Camelliae sinensis.
Background technology
Folium camelliae assamicae is that distinctive large leaf shines Folium Camelliae sinensis with Yunnan is raw material, adopts specific technique to process through after fermentation. Folium camelliae assamicae is prevailing in all over the world because of the health-care effect of its brilliance. The volatile component that Folium camelliae assamicae (includes raw tea and ripe tea) is to weigh one of Folium camelliae assamicae quality major criterion, the feedstock grade of Folium camelliae assamicae, the place of production, season, these volatile ingredients and content are caused notable difference by processing technique, the time deposited and mode. But the composition about Folium camelliae assamicae volatile ingredient is still not clear at present, and the formulation of Folium camelliae assamicae quality standard is brought certain difficulty. Thus, set up and a kind of carry out accurately qualitative for Folium camelliae assamicae volatile component and determine quantitative analysis method and seem extremely important.
Summary of the invention
Solve the problems referred to above and be employed technical scheme comprise that the analysis method of volatile component in a kind of Folium Camelliae sinensis.
The analysis method of volatile component in a kind of Folium Camelliae sinensis provided by the invention, comprises the following steps:
Sample preparation steps:
Aqueous extraction step: tea-leaf power ultrasonic lixiviate in water, sucking filtration are obtained water and carry solution;
Petroleum ether extraction step: carry solution addition petroleum ether at described water and extract, separate petroleum ether layer and obtain petroleum ether extraction matter sample;
Chlorform extraction step: extract described water with chloroform and carry solution water layer after petroleum ether extraction, it is thus achieved that chloroform extract sample;
Petroleum ether extraction step: tea-leaf power ultrasonic lixiviate in petroleum ether, sucking filtration are obtained Petroleum ether extraction matter sample;
Sample test step:
Gas chromatography-mass spectrum work station is adopted to be analyzed obtaining total ion current figure to described petroleum ether extraction matter sample, chloroform extract sample, Petroleum ether extraction matter sample respectively.
Preferably, tea-leaf power described in described aqueous extraction step with the mass volume ratio of water is: tea-leaf power (g): water (ml)=1:(5-30).
Preferably, in described aqueous extraction step: water temperature raising degree is 80-100 DEG C, it is 30-60min that water carries the time.
Preferably, in described petroleum ether extraction step: it is 1:(1-3 that water carries solution with petroleum ether volume ratio).
In described chlorform extraction step: it is 1:3 that chloroform and water put forward solution water layer volume ratio after petroleum ether extraction.
Preferably, tea-leaf power described in described Petroleum ether extraction step with the mass volume ratio of petroleum ether is: tea-leaf power (g): water (ml)=1:(5-10).
Preferably, in described sample test step, GC conditions is:
Carrier gas: He gas, flow velocity is 1.2ml/min; Chromatographic column: AgilentHP-5MS; Sample introduction pattern: constant current; Mode: do not tap; Injector temperature 250 DEG C; Connector temperature 250 DEG C; Column temperature gradient: initial temperature 45 DEG C, with the ramp of 15 DEG C/min to 210 DEG C, keeps 1min, then with the ramp of 5 DEG C/min to 240 DEG C, after with the ramp of 10 DEG C/min to 300 DEG C, keep 6min.
Preferably, in described sample test step, Mass Spectrometry Conditions is:
Electron bombardment source temperature 230 DEG C, voltage 70eV; Mass scan range: 50-2000AMU, scans 0.3s, interval 0.2s every time.
The analysis method of volatile component in the Folium Camelliae sinensis of the present invention, owing to using petroleum ether extraction after adopting water to carry again, then adopt gas chromatography-mass spectrum work station that the chemical composition of volatile ingredient is measured, carry out obtaining more volatile ingredient, and determine the relative amount of volatile ingredient, be conducive to the control of tea leaf quality.
Accompanying drawing explanation
Fig. 1 adopts different extracting method to obtain the mass spectrum of the volatile component of the Folium Camelliae sinensis of Pu'er raw tea in sample in the embodiment of the present invention 1.
Fig. 2 adopts different extracting method to obtain the mass spectrum of the volatile component of the Folium Camelliae sinensis of Folium camelliae assamicae (processed) in sample in the embodiment of the present invention 2.
Detailed description of the invention
For making those skilled in the art be more fully understood that technical scheme, below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.
Embodiment 1:
The present embodiment provides a kind of analysis method of volatile component in Folium Camelliae sinensis, comprises the following steps:
Sample preparation steps:
Aqueous extraction step: weigh the tea-leaf power 15g of the Pu'er raw tea of 50 orders, adds 150ml water, ultrasonic 30min, then jolting 30min at 100 DEG C, filters, take 50ml filtrate;
Petroleum ether extraction step: with the petroleum ether extraction of 150ml volume, use rotation to steam instrument concentration at 25 DEG C and be evaporated, obtain the petroleum ether extraction matter sample of light green color solid-state.
Chlorform extraction step: extract, with the chloroform of 3 times of volumes, the aqueous solution that above-mentioned petroleum ether extraction is crossed, extract 3 times, combined chloroform extract, uses rotation to steam instrument concentration at 25 DEG C and is evaporated, obtain the chloroform extract of light green color powdery.
Petroleum ether extraction step: weigh the tea-leaf power 15g of the Pu'er raw tea of 50 orders, adds 150ml petroleum ether, ultrasonic 30min, then jolting 30min, filters, take 50ml filtrate; Use rotation to steam instrument concentration at 25 DEG C to be evaporated, obtain the Petroleum ether extraction matter sample of bottle green oily.
Sample test step:
Gas chromatography-mass spectrum work station is adopted to be analyzed obtaining total ion current figure to described petroleum ether extraction matter sample, chloroform extract sample, Petroleum ether extraction matter sample respectively.
Specifically, above-mentioned acquisition petroleum ether extraction matter sample, chloroform extract sample, Petroleum ether extraction matter sample is dissolved respectively with methanol, then filtering acquisition test sample respectively with 0.45 ��m of filter membrane, three kinds of test sample sample introductions respectively are tested to Agilent7200GC/Q-TOF type gas chromatography-mass spectrum work station;
Wherein, GC conditions is:
Carrier gas: He gas, flow velocity is 1.2ml/min; Chromatographic column: AgilentHP-5MS (30m �� 0.25mm �� 0.25 ��m); Sample introduction pattern: constant current; Input mode: do not tap; Injector temperature 250 DEG C; Connector temperature 250 DEG C; Column temperature gradient: initial temperature 45 DEG C, with the ramp of 15 DEG C/min to 210 DEG C, keeps 1min, then with the ramp of 5 DEG C/min to 240 DEG C, after with the ramp of 10 DEG C/min to 300 DEG C, keep 6min.
Mass Spectrometry Conditions is:
Electron bombardment source temperature 230 DEG C, voltage 70eV; Mass scan range: 50-2000AMU, scans 0.3s, interval 0.2s every time.
The present embodiment is tested the total ion current figure of three samples acquisitions respectively and is seen Fig. 1, wherein, a part is the total ion current figure that total ion current figure, c part is chloroform extract sample that total ion current figure, b part is Petroleum ether extraction matter sample of petroleum ether extraction matter sample.
Preferably, also include carrying out each total ion current figure processing the step obtaining relative peak area. Specifically, adopt the data handling system (MassHunter) that gas chromatography-mass spectrum work station carries that acquisition maximum peak area is defined as 100%, other peak area adopts and represents relative to the relative value of this maximum peak area, it is specifically shown in table 1, wherein, it is caffeine for petroleum ether extraction matter sample and its maximum peak area tie element of chloroform extract sample, is desmosterol for its maximum peak area tie element of Petroleum ether extraction matter sample.
The mass spectrometric data storehouse utilizing gas chromatography-mass spectrum work station carries out retrieval coupling to obtaining mass spectrum and manually resolves. Check associated mass spectrometry data, the aspects such as the retention time of quasi-molecular ions, mass-to-charge ratio and relative peak area are analyzed, respectively mass spectra peak are confirmed in conjunction with fragment ion peak, the composition that preliminary obtaining portion sub-prime spectral peak is corresponding, be specifically shown in table 1; The relative amount of each composition further 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 Folium Camelliae sinensis, comprises the following steps:
Sample preparation steps:
Aqueous extraction step: weigh the tea-leaf power 15g of the Folium camelliae assamicae (processed) of 50 orders, adds 150ml water, ultrasonic 30min, then jolting 30min at 100 DEG C, filters, take 50ml filtrate;
Petroleum ether extraction step: with the petroleum ether extraction of 150ml volume, use rotation to steam instrument concentration at 25 DEG C and be evaporated, obtain the petroleum ether extraction matter sample of light green color solid-state.
Chlorform extraction step: extract, with the chloroform of 3 times of volumes, the aqueous solution that above-mentioned petroleum ether extraction is crossed, extract 3 times, combined chloroform extract, uses rotation to steam instrument concentration at 25 DEG C and is evaporated, obtain the chloroform extract of light green color powdery.
Petroleum ether extraction step: weigh the tea-leaf power 15g of the Folium camelliae assamicae (processed) of 50 orders, adds 150ml petroleum ether, ultrasonic 30min, then jolting 30min, filters, take 50ml filtrate; Use rotation to steam instrument concentration at 25 DEG C to be evaporated, obtain the Petroleum ether extraction matter sample of bottle green oily.
Sample test step:
Gas chromatography-mass spectrum work station is adopted to be analyzed obtaining total ion current figure to described petroleum ether extraction matter sample, chloroform extract sample, Petroleum ether extraction matter sample respectively.
Specifically, specifically, above-mentioned acquisition petroleum ether extraction matter sample, chloroform extract sample, Petroleum ether extraction matter sample is dissolved respectively with methanol, then filtering acquisition test sample respectively with 0.45 ��m of filter membrane, three kinds of test sample sample introductions respectively are tested to Agilent7200GC/Q-TOF type gas chromatography-mass spectrum work station;
Wherein, GC conditions is:
Carrier gas: He gas, flow velocity is 1.2ml/min; Chromatographic column: AgilentHP-5MS (30m �� 0.25mm �� 0.25 ��m); Sample introduction pattern: constant current; Input mode: do not tap; Injector temperature 250 DEG C; Connector temperature 250 DEG C; Column temperature gradient: initial temperature 45 DEG C, with the ramp of 15 DEG C/min to 210 DEG C, keeps 1min, then with the ramp of 5 DEG C/min to 240 DEG C, after with the ramp of 10 DEG C/min to 300 DEG C, keep 6min.
Mass Spectrometry Conditions is:
Electron bombardment source temperature 230 DEG C, voltage 70eV; Mass scan range: 50-2000AMU, scans 0.3s, interval 0.2s every time.
The present embodiment is tested the total ion current figure of three samples acquisitions respectively and is seen Fig. 2, wherein, a part is the total ion current figure that total ion current figure, c part is chloroform extract sample that total ion current figure, b part is Petroleum ether extraction matter sample of petroleum ether extraction matter sample.
Preferably, also include carrying out each total ion current figure processing the step obtaining relative peak area. Specifically, adopt the data handling system (MassHunter) that gas chromatography-mass spectrum work station carries that acquisition maximum peak area is defined as 100%, other peak area adopts and represents relative to the relative value of this maximum peak area, it is specifically shown in table 1, wherein, it is caffeine for petroleum ether extraction matter sample and its maximum peak area tie element of chloroform extract sample, is 9 for its maximum peak area tie element of Petroleum ether extraction matter sample, 12,15-jeceric acid.
The mass spectrometric data storehouse utilizing gas chromatography-mass spectrum work station carries out retrieval coupling to obtaining mass spectrum and manually resolves. Check associated mass spectrometry data, the aspects such as the retention time of quasi-molecular ions, mass-to-charge ratio and relative peak area are analyzed, respectively mass spectra peak are confirmed in conjunction with fragment ion peak, the composition that preliminary obtaining portion sub-prime spectral peak is corresponding, be specifically shown in table 2; The relative amount of each composition further can be obtained according to the relative area of each mass spectra peak.
The present invention by Pu'er raw tea is carried out volatile ingredient under Different Extraction Method measurement (embodiment 1) and Folium camelliae assamicae (processed) is carried out the measurement (embodiment 2) of volatile ingredient under Different Extraction Method find to adopt above-mentioned water is carried-petroleum ether extraction-chloroform extraction method and Petroleum ether extraction method combine and obtain the sample of three kinds of volatile ingredients, can detect and obtain more Folium camelliae assamicae volatile ingredient, be suitable for controlling the quality of Folium camelliae assamicae (including raw tea and ripe tea); And obtaining corresponding mass spectrum by gas chromatography-mass spectrum work station, the convenient quality to Folium camelliae assamicae carries out qualitative and quantitative control.
The raw tea Different Extraction Method of table 1 Folium camelliae assamicae obtains volatile component and retention time, peak area relative percentage
Table 2 puerh tea Different Extraction Method obtains volatile component and retention time, peak area relative percentage
It is understood that the principle that is intended to be merely illustrative of the present of embodiment of above and the illustrative embodiments that adopts, but the invention is not limited in this. For those skilled in the art, without departing from the spirit and substance in the present invention, it is possible to make various modification and improvement, these modification and improvement are also considered as protection scope of the present invention.
Claims (8)
1. the analysis method of volatile component in a Folium Camelliae sinensis, it is characterised in that comprise the following steps:
Sample preparation steps:
Aqueous extraction step: tea-leaf power ultrasonic lixiviate in water, sucking filtration are obtained water and carry solution;
Petroleum ether extraction step: carry solution addition petroleum ether at described water and extract, separate petroleum ether layer and obtain petroleum ether extraction matter sample;
Chlorform extraction step: extract described water with chloroform and carry solution water layer after petroleum ether extraction, it is thus achieved that chloroform extract sample;
Petroleum ether extraction step: tea-leaf power ultrasonic lixiviate in petroleum ether, sucking filtration are obtained Petroleum ether extraction matter sample;
Sample test step:
Gas chromatography-mass spectrum work station is adopted to be analyzed obtaining total ion current figure to described petroleum ether extraction matter sample, chloroform extract sample, Petroleum ether extraction matter sample respectively.
2. the analysis method of volatile component in Folium Camelliae sinensis as claimed in claim 1, it is characterized in that, the mass volume ratio of tea-leaf power described in described aqueous extraction step and water is: tea-leaf power (g): water (ml)=1:(5-30).
3. the analysis method of volatile component in Folium Camelliae sinensis as claimed in claim 1, it is characterised in that in described aqueous extraction step: water temperature raising degree is 80-100 DEG C, it is 30-60min that water carries the time.
4. the analysis method of volatile component in Folium Camelliae sinensis as claimed in claim 1, it is characterised in that in described petroleum ether extraction step: it is 1:(1-3 that water carries solution with petroleum ether volume ratio).
5. the analysis method of volatile component in Folium Camelliae sinensis as claimed in claim 1, it is characterised in that in described chlorform extraction step: it is 1:3 that chloroform and water put forward solution water layer volume ratio after petroleum ether extraction.
6. the analysis method of volatile component in Folium Camelliae sinensis as claimed in claim 1, it is characterized in that, the mass volume ratio of tea-leaf power described in described Petroleum ether extraction step and petroleum ether is: tea-leaf power (g): water (ml)=1:(5-10).
7. the analysis method of volatile component in Folium Camelliae sinensis as claimed in claim 1, it is characterised in that in described sample test step, GC conditions is:
Carrier gas: He gas, flow velocity is 1.2ml/min; Chromatographic column: AgilentHP-5MS; Sample introduction pattern: constant current; Input mode: do not tap; Injector temperature 250 DEG C; Connector temperature 250 DEG C; Column temperature gradient: initial temperature 45 DEG C, with the ramp of 15 DEG C/min to 210 DEG C, keeps 1min, then with the ramp of 5 DEG C/min to 240 DEG C, after with the ramp of 10 DEG C/min to 300 DEG C, keep 6min.
8. the analysis method of volatile component in Folium Camelliae sinensis as claimed in claim 1, it is characterised in that in described sample test step, Mass Spectrometry Conditions is:
Electron bombardment source temperature 230 DEG C, voltage 70eV; Mass scan range: 50-2000AMU, scans 0.3s, interval 0.2s every time.
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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 |
|---|
| 丁林芳等: "SDE-GC-MS法测定茶叶中的挥发成分", 《中国酿造》 * |
| 吕海鹏等: "普洱茶挥发性成分指纹图谱研究", 《茶叶科学》 * |
| 揭国良等: "普洱茶抗氧化特性的初步研究", 《茶叶》 * |
| 罗发美等: "SPME—GC—MS分析普洱茶的挥发性成分", 《林产化学与工业》 * |
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