CN106018623A - Identification method for nitrogen-containing compound in Keemun black tea - Google Patents
Identification method for nitrogen-containing compound in Keemun black tea Download PDFInfo
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- CN106018623A CN106018623A CN201610552952.3A CN201610552952A CN106018623A CN 106018623 A CN106018623 A CN 106018623A CN 201610552952 A CN201610552952 A CN 201610552952A CN 106018623 A CN106018623 A CN 106018623A
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- G—PHYSICS
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- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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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
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
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Abstract
The invention provides an identification method for a nitrogen-containing compound in Keemun black tea, and belongs to the technical field of analysis and detection. The method comprises a step of extracting the nitrogen-containing compound in the Keemun black tea, and a step of detecting and analyzing the obtained nitrogen-containing compound in the Keemun black tea by virtue of a gas chromatography-nitrogen phosphorus detector-mass spectrometry coupling technology and qualitatively and quantitatively analyzing the nitrogen-containing compound. According to the method, the nitrogen-containing compound in the Keemun black tea is analyzed by combining static headspace solid phase microextraction and the gas chromatography-nitrogen phosphorus detector-mass spectrometry coupling technology, and a set of qualitative and quantitative analysis method for the nitrogen-containing compound in the Keemun black tea is formed, and is easy to operate and high in applicability.
Description
Technical field
The invention belongs to technical field of analysis and detection, particularly relate to a kind of method analyzing teas nitrogen-containing compound, especially
It it is the detection method of nitrogen-containing compound in a kind of keemun black tea.
Background technology
Keemun black tea is Chinese history well-known tea, away from the production history of existing over one hundred year of the present；Keemun black tea is famous black tea
Fine work, is called for short keemun, originate in Qimen, Anhui Province, to the east of, Guichi, Shitai County, Yixian County, and the Fuliang one in Jiangxi carries.Keemun profile
Bar rope is the most neat and the best spaced, and cutting edge of a knife or a sword Seedling is beautiful, and color and luster Wu Run (is commonly called as " precious light ")；Fragrance exactly likes fruital, and band Cymbidium ensifolium (L.) Sw. perfume (is known as " Qimen again
Fragrant "), strong fragrant lasting；Soup color is red gorgeous bright, and flavour is sweet fresh mellow, (tea grounds steeped) glow at the bottom of leaf.Keemun black tea, is " red
Tea " in outstanding person, be renown far and wide absolutely in generation to " fragrant height, taste alcohol, shape U.S., color gorgeous " four；" Qimen is fragrant " of floweriness, seemingly fruit, seemingly honey
With well-known, occupy first of the big high-quality slender joss stick well-known tea in the world three；A kind of special fragrance is had again because of keemun black tea；Therefore foreign country people claims Qi
Door black tea be " Qimen fragrant ", " prince's perfume ", " beautiful and fragrant flowers ", " black tea queen ".
Nitrogen-containing compound in keemun black tea is the key factor constituting keemun black tea local flavor as other materials, determines
The local flavor of keemun black tea and typicality.Researcher uses the way of qualitative, quantitative to identify much kind decision Qimen both at home and abroad
The material of black tea local flavor.In recent years keemun black tea flavor substances Quality Research was found that while that nitrogen-containing compound contained in keemun black tea
Measuring little, so this compounds taste threshold is low, has nutty and bakes the pleasant local flavors such as perfume, and having other fragrance matters
Significantly set off superposition by contrast, be the aroma compound that in keemun black tea, a class is important, but the most both at home and abroad in keemun black tea
The research of nitrogen-containing compound still at an early stage, gas chromatography (fid detector) direct injection analysis that application is conventional
There is certain difficulty.It is contemplated that use Static Headspace solid-phase microextraction to combine gas chromatogram-nitrogen phosphorous detector-mass spectrometry
Technology, is analyzed research, sets up nitrogen in a set of keemun black tea the nitrogen-containing compound in keemun black tea tea sample on the market
The qualitative and quantitative analysis method of compound, simple to operate, easy, the suitability is extensive.
Summary of the invention
For above-mentioned technical problem of the prior art, the invention provides the mirror of nitrogen-containing compound in a kind of keemun black tea
Determine method, described this method prior art to be solved measures the nitrogen-containing compound composition in keemun black tea and concentration is forbidden
True technical problem.
In a kind of keemun black tea of the present invention, the detection method of nitrogen-containing compound, comprises the following steps:
1) one is extracted the step of nitrogen-containing compound in keemun black tea: first put down in the thermostat water bath of 80 DEG C by distilled water
Weighing apparatus 10min, adds keemun black tea, and described keemun black tea is 1:10 with the mass ratio of distilled water, shakes up, and sieves after soaking 10min
Net filtration, puts in 4 DEG C of refrigerators standby after millet paste cooling；Then take this millet paste of 5g, add 1g sodium chloride, add 10 μ L concentration and be
2-methoxyl group-3-the methylpyrazine of 4mg/L is placed in 15mL or 20mL ml headspace bottle, and ml headspace bottle silica gel lift seals, SPME bar
Part is: extracting head be inserted in ml headspace bottle, and makes extracting head be on sample 3～4cm, water bath with thermostatic control temperature 45～50 DEG C
Under, extract 50～55min；After having extracted, rapidly extracting head is inserted gas chromatogram-nitrogen phosphorous detector-GC-MS and enters
Sample mouth, desorbing 3～5min at 250 DEG C；
2) one utilizes gas chromatogram-nitrogen phosphorous detector-mass spectrometric hyphenated technique detection analytical procedure 1) obtained by Qimen
The step of the nitrogen-containing compound in black tea infusion:
GC conditions: DB-5 capillary chromatographic column, its parameter is 60m × 0.25mm, 0.25 μm；Manually it is not diverted into
Sample, injector temperature 250 DEG C；Temperature programming: initial temperature 40 DEG C, keeps 6min, rises to 100 DEG C with the speed of 3 DEG C/min, no
Keep, rise to 230 DEG C with the speed of 5 DEG C/min, keep 10min；
NPD temperature: 250 DEG C；Hydrogen flow rate: 2.0mL/min；Air velocity: 60mL/min；Carrier gas He, flow velocity 30mL/
min；
MS condition: EI ionization source, electron energy 70eV, sweep limits 30～450amu, ion source temperature 230 DEG C；Transmission
Line temperature 280 DEG C；Quadrupole rod temperature 150 DEG C；
3) nitrogen-containing compound to detection carries out the step of qualitative analysis, the mass spectrum of unknown compound by with
Wiley7n, NIST 11 and standard substance contrast carry out qualitative；
4) nitrogen-containing compound to detection carries out the step of quantitative analysis, weighs a certain amount of standard substance, is formulated in steaming
As single mark stock solution in distilled water, accurately draw a certain amount of Standard Reserving Solution distilled water and be configured to the mixing of a series of concentration
Standard specimen；Wherein internal standard material is 2-methoxyl group-3-methylpyrazine.
Further, described analysis and detecting instrument is gas chromatogram-nitrogen phosphorous detector-GC-MS.
Further, described quantitative approach is that Internal standard curve method is quantitative.
Present invention employs Static Headspace solid-phase microextraction and combine gas chromatogram-nitrogen phosphorous detector-mass spectrometric hyphenated technique, right
Nitrogen-containing compound in keemun black tea is analyzed research, sets up a set of nitrogen-containing compound effectively fixed be applicable to keemun black tea
Property quantitative analysis method.The present invention is simple to operate, easy, has reached satisfied production and has quickly detected the purpose of demand, and the suitability is wide
General.
Accompanying drawing explanation
Fig. 1 is the nitrogen-containing compound chromatogram in commercially available keemun black tea gained millet paste.
Detailed description of the invention
Static Headspace solid-phase microextraction is used to combine gas chromatogram-nitrogen phosphorous detector-mass spectrometry skill for explaination further
Art quickly detects and the method for nitrogen-containing compound in qualitative, quantitative keemun black tea, is described in more detail below in conjunction with example.
Embodiment 1
This method mainly uses Static Headspace solid-phase microextraction to combine gas chromatogram-nitrogen phosphorous detector-mass spectrometric hyphenated technique
Nitrogen-containing compound in keemun black tea is used for quickly detecting and qualitative, quantitative, specifically comprises the following steps that
1) one is extracted the step of nitrogen-containing compound in keemun black tea: first prepares keemun black tea millet paste, first weighs 80g80
DEG C distilled water in the tool plug conical flask of 250mL, in the thermostat water bath of 80 DEG C balance 10min, add 8g tea sample, every
2min shakes up, and soaks 10min, and screen filtration, millet paste cools down rapidly, puts in 4 DEG C of refrigerators standby.Then take this millet paste of 5g, add
Adding 1g sodium chloride, add the 2-methoxyl group-3-methylpyrazine that 10 μ L concentration are 4mg/L and be placed in 15mL ml headspace bottle, ml headspace bottle is used
Silica gel lift seals, and SPME condition is: extracting head be inserted in ml headspace bottle, and makes extracting head be in 3.2cm on sample, permanent
Under tepidarium temperature 50 C, extract 55min；After having extracted, rapidly extracting head is inserted gas chromatogram-nitrogen phosphorous detector-matter
Spectrum combined instrument injection port, desorbing 5min at 250 DEG C；
2) by gas chromatogram-nitrogen phosphorous detector-mass spectrometric hyphenated technique detection analytical procedure 1) obtained by keemun black tea in
Nitrogen-containing compound and its nitrogen-containing compound is carried out qualitative and quantitative analysis:
GC conditions: DB-5 capillary chromatographic column, its parameter is 60m × 0.25mm, 0.25 μm；Manually it is not diverted into
Sample, injector temperature 250 DEG C；Temperature programming: initial temperature 40 DEG C, keeps 6min, rises to 100 DEG C with the speed of 3 DEG C/min, no
Keep, rise to 230 DEG C with the speed of 5 DEG C/min, keep 10min；
NPD temperature: 250 DEG C；Hydrogen flow rate: 2.0mL/min；Air velocity: 60mL/min；Carrier gas He, flow velocity 30mL/
min；
MS condition: EI ionization source, electron energy 70eV, sweep limits 30～450amu, ion source temperature 230 DEG C；Transmission
Line temperature 280 DEG C；Quadrupole rod temperature 150 DEG C；
3) detection material qualitative: the mass spectrum of unknown compound by with wiley7n, NIST 11 and standard substance contrast into
Row is qualitative；
4) quantitative analysis: weigh a certain amount of standard substance, is formulated in distilled water as single mark stock solution, accurately draws certain
The Standard Reserving Solution distilled water of amount is configured to the mixed sample of a series of concentration；Wherein internal standard material is 2-methoxyl group-3-first
Base pyrazine.
Nitrogen-containing compound qualification result in table 1 the inventive method keemun black tea
As shown in Table 1, gas chromatogram-nitrogen phosphorous detector-mass spectrometric hyphenated technique is utilized to identify in keemun black tea 14 kinds altogether
Nitrogen-containing compound, wherein thiazoles 3 kinds, Pyrazine 9 kinds, pyroles 2 kinds.The method energy fast qualitative goes out multiple nitrogenous chemical combination
Thing, Accurate Determining goes out the content of nitrogen-containing compound in keemun black tea.
Claims (3)
1. the authentication method of nitrogen-containing compound in a keemun black tea, it is characterised in that comprise the following steps:
1) one is extracted the step of nitrogen-containing compound in keemun black tea: first balanced in the thermostat water bath of 80 DEG C by distilled water
10min, adds keemun black tea, and described keemun black tea is 1:10 with the mass ratio of distilled water, shakes up, and soaks screen cloth after 10min
Filter, put in 4 DEG C of refrigerators standby after millet paste cooling；Then take this millet paste of 5g, add 1g sodium chloride, add 10 μ L concentration and be
2-methoxyl group-3-the methylpyrazine of 4mg/L is placed in 15mL or 20mL ml headspace bottle, and ml headspace bottle silica gel lift seals, SPME bar
Part is: extracting head be inserted in ml headspace bottle, and makes extracting head be on sample 3～4cm, water bath with thermostatic control temperature 45～50 DEG C
Under, extract 50～55min；After having extracted, rapidly extracting head is inserted gas chromatogram-nitrogen phosphorous detector-GC-MS and enters
Sample mouth, desorbing 3～5min at 250 DEG C；
2) one utilizes gas chromatogram-nitrogen phosphorous detector-mass spectrometric hyphenated technique detection analytical procedure 1) obtained by keemun black tea
The step of the nitrogen-containing compound in millet paste:
GC conditions: DB-5 capillary chromatographic column, its parameter is 60m × 0.25mm, 0.25 μm；Manual Splitless injecting samples,
Injector temperature 250 DEG C；Temperature programming: initial temperature 40 DEG C, keeps 6min, rises to 100 DEG C with the speed of 3 DEG C/min, do not protect
Hold, rise to 230 DEG C with the speed of 5 DEG C/min, keep 10min；
NPD temperature: 250 DEG C；Hydrogen flow rate: 2.0mL/min；Air velocity: 60mL/min；Carrier gas He, flow velocity 30mL/min；
MS condition: EI ionization source, electron energy 70eV, sweep limits 30～450amu, ion source temperature 230 DEG C；Transmission line temperature
Spend 280 DEG C；Quadrupole rod temperature 150 DEG C；
3) nitrogen-containing compound to detection carries out the step of qualitative analysis, the mass spectrum of unknown compound by with wiley7n,
NIST 11 and standard substance contrast carry out qualitative；
4) nitrogen-containing compound to detection carries out the step of quantitative analysis, weighs a certain amount of standard substance, is formulated in distilled water
Middle as single mark stock solution, accurately draw a certain amount of Standard Reserving Solution distilled water and be configured to the mixing mark of a series of concentration
Sample；Wherein internal standard material is 2-methoxyl group-3-methylpyrazine.
The authentication method of nitrogen-containing compound in a kind of keemun black tea the most according to claim 1, it is characterised in that: described
Analysis and detecting instrument is gas chromatogram-nitrogen phosphorous detector-GC-MS.
The authentication method of nitrogen-containing compound in a kind of keemun black tea the most according to claim 1, it is characterised in that: described
Quantitative approach is that Internal standard curve method is quantitative.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115436519A (en) * | 2022-09-07 | 2022-12-06 | 浙江希格骊特科技有限公司 | Method for analyzing volatile substance components in tea leaves and tea extracts |
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2016
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| DE10159846A1 (en) * | 2001-12-03 | 2003-06-12 | Univ Schiller Jena | For the detection of separate substances of 1-3C alkyl phenols, they are given an added internal standard, for narrow band condensation on a chiral column for gas chromatography and mass spectrometry |
| CN101017159A (en) * | 2007-02-08 | 2007-08-15 | 江南大学 | Method for determining pyrazine compound in spirit |
| JP2009047573A (en) * | 2007-08-21 | 2009-03-05 | Kirin Brewery Co Ltd | Analyzing method of trans-2-nonenal in beverage or wort using spme-gc/ms |
| CN101487825A (en) * | 2009-03-03 | 2009-07-22 | 中国农业大学 | Method for recognizing tea kinds and/or grades |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115436519A (en) * | 2022-09-07 | 2022-12-06 | 浙江希格骊特科技有限公司 | Method for analyzing volatile substance components in tea leaves and tea extracts |
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Application publication date: 20161012 |