CN116559353A - High-precision black tea aroma analysis method and application thereof - Google Patents
High-precision black tea aroma analysis method and application thereof Download PDFInfo
- Publication number
- CN116559353A CN116559353A CN202310504895.1A CN202310504895A CN116559353A CN 116559353 A CN116559353 A CN 116559353A CN 202310504895 A CN202310504895 A CN 202310504895A CN 116559353 A CN116559353 A CN 116559353A
- Authority
- CN
- China
- Prior art keywords
- aroma
- black tea
- temperature
- tea
- sample
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 244000269722 Thea sinensis Species 0.000 title claims abstract description 83
- 235000006468 Thea sinensis Nutrition 0.000 title claims abstract description 47
- 235000020279 black tea Nutrition 0.000 title claims abstract description 47
- 238000004458 analytical method Methods 0.000 title claims abstract description 15
- 235000013616 tea Nutrition 0.000 claims abstract description 36
- 239000000126 substance Substances 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 24
- 230000014759 maintenance of location Effects 0.000 claims abstract description 22
- 238000001514 detection method Methods 0.000 claims abstract description 18
- 238000000605 extraction Methods 0.000 claims abstract description 18
- 239000003463 adsorbent Substances 0.000 claims abstract description 15
- 238000002470 solid-phase micro-extraction Methods 0.000 claims abstract description 10
- 238000011156 evaluation Methods 0.000 claims abstract description 8
- 238000001819 mass spectrum Methods 0.000 claims abstract description 6
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 claims description 12
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 10
- MWKFXSUHUHTGQN-UHFFFAOYSA-N n-decyl alcohol Natural products CCCCCCCCCCO MWKFXSUHUHTGQN-UHFFFAOYSA-N 0.000 claims description 9
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 claims description 7
- 150000001875 compounds Chemical class 0.000 claims description 7
- 150000002500 ions Chemical class 0.000 claims description 7
- 230000005540 biological transmission Effects 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 5
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims description 5
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 5
- 239000011780 sodium chloride Substances 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 239000012159 carrier gas Substances 0.000 claims description 3
- 238000003795 desorption Methods 0.000 claims description 3
- 235000019225 fermented tea Nutrition 0.000 claims description 3
- 239000001307 helium Substances 0.000 claims description 3
- 229910052734 helium Inorganic materials 0.000 claims description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 3
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 claims description 3
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- 239000005968 1-Decanol Substances 0.000 claims description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000002808 molecular sieve Substances 0.000 claims description 2
- -1 polydimethylsiloxane Polymers 0.000 claims description 2
- 238000004451 qualitative analysis Methods 0.000 claims description 2
- 238000004445 quantitative analysis Methods 0.000 claims description 2
- 230000000630 rising effect Effects 0.000 claims description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 235000014347 soups Nutrition 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 238000001319 headspace solid-phase micro-extraction Methods 0.000 claims 1
- 239000002699 waste material Substances 0.000 abstract 1
- 238000002474 experimental method Methods 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 4
- 239000003205 fragrance Substances 0.000 description 3
- 235000019224 Camellia sinensis var Qingmao Nutrition 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 230000012447 hatching Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 235000020339 pu-erh tea Nutrition 0.000 description 2
- 230000001953 sensory effect Effects 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 231100000757 Microbial toxin Toxicity 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000035622 drinking Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011067 equilibration Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 210000000196 olfactory nerve Anatomy 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 238000010200 validation analysis Methods 0.000 description 1
Classifications
-
- 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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
-
- 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
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention relates to the field of chemical detection, and discloses a black tea aroma analysis method with high accuracy and application thereof; preparing a pre-extracted sample from black tea and a standard substance, extracting aroma components by adopting HS-SPME, balancing the pre-extracted sample, extracting by using an extraction head with an adsorbent, adsorbing the aroma components on the adsorbent, introducing the adsorbent into a chromatograph GC, desorbing, and respectively introducing the aroma components flowing out of the GC into a mass spectrum MS and an olfactometer O in a 1:1 split mode to obtain detection results of the two groups of aroma components, and comparing the detection results of the two groups of aroma components of the standard substance; the method also comprises the steps of directly sniffing samples and standard substances by a plurality of tea evaluation staff, and recording the retention time, aroma description and aroma intensity. Can effectively prevent the waste of volatile substances in the black tea, and the accuracy can achieve the purposes of accurately grading the black tea and identifying harmful substances mixed into the tea.
Description
Technical Field
The invention relates to the field of chemical detection, in particular to a black tea aroma analysis method with high accuracy and application thereof.
Background
The black tea is one of six kinds of Chinese tea, has long history and unique process, is favored by consumers in recent years due to unique sensory characteristics and various health care effects, determines key aroma components of the black tea, provides theoretical basis for analysis and evaluation of the quality of the black tea and research and development of novel black tea, but has the characteristics of large required quantity and high use frequency when being taken as a healthy partner drink for daily life of the consumers, and can bring irreversible harm to the consumers in long-term drinking even if harmful substances such as pesticides or microbial toxins are mixed in the black tea, and can reduce the damage of tea production places and consumers only by timely detecting inferior black tea, but has strong aroma, and the harmful substances mixed in the black tea cannot be accurately detected by adopting an odor detection method with high precision; meanwhile, the high-precision odor detection method is adopted to accurately classify and price varieties of different grades of black tea, and the method is also beneficial to protecting the economic benefits of tea production places and consumers.
The smell quality is taken as one of the most important factors for evaluating the quality of the black tea, the essence of the smell quality is that different aromatic substances are combined in different concentrations, the peculiar smell of the tea formed by the comprehensive action of olfactory nerves can be qualitatively and quantitatively analyzed by adopting a gas chromatography-mass spectrometry combined technology GC-MS, but the volatile components of the tea are complex, and the contribution of the components to the overall fragrance of the tea is difficult to determine in the GC-MS, so that the smell instrument O is used for detecting the volatile components of the tea; meanwhile, it should be noted that the volatile components of the tea are easy to lose or decompose, whether the obtained volatile components are accurate enough or suitable for subsequent instrument detection or not, and a proper extraction method is still needed to solve the problem, so that the adoption of the HS-SPME extraction technology is a focus of attention.
Chinese paper, "HS-SPME-GC-MS-GC-O analysis of key aroma components in Pu 'er tea powder," discloses adding KCl into Pu' er tea powder, soaking in boiling water, extracting with HS-SPME, flowing into GC-MS-GC, and flowing into a sniffing instrument for artificial aroma smell; however, the method omits practical applications such as precise classification of black tea, identification of harmful substances mixed into the tea and the like.
Disclosure of Invention
In order to overcome the defect of the prior art of the practical application method for accurately classifying marketized black tea and identifying harmful substances, the invention provides the black tea aroma analysis method with high accuracy, which can accurately classify the black tea and identify the harmful substances mixed into the tea; the invention also provides application of the black tea aroma analysis method with high precision, which is used for accurately classifying the black tea and identifying harmful substances mixed into the tea.
The invention is realized by the following technical scheme:
a high-precision black tea aroma analysis method comprises the steps of preparing a pre-extracted sample from black tea and a standard substance, extracting aroma components by adopting HS-SPME, balancing the pre-extracted sample, extracting by using an extraction head with an adsorbent, adsorbing the aroma components on the adsorbent, introducing the adsorbent into a chromatograph GC, desorbing, and then enabling the aroma components flowing out from the GC to be 1:1 respectively entering a mass spectrum MS and an olfactory instrument O in a split-flow mode to obtain detection results of two groups of aroma components for comparison, and simultaneously obtaining detection results of two groups of aroma components of a standard substance;
the method also comprises the steps of directly sniffing samples and standard substances by a plurality of tea evaluation staff, and recording the retention time, aroma description and aroma intensity.
Preferably, the preparation method of the pre-extracted sample is as follows:
weighing black tea, grinding, placing into a container, respectively adding sodium chloride, water and internal standard 1-decyl alcohol to prepare an extraction sample, performing the HS-SPME procedure by using a Thermo automatic sampler, and extracting the sample in an incubator by using the extraction head with the adsorbent after balancing.
Preferably, the mixing ratio of the black tea, the sodium chloride, the water and the internal standard 1-decyl alcohol is 0.8-1.2 g to 0.3-0.8 g to 4-6 mL to 8 mu L-10 mu L; the equilibrium time is 8min-12min, the extraction temperature and the extraction time are respectively set at 70-90 ℃ for 30min-50min, the extraction head is DVB/CAR/PDMS, and the adsorbent is one of divinylbenzene, carbon molecular sieve and polydimethylsiloxane.
Preferably, the adsorbent having the aroma component adsorbed thereon is introduced into a GC sample inlet for desorption at 180 to 280 ℃ for 5 to 10 minutes and then analyzed.
Preferably, the qualitative analysis of the GC-MS is characterized in that sample mass spectrum data is searched and matched with a NIST mass spectrum database, and retention time is recorded to calculate retention index qualitative of aroma components; the GC-MS quantitative analysis is to respectively quantify each aroma component according to the peak area of the aroma component by taking the peak area of the 1-decyl alcohol internal standard as a reference, and the quantitative formula is the content The ratio is the ratio of the peak area of the compound to the peak area of the internal standard, M is the mass of the pre-extracted sample, and the unit is g.
Preferably, GC conditions: adopting a chromatographic column RTX-5MS (30 m multiplied by 0.25mm multiplied by 0.25 mu m), taking helium as carrier gas, adopting a sample inlet temperature of 250 ℃ and a column flow rate of 1mL/min, and adopting a non-split flow mode; the temperature rising process of the sample inlet is as follows: the initial temperature is 50 ℃, the temperature is kept for 2min, the temperature is increased to 100 ℃ at 6 ℃/min, the temperature is kept for 1min, the temperature is increased to 120 ℃ at 4 ℃/min, the temperature is kept for 1min at 1.5 ℃/min to 140 ℃, the temperature is kept for 1min, the temperature is increased to 180 ℃ at 3 ℃/min, the temperature is kept for 1min, and the temperature is kept for 1min at 8 ℃/min to 250 ℃.
Preferably, MS conditions: an ion source EI source, EI source energy of 70ev; the temperature of the ion source is 250 ℃, and the temperature of the transmission line is 250 ℃;
full scan mode (scan): mass scanning range m/z is 35 amu-400 amu, and solvent delay time is avoided.
Preferably, sniffing instrument O conditions: the transmission line temperature was 250 ℃.
Preferably, the method also comprises the step of detecting tea soup by the electronic tongue.
The application of the black tea aroma analysis method with high accuracy in black tea classification and black tea harmful substance detection is provided.
The invention has the beneficial effects that:
(1) The invention uses the chromatograph-mass spectrometer to lead the detection precision to reach the volatile molecular level, and can accurately give out key contribution molecules with different fragrances.
(2) The black tea sample pretreatment flow effectively prevents the loss of aroma molecules.
(3) The high-precision detection ensures that the method is beneficial to the application and popularization of the black tea precise classification and trace harmful substance detection.
(4) The introduction of the sniffer and the experience judgment of the expert lead to stable detection results and high interpretability, and are beneficial to further research of dark tea.
Drawings
Fig. 1 is a total ion flow diagram of Liupu tea.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the following examples; it should be understood that the detailed description and specific examples, while indicating the invention, are intended for purposes of illustration only and are not intended to limit the invention; in the examples, all means used are conventional in the art unless otherwise specified; the terms "comprises," "comprising," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion; in addition, technical features of the embodiments of the present invention described below may be combined with each other as long as they do not collide with each other; the experimental raw materials of the invention are all commercial products.
Example 1
A black tea aroma analysis method with high accuracy comprises the following steps:
(1) Sample selection: the sample is Liupu tea sample, which is selected from Guangzhou City of Guangxi province, and aged fragrance Liupu tea sample is selected. The evaluation method adopts GB/T23776-2018 tea sensory evaluation method standard, and 6 (3 female 3 male) evaluation persons all obtain certificates of tea evaluating persons of medium grade and above.
(2) Grinding the sample: and (3) grinding the ground tea sample according to the preparation of the ground tea sample of GB8303-2013 and the dry matter content measurement standard, and sealing and preserving the ground tea sample to avoid loss of stale aroma components in the tea stems without sieving.
(3) HS-SPME: 1g of the ground sample was weighed, placed in a 20mL headspace bottle, 0.5g of sodium chloride was added, 5mL of boiled deionized water was added, 8. Mu.L of internal standard 1-decanol was added, HS-SPME procedure was performed using Thermo autosampler, after 10min of equilibration of the prepared sample in a hatching oven, extraction was performed for 40min at 80℃and analysis was performed by immediately placing GC-MS sample injection port for desorption for 5min after extraction in a hatching oven using 50 μm DVB/CAR/PDMS extraction head, and the sample was repeated three times.
(4) GC-MS detection: GC conditions: the chromatographic column RTX-5MS (30 m multiplied by 0.25mm multiplied by 0.25 mu m) is adopted, the carrier gas is helium (purity > 99.999%), the temperature of the sample inlet is 250 ℃, the flow rate of the column is 1mL/min, and the non-split flow mode is adopted. Heating to 50deg.C, maintaining for 2min, and heating to 100deg.C at 6deg.C/min for 1min; raising the temperature to 120 ℃ at 4 ℃/min, and keeping for 1min; raising the temperature to 140 ℃ at 1.5 ℃/min, and keeping for 1min; raising the temperature to 180 ℃ at 3 ℃/min, and keeping for 1min; raising the temperature to 250 ℃ at 8 ℃/min and keeping the temperature for 1min.
MS conditions: the ion source EI source, electron energy 70eV, transmission line temperature 250 ℃. The temperature of the ion source is 250 ℃; solvent-free delay time, full Scan (Scan) mode, mass Scan range: 35amu to 400amu.
(a) Characterization of volatile components: carrying out retrieval matching on mass spectrum information of each chromatographic peak of Liupu tea obtained by GC-MS analysis and NIST 17 standard spectrum library, wherein the matching index is more than 70% as an identification standard; based on the retention time of the test substance, a Retention Index (RI) is calculated, combined with literature and database retention index identification.
The retention index calculation formula is ri=100n+100× [ (RTx-RTn)/(rtn+1-RTn) ] formula: RI is the retention index of the substance to be tested; RTx is the retention time of the substance to be measured; RTn is n-carbon n-alkane retention time; RT (n+1) is the retention time of n-alkane with the number of (n+1) carbon atoms.
(b) Quantification of volatile components: calculation of the peaks of the volatile Compounds to be tested and 1-decanolThe area ratio is used for obtaining the content of the componentsWherein the ratio is the ratio of the peak area of the compound to the peak area of the internal standard, and M is 1.0g of the tea sample.
(5) GC-O analysis: the conditions are consistent with GC-MS, the temperature of a transmission line is 250 ℃, the temperature of a sniffing instrument is 250 ℃, and the components flowing out of the chromatographic column enter a detector and the sniffing instrument respectively in a 1:1 split mode.
The method is characterized in that the direct intensity method is adopted to analyze the volatile components of Liupu tea, 6 tea evaluation operators smell the Liupu tea and record the volatile components (retention time, aroma description and aroma intensity), the aroma intensity is divided into 4 grades, and the aroma intensity is gradually increased from 1 to 4 grades. Three and more smellers smelled the same aroma-describing compounds at the same retention time and the intensity was greater than 1, the aroma was determined as a valid experimental result. Each sample was repeated 3 times and the results are shown in table 1.
Standard compound validation: sample injection is carried out on the key smelled aroma components by adopting a standard substance under the same GC-MS condition, and RI values, spectrum library retrieval matching degree, aroma description and retention time and mass spectrogram of the key smelled aroma components are compared. If the four are the same, it can be determined that the key aroma component is present.
In order to further explain the accuracy, reliability and stability of qualitative and quantitative determination of key aroma components, reproducibility, precision and stability experiments are performed after the key aroma components of Liupu tea are quantitatively determined.
Reproducibility experiments: taking the same Chenxiang Liupu tea sample, preparing 3 parallel samples, continuously feeding three times, calculating the retention time and peak area of a common target peak and the Relative Standard Deviation (RSD) of positive and negative matching degree, wherein the smaller the RSD value is (< 10), the better the reproducibility is.
Precision experiment: taking the same Liupu tea sample, sampling for 3 times continuously, calculating the relative standard deviation of the retention time and the relative peak area of each peak, and calculating the relative standard deviation RSD <10, wherein the precision is good, and the obtained result is shown in Table 2.
Stability experiment: 3 parts of the same aged six fort tea sample are taken, three days of continuous testing are carried out, the retention time, peak area and RSD of positive and negative matching degree of the daytime target compound are calculated, the smaller the RSD value is, the better the stability is, and the obtained result is shown in Table 3.
Table 1 Chen Xiangliu Bao tea key aroma components
TABLE 2 results of precision experiments
TABLE 3 daytime stability test results
As can be seen from tables 2 and 3, the retention time and peak area of the key aroma components and the RSD of the positive and negative matching degree are all below 10%, which indicates that the instrument state and the pretreatment method have good repeatability, good precision and high stability, the key aroma components in the black tea can be effectively and qualitatively measured out, under the same conditions, the key aroma components can be found out obviously from the different varieties of the black tea, the classification can be precisely given out, and trace harmful substances mixed in the strong aroma of the black tea can be identified due to the good reproducibility, good density and high stability.
Although embodiments of the present invention have been illustrated and described in detail hereinabove, it will be apparent to those skilled in the art that various modifications and improvements can be made therein without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (10)
1. The black tea aroma analysis method with high precision is characterized by comprising the steps of preparing a pre-extracted sample from black tea and a standard substance, extracting aroma components by adopting headspace solid-phase microextraction HS-SPME, balancing the pre-extracted sample, extracting by using an extraction head with an adsorbent, adsorbing the aroma components on the adsorbent, introducing the adsorbent into a chromatograph GC, desorbing, and respectively introducing the aroma components flowing out of the GC into a mass spectrum MS and an olfactometer O in a 1:1 split mode to obtain detection results of the two groups of aroma components, and comparing the detection results of the two groups of aroma components of the standard substance;
the method also comprises the steps of directly sniffing samples and standard substances by a plurality of tea evaluation staff, and recording the retention time, aroma description and aroma intensity.
2. The method for analyzing aroma of black tea with high precision according to claim 1, wherein the pre-extracted sample is prepared by the following steps:
weighing black tea, grinding, placing into a container, respectively adding sodium chloride, water and internal standard 1-decyl alcohol to prepare an extraction sample, performing the HS-SPME procedure by using a Thermo automatic sampler, and extracting the sample in an incubator by using the extraction head with the adsorbent after balancing.
3. The method for analyzing aroma of dark tea with high precision according to claim 1 or 2, wherein the mixing ratio of dark tea, sodium chloride, water and internal standard 1-decanol is 0.8-1.2 g:0.3-0.8 g:4-6 ml:8-10 μl; the equilibrium time is 8min-12min, the extraction temperature and the extraction time are respectively set at 70-90 ℃ for 30min-50min, the extraction head is used for solid-phase microextraction of DVB/CAR/PDMS, and the adsorbent is one of divinylbenzene, carbon molecular sieve and polydimethylsiloxane.
4. The method for analyzing aroma of black tea according to claim 1, wherein the adsorbent having the aroma component adsorbed thereon is introduced into a GC sample inlet for desorption at 180 to 280 ℃ for 5 to 10 minutes and then analyzed.
5. A method for analyzing aroma of black tea with high accuracy according to any one of claims 1, 2 and 4, wherein,
the qualitative analysis of the GC-MS is to search and match the mass spectrogram data of the sample with a database of an NIST mass spectrogram database, record the retention time and calculate the retention index qualitative of the aroma components;
the GC-MS quantitative analysis is to respectively quantify each aroma component according to the peak area of the aroma component by taking the peak area of the 1-decyl alcohol internal standard as a reference, and the quantitative formula is the content The ratio is the ratio of the peak area of the compound to the peak area of the internal standard, M is the mass of the pre-extracted sample, and the unit is g.
6. A method for analyzing aroma of black tea with high accuracy according to any one of claims 1, 2 and 4, wherein GC conditions: adopting a chromatographic column RTX-5MS (30 m multiplied by 0.25mm multiplied by 0.25 mu m), taking helium as carrier gas, adopting a sample inlet temperature of 250 ℃ and a column flow rate of 1mL/min, and adopting a non-split flow mode; the temperature rising process of the sample inlet is as follows: the initial temperature is 50 ℃, the temperature is kept for 2min, the temperature is increased to 100 ℃ at 6 ℃/min, the temperature is kept for 1min, the temperature is increased to 120 ℃ at 4 ℃/min, the temperature is kept for 1min at 1.5 ℃/min to 140 ℃, the temperature is kept for 1min, the temperature is increased to 180 ℃ at 3 ℃/min, the temperature is kept for 1min, and the temperature is kept for 1min at 8 ℃/min to 250 ℃.
7. A method for analyzing aroma of black tea with high accuracy according to any one of claims 1, 2 and 4, wherein MS conditions: an ion source EI source, EI source energy of 70ev; the temperature of the ion source is 250 ℃, and the temperature of the transmission line is 250 ℃;
full scan mode (scan): mass scanning range m/z is 35 amu-400 amu, and solvent delay time is avoided.
8. A method for analyzing aroma of black tea with high accuracy according to any one of claims 1, 2 and 4, wherein the sniffing instrument O conditions: the transmission line temperature was 250 ℃.
9. The method for analyzing aroma of black tea with high accuracy according to any one of claims 1, 2 and 4, further comprising the step of detecting tea soup in combination with an electronic tongue.
10. Use of a highly accurate aroma analysis method according to any one of claims 1 to 9 for classification of black tea and detection of harmful substances in black tea.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310504895.1A CN116559353A (en) | 2023-05-06 | 2023-05-06 | High-precision black tea aroma analysis method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310504895.1A CN116559353A (en) | 2023-05-06 | 2023-05-06 | High-precision black tea aroma analysis method and application thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116559353A true CN116559353A (en) | 2023-08-08 |
Family
ID=87499488
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310504895.1A Pending CN116559353A (en) | 2023-05-06 | 2023-05-06 | High-precision black tea aroma analysis method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116559353A (en) |
-
2023
- 2023-05-06 CN CN202310504895.1A patent/CN116559353A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Lim et al. | Non-destructive profiling of volatile organic compounds using HS-SPME/GC–MS and its application for the geographical discrimination of white rice | |
| CN110441423B (en) | Method and system for measuring grain aroma components | |
| CN106053628B (en) | A kind of method that fast qualitative quantifies fragrance component in tealeaves | |
| CN110687240B (en) | Method for rapidly identifying production place of ham | |
| CN107478736B (en) | Method for judging freshness of hops based on volatile component composition | |
| CN103076411A (en) | Analytical method for determining aromatic constituents in tea | |
| CN107367565B (en) | Method for rapidly identifying quality of maca by using odor fingerprint | |
| CN111398470A (en) | GC-IMS pear producing area distinguishing method based on aroma substance fingerprint spectrum | |
| CN102507800B (en) | Rapid aroma fingerprint identification method for geographical indication protection product of vinegar | |
| CN113358798B (en) | Method for detecting heterocyclic odor substances by thermal desorption-gas chromatography mass spectrometry | |
| KR20190042476A (en) | Biomarker for the discrimination of geographical origins of the soybeans and method for discriminating of geographical origin using the same | |
| CN113960191A (en) | Method for determining content of PC, PP, PS and PE micro-plastics in soil by cracking gas chromatography | |
| CN112578046A (en) | Method for rapidly identifying mango varieties based on gas chromatography-ion mobility spectrometry technology | |
| CN112924584A (en) | Quantitative detection method for aroma active compounds in pickled vegetables | |
| CN115541770A (en) | Method for quickly evaluating suitability of storage conditions of instant cubilose based on flavor substance difference analysis | |
| Tokida et al. | Fully automated, high‐throughput instrumentation for measuring the δ13C value of methane and application of the instrumentation to rice paddy samples | |
| CN103499666A (en) | Method for detecting rape honey aroma components by solid phase microextraction | |
| CN114994202A (en) | Garlic producing area identification method based on GC-IMS technology | |
| CN116559353A (en) | High-precision black tea aroma analysis method and application thereof | |
| CN111487329A (en) | Method for simultaneously measuring ethanol non-oxidized metabolites in blood and vitreous humor | |
| CN113607850A (en) | Method for analyzing and identifying wheat varieties by utilizing volatile organic compounds | |
| CN114609304A (en) | Grain and oil food flavor substance data analysis method and application thereof | |
| CN111175368B (en) | Method for identifying addition of synthetic acetic acid in brewed vinegar | |
| CN115219620B (en) | Jingyang Fu tea specific identification volatile component combination, preparation method and application thereof, and Jingyang Fu tea identification method | |
| CN113311076A (en) | Method for rapidly distinguishing different varieties of rice based on aldehyde compounds |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |