CN109541073A - A kind of francolin congo red, the GC-MS analysis method of green fresh leaf volatile component - Google Patents
A kind of francolin congo red, the GC-MS analysis method of green fresh leaf volatile component Download PDFInfo
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- CN109541073A CN109541073A CN201910005999.1A CN201910005999A CN109541073A CN 109541073 A CN109541073 A CN 109541073A CN 201910005999 A CN201910005999 A CN 201910005999A CN 109541073 A CN109541073 A CN 109541073A
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- fresh leaf
- francolin
- alkene
- volatile component
- red
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- IQFVPQOLBLOTPF-HKXUKFGYSA-L congo red Chemical compound [Na+].[Na+].C1=CC=CC2=C(N)C(/N=N/C3=CC=C(C=C3)C3=CC=C(C=C3)/N=N/C3=C(C4=CC=CC=C4C(=C3)S([O-])(=O)=O)N)=CC(S([O-])(=O)=O)=C21 IQFVPQOLBLOTPF-HKXUKFGYSA-L 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 23
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- 238000004987 plasma desorption mass spectroscopy Methods 0.000 claims abstract description 13
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- 238000004458 analytical method Methods 0.000 claims abstract description 12
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- IIYFAKIEWZDVMP-UHFFFAOYSA-N tridecane Chemical compound CCCCCCCCCCCCC IIYFAKIEWZDVMP-UHFFFAOYSA-N 0.000 claims description 6
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- NZGWDASTMWDZIW-MRVPVSSYSA-N (+)-pulegone Chemical compound C[C@@H]1CCC(=C(C)C)C(=O)C1 NZGWDASTMWDZIW-MRVPVSSYSA-N 0.000 claims description 3
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- SPCXZDDGSGTVAW-XIDUGBJDSA-N (-)-alpha-gurjunene Chemical compound C[C@@H]1CC[C@H]2C(C)(C)[C@H]2C2=C(C)CC[C@H]12 SPCXZDDGSGTVAW-XIDUGBJDSA-N 0.000 claims description 2
- 229930014548 (-)-alpha-gurjunene Natural products 0.000 claims description 2
- 240000003421 Dianthus chinensis Species 0.000 claims description 2
- FJNHFUOCVLERHW-UHFFFAOYSA-N alpha-gurjunene Natural products CC1CCC2C(C3=CCCC13)C2(C)C FJNHFUOCVLERHW-UHFFFAOYSA-N 0.000 claims description 2
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- UIDUJXXQMGYOIN-UHFFFAOYSA-N aromadendrin Natural products CC1(C)C2C1CCC(C)C1C2C(C)CC1 UIDUJXXQMGYOIN-UHFFFAOYSA-N 0.000 claims description 2
- DUYRYUZIBGFLDD-UHFFFAOYSA-N gamma-gurjunene Natural products CC1CCC(C(C)=C)C=C2C(C)CCC21 DUYRYUZIBGFLDD-UHFFFAOYSA-N 0.000 claims description 2
- 244000269722 Thea sinensis Species 0.000 claims 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N formaldehyde Natural products O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims 2
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/47—Euphorbiaceae (Spurge family), e.g. Ricinus (castorbean)
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Abstract
The invention belongs to botany analysis technical field, a kind of francolin congo red, the GC-MS analysis method of green fresh leaf volatile component are disclosed;PDMS/DVB solid phase micro-extracting head aging: equal 250 DEG C of extracting head preparatory aging 15min before each sample introduction;GC conditions: chromatographic column Agilent HP-5MS, carrier gas are high-purity helium, 250 DEG C of injector temperature, are not shunted, temperature programming: 40 DEG C of initial temperature, 4min is kept, rises to 80 DEG C with 5 DEG C/min, then 260 DEG C are risen to 10 DEG C/min, keeps 10min, flow velocity 1mL/min;Mass Spectrometry Conditions: ion source temperature: 230 DEG C, 150 DEG C of level four bars;Ionization voltage 70eV;Scanning range: 35.0-800.0aum;65 μm of solid phase micro-extracting heads of PDMS/DVB are inserted into injection port, carry out instrument analysis by gas-chromatography and Mass Spectrometry Conditions, until chromatogram does not have peak appearance.
Description
Technical field
The invention belongs to botany analysis technical field more particularly to a kind of francolin congo red, green fresh leaf volatile component
GC-MS analysis method.
Background technique
Currently, the prior art commonly used in the trade is such that francolin tea is also known as mountain herb mixtures tea, tea in May etc., it is that Euphorbiaceae is wild
Paulownia category evergreen shrubs or dungarunga, 2~12m of plant height can give out strong holy basil gas after plant leaf blade is dry.Hainan francolin
Tea has deep cultural deposits, unique geographical advantage, suitable for people of all ages drinks characteristic and unique functional character, energy
The functions such as eliminating the phlegm, cough-relieving, wind dispelling, expelling parasite, analgesia, antidepression, antibacterial, antianxiety, antitumor, by successive dynasties men of literature and writing's great kindness,
And there is the good reputation of " polyporus lucidus " in tea product.Hainan francolin tea is throughout each counties and cities in Hainan Island, outstanding Yi Ledong, Wenchang, Wanning, mound
Water, Sanya, white sand, Dingan County, east, in fine jade, the counties and cities such as Bao Ting and Chang River it is in the majority.Headspace solid-phase microextraction has been widely used
In a kind of effective extractive technique of various sample volatile components, distillation extraction (SDE) is compared while with using more in the past,
Have many advantages, such as simple, reliable, high sensitivity, favorable reproducibility, does not need any organic solvent, automatic sampling.Especially head space
Solid phase microextraction (HS-SPME), using fiber vibration mode, from parameter setting to sample control all by software Automatic Control,
Reduce human error, avoids dirt of the extraction solid phase by polymer substance and involatile substance in certain sample substrates
Dye, shortens equilibration time, improves accuracy, and can be with a large amount of samples of METHOD FOR CONTINUOUS DETERMINATION, precisely to analyze different leaf colors, no
The volatile components such as same population, different harvest time and different recovery sites are of great significance.Thus, select HS-SPME/
GC-MS is a kind of more satisfactory tealeaves analysis of volatile components technology.
Francolin tea blade has the function such as eliminating the phlegm, cough-relieving, wind dispelling, expelling parasite, analgesia, antidepression, antibacterial, antianxiety, antitumor
Can, Hainan and its overseas Chinese generations are dual-purpose with francolin tea blade tea medicine, the sexual function however, different leaf color francolin teas volatilize
Always bone of contention.
In conclusion problem of the existing technology is: 65 μm of PDMS/DVB extracting heads of selection carry out extraction ageing time
It is too long, extracting head is caused to damage and increase experimental period, it is too short or do not carry out aging, then it can there are last time experiment residuals
Object influences to test accuracy, so that experiment is undesirable;The too long volatilization that will lead to some minor compounds in sample of extraction time
Property ingredient it is capped, extraction time is too short, and sample can be made not extract sufficiently, and sample to be tested ingredient is caused to lack.By repeatedly into
Row extraction, finds its preferable extraction time, obtains relatively good experimental data.
Solve the difficulty and meaning of above-mentioned technical problem:
(1) according to bibliographic reference, 65 μm of PDMS/DVB extracting heads are selected to be extracted, it is suitable for volatile materials, amine
The extraction of class, nitryl aromatic class compound, and more ingredients can be obtained.Ageing time is too long extracting head can be caused damage and
Increase experimental period, it is too short or do not carry out aging, then can there are the last times to test residue, influence to test accuracy so that
It tests undesirable.
(2) the too long volatile component that will lead to some minor compounds in sample of extraction time is capped, extraction time
It is too short, sample can be made not extract sufficiently, sample to be tested ingredient is caused to lack.By repeatedly being extracted, finds it and preferably extract
Time obtains relatively good experimental data.
(3) setting of chromatographic mass spectrometry condition: carrier gas and flow velocity, carrier gas and flow velocity, the selection of column temperature, the selection of column temperature, color
The settings such as the selection of column length and internal diameter, the selection of column length and internal diameter are composed, the accuracy of experiment can be all influenced.By repeatedly real
The preferable condition for obtaining its setting is tested, to reduce experimental error.
Summary of the invention
In view of the problems of the existing technology, the present invention provides a kind of francolin congo red, the GC- of green fresh leaf volatile component
MS analysis method.
The invention is realized in this way the GC-MS analysis method of a kind of francolin congo red, green fresh leaf volatile component, described
Francolin congo red, the GC-MS analysis method of green fresh leaf volatile component the following steps are included:
(1) PDMS/DVB solid phase micro-extracting head aging: equal 250 DEG C of extracting head preparatory aging 15min before each sample introduction;
(2) GC conditions: chromatographic column Agilent HP-5MS, carrier gas are high-purity helium, injector temperature 250
DEG C, it does not shunt, temperature programming: 40 DEG C of initial temperature, keeping 4min, rise to 80 DEG C with 5 DEG C/min, then risen to 10 DEG C/min
260 DEG C, keep 10min, flow velocity 1mL/min;
(3) Mass Spectrometry Conditions: ion source: the source electron bombardment EI;Ion source temperature: 230 DEG C, 150 DEG C of level four bars;Ionization voltage
70eV;Scanning range: 35.0-800.0aum, full scan acquisition mode;By 65 μm of solid phase micro-extracting heads of PDMS/DVB be inserted into
Sample mouth carries out instrument analysis by above-mentioned gas-chromatography and Mass Spectrometry Conditions, until chromatogram does not have peak appearance;
(4) extracting head is distinguished in mixing comparison ml headspace bottle and francolin tea sample bottle and extracts, sample introduction parses the time as 120S;
Optimized Extraction temperature and time carries out extraction absorption using 25 DEG C of extraction temperature and time 40min;The chromatographic peak of acquisition is done this
After bottom buckle is removed, the compound mass spectrogram for deducting background is obtained, while calculating each ingredient percentage with peak area normalization method and containing
Amount, 3 repetition experiments are averaged.
Further, the francolin tea red fresh leaf leaf of the francolin congo red, the GC-MS analysis method of green fresh leaf volatile component
Piece volatile component identifies 30 kinds, and green fresh leaf blade volatile component identifies 31 kinds, red, green fresh leaf it is jointly owned at
Divide 26 kinds, the total ingredient 74.29% of Zhan;
The type and percentage contents of francolin tea red fresh leaf major volatile constituents are as follows: carypohyllene 25.65%, rule grass
Alkene 14.93%, 4- hexen-1-ol acid esters 11%, α-guaiene 9.11%, beta waves side alkene 7.42%, big bicyclogermacrene D
6.71%, A- cloth Chenopodiaceae alkene 5.60%, copaene 3.53%, (-)-α-cubebene 1.67% etc.;Wherein 4- hexen-1-ol acid
Ester, carypohyllene and humulene account for the 51.58% of volatilization oil chromatography total amount, but are free of tridecane, (-)-α-Gu Yun in red fresh leaf
Alkene, d- cadinene, aromadendrene, ledol,-two ring [4.4.0] decyl- 1- alkene of isopropyl -5- methyl -9- methylene.
The type and percentage contents of major volatile constituents in francolin tea green fresh leaf are as follows: carypohyllene 13.90%, rule
Oxalene 1.85%, 4- hexen-1-ol acid esters 9.53%, α-guaiene 8.19%, beta waves side alkene 5.36%, big bicyclogermacrene D
5.66%, A- cloth Chenopodiaceae alkene 5.11%, copaene 12.35%, (-)-α-cubebene 9.17% etc.;Wherein 4- hexen-1-ol
Acid esters, carypohyllene and humulene account for the 25.28% of volatilization oil chromatography total amount, but are free of pulegone, [1R- in green fresh leaf
(1a, 4a, 8a)] -1,2,4a, 5,6,8a- hexahydro -4,7- dimethyl -1- (1- Methylethyl) naphthalene, patchoulane and 3,4- bis-
Methyl -3- cyclohexene-1-formaldehyde.
Another object of the present invention is to provide the GC-MS of francolin congo red, green fresh leaf volatile component described in one kind points
Volatilization oil product that analysis method obtains, described volatilization oil product include carypohyllene, humulene, copaene, cadinene, (-)-α-Bi
Clear eggplant oil alkene, elemene, α-guaiene, beta waves side alkene.
Another object of the present invention is to provide eliminating the phlegm, the cough-relievings, wind dispelling drug of volatilization oil product preparation described in one kind.
Another object of the present invention is to provide the expelling parasite of volatilization oil product preparation described in one kind, analgesia, antidepression, resist
Bacterium drug.
Another object of the present invention is to provide the antianxieties of volatilization oil product preparation described in one kind, anti-tumor drug.
In conclusion advantages of the present invention and good effect are as follows: the present invention using francolin congo red, green fresh leaf as research pair
As analyzing their volatile component using HS-SPME/GC-MS method, and composition to their volatile component and its opposite
Percentage composition is compared, and verifies the difference of francolin tea difference leaf color volatile component, develops characteristic tealeaves " francolin for Hainan
Tea " tea product provides certain theoretical basis and technical support.
Detailed description of the invention
Fig. 1 is francolin congo red provided in an embodiment of the present invention, the GC-MS analysis method process of green fresh leaf volatile component
Figure.
Fig. 2 be francolin tea red fresh leaf blade volatile component HS-SPME-GC-MS provided in an embodiment of the present invention always from
Subflow figure.
Fig. 3 be francolin tea green fresh leaf blade volatile component HS-SPME-GC-MS provided in an embodiment of the present invention always from
Subflow figure.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
Application principle of the invention is explained in detail with reference to the accompanying drawing.
As shown in Figure 1, the GC-MS analysis method of francolin congo red provided in an embodiment of the present invention, green fresh leaf volatile component
The following steps are included:
S101;PDMS/DVB solid phase micro-extracting head aging: equal 250 DEG C of extracting head preparatory aging 15min before each sample introduction;
S102: GC conditions: chromatographic column Agilent HP-5MS (0.25 μm of the μ m of 30m × 250), carrier gas are high-purity
It spends helium (purity 99.999%), 250 DEG C of injector temperature, does not shunt, temperature programming: 40 DEG C of initial temperature, keeping 4min, with
5 DEG C/min rises to 80 DEG C, then rises to 260 DEG C with 10 DEG C/min, keeps 10min, flow velocity 1mL/min;
S103: Mass Spectrometry Conditions: ion source: the source electron bombardment (EI);Ion source temperature: 230 DEG C, 150 DEG C of level four bars;Ionization
Voltage 70eV;Scanning range: 35.0-800.0aum, full scan acquisition mode.65 μm of solid phase micro-extracting heads of PDMS/DVB are inserted
Enter injection port, carry out instrument analysis by above-mentioned gas-chromatography and Mass Spectrometry Conditions, until chromatogram does not have peak appearance;
S104: extracting head being distinguished in mixing comparison ml headspace bottle and francolin tea sample bottle and is extracted, sample introduction parsing the time be
120S;Optimized Extraction temperature and time carries out extraction absorption using more satisfactory extraction temperature and time, it may be assumed that and 25 DEG C,
40min;After the chromatographic peak of acquisition is done background rejection with Agilent MSD Chemstation E2.02, obtains and deduct background
Compound mass spectrogram, while MSD Chemstation E2.02 is used, each ingredient percentage is calculated with peak area normalization method
Content, 3 repetition experiments are averaged.
Application effect of the invention is explained in detail below with reference to experiment.
1 materials and methods
Laboratory apparatus
Agilent6890A+5975C gas chromatograph-mass spectrometer (GC-MS) (Agilent company of the U.S.), HP-5MS chromatographic column (beauty
State's agilent company), PDMS/DVB 65m solid phase micro-extracting head (Supelco company, the U.S.).
1.2 experimental material
Red, the green fresh blade of francolin tea contemporaneity derives from University Of Hainan torrid zone agricultural institute Experimental Base, acquisition
Time is on August 3rd, 2017.
1.3 experimental method
1.3.1 sample preparation
It will be crushed without worm channel francolin tealeaves, 2g is taken to be put into 20ml ml headspace bottle, and be control with empty ml headspace bottle.
1.3.2GC-MS method
PDMS/DVB solid phase micro-extracting head aging: equal 250 DEG C of extracting head preparatory aging 15min before each sample introduction.
GC conditions: chromatographic column Agilent HP-5MS (0.25 μm of the μ m of 30m × 250), carrier gas are high-purity helium
Gas (purity 99.999%), does not shunt, temperature programming by 250 DEG C of injector temperature: 40 DEG C of initial temperature, keep 4min, with 5 DEG C/
Min rises to 80 DEG C, then rises to 260 DEG C with 10 DEG C/min, keeps 10min, flow velocity 1mL/min.
Mass Spectrometry Conditions: ion source: the source electron bombardment (EI);Ion source temperature: 230 DEG C, 150 DEG C of level four bars;Ionization voltage
70eV;Scanning range: 35.0-800.0aum, full scan acquisition mode.By 65 μm of solid phase micro-extracting heads of PDMS/DVB be inserted into
Sample mouth carries out instrument analysis by above-mentioned gas-chromatography and Mass Spectrometry Conditions, until chromatogram does not have peak appearance.By extracting head point
It is extracted in other mixing comparison ml headspace bottle and francolin tea sample bottle, sample introduction parses the time as 120S.Optimized Extraction temperature and time, is answered
Extraction absorption is carried out with more satisfactory extraction temperature and time, it may be assumed that 25 DEG C, 40min.With Agilent MSD Chemstation
After the chromatographic peak of acquisition is done background rejection by E2.02, the compound mass spectrogram for deducting background is obtained, with American National Standard and skill
Art research institute standard mass spectrum picture library carries out substance retrieval (NIST11.0), checks in conjunction with document, while using MSD
Chemstation E2.02 calculates each ingredient percentage contents with peak area normalization method, and 3 repetition experiments are averaged.
2 results and analysis
The chemical component of 2.1 francolin tea red blades and green blade volatile materials
With HS-SPME-GC-MS measure red, greenery color francolin fresh tea leaves blade percentage contents be detailed in following table and always from
Subflow chromatogram is shown in that Fig. 2, Fig. 3, abscissa are retention time, and ordinate is the intensity of total ion current.
The volatile component and relative amount of 1 francolin congo red of table, green fresh leaf blade
Continued 1
Fig. 2, Fig. 3 and table 1, table 2 the result shows that, francolin tea red fresh leaf blade volatile component identifies 30 kinds, green
Fresh leaf blade volatile component identifies 31 kinds, jointly owned 26 kinds of ingredient of red, green fresh leaf, the total ingredient 74.29% of Zhan.Francolin
The type and percentage contents of congo red color fresh leaf major volatile constituents are as follows: carypohyllene 25.65%, humulene 14.93%, 4-
Hexen-1-ol acid esters 11%, α-guaiene 9.11%, beta waves side alkene 7.42%, big bicyclogermacrene D 6.71%, A- cloth Chenopodiaceae alkene
5.60%, copaene 3.53%, (-)-α-cubebene 1.67% etc.;Wherein 4- hexen-1-ol acid esters, carypohyllene and rule grass
Alkene accounts for the 51.58% of volatilization oil chromatography total amount, but is free of tridecane, (-)-α-gurjunene, d- cadinene, Xiang Shu in red fresh leaf
Alkene, ledol,-two ring [4.4.0] decyl- 1- alkene of isopropyl -5- methyl -9- methylene.It is mainly waved in francolin tea green fresh leaf
The type and percentage contents of hair property ingredient are as follows: carypohyllene 13.90%, humulene 1.85%, 4- hexen-1-ol acid esters
9.53%, α-guaiene 8.19%, beta waves side alkene 5.36%, big bicyclogermacrene D 5.66%, A- cloth Chenopodiaceae alkene 5.11%, copaene
12.35%, (-)-α-cubebene 9.17% etc.;Wherein 4- hexen-1-ol acid esters, carypohyllene and humulene account for volatilization oil colours
The 25.28% of total amount is composed, but without pulegone, [1R- (1a, 4a, 8a)] -1,2,4a, 5,6,8a- hexahydros-in green fresh leaf
4,7- dimethyl -1- (1- Methylethyl) naphthalene, patchoulane and 3,4- dimethyl -3- cyclohexene-1-formaldehyde.In terms of result of study
Out, the main volatile components of the green fresh leaf of francolin congo red are largely identical, but percentage contents difference is larger.
2 francolin congo red of table, green fresh leaf major volatile constituents and relative amount
The structure characteristic analysis of 2.2 francolin congo red, green fresh leaf blade volatile component
For the chemical structure characteristic for further analyzing and belonging to flavor component chromatographic peak, by francolin tea red fresh leaf blade and
Green fresh leaf blade volatile component is sorted out, olefines, alkanes, aldehydes, ketone and alcohol in red fresh leaf volatile component
Class accounts for 77%, 7%, 3%, 3%, the 10% of total amount respectively, olefines, alkanes and alcohols point in green fresh leaf volatile component
77%, 10%, the 13% of total amount is not accounted for, and aldehydes and ketone do not detect.It is recognised that francolin tea blade volatility main component
It is olefines and alcohols material.
Different leaf color francolin volatile component medical values, carypohyllene are a kind of double bond containing natural products, Chinese GB
2760-1996 be approved as allowing using food flavor, have α-, β-, γ-three kinds of isomers, the common carypohyllene master of fragrance circle
Refer to that β-carypohyllene, α-carypohyllene are known as humulene.Report according to pertinent literature: β-carypohyllene has eliminating the phlegm, cough-relieving, wind dispelling, hair
Sweat, expelling parasite, analgesia, antidepression, antibacterial, anti-inflammatory, antianxiety, antitumor, anti-oxidant and other effects, guaiene anti-inflammatory, antirheumatic,
Promote the sexual maturity, restrain, having curative effect face cream, diuresis, hypocatharsis, inspire sweat;Humulene have relieving asthma, antibechic, eliminating the phlegm, treat tracheitis function
Effect, cadinene play the role of eliminating the phlegm.Copaene has antibacterial, anti-true, heart tonifying, diuresis, haemocylolysis (most strong);The function such as calmness
Effect.α-cubebene has antioxidant activity, can be used for food preservative, it is anti-that elemene was approved as national two classes in 1994
Tumour new drug, numerous studies prove: elemene injection has broad spectrum activity, high efficiency and hypotoxicity, can press down that kill kinds of tumors thin
Born of the same parents, and inducing apoptosis of tumour cell and differentiation, improve immunity of organisms the features such as, malignant pleural effusion, a variety of solid tumors and
It is widely applied in the illnesss such as brain metastases.Different leaf color francolin teas all have heat-clearing, removing toxic substances, aid digestion, the greasy, anti-inflammatory of solution, anti-
Analgesia, antidepression, antibacterial antianxiety, antitumor, anti-oxidant and other effects.
Result of study is shown: in the red fresh blade of francolin tea, identifying main volatile component compound has: China pink
Alkene 25.65%, humulene 14.93%, 4- hexen-1-ol acid esters 11%, α-guaiene 9.11%, alkene 7.42% by beta waves,
Big bicyclogermacrene D 6.71%, A- cloth Chenopodiaceae alkene 5.60%, copaene 3.53%, (-)-α-cubebene 1.67% etc.;It volatilizees
Property the sum of ingredient percentage composition be 85.62%;And in the fresh blade of green francolin tea, identify main volatile component chemical combination
Object has: carypohyllene 13.90%, humulene 1.85%, 4- hexen-1-ol acid esters 9.53%, α-guaiene 8.19%, by beta waves
Alkene 5.36%, big bicyclogermacrene D 5.66%, A- cloth Chenopodiaceae alkene 5.11%, copaene 12.35%, (-)-α-cubebene 9.17%
Deng the sum of volatile component percentage composition are as follows: 71.12%.It was found from result of study: same population difference leaf color francolin tea function
Can ingredient percentage contents it is widely different, same population difference harvest time and different recovery site Volatility Levels and function
It can be still the point at issue at being grouped as etc..Therefore, system studies francolin tea comprehensively and to excavate excellent germplasm extremely urgent.
The present invention thinks that head space is solid by analyzing after francolin tea volatile oil component compares with other scholars using SDE method
Phase extraction method can preferably realize the extraction to francolin tea volatile component, preferably embody the original aroma information of tealeaves.
This research analyzes the green fresh leaf volatile component of francolin congo red by headspace solid-phase microextraction combination GC-MS method, and to its volatility
Ingredient is compared discovery: can identify fragrance component component and percentage contents, volatility in red, greenery francolin tea
For ingredient based on olefines, aldehydes, ketone and alkanes content are lower;By comparison, it was found that francolin tea red fresh leaf and green
Color fresh leaf volatile composition components detection sum and special volatile compound number are essentially identical, but corresponding percentage composition is distinguished
Larger, such as: the carypohyllene and humulene proportion in red francolin tea blade are larger.
The sum of percentage composition in main medicinal function ingredient same composition compares: the francolin tea of red blade
(85.62%) > green blade francolin tea (71.12%), the sum of humulene and carypohyllene in red fresh leaf francolin tea
(40.58%) the sum of humulene and carypohyllene (15.75%) in > green fresh leaf francolin tea.Therefore, red blade francolin tea is being dispelled
Phlegm, cough-relieving, wind dispelling, expelling parasite, analgesia, antidepression, antibacterial, antianxiety, antitumor etc. are better than green blade francolin tea.
In conclusion being rich in carypohyllene, humulene, copaene, cadinene, α-cubeb oil in francolin tea blade volatile oil
Alkene, elemene, α-guaiene, the functional components such as alkene by beta waves, thus different leaf color francolin teas all have eliminating the phlegm, cough-relieving, wind dispelling,
The functions such as expelling parasite, analgesia, antidepression, antibacterial, antianxiety, antitumor.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (6)
1. the GC-MS analysis method of a kind of francolin congo red, green fresh leaf volatile component, which is characterized in that the francolin congo red, green
The GC-MS analysis method of fresh leaf volatile component the following steps are included:
(1) PDMS/DVB solid phase micro-extracting head aging: equal 250 DEG C of extracting head preparatory aging 15min before each sample introduction;
(2) GC conditions: chromatographic column AgilentHP-5MS, carrier gas be high-purity helium, 250 DEG C of injector temperature, regardless of
Stream, temperature programming:, keeping 4min, rise to 80 DEG C with 5 DEG C/min, then rise to 260 DEG C with 10 DEG C/min by 40 DEG C of initial temperature,
Keep 10min, flow velocity 1mL/min;
(3) Mass Spectrometry Conditions: ion source: the source electron bombardment EI;Ion source temperature: 230 DEG C, 150 DEG C of level four bars;Ionization voltage
70eV;Scanning range: 35.0-800.0aum, full scan acquisition mode;PDMS/DVB65 μm of solid phase micro-extracting head is inserted into sample introduction
Mouthful, instrument analysis is carried out by above-mentioned gas-chromatography and Mass Spectrometry Conditions, until chromatogram does not have peak appearance;
(4) extracting head is distinguished in mixing comparison ml headspace bottle and francolin tea sample bottle and extracts, sample introduction parses the time as 120S;Optimization
Extraction temperature and time carry out extraction absorption using 25 DEG C of extraction temperature and time 40min;The chromatographic peak of acquisition is done into this bottom buckle
After removing, the compound mass spectrogram for deducting background is obtained, while using each ingredient percentage contents of peak area normalization method calculating, 3
Secondary repetition experiment is averaged.
2. the GC-MS analysis method of francolin congo red as described in claim 1, green fresh leaf volatile component, which is characterized in that institute
State the francolin tea red fresh leaf blade volatile component identification of francolin congo red, the GC-MS analysis method of green fresh leaf volatile component
30 kinds out, green fresh leaf blade volatile component identifies 31 kinds, jointly owned 26 kinds of ingredient of red, green fresh leaf, the total ingredient of Zhan
74.29%;
The type and percentage contents of francolin tea red fresh leaf major volatile constituents are as follows: carypohyllene 25.65%, humulene
14.93%, 4- hexen-1-ol acid esters 11%, α-guaiene 9.11%, alkene 7.42% by beta waves, big bicyclogermacrene D6.71%,
A- cloth Chenopodiaceae alkene 5.60%, copaene 3.53%, (-)-α-cubebene 1.67% etc.;Wherein 4- hexen-1-ol acid esters, China pink
Alkene and humulene account for the 51.58% of volatilization oil chromatography total amount, but without tridecane, (-)-α-gurjunene, d- Du in red fresh leaf
Loose alkene, aromadendrene, ledol,-two ring [4.4.0] decyl- 1- alkene of isopropyl -5- methyl -9- methylene;
The type and percentage contents of major volatile constituents in francolin tea green fresh leaf are as follows: carypohyllene 13.90%, humulene
1.85%, 4- hexen-1-ol acid esters 9.53%, α-guaiene 8.19%, alkene 5.36% by beta waves, big bicyclogermacrene D5.66%,
A- cloth Chenopodiaceae alkene 5.11%, copaene 12.35%, (-)-α-cubebene 9.17% etc.;Wherein 4- hexen-1-ol acid esters, stone
Bamboo alkene and humulene account for the 25.28% of volatilization oil chromatography total amount, but in green fresh leaf without pulegone, [1R- (and 1a, 4a,
8a)] -1,2,4a, 5,6,8a- hexahydro -4,7- dimethyl -1- (1- Methylethyl) naphthalene, patchoulane and 3,4- dimethyl -3- ring
Hexene -1- formaldehyde.
3. the volatilization that a kind of francolin congo red as described in claim 1, the GC-MS analysis method of green fresh leaf volatile component obtain
Oil product, which is characterized in that described volatilization oil product includes carypohyllene, humulene, copaene, cadinene, (-)-α-piper cubeba
Oily alkene, elemene, α-guaiene, beta waves side alkene.
4. a kind of eliminating the phlegm, the cough-relieving, wind dispelling drug of volatilization oil product preparation as described in claim 1.
5. a kind of expelling parasite, the analgesia, antidepression, antibacterials of volatilization oil product preparation as described in claim 1.
6. a kind of antianxiety of volatilization oil product preparation as described in claim 1, anti-tumor drug.
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CN110243959A (en) * | 2019-06-11 | 2019-09-17 | 华中农业大学 | A kind of separation of endogenous fragrance component in Carnation flowers and identification method |
CN113848275A (en) * | 2021-07-30 | 2021-12-28 | 海南大学 | Analysis method of flavor components of golden pomfret slices |
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CN115236239A (en) * | 2022-08-09 | 2022-10-25 | 多特瑞(上海)商贸有限公司 | Method for detecting content of alpha-copal in schisandra essential oil |
CN115236239B (en) * | 2022-08-09 | 2023-12-29 | 多特瑞(上海)商贸有限公司 | Method for detecting content of alpha-copaene in schisandra essential oil |
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