CN109212102A - A method of cape jasmine oil is identified based on characteristic component gas chromatography-mass spectrum finger-print - Google Patents
A method of cape jasmine oil is identified based on characteristic component gas chromatography-mass spectrum finger-print Download PDFInfo
- Publication number
- CN109212102A CN109212102A CN201811336908.4A CN201811336908A CN109212102A CN 109212102 A CN109212102 A CN 109212102A CN 201811336908 A CN201811336908 A CN 201811336908A CN 109212102 A CN109212102 A CN 109212102A
- Authority
- CN
- China
- Prior art keywords
- cape jasmine
- mass
- jasmine oil
- oil
- gas chromatography
- 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.)
- Granted
Links
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
-
- 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
-
- 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
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 discloses a kind of methods for identifying cape jasmine oil based on characteristic component gas chromatography-mass spectrum finger-print, set about from the volatile component of cape jasmine oil, using headspace solid-phase microextraction, in conjunction with Gas chromatographyMass spectrometry, the volatile feature components of analysis detection cape jasmine and cape jasmine oil, establish the gas chromatography-mass spectrum characteristic fingerprint pattern of the volatile component of cape jasmine and cape jasmine oil, it is compared by effective peak of the evaluation software to characteristic fingerprint pattern, to realize the identification to cape jasmine oil.There is the characteristic component of characteristic fingerprint pattern to retain completion, identify accuracy rate height for this method, and anti-interference strong, simple operation and other advantages are a kind of detection methods that can quickly identify cape jasmine oil.
Description
Technical field
The invention belongs to detection technique fields, and in particular to one kind is based on characteristic component gas chromatography-mass spectrum finger-print
Identify the method for cape jasmine oil.
Background technique
Cape jasmine is a kind of small-sized evergreen shrubs of Rubiaceae Gardenia Ellis, and widely distributed in China, the fruit of cape jasmine is in tradition
Medicine belongs to the l batches of dual-purpose of drug and food resources that the Ministry of Public Health promulgates, research in recent years finds that the oil content of cape jasmine and soybean are close, fat
Acid predominantly linoleic acid, oleic acid and palmitinic acid are a kind of functional oil plant full of nutrition, Cape jasmine respectively up to 50%, 20% and 20%
The distinctive smell of son has the function of calmness, hypnosis, anticonvulsion and promotion learning and memory, utilizes cape jasmine and the spy of cape jasmine oil
Smell is levied, the gas chromatography-mass spectrum finger-print of cape jasmine oil characteristic component is established, can be used as a kind of inspection that identification cape jasmine oil is true and false
Survey method.
Currently, the identification of edible oil and fat mainly has following three kinds of methods: (1) generating fatty acid methyl ester using transesterification, so
The content for measuring wherein each fatty acid using gas chromatography afterwards, to judge the kind of grease.The main component of cape jasmine oil is
Linoleic acid, oleic acid and palmitinic acid, this is similar to the main component of a variety of other edible vegetable oils, so the method for fatty acid methyl ester
The characteristic component of cape jasmine oil can not be found out, can not be to true and false the identifying of cape jasmine oil, it can only be by each content of fatty acid not
Judge with the accordance to grease.And the method pre-treatment is complex, agents useful for same is more toxic.(2) distillation is utilized
Method extracts the volatile ingredient of edible oil and fat, separates qualitative analysis volatile component through gas-chromatography, and then pass through volatility group
Divide to constitute and the type of edible oil is identified.But the way of distillation time is longer, while distilling it is also possible that certain volatility objects
Matter by high temperature destruction and recurring structure change, and gas chromatography can not directly to component carry out qualitative analysis, so this
Method is also not used to identify the true and false of cape jasmine oil.(3) it is measured to form finger-print using the volatile component of edible oil,
Edible oil is identified by finger-print.But existing finger print method only surveys the volatile component of edible oil
It is shaped as finger-print, all the volatile component of its raw material is not measured to form common finger-print.Since raw material is adding
After work is at edible oil, the content of some feature volatile components in the oil has and significantly reduces, although still having on spectrogram
Peak exists, but since peak area is smaller, when forming finger-print, may be ignored, and these components are just these
The important feature of edible oil.So the volatile component just with edible oil forms finger-print, cannot achieve to edible oil
Accurate identification.Currently, reliably the method for the identification cape jasmine oil based on volatile ingredients fingerprint is reported not yet.
Summary of the invention
The main object of the present invention is to identify difficult problem for cape jasmine oil, is developed a kind of based on the micro- extraction of head space solid phase
It takes, the new method of Gas chromatographyMass spectrometry analysis detection cape jasmine oil volatile feature components, based on the analysis established
The gas chromatography-mass spectrum finger-print for the cape jasmine oil volatile feature components that method is established provides one kind to identify cape jasmine oil
Convenient, the reliable method of inspection.
To achieve the above object, the present invention uses following technological means:
The present invention sets about from the volatile component of cape jasmine oil, using headspace solid-phase microextraction, in conjunction with gas chromatography-mass spectrography skill
The volatile feature components of art, analysis detection cape jasmine and cape jasmine oil establish the gas phase color of the volatile component of cape jasmine and cape jasmine oil
Spectrum-mass spectral characteristic finger-print is compared by effective peak of the evaluation software to characteristic fingerprint pattern, to realize to cape jasmine
The identification of oil.There is the characteristic component of characteristic fingerprint pattern to retain completion, identify accuracy rate height for this method, anti-interference strong, operation
The advantages that simple is a kind of detection method that can quickly identify cape jasmine oil.
Specifically comprise the following steps:
The gas chromatography-mass spectrometry analysis of step (1) cape jasmine and authentic cape jasmine oil volatile component.It is specific as follows: to take the cape jasmine of 1g
(pulverizer crushes after 70 DEG C of freeze-day with constant temperature) or the cape jasmine oil of 1mL are placed in 20mL headspace sampling bottle, are sealed rapidly, insertion 50/
Extracting fiber is extracted and is inserted rapidly after 60 DEG C of absorption volatile component 40min by 30 μm of DVB/CAR/PDMS extracting fibers
Enter gas chromatograph injection port and desorbs 5 min.It is right using under gas chromatograph-mass spectrometer (GC-MS) chromatography below and Mass Spectrometry Conditions
Volatile component carries out separation and qualitative analysis, retrieves to each peak in total ion current figure through mass spectrum computer data system and core
To NIST14 LIBRARY standard mass spectrogram, compound of the matching degree greater than 85% can be used as qualification result, obtain cape jasmine and orthodox school
The gas chromatography-mass spectrum spectrogram (see figure 1) of cape jasmine oil volatile component.
GC conditions: chromatographic column, DB-5MS(30m × 0.25mm × 0.25 μm) capillary column；Temperature programming: 40 DEG C
4 min are kept, 70 DEG C is warming up to the speed of 6 DEG C/min, keeps 8 min, 180 DEG C is warming up to the speed of 6 DEG C/min, protects
Hold 3min；250 DEG C of injector temperature；Carrier gas He, flow velocity 1mL/min；It does not shunt, solvent delay 4min.
Mass Spectrometry Conditions: EI ion source, electron energy 70eV, scanning range m/z50.00-500.00, ion source temperature 200
DEG C, 250 DEG C of interface temperature.
The foundation of the characteristic fingerprint pattern of step (2) cape jasmine oil volatile component gas chromatography-mass spectrum.According to step (1)
The gas chromatography-mass spectrometry analysis of cape jasmine and authentic cape jasmine oil volatile component is as a result, choose the common of 11 cape jasmines and cape jasmine oil
Characteristic peak: (1) appearance time 5.631 minutes, Hexanal(hexanal), mass-to-charge ratio 56.05 and 72.10；(2) appearance time
8.506 minutes, 1,3,5,7-Cyclooctatetraene(cyclo-octatetraene), mass-to-charge ratio 51.05,78.05 and 104.10；(3) go out
Peak time 12.290 minutes, Furan, 2-pentyl-(2- n-pentyl furans), mass-to-charge ratio 53.05,81.05 and 138.15；(4)
Appearance time 13.506 minutes, 2,2,5,5-Tetramethyl-3-cyclopenten-1-one(2,2,5,5- tetramethyl -3-
Cyclopentene-1-one), mass-to-charge ratio 70.05,95.10 and 110.15；(5) appearance time 14.071 minutes, Benzene, 1,2,3-
Trimethyl-(1,2,3- trimethylbenzenes), mass-to-charge ratio 104.10 and 120.15；(6) appearance time 21.266 minutes,
Isophorone(isophorone), mass-to-charge ratio 54.05,82.10 and 138.15；(7) appearance time 22.239 minutes, 2,6,6-
Trimethyl-2-cyclohexene-1,4-dione(4- oxoisophorone), mass-to-charge ratio 68.00,96.05 and 152.10；
(8) appearance time 24.096 minutes, 1,3-Cyclohexadiene-1-carboxaldehyde, 2,6,6-trimethyl-
(safranal), mass-to-charge ratio 91.10,107.10,121.15 and 150.15；(9) appearance time 25.048 minutes, 4-
Methyleneisophorone4-(methylene isophorone), mass-to-charge ratio 91.05,107.10 and 150.15；(10) appearance time
27.662 minutes, Nonanoic acid(n-nonanoic acid), mass-to-charge ratio 60.00,73.05 and 115.10；(11) appearance time 30.408 divides
Clock, 2,4,7,9-Tetramethyl-5-decyn-4,7-diol(2,4,7,9- tetramethyl -5- decine -4,7- glycol), matter lotus
Than 109.10 and 151.15.The characteristic fingerprint pattern (see figure 2) of gas chromatography-mass spectrum as cape jasmine oil.
The identification of step (3) cape jasmine oil.Commercially available cape jasmine oil or unknown edible vegetable oil is taken to obtain its volatility by step (1)
The gas chromatography-mass spectrum spectrogram of ingredient utilizes the gas phase color of similarity evaluation comparison cape jasmine oil
The gas-chromatography-of the volatile component of spectrum-mass spectrographic characteristic fingerprint pattern (Fig. 2) and commercially available cape jasmine oil or unknown edible vegetable oil
Mass spectrogram confirms the common trait peak of 11 cape jasmines and cape jasmine oil, is less than 0.1min, matter lotus by retention time difference
It is greater than 0.5% less than 0.05, relative peak area than difference to be differentiated for effective peak, 11 common trait peaks occur 9 and are confirmed as
Cape jasmine oil is confirmed as non-cape jasmine oil less than 9.
The beneficial effects of the present invention are:
(1) present invention is for true and false the identifying to cape jasmine oil, using gaschromatographic mass spectrometric analysis to the feature in cape jasmine oil
Finger-print is completely analyzed and formed to volatile component, to improve the accuracy and reliability of identification, compensates for sense
The more abstract deficiency of official's analysis.
(2) finger-print includes 11 common trait peaks of cape jasmine and cape jasmine oil, accuracy and reliability height, applicability
Extensively, speed is fast, at low cost, the method established can quickly identify cape jasmine oil, identify the time less than 90 minutes, accuracy rate it is reachable
100%, it is only head space bottle cap that each sample, which identifies consumptive material, and cost is lower than 10 yuan.
(3) to be stored in work with the finger-print data that the common trait peak of cape jasmine and the volatile component of cape jasmine oil is made into soft
It can be used for a long time in part, without calibration.
Detailed description of the invention
Fig. 1 is cape jasmine of the embodiment of the present invention (a) and oily (b) volatile component gas chromatography-mass spectrometry analysis spectrogram of cape jasmine；
Fig. 2 is that the embodiment of the present invention includes the common trait peaks of 11 cape jasmines and cape jasmine oil, the gas-chromatography-as cape jasmine oil
Mass spectral characteristic finger-print；
Fig. 3 is identification (the volatile component gas chromatography-mass spectrum spectrogram and Cape jasmine of commercially available cape jasmine oil of the commercially available cape jasmine oil of embodiment
The comparison of the gas chromatography-mass spectrum characteristic fingerprint pattern of seed oil)；
Fig. 4 is identification (the volatile component gas chromatography-mass spectrum of commercially available other plant oil of the commercially available other plant oil of embodiment
The comparison of the gas chromatography-mass spectrum characteristic fingerprint pattern of spectrogram and cape jasmine oil).
Specific embodiment
Below in conjunction with specific embodiment, the present invention will be further described, but the present invention is not limited only to these embodiments.
Embodiment 1
The identification of commercially available cape jasmine oil, specifically comprises the following steps:
The gas chromatography-mass spectrometry analysis of step (1) cape jasmine and authentic cape jasmine oil volatile component.It is specific as follows: to take the cape jasmine of 1g
(pulverizer crushes after 70 DEG C of freeze-day with constant temperature) or the cape jasmine oil of 1mL are placed in 20mL headspace sampling bottle, are sealed rapidly, insertion 50/
Extracting fiber is extracted and is inserted rapidly after 60 DEG C of absorption volatile component 40min by 30 μm of DVB/CAR/PDMS extracting fibers
Enter gas chromatograph injection port and desorbs 5 min.It is right using under gas chromatograph-mass spectrometer (GC-MS) chromatography below and Mass Spectrometry Conditions
Volatile component carries out separation and qualitative analysis, retrieves to each peak in total ion current figure through mass spectrum computer data system and core
To NIST14 LIBRARY standard mass spectrogram, compound of the matching degree greater than 85% can be used as qualification result, obtain cape jasmine and orthodox school
The gas chromatography-mass spectrum spectrogram (see figure 1) of cape jasmine oil volatile component.
GC conditions: chromatographic column, DB-5MS(30m × 0.25mm × 0.25 μm) capillary column；Temperature programming: 40 DEG C
4 min are kept, 70 DEG C is warming up to the speed of 6 DEG C/min, keeps 8 min, 180 DEG C is warming up to the speed of 6 DEG C/min, protects
Hold 3min；250 DEG C of injector temperature；Carrier gas He, flow velocity 1mL/min；It does not shunt, solvent delay 4min.
Mass Spectrometry Conditions: EI ion source, electron energy 70eV, scanning range m/z50.00-500.00, ion source temperature 200
DEG C, 250 DEG C of interface temperature.
The foundation of the characteristic fingerprint pattern of step (2) cape jasmine oil volatile component gas chromatography-mass spectrum.According to step (1)
The gas chromatography-mass spectrometry analysis of cape jasmine and authentic cape jasmine oil volatile component is as a result, choose the common of 11 cape jasmines and cape jasmine oil
Characteristic peak: (1) appearance time 5.631 minutes, Hexanal(hexanal), mass-to-charge ratio 56.05 and 72.10；(2) appearance time
8.506 minutes, 1,3,5,7-Cyclooctatetraene(cyclo-octatetraene), mass-to-charge ratio 51.05,78.05 and 104.10；(3) go out
Peak time 12.290 minutes, Furan, 2-pentyl-(2- n-pentyl furans), mass-to-charge ratio 53.05,81.05 and 138.15；(4)
Appearance time 13.506 minutes, 2,2,5,5-Tetramethyl-3-cyclopenten-1-one(2,2,5,5- tetramethyl -3-
Cyclopentene-1-one), mass-to-charge ratio 70.05,95.10 and 110.15；(5) appearance time 14.071 minutes, Benzene, 1,2,3-
Trimethyl-(1,2,3- trimethylbenzenes), mass-to-charge ratio 104.10 and 120.15；(6) appearance time 21.266 minutes,
Isophorone(isophorone), mass-to-charge ratio 54.05,82.10 and 138.15；(7) appearance time 22.239 minutes, 2,6,6-
Trimethyl-2-cyclohexene-1,4-dione(4- oxoisophorone), mass-to-charge ratio 68.00,96.05 and 152.10；
(8) appearance time 24.096 minutes, 1,3-Cyclohexadiene-1-carboxaldehyde, 2,6,6-trimethyl-
(safranal), mass-to-charge ratio 91.10,107.10,121.15 and 150.15；(9) appearance time 25.048 minutes, 4-
Methyleneisophorone4-(methylene isophorone), mass-to-charge ratio 91.05,107.10 and 150.15；(10) appearance time
27.662 minutes, Nonanoic acid(n-nonanoic acid), mass-to-charge ratio 60.00,73.05 and 115.10；(11) appearance time 30.408 divides
Clock, 2,4,7,9-Tetramethyl-5-decyn-4,7-diol(2,4,7,9- tetramethyl -5- decine -4,7- glycol), matter lotus
Than 109.10 and 151.15.The characteristic fingerprint pattern (see figure 2) of gas chromatography-mass spectrum as cape jasmine oil.
Step (3) identifies: take commercially available cape jasmine oil to obtain the gas chromatography-mass spectrum spectrogram of its volatile component by step (1),
Utilize the characteristic fingerprint pattern (figure of the gas chromatography-mass spectrum of similarity evaluation comparison cape jasmine oil
2) and the gas chromatography-mass spectrum spectrogram of the volatile component of commercially available cape jasmine oil, to the common trait peak of 11 cape jasmines and cape jasmine oil
Confirmed, being less than 0.1min, mass-to-charge ratio difference less than 0.05, relative peak area by retention time difference is effective greater than 0.5%
Peak is differentiated occur 9 and be confirmed as cape jasmine oil, and non-cape jasmine oil is confirmed as less than 9.
Fig. 3 is the feature of the gas chromatography-mass spectrum of commercially available cape jasmine oil volatile component gaschromatographic mass spectrometry figure and cape jasmine oil
The comparison diagram of finger-print shows 11 common trait peaks in commercially available cape jasmine oil volatile component gas chromatography-mass spectrum spectrogram
In can find out (see figure 3).
Embodiment 2
The identification of commercially available other plant oil, specifically comprises the following steps:
The gas chromatography-mass spectrometry analysis of step (1) cape jasmine and authentic cape jasmine oil volatile component.It is specific as follows: to take the cape jasmine of 1g
(pulverizer crushes after 70 DEG C of freeze-day with constant temperature) or the cape jasmine oil of 1mL are placed in 20mL headspace sampling bottle, are sealed rapidly, insertion 50/
Extracting fiber is extracted and is inserted rapidly after 60 DEG C of absorption volatile component 40min by 30 μm of DVB/CAR/PDMS extracting fibers
Enter gas chromatograph injection port and desorbs 5 min.It is right using under gas chromatograph-mass spectrometer (GC-MS) chromatography below and Mass Spectrometry Conditions
Volatile component carries out separation and qualitative analysis, retrieves to each peak in total ion current figure through mass spectrum computer data system and core
To NIST14 LIBRARY standard mass spectrogram, compound of the matching degree greater than 85% can be used as qualification result, obtain cape jasmine and orthodox school
The gas chromatography-mass spectrum spectrogram (see figure 1) of cape jasmine oil volatile component.
GC conditions: chromatographic column, DB-5MS(30m × 0.25mm × 0.25 μm) capillary column；Temperature programming: 40 DEG C
4 min are kept, 70 DEG C is warming up to the speed of 6 DEG C/min, keeps 8 min, 180 DEG C is warming up to the speed of 6 DEG C/min, protects
Hold 3min；250 DEG C of injector temperature；Carrier gas He, flow velocity 1mL/min；It does not shunt, solvent delay 4min.
Mass Spectrometry Conditions: EI ion source, electron energy 70eV, scanning range m/z50.00-500.00, ion source temperature 200
DEG C, 250 DEG C of interface temperature.
The foundation of the characteristic fingerprint pattern of step (2) cape jasmine oil volatile component gas chromatography-mass spectrum.According to step (1)
The gas chromatography-mass spectrometry analysis of cape jasmine and authentic cape jasmine oil volatile component is as a result, choose the common of 11 cape jasmines and cape jasmine oil
Characteristic peak: (1) appearance time 5.631 minutes, Hexanal(hexanal), mass-to-charge ratio 56.05 and 72.10；(2) appearance time
8.506 minutes, 1,3,5,7-Cyclooctatetraene(cyclo-octatetraene), mass-to-charge ratio 51.05,78.05 and 104.10；(3) go out
Peak time 12.290 minutes, Furan, 2-pentyl-(2- n-pentyl furans), mass-to-charge ratio 53.05,81.05 and 138.15；(4)
Appearance time 13.506 minutes, 2,2,5,5-Tetramethyl-3-cyclopenten-1-one(2,2,5,5- tetramethyl -3-
Cyclopentene-1-one), mass-to-charge ratio 70.05,95.10 and 110.15；(5) appearance time 14.071 minutes, Benzene, 1,2,3-
Trimethyl-(1,2,3- trimethylbenzenes), mass-to-charge ratio 104.10 and 120.15；(6) appearance time 21.266 minutes,
Isophorone(isophorone), mass-to-charge ratio 54.05,82.10 and 138.15；(7) appearance time 22.239 minutes, 2,6,6-
Trimethyl-2-cyclohexene-1,4-dione(4- oxoisophorone), mass-to-charge ratio 68.00,96.05 and 152.10；
(8) appearance time 24.096 minutes, 1,3-Cyclohexadiene-1-carboxaldehyde, 2,6,6-trimethyl-
(safranal), mass-to-charge ratio 91.10,107.10,121.15 and 150.15；(9) appearance time 25.048 minutes, 4-
Methyleneisophorone4-(methylene isophorone), mass-to-charge ratio 91.05,107.10 and 150.15；(10) appearance time
27.662 minutes, Nonanoic acid(n-nonanoic acid), mass-to-charge ratio 60.00,73.05 and 115.10；(11) appearance time 30.408 divides
Clock, 2,4,7,9-Tetramethyl-5-decyn-4,7-diol(2,4,7,9- tetramethyl -5- decine -4,7- glycol), matter lotus
Than 109.10 and 151.15.The characteristic fingerprint pattern (see figure 2) of gas chromatography-mass spectrum as cape jasmine oil.
Step (3) identifies: unknown edible vegetable oil being taken to obtain the gas chromatography-mass spectrum of its volatile component by step (1)
Spectrogram utilizes the characteristic fingerprint figure of the gas chromatography-mass spectrum of similarity evaluation comparison cape jasmine oil
The gas chromatography-mass spectrum spectrogram for composing the volatile component of (Fig. 2) and unknown edible vegetable oil, is total to 11 cape jasmines and cape jasmine oil
Confirmed with characteristic peak, is less than 0.1min, mass-to-charge ratio difference by retention time difference and is greater than less than 0.05, relative peak area
0.5% is differentiated for effective peak, and 11 common trait peaks occur 9 and are confirmed as cape jasmine oil, and non-cape jasmine oil is confirmed as less than 9.
Fig. 4 is the volatile component gaschromatographic mass spectrometry figure of commercially available corn oil, rapeseed oil, peanut oil, camellia oil, soybean oil
With the comparison diagram of the characteristic fingerprint pattern of the gas chromatography-mass spectrum of cape jasmine oil, show 11 common trait peaks in each product oil
Occurring number in volatile component gaschromatographic mass spectrometry figure is respectively corn oil 3, rapeseed oil 3,4 oil of peanut, camellia oil 3
It is a, soybean oil 3.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, is all covered by the present invention.
Claims (4)
1. a kind of method for identifying cape jasmine oil based on characteristic component gas chromatography-mass spectrum finger-print, which is characterized in that from cape jasmine
The volatile component of oil is set about, and is combined art, analysis detection cape jasmine using headspace solid-phase microextraction, in conjunction with gas chromatography-mass spectrum skill
And the volatile feature components of cape jasmine oil, establish the gas chromatography-mass spectrum characteristic fingerprint of the volatile component of cape jasmine and cape jasmine oil
Map is compared by effective peak of the evaluation software to characteristic fingerprint pattern, to realize the identification to cape jasmine oil.
2. a kind of side for identifying cape jasmine oil based on characteristic component gas chromatography-mass spectrum finger-print according to claim 1
Method, which comprises the steps of:
The gas chromatography-mass spectrometry analysis of step (1) cape jasmine and authentic cape jasmine oil volatile component: by cape jasmine through 70 DEG C of freeze-day with constant temperature
Pulverizer crushes afterwards, and the cape jasmine oil of the gardenia powder or 1mL that take 1g is placed in 20mL headspace sampling bottle, seals rapidly, insertion 50/30
Extracting fiber is extracted and is rapidly inserted into after 60 DEG C of absorption volatile component 40min by μm DVB/CAR/PDMS extracting fiber
Gas chromatograph injection port desorbs 5 min, using gas chromatograph-mass spectrometer (GC-MS), carries out separation and qualitative to volatile component
Analysis, retrieves and checks NIST14 LIBRARY standard mass spectrum through mass spectrum computer data system to each peak in total ion current figure
Figure, compound of the matching degree greater than 85% obtain the gas phase color of cape jasmine and authentic cape jasmine oil volatile component as qualification result
Spectrum-mass spectrogram；
The foundation of the characteristic fingerprint pattern of step (2) cape jasmine oil volatile component gas chromatography-mass spectrum: according to step (1) cape jasmine
Gas chromatography-mass spectrometry analysis with authentic cape jasmine oil volatile component is as a result, choose the common trait of 11 cape jasmines and cape jasmine oil
Peak: (1) appearance time 5.631 minutes, hexanal, mass-to-charge ratio 56.05 and 72.10；(2) appearance time 8.506 minutes, ring pungent four
Alkene, mass-to-charge ratio 51.05,78.05 and 104.10；(3) appearance time 12.290 minutes, 2- n-pentyl furans, mass-to-charge ratio 53.05,
81.05 with 138.15；(4) appearance time 13.506 minutes, 2,2,5,5- tetramethyl -3- cyclopentene-1-ones, mass-to-charge ratio 70.05,
95.10 with 110.15；(5) appearance time 14.071 minutes, 1,2,3- trimethylbenzene, mass-to-charge ratio 104.10 and 120.15；(6) go out
Peak time 21.266 minutes, isophorone, mass-to-charge ratio 54.05,82.10 and 138.15；(7) appearance time 22.239 minutes, 4-
Oxoisophorone, mass-to-charge ratio 68.00,96.05 and 152.10；(8) appearance time 24.096 minutes, safranal, mass-to-charge ratio
91.10,107.10,121.15 and 150.15；(9) appearance time 25.048 minutes, 4-(methylene isophorone), mass-to-charge ratio
91.05,107.10 and 150.15；(10) appearance time 27.662 minutes, n-nonanoic acid, mass-to-charge ratio 60.00,73.05 and 115.10；
(11) appearance time 30.408 minutes, 2,4,7,9- tetramethyl -5- decine -4,7- glycol, mass-to-charge ratio 109.10 and 151.15；Make
For the characteristic fingerprint pattern of the gas chromatography-mass spectrum of cape jasmine oil；
The identification of step (3) cape jasmine oil: commercially available cape jasmine oil or unknown edible vegetable oil is taken to obtain its volatile component by step (1)
Gas chromatography-mass spectrum spectrogram, utilize similarity evaluation comparison cape jasmine oil gas-chromatography-matter
The gas chromatography-mass spectrum spectrogram of the volatile component of the characteristic fingerprint pattern of spectrum and commercially available cape jasmine oil or unknown edible vegetable oil,
The common trait peak of 11 cape jasmines and cape jasmine oil is confirmed, it is small to be less than 0.1min, mass-to-charge ratio difference by retention time difference
It is greater than 0.5% in 0.05, relative peak area to be differentiated for effective peak, 11 common trait peaks occur 9 and are confirmed as cape jasmine oil,
Non- cape jasmine oil is confirmed as less than 9.
3. a kind of side for identifying cape jasmine oil based on characteristic component gas chromatography-mass spectrum finger-print according to claim 2
Method, which is characterized in that in step (1), GC conditions: chromatographic column, DB-5MS capillary column 30m × 0.25mm × 0.25 μ
m；Temperature programming: 40 DEG C of 4 min of holding are warming up to 70 DEG C with the speed of 6 DEG C/min, 8 min are kept, with the speed of 6 DEG C/min
Degree is warming up to 180 DEG C, keeps 3min；250 DEG C of injector temperature；Carrier gas He, flow velocity 1mL/min；It does not shunt, solvent delay
4min。
4. a kind of side for identifying cape jasmine oil based on characteristic component gas chromatography-mass spectrum finger-print according to claim 2
Method, which is characterized in that in step (1), Mass Spectrometry Conditions: EI ion source, electron energy 70eV, scanning range m/z50.00-
500.00,200 DEG C of ion source temperature, 250 DEG C of interface temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811336908.4A CN109212102B (en) | 2018-11-12 | 2018-11-12 | Method for identifying gardenia oil based on characteristic component gas chromatography-mass spectrum fingerprint |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811336908.4A CN109212102B (en) | 2018-11-12 | 2018-11-12 | Method for identifying gardenia oil based on characteristic component gas chromatography-mass spectrum fingerprint |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109212102A true CN109212102A (en) | 2019-01-15 |
| CN109212102B CN109212102B (en) | 2021-07-30 |
Family
ID=64995147
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811336908.4A Active CN109212102B (en) | 2018-11-12 | 2018-11-12 | Method for identifying gardenia oil based on characteristic component gas chromatography-mass spectrum fingerprint |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109212102B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110243960A (en) * | 2019-06-11 | 2019-09-17 | 华中农业大学 | The separation of Carnation flowers external source volatilization fragrance component and identification method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102091283A (en) * | 2009-12-11 | 2011-06-15 | 无锡济民可信山禾药业股份有限公司 | Method for detecting Xingnaojing injection |
-
2018
- 2018-11-12 CN CN201811336908.4A patent/CN109212102B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102091283A (en) * | 2009-12-11 | 2011-06-15 | 无锡济民可信山禾药业股份有限公司 | Method for detecting Xingnaojing injection |
Non-Patent Citations (3)
| Title |
|---|
| 于生兰 主编: "《中药鉴定技术》", 30 September 2007 * |
| 刘百战 等: "固相微萃取-气相色谱/质谱分析栀子花的头香成分", 《色谱》 * |
| 李雨田 等: "GC-MS分析栀子姜制前后挥发油的化学组成成分变化", 《中国中药杂志》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110243960A (en) * | 2019-06-11 | 2019-09-17 | 华中农业大学 | The separation of Carnation flowers external source volatilization fragrance component and identification method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109212102B (en) | 2021-07-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Choi et al. | Determination of coffee origins by integrated metabolomic approach of combining multiple analytical data | |
| Carvalho et al. | Non-targeted and targeted analysis of wild toxic and edible mushrooms using gas chromatography–ion trap mass spectrometry | |
| CN101808531B (en) | Tagging method | |
| Guo et al. | Characterization and authentication of significant Chinese edible oilseed oils by stable carbon isotope analysis | |
| CN103105440A (en) | Method for identifying volatile flavor substance in bolete | |
| CN107085051B (en) | A kind of construction method and discrimination method of Huanghua Pear redwood tree species finger-print | |
| CN105806974B (en) | Rubus biflorus fruit aroma component detection method | |
| CN108693290B (en) | Method for analyzing volatile components of coffee beans by using automatic solid-phase microextraction technology | |
| CN103823033B (en) | A kind of analyzing detecting method of white wine flavor compound | |
| CN106353419A (en) | Method for measuring aroma components in main stream smoke of cigarettes | |
| CN109541073A (en) | A kind of francolin congo red, the GC-MS analysis method of green fresh leaf volatile component | |
| Cui et al. | Simultaneous determination and difference evaluation of volatile components generated from ginseng fruit by HS-SPME Coupled with GC-MS according to fruit color | |
| Tian et al. | Development of a fatty acid fingerprint of white apricot almond oil by gas chromatography and gas chromatography–mass spectrometry | |
| CN106053645A (en) | Method for identifying authenticity of agilawood | |
| CN101487826A (en) | Method for recognizing odor type and/or grade of Chinese spirit | |
| CN108845041A (en) | A kind of detection method measuring redwood volatilization and half volatile chemical component | |
| CN109212102A (en) | A method of cape jasmine oil is identified based on characteristic component gas chromatography-mass spectrum finger-print | |
| CN102279230A (en) | Method for establishing volatile ingredient fingerprint map of agricultural product and processed product of agricultural product | |
| CN102095820A (en) | Method for detecting fruity substance in fruit flavoring agent | |
| CN105954449B (en) | A kind of method for quick of tobacco leaf volatile ingredient | |
| CN108195985A (en) | It is a kind of that pseudo- method is mixed based on volatile ingredient combination PCA and CSA Model checking hops | |
| Xin-Hua et al. | Essential oils composition from roots of Santalum album L. | |
| CN106568882B (en) | A method of analysis shampoo fragrance component | |
| Roskiana Ahmad | Standardization And Characterization Of Essential Oil Of Patchouli Stem (Pogostemon Cablin Benth.) By Chromatography-Mass Spectrometry (GC-MS) Method | |
| CN114062568A (en) | Method for identifying variety of cherry by GC-IMS technology |
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 | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |