CN107677754A - A kind of medicinal extract class tobacco aromaticss analysis of aroma components pre-treating method - Google Patents
A kind of medicinal extract class tobacco aromaticss analysis of aroma components pre-treating method Download PDFInfo
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- CN107677754A CN107677754A CN201710371055.7A CN201710371055A CN107677754A CN 107677754 A CN107677754 A CN 107677754A CN 201710371055 A CN201710371055 A CN 201710371055A CN 107677754 A CN107677754 A CN 107677754A
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- 239000000284 extract Substances 0.000 title claims abstract description 41
- 238000004458 analytical method Methods 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 27
- 241000208125 Nicotiana Species 0.000 title claims abstract description 19
- 235000002637 Nicotiana tabacum Nutrition 0.000 title claims abstract description 19
- 238000000605 extraction Methods 0.000 claims abstract description 11
- 238000002470 solid-phase micro-extraction Methods 0.000 claims abstract description 10
- 239000002798 polar solvent Substances 0.000 claims abstract description 7
- 230000032683 aging Effects 0.000 claims abstract description 5
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 5
- 239000008236 heating water Substances 0.000 claims abstract description 5
- 229920005573 silicon-containing polymer Polymers 0.000 claims abstract description 5
- 238000002347 injection Methods 0.000 claims abstract description 4
- 239000007924 injection Substances 0.000 claims abstract description 4
- 239000000835 fiber Substances 0.000 claims abstract description 3
- 235000019504 cigarettes Nutrition 0.000 claims description 16
- 239000007789 gas Substances 0.000 claims description 16
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 12
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 8
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 5
- 239000012071 phase Substances 0.000 claims description 5
- 238000001819 mass spectrum Methods 0.000 claims description 4
- 238000004451 qualitative analysis Methods 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 230000005540 biological transmission Effects 0.000 claims description 3
- 239000012159 carrier gas Substances 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 3
- 239000005350 fused silica glass Substances 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
- 238000004949 mass spectrometry Methods 0.000 claims description 3
- 239000000839 emulsion Substances 0.000 claims description 2
- 239000003208 petroleum Substances 0.000 claims description 2
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 abstract description 26
- 231100000693 bioaccumulation Toxicity 0.000 abstract description 5
- 150000001875 compounds Chemical class 0.000 abstract description 3
- 238000001514 detection method Methods 0.000 abstract description 3
- 238000010790 dilution Methods 0.000 abstract description 3
- 239000012895 dilution Substances 0.000 abstract description 3
- 238000012545 processing Methods 0.000 abstract description 2
- 230000035945 sensitivity Effects 0.000 abstract description 2
- 238000002604 ultrasonography Methods 0.000 abstract description 2
- 238000003672 processing method Methods 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 17
- 241000208140 Acer Species 0.000 description 9
- 235000019082 Osmanthus Nutrition 0.000 description 9
- 241000333181 Osmanthus Species 0.000 description 9
- 239000000470 constituent Substances 0.000 description 8
- 239000000203 mixture Substances 0.000 description 6
- 235000013599 spices Nutrition 0.000 description 6
- 238000002203 pretreatment Methods 0.000 description 5
- 238000000638 solvent extraction Methods 0.000 description 5
- 239000003205 fragrance Substances 0.000 description 4
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 238000000622 liquid--liquid extraction Methods 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000009835 boiling Methods 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 244000242564 Osmanthus fragrans Species 0.000 description 1
- 235000019083 Osmanthus fragrans Nutrition 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004853 microextraction Methods 0.000 description 1
- 239000012982 microporous membrane Substances 0.000 description 1
- 210000004400 mucous membrane Anatomy 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000002304 perfume Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 230000000391 smoking effect Effects 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000001256 steam distillation Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- 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
- G01N30/08—Preparation using an enricher
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
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- 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)
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Abstract
The present invention provides a kind of medicinal extract class tobacco aromaticss analysis of aroma components pre-treating method.The processing method concretely comprises the following steps:Medicinal extract class tobacco aromaticss sample is taken to extrude into container using syringe, and weak polar solvent ultrasound dilution is added into container, then manual solid-phase micro-extraction device is taken, using 100m dimethyl silicone polymer fibre abstraction heads and aging is carried out to it, the medicinal extract sample after dilution is placed in heating water bath in ml headspace bottle again, then 1 10min is extracted manually using manual solid-phase micro-extraction device, extracting head is finally inserted into gas chromatography-mass spectrometry injection port and desorbs 5 10min, the component being adsorbed onto using gas chromatography-mass spectrometry analytical extraction head.The present invention has the advantages that hypotoxicity, easy to operate, cost is low, bioaccumulation efficiency is high, more volatile and semi-volatile compounds that content is low, detection sensitivity is low in medicinal extract class tobacco aromaticss can be effectively enriched with, more chromatographic peaks are can obtain with GC/MS after processing, identify more multicomponent.
Description
Technical field
The invention belongs to tobacco aromaticss analysis field, and in particular to locate before a kind of medicinal extract class tobacco aromaticss analysis of aroma components
Reason method.
Background technology
Extract type spice is usually to extract natural plants, filtered, the sticky or paste that is concentrated to give with low polar solvent
Spices, conventional tobacco extract has maple extract, Peru's medicinal extract, osmanthus concrete, smoked plum medicinal extract etc., added in cigarette, with cigarette
Fragrant harmony, it can improve and smell fragrant, improvement cigarette quality, relax mucous membrane of mouth and experience characteristic, suppress to stimulate pungent and make smoke soft
Moisten and strong.
Analysis for volatile and semi-volatile compounds in tobacco aromaticss, the method for commonly using gas chromatography mass spectrometry (GC-MS).Gas
Matter combination (GC-MS) is a kind of method that can while be qualitatively and quantitatively analyzed complex component, but needs to enter sample
Row pre-treatment.Conventional pre-treating method has steam distillation, solvent extraction, Simultaneous distillation-extraction, Static Headspace, the micro- extraction of solid phase
Take, these methods respectively there are advantage and disadvantage.
The method for most commonly using liquid-liquid extraction, with dichloromethane, ethanol or ethyl acetate equal solvent to spices sample
Product are extracted, and organic phase clarified solution is taken after layering, through the laggard Instrumental Analysis of filtering with microporous membrane.Simultaneous distillation-extraction is to volatilization
Property, the bioaccumulation efficiency of half volatile composition are very high, and especially clean-up effect is good, and the sample such as extract, medicinal extract can use
The method carries out pre-treatment.Principle of the SPE based on liquid chromatogram, sample solution retain wherein measured object by adsorbent
Matter, then impurity is washed away from appropriate strength solvents, measured matter is then eluted rapidly with a small amount of solvent, so as to reach quick separating
The purpose of purification and concentration.SPME is on the basis of SPE, remains the advantages of its is all, and having abandoned it needs
Want column packing and the disadvantage desorbed using solvent;Integrate sampling, extraction, concentration, sample introduction, can be with various analysis sides
Method combines, and greatly accelerates the speed of analysis detection.
Volatilized although these pretreatment modes can handle medicinal extract class tobacco aromaticss to analyze volatility therein and half
Property composition, but still some obvious shortcoming and defect be present, for example separating step is more, analytical cycle is long, time and effort consuming, reproduction
Property it is bad, treatment effeciency is low etc., as the cleaning and extraction of SDE method are all time-consuming longer, from operation is started to completion
Analysis sample generally requires more than 5 hours, therefore is not suitable for the analysis work of a large amount of samples.Meanwhile medicinal extract class tobacco aromaticss
Most all more sticky, poor fluidity, the problems such as there is being not easy to sample, easily emulsifying, it is low in turn result in solvent extraction efficiency, obtains
The effective chromatographic peak arrived is seldom, it is impossible to reflects the interior quality of the spices completely.
The content of the invention
For difficult existing for prior art, the present invention provides a kind of medicinal extract class cigarette easy, easy to operate, bioaccumulation efficiency is high
With spices analysis of aroma components pre-treating method, this method is using solubilizer ultrasound dilution, then with the method for SPME
Directly extract, carry out chromatography manually, the fragrance component that effectively can be enriched with and extract in medicinal extract class tobacco aromaticss, obtain more
More effective chromatographic peaks.
Technical scheme provided by the invention is:A kind of medicinal extract class tobacco aromaticss analysis of aroma components pre-treating method,
It is characterized in that comprise the following steps that:
(1) medicinal extract class tobacco aromaticss sample is taken to extrude into container using syringe, and addition low pole is molten into container
Agent, the ultrasonic 15-30min under conditions of frequency is 150Hz~250Hz, the sample being diluted;Wherein described medicinal extract class cigarette
It is 1 with the mass ratio of fragrance sample and weak polar solvent:2~1:10, the weak polar solvent is ethylene glycol, ethyl acetate, just
One or both of hexane, ether, petroleum ether (30-60 DEG C);
(2) manual solid-phase micro-extraction device is taken, using 100m dimethyl silicone polymer fibre abstraction heads, at 200~280 DEG C
Under conditions of 20~40min of aging;
(3) sample being diluted obtained in step 1 is placed in ml headspace bottle, and the heating water bath under the conditions of 50-80 DEG C,
Then use the manual solid-phase micro-extraction device in step (2) to extract 1-10min manually, and by extracting head insert gas-chromatography-
GC-MS injection port desorbs 5-10min;
(4) component being finally adsorbed onto using gas chromatograph-mass spectrometer (GC-MS) analytical extraction head, with NIST2005 and
Wiley7 spectrums storehouse is retrieved and qualitative analysis.
The further technical scheme of the present invention:The condition of work that gas chromatograph-mass spectrometer (GC-MS) is analyzed in the step (4)
It is as follows:
Gas phase condition:Chromatographic column selects HP-5MS fused-silica capillary columns (30m × 0.25mm i.d. × 0.25 μm
D.f.), 250 DEG C of injector temperature, 50 DEG C of initial temperature, 2min is kept, is raised to 240 DEG C with 4 DEG C/min speed, keeps 2min,
280 DEG C are raised to 15 DEG C/min speed again, keeps 20min;Carrier gas:Helium, flow velocity 1.0ml/min, split ratio 50:1;
Mass Spectrometry Conditions:250 DEG C of transmission line temperature, ionize mode EI, 230 DEG C, ionizing energy 70eV of ion source temperature, mass spectrum
Scan mode is full scan (scan), 30~450amu of scanning range, solvent delay 3min.
The present invention preferably technical scheme:In step (3) in extraction process, if there is emulsion, then from
Centrifugation 3-5min carries out centrifugation layering to it under conditions of heart speed is 3000r/min.
The present invention has the advantages that hypotoxicity, easy to operate, cost is low, bioaccumulation efficiency is high, can effectively be enriched with medicinal extract class cigarette
With more volatile and semi-volatile compounds that content is low, detection sensitivity is low in spices, can obtain more with GC/MS after processing
Chromatographic peak, identify more multicomponent;Sample-pretreating method that the present invention uses is easy to operate, bioaccumulation efficiency is high, can be obvious
Test efficiency is improved, suitable for the pre-treatment of medicinal extract class tobacco aromaticss.
Brief description of the drawings
Fig. 1 is the GC/MS constituent analysis chromatograms of traditional liquid-liquid extraction osmanthus concrete;
Fig. 2 is the GC/MS constituent analysis chromatograms of the osmanthus concrete after pre-treatment of the present invention in embodiment one;
Fig. 3 is the GC/MS constituent analysis chromatograms of traditional liquid-liquid extraction maple extract;
Fig. 4 is the GC/MS constituent analysis chromatograms of the maple extract after pre-treatment of the present invention in embodiment two.
Embodiment
With reference to embodiment, the invention will be further described, but does not limit protection scope of the present invention.
A kind of embodiment one, cigarette osmanthus concrete fragrance phase composition analysis pre-treating method, is comprised the following steps that:Take one
5mL syringes, pull out piston core pin, and osmanthus concrete sample is loaded in syringe, piston core pin is reloaded into, is expressed to and is placed in electronics
In triangular flask on balance, 0.5506g is weighed, adds 3mL ether, ultrasonic 15min, is diluted under the conditions of 150Hz
Sample;Take manual SPME devices, 100 μm of dimethyl silicone polymer extracting heads, under conditions of 200~280 DEG C aging 20~
40min;The osmanthus concrete sample being diluted is placed in ml headspace bottle, 60 DEG C of heating water baths, extracts 5min, then insert extracting head
Enter gas chromatograph injection port desorption 8min;The component being adsorbed onto using gas chromatograph-mass spectrometer (GC-MS) analytical extraction head, use
NIST2005 and Wiley7 spectrums storehouse is retrieved and qualitative analysis, and it is as shown in Figure 2 to obtain GC/MS constituent analysis chromatograms.
Embodiment two:A kind of cigarette maple extract fragrance phase composition analysis pre-treating method, is comprised the following steps that:Take one
5mL syringes, pull out piston core pin, and maple extract sample is loaded in syringe, piston core pin is reloaded into, is expressed to and is placed in electronics
In triangular flask on balance, 0.6022g is weighed, 5mL ethyl acetate is added, the ultrasonic 20min under the conditions of 150Hz, obtains dilute
The sample released;Manual SPME devices are taken, 100 μm of dimethyl silicone polymers extract extracting head, by requirement aging;It will be diluted
Maple extract sample be placed in ml headspace bottle, 65 DEG C of heating water baths, extract 8min, then by extracting head insertion gas chromatograph enter
Sample mouth desorbs 10min;The component being adsorbed onto using gas chromatograph-mass spectrometer (GC-MS) analytical extraction head, with NIST2005 and
Wiley7 spectrums storehouse is retrieved and qualitative analysis, obtained GC/MS constituent analysis chromatograms are as shown in Figure 4.
The condition of work of gas chromatograph-mass spectrometer (GC-MS) analysis in embodiment one and embodiment two is as follows:
Gas phase condition:Chromatographic column selects HP-5MS fused-silica capillary columns (30m × 0.25mm i.d. × 0.25 μm
D.f.), 250 DEG C of injector temperature, 50 DEG C of initial temperature, 2min is kept, is raised to 240 DEG C with 4 DEG C/min speed, keeps 2min,
280 DEG C are raised to 15 DEG C/min speed again, keeps 20min;Carrier gas:Helium, flow velocity 1.0ml/min, split ratio 50:1;
Mass Spectrometry Conditions:250 DEG C of transmission line temperature, ionize mode EI, 230 DEG C, ionizing energy 70eV of ion source temperature, mass spectrum
Scan mode is full scan (scan), 30~450amu of scanning range, solvent delay 3min.
Contrast test 1:Cigarette untreated in embodiment one is directly used into gas chromatography-mass spectrometry with osmanthus concrete
Analyzed with instrument, the condition of work of its gas chromatograph-mass spectrometer (GC-MS) is identical with the condition of work of embodiment one, and it is analyzed
It is as shown in Figure 1 to GC/MS constituent analysis chromatograms;And divided with the cigarette after being handled in embodiment one with osmanthus concrete GC/MS compositions
Analysis chromatogram is contrasted, it can be seen that although the total peak number difference of chromatogram that two methods obtain is little, each chromatographic peak in Fig. 2
Between ratio be substantially better than Fig. 1, and the appearance number in different temperatures section is different, especially high-boiling fration, in Fig. 1
Chromatogram peak number is 12 between 200 DEG C -250 DEG C, is 9 in Fig. 2, and content difference is also bigger, and this moieties soaks to sweet osmanthus
Cream improves aroma quality in cigarette and is made that contribution in terms of improving pleasant impression, therefore these comparison of ingredients are important, also illustrate that and adopt
The active ingredient of osmanthus concrete can more completely be reflected relatively with the inventive method.
Contrast test 2:Cigarette untreated in embodiment two is directly used into gas chromatography-mass spectrometry with maple extract
Analyzed with instrument, the condition of work of its gas chromatograph-mass spectrometer (GC-MS) is identical with the condition of work of embodiment two, and it is analyzed
It is as shown in Figure 3 to GC/MS constituent analysis chromatograms;And divided with the cigarette after being handled in embodiment two with maple extract GC/MS compositions
Analysis chromatogram is contrasted, and the chromatographic peak quantity obtained using two methods that can visually see is significantly different, and especially 150
Chromatogram peak number differs greatly in DEG C -200 DEG C of temperature ranges, and this moieties belongs to medium boiling portion, relevant with note, can
Reflecting maple extract has the function that abundant cigarette perfume in cigarette, improves aroma quality, consistent with smoking result, illustrates using this
The analysis pre-treating method of invention is better than traditional pre-treating method.
Claims (3)
1. a kind of medicinal extract class tobacco aromaticss analysis of aroma components pre-treating method, it is characterised in that comprise the following steps that:
(1) take medicinal extract class tobacco aromaticss sample to extrude into container using syringe, and weak polar solvent is added into container,
Frequency is ultrasonic 15-30min under conditions of 150Hz~250Hz, the sample being diluted;Wherein described medicinal extract class cigarette is fragrant
The mass ratio for expecting sample and weak polar solvent is 1:2~1:10, the weak polar solvent be ethylene glycol, ethyl acetate, n-hexane,
One or both of ether, petroleum ether (30-60 DEG C);
(2) manual solid-phase micro-extraction device is taken, using 100m dimethyl silicone polymer fibre abstraction heads, in 200~280 DEG C of bar
20~40min of aging under part;
(3) sample being diluted obtained in step 1 is placed in ml headspace bottle, and the heating water bath under the conditions of 50-80 DEG C, then
1-10min is extracted manually using the manual solid-phase micro-extraction device in step (2), and extracting head is inserted into gas chromatography-mass spectrum
Combined instrument injection port desorbs 5-10min;
(4) component being finally adsorbed onto using gas chromatograph-mass spectrometer (GC-MS) analytical extraction head, composed with NIST2005 and Wiley7
Storehouse is retrieved and qualitative analysis.
A kind of 2. medicinal extract class tobacco aromaticss analysis of aroma components pre-treating method according to claim 1, it is characterised in that
The condition of work that gas chromatograph-mass spectrometer (GC-MS) is analyzed in the step (4) is as follows:
Gas phase condition:Chromatographic column selects HP-5MS fused-silica capillary columns (30m × 0.25mm i.d. × 0.25 μm d.f.),
250 DEG C of injector temperature, 50 DEG C of initial temperature, 2min is kept, be raised to 240 DEG C with 4 DEG C/min speed, keep 2min, then with 15
DEG C/min speed is raised to 280 DEG C, keep 20min;Carrier gas:Helium, flow velocity 1.0ml/min, split ratio 50:1;
Mass Spectrometry Conditions:250 DEG C of transmission line temperature, ionize mode EI, 230 DEG C, ionizing energy 70eV of ion source temperature, scanning of the mass spectrum
Mode is full scan (scan), 30~450amu of scanning range, solvent delay 3min.
3. according to claim a kind of medicinal extract class tobacco aromaticss analysis of aroma components pre-treating method, it is characterised in that:
In the extraction process of step (3), if there is emulsion, then 3- is centrifuged under conditions of centrifugal speed is 3000r/min
5min carries out centrifugation layering to it.
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