CN106442845B - A kind of method of thin-layer chromatography coupling gas chromatography combined with mass spectrometry technical Analysis tobacco pollutant - Google Patents
A kind of method of thin-layer chromatography coupling gas chromatography combined with mass spectrometry technical Analysis tobacco pollutant Download PDFInfo
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- CN106442845B CN106442845B CN201610813611.7A CN201610813611A CN106442845B CN 106442845 B CN106442845 B CN 106442845B CN 201610813611 A CN201610813611 A CN 201610813611A CN 106442845 B CN106442845 B CN 106442845B
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- 238000004809 thin layer chromatography Methods 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 32
- 239000003344 environmental pollutant Substances 0.000 title claims abstract description 29
- 231100000719 pollutant Toxicity 0.000 title claims abstract description 29
- 241000208125 Nicotiana Species 0.000 title claims abstract description 23
- 235000002637 Nicotiana tabacum Nutrition 0.000 title claims abstract description 23
- 238000004458 analytical method Methods 0.000 title claims abstract description 21
- 238000004817 gas chromatography Methods 0.000 title claims abstract description 19
- 238000004949 mass spectrometry Methods 0.000 title claims abstract description 18
- 230000008878 coupling Effects 0.000 title claims abstract description 11
- 238000010168 coupling process Methods 0.000 title claims abstract description 11
- 238000005859 coupling reaction Methods 0.000 title claims abstract description 11
- 239000002904 solvent Substances 0.000 claims abstract description 29
- 238000004090 dissolution Methods 0.000 claims abstract description 20
- 239000006228 supernatant Substances 0.000 claims abstract description 19
- 235000019504 cigarettes Nutrition 0.000 claims abstract description 16
- 239000012530 fluid Substances 0.000 claims abstract description 13
- 238000010828 elution Methods 0.000 claims abstract description 7
- 230000003595 spectral effect Effects 0.000 claims abstract description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 38
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 17
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 230000005540 biological transmission Effects 0.000 claims description 6
- 239000012159 carrier gas Substances 0.000 claims description 6
- 230000014759 maintenance of location Effects 0.000 claims description 6
- 238000005070 sampling Methods 0.000 claims description 6
- 230000004913 activation Effects 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 5
- 238000000605 extraction Methods 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 238000001228 spectrum Methods 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 8
- 238000012216 screening Methods 0.000 abstract description 5
- 238000009833 condensation Methods 0.000 abstract description 3
- 230000005494 condensation Effects 0.000 abstract description 3
- 230000007062 hydrolysis Effects 0.000 abstract description 3
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 3
- 230000008901 benefit Effects 0.000 abstract description 2
- 239000000523 sample Substances 0.000 description 43
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 238000001035 drying Methods 0.000 description 8
- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 8
- RSJKGSCJYJTIGS-UHFFFAOYSA-N undecane Chemical compound CCCCCCCCCCC RSJKGSCJYJTIGS-UHFFFAOYSA-N 0.000 description 8
- 239000007789 gas Substances 0.000 description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 238000001914 filtration Methods 0.000 description 5
- 238000001819 mass spectrum Methods 0.000 description 5
- 238000000079 presaturation Methods 0.000 description 5
- 125000004200 2-methoxyethyl group Chemical group [H]C([H])([H])OC([H])([H])C([H])([H])* 0.000 description 4
- 150000002148 esters Chemical class 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 230000001737 promoting effect Effects 0.000 description 4
- 239000001384 succinic acid Substances 0.000 description 4
- 230000001174 ascending effect Effects 0.000 description 3
- 238000004587 chromatography analysis Methods 0.000 description 3
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 description 3
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 2
- 239000012046 mixed solvent Substances 0.000 description 2
- 239000012488 sample solution Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 238000013480 data collection Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002304 perfume Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012106 screening analysis Methods 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 235000019505 tobacco product Nutrition 0.000 description 1
- 125000003944 tolyl group Chemical group 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
- G01N30/90—Plate chromatography, e.g. thin layer or paper 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
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- 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)
- Sampling And Sample Adjustment (AREA)
Abstract
The present invention relates to a kind of method of thin-layer chromatography coupling gas chromatography combined with mass spectrometry technical Analysis tobacco pollutant, belong to the detection field of tobacco.This method comprises the following steps：1) extractant is added into offal sample to be extracted, filter, obtain supernatant；2) take supernatant to carry out thin-layer chromatography, component spot disconnected from each other is obtained on lamellae；3) remove component spot and add solvent and carry out elution dissolution, obtain dissolution fluid；4) sample spectrogram is obtained；By sample spectrogram compared with the spectrogram of standard cigarette sample, difference chromatographic peak is determined；Spectral peak information according to difference chromatographic peak determines pollutant.This method comprehensively utilizes thin-layer chromatography and gas phase hydrolysis and condensation is analyzed offal sample, by the way that compared with the spectral peak of standard cigarette sample, qualitatively screening goes out pollutant, has the advantages of strong applicability, simple to operate, detection time is short.
Description
Technical field
The invention belongs to tobacco and the Screening analysis technical field of the pollution compound of tobacco product, and in particular to a kind of thin
The method that layer chromatography couples gas chromatography combined with mass spectrometry technical Analysis tobacco pollutant.
Background technology
Tobacco leaf can be polluted during production, transport and storage by allogenic material, so as to influence the perfume (or spice) of tobacco leaf
Gas and jealous.But the tobacco leaf being contaminated is by which kind of Substances Pollution, and the problems such as pollution sources are come wherefrom, in reality actually
Relatively it is difficult to resolve certainly in the work of border.
The content of the invention
It is an object of the invention to provide a kind of thin-layer chromatography to couple gas chromatography combined with mass spectrometry technical Analysis tobacco pollutant
Method, it has the characteristics of process is simple, detection time is short, can effectively improve the screening efficiency of tobacco pollutant.
In order to realize the above object the technical solution adopted in the present invention is：
A kind of method of thin-layer chromatography coupling gas chromatography combined with mass spectrometry technical Analysis tobacco pollutant, including following step
Suddenly：
1) extractant is added into offal sample to be extracted, filter, obtain supernatant；
2) take supernatant to carry out thin-layer chromatography, component spot disconnected from each other is obtained on lamellae；
3) remove component spot and add solvent and carry out elution dissolution, obtain dissolution fluid；
4) dissolution fluid is subjected to gas chromatography combined with mass spectrometry analysis, obtains sample spectrogram；By sample spectrogram and standard cigarette sample
Spectrogram be compared, determine difference chromatographic peak；Spectral peak information according to difference chromatographic peak determines pollutant.
Thin-layer chromatography (TLC) is called thin plate chromatography, its be adsorbent, carrier or other active materials are uniformly coated on it is flat
On panel, after forming thin layer, the analysis method of chromatography is carried out on this thin layer.The main operational steps bag of thin-layer chromatography
Include：The preparation of lamellae, the dropwise addition of sample, expansion, develop the color, compare Rf values and quantitative analysis etc..Due to each component in sample
Property is different, after mobile deploy, the component spot that must can be separated from each other.
Gas chromatograph is attached by gas chromatography combined with mass spectrometry technology with mass spectrograph by interface module, with gas phase
The means that chromatogram is separated as sample, prepared, qualitative, quantitative point is carried out using mass spectrum as the on-line checking means of gas-chromatography
Analysis, is aided with corresponding Data Collection and a kind of built-up chromatograph-mass spectrometer coupling technology of control system.
The present invention is to utilize to combine thin-layer chromatography and gas phase hydrolysis and condensation, establishes tobacco leaf exogenous material
Screening method, a kind of new way is provided to find out the pollution sources of tobacco leaf.This method is using each component in cigarette sample in a certain material
In absorption or solubility property it is different, or the difference with other material affinity interaction performances realizes different solute quick separatings；Again
The research of trace sample is carried out using gas chromatography-mass spectrometry；The combination of thin-layer chromatography and gas phase hydrolysis and condensation
Examination for pollutant in cigarette sample has extremely strong applicability, can preferably promote Fourier transform infrared analyzer-gas
Application of the phase chromatograph-mass spectrometer technology in pollution thing examination field.This method makes full use of the advantage of two kinds of technologies,
With the characteristics of simple to operate, detection time is short, the screening efficiency of tobacco pollutant can be effectively improved.
In step 1), the extractant is any one or more in hexamethylene, toluene, acetone, water.Further preferably
, the extractant is toluene and/or acetone.Per in 20mL~30mL extractants, the addition of offal sample is 1.0g；Extraction
When, 30min is vibrated under 150rpm, is stood, filtering, produces supernatant.
In step 2), during thin-layer chromatography, solvent used is any one in acetone, methanol, hexamethylene, ethyl acetate
It is or a variety of.It is further preferred that the solvent is methanol and/or acetone.
During thin-layer chromatography, lamellae used can be made by oneself or using market conventional products.To reduce test period, work is reduced
Amount, test accuracy is improved, can directly select the commercially available fluorescent thin layer plate through overactivation.
During point sample, the dropwise addition of sample is preferably carried out in closed container, avoids reducing activating plate because of moisture in air
Adsorptivity.If being added dropwise in atmosphere, 10min is usually no more than.The method that sample is added dropwise is similar to paper chromatgraphy：Sample size is 5
~10 μ g, the origin diffusion diameter after dropwise addition are no more than 0.5cm, and distance is not less than 1.5cm, point sample start point distance lamellae between sampling point
Bottom margin at least 1.5cm.
During thin-layer chromatography, the depth that lamellae immerses solvent is no more than 0.5cm.During expansion, it can be glued in expansion container
The dipped filter paper bar of attached solvent realizes the presaturation to deploying container to accelerate the saturation of steam.The development distance of lamellae
For 10~14cm, duration of run is 30~60min, after solvent reaches the forward position pulled in advance with pencil, withdrawing plate, at 100 DEG C
20~30 minutes or air drying are heated, then with 254nm ultra violet lamps, observes phenomenon.An ascending method, double can be used
Deployed to ascending method or successive ascending method.Thin-layer chromatography device can use prior art, or using Application No.
Thin-layer chromatography device disclosed in CN201620567847.2 patent.
In step 3), the solvent is acetone.
In step 4), the analysis condition of gas chromatography combined with mass spectrometry analysis is：Chromatographic column：HP-5MS(60m*250μm*
0.25 μm) capillary column；Injector temperature：280℃；Carrier gas：He, 1ml/min；Transmission line temperature：270℃；EI sources electronic energy
Amount：70eV；Multiplier voltage：1450V；Mass scan range：30~550amu；Ion source temperature：230℃；Level Four bar temperature：
150℃；Sample size：1μL；Split ratio：1:10；Temperature programming：Initial temperature：50 DEG C, 2min is kept, then with 5 DEG C/min liters
Temperature keeps 6min to 250 DEG C；The solvent delay time is 6min.
In step 4), according to the retention time of difference chromatographic peak, retrieved in spectral peak database, you can it is determined that pollution
Thing.NIST storehouses may be selected in spectral peak database.
The method of the thin-layer chromatography coupling gas chromatography combined with mass spectrometry technical Analysis tobacco pollutant of the present invention, it is determined that extraction
Take, the analysis condition of thin-layer chromatography and gas chromatography combined with mass spectrometry analysis, optimize sample treatment and chromatographic condition, can be with
Simplicity, tobacco pollutant is fast and effectively determined, improve the screening efficiency to tobacco pollutant.
Brief description of the drawings
Fig. 1 is the flow chart of the assay method of the present invention；
Fig. 2 is the chromatogram of the pollution cigarette sample solution of embodiment 1.
Embodiment
With reference to specific embodiment, the invention will be further described.
Embodiment 1
The method of the thin-layer chromatography coupling gas chromatography combined with mass spectrometry technical Analysis tobacco pollutant of the present embodiment, flow are shown
It is intended to as shown in figure 1, comprising the following steps：
1) 20mL acetone and 1.0g offal samples are added into 50mL triangular flask, triangular flask is placed in oscillator
30min is vibrated under 150rpm, is stood, filtering, obtains supernatant；
2) take supernatant to carry out thin-layer chromatography, use lamellae to comprise the following steps for the fluorescent thin layer plate of activation：
1. quantitatively pipetting 4 μ L of supernatant liquid with 10 μ L liquid-transfering guns carries out point sample；Point sample diameter is no more than 0.5cm, sampling point spacing
From being 1.5cm for 1.5cm, point sample start point distance lamellae bottom margin；
2. deployed using acetone as solvent in closed container；Before expansion, presaturation is carried out to expansion container；Expansion
When, the depth that lamellae enters solvent is no more than 0.5cm, and after 50min, expansion reaches 12.2cm, and lamellae is added at 100 DEG C
Hot 20min drying；The component spot being separated from each other is observed after drying under 254nm uviol lamps；
3) iris out component spot with pencil and scrape, add acetone elution dissolution, obtain dissolution fluid；Dissolution fluid is entered into promoting the circulation of qi
Phase chromatograph mass spectrum analysis, analysis condition are：Chromatographic column：HP-5MS (60m*250 μm * 0.25 μm) capillary column；Injector temperature：
280℃；Carrier gas：He, 1ml/min；Transmission line temperature：270℃；EI sources electron energy：70eV；Multiplier voltage：1450V；Matter
Measure scanning range：30~550amu；Ion source temperature：230℃；Level Four bar temperature：150℃；Sample size：1μL；Split ratio：1:
10；Temperature programming：Initial temperature：50 DEG C, 2min is kept, is then warming up to 250 DEG C with 5 DEG C/min, keeps 6min；Solvent delay
Time is 6min；
4) compare the spectrogram difference of pollution cigarette sample and standard cigarette sample, the retention time of difference chromatographic peak is determined, in NIST storehouses
Respective compound is retrieved, determines pollutant.
In the embodiment, pollute cigarette sample solution chromatogram as indicated with 2, according to difference characteristic peak information, the dirt that examination goes out
Dye thing is succinic acid 2- methoxy ethyl hendecane base esters, and No. CAS is 1000325-81-1.
Embodiment 2
The method of the thin-layer chromatography coupling gas chromatography combined with mass spectrometry technical Analysis tobacco pollutant of the present embodiment, including with
Lower step：
1) 30mL toluene and 1.0g offal samples are added into 50mL triangular flask, triangular flask is placed in oscillator
30min is vibrated under 150rpm, is stood, filtering, obtains supernatant；
2) take supernatant to carry out thin-layer chromatography, use lamellae to comprise the following steps for the fluorescent thin layer plate of activation：
1. quantitatively pipetting 4 μ L of supernatant liquid with 10 μ L liquid-transfering guns carries out point sample；Point sample diameter is no more than 0.5cm, sampling point spacing
From being 1.5cm for 1.5cm, point sample start point distance lamellae bottom margin；
2. deployed using acetone as solvent in closed container；Before expansion, presaturation is carried out to expansion container；Expansion
When, the depth that lamellae enters solvent is no more than 0.5cm, and after 50min, expansion reaches 12.2cm, and lamellae is added at 100 DEG C
Hot 20min drying；The component spot being separated from each other is observed after drying under 254nm uviol lamps；
3) iris out component spot with pencil and scrape, add acetone elution dissolution, obtain dissolution fluid；Dissolution fluid is entered into promoting the circulation of qi
Phase chromatograph mass spectrum analysis, analysis condition are：Chromatographic column：HP-5MS (60m*250 μm * 0.25 μm) capillary column；Injector temperature：
280℃；Carrier gas：He, 1ml/min；Transmission line temperature：270℃；EI sources electron energy：70eV；Multiplier voltage：1450V；Matter
Measure scanning range：30~550amu；Ion source temperature：230℃；Level Four bar temperature：150℃；Sample size：1μL；Split ratio：1:
10；Temperature programming：Initial temperature：50 DEG C, 2min is kept, is then warming up to 250 DEG C with 5 DEG C/min, keeps 6min；Solvent delay
Time is 6min；
4) compare the spectrogram difference of pollution cigarette sample and standard cigarette sample, the retention time of difference chromatographic peak is determined, in NIST storehouses
Respective compound is retrieved, determines pollutant.
In the embodiment, the pollutant that examination goes out is succinic acid 2- methoxy ethyl hendecane base esters, and No. CAS is
1000325-81-1。
Embodiment 3
The method of the thin-layer chromatography coupling gas chromatography combined with mass spectrometry technical Analysis tobacco pollutant of the present embodiment, including with
Lower step：
1) 20mL toluene and 1.0g offal samples are added into 50mL triangular flask, triangular flask is placed in oscillator
30min is vibrated under 150rpm, is stood, filtering, obtains supernatant；
2) take supernatant to carry out thin-layer chromatography, use lamellae to comprise the following steps for the fluorescent thin layer plate of activation：
1. quantitatively pipetting 4 μ L of supernatant liquid with 10 μ L liquid-transfering guns carries out point sample；Point sample diameter is no more than 0.5cm, sampling point spacing
From being 1.5cm for 1.5cm, point sample start point distance lamellae bottom margin；
2. deployed using methanol as solvent in closed container；Before expansion, presaturation is carried out to expansion container；Expansion
When, the depth that lamellae enters solvent is no more than 0.5cm, and after 50min, expansion reaches 10.8cm, and lamellae is added at 100 DEG C
Hot 20min drying；The component spot being separated from each other is observed after drying under 254nm uviol lamps；
3) iris out component spot with pencil and scrape, add acetone elution dissolution, obtain dissolution fluid；Dissolution fluid is entered into promoting the circulation of qi
Phase chromatograph mass spectrum analysis, analysis condition are：Chromatographic column：HP-5MS (60m*250 μm * 0.25 μm) capillary column；Injector temperature：
280℃；Carrier gas：He, 1ml/min；Transmission line temperature：270℃；EI sources electron energy：70eV；Multiplier voltage：1450V；Matter
Measure scanning range：30~550amu；Ion source temperature：230℃；Level Four bar temperature：150℃；Sample size：1μL；Split ratio：1:
10；Temperature programming：Initial temperature：50 DEG C, 2min is kept, is then warming up to 250 DEG C with 5 DEG C/min, keeps 6min；Solvent delay
Time is 6min；
4) compare the spectrogram difference of pollution cigarette sample and standard cigarette sample, the retention time of difference chromatographic peak is determined, in NIST storehouses
Respective compound is retrieved, determines pollutant.
In the embodiment, the pollutant that examination goes out is succinic acid 2- methoxy ethyl hendecane base esters, and No. CAS is
1000325-81-1。
Embodiment 4
The method of the thin-layer chromatography coupling gas chromatography combined with mass spectrometry technical Analysis tobacco pollutant of the present embodiment, including with
Lower step：
1) 20mL acetone and 1.0g offal samples are added into 50mL triangular flask, triangular flask is placed in oscillator
30min is vibrated under 150rpm, is stood, filtering, obtains supernatant；
2) take supernatant to carry out thin-layer chromatography, use lamellae to comprise the following steps for the fluorescent thin layer plate of activation：
1. quantitatively pipetting 4 μ L of supernatant liquid with 10 μ L liquid-transfering guns carries out point sample；Point sample diameter is no more than 0.5cm, sampling point spacing
From being 1.5cm for 1.5cm, point sample start point distance lamellae bottom margin；
2. deployed using methanol as solvent in closed container；Before expansion, presaturation is carried out to expansion container；Expansion
When, the depth that lamellae enters solvent is no more than 0.5cm, and after 50min, expansion reaches 10.8cm, and lamellae is added at 100 DEG C
Hot 20min drying；The component spot being separated from each other is observed after drying under 254nm uviol lamps；
3) iris out component spot with pencil and scrape, add acetone elution dissolution, obtain dissolution fluid；Dissolution fluid is entered into promoting the circulation of qi
Phase chromatograph mass spectrum analysis, analysis condition are：Chromatographic column：HP-5MS (60m*250 μm * 0.25 μm) capillary column；Injector temperature：
280℃；Carrier gas：He, 1ml/min；Transmission line temperature：270℃；EI sources electron energy：70eV；Multiplier voltage：1450V；Matter
Measure scanning range：30~550amu；Ion source temperature：230℃；Level Four bar temperature：150℃；Sample size：1μL；Split ratio：1:
10；Temperature programming：Initial temperature：50 DEG C, 2min is kept, is then warming up to 250 DEG C with 5 DEG C/min, keeps 6min；Solvent delay
Time is 6min；
4) compare the spectrogram difference of pollution cigarette sample and standard cigarette sample, the retention time of difference chromatographic peak is determined, in NIST storehouses
Respective compound is retrieved, determines pollutant.
In the embodiment, the pollutant that examination goes out is succinic acid 2- methoxy ethyl hendecane base esters, and No. CAS is
1000325-81-1。
Comparative example 1
The detection method of comparative example 1, in step 1), using hexamethylene as extractant, expansion is used as using acetone in step 2)
Agent, thin-layer chromatography, 50min expansion 12cm, it is impossible to it was observed that component spot are carried out using method same as Example 1.
Comparative example 2
The detection method of comparative example 2, in step 1), using water as extractant, using acetone as solvent in step 2), adopt
Thin-layer chromatography is carried out with method same as Example 1,50min expansion 13.2cm, there is underlap, explanation at extension 0-4cm
Sample impurity content is more, is unsuitable for for follow-up GC-MS analyses.
Comparative example 3
The detection method of comparative example 3, in step 1), using toluene as extractant, using volume ratio as 1 in step 2):1 ring
Hexane, the mixed solvent of ethyl acetate carry out thin-layer chromatography, 50min exhibitions as solvent using method same as Example 1
Open 10.8cm, it is impossible to it was observed that component spot.
Comparative example 4
The detection method of comparative example 4, in step 1), using acetone as extractant, using volume ratio as 1 in step 2):1 ring
Hexane, the mixed solvent of ethyl acetate carry out thin-layer chromatography, 50min exhibitions as solvent using method same as Example 1
Open 5.8cm, it is impossible to it was observed that component spot.
Claims (7)
- A kind of 1. method of thin-layer chromatography coupling gas chromatography combined with mass spectrometry technical Analysis tobacco pollutant, it is characterised in that bag Include following steps：1）Extractant is added into offal sample to be extracted, and is filtered, is obtained supernatant；2）Take supernatant to carry out thin-layer chromatography, component spot disconnected from each other is obtained on lamellae；3）Remove component spot and add solvent and carry out elution dissolution, obtain dissolution fluid；4）Dissolution fluid is subjected to gas chromatography combined with mass spectrometry analysis, obtains sample spectrogram；By the spectrum of sample spectrogram and standard cigarette sample Figure is compared, and determines difference chromatographic peak；Spectral peak information according to difference chromatographic peak determines pollutant；Step 1）In, the extraction Agent is taken as any one in toluene, acetone or two kinds；Step 2）In, during thin-layer chromatography, solvent used is in acetone, methanol Any one or two kinds.
- 2. the method as described in claim 1, it is characterised in that step 2）In, the lamellae is the fluorescent thin layer plate of activation.
- 3. the method as described in claim 1, it is characterised in that step 2）In, during thin-layer chromatography, point sample diameter is no more than 0.5cm, distance is not less than 1.5cm, point sample start point distance lamellae bottom margin at least 1.5cm between sampling point.
- 4. the method as described in claim 1, it is characterised in that step 2）In, during thin-layer chromatography, lamellae immerses solvent Depth is no more than 0.5cm.
- 5. the method as described in claim 1, it is characterised in that step 3）In, the solvent is acetone.
- 6. the method as described in claim 1 or 5, it is characterised in that step 4）In, the analysis of gas chromatography combined with mass spectrometry analysis Condition is：Chromatographic column：60m*250 μm * 0.25 μm of HP-5MS capillary columns；Injector temperature：280 ℃；Carrier gas：He, 1 ml/min；Transmission line temperature：270 ℃；EI sources electron energy：70 eV；Multiplier voltage：1450V；Mass scan range：30 ~550 amu；Ion source temperature：230 ℃；Level Four bar temperature：150 ℃；Sample size：1μL；Split ratio：1:10；Program liter Temperature：Initial temperature：50 DEG C, 2min is kept, is then warming up to 250 DEG C with 5 DEG C/min, keeps 6min；The solvent delay time is 6min。
- 7. the method as described in claim 1, it is characterised in that step 4）In, according to the retention time of difference chromatographic peak, composing Peak data is retrieved in storehouse, you can determines pollutant.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610813611.7A CN106442845B (en) | 2016-09-09 | 2016-09-09 | A kind of method of thin-layer chromatography coupling gas chromatography combined with mass spectrometry technical Analysis tobacco pollutant |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610813611.7A CN106442845B (en) | 2016-09-09 | 2016-09-09 | A kind of method of thin-layer chromatography coupling gas chromatography combined with mass spectrometry technical Analysis tobacco pollutant |
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| Publication Number | Publication Date |
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| CN106442845A CN106442845A (en) | 2017-02-22 |
| CN106442845B true CN106442845B (en) | 2018-04-03 |
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| US6703244B2 (en) * | 2001-07-20 | 2004-03-09 | William A. Croft | Method for confirming presence of mycotoxicosis |
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| CN104833700A (en) * | 2015-03-20 | 2015-08-12 | 红云红河烟草(集团)有限责任公司 | Online mildew detection method for cigarette production line |
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| US6786221B2 (en) * | 1997-04-21 | 2004-09-07 | Kerry Scott Lane | Method and system for assay and removal of harmful toxins during processing of tobacco products |
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