CN106442845A - Method for analyzing tobacco pollutants by utilizing thin-layer chromatography coupled gas chromatography-mass spectrometry linked technique - Google Patents
Method for analyzing tobacco pollutants by utilizing thin-layer chromatography coupled gas chromatography-mass spectrometry linked technique Download PDFInfo
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- CN106442845A CN106442845A CN201610813611.7A CN201610813611A CN106442845A CN 106442845 A CN106442845 A CN 106442845A CN 201610813611 A CN201610813611 A CN 201610813611A CN 106442845 A CN106442845 A CN 106442845A
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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
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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
Abstract
The invention relates to a method for analyzing tobacco pollutants by utilizing a thin-layer chromatography coupled gas chromatography-mass spectrometry linked technique, and belongs to the field of detection of tobaccos. The method comprises the following steps: 1) adding an extracting agent into a tobacco powder sample and extracting; filtering to obtain supernatant; 2) carrying out thin layer chromatography on the supernatant to obtain component spots, which are separated from one other, on a thin-layer plate; 3) taking off the component spots and adding the component spots into a solvent for eluting and dissolving out to obtain a digested solution; 4) obtaining a sample spectrogram; comparing the sample spectrogram with a spectrogram of a standard tobacco sample and determining a difference chromatographic peak; determining the pollutants according to spectrum peak information of the difference chromatographic peak. According to the method provided by the invention, the tobacco powder sample is analyzed by comprehensively utilizing the thin-layer chromatography coupled gas chromatography-mass spectrometry linked technique; the tobacco powder sample is compared with a spectrum peak of the standard tobacco sample so as to qualitatively screen the pollutants; the method has the advantages of high applicability, simplicity in operation and short detection time.
Description
Technical field
The invention belongs to the Screening analysis technical field of the pollution compound of Nicotiana tabacum L. and tobacco product, and in particular to a kind of thin
The method of layer chromatography coupling gas chromatography combined with mass spectrometry technical Analysis Nicotiana tabacum L. pollutant.
Background technology
Nicotiana tabacum L. can be polluted by allogenic material during production, transport and storage, so as to affect the perfume (or spice) of Nicotiana tabacum L.
Gas and jealous.But the Nicotiana tabacum L. being contaminated be actually by which kind of Substances Pollution, and the problems such as polluter comes wherefrom, in reality
Relatively it is difficult to resolve certainly in the work of border.
Content of the invention
It is an object of the invention to provide a kind of thin layer chromatography couples gas chromatography combined with mass spectrometry technical Analysis Nicotiana tabacum L. pollutant
Method, which has the characteristics that, and operation is simple, detection time is short, can effectively improve the screening efficiency of Nicotiana tabacum L. pollutant.
In order to realize object above, the technical solution adopted in the present invention is：
A kind of method that thin layer chromatography couples gas chromatography combined with mass spectrometry technical Analysis Nicotiana tabacum L. pollutant, including following step
Suddenly：
1) in offal sample, add extractant to be extracted, filter, obtain supernatant；
2) taking supernatant carries out thin layer chromatography, obtains component speckle disconnected from each other on lamellae；
3) remove component speckle and add solvent that eluting dissolution is carried out, obtain dissolution fluid；
4) dissolution fluid is carried out gas chromatography combined with mass spectrometry analysis, obtains sample spectrogram；By sample spectrogram and standard cigarette sample
Spectrogram be compared, determine difference chromatographic peak；Pollutant are determined according to the spectral peak information of difference chromatographic peak.
Thin layer chromatography (TLC) be thin plate chromatography again, its be adsorbent, carrier or other active substances are uniformly coated on 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 Deca of sample, launch, develop the color, comparing Rf value and quantitative analyses etc..Due to each component in sample
Property difference, through moving after expansion, the component speckle that can be separated from each other.
Gas chromatography combined with mass spectrometry technology will gas chromatograph be attached by interface module with mass spectrograph, with gas phase
The means that chromatograph is separated as sample, prepared, mass spectrum is carried out qualitative, quantitative point as the on-line checking means of gas chromatogram
Analysis, is aided with a kind of corresponding data collection chromatograph-mass spectrometer coupling technology built-up with control system.
The present invention is in conjunction with thin layer chromatography and gas phase hydrolysis and condensation, sets up Nicotiana tabacum L. exogenous material
Screening method, the polluter for finding out Nicotiana tabacum L. provides a kind of new way.The method is using each component in cigarette sample in a certain material
In absorption or solubility property difference, or the difference with other material affinity interaction performances, realize different solute sharp separation；Again
The research of trace sample is carried out using gas chromatograph-mass spectrometer；Thin layer chromatography and the combination of gas phase hydrolysis and condensation
Examination for pollutant in cigarette sample has the extremely strong suitability, can preferably promote Fourier transform infrared analyser-gas
Phase chromatograph-mass spectrometer technology is in the application in pollution thing examination field.The method makes full use of the advantage of two kinds of technology,
Short have the characteristics that simple to operate, detection time, the screening efficiency of Nicotiana tabacum L. pollutant can be effectively improved.
Step 1) in, the extractant is hexamethylene, toluene, acetone, any one or more in water.Further preferably
, the extractant is toluene and/or acetone.In per 20mL～30mL extractant, the addition of offal sample is 1.0g；Extraction
When, 30min being vibrated under 150rpm, stand, filters, obtain final product supernatant.
Step 2) in, during thin layer chromatography, developing solvent used is acetone, methanol, hexamethylene, any one in ethyl acetate
Or it is multiple.It is further preferred that the developing solvent is methanol and/or acetone.
During thin layer chromatography, lamellae used can be made by oneself or using market conventional products.For reducing test period, reduce work
Amount, improves test accuracy, can directly select the commercially available fluorescent thin layer plate through overactivation.
During point sample, the Deca of sample is preferably carried out in closed container, it is to avoid reduce activating plate because of moisture in air
Adsorptivity.If Deca, is usually no more than 10min in atmosphere.The method of sample Deca is similar to paper chromatgraphy：Sample size is 5
～10 μ g, the initial point diffusion diameter after Deca is less than 0.5cm, and between sampling point, distance is not less than 1.5cm, point sample start point distance lamellae
Bottom margin at least 1.5cm.
During thin layer chromatography, the depth of lamellae immersion developing solvent is less than 0.5cm.During expansion, can launch to glue in container
The dipped filter paper bar of attached developing solvent realizes the presaturation to launching container to accelerate the saturation of steam.The development distance of lamellae
For 10～14cm, duration of run is that after 30～60min, solvent reaches the forward position for being pulled in advance with pencil, withdrawing plate, at 100 DEG C
Heating 20～30 minutes or normal temperature drying, then use 254nm ultra violet lamp, observe phenomenon.Ascending method, double can be adopted
Launched to ascending method or successive ascending method.Thin layer chromatography device can adopt prior art, or adopt Application No.
Thin layer chromatography device disclosed in the patent of CN201620567847.2.
Step 3) in, the solvent is acetone.
Step 4) in, 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 source 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 liter
Temperature keeps 6min to 250 DEG C；The solvent delay time is 6min.
Step 4) in, according to the retention time of difference chromatographic peak, in spectral peak data base, enter line retrieval, you can determine pollution
Thing.Spectral peak data base may be selected NIST storehouse.
The method of the thin layer chromatography coupling gas chromatography combined with mass spectrometry technical Analysis Nicotiana tabacum L. pollutant of the present invention, it is determined that extraction
Take, thin layer chromatography and gas chromatography combined with mass spectrometry analysis analysis condition, optimize sample treatment and chromatographic condition, permissible
Simplicity, fast and effectively measure Nicotiana tabacum L. pollutant, improve the screening efficiency to Nicotiana tabacum L. pollutant.
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.
Specific 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 Nicotiana tabacum L. pollutant of the present embodiment, flow process is shown
It is intended to as shown in figure 1, comprising the following steps：
1) 20mL acetone and 1.0g offal sample are added in the triangular flask of 50mL, triangular flask is placed in agitator
30min being vibrated under 150rpm, stand, filters, obtain supernatant；
2) taking supernatant carries out thin layer chromatography, using lamellae be activation fluorescent thin layer plate, comprise the following steps：
1. quantitatively pipetting 4 μ L of supernatant liquid with 10 μ L liquid-transfering guns carries out point sample；Point sample diameter is less than 0.5cm, sampling point spacing
From for 1.5cm, point sample start point distance lamellae bottom margin be；
2. launched in hermetic container with acetone as developing solvent；Before expansion, presaturation is carried out to launching container；Launch
When, lamellae enters the depth of developing solvent less than after 0.5cm, 50min, launching to reach 12.2cm, and lamellae is added at 100 DEG C
Hot 20min is dried；The component speckle being separated from each other is observed after drying under 254nm uviol lamp；
3) component speckle being irised out with pencil and scrape, adds acetone eluting dissolution, obtain dissolution fluid；Dissolution fluid is entered circulation of qi promoting
Phase chromatograph mass spectrum analysis, analysis condition is：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 source electron energy：70eV；Multiplier voltage：1450V；Matter
Amount sweep limitss：30～550amu；Ion source temperature：230℃；Level Four bar temperature：150℃；Sample size：1μL；Split ratio：1:
10；Temperature programming：Initial temperature：, 2min being kept, then 250 DEG C is warmed up to 5 DEG C/min, keeps 6min by 50 DEG C；Solvent delay
Time is 6min；
4) compare the spectrogram difference of pollution cigarette sample and standard cigarette sample, determine the retention time of difference chromatographic peak, in NIST storehouse
Respective compound is retrieved, determines pollutant.
In the embodiment, the chromatogram of cigarette sample solution is polluted 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 ester, and No. CAS is 1000325-81-1.
Embodiment 2
The present embodiment thin layer chromatography coupling gas chromatography combined with mass spectrometry technical Analysis Nicotiana tabacum L. pollutant method, including with
Lower step：
1) 30mL toluene and 1.0g offal sample are added in the triangular flask of 50mL, triangular flask is placed in agitator
30min being vibrated under 150rpm, stand, filters, obtain supernatant；
2) taking supernatant carries out thin layer chromatography, using lamellae be activation fluorescent thin layer plate, comprise the following steps：
1. quantitatively pipetting 4 μ L of supernatant liquid with 10 μ L liquid-transfering guns carries out point sample；Point sample diameter is less than 0.5cm, sampling point spacing
From for 1.5cm, point sample start point distance lamellae bottom margin be；
2. launched in hermetic container with acetone as developing solvent；Before expansion, presaturation is carried out to launching container；Launch
When, lamellae enters the depth of developing solvent less than after 0.5cm, 50min, launching to reach 12.2cm, and lamellae is added at 100 DEG C
Hot 20min is dried；The component speckle being separated from each other is observed after drying under 254nm uviol lamp；
3) component speckle being irised out with pencil and scrape, adds acetone eluting dissolution, obtain dissolution fluid；Dissolution fluid is entered circulation of qi promoting
Phase chromatograph mass spectrum analysis, analysis condition is：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 source electron energy：70eV；Multiplier voltage：1450V；Matter
Amount sweep limitss：30～550amu；Ion source temperature：230℃；Level Four bar temperature：150℃；Sample size：1μL；Split ratio：1:
10；Temperature programming：Initial temperature：, 2min being kept, then 250 DEG C is warmed up to 5 DEG C/min, keeps 6min by 50 DEG C；Solvent delay
Time is 6min；
4) compare the spectrogram difference of pollution cigarette sample and standard cigarette sample, determine the retention time of difference chromatographic peak, in NIST storehouse
Respective compound is retrieved, determines pollutant.
In the embodiment, the pollutant that examination goes out are succinic acid 2- methoxy ethyl hendecane base ester, and No. CAS is
1000325-81-1.
Embodiment 3
The present embodiment thin layer chromatography coupling gas chromatography combined with mass spectrometry technical Analysis Nicotiana tabacum L. pollutant method, including with
Lower step：
1) 20mL toluene and 1.0g offal sample are added in the triangular flask of 50mL, triangular flask is placed in agitator
30min being vibrated under 150rpm, stand, filters, obtain supernatant；
2) taking supernatant carries out thin layer chromatography, using lamellae be activation fluorescent thin layer plate, comprise the following steps：
1. quantitatively pipetting 4 μ L of supernatant liquid with 10 μ L liquid-transfering guns carries out point sample；Point sample diameter is less than 0.5cm, sampling point spacing
From for 1.5cm, point sample start point distance lamellae bottom margin be；
2. launched in hermetic container with methanol as developing solvent；Before expansion, presaturation is carried out to launching container；Launch
When, lamellae enters the depth of developing solvent less than after 0.5cm, 50min, launching to reach 10.8cm, and lamellae is added at 100 DEG C
Hot 20min is dried；The component speckle being separated from each other is observed after drying under 254nm uviol lamp；
3) component speckle being irised out with pencil and scrape, adds acetone eluting dissolution, obtain dissolution fluid；Dissolution fluid is entered circulation of qi promoting
Phase chromatograph mass spectrum analysis, analysis condition is：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 source electron energy：70eV；Multiplier voltage：1450V；Matter
Amount sweep limitss：30～550amu；Ion source temperature：230℃；Level Four bar temperature：150℃；Sample size：1μL；Split ratio：1:
10；Temperature programming：Initial temperature：, 2min being kept, then 250 DEG C is warmed up to 5 DEG C/min, keeps 6min by 50 DEG C；Solvent delay
Time is 6min；
4) compare the spectrogram difference of pollution cigarette sample and standard cigarette sample, determine the retention time of difference chromatographic peak, in NIST storehouse
Respective compound is retrieved, determines pollutant.
In the embodiment, the pollutant that examination goes out are succinic acid 2- methoxy ethyl hendecane base ester, and No. CAS is
1000325-81-1.
Embodiment 4
The present embodiment thin layer chromatography coupling gas chromatography combined with mass spectrometry technical Analysis Nicotiana tabacum L. pollutant method, including with
Lower step：
1) 20mL acetone and 1.0g offal sample are added in the triangular flask of 50mL, triangular flask is placed in agitator
30min being vibrated under 150rpm, stand, filters, obtain supernatant；
2) taking supernatant carries out thin layer chromatography, using lamellae be activation fluorescent thin layer plate, comprise the following steps：
1. quantitatively pipetting 4 μ L of supernatant liquid with 10 μ L liquid-transfering guns carries out point sample；Point sample diameter is less than 0.5cm, sampling point spacing
From for 1.5cm, point sample start point distance lamellae bottom margin be；
2. launched in hermetic container with methanol as developing solvent；Before expansion, presaturation is carried out to launching container；Launch
When, lamellae enters the depth of developing solvent less than after 0.5cm, 50min, launching to reach 10.8cm, and lamellae is added at 100 DEG C
Hot 20min is dried；The component speckle being separated from each other is observed after drying under 254nm uviol lamp；
3) component speckle being irised out with pencil and scrape, adds acetone eluting dissolution, obtain dissolution fluid；Dissolution fluid is entered circulation of qi promoting
Phase chromatograph mass spectrum analysis, analysis condition is：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 source electron energy：70eV；Multiplier voltage：1450V；Matter
Amount sweep limitss：30～550amu；Ion source temperature：230℃；Level Four bar temperature：150℃；Sample size：1μL；Split ratio：1:
10；Temperature programming：Initial temperature：, 2min being kept, then 250 DEG C is warmed up to 5 DEG C/min, keeps 6min by 50 DEG C；Solvent delay
Time is 6min；
4) compare the spectrogram difference of pollution cigarette sample and standard cigarette sample, determine the retention time of difference chromatographic peak, in NIST storehouse
Respective compound is retrieved, determines pollutant.
In the embodiment, the pollutant that examination goes out are succinic acid 2- methoxy ethyl hendecane base ester, and No. CAS is
1000325-81-1.
Comparative example 1
The detection method of comparative example 1, step 1) in, using hexamethylene as extractant, step 2) in using acetone as expansion
Agent, carries out thin layer chromatography using method same as Example 1, and 50min launches 12cm, it is impossible to observe component speckle.
Comparative example 2
The detection method of comparative example 2, step 1) in, using water as extractant, step 2) in using acetone as developing solvent, adopt
Thin layer chromatography is carried out with method same as Example 1,50min launches 13.2cm, has underlap, explanation at extension 0-4cm
Sample impurity content is many, is unsuitable for analyzing for follow-up GC-MS.
Comparative example 3
The detection method of comparative example 3, step 1) in, using toluene as extractant, step 2) in volume ratio as 1:1 ring
Hexane, the mixed solvent of ethyl acetate carry out thin layer chromatography, 50min exhibition as developing solvent using method same as Example 1
Open 10.8cm, it is impossible to observe component speckle.
Comparative example 4
The detection method of comparative example 4, step 1) in, using acetone as extractant, step 2) in volume ratio as 1:1 ring
Hexane, the mixed solvent of ethyl acetate carry out thin layer chromatography, 50min exhibition as developing solvent using method same as Example 1
Open 5.8cm, it is impossible to observe component speckle.
Claims (9)
1. a kind of method that thin layer chromatography couples gas chromatography combined with mass spectrometry technical Analysis Nicotiana tabacum L. pollutant, it is characterised in that bag
Include following steps：
1) in offal sample, add extractant to be extracted, filter, obtain supernatant；
2) taking supernatant carries out thin layer chromatography, obtains component speckle disconnected from each other on lamellae；
3) remove component speckle and add solvent that eluting dissolution is carried out, obtain dissolution fluid；
4) dissolution fluid is carried out gas chromatography combined with mass spectrometry analysis, obtains sample spectrogram；Spectrum by sample spectrogram and standard cigarette sample
Figure is compared, and determines difference chromatographic peak；Pollutant are determined according to the spectral peak information of difference chromatographic peak.
2. the method for claim 1, it is characterised in that step 1) in, the extractant is hexamethylene, toluene, acetone,
Any one or more in water.
3. the method for claim 1, it is characterised in that step 2) in, during thin layer chromatography, developing solvent used is acetone,
Any one or more in methanol, hexamethylene, ethyl acetate.
4. the method as described in claim 1 or 3, it is characterised in that step 2) in, the lamellae is the fluorescence thin layer of activation
Plate.
5. the method as described in claim 1 or 3, it is characterised in that step 2) in, during thin layer chromatography, point sample diameter is less than
0.5cm, between sampling point, distance is not less than 1.5cm, point sample start point distance lamellae bottom margin at least 1.5cm.
6. the method as described in claim 1 or 3, it is characterised in that step 2) in, during thin layer chromatography, lamellae immersion launches
The depth of agent is less than 0.5cm.
7. the method for claim 1, it is characterised in that step 3) in, the solvent be.
8. the method as described in claim 1,3 or 7, it is characterised in that step 4) in, gas chromatography combined with mass spectrometry analysis point
Analysis condition is：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 source electron energy：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：Starting
Temperature：, 2min being kept, then 250 DEG C is warmed up to 5 DEG C/min, keeps 6min by 50 DEG C；The solvent delay time is 6min.
9. the method for claim 1, it is characterised in that step 4) in, according to the retention time of difference chromatographic peak, in spectrum
Peak data enters line retrieval in storehouse, you can determine pollutant.
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| 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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Cited By (1)
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| CN112014395A (en) * | 2020-09-01 | 2020-12-01 | 上海烟草集团有限责任公司 | Method for identifying cigarette surface insect spots based on characteristic fingerprint spectrum |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112014395A (en) * | 2020-09-01 | 2020-12-01 | 上海烟草集团有限责任公司 | Method for identifying cigarette surface insect spots based on characteristic fingerprint spectrum |
| CN112014395B (en) * | 2020-09-01 | 2022-10-04 | 上海烟草集团有限责任公司 | Method for identifying cigarette surface insect spots based on characteristic fingerprint spectrum |
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