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
- Publication number
- 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
- Authority
- CN
- China
- Prior art keywords
- sample
- thin
- layer chromatography
- pollutant
- lamellae
- 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.)
- Active
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
- G01N30/90—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
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 |
Applications Claiming Priority (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 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106442845A CN106442845A (en) | 2017-02-22 |
| CN106442845B true CN106442845B (en) | 2018-04-03 |
Family
ID=58167577
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610813611.7A Active 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 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106442845B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1384714A (en) * | 1997-04-21 | 2002-12-11 | 凯丽·斯科特·莱恩 | Method and system for assay and removal of harmful toxins during pocess of tobacco products |
| US6703244B2 (en) * | 2001-07-20 | 2004-03-09 | William A. Croft | Method for confirming presence of mycotoxicosis |
| 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 |
| CN104820052A (en) * | 2015-04-28 | 2015-08-05 | 国家烟草质量监督检验中心 | Method for rapidly warning mildewing of tobacco and tobacco products |
| CN104833700A (en) * | 2015-03-20 | 2015-08-12 | 红云红河烟草(集团)有限责任公司 | On-line mildewing detection method on cigarette production line |
-
2016
- 2016-09-09 CN CN201610813611.7A patent/CN106442845B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1384714A (en) * | 1997-04-21 | 2002-12-11 | 凯丽·斯科特·莱恩 | Method and system for assay and removal of harmful toxins during pocess of tobacco products |
| 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 |
| US6703244B2 (en) * | 2001-07-20 | 2004-03-09 | William A. Croft | Method for confirming presence of mycotoxicosis |
| CN104833700A (en) * | 2015-03-20 | 2015-08-12 | 红云红河烟草(集团)有限责任公司 | On-line mildewing detection method on cigarette production line |
| CN104820052A (en) * | 2015-04-28 | 2015-08-05 | 国家烟草质量监督检验中心 | Method for rapidly warning mildewing of tobacco and tobacco products |
Non-Patent Citations (2)
| Title |
|---|
| Identification of Lepidium meyenii (Walp.) based on spectra and chromatographic characteristics of its principal functional ingredients;Wenwen Jin 等;《Journal of the Science of Food and Agriculture》;20070730;第87卷(第12期);2251-2258 * |
| 卷烟烟气中多环芳烃的测定;王进 等;《环境化学》;20050131;第24卷(第1期);101-103 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106442845A (en) | 2017-02-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Orasche et al. | In-situ derivatization thermal desorption GC-TOFMS for direct analysis of particle-bound non-polar and polar organic species | |
| Tamayo et al. | Molecularly imprinted polymers for solid-phase extraction and solid-phase microextraction: Recent developments and future trends | |
| Fang et al. | Multi‐residue determination of organophosphorus and organochlorine pesticides in environmental samples using solid‐phase extraction with cigarette filter followed by gas chromatography–mass spectrometry | |
| CN101140268B (en) | Analysis method for semi-volatility component in cigarette main stream flue gas | |
| Beiranvand et al. | Simple, low-cost and reliable device for vacuum-assisted headspace solid-phase microextraction of volatile and semivolatile compounds from complex solid samples | |
| Rani et al. | Quantification of tricyclic and nontricyclic antidepressants in spiked plasma and urine samples using microextraction in packed syringe and analysis by LC and GC-MS | |
| Hsieh et al. | Automated on-line liquid–liquid extraction system for temporal mass spectrometric analysis of dynamic samples | |
| CN106442845B (en) | A kind of method of thin-layer chromatography coupling gas chromatography combined with mass spectrometry technical Analysis tobacco pollutant | |
| Kaur et al. | Simple and rapid determination of phthalates using microextraction by packed sorbent and gas chromatography with mass spectrometry quantification in cold drink and cosmetic samples | |
| Ho et al. | Development of molecular imprinted polymer for selective adsorption of benz [a] pyrene among airborne polycyclic aromatic hydrocarbon compounds | |
| Wilson et al. | Planar chromatography–Current practice and future prospects | |
| Gorassini et al. | Polymeric reversed phase and small particle size silica gel solid phase extractions for rapid analysis of sterols and triterpene dialcohols in olive oils by GC-FID | |
| Luiz Oenning et al. | Evaluation of two membrane‐based microextraction techniques for the determination of endocrine disruptors in aqueous samples by HPLC with diode array detection | |
| Nolvachai et al. | Miniaturized molecularly imprinted polymer extraction method for the gas chromatographic analysis of flavonoids | |
| Mokhtar et al. | Direct ionic liquid extractant injection for volatile chemical analysis–a gas chromatography sampling technique | |
| Pietrzyńska et al. | Optimization of the in-needle extraction device for the direct flow of the liquid sample through the sorbent layer | |
| CN107576746A (en) | The method that Glycerin, mixed triester with caprylic acid capric acid in analysis essence is separated using gaschromatographic mass spectrometry | |
| Hyder et al. | Hollow-fiber liquid phase microextraction for lignin pyrolysis acids in aerosol samples and gas chromatography–mass spectrometry analysis | |
| Tong et al. | Liquid chromatographic-mass spectrometric method for detection of estrogen in commercial oils and in fruit seed oils | |
| Pavlova et al. | Trace analysis of hydrophobic micropollutants in aqueous samples using capillary traps | |
| Sha et al. | Determination of volatile organic acids in tobacco by single‐drop microextraction with in‐syringe derivatization followed by GC‐MS | |
| Ghiasvand et al. | Use of volatile organic solvents in headspace liquid‐phase microextraction by direct cooling of the organic drop using a simple cooling capsule | |
| Possi-Pezzali et al. | Evaluation of electrospun fibers as solid phase extraction sorbents for sample preparation in HPLC-MS/MS confirmatory doping control analysis of dexamethasone and betamethasone | |
| CN106526059B (en) | A kind of method of thin-layer chromatography coupling infrared technique analysis tobacco pollutant | |
| Knupp et al. | Identification of flavor components in perfumes by headspace solid-phase microextraction and gas chromatography-mass spectrometry |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |