CN102735775A - On-line entrapment and sample introduction method for gas chromatography-mass spectrometry analysis of pyrolyzate of material used for cigarette - Google Patents
On-line entrapment and sample introduction method for gas chromatography-mass spectrometry analysis of pyrolyzate of material used for cigarette Download PDFInfo
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Abstract
The invention relates to an on-line entrapment and sample introduction method for a gas chromatography-mass spectrometry analysis of pyrolyzate of a material used for cigarette, which belongs to the pyrolytic cracking analytical technology field. The method comprises the following steps: waterless air or oxygen nitrogen mixed gas is taken as a cracking reaction gas and continuously passed through a cracking chamber; a material sample used for cigarette is filled in a cracking tube and placed in the cracking chamber of a heated filament cracking device for cracking reaction, the cracking products is subjected to on-line purge to cold trap by the cracking reaction gas, and condensed in the cold trap, uncondensed cracking reaction gas is shunted and discharged; after the cracking reaction is completed, the cracking chamber and the cold trap are purged by inert gas for 0.5-1 minutes for displacing the residual reaction gas, and a heating program of the cold trap is set, the entrapped cracking products at low temperature is volatilized and sent to a gas chromatograph-mass spectrometer by helium for analysis. The invention has the advantages that under the condition of aerobic cracking, the on-line entrapment and sample introduction of cracking products of the material used for cigarette can be realized, the on-line entrapment and sample introduction process is more complete, and the invention provides more scientific and comprehensive analysis data and theory support for screening availability the materials used for cigarette.
Description
Technical field:
The present invention relates to online capture and sample injection method that a kind of smoking material thermal cracking products gas chromatography mass spectrometry is analyzed, belong to the thermal cracking analysis technical field.
Background technology:
Cigarette product is consumed after the experience combustion process; Therefore the cigarette product research staff pays special attention to the formation and the content of its products of combustion when selection is used for the material of cigarette product manufacturing; Make every effort to when reaching application target, avoid the generation of objectionable constituent as far as possible.Heat up fast because of pyrolysis technology has, maximum temperature is higher than the advantage that cigarette props up maximum combustion temperature, thereby can be used for simulating cigarette and burns and sucks environment, estimates the effect of associated materials in cigarette and the security of use thereof.Therefore because of cigarette product is in aerobic environment, to burn, simulate the oxygen that breaking test that cigarette burns and sucks environment need be introduced certain content, and the existence of oxygen can influence the gas chromatography compartment analysis of follow-up pyrolysis product.For addressing this problem; The tobacco worker has carried out series of studies; As adopt the filament pyrolyzer in the cracking reaction chamber of design voluntarily, to carry out the aerobic cracking; Promptly in advance the atmosphere in the cracking reaction chamber is adjusted to certain oxygen level, under static condition, accomplishes the cracking of sample then, use simultaneously SPME to pyrolysis product extract, air inlet matter combined instrument carries out product analysis.Like Hou Ying, Yang Yan, Chen Yongkuan
[1-4]Deng to xenthophylls, fig medicinal extract, polyhydroxy pyrazine, 2,3-dihydro-3, the Study on Cleavage of 5-dihydroxy-6-methyl-4 (H) pyrans-4-ketone, rutin etc.But this method is because of the loading capacity of SPME and the selectivity of extraction, and there is defective in its total analysis for pyrolysis product, and the cracking reaction chamber of designing voluntarily, and gas does not flow when cracking reaction, thereby is not inconsistent with the actual aspiration phases of cigarette.Kong Haohui etc.
[5]Use the filament pyrolyzer; Cracking reaction gas is that oxygen concentration is higher than 20% nitrogen oxygen atmosphere, uses absorption pyrolysis product under the online adsorption trap normal temperature, the desorption that then heats up pyrolysis product; Tobacco is carried out the cracking experiment, realized that aerobic cracking and online product capture sample introduction.But there is selectivity in the employed filler of adsorption trap to the absorption and the desorption of product, is unfavorable for the multianalysis to pyrolysis product.
List of references:
[1] Hou Ying, Xu Jicang, Wang Baoxing etc. the pyrolysis product analysis [J] of xenthophylls. tobacco chemistry, 2007,12:27～32
[2] Yang Yan, Cao Qiue, Xu Jicang etc., the thermal cracking products research [J] of cigarette bobbin paper adjuvant. the .2006 of spectrographic laboratory (6): 1292～1295
[3] Yang Yan, Cao Qiue, Xu Jicang etc., the thermal cracking products research [J] of tobacco aromatics using Fructus Fici extract. spectrographic laboratory, 2006 (6): 1288～1291
[4] Chen Yongkuan, Kong Ningchuan .2 such as Wu Yi, 3-dihydro-3, the synthetic and thermal cracking behavior [J] of 5-dihydroxy-6-methyl-4 (H) pyrans-4-ketone. chemical research and application, 2003,2 (1): 45～47
[5] Kong Haohui. tobacco pyrolytic cracking analytical method application number 200810026374.5
Summary of the invention:
The objective of the invention is to overcome the deficiency of prior art, and the online capture and the sample injection method that provide a kind of smoking material thermal cracking products gas chromatography mass spectrometry to analyze.
Method of the present invention is: anhydrous air or volume ratio be 9: 91 oxygen-nitrogen mixture as cracking reaction gas, and regulate its flow through the cracking appearance, make its when cracking continuously through the cracking chamber; Be seated in the smoking material sample of treating cracking in the cracking tube earlier; Cracking tube be positioned over filament pyrolyzer's cracking chamber thereafter; Start the cracking reaction program; Pyrolysis product generates and is purged to cold-trap by excessive cracking reaction gas is online, and pyrolysis product is condensed in the cold-trap, and cracking reaction gas is not because of being condensed by the shunting discharge; After cracking reaction is accomplished; Switch to inert gas purge cracking chamber and cold-trap 0.5min-1min; To replace residual reaction gas, then set the heating schedule of cold-trap, with cryogenic trapping to pyrolysis product evaporate and send into gas chromatograph-mass spectrometer analysis with helium; Wherein:
A. breaking test condition
Cracking temperature: initial temperature is 300 ℃, and keeps 5s, then with 30 ℃ of .s
-1Rise to 900 ℃ and keep 5s;
Or isothermal cracking: temperature is set at 300 ℃, keeps 5s;
The cracking atmosphere: anhydrous air or volume ratio are 9: 91 oxygen-nitrogen mixture, and gas flow rate is 40-260mL/min;
Pyrolysis product condensing trapping temperature :-120 ℃ to-40 ℃;
B. after cracking reaction is accomplished, switch to inert gas helium purge cracking chamber and cold-trap 0.5min-1min, to replace residual reaction gas;
C. cold-trap intensification condition: from-40 ℃ ,-60 ℃ or-120 ℃ with 12 ℃ of .s
-1Rise to 260 ℃ and keep 1min, again with 10 ℃ of .s
-1Rise to 300 ℃ or 350 ℃, keep 3min or 5min;
The d.GC/MS analysis condition:
The HP-INNOWAX post; Specification: 30m * 0.25mm * 0.25 μ m; The gas phase heating gradient: 40 ℃ keep 3min or 50 ℃ of maintenance 1min; Rise to 120 ℃ or 220 ℃ with 8 ℃/min, keep 5min, rise to 200 ℃ or rise to 240 ℃ with 10 ℃/min and keep 5min or with 8 ℃/min again with 20 ℃ of .min
-1Rise to 280 ℃ and keep 5min then; Mass ion source temperature: 230 ℃; Transmission line temperature: 240 ℃ or 280 ℃; Quadrupole rod temperature: 150 ℃;
Or: HP-5MS post, specification: 30m * 0.25mm * 0.25 μ m; The gas phase heating gradient: 50 ℃ keep 1min, with 8 ℃ of .min
-1Rise to 220 ℃, again with 20 ℃ of .min
-1Rise to 280 ℃ and keep 5min; The mass ion source temperature: 230 ℃, the transmission line temperature: 280 ℃, quadrupole rod temperature: 150 ℃.
The equipment of this method adopts conventional thermal cracking appearance, cold sampling system and gas chromatograph-mass spectrometer equipment.
The invention has the advantages that: in the capture process of pyrolysis product; Avoided in the cracking reaction gas oxygen for the influence of gas chromatographic analysis; Simultaneously more abundant for the capture of each component in the pyrolysis product; When sample introduction, can the highlyest be warming up to 350 ℃, guaranteed in gas chromatography, can detect the complete sample introduction of composition.The screening smoking material that is developed as of this method provides more scientific comprehensive analysis data to support with theoretical.
Description of drawings:
Gas flow path figure when Fig. 1 is sample dissociation.
Gas flow path figure when Fig. 2 is sample feeding.
Gas flow path figure when Fig. 3 is sample analysis.
Embodiment
Used instrument and reagent in following examples:
CDS5200 thermal cracking appearance (U.S. CDS company); GC6890N/5975 gas chromatography appearance, ADM1000 current meter (U.S. Anjelen Sci. & Tech. Inc); CIS 3 cold injection ports (German Gerstel company), AG204 analytical balance (sensibility reciprocal 0.0001g, Switzerland METTLER TOLEDO company), helium, oxygen, anhydrous air, nitrogen; Liquid nitrogen is used in cooling; Chromatographically pure ethanol, chromatographically pure methylene chloride, chromatographically pure normal hexane; The residual level of farming silica wool.
The thermal cracking of embodiment one, essence spice for cigarette sample
1. breaking test condition
Cracking temperature: initial temperature is 300 ℃, and keeps 5s, then with 30 ℃ of .s
-1Rise to 900 ℃ and keep 5s;
The cracking atmosphere: oxygen-nitrogen mixture (volume ratio 9: 91), gas flow rate is 260mL/min;
Pyrolysis product condensing trapping temperature :-60 ℃;
Cracking reaction switches to inert gas helium purge cracking chamber and cold-trap 0.5min after accomplishing, and to replace residual reaction gas, volatile matter is sent into GC-MS.
Pyrolysis product sampling condition (cold-trap intensification condition): from-60 ℃ with 12 ℃ of .s
-1Rise to 260 ℃ and keep 1min, again with 10 ℃ of .s
-1Rise to 350 ℃, keep 5min.
GC/MS analysis condition: HP-INNOWAX post; Specification: 30m (length) * 0.25mm (internal diameter) * 0.25 μ m (thickness); The gas phase heating gradient: 40 ℃ keep 3min, rise to 120 ℃ with 8 ℃/min, keep 5min, rise to 200 ℃ with 8 ℃/min again and keep 5min, rise to 240 ℃ with 10 ℃/min again and keep 5min; Mass ion source temperature: 230 ℃; Transmission line temperature: 240 ℃; Quadrupole rod temperature: 150 ℃;
2. breaking test and result
One of the special-purpose crystalline silica cracking tube of heat-obtaining cracking appearance is packed into the residual level of farming silica wool 1-2mg in the middle, draws 2-5 μ L sample solution (if excessive concentration is used the dilution of ethanol or methylene chloride or normal hexane) with the micro-sampling pin and is injected on the silica wool of being filled.Inadequate for essence and flavoring agent sample that is not dissolved in above-mentioned solvent or existence dissolving, adopt direct weighing method, promptly fill silica wool earlier in cracking quartz ampoule one side, then load the 2-5mg sample, the silica wool of recharging is sealed opposite side.After the equipment of treating is ready, place the cracking chamber to carry out cracking cracking tube.Table 1 is separated the result for 5 secondary fissures of certain essence sample for tobacco.
Table 1 certain essence sample 5 thermal cracking products peak areas percentage result and RSD value
The thermal cracking of embodiment two, cigarette paper sample
1. breaking test condition
Cracking temperature: 300 ℃ and keep 5s, from 300 ℃ with 30 ℃ of .s
-1Rise to 900 ℃ and keep 5s;
The cracking atmosphere: anhydrous air, gas flow rate are 40mL/min;
Pyrolysis product condensing trapping temperature :-120 ℃;
Cracking reaction switches to inert gas helium purge cracking chamber and cold-trap 1.0min after accomplishing, and to replace residual reaction gas, volatile matter is sent into GC-MS.
Pyrolysis product sampling condition (cold-trap intensification condition): from-120 ℃ with 12 ℃ of .s
-1Rise to 260 ℃ and keep 1min, again with 10 ℃ of .s
-1Rise to 300 ℃, keep 3min.
GC/MS analysis condition: gas chromatographic column: HP-5MS post, specification: 30m (length) * 0.25mm (internal diameter) * 0.25 μ m (thickness); The gas phase heating gradient: 50 ℃ keep 1min, with 8 ℃ of .min
-1Rise to 220 ℃, again with 20 ℃ of .min
-1Rise to 280 ℃ and keep 5min then; The mass ion source temperature: 230 ℃, the transmission line temperature: 280 ℃, quadrupole rod temperature: 150 ℃
2. breaking test and result
Cigarette paper is peeled off on cigarette props up, be cut into fine strip shape, be wound in fluffy little group and be placed on thermal cracking pipe middle position, after the equipment of treating is ready, place the cracking chamber to carry out cracking cracking tube.Table 2 is the cracking result of certain cigarette paper sample.
Certain cigarette paper sample thermal cracking products analysis result of table 2
The thermal cracking of embodiment three, cigarette glue sample
1. breaking test condition
Cracking temperature: isothermal cracking, temperature are set at 300 ℃ and keep 5s;
Pyrolysis product condensing trapping temperature :-40 ℃;
Cracking reaction switches to inert gas helium purge cracking chamber and cold-trap 0.8min after accomplishing, and to replace residual reaction gas, volatile matter is sent into GC-MS.
Pyrolysis product sampling condition (cold-trap intensification condition): from-40 ℃ with 12 ℃ of .s
-1Rise to 260 ℃ and keep 1min, again with 10 ℃ of .s
-1Rise to 300 ℃, keep 3min.
GC/MS analysis condition: gas chromatographic column: HP-5MS post, specification: 30m (length) * 0.25mm (internal diameter) * 0.25 μ m (thickness); The gas phase heating gradient: 50 ℃ keep 1min, with 8 ℃ of .min
-1Rise to 220 ℃, again with 20 ℃ of .min
-1Rise to 280 ℃ and keep 5min then; The mass ion source temperature: 230 ℃, the transmission line temperature: 280 ℃, quadrupole rod temperature: 150 ℃
2. breaking test and result
Thermal cracking pipe middle position filling 1-2mg silica wool, get cigarette glue sample 2-3mg with heparin tube and be added on the silica wool in advance, the application of sample end 1-2mg silica wool of recharging, after the equipment of treating is ready, place the cracking chamber to carry out cracking cracking tube thereafter.Table 3 is the thermal cracking products analysis result of certain cigarette glue sample.
Table 3 cigarette glue sample thermal cracking products analysis result
Claims (1)
1. online capture and the sample injection method analyzed of a smoking material thermal cracking products gas chromatography mass spectrometry; It is characterized in that this method carries out thermal cracking with smoking material under aerobic conditions; Pyrolysis product is blown into condensation in the online cold-trap continuously by oxygen containing cracking reaction gas; After cracking was accomplished, the heating cold-trap was sent volatile matter into GC-MS analysis with inert gas again to volatilize the pyrolysis product that is condensed; Wherein:
A. breaking test condition
Cracking temperature: initial temperature is 300 ℃, and keeps 5s, then with 30 ℃ of .s
-1Rise to 900 ℃ and keep 5s;
Or isothermal cracking: temperature is set at 300 ℃, keeps 5s;
The cracking atmosphere: anhydrous air or volume ratio are 9: 91 oxygen-nitrogen mixture, and gas flow rate is 40-260mL/min;
Pyrolysis product condensing trapping temperature :-120 ℃ to-40 ℃;
B. after cracking reaction is accomplished, switch to inert gas helium purge cracking chamber and cold-trap 0.5min-1min, to replace residual reaction gas;
C. cold-trap intensification condition: from-40 ℃ to-120 ℃ with 12 ℃ of .s
-1Rise to 260 ℃ and keep 1min, again with 10 ℃ of .s
-1Rise to 300 ℃ or 350 ℃, keep 3min or 5min;
D.GC/MS analysis condition: HP-INNOWAX post; Specification: 30m * 0.25mm * 0.25 μ m; The gas phase heating gradient: 40 ℃ keep 3min or 50 ℃ of maintenance 1min; Rise to 120 ℃ or 220 ℃ with 8 ℃/min, keep 5min, rise to 200 ℃ or rise to 240 ℃ with 10 ℃/min and keep 5min or with 8 ℃/min again with 20 ℃ of .min
-1Rise to 280 ℃ and keep 5min then; Mass ion source temperature: 230 ℃; Transmission line temperature: 240 ℃ or 280 ℃; Quadrupole rod temperature: 150 ℃;
Or: HP-5MS post, specification: 30m * 0.25mm * 0.25 μ m; The gas phase heating gradient: 50 ℃ keep 1min, with 8 ℃ of .min
-1Rise to 220 ℃, again with 20 ℃ of .min
-1Rise to 280 ℃ and keep 5min; The mass ion source temperature: 230 ℃, the transmission line temperature: 280 ℃, quadrupole rod temperature: 150 ℃.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103698456A (en) * | 2013-12-24 | 2014-04-02 | 上海烟草集团有限责任公司 | Online detection method for pyrolysis gas-phase components of tobacco additive or tobacco material |
| CN104950065A (en) * | 2015-07-21 | 2015-09-30 | 云南中烟工业有限责任公司 | Full smoke trapping and online analysis device and method |
| CN106950147A (en) * | 2017-05-04 | 2017-07-14 | 中国石油大学(华东) | The micro evaluating apparatus and method of a kind of heavy oil catalytic pyrolysis performance |
| CN107121352A (en) * | 2017-05-04 | 2017-09-01 | 中国石油大学(华东) | The micro evaluating apparatus and method of a kind of thermal cracking of heavy oil performance |
| CN107422051A (en) * | 2017-05-26 | 2017-12-01 | 上海烟草集团有限责任公司 | A kind of method that gas phase composition is cracked under on-line checking tobacco additive agent or smoking material different temperatures |
| CN107449833A (en) * | 2016-05-31 | 2017-12-08 | 中国科学院青岛生物能源与过程研究所 | A kind of method for detecting microalgae volatile oil component |
| CN111707774A (en) * | 2020-07-16 | 2020-09-25 | 中国检验检疫科学研究院 | Method for detecting volatile compounds in tobacco |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103698456A (en) * | 2013-12-24 | 2014-04-02 | 上海烟草集团有限责任公司 | Online detection method for pyrolysis gas-phase components of tobacco additive or tobacco material |
| CN103698456B (en) * | 2013-12-24 | 2015-07-15 | 上海烟草集团有限责任公司 | Online detection method for pyrolysis gas-phase components of tobacco additive or tobacco material |
| CN104950065A (en) * | 2015-07-21 | 2015-09-30 | 云南中烟工业有限责任公司 | Full smoke trapping and online analysis device and method |
| CN107449833A (en) * | 2016-05-31 | 2017-12-08 | 中国科学院青岛生物能源与过程研究所 | A kind of method for detecting microalgae volatile oil component |
| CN106950147A (en) * | 2017-05-04 | 2017-07-14 | 中国石油大学(华东) | The micro evaluating apparatus and method of a kind of heavy oil catalytic pyrolysis performance |
| CN107121352A (en) * | 2017-05-04 | 2017-09-01 | 中国石油大学(华东) | The micro evaluating apparatus and method of a kind of thermal cracking of heavy oil performance |
| CN107121352B (en) * | 2017-05-04 | 2020-12-08 | 中国石油大学(华东) | Trace evaluation device and method for thermal cracking performance of heavy oil |
| CN107422051A (en) * | 2017-05-26 | 2017-12-01 | 上海烟草集团有限责任公司 | A kind of method that gas phase composition is cracked under on-line checking tobacco additive agent or smoking material different temperatures |
| CN107422051B (en) * | 2017-05-26 | 2020-08-11 | 上海烟草集团有限责任公司 | Method for on-line detection of pyrolysis gas-phase components of tobacco additive or tobacco material at different temperatures |
| CN111707774A (en) * | 2020-07-16 | 2020-09-25 | 中国检验检疫科学研究院 | Method for detecting volatile compounds in tobacco |
| CN111707774B (en) * | 2020-07-16 | 2023-05-12 | 中国检验检疫科学研究院 | Method for detecting volatile compounds in tobacco |
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Application publication date: 20121017 |