CN101871922B - Method for pyrolyzing tobacco additive and trapping and analyzing pyrolysis product - Google Patents
Method for pyrolyzing tobacco additive and trapping and analyzing pyrolysis product Download PDFInfo
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Abstract
The invention relates to a method for pyrolyzing a tobacco additive and trapping and analyzing a pyrolysis product, and belongs to the technical field of detection of the tobacco additive. The method comprises the following steps of: putting an additive sample into a pyrolysis tube of a pyrolyzer, introducing nitrogen-oxygen mixed gas serving as pyrolysis reaction gas into the pyrolyzer, controlling different pyrolysis temperatures and pyrolysis time by using a heating wire and performing pyrolysis on the additive, continuously blowing the pyrolysis product into an on-line adsorption trap in the pyrolysis process by using the pyrolysis reaction gas and making the pyrolysis product adsorbed by the adsorption trap, heating the adsorption trap to desorb the adsorbed pyrolysis product after the pyrolysis is finished, and feeding the desorbed product into a gas chromatograph-mass spectrometer by using inert gas and analyzing the product. The method has the advantages of realizing on-line entrapment and sample introduction of the pyrolysis product of the additive under the condition of aerobic pyrolysis, and providing more scientific and comprehensive analysis data and theoretical support for availability screening of the tobacco additive, particularly for safety evaluation because the pyrolysis result proves that the simulation of the process of the additive when a cigarette is burned and adsorbed is available.
Description
Technical field:
The present invention relates to the capture and the analytical approach of a kind of cigarette additive thermal cracking and product thereof, belong to cigarette additive detection technique field.
Background technology:
In the production of cigarettes process, needing to add cigarette additive is used for improving, stablizes and promote cigarette or its product property or give the cigarette product specific style.Along with, the whole society is to the attention of food additives security, and smoking and healthy care, and the availability of assessment cigarette additive and the work of security just seem extremely important.Cigarette additive will be participated in burning because of it, thereby pyrolysis technology becomes requisite means.The tobacco researcher has carried out big quantity research to cleavage method (comprising cracking equipment etc.), with the relation of discussion tobacco additive agent and smoke components (especially objectionable constituent), thereby adjuvant is assessed and is screened, and representative work is summarized as follows.
Peng Xinhui etc.
[1]Utilize the method for the built-in crack tank of muffle furnace to design a kind of high temperature carbonization thermal cracker under the inert atmosphere, the pyrolysis product of adjuvant etc. is used sample introduction analysis after the solvent absorbing that places cold-trap, Zhang Duntie etc.
[2]Adopt high temp. salt melting method self-control cracker, pyrolysis product is used methylene chloride and is absorbed back sample introduction analysis, Li Shengqun etc.
[3]Adopt bottled gas, the tubular heater that has temperature controller, cambridge filter drip catcher and gas collection bag (or solvent absorbing bottle) etc. to constitute the multifunctional off-line thermal cracker; The multi-form adjuvant pyrolysis product of collecting is analyzed respectively, and can be realized the thermal cracking under the aerobic state.Above-mentioned cracking mode does not have commercialization because of equipment, and all there is query in the maximum temperature that heating rate maybe can reach etc., seldom is applied to the Study on Cleavage of tobacco additive agent at present.
Gu Yueling
[4-5]Deng the application Curie point pyrolyzer hesperidin, trisodium glycyrrhetinate have been carried out Study on Cleavage, this mode has the characteristics of cracking quick heating, but because of its maximum temperature is limited by the ferrimagnet that is adopted, current application is less.Wu Yiqin
[6,7, permitted forever
[8,9], Qin Yunhua
[10]Deng application tube furnace pyrolyzer (Australian SGE Pyrojector I of company or II) cigarette additives such as 4-oxo-beta-damascenone, black tonka-bean tincture, Hang Zhou chrysanthemum flower extract, clove bud oil, balloonflower root medicinal extract have been carried out cracking; Inert carrier gas in the cracking process (simultaneously as cracking reaction gas) continues to flow, and pyrolysis product gets into gas chromatographic column with carrier gas to be separated.This kind cracking mode temperature-controlled precision that research is chosen is high; Be applicable to all kinds and more a large amount of samples, but this mode can not realize the temperature programme cracking of sample, and secondary reaction is outstanding; Only can carry out the thermal cracking under the inert atmosphere, the atmosphere of the Actual combustion of propping up with cigarette there are differences.
Along with heating up fast, cracking temperature is adjustable continuously, and control accuracy is high, filament pyrolyzer's commercialization of cracking favorable reproducibility, and such cracker becomes the main flow that current cigarette additive thermal cracking is used.Song Yubing
[11], Lu Binbin
[12]Under atmosphere of inert gases, essence and flavoring agent is carried out cracking Deng using filament pyrolyzer (Pyroprobe of U.S. CDS company 2000), so that its effect is estimated, thereby reach the purpose of screening adjuvant, and applied for patent.Same this type work also is under inert atmosphere, to carry out, and the atmosphere that props up burning with cigarette there are differences.
Hou Ying, Yang Yan, Chen Yongkuan
[13-16]Deng employing filament pyrolyzer (Pyroprobe of U.S. CDS company 2000); And design voluntarily the cracking reaction chamber use simultaneously solid phase micro-extraction technique to pyrolysis product extract, the sample introduction analysis; To xenthophylls, fig medicinal extract, polyhydroxy pyrazine, 2; 3-dihydro-3,5-dihydroxy-6-methyl-4 (H) pyrans-4-ketone, rutin etc. have carried out the thermal cracking research under the aerobic state.But because of the solid-phase micro extraction capacity is limit, there is defective for the total analysis of pyrolysis product, and the cracking reaction chamber of design voluntarily, its atmosphere is pre-set, gas does not flow when cracking reaction, is not inconsistent with actual cigarette smoking state.
Kong Haohui etc.
[17]Use the filament pyrolyzer; Cracking reaction gas is used oxygen concentration and is higher than 20% nitrogen oxygen atmosphere; The absorption of on-line adsorption trap is carried out the cracking experiment to tobacco, has realized that aerobic cracking and online product capture; But exist differently with object, atmosphere and gas flow rate etc. that the present invention uses, and the result of the method that provides does not carry out data with full smoke components and content analysis and compares.
To sum up, prior art extensive work aspect the thermal cracking of cigarette additive carries out based on inert atmosphere, because of cigarette additive is participated in burning in cigarette props up; The thermograde of its experience is very wide in range; The rate of heat addition is high, and the difference oxygen levels there are differences, and above-mentioned test is because of the restriction of instrument and equipment etc.; As can not carry out the alternating temperature thermal cracking that the aerobic cracking maybe can not be carried out temperature programme; Thereby design and the adjustment that thermal cracking condition and cracking reaction gas carry out do not reached optimum, the result who makes cigarette additive thermal cracking analysis result and its experience cigarette Zhi Shiji burn and suck generation there are differences, and can not compare with the result that smoke chemistry is studied.And current tobacco business is when estimating the tobacco additive agent security; Clearly must carry out the thermal cracking research of adjuvant; Thereby the experiment condition of thermal cracking must at utmost simulate the internal environment of cigarette combustion zone, could improve the availability of cigarette additive thermal cracking result data.
List of references:
[1] Peng Xinhui, Yi Jianhua, Zhao Yu. a kind of high temperature carbonization thermal cracker, utility model patent Granted publication instructions, CN200620050769.5
[2] Zhang Duntie, Yin Faqiang, He Jiawen. the thermal cracking research of three kinds of Amadori compounds, Chinese tobacco journal, 2006,12 (2): 13-16
[3] Li Sheng crowd Wang Yi meets ripple etc. slowly. multifunctional off-line thermal cracker utility model patent Granted publication instructions, 200820239371.5
[4] Gu Yueling, the cracking GC/MS of hesperidin analyzes, mass spectrum journal, 1998,19 (2): 79-80
[5] Gu Yueling, Hu Gengyuan, Chen Yongkuan, the cracking of trisodium glycyrrhetinate/GC/MS analyzes [J], mass spectrum journal, 1995,16 (4): 76-78
[6] Wu Yiqin, willow, Liu Fang etc. the thermal cracking behavior [J] of online pyrolysis gas chromatograph/mass spectrometry method research 4-oxo-beta-damascenone. chromatogram, 2007,3:408～412
[7] Wu Yiqin, willow, Meng Zhaoyu etc. the thermal cracking behavior [J] of the black tonka-bean tincture of pyrolysis gas chromatograph one mass spectrometric hyphenated technique research. assay office, 2008,1:80～83
[8] permitted forever, Xiang Nengjun, high alizarin. the GC/MS of Hang Zhou chrysanthemum flower extract thermal cracking products analyzes [J]. fine chemistry industry, 2008,8:766～770
[9] permitted forever Xiang Nengjun, Wu Yiqin etc., the thermal cracking behavior of thermal cracking gas chromatography one mass spectrometry method research clove bud oil, physical and chemical inspection-chemical fascicle, 2008 (44): 969-971
[10] Qin Yunhua, Xiang Nengjun, Xu Yong etc., pyrolysis gas chromatograph-mass spectrometry method is to the thermal cracking products analysis of balloonflower root medicinal extract, physical and chemical inspection-chemical fascicle, 2008 (44): 1038-1041
[11] Song Yubing, Li Peng, Zong Yongli, Li Yanqiang, Sun Shihao. based on the cigarette of thermal cracking-gas chromatograph mass spectrometric hyphenated technique with perfume material screening technique application number 200810140820.5
[12] Lu Binbin, Zong Yongli. adopt the method application number 200810141443.7 of pyrolysis experiment assessment perfume monomer to the cigarette effect
[13] Hou Ying, Xu Jicang, Wang Baoxing etc. the pyrolysis product analysis [J] of xenthophylls. tobacco chemistry, 2007,12:27～32
[14] 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
[15] 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
[16] 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
[17] Kong Haohui. tobacco pyrolytic cracking analytical method application number 200810026374.5
[18]I.Schmeltz，A.Wenger，D.Hoffmann，T.C.Tso，J.Agric.Food?Chem.27(1979)602-608.
[19]N.A.Stevens，M.F.Borgerding，Anal.Chem.71(1999)2179-2185.
[20]R.W.Jenkins?Jr.，R.H.Newman，M.K.Chavis，Beitr.Tabakforsch.5(1970)299-301.
[21]J.D.Green，J.Chalmers，P.J.Kinnard，Beitr.Tabakforsch.Int.14(1989)283-288.
[22]S.J.Stotesbury，L.J.Willoughby，A.Couch，Beitr.Tabakforsch.Int.19(2000)55-64.
[23]S.A.Eble，in：Proceedings?of?the?International?Conference?on?the?Physical?and?Chemical?Processes?Occurring?in?a?Burning?Cigarette，R.J.Reynolds?Tobacco?Co.，Winston-Salem，NC，USA，1987，pp.261-279.
Summary of the invention:
The objective of the invention is to overcome the deficiency of prior art, and the capture and the analytical approach of a kind of cigarette additive thermal cracking and product thereof are provided.
The present invention adopts filament pyrolyzer's temperature programme cracking pattern; On current research work basis; Further optimize cracking and product and capture analysis condition; The cracking result has carried out comparative analysis through the result with isotope-labeled smoke chemistry research, and the result is more consistent, is the method that can better simulate the actual aspiration procedure of cigarette.
Method of the present invention is: cigarette additive sample application CDS 5200 type thermal cracking appearance carry out cracking, and the reaction atmosphere of cracking is nitrogen oxygen mixed gas (volume ratio is 91: 9), and the flow of mixed gas is at 40-260mLmin
-1Set in the scope, with the different cracking temperature of heating wire control and cracking time to adjuvant carry out cracking (300 ℃ and keep 5S, from 300 ℃ with 30 ℃ of S
-1Rise to 900 ℃ and keep 5S), pyrolysis product is used the cracking reaction air-blowing and is swept to the on-line adsorption trap and is adsorbed at a lower temperature, after cracking is accomplished; Switch to inert gas purge cracking bar and adsorption trap certain hour; To replace residual reaction gas, set the adsorption trap heating schedule thereafter, with pyrolysis product desorption (275 ℃ of the desorption temperatures of absorption; Desorption time 2min), the desorption product is used inert gas and is brought gas chromatograph-mass spectrometer analysis into.
The invention has the advantages that: for simulating the cigarette burning situation conscientiously; Under aerobic cracking situation; Realized online capture of pyrolysis product and sample introduction, cracking is through comparing with the smoke chemistry analysis result, prove its simulation adjuvant cigarette prop up when burning and sucking the course of process be effective; Thereby, cigarette additive availability screening, especially safety evaluatio support with theoretical for providing more scientific comprehensive analysis data.
Embodiment:
One, experimental section
1. instrument and reagent
CDS5200 thermal cracking appearance (U.S. CDS company); GC6890N/5975 gas chromatography appearance, ADM1000 current meter (U.S. Anjelen Sci. & Tech. Inc); AG204 analytical balance (sensibility reciprocal 0.0001g, Switzerland METTLER TOLEDO company), helium, oxygen, nitrogen; Chromatographically pure ethanol, chromatographically pure methylene chloride, chromatographically pure normal hexane; The residual level of farming glass wool; The cigarette additive sample.
2. the preparation of cigarette additive sample:
Accurately take by weighing the cigarette additive sample of a certain amount of (20-200mg), use ethanol (or methylene chloride or normal hexane) dissolving, constant volume, subsequent use.One of the special-purpose crystalline silica cracking tube of heat-obtaining cracking appearance is packed into the residual level of farming glass wool some (1-2mg) in the middle, accurately draws a certain amount of sample solution with the micro-sampling pin.Be injected on the silica wool of being filled.Inadequate for additive samples that is not dissolved in above-mentioned solvent or existence dissolving, adopt direct weighing method (2-5mg), promptly, after weighing finishes, fill silica wool at opposite side cracking quartz ampoule one side elder generation filling silica wool.The cracking quartz ampoule that fills sample is inserted the cracking appearance, treat cracking.
3. experimental procedure
The thermal cracking condition:
Initial temperature: 300 ℃ and keep 5S, from 300 ℃ with 30 ℃ of S
-1Rise to 900 ℃ and keep 5S, the cracking atmosphere is that 9% oxygen is in nitrogen.
The GC/MS analysis condition:
The HP-5MS post, injector temperature: 240 ℃, heating gradient: 40 ℃ keep 1min, with 8 ℃ of min
-1Rise to 220 ℃, with 20 ℃ of min
-1Rise to 280 ℃ and keep 5min then.Mass spectrum transmission line temperature: 280 ℃; Ion source temperature: 220 ℃, the solvent delay time is 3.5min.
Pyrolysis product captures and sample introduction:
Pyrolysis product is used the cracking reaction air-blowing and is swept to that to contain solid adsorption material, initial temperature be in 50 ℃ the adsorption trap, and after cracking was accomplished, heating adsorption trap to 275 ℃ kept 2.0min, accomplishes the desorption sample introduction
Two, result and discussion
1. condition optimizing
1.1 cracking condition is selected
Because of different cracking conditions will produce different cracking results; Therefore through comparing with isotope-labeled smoke chemistry result of study; Report in conjunction with aforementioned documents; Heating schedule, heating rate and different temperatures section (point) retention time and the cracked gas atmosphere of adjustment cracking silk through a plurality of standard model tests, have comprehensively been confirmed preferable cracking heating schedule.That is: 300 ℃ of cracking silk initial temperature and keep 5S, from 300 ℃ with 30 ℃ of S
-1Rise to 900 ℃ and keep 5S, the cracking atmosphere is that 9% oxygen is in nitrogen.
1.2 reaction gas flow velocity:
Use conduct investigation objects such as nicotine, under different reaction gas flow velocitys, the condition of application 1 .1 is carried out breaking test, and peak area normalization percentage composition (%) result of gained thermal cracking products sees table 1:
The peak area normalization percentage composition of nicotine pyrolysis product under the different pyrolysis gas flow velocitys of table 1
Can find out by The above results, at 40-260mLmin
-1In the reaction gas flow velocity scope, the analysis result of pyrolysis product is approaching.
Table 2 is listed other several kinds of standard substances its primary product of cracking (being standard substance self) peak area normalization percentage composition under the differential responses gas velocity, also can find out at 40-260mLmin from the cracking result
-1The analysis result of pyrolysis product is approaching in the reaction gas flow velocity scope.
Several kinds of its primary products of standard substance cracking (standard substance self) peak area normalization percentage composition under the table 2 differential responses gas velocity
1.3 method validation
Table 3 has been listed part of standards material cracking result with the comparison that flue gas isotope labeling result of study is arranged; Can find out from table 3; The pyrolysis product analysis result that the applied a whole set of method of the present invention obtains with flue gas isotope analysis result near (the isotope labeling research document of being quoted see reference document [18-23]); The method that reflects has been simulated cigarette preferably and has been burnt and sucked environment, has improved the availability of data greatly.
Table 3 standard substance cracking result with flue gas isotope labeling result of study relatively
2. the repeatability of method
Use method of the present invention the phenmethylol standard model is carried out the repetition breaking test six times, the result sees table 4.Can find out that from table 4 the RSD value of six its main pyrolysis product peak areas of cracking of sample is between 1.8%-8.5%, because the limitation of GC/MS method, be lower than total normalized area below 1% for peak area, its RSD value is higher.
Its main pyrolysis product peak area of 6 cracking of table 4 phenmethylol sample and RSD (n=6) value
3. sample analysis result
Use this method, part tobacco additive agent (tobacco additive agent involved in the present invention meets the definition of YC/T 195 to it) has been carried out cracking and product analysis thereof.
Embodiment 1: (the reaction gas flow velocity is set at: 66mLmin for the thermal cracking of certain pure tobacco oil and result thereof
-1), the pyrolysis product analysis result is seen table 5.
The main pyrolysis product peak area of certain pure tobacco oil of table 5 normalization percentage composition
Embodiment 2: (the reaction gas flow velocity is set at: 200mLmin for certain smoked plum extractive thermal cracking and result thereof
-1), the pyrolysis product analysis result is seen table 6.
Certain smoked plum extractive cracking primary product peak area normalization percentage composition of table 6
Claims (1)
1. the capture and the analytical approach of cigarette additive thermal cracking and product thereof; It is characterized in that additive samples is placed thermal cracking appearance cracking tube; The cracking appearance is inserted nitrogen oxygen mixed gas as cracking reaction gas, control different cracking temperature and the cracking time with heating wire adjuvant is carried out cracking, pyrolysis product application cracking reaction gas is continuously blown in the on-line adsorption trap in the cracking process; And be adsorbed; After cracking is accomplished, the pyrolysis product that the heating adsorption trap is adsorbed with desorption, and use inert gas the desorption thing is sent into GC-MS analysis; Wherein:
The volume ratio of said nitrogen oxygen mixed gas is 91: 9, and the flow range of mixed gas is 40-260mLmin
-1
Said cracking temperature and cracking time are initial temperature: 300 ℃ and keep 5S, from 300 ℃ with 30 ℃ of S
-1Rise to 900 ℃ and keep 5S;
The pyrolysis product desorption temperature of said absorption is 275 ℃, and desorption time is 2min.
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| CN102221591B (en) * | 2011-03-21 | 2013-03-20 | 川渝中烟工业有限责任公司 | Method for evaluating adsorption effect of filter tip additive on phenolic compound in smoke |
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