CN107328873A - A kind of tobacco of dynamic pin trapping gas chromatography combined with mass spectrometry causes fragrant analysis of components method - Google Patents
A kind of tobacco of dynamic pin trapping gas chromatography combined with mass spectrometry causes fragrant analysis of components method Download PDFInfo
- Publication number
- CN107328873A CN107328873A CN201710479353.8A CN201710479353A CN107328873A CN 107328873 A CN107328873 A CN 107328873A CN 201710479353 A CN201710479353 A CN 201710479353A CN 107328873 A CN107328873 A CN 107328873A
- Authority
- CN
- China
- Prior art keywords
- dynamic
- pin
- trapping
- sample
- tobacco
- 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.)
- Pending
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
- G01N30/02—Column 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/08—Preparation using an enricher
-
- 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
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
Abstract
Fragrant analysis of components method is caused the invention discloses a kind of tobacco of dynamic pin trapping gas chromatography combined with mass spectrometry, after being connected with headspace sample bottle of the dynamic trapping pin insertion equipped with cigarette shreds sample of cycle purge device, ON cycle blow device is simultaneously heated to sample bottle, heated at 90 DEG C after 30min, by dynamic trapping pin insertion injection port desorption, analyzed after desorbing 5min by GC MS.The present invention is greatly improved bioaccumulation efficiency to small molecule fragrance ingredient, by continuously being purged to sample, volatile component in sample is purged out, using the dynamic trapping pin trapping adsorption sampling for being filled with adsorbent, detector is entered after desorption and is analyzed, can enriched with trace component, it is salable after absorption to preserve, accessory substance is few in adsorption process, simple to operate, has the advantages that sensitivity is high, adsorption range is wide, favorable reproducibility, easy to operate.Because dynamic trapping pin is can to fill the dynamic trapping pin of different adsorbents, analysis object will not be produced and discriminate against effect, dynamic trapping pin is reproducible.
Description
Technical field
Closed cycle is dynamically trapped into pin and gas chromatograph-mass spectrometer the present invention relates to one kind（GC-MS）Associated with analyze
Method.
Background technology
The chemical analysis of tobacco is sufficiently complex, wherein the principal element of influence quality of tobacco depends on causing the species of fragrant composition
With content, therefore, the research of fragrant composition is caused to also result in extensive concern to tobacco leaf.Tradition determines the method master that tobacco causes fragrant composition
There is SPME（SPME）, Simultaneous distillation-extraction（SDE）, the method such as solvent extraction.SDE reappearance preferably, but extracts
Take the time longer, and accessory substance is easily produced under high temperature；SPME, can be with extracting and enriching tobacco leaf as a kind of passive sampling technology
The fragrant composition of main cause, without solvent, but SPME extracting fibers are easily damaged, and it is higher that coating easily peels off cost；In addition,
SPME is limited by coating, and analysis sample is produced and discriminates against effect.
The content of the invention
The present invention provides a kind of tobacco of dynamic pin trapping-gas chromatography-mass spectrography and causes fragrant analysis of components method, to solve
The problem of certainly prior art is present.
The present invention is realized by following technique measures：
After being connected with headspace sample bottle of the dynamic trapping pin insertion equipped with cigarette shreds sample of cycle purge device, open
Cycle purge device is simultaneously heated to sample bottle, is filled with adsorbent in the dynamic trapping pin, 30min is heated at 90 DEG C
Afterwards, dynamic trapping pin insertion GC-MS injection ports are desorbed, after desorption 5min, passes through GC-MS qualitative analyses；
The GC/MS analyzes condition determination：
Chromatographic column：HP-5 capillary columns（30m×0.25mm×0.25μm）；Carrier gas：High-purity He；Flow velocity：1.0mL/min, sample introduction
Mouth temperature：250 DEG C, sample introduction pattern：Do not shunt；Temperature programming：40℃（5min） →170℃（5min）→210℃（60min）；
Ion gun：EI；Electron energy：70eV；Ion source temperature：230℃；Transmission line temperature：220℃；Mass analyzer：Level Four bar；
Scan pattern：SCAN.
The technological progress that the present invention is obtained：
Dynamic trapping pin be it is a kind of can the different adsorbents of self-service selection capturing device, by cycle purge device by cigarette shreds
After volatile materials " blowing " comes out in sample, adsorbed by adsorbent in dynamically trapping pin, then by dynamic trapping pin insertion GC-MS
Injection port carries out hand sampling, finally carries out sample analysis, compared with existing analysis method, the inventive method has following excellent
Gesture：1st, because the present invention is using nonequilibrium state, continuous adsorption process, especially to small molecule fragrance ingredient, it is greatly improved
The bioaccumulation efficiency of sample, by continuously being purged to sample, volatile component in sample is purged out, using being filled with
The dynamic trapping pin of Carboxen1000 adsorbents（Needle trap,NT）Adsorption sampling is trapped, into detector point after desorption
Analysis, can enriched with trace component, have the advantages that sensitivity is high, adsorption range is wide, favorable reproducibility, easy to operate.2nd, because dynamic is caught
Collection pin is can to fill the dynamic trapping pin of different adsorbents, analysis object will not be produced and discriminate against effect；3rd, using dynamic trapping
Pin is reproducible.From the following table 1, it can be seen that the RSD of the peak area of 6 parallel analysis there are 10 kinds less than 5%, important cause is accounted for fragrant
The 50% of composition；Only a kind of more than 10%, illustrates the repeatability of dynamic trapping pin preferably.4th, dynamic trapping pin can enriched with trace
Component, it is salable after absorption to preserve；Accessory substance is few in adsorption process, simple to operate, lasts a long time.
Brief description of the drawings
Fig. 1 is sealing and circulating blow device structural representation.
Fig. 2 is dynamic trapping needle construction schematic diagram.
Embodiment
The present invention is described in further detail with reference to accompanying drawing.As shown in Figure 1 and Figure 2,0.5g pipe tobaccos are placed in headspace sample first
Bottle 3 in, afterwards access sealing and circulating blow device, sealing and circulating blow device include peristaltic pump 5 and by air delivering pipeline 4 with it is compacted
The connected scavenging conduit 2 of dynamic pump 5, dynamic trapping pin 6 is inserted in ml headspace bottle 3, opens heater 1 in headspace sample bottle 3
Tobacco sample 7 is heated, while opening peristaltic pump 5, the air-flow velocity of peristaltic pump 5 is set as into 20mL/min, at 90 DEG C
Under laser heating 30min states, the air-flow that peristaltic pump 5 is exported is passed through tobacco sample 7 by cigarette through air delivering pipeline 4, scavenging conduit 2 successively
Fragrant composition blowout is caused in silk, the adsorbent that the fragrant composition of cause continuously blown out is filled in dynamic trapping pin 6 is constantly adsorbed, and is passed through
An air-flow part after adsorbent absorption flows out through the side opening 8 on the dynamic trapping needle body of pin 6, and other parts return to wriggling by the road
The entrance of pump 5 is circulated, and blocks the syringe needle and backshank of dynamic trapping pin 6 after absorption 30min with plastic plug, and slip cap is caught mounted in dynamic
Collect the sliding block on pin 6 to block the side opening 8 on dynamic trapping pin 6.The plastic plug at the top of dynamic trapping pin 6 is extracted during sample introduction, it is sliding
Side opening 8 is together stretched into GC-MS injection ports and desorbed by movable slider, and qualitative analysis is carried out by GC-MS after desorption 5min.
GC/MS analyzes condition determination：
Chromatographic column：HP-5 capillary columns（30m×0.25mm×0.25μm）；Carrier gas：High-purity He；Flow velocity：1.0mL/min, sample introduction
Mouth temperature：250 DEG C, sample introduction pattern：Do not shunt；Temperature programming：40℃（5min） →170℃（5min）→210℃（60min）；
Ion gun：EI；Electron energy：70eV；Ion source temperature：230℃；Transmission line temperature：220℃；Mass analyzer：Level Four bar；
Scan pattern：SCAN.Measurement result such as table 1 below：
The GC-MS measurement results of the main fragrant composition of cause in the pipe tobacco of table 1（n=6）
Claims (1)
1. a kind of tobacco of dynamic pin trapping-gas chromatography-mass spectrography causes fragrant analysis of components method, it is characterised in that will connect
After having in headspace sample bottle of the dynamic trapping pin insertion equipped with cigarette shreds sample of cycle purge device, ON cycle purging dress
Put and sample bottle is heated, be filled with adsorbent in the dynamic trapping pin, heated at 90 DEG C after 30min, will dynamic
Trapping pin insertion GC-MS injection ports are desorbed, and after desorption 5min, pass through GC-MS qualitative analyses；
The GC/MS analyzes condition determination：
Chromatographic column：HP-5 capillary columns（30m×0.25mm×0.25μm）；Carrier gas：High-purity He；Flow velocity：1.0mL/min, sample introduction
Mouth temperature：250 DEG C, sample introduction pattern：Do not shunt；Temperature programming：40℃（5min） →170℃（5min）→210℃（60min）；
Ion gun：EI；Electron energy：70eV；Ion source temperature：230℃；Transmission line temperature：220℃；Mass analyzer：Level Four bar；
Scan pattern：SCAN.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710479353.8A CN107328873A (en) | 2017-06-22 | 2017-06-22 | A kind of tobacco of dynamic pin trapping gas chromatography combined with mass spectrometry causes fragrant analysis of components method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710479353.8A CN107328873A (en) | 2017-06-22 | 2017-06-22 | A kind of tobacco of dynamic pin trapping gas chromatography combined with mass spectrometry causes fragrant analysis of components method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107328873A true CN107328873A (en) | 2017-11-07 |
Family
ID=60194632
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710479353.8A Pending CN107328873A (en) | 2017-06-22 | 2017-06-22 | A kind of tobacco of dynamic pin trapping gas chromatography combined with mass spectrometry causes fragrant analysis of components method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107328873A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108355378A (en) * | 2018-02-08 | 2018-08-03 | 云南警官学院 | A kind of head space microcirculation solid-phase micro-extracting device |
| CN110412183A (en) * | 2019-09-05 | 2019-11-05 | 中国科学院新疆生态与地理研究所 | A kind of needle trapping-gas chromatography-mass spectrography is to rose aroma analysis of components method |
| CN113777201A (en) * | 2021-09-13 | 2021-12-10 | 上海烟草集团有限责任公司 | Method for analyzing aroma components in tobacco |
| CN115201371A (en) * | 2022-07-12 | 2022-10-18 | 榆林学院 | Aromatic plant aroma component detection method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104713965A (en) * | 2015-03-17 | 2015-06-17 | 上海烟草集团有限责任公司 | Method for extracting tobacco volatile and semi-volatile aroma components |
| CN105784862A (en) * | 2016-03-09 | 2016-07-20 | 上海烟草集团有限责任公司 | Analysis method for volatile and semi-volatile components in tobacco |
-
2017
- 2017-06-22 CN CN201710479353.8A patent/CN107328873A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104713965A (en) * | 2015-03-17 | 2015-06-17 | 上海烟草集团有限责任公司 | Method for extracting tobacco volatile and semi-volatile aroma components |
| CN105784862A (en) * | 2016-03-09 | 2016-07-20 | 上海烟草集团有限责任公司 | Analysis method for volatile and semi-volatile components in tobacco |
Non-Patent Citations (5)
| Title |
|---|
| 吴恒等: "Needle trap-GC-MS法分析云南不同产地薄荷的挥发性成分", 《云南大学学报(自然科学版)》 * |
| 张丽等: "吹扫捕集-气相色谱/质谱法分析卷烟烟丝的嗅香成分", 《烟草科技》 * |
| 李想，陈建民: "新型动态针捕集阱技术分析大气中低浓度的VOCs", 《环境科学》 * |
| 覃光炯等: "静态顶空-气质联用法分析烤烟中香味物质", 《广州化工》 * |
| 高松等: "闭路循环动态针捕集-气相色谱法分析地下水中的硝基苯和苯胺", 《分析化学》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108355378A (en) * | 2018-02-08 | 2018-08-03 | 云南警官学院 | A kind of head space microcirculation solid-phase micro-extracting device |
| CN110412183A (en) * | 2019-09-05 | 2019-11-05 | 中国科学院新疆生态与地理研究所 | A kind of needle trapping-gas chromatography-mass spectrography is to rose aroma analysis of components method |
| CN110412183B (en) * | 2019-09-05 | 2022-04-15 | 中国科学院新疆生态与地理研究所 | Rose fragrance component analysis method by needle capture-gas chromatography-mass spectrometry |
| CN113777201A (en) * | 2021-09-13 | 2021-12-10 | 上海烟草集团有限责任公司 | Method for analyzing aroma components in tobacco |
| CN115201371A (en) * | 2022-07-12 | 2022-10-18 | 榆林学院 | Aromatic plant aroma component detection method |
| CN115201371B (en) * | 2022-07-12 | 2024-03-19 | 榆林学院 | Method for detecting aroma components of aromatic plants |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107328873A (en) | A kind of tobacco of dynamic pin trapping gas chromatography combined with mass spectrometry causes fragrant analysis of components method | |
| CN104569228B (en) | A kind of sampling device | |
| CN101949906B (en) | Decompressed purge-and-trap processing equipment for non-volatile organic compound in water sample and processing method thereof | |
| CN104950065B (en) | A kind of whole smoke trapping and on-line analysis apparatus and method | |
| CN103364484B (en) | A kind of cigarette mainstream flue gas on-line analysis device and method | |
| CN105784862B (en) | One grow tobacco it is middle volatilization and half volatile ingredient analysis method | |
| CN102175796B (en) | Dynamic headspace-cold focusing-GC (Gas Chromatography)-MS (Mass Spectrometer) tobacco headspace element analysis method | |
| CN107703246A (en) | A kind of electronics tobacco tar analysis of components method of dynamic pin trapping gas chromatography combined with mass spectrometry | |
| CN108645940A (en) | A kind of tobacco flavor ingredient extracting process | |
| CN104049050B (en) | A kind of assay method based on benzo [a] pyrene in the cigarette mainstream flue gas of Magnetic solid phases extraction | |
| CN104713959A (en) | On-line real-time analysis method for tobacco smoke | |
| CN104716001B (en) | A kind of liquid continuous sample introduction device of heating and gasifying | |
| CN204789503U (en) | Full flue gas entrapment and online analysis device | |
| CN108593816B (en) | Method for improving purging efficiency of volatile components in tobacco | |
| CN106501438A (en) | For analyzing analytical equipment and the analysis method of tobacco juice composition | |
| CN204302250U (en) | A kind of sampling device | |
| CN208297430U (en) | A kind of secondary parsing thermal desorption device of binary channels | |
| CN116465996A (en) | Analysis method and application of main stream smoke components of cigarettes | |
| CN206411077U (en) | Analytical equipment for analyzing tobacco juice composition | |
| CN109342618A (en) | A kind of automation pre-processing device for VOCs in gas chromatographic detection material | |
| CN113777201A (en) | Method for analyzing aroma components in tobacco | |
| CN213275046U (en) | Flue gas trapping device | |
| CN104266881B (en) | Linear pattern smoking machine capturing device and its analysis test method with adsorption tube | |
| CN113970600A (en) | On-line analysis and detection device and method for smoke of heated cigarette | |
| CN107144450B (en) | Cigarette holder suitable for rotary disc type smoking machine and provided with adsorption cavity and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20171107 |