CN106770795B - The method for heating 14 kinds of fragrant and sweet ingredients of coke in non-burning cigarette smoke is measured simultaneously - Google Patents
The method for heating 14 kinds of fragrant and sweet ingredients of coke in non-burning cigarette smoke is measured simultaneously Download PDFInfo
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- CN106770795B CN106770795B CN201710051144.3A CN201710051144A CN106770795B CN 106770795 B CN106770795 B CN 106770795B CN 201710051144 A CN201710051144 A CN 201710051144A CN 106770795 B CN106770795 B CN 106770795B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
Abstract
The invention discloses a kind of methods for measuring heat 14 kinds of fragrant and sweet ingredients of coke in non-burning cigarette smoke simultaneously, include the following steps: after 1) heating non-burning cigarette smoke granule phase substance with cambridge filter trapping, cambridge filter is transferred to extraction vessel, internal standard and aqueous isopropanol is added, concussion extraction is carried out, supernatant is taken to obtain fume sample；2) fume sample is detected using GC-MS, 14 kinds of fragrant and sweet component contents of coke is detected by internal standard quanitation.The present invention uses solvent extraction-combined gas chromatography mass spectrometry, can measure the content for heating 14 kinds of fragrant and sweet ingredients of coke in non-burning cigarette smoke simultaneously, has the advantages that quick detection, high sensitivity, selectivity is good, accuracy is high；The content of burnt fragrant and sweet ingredient non-burning cigarette smoke is heated suitable for measuring.
Description
Technical field
The invention belongs to fragrance component detection technique fields, and in particular to a kind of to measure the non-burning cigarette smoke of heating simultaneously
In 14 kinds of fragrant and sweet ingredients of coke method.
Background technique
Heating non-burning cigarette is a kind of novel tobacco product, contained tobacco-containing material can be promoted non-by heating
The smog sucked for consumer, compared with traditional cigarette, the release of side-stream smoke and part harmful substance are generated under combustion state
It significantly reduces.It heats non-burning cigarette to be released by Reynolds Tobacco Company earliest, although the extensive of market is not yet received in such product
Approve, but due to the lasting increase of global range tobacco control dynamics and its reducing environmental pollution and healthy potential risk of smoking
Clear superiority existing for aspect, international Field of Tobacco think always such product be the development of following tobacco product important directions it
One.
Burnt fragrant and sweet rhythm is one of benign note important in flue gas, has vital influence to flue gas organoleptic quality, by
To the extensive concern of domestic and international tobacco company.Quantitative analysis is carried out to fragrant and sweet ingredient burnt in flue gas, it is special that burnt fragrant and sweet rhythm can be investigated
Levy distributional difference in different type flue gas of key component and each key component, be conducive to refinement to smoke chemistry ingredient with
The understanding of relationship between organoleptic quality can simulate cigarette style and provide to improve flue gas organoleptic quality and new tobacco products
Basic support.The measurement report about fragrant and sweet ingredient burnt in flue gas more existing at present concentrates in traditional cigarette, (Hong Hua
Pretty, Guo Ziming, Yi Ke wait the Neutral Aroma Components of cigarette mainstream flue gas to analyze [J] Agricultural University Of Hunan journal: natural
Scientific version, 2008,34 (2): 164-167；Zou Peng, Shu Junsheng, Guo Dongfeng wait potassium carbonate to neutral in flue-cured tobacco main flume
Influence [J] Chinese tobacco journal of flavor component production quantity, 2014 (3): 16-22.), it heats burnt in non-burning cigarette smoke
The measurement of fragrant and sweet ingredient is not reported then.Meanwhile these measuring methods usually choose common composition such as furfural, furfuryl alcohol etc. in cigarette
Furans are as research object, the big cyclopentenone of many fragrant and sweet contributions burnt for main flume, furanone, pyranone
If ingredient such as maltol, ethylcyclopentenolone etc. without reference to.In pertinent literature the fragrant and sweet ingredient type of coke of detection simultaneously compared with
It is few, therefore, develops a kind of while measuring quick, the sensitive new method for heating a variety of fragrant and sweet ingredients of coke in non-burning cigarette smoke
It is very necessary.
Summary of the invention
The object of the present invention is to provide a kind of quickly detection, high sensitivity, selectivity is good, accuracy is high while measure and add
The method of 14 kinds of fragrant and sweet ingredients of coke in the non-burning cigarette smoke of heat.
The purpose of the present invention is achieved through the following technical solutions:
Method that is a kind of while measuring 14 kinds of fragrant and sweet ingredients of coke in cigarette smoke, the specific steps are as follows:
1) after heating non-burning cigarette smoke granule phase substance with cambridge filter trapping, cambridge filter is transferred to extraction vessel, is added
Enter inner mark solution and isopropanol carries out concussion extraction, supernatant is taken to obtain fume sample；
Styralyl propionate is designated as in described, the amount of inner mark solution used is 10 ~ 100 μ L, and isopropanol used is 10 ~ 100
mL；The time that the concussion is extracted is 20 ~ 40 min.
2) fume sample is detected using GC-MS, 14 kinds of fragrant and sweet component contents of coke is detected by internal standard quanitation.
Chromatographic condition are as follows: chromatographic column: DB-5MS (mm × 0.25 μm 60 m × 0.25)；Carrier gas: He；Column flow: 1
mL/min；Injector temperature: 250 DEG C；Temperature programming: 50 DEG C (1 min), 5 DEG C/min → 160 DEG C (1 min)；Split ratio 2:
1。
Mass Spectrometry Conditions are as follows: GC/MS transmission line temperature: 250 DEG C, EI ion source temperature: 230 DEG C, level four bars temperature: 150
℃；EI ionizing energy: 70 eV；Scan pattern: selection ion scan divides the period according to retention time.
In internal standard quanitation detection, the fragrant and sweet ingredient of 14 kinds of cokes and a kind of internal standard mark are contained in hybrid standard working solution used
Quasi- object, solvent are isopropanol；The concentration of internal standard styralyl propionate is 2 μ g/mL, standard work in all standard working solutions
Make furfural in solution, furfuryl alcohol, 5 methyl furfural, 3- methyl -2- cyclopentene-1-one, methyl cyclopentenyl ketone, ethylcyclopentene alcohol
Ketone, maltol, the concentration magnitude of 4- hydroxyl -2,5- dimethyl -3 (2H) furanone is followed successively by 0.2 from low to high, 0.5,1,2,5,
10,20 μ g/mL, and this 8 kinds of fragrant and sweet constituent concentrations of coke are equal under each concentration magnitude；3- methyl -2 (5H)-furanone, when
The concentration magnitude of lactone is returned to be followed successively by 0.02,0.05,0.1,0.2,0.5,1,2 μ g/mL, and each concentration magnitude from low to high
This lower 2 kinds of fragrant and sweet constituent concentrations of coke are equal；2- cyclopentene-Isosorbide-5-Nitrae-diketone, 3,4- dimethylcyclopentene alcohol ketone, 4- methyl -2
(5H)-furanone, the concentration magnitude of cyclohexanedione are followed successively by 0.04,0.1,0.2,0.4,1,2,4 μ g/mL from low to high；And it is every
This 4 kinds of fragrant and sweet constituent concentrations of coke are equal under one concentration magnitude.
The quantitation curves of 14 kinds of fragrant and sweet ingredients of coke, the range of linearity, detection limit, quantitative limit are as shown in table 2.
The present invention uses solvent extraction-combined gas chromatography mass spectrometry, can measure simultaneously in the non-burning cigarette smoke of heating
The content of 14 kinds of fragrant and sweet ingredients of coke.Have the advantages that quick detection, high sensitivity, selectivity is good, accuracy is high；Extractant is different
The use of propyl alcohol, it is possible to prevente effectively from the aldolisation that the common extractant such as methanol, ethyl alcohol occurs with furfural when in use, is fitted
For measuring the content for heating burnt fragrant and sweet ingredient in non-burning cigarette smoke.
Detailed description of the invention
Fig. 1 is that the SIM of the fragrant and sweet ingredient standard specimen of 14 kinds of cokes schemes；
Fig. 2 is the SIM figure of 14 kinds of fragrant and sweet ingredients of coke in the non-burning cigarette smoke of heating of embodiment 2；
Each chromatographic peak serial number is corresponding with 1 title of table in figure.
Specific embodiment
The present invention is further illustrated With reference to embodiment.
Embodiment 1
The method that 14 kinds of fragrant and sweet ingredients of coke in non-burning cigarette smoke are heated in measurement while the present embodiment, including following step
It is rapid:
1) the non-burning cigarette of the heating of the trade mark 1 is heated according to product operation instruction, with reference to as defined in ISO 3308
Pumping volume and granule phase substance capture method carry out suction and granule phase substance trapping.It is non-burning that 6 heating are trapped with two cambridge filters
After cigarette smoke granule phase substance, cambridge filter is placed in 50 mL stuffed conical flasks and is laid in bottom of bottle, it is molten that 20 μ L internal standard compounds are added
Liquid and 20 mL aqueous isopropanols, vibrate 20min at room temperature, take 2 mL supernatants, obtain fume sample；
2) fume sample obtained by step 1) is detected using GC-MS；
Chromatographic condition are as follows: chromatographic column: DB-5MS (mm × 0.25 μm 60 m × 0.25)；Carrier gas: He；Column flow: 1
mL/min；Injector temperature: 250 DEG C；Temperature programming: 50 DEG C (1 min), 5 DEG C/min → 160 DEG C (1 min)；Split ratio 2:
1。
Mass Spectrometry Conditions are as follows: GC/MS transmission line temperature: 250 DEG C, EI ion source temperature: 230 DEG C, level four bars temperature: 150
℃；EI ionizing energy: 70 eV；Scan pattern: selection ion scan divides the period according to retention time.
Volume of the method to the trade mark 1 of 14 kinds of fragrant and sweet ingredients of coke in non-burning cigarette smoke is heated in measurement while the present embodiment
Cigarette testing result is as shown in table 3.
Embodiment 2
The method that 14 kinds of fragrant and sweet ingredients of coke in non-burning cigarette smoke are heated in measurement while the present embodiment, including following step
It is rapid:
1) the non-burning cigarette of the heating of the trade mark 2 is heated according to product operation instruction, with reference to as defined in ISO 3308
Pumping volume and granule phase substance capture method carry out suction and granule phase substance trapping.It is non-burning that 6 heating are trapped with two cambridge filters
After cigarette smoke granule phase substance, cambridge filter is placed in 50 mL stuffed conical flasks and is laid in bottom of bottle, 30 μ L internal standard compounds are added
Solution and 30 mL aqueous isopropanols, vibrate 25min at room temperature, take 2 mL supernatants, obtain fume sample；
2) fume sample obtained by step 1) is detected using GC-MS；
Chromatographic condition and Mass Spectrometry Conditions are the same as embodiment 1.
Volume of the method to the trade mark 2 of 14 kinds of fragrant and sweet ingredients of coke in non-burning cigarette smoke is heated in measurement while the present embodiment
Cigarette testing result is as shown in table 3.
Embodiment 3
The method that 14 kinds of fragrant and sweet ingredients of coke in non-burning cigarette smoke are heated in measurement while the present embodiment, including following step
It is rapid:
1) the non-burning cigarette of the heating of the trade mark 3 is heated according to product operation instruction, with reference to as defined in ISO 3308
Pumping volume and granule phase substance capture method carry out suction and granule phase substance trapping.It is non-burning that 6 heating are trapped with two cambridge filters
After cigarette smoke granule phase substance, cambridge filter is placed in 50 mL stuffed conical flasks and is laid in bottom of bottle, 50 μ L internal standard compounds are added
Solution and 50 mL aqueous isopropanols, vibrate 30min at room temperature, take 2 mL supernatants, obtain fume sample；
2) fume sample obtained by step 1) is detected using GC-MS；
Chromatographic condition and Mass Spectrometry Conditions are the same as embodiment 1.
Volume of the method to the trade mark 3 of 14 kinds of fragrant and sweet ingredients of coke in non-burning cigarette smoke is heated in measurement while the present embodiment
Cigarette testing result is as shown in table 3.
Embodiment 4
The method that 14 kinds of fragrant and sweet ingredients of coke in non-burning cigarette smoke are heated in measurement while the present embodiment, including following step
It is rapid:
1) the non-burning cigarette of the heating of the trade mark 4 is heated according to product operation instruction, with reference to as defined in ISO 3308
Pumping volume and granule phase substance capture method carry out suction and granule phase substance trapping.It is non-burning that 6 heating are trapped with two cambridge filters
After cigarette smoke granule phase substance, cambridge filter is placed in 50 mL stuffed conical flasks and is laid in bottom of bottle, 70 μ L internal standard compounds are added
Solution and 70 mL aqueous isopropanols, vibrate 40 min at room temperature, take 2 mL supernatants, obtain fume sample；
2) fume sample obtained by step 1) is detected using GC-MS；
Chromatographic condition and Mass Spectrometry Conditions are the same as embodiment 1.
Volume of the method to the trade mark 3 of 14 kinds of fragrant and sweet ingredients of coke in non-burning cigarette smoke is heated in measurement while the present embodiment
Cigarette testing result is as shown in table 3.
Experimental example 5
The non-burning cigarette of the heating of the trade mark 2 is heated according to product operation instruction, is taken out with reference to as defined in ISO 3308
It inhales capacity and granule phase substance capture method carries out suction and granule phase substance trapping.6 heating non-combustion-cigarettes are trapped with two cambridge filters
The Smoke Particulate that fiber tube generates.It is measured according to 2 method of example, is measured in parallel 6 groups, 6 times of 14 kinds of fragrant and sweet ingredients of coke are flat
The RSD value of row measured value (see Table 4) between 4%-10%, it was demonstrated that precision of method of the invention is higher, reproducible.
Claims (3)
1. a kind of measure the method for heating 14 kinds of fragrant and sweet ingredients of coke in non-burning cigarette smoke simultaneously, it is characterised in that: including with
Lower step:
1) after heating non-burning cigarette smoke granule phase substance with cambridge filter trapping, cambridge filter is transferred to extraction vessel, in addition
Mark solution and isopropanol carry out concussion extraction, and supernatant is taken to obtain fume sample；
2) fume sample is detected using GC-MS, 14 kinds of fragrant and sweet component contents of coke is detected by internal standard quanitation, 14 kinds
Burnt fragrant and sweet ingredient is respectively furfural, furfuryl alcohol, angelica lactone, 2- cyclopentene -1,4- diketone, 5 methyl furfural, 3- methyl -2- ring penta
Alkene -1- ketone, 3- methyl -2 (5H)-furanone, cyclohexanedione, methyl cyclopentenyl ketone, 4- methyl -2 (5H)-furanone, 4- hydroxyl
Base -2,5- dimethyl -3 (2H) furanone, 3,4- dimethylcyclopentene alcohol ketone, maltol, ethylcyclopentenolone；
Chromatographic condition are as follows: chromatographic column: mm × 0.25 μm DB-5MS, specification 60 m × 0.25；Carrier gas: He；Column flow: 1 mL/
min；Injector temperature: 250 DEG C；Temperature programming:, keeping 1 min, then rise to 160 DEG C with the rate of 5 DEG C/min by 50 DEG C,
Keep 1 min；Split ratio 2:1；
Mass Spectrometry Conditions are as follows: GC/MS transmission line temperature: 250 DEG C, EI ion source temperature: 230 DEG C, level four bars temperature: 150 DEG C；EI
Ionizing energy: 70 eV；Scan pattern: selection ion scan divides the period according to retention time.
2. method that is according to claim 1 while measuring 14 kinds of fragrant and sweet ingredients of coke in the non-burning cigarette smoke of heating,
It is characterized in that: being designated as styralyl propionate in described, the amount of inner mark solution is 10 ~ 100 μ L, and the concentration of inner mark solution is 2 mg/
mL。
3. method that is according to claim 1 while measuring 14 kinds of fragrant and sweet ingredients of coke in the non-burning cigarette smoke of heating,
Be characterized in that: the time for shaking extraction is 20 ~ 40 min.
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| CN111220741B (en) * | 2020-03-18 | 2022-09-30 | 福建中烟工业有限责任公司 | Method for separating and screening sweet components of scorched sweet flavor in Sanming Yuxi tobacco leaves |
| CN111289657B (en) * | 2020-03-31 | 2022-12-20 | 中国烟草总公司郑州烟草研究院 | Method for detecting fruit flavor components in main stream smoke of cigarette |
| CN111272906B (en) * | 2020-03-31 | 2022-12-20 | 中国烟草总公司郑州烟草研究院 | Method for determining flower fragrance components in main stream smoke of cigarette |
| CN114113368A (en) * | 2021-10-27 | 2022-03-01 | 河南中烟工业有限责任公司 | Mouth-by-mouth transfer control method for heating sweet and fragrant monomers in cigarettes |
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