CN106802331A - 19 kinds of methods of sootiness perfume composition in heating non-burning cigarette smoke are determined simultaneously - Google Patents
19 kinds of methods of sootiness perfume composition in heating non-burning cigarette smoke are determined simultaneously Download PDFInfo
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- CN106802331A CN106802331A CN201710050409.8A CN201710050409A CN106802331A CN 106802331 A CN106802331 A CN 106802331A CN 201710050409 A CN201710050409 A CN 201710050409A CN 106802331 A CN106802331 A CN 106802331A
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- burning cigarette
- cigarette smoke
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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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
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
- G01N2030/884—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample organic compounds
Abstract
The invention discloses a kind of while the methods for determining 19 kinds of sootiness perfume composition in heating non-burning cigarette smoke, comprise the following steps：1）After trapping heating non-burning cigarette smoke granule phase substance with cambridge filter, cambridge filter is transferred to extraction vessel, adds inner mark solution, adding ethanol carries out concussion extraction, takes supernatant and obtains fume sample；2）Fume sample is detected using GC MS, 19 kinds of sootiness perfume component contents are detected by internal standard quanitation.The present invention uses solvent extraction combined gas chromatography mass spectrometry, can simultaneously determine 19 kinds of contents of sootiness perfume composition in heating non-burning cigarette smoke, has the advantages that quick detection, sensitivity are high, selectivity is good, accuracy is high；It is particularly well-suited to determine the content of sootiness perfume composition in heating non-burning cigarette smoke.
Description
Technical field
The invention belongs to fragrance component detection technique field, and in particular to a kind of to determine heating non-burning cigarette smoke simultaneously
In 19 kinds of sootiness perfume composition methods.
Background technology
Heating non-burning cigarette is a kind of new tobacco product, can promote contained tobacco-containing material non-by heating
The smog sucked for consumer is produced under fired state, compared with traditional cigarette, the release of side-stream smoke and part harmful substance
Significantly reduce.Heating non-burning cigarette is released by Reynolds Tobacco Company earliest, although such product not yet obtains the extensive of market
Accreditation, but lasting increase due to global range Tobacco Control dynamics and its reducing environmental pollution and smoking health potential risk
The clear superiority that aspect is present, international Field of Tobacco thinks that such product is the important directions of following tobacco product development always.
Sootiness note is one of important note of flue gas.Similar with traditional cigarette, sootiness is fragrant in heating non-combustion-type cigarette
The main component of rhythm is some phenolic compounds.The measure report on phenolic compound in smoke is main with traditional cigarette at present
It is object（Mao Duobin, Ma Yuping, Zhang Junsong, etc. the analysis of aldehydes matter in domestic and international blended type cigarette main flume, tobacco
Science and technology, 2002 (4): 17-20；Chinese granted patent CN 102313782A, CN103558319A etc.）, it is less non-for heating
Burning cigarette.Meanwhile, these assay methods generally choose harmful phenols component such as phenol, diphenol as research object, for being permitted
Thickness stacte contributes very big phenols component such as 4- vinyl guaiacols, 2,6- syringol etc., and these methods are often
Asynchronously it is related to.Therefore, develop a kind of while determining the direct, quick of various sootiness perfume compositions in heating non-burning cigarette smoke
New method for overall merit heating non-burning cigarette smoke sootiness note material base be very necessary.
The content of the invention
It is an object of the invention to provide a kind of quick detection, sensitivity is high, selectivity is good, accuracy is high while determine plus
19 kinds of methods of sootiness perfume composition in hot non-burning cigarette smoke.
In order to realize the above object the technical solution adopted in the present invention is：Heating non-burning cigarette smoke is determined simultaneously
In 19 kinds of sootiness perfume compositions（As table 1 shows）Method, comprise the following steps:
1）After trapping heating non-burning cigarette smoke granule phase substance with cambridge filter, cambridge filter is transferred to extraction vessel, added interior
Mark solution, adding ethanol carries out concussion extraction, takes supernatant and obtains fume sample；
The amount of inner mark solution used is 10 ~ 100 μ L, and internal standard compound is parachlorophenol, and inner mark solution concentration is 1 mg/mL.
Ethanol used is 10 ~ 100 mL；The time that the concussion is extracted is 20 ~ 40 min.
2）Fume sample is detected using GC-MS, 19 kinds of sootiness perfume component contents are detected by internal standard quanitation.
Chromatographic condition is：Chromatographic column：DB-WAXETR (60 m×0.25 mm×0.25 μm)；Carrier gas：He；Column flow：1
mL/min；Injector temperature：250℃；Temperature programming：50 DEG C (1 min), 10 DEG C/min → 160 DEG C (10 min), 3 DEG C/
min→240℃(20 min)；Not shunt mode.
Mass Spectrometry Conditions are：GC/MS transmission line temperature：250 DEG C, EI ion source temperatures：230 DEG C, level Four bar temperature：150
℃；EI ionizing energies：70 eV；Scan pattern：Selection ion scan, the time period is divided according to retention time.
In internal standard quanitation detection, containing 19 kinds of sootiness perfume compositions and a kind of internal standard mark in hybrid standard working solution used
Quasi- thing, solvent is ethanol；The concentration of internal standard parachlorophenol is 1 μ g/mL, standard working solution in all standard working solutions
Middle orthoresol, guaiacol, 2,4- xylenols, paracresol, 4- vinyl guaiacols, 2,6- xylenols, isobutyl
The concentration magnitude of fragrant phenol is followed successively by 0.01,0.02,0.05,0.1,0.2,0.5,1 μ g/mL, and each concentration magnitude from low to high
Lower this 7 kinds of sootiness perfume constituent concentrations are equal；MX, 2- (4- hydroxyphenyls) ethanol, 3- hydroxy benzaldehydes it is dense
Measurement level is followed successively by this 3 kinds under 0.028,0.07,0.14,0.28,0.7,1.4 μ g/mL, and each concentration magnitude from low to high
Sootiness perfume constituent concentration is equal；The concentration magnitude of phenol is followed successively by 0.02,0.08,0.2,0.4,0.8,2,4 μ from low to high
g/mL；2,4,6- pseudocuminols, 2,6- syringol, 4-ethyl guaiacol, the concentration magnitude of eugenol from it is low to
Height is followed successively by this 4 kinds of sootiness perfume (or spice) under 0.002,0.004,0.01,0.02,0.04,0.1,0.2 μ g/mL, and each concentration magnitude
Constituent concentration is equal；2,3- xylenols, the concentration magnitude of 3,4- xylenols is followed successively by 0.0028 from low to high,
0.0056th, this 2 kinds of sootiness perfume constituent concentrations under 0.014,0.028,0.056,0.14,0.28 μ g/mL, and each concentration magnitude
It is equal；2,5- xylenols, the concentration magnitude of 3- hydroxy acetophenones is followed successively by 0.0056 from low to high, 0.0112,
0.028th, this 2 kinds of sootiness perfume constituent concentrations are equal under 0.056,0.112,0.28,0.56 μ g/mL, and each concentration magnitude.
19 kinds of quantitation curves of sootiness perfume composition, the range of linearity, detection limit, quantitative limits are as shown in table 2.
The present invention use solvent extraction-combined gas chromatography mass spectrometry, can determine simultaneously heating non-burning cigarette smoke in
19 kinds of contents of sootiness perfume composition.And have the advantages that quick detection, sensitivity are high, selectivity is good, accuracy is high；Same acetone,
The common solvents such as dichloromethane, tetrahydrofuran are compared, ethanol extraction efficiency highest, it is adaptable to determine heating non-burning cigarette smoke
The content of middle sootiness perfume composition.
Brief description of the drawings
Fig. 1 is 19 kinds of SIM figures of sootiness perfume composition standard specimen；
Fig. 2 is the SIM figures of the sootiness perfume composition of the cigarette mainstream flue gas numbering 1,2 of embodiment 1；
Fig. 3 is the SIM figures of the sootiness perfume composition of the cigarette mainstream flue gas numbering 5 of embodiment 1；
Fig. 4 is the SIM figures of the sootiness perfume composition of the cigarette mainstream flue gas numbering 3,4 of embodiment 1；
Fig. 5 is the SIM figures of the sootiness perfume composition of the cigarette mainstream flue gas numbering 6,7,8 of embodiment 1；
Fig. 6 is the SIM figures of the sootiness perfume composition of the cigarette mainstream flue gas numbering 9 of embodiment 1；
Fig. 7 is the SIM figures of the sootiness perfume composition of the cigarette mainstream flue gas numbering 10-14 of embodiment 1；
Fig. 8 is the SIM figures of the sootiness perfume composition of the cigarette mainstream flue gas numbering 15,16 of embodiment 1；
Fig. 9 is the SIM figures of the sootiness perfume composition of the cigarette mainstream flue gas numbering 17,18,19 of embodiment 1.
Specific embodiment
With reference to specific embodiment, the present invention is further illustrated.
Embodiment 1
19 kinds of methods of sootiness perfume composition in heating non-burning cigarette smoke are determined while the present embodiment, is comprised the following steps：
1）The heating non-burning cigarette of the trade mark 1 is heated according to product operation instruction, with reference to the suction that ISO 3308 specifies
Capacity and granule phase substance capture method carry out suction and granule phase substance trapping.6 heating non-burning cigarette are trapped with two cambridge filters
After the Smoke Particulate of generation, cambridge filter is placed in 50 mL conical flask with cover and bottom of bottle is laid in, add 10 mL ethanol
Solution and 10 μ L inner mark solutions, vibrate 20min at room temperature, take 2 mL supernatants, obtain fume sample；
2）Using GC-MS to step 1）Gained fume sample is detected；
Chromatographic condition is：Chromatographic column：DB-WAXETR (60 m×0.25 mm×0.25 μm)；Carrier gas：He；Column flow：1 mL/
min；Injector temperature：250℃；Temperature programming：50 DEG C (1min), 10 DEG C/min → 160 DEG C (10min), 3 DEG C/min →
240℃(20min)；Not shunt mode.
Mass Spectrometry Conditions are：GC/MS transmission line temperature：250 DEG C, EI ion source temperatures：230 DEG C, level Four bar temperature：150
℃；EI ionizing energies：70 eV；Scan pattern：Selection ion scan, the time period is divided according to retention time.
Volume of 19 kinds of methods of sootiness perfume composition to the trade mark 1 in measure heating non-burning cigarette smoke while the present embodiment
Cigarette testing result is as shown in table 3.
Embodiment 2
19 kinds of methods of sootiness perfume composition in heating non-burning cigarette smoke are determined while the present embodiment, is comprised the following steps：
1）The heating non-burning cigarette of the trade mark 2 is heated according to product operation instruction, with reference to the suction that ISO 3308 specifies
Capacity and granule phase substance capture method carry out suction and granule phase substance trapping.6 heating non-burning cigarette are trapped with two cambridge filters
After the Smoke Particulate of generation, cambridge filter is placed in 50 mL conical flask with cover and bottom of bottle is laid in, add 20 mL ethanol
Solution and 20 μ L inner mark solutions, vibrate 25min at room temperature, take 2 mL supernatants, obtain fume sample；
2）Using GC-MS to step 1）Gained fume sample is detected；
Chromatographic condition and Mass Spectrometry Conditions are with embodiment 1.
Volume of 19 kinds of methods of sootiness perfume composition to the trade mark 2 in measure heating non-burning cigarette smoke while the present embodiment
Cigarette testing result is as shown in table 3.
Embodiment 3
19 kinds of methods of sootiness perfume composition in heating non-burning cigarette smoke are determined while the present embodiment, is comprised the following steps：
1）The heating non-burning cigarette of the trade mark 3 is heated according to product operation instruction, with reference to the suction that ISO 3308 specifies
Capacity and granule phase substance capture method carry out suction and granule phase substance trapping.6 heating non-burning cigarette are trapped with two cambridge filters
After the Smoke Particulate of generation, cambridge filter is placed in 50 mL conical flask with cover and bottom of bottle is laid in, add 30 mL ethanol
Solution and 30 μ L inner mark solutions, vibrate 30min at room temperature, take 2 mL supernatants, obtain fume sample；
2）Using GC-MS to step 1）Gained fume sample is detected；
Chromatographic condition and Mass Spectrometry Conditions are with embodiment 1.
Volume of 19 kinds of methods of sootiness perfume composition to the trade mark 3 in measure heating non-burning cigarette smoke while the present embodiment
Cigarette testing result is as shown in table 3.
Embodiment 4
19 kinds of methods of sootiness perfume composition in heating non-burning cigarette smoke are determined while the present embodiment, is comprised the following steps：
1）The heating non-burning cigarette of the trade mark 4 is heated according to product operation instruction, with reference to the suction that ISO 3308 specifies
Capacity and granule phase substance capture method carry out suction and granule phase substance trapping.6 heating non-burning cigarette are trapped with two cambridge filters
After the Smoke Particulate of generation, cambridge filter is placed in 50 mL conical flask with cover and bottom of bottle is laid in, add 40 mL ethanol
Solution and 40 μ L inner mark solutions, vibrate 35min at room temperature, take 2 mL supernatants, obtain fume sample；
2）Using GC-MS to step 1）Gained fume sample is detected；
Chromatographic condition and Mass Spectrometry Conditions are with embodiment 1.
Volume of 19 kinds of methods of sootiness perfume composition to the trade mark 4 in measure heating non-burning cigarette smoke while the present embodiment
Cigarette testing result is as shown in table 3.
Experimental example 5
The heating non-burning cigarette of the trade mark 2 is heated according to product operation instruction, the suction specified with reference to ISO 3308 is held
Amount and granule phase substance capture method carry out suction and granule phase substance trapping.6 heating non-burning cigarette are trapped with two cambridge filters to produce
Raw Smoke Particulate.Method according to example 1 is measured, 6 groups of parallel determination, 19 kinds of 6 parallel surveys of sootiness perfume composition
The RSD values of definite value are between 3%-10%（It is shown in Table 4）, it was demonstrated that method of the present invention accuracy is higher, reproducible.
Claims (5)
- It is 1. a kind of to heat 19 kinds of methods of sootiness perfume composition in non-burning cigarette smoke while determining, it is characterised in that：Specific step It is rapid as follows：1）After trapping heating non-burning cigarette smoke granule phase substance with cambridge filter, cambridge filter is transferred to extraction vessel, added interior Mark solution, adding ethanol carries out concussion extraction, takes supernatant and obtains fume sample；2）Fume sample is detected using GC-MS, 19 kinds of sootiness perfume component contents are detected by internal standard quanitation；Chromatographic condition is：Chromatographic column：DB-WAXETR, m × 0.25 mm × 0.25 μm of specification 60；Carrier gas：He；Column flow：1 mL/min；Injector temperature：250℃；Temperature programming：50 DEG C, 1 min is kept, then rises to 160 DEG C with 10 DEG C/min speed, Keep 10 min；It is last to rise to 240 DEG C with 3 DEG C/min speed, keep 20 min；Not shunt mode；Mass Spectrometry Conditions are：GC/MS transmission line temperature：250 DEG C, EI ion source temperatures：230 DEG C, level Four bar temperature：150℃；EI Ionizing energy：70 eV；Scan pattern：Selection ion scan, the time period is divided according to retention time.
- 2. it is according to claim 1 to heat 19 kinds of methods of sootiness perfume composition in non-burning cigarette smoke while determining, its It is characterised by：19 kinds of sootiness perfume compositions are respectively：Guaiacol, 2,6- xylenols, 2,4,6- pseudocuminols, adjacent first Phenol, phenol, 4-ethyl guaiacol, 2,5- xylenols, 2,4- xylenols, paracresol, 2,3- xylenols, fourth Fragrant phenol, 3,5- xylenols, 4- vinyl guaiacols, 3,4- xylenols, 2,6- syringol, isobutyl are fragrant Phenol, 3- hydroxy benzaldehydes, 3- hydroxy acetophenones, 2- (4- hydroxyphenyls) ethanol.
- 3. it is according to claim 1 to heat 19 kinds of methods of sootiness perfume composition in non-burning cigarette smoke while determining, its It is characterised by：Parachlorophenol is designated as in described, the amount of inner mark solution is 10 ~ 100 μ L, and the concentration of inner mark solution is 1 mg/mL.
- 4. it is according to claim 1 to heat 19 kinds of methods of sootiness perfume composition in non-burning cigarette smoke while determining, its It is characterised by：The consumption of ethanol is 10 ~ 100 mL.
- 5. it is according to claim 1 to heat 19 kinds of methods of sootiness perfume composition in non-burning cigarette smoke while determining, its It is characterised by：The time that the concussion is extracted is 20 ~ 40 min.
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Cited By (3)
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| CN111289677A (en) * | 2020-03-31 | 2020-06-16 | 中国烟草总公司郑州烟草研究院 | Method for measuring spicy components in main stream smoke of cigarette |
| CN113156006A (en) * | 2021-04-13 | 2021-07-23 | 中国烟草总公司郑州烟草研究院 | Method for trapping, analyzing and measuring main chemical components in smoke exhaled by heated non-combustible cigarette |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111289677A (en) * | 2020-03-31 | 2020-06-16 | 中国烟草总公司郑州烟草研究院 | Method for measuring spicy components in main stream smoke of cigarette |
| CN113156006A (en) * | 2021-04-13 | 2021-07-23 | 中国烟草总公司郑州烟草研究院 | Method for trapping, analyzing and measuring main chemical components in smoke exhaled by heated non-combustible cigarette |
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