CN108776184A - A method of cigarette smoke component of not burning is heated in detection - Google Patents
A method of cigarette smoke component of not burning is heated in detection Download PDFInfo
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- CN108776184A CN108776184A CN201810608156.6A CN201810608156A CN108776184A CN 108776184 A CN108776184 A CN 108776184A CN 201810608156 A CN201810608156 A CN 201810608156A CN 108776184 A CN108776184 A CN 108776184A
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- cigarette
- suction
- heating
- standard
- burn
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- 235000019504 cigarettes Nutrition 0.000 title claims abstract description 94
- 238000000034 method Methods 0.000 title claims abstract description 28
- 238000001514 detection method Methods 0.000 title claims abstract description 22
- 239000000779 smoke Substances 0.000 title claims abstract description 19
- 238000010438 heat treatment Methods 0.000 claims abstract description 49
- 239000008187 granular material Substances 0.000 claims abstract description 28
- 230000000391 smoking effect Effects 0.000 claims abstract description 26
- 239000000243 solution Substances 0.000 claims abstract description 24
- 238000000605 extraction Methods 0.000 claims abstract description 8
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- 239000012224 working solution Substances 0.000 claims abstract description 7
- 238000005259 measurement Methods 0.000 claims abstract description 4
- 238000010813 internal standard method Methods 0.000 claims abstract description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 52
- URAYPUMNDPQOKB-UHFFFAOYSA-N triacetin Chemical compound CC(=O)OCC(OC(C)=O)COC(C)=O URAYPUMNDPQOKB-UHFFFAOYSA-N 0.000 claims description 34
- 235000011187 glycerol Nutrition 0.000 claims description 26
- 229960005150 glycerol Drugs 0.000 claims description 26
- SNICXCGAKADSCV-JTQLQIEISA-N (-)-Nicotine Chemical compound CN1CCC[C@H]1C1=CC=CN=C1 SNICXCGAKADSCV-JTQLQIEISA-N 0.000 claims description 25
- 229960002715 nicotine Drugs 0.000 claims description 25
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 claims description 25
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 21
- NOOLISFMXDJSKH-UTLUCORTSA-N (+)-Neomenthol Chemical compound CC(C)[C@@H]1CC[C@@H](C)C[C@@H]1O NOOLISFMXDJSKH-UTLUCORTSA-N 0.000 claims description 20
- NOOLISFMXDJSKH-UHFFFAOYSA-N DL-menthol Natural products CC(C)C1CCC(C)CC1O NOOLISFMXDJSKH-UHFFFAOYSA-N 0.000 claims description 20
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 20
- 229940041616 menthol Drugs 0.000 claims description 20
- 239000001087 glyceryl triacetate Substances 0.000 claims description 17
- 235000013773 glyceryl triacetate Nutrition 0.000 claims description 17
- 229960002622 triacetin Drugs 0.000 claims description 17
- 239000007789 gas Substances 0.000 claims description 14
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 12
- 229960004063 propylene glycol Drugs 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000004587 chromatography analysis Methods 0.000 claims description 8
- AXPZIVKEZRHGAS-UHFFFAOYSA-N 3-benzyl-5-[(2-nitrophenoxy)methyl]oxolan-2-one Chemical compound [O-][N+](=O)C1=CC=CC=C1OCC1OC(=O)C(CC=2C=CC=CC=2)C1 AXPZIVKEZRHGAS-UHFFFAOYSA-N 0.000 claims description 7
- 239000012159 carrier gas Substances 0.000 claims description 6
- 239000001307 helium Substances 0.000 claims description 6
- 229910052734 helium Inorganic materials 0.000 claims description 6
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 6
- 238000005070 sampling Methods 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000005350 fused silica glass Substances 0.000 claims description 3
- 238000004458 analytical method Methods 0.000 abstract description 8
- 230000035945 sensitivity Effects 0.000 abstract description 3
- 238000002474 experimental method Methods 0.000 abstract description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 23
- 239000003546 flue gas Substances 0.000 description 22
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 17
- 241000208125 Nicotiana Species 0.000 description 14
- 239000000443 aerosol Substances 0.000 description 14
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 8
- 238000011084 recovery Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 4
- 230000014759 maintenance of location Effects 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 244000061176 Nicotiana tabacum Species 0.000 description 3
- 238000004817 gas chromatography Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000005086 pumping Methods 0.000 description 3
- 229940058015 1,3-butylene glycol Drugs 0.000 description 2
- KMZHZAAOEWVPSE-UHFFFAOYSA-N 2,3-dihydroxypropyl acetate Chemical compound CC(=O)OCC(O)CO KMZHZAAOEWVPSE-UHFFFAOYSA-N 0.000 description 2
- 235000019437 butane-1,3-diol Nutrition 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 235000009508 confectionery Nutrition 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000796 flavoring agent Substances 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 238000003780 insertion Methods 0.000 description 2
- 230000037431 insertion Effects 0.000 description 2
- 230000035479 physiological effects, processes and functions Effects 0.000 description 2
- 238000004445 quantitative analysis Methods 0.000 description 2
- 238000007613 slurry method Methods 0.000 description 2
- 239000012086 standard solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- ILJSQTXMGCGYMG-UHFFFAOYSA-N triacetic acid Chemical compound CC(=O)CC(=O)CC(O)=O ILJSQTXMGCGYMG-UHFFFAOYSA-N 0.000 description 2
- MDYZKJNTKZIUSK-UHFFFAOYSA-N tyloxapol Chemical compound O=C.C1CO1.CC(C)(C)CC(C)(C)C1=CC=C(O)C=C1 MDYZKJNTKZIUSK-UHFFFAOYSA-N 0.000 description 2
- 235000006679 Mentha X verticillata Nutrition 0.000 description 1
- 235000002899 Mentha suaveolens Nutrition 0.000 description 1
- 235000001636 Mentha x rotundifolia Nutrition 0.000 description 1
- 240000002853 Nelumbo nucifera Species 0.000 description 1
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 1
- 235000006510 Nelumbo pentapetala Nutrition 0.000 description 1
- 244000269722 Thea sinensis Species 0.000 description 1
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical compound ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000686 essence Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 235000013355 food flavoring agent Nutrition 0.000 description 1
- 125000005456 glyceride group Chemical group 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 238000012417 linear regression Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 235000013372 meat Nutrition 0.000 description 1
- 239000012982 microporous membrane Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- XKLJHFLUAHKGGU-UHFFFAOYSA-N nitrous amide Chemical compound ON=N XKLJHFLUAHKGGU-UHFFFAOYSA-N 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 230000010076 replication Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000035807 sensation Effects 0.000 description 1
- 235000019615 sensations Nutrition 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- -1 using 1 Chemical compound 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
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
-
- 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
- G01N30/14—Preparation by elimination of some components
-
- 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
- G01N30/64—Electrical detectors
- G01N30/66—Thermal conductivity detectors
-
- 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
- G01N2030/042—Standards
- G01N2030/045—Standards internal
-
- 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
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Investigating Or Analysing Biological Materials (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The present invention provides a kind of method that cigarette smoke component of not burning is heated in detection, includes the following steps：(1) preparation of inner mark solution；(2) preparation of standard working solution；(3) cigarette that do not burn is heated in suction, and cambridge filter collects total granules；(4) extraction of total granules；(5) gas Chromatographic Determination；(6) double internal standard methods calculate measurement result.The method that the present invention establishes is heated the trapping of the suction and total granules of the cigarette that do not burn using traditional cigarette smoking machine, without heating the special smoking machine of cigarette that do not burn；Realize analysis detection while 6 kinds of target components are completed in primary experiment；It is quantitative determined using double internal standards, quantitative result is more accurate；Sample suction, total granules trapping and extracting operation are simple, and gas Chromatographic Determination is convenient, and stability is good, has many advantages, such as that linear dependence is good, and practicability is good, high sensitivity, reproducible.
Description
Technical field
The present invention relates to tobacco detection technique field, the side for cigarette smoke component of not burning is heated in specifically a kind of detection
Method detects heating and does not burn moisture in cigarette smoke, nicotine, glycerine, 1,2-PD, glyceryl triacetate and thin simultaneously
The method of lotus alcohol burst size.
Background technology
Low temperature cigarette is also named and heats the cigarette (heat-not-burn cigarette) that do not burn, by external heat source to cigarette
Careless substance is heated, and the atomizing medium, flavor component and outer flavoring in tobacco material are similar to conventional roll by heating to generate
The smog that cigarette is burnt and sucked makes consumer obtain physiology satisfaction.Tobacco material in low temperature cigarette is only heated without burning, and is heated
(250 DEG C~350 DEG C) ignition temperatures (800 DEG C -900 DEG C) for being far below traditional cigarette of temperature, therefore, harmful ingredients in flue gas and life
Object toxicity is greatly reduced, and side-stream smoke and environment flue gas are also greatly lowered.
The cigarette that do not burn is heated to be researched and developed by the international major company such as PM (Philip Morris) earliest.In recent years, international
Occurs glo, JT (Japan of iQOS, BAT (British American Tobacco) company of PM companies in the market
Tobacco) a collection of market manifestation such as Ploom of company is good heats the cigarette product that do not burn, and market scale expands rapidly, deep
Obtain the favor of consumer.The existing cigarette that do not burn that heats includes sequentially connected filter tip and tobacco segment, the general 45- of total length
55mm, hence it is evident that shorter than traditional cigarette total length (general 84mm or so), the general 15-20mm of length of wherein tobacco segment, hence it is evident that short
In traditional cigarette tobacco segment length (general 50-64mm).Existing heating is not burnt, and there are mainly two types of forms for cigarette tobacco segment：Orderly
The sheet and shreds or pipe tobacco of arrangement, disorderly arranged sheet and shreds or pipe tobacco.
The amount of smoke similar to traditional cigarette is generated when to ensure suction, heating load in the pipe tobacco for the cigarette that do not burn has greatly
The Alevaire glycerine and propylene glycol of amount.Since the pipe tobacco of traditional cigarette is difficult to load a large amount of Alevaire, the cigarette that do not burn is heated
Pipe tobacco generally all using roll-in method (or thick slurry method) sheet and shreds or main body, using roll-in method (or thick slurry method), sheet and shreds are simultaneously
The pipe tobacco for being aided with a small amount of traditional cigarette carries out inhaling taste adjusting, therefore heats the cigarette of the pipe tobacco composition and traditional cigarette of the cigarette that do not burn
Silk has larger difference；To achieve the effect that cool down rapidly, heating all can compound traditional cigarette in the mouth stick for the cigarette that do not burn
In the cooling material that will not use, therefore, the mouth stick structure and material of cigarette is not burnt in heating and the mouth stick of traditional cigarette also has
Larger difference；Along with (250 DEG C~350 DEG C) (800 DEG C -900 of ignition temperatures for being far below traditional cigarette of heating temperature
DEG C), therefore, the flue gas of the flue gas composition and traditional cigarette that heat the cigarette that do not burn has notable difference, heats the cigarette that do not burn
The main component of flue gas aerosol includes water, glycerine, 1,2-PD, nicotine etc., wherein moisture, glycerine, 1,2- the third two
The content accounting of alcohol has a greater change compared to traditional cigarette flue gas, and carbon monoxide, polycyclic aromatic hydrocarbon, tobacco-specific nitrosamine
Deng content decline to a great extent.Heating does not burn cigarette as the new things just occurred soon, currently, there are no needles both at home and abroad
It does not burn the detection method of cigarette smoke component for heating, without not burning cigarette by the generally heating of verification and approval yet
Special smoking machine.The analysis method of existing traditional cigarette flue gas composition is usually all by the components such as nicotine, moisture, polyalcohols point
Class detects, relatively time consuming effort, and testing cost is higher.The method of the present invention makes full use of traditional cigarette smoking machine to be heated not
The trapping of the suction and total granules of burning cigarette, to heating moisture, nicotine, glycerine, 1,2- third in the cigarette smoke that do not burn
Glycol, glyceryl triacetate and menthol are carried out while being detected.
The present inventor has found by research in the implementation of the present invention：Heating is not burnt in cigarette flue gas aerosol
Moisture influences the suctions impression such as irritation, dry sensation and moisture feeling when consumer's suction；Heat the cigarette flue gas aerosol that do not burn
In nicotine, directly affect consumer suction when physiology satisfaction；Heat the glycerine in the cigarette flue gas aerosol that do not burn
And 1,2-PD, directly affect amount of smoke when consumer's suction；It does not burn cigarette for the heating of mint aroma, flue gas
Menthol in aerosol directly affects cool degree impression when consumer's suction；Glyceryl triacetate is colourless oil liquid, is had
Important fixation in the main plasticizer and essence and flavoring agent that are used in faint fruity, the taste of meat sweet tea and cigarette filter rod production
Agent, heats the glyceryl triacetate in the cigarette flue gas aerosol that do not burn, and too high levels can also influence consumer's pumping to a certain degree
Suction taste when suction.Therefore, to heating the moisture in the cigarette flue gas aerosol that do not burn, nicotine, glycerine, 1,2-PD, three
Acetin and menthol are detected, and are of great significance.
Invention content
The technical problem to be solved by the present invention is to be directed to heating not burn cigarette, a kind of detection is provided and heats the cigarette that do not burn
The method of flue gas composition, i.e., to heating the moisture in the cigarette flue gas aerosol that do not burn, nicotine, glycerine, 1,2-PD, three
Acetin and menthol are carried out at the same time detection.
Technical solution provided by the invention：A method of cigarette smoke component of not burning is heated in detection, including walks as follows
Suddenly：
(1) preparation of inner mark solution：Internal standard sample n-butanol, 1,3-BDO are weighed, using chromatographic pure isopropanol as molten
Agent constant volume, obtains inner mark solution；
(2) preparation of standard working solution：It is sweet to weigh a certain amount of water, nicotine, glycerine, 1,2- propylene glycol, triacetic acid
Grease, menthol standard items obtain standard reserving solution using chromatographic pure isopropanol as solvent constant volume；5 or more are taken to extract
Bottle, after being separately added into standard reserving solution by gradient, is added the inner mark solution of same volume, and it is molten to be configured to 5 grades or more standard work
Liquid；
(3) cigarette that do not burn is heated in suction, and cambridge filter collects total granules；
(4) total granules collected to step (3) cambridge filter, is extracted with the inner mark solution of step (1), is obtained total
The extract liquor of granule phase substance；
(5) extract liquor of the total granules obtained to step (4) carries out gas Chromatographic Determination；
(6) internal standard method calculates measurement result：Quantitative determined using double internal standards, wherein n-butanol as internal standard to moisture
It is quantified, 1,3-BDO determines nicotine, 1,2-PD, glycerine, glyceryl triacetate, menthol as internal standard
It is fixed to measure.
Further, suction heating is not burnt cigarette in the step (3), collect total granules the specific steps are：By biography
After system cigarette smoking method gets out smoking machine, heating is not burnt, and heating utensil is inserted at Cigarette end, mouth stick end is inserted into and is inhaled
Smoke machine clamper, heater tool switch preheating, after reaching preheating time, smoking machine starts to aspirate, and collects total granules.
Any one in Canadian depth suction mode and iso standard suction mode can be used in smoking machine suction.According to suction mode
Puff number is determined with the heating time of heating utensil setting, and after reaching puff number, suction is completed.
Further, in the step (4) total granules extraction the specific steps are：Total grain will be trapped in step (3)
The cambridge filter of phase object is put into extraction flask, and the inner mark solution of 20-50mL steps (1) is added, is filtered after fully vibrating 0.5-2h,
Obtain the extract liquor of total granules.
Further, the detector of gas-chromatography is thermal conductivity detector (TCD) (TCD) in the step (5).
Further, the condition of gas-chromatography is in the step (5)：DB-1701 fused quartz capillary chromatography columns, ruler
Very little is 30m × 0.32mm × 1.0 μm；Injector temperature is 260 DEG C；Temperature programming：80 DEG C of initial temperature holding 2.5min, with 40 DEG C/
The rate of min rises to 250 DEG C, keeps 3min；Carrier gas is helium, flow rate of carrier gas 1.5mL/min, constant current mode；Make-up gas helium
30mL/min；Sampling volume is 1 μ L, split sampling, split ratio 5:1；260 DEG C of TCD detector temperatures.
Due to not burning the special smoking machine of cigarette currently without the heating by generally verifying and approving, the present invention is in tradition
Do not burn the suction of cigarette and the collection of total granules are heated on cigarette smoking machine.It is ready to by traditional cigarette suction method
After smoking machine, heating is not burnt, and heating utensil is inserted at Cigarette end, smoking machine clamper, heater are inserted into mouth stick end
Tool switch preheating, after reaching preheating time, smoking machine starts to aspirate, and collects total granules.Wherein, to avoid in aspiration procedure
Heating do not burn Cigarette bending or fracture, can artificially to heating utensil carry out help or heating utensil transfer glove body into
Row support.Smoking machine use the condition of Canadian depth suction mode for：Every mouthful of pumping volume 55mL, every mouthful of suction time 2 seconds,
Interval time 28 seconds between different puff numbers；Smoking machine use the condition of iso standard suction mode for：Every mouthful of pumping volume
35mL, every mouthful of suction time 2 seconds, 58 seconds interval times between different puff numbers.Therefore, Canadian every point of depth suction mode
Smokable 2 mouthfuls of clock, smokable 1 mouthful per minute of iso standard suction mode.The time for heating the energy continuous heating of utensil setting is general
It it is 3-6 minutes, therefore, Canadian depth suction mode is 6-12 mouthfuls smokable, and iso standard suction mode is 3-6 mouthfuls smokable, reaches
After puff number, suction is completed.
Due to moisture in total granules and nicotine, the content of 1,2- propylene glycol, glycerine, glyceryl triacetate, menthol
It differs greatly, therefore, the method for the present invention is quantitative determined using double internal standards, it is ensured that quantitative accurate of all target components
Property, i.e., quantify moisture as internal standard using n-butanol, using 1,3-BDO as internal standard to nicotine, 1,2- the third two
Alcohol, glycerine, glyceryl triacetate, menthol are quantitative determined.The retention time of n-butanol and 1,3 butylene glycol is respectively
3.67min and 5.73min, non-overlapping with the other ingredients of sample, peak shape symmetry is preferable, is suitable as internal standard.
Inventor has investigated the separation of DB-1, DB-5, DB-1701 and DB-INNOWAX chromatographic column of totally four kinds of opposed polarities
Effect.1,2-PD, the glycerine peak type in DB-5 and DB-1 chromatographic columns are short and stout, chromatographic peak trailing phenomenon occur；Nicotine and
1,2- propylene glycol not appearance in highly polar DB-INNOWAX chromatographic columns.6 kinds of mesh can preferably be detached using DB-1701 chromatographic columns
Object is marked, each object chromatographic peak peak type is sharply symmetrical, does not trail, analysis time is shorter, it is only necessary to which 10min is separable complete, can
To meet the detection sensitivity of low concentration nicotine in extract liquor, while the sample introduction of the 1,2-PD of high concentration, glycerine is examined
Nonoverload is measured, extract liquor need not be further diluted, therefore selects DB-1701 chromatographic columns to carry out sample analysis.
Increase the qualitative of the chromatographic peak of method 6 objects of progress using retention time and peak height.Compare glycerine, 1,2- third
Glycol, glyceryl triacetate, nicotine, menthol and moisture gas chromatogram in standard specimen retention time and flue gas extract liquor in
The retention time of component determines object in gas chromatogram；Increase method using peak height to confirm object, by standard simultaneously
After sample is added in extract liquor, with not plus compared with the sample chromatogram of standard sample, if peak height increases, that is, the mark being added is thought
Quasi- object is divided into same compound with to be measured group in sample.
The method of the present invention has following excellent results compared with prior art：
1, the present invention, which establishes one kind while detecting, heats moisture, nicotine, glycerine, 1,2- third in the cigarette smoke that do not burn
The method of glycol, glyceryl triacetate and menthol burst size.
2, the present invention, which realizes primary experiment while measuring, heats 6 kinds of target components in the cigarette smoke that do not burn, saves inspection
Survey cost.
3, method of the invention can make full use of traditional cigarette smoking machine to be heated the suction for the cigarette that do not burn and total grain
The trapping of phase object, without heating the special smoking machine of cigarette that do not burn.
4, the present invention is quantitative determined using double internal standards, i.e., n-butanol quantifies moisture as internal standard, 1,3- fourth
Glycol quantitative determines nicotine, 1,2-PD, glycerine, glyceryl triacetate, menthol as internal standard, quantitative result
It is more accurate.
5, inventive samples suction, total granules trapping and extracting operation are simple, and gas Chromatographic Determination is convenient, stability
It is good, have preferable linear dependence, practicability good.
6, the method for the present invention high sensitivity and reproducible.Moisture, nicotine, glycerine, 1,2- propylene glycol, triacetic acid glycerine
The detection limit of ester and menthol is respectively 0.63mg/ branch, 0.035mg/ branch, 0.059mg/ branch, 0.048mg/ branch, 0.046mg/ branch
With 0.031mg/ branch, recovery of standard addition between 95.1%~109.2%, relative standard deviation 1.77%~4.28% it
Between.
Description of the drawings
Fig. 1 is the chromatogram of standard sample；
Fig. 2 is the chromatogram of 1 sample of the embodiment of the present invention.
Specific implementation mode
With reference to specific embodiment and figure, the present invention will be further described.
Embodiment 1
(1) preparation of inner mark solution：Accurately weigh internal standard sample n-butanol (purity >=99%) 2.000g, 1,3 butylene glycol
(purity >=99%) 0.2000g obtains inner mark solution using chromatographic pure isopropanol as solvent constant volume in 1000mL volumetric flasks；
A concentration of 2mg/mL of internal standard compound n-butanol in inner mark solution, a concentration of 0.2mg/mL of 1,3-BDO.
(2) preparation of standard working solution：Accurately weigh pure water 6.000g, glycerine standard items (purity >=99%)
3.000g, nicotine standard product (purity >=99%) 0.6000g, 1,2- propylene glycol standard items (purity >=99%) 0.6000g, three second
Acid glyceride standard items (purity >=99.5%) 0.6000g, menthol standard items (purity >=99%) 0.6000g, with chromatographically pure
Isopropanol in 100mL volumetric flasks, obtains standard reserving solution as solvent constant volume, wherein a concentration of 60mg/mL of water, the third three
A concentration of 30mg/mL of alcohol, remaining material concentration are 6mg/mL；Take 5 extraction flasks, be separately added into 0.1mL, 0.2mL, 0.5mL,
After 1mL, 2mL standard reserving solution, the inner mark solution of 20mL is added, is configured to 5 grades of standard working solutions.
(3) series standard working solution is subjected to gas chromatographic analysis, the detection of TCD detectors.The condition of gas-chromatography is：
DB-1701 fused quartz capillary chromatography columns, size are 30m × 0.32mm × 1.0 μm；Injector temperature is 260 DEG C；Program liter
Temperature：80 DEG C of holding 2.5min of initial temperature, rise to 250 DEG C with the rate of 40 DEG C/min, keep 3min；Carrier gas is helium, flow rate of carrier gas
1.5mL/min, constant current mode；Make-up gas helium 30mL/min；Sampling volume is 1 μ L, split sampling, split ratio 5:1；TCD is examined
Survey 260 DEG C of device temperature.It is quantitative determined using double internal standards, n-butanol quantifies moisture as internal standard, 1,3-BDO
Nicotine, 1,2- propylene glycol, glycerine, glyceryl triacetate, menthol are quantitative determined as internal standard.
(4) standard working curve is limited with detection：With corresponding the ratio between the interior target peak area of the peak area of each object
With the ratio between each target concentration and internal standard concentration carry out linear regression analysis, obtain each target compound criteria working curve and
Related coefficient；By the standard solution sample introduction 8 times of Cmin, the standard deviation of measurement result is calculated, respectively with the 3 of standard deviation
Again and 10 times determine that detection limit and quantitative limit, result of calculation are as shown in table 1.The result shows that the working curve of 6 kinds of objects is linear
Well, related coefficient is above 0.999；The quantitative limit of each object is far below the content of object in extract liquor, is suitble to quantitative
Analysis.
1 standard working curve of table is limited with detection
(5) after getting smoking machine ready by traditional cigarette suction method note, cigarette sample A cigarettes end insertion of not burning will be heated and added
Hot utensil heats the cigarette filter tip end insertion smoking machine clamper that do not burn, after heater tool switch preheats 2min, smoking machine
Start to aspirate, cambridge filter collects total granules.Smoking machine is using Canadian depth suction mode, the heating of heating utensil setting
Time is 4min, and after 8 mouthfuls of suction, suction is completed.
(6) cambridge filter for having trapped total granules is put into extraction flask, 20mL inner mark solutions is added, fully vibrate
After 40min, 0.45 μm of filtering with microporous membrane obtains the extract liquor of total granules.
(7) extract liquor of total granules is subjected to gas chromatographic analysis, the detection of TCD detectors according to the condition of step (3).
Standard working curve is substituted into respectively with the ratio between the interior target peak area that the peak area of each object is corresponding, acquires sample A cigarettes
The content of each object, the results are shown in Table 2 in gas aerosol.
26 embodiments of table heat cigarette sample analysis result (mg/ branch) of not burning
(8) precision is tested with the rate of recovery.Flue gas extract liquor is divided into four parts, wherein 1 part is reference, in addition 3 parts of difference
Water, 1,2- propylene glycol, glycerine, menthol, glyceryl triacetate and the nicotine standard of high, medium and low various concentration level is added
Solution, 2 samples of each pitch-based sphere replication.Sample carries out pre-treatment and chromatography by selected condition, and by extracting
Former content, mark-on amount and mark-on measured quantity in liquid is taken to calculate the rate of recovery (table 3).The result shows that water, 1,2-PD, third
Triol, menthol, glyceryl triacetate and nicotine recovery of standard addition respectively 95.1%~107.7%, 96.1%~
104.2%, 98.5%~109.2%, 101.4%~103.9%, 96.3%~104.3% and 96.0%~108.0% it
Between.To be added the extract liquor sample replicate analysis 6 times of intermediate concentration standard solution, water, 1,2-PD, glycerine, menthol,
Relative standard deviation (RSD) result of calculation of glyceryl triacetate and nicotine is respectively 1.77%, 4.13%, 3.37%,
2.26%, 4.28% and 2.87%.Therefore, this method precision is preferable, and the rate of recovery is higher, is suitble to heat the cigarette cigarette that do not burn
The quantitative analysis of water, 1,2- propylene glycol, glycerine, menthol, glyceryl triacetate and nicotine in gas extract liquor.
The recovery of standard addition of 3 analysis method of table
Embodiment 2
As described in Example 1, it is detected to heating the cigarette sample B that do not burn, all steps are same as Example 1, sample
The content of each object, the results are shown in Table 2 in product B flue gas aerosols.
Embodiment 3
As described in Example 1, it is detected to heating the cigarette sample C that do not burn, all steps are same as Example 1, sample
The content of each object, the results are shown in Table 2 in product C flue gas aerosols.
Embodiment 4
As described in Example 1, it is detected to heating the cigarette sample D that do not burn, all steps are same as Example 1, sample
The content of each object, the results are shown in Table 2 in product D flue gas aerosols.
Embodiment 5
As described in Example 1, it is detected to heating the cigarette sample E that do not burn, all steps are same as Example 1, sample
The content of each object, the results are shown in Table 2 in product E flue gas aerosols.
Embodiment 6
As described in Example 1, it is detected to heating the cigarette sample F that do not burn, wherein smoking machine is taken out using iso standard
The heating time of suction mode, heating utensil setting is 4min, and after 4 mouthfuls of suction, suction is completed.Other steps are same as Example 1,
The content of each object, the results are shown in Table 2 in sample F flue gas aerosol.
The foregoing is merely the detailed descriptions of specific embodiments of the present invention, do not limit the present invention with this, all at this
All any modification, equivalent and improvement etc. made by the mentality of designing of invention, should be included in protection scope of the present invention it
It is interior.
Claims (5)
- A kind of method of cigarette smoke component 1. detection heating is not burnt, it is characterised in that include the following steps：(1) preparation of inner mark solution：Internal standard sample n-butanol, 1,3-BDO are weighed, is determined using chromatographic pure isopropanol as solvent Hold, obtains inner mark solution；(2) preparation of standard working solution：Weigh a certain amount of water, nicotine, glycerine, 1,2- propylene glycol, glyceryl triacetate, Menthol standard items obtain standard reserving solution using chromatographic pure isopropanol as solvent constant volume；5 or more extraction flasks are taken, by ladder After degree is separately added into standard reserving solution, the inner mark solution of same volume is added, is configured to 5 grades or more standard working solutions；(3) cigarette that do not burn is heated in suction, and cambridge filter collects total granules；(4) total granules collected to step (3) cambridge filter, is extracted with the inner mark solution of step (1), obtains total grain phase The extract liquor of object；(5) extract liquor of the total granules obtained to step (4) carries out gas Chromatographic Determination；(6) internal standard method calculates measurement result：It is quantitative determined using double internal standards, wherein n-butanol carries out moisture as internal standard Quantitative, 1,3-BDO carries out quantitative survey as internal standard to nicotine, 1,2-PD, glycerine, glyceryl triacetate, menthol It is fixed.
- The method of cigarette smoke component 2. a kind of detection heating as described in claim 1 is not burnt, is aspirated in the step (3) Heating is not burnt cigarette, collect total granules the specific steps are：After getting out smoking machine by traditional cigarette suction method, it will heat Not burning, heating utensil is inserted at Cigarette end, smoking machine clamper is inserted at mouth stick end, and heater tool switch preheating reaches After preheating time, smoking machine starts to aspirate, and cambridge filter collects total granules.Canadian depth suction can be used in smoking machine suction Any one in pattern and iso standard suction mode.It is determined and is taken out according to the heating time of suction mode and heating utensil setting Suction inlet number, after reaching puff number, suction is completed.
- The method of cigarette smoke component 3. a kind of detection heating as described in claim 1 is not burnt, total grain in the step (4) The extraction of phase object：The cambridge filter for having trapped total granules in step (3) is put into extraction flask, 20-50mL steps (1) are added Inner mark solution, fully vibrate 0.5-2h after filter, obtain the extract liquor of total granules.
- The method of cigarette smoke component 4. a kind of detection heating as described in claim 1 is not burnt, gas phase in the step (5) The detector of chromatography is thermal conductivity detector (TCD) (TCD).
- The method of cigarette smoke component 5. a kind of detection heating as described in claim 1 is not burnt, gas phase in the step (5) The condition of chromatography is：DB-1701 fused quartz capillary chromatography columns, size are 30m × 0.32mm × 1.0 μm；Injector temperature It is 260 DEG C；Temperature programming：80 DEG C of holding 2.5min of initial temperature, rise to 250 DEG C with the rate of 40 DEG C/min, keep 3min；Carrier gas is Helium, flow rate of carrier gas 1.5mL/min, constant current mode；Make-up gas helium 30mL/min；Sampling volume is 1 μ L, and split sampling divides Flow ratio 5:1；260 DEG C of TCD detector temperatures.
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| CN114740126A (en) * | 2022-05-14 | 2022-07-12 | 河南中烟工业有限责任公司 | Method for determining quality of cigarette product containing bead blasting heating by using HPLC-IR-MS |
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