CN116465996A - Analysis method and application of main stream smoke components of cigarettes - Google Patents
Analysis method and application of main stream smoke components of cigarettes Download PDFInfo
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- CN116465996A CN116465996A CN202310440019.7A CN202310440019A CN116465996A CN 116465996 A CN116465996 A CN 116465996A CN 202310440019 A CN202310440019 A CN 202310440019A CN 116465996 A CN116465996 A CN 116465996A
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- 239000000779 smoke Substances 0.000 title claims abstract description 97
- 235000019504 cigarettes Nutrition 0.000 title claims abstract description 91
- 238000004458 analytical method Methods 0.000 title claims abstract description 73
- 238000001179 sorption measurement Methods 0.000 claims abstract description 61
- 238000000034 method Methods 0.000 claims abstract description 40
- 238000004451 qualitative analysis Methods 0.000 claims abstract 2
- 238000004445 quantitative analysis Methods 0.000 claims abstract 2
- 239000007789 gas Substances 0.000 claims description 53
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 30
- 239000002904 solvent Substances 0.000 claims description 20
- 239000002245 particle Substances 0.000 claims description 18
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 16
- 239000003463 adsorbent Substances 0.000 claims description 16
- 238000000605 extraction Methods 0.000 claims description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 14
- KNXMUFRWYNVISA-UHFFFAOYSA-N ethyl heptadecanoate Chemical compound CCCCCCCCCCCCCCCCC(=O)OCC KNXMUFRWYNVISA-UHFFFAOYSA-N 0.000 claims description 14
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
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- 238000000926 separation method Methods 0.000 claims description 10
- 229910052799 carbon Inorganic materials 0.000 claims description 8
- IAFQYUQIAOWKSB-UHFFFAOYSA-N Ethyl undecanoate Chemical compound CCCCCCCCCCC(=O)OCC IAFQYUQIAOWKSB-UHFFFAOYSA-N 0.000 claims description 7
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- 239000012159 carrier gas Substances 0.000 claims description 3
- 239000001307 helium Substances 0.000 claims description 3
- 229910052734 helium Inorganic materials 0.000 claims description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 3
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- 238000004949 mass spectrometry Methods 0.000 claims description 2
- 239000002808 molecular sieve Substances 0.000 claims description 2
- 238000004064 recycling Methods 0.000 claims description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 2
- 238000001514 detection method Methods 0.000 abstract description 22
- 150000001875 compounds Chemical class 0.000 abstract description 12
- 238000009835 boiling Methods 0.000 abstract description 11
- 230000035945 sensitivity Effects 0.000 abstract description 6
- 238000005259 measurement Methods 0.000 abstract description 2
- 239000012071 phase Substances 0.000 description 49
- 239000012808 vapor phase Substances 0.000 description 29
- 230000000391 smoking effect Effects 0.000 description 15
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 13
- 239000000126 substance Substances 0.000 description 10
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 8
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- 239000003480 eluent Substances 0.000 description 5
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- SNICXCGAKADSCV-JTQLQIEISA-N (-)-Nicotine Chemical compound CN1CCC[C@H]1C1=CC=CN=C1 SNICXCGAKADSCV-JTQLQIEISA-N 0.000 description 4
- 229910002091 carbon monoxide Inorganic materials 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 229960002715 nicotine Drugs 0.000 description 4
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000003795 desorption Methods 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- 239000002594 sorbent Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 2
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- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical compound CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 description 2
- 241000208125 Nicotiana Species 0.000 description 2
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 2
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- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- -1 aldehyde ketones Chemical class 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- HUMNYLRZRPPJDN-UHFFFAOYSA-N benzaldehyde Chemical compound O=CC1=CC=CC=C1 HUMNYLRZRPPJDN-UHFFFAOYSA-N 0.000 description 2
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- LELOWRISYMNNSU-UHFFFAOYSA-N hydrogen cyanide Chemical compound N#C LELOWRISYMNNSU-UHFFFAOYSA-N 0.000 description 2
- XMGQYMWWDOXHJM-UHFFFAOYSA-N limonene Chemical compound CC(=C)C1CCC(C)=CC1 XMGQYMWWDOXHJM-UHFFFAOYSA-N 0.000 description 2
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- 238000009423 ventilation Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- BSAXWMSAVVOOHO-UHFFFAOYSA-N 2,2-dioxo-1,5-dihydroimidazo[4,5-c][1,2,6]thiadiazin-4-one Chemical compound O=C1NS(=O)(=O)NC2=C1NC=N2 BSAXWMSAVVOOHO-UHFFFAOYSA-N 0.000 description 1
- HORQAOAYAYGIBM-UHFFFAOYSA-N 2,4-dinitrophenylhydrazine Chemical compound NNC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O HORQAOAYAYGIBM-UHFFFAOYSA-N 0.000 description 1
- NOEGNKMFWQHSLB-UHFFFAOYSA-N 5-hydroxymethylfurfural Chemical compound OCC1=CC=C(C=O)O1 NOEGNKMFWQHSLB-UHFFFAOYSA-N 0.000 description 1
- 244000198134 Agave sisalana Species 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
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- 150000001299 aldehydes Chemical class 0.000 description 1
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- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- QABCGOSYZHCPGN-UHFFFAOYSA-N chloro(dimethyl)silicon Chemical compound C[Si](C)Cl QABCGOSYZHCPGN-UHFFFAOYSA-N 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 239000003517 fume Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- RJGBSYZFOCAGQY-UHFFFAOYSA-N hydroxymethylfurfural Natural products COC1=CC=C(C=O)O1 RJGBSYZFOCAGQY-UHFFFAOYSA-N 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 229940087305 limonene Drugs 0.000 description 1
- 235000001510 limonene Nutrition 0.000 description 1
- 238000001819 mass spectrum Methods 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- QNGNSVIICDLXHT-UHFFFAOYSA-N para-ethylbenzaldehyde Natural products CCC1=CC=C(C=O)C=C1 QNGNSVIICDLXHT-UHFFFAOYSA-N 0.000 description 1
- 239000013618 particulate matter Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 238000000513 principal component analysis Methods 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
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- 238000010998 test method Methods 0.000 description 1
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- 239000012855 volatile organic compound Substances 0.000 description 1
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Classifications
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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
-
- 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
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/30—Control of physical parameters of the fluid carrier of temperature
-
- 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
- G01N30/50—Conditioning of the sorbent material or stationary liquid
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
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- 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)
Abstract
The invention discloses an analysis method of cigarette main stream smoke components, which comprises the steps of firstly capturing cigarette main stream smoke, then forming a sample to be tested from the captured cigarette main stream smoke components, and then carrying out qualitative and quantitative analysis by adopting a gas chromatography-mass spectrometer. The working conditions of the gas chromatograph-mass spectrometer comprise: two DB-WAX capillary columns were used in series. The analysis method is simple and efficient, effectively improves the detection rate of low boiling point compounds, and fills the blank in the field of detection of total components of main stream smoke of cigarettes for the first time; meanwhile, the method is also suitable for the independent detection and analysis of the components trapped by the Cambridge filter disc or the components trapped by the adsorption tube, and the measurement result has high sensitivity and accuracy and good repeatability. The analysis method can also be applied to distinguishing cigarettes of different specifications through the main stream smoke components of the cigarettes.
Description
Technical Field
The invention belongs to the technical field of tobacco chemistry, and particularly relates to an analysis method and application of a main stream smoke component of cigarettes.
Background
Cigarette smoke is the most complex system known in composition, and the number of chemical components currently identified from cigarette smoke is over 5000. The main stream smoke analysis of cigarettes firstly involves the generation and collection of smoke, the main stream smoke is generated by smoking a cigarette by a smoking machine, the smoke is divided into two parts of particle phase matters and gas phase matters by a Cambridge filter disc, the matters collected on the filter disc are defined as particle phase matters, the matters passing through the filter disc are defined as gas phase matters, and the gas phase matters are collected by a gas collecting bag. The entrapment efficiency of the Cambridge filter disc on particles with the diameter of 0.1 mu m and above reaches 99.7 percent, and the entrapment rate of nicotine on the Cambridge filter disc is almost 100 percent. The total particulate matter is obtained by subtracting nicotine and water, and is the dry tar. The carbon monoxide permanent gas is not trapped on the filter disc, and can not be adsorbed or reacted in the gas collecting bag, and the carbon monoxide content can be directly measured by an infrared method. Therefore, the conventional testing (tar, nicotine and carbon monoxide) method of the main stream smoke of the cigarette is mature and reliable.
However, this does not mean that all the smoke constituents can be clearly separated into two phases of gas particles, and that a large amount of volatile or semi-volatile smoke constituents are distributed in both phases of gas particles. The gas particles are distributed in two phases at different degrees due to the moisture of the flue gas and the volatile organic compounds with the molecular weight of 60-200. The gas-particle two-phase coexisting material is generally referred to as "organic vapor phase" (organic vapor phase) or simply "vapor phase" (vapor phase). According to the analysis by Norman et al, lorilard tobacco Inc., U.S., the mass composition of mainstream cigarette smoke is approximately as follows: 58% of nitrogen, 12% of oxygen, 13% of carbon dioxide, 3.5% of carbon monoxide, 0.5% of hydrogen and argon, 8% of particulate matters and 5% of vapor phase. The vapor phase further comprises: 40% of hydrocarbon, 20% of water, 14% of aldehyde, 9% of ketone, 6% of nitrile, 1.5% of alcohol, 1.5% of oxygen-containing heterocycle, 1% of ester and 7% of miscellaneous items. Many vapor phase components have flavor or irritation, have a close relationship with the quality of the flue gas, and also belong to harmful components such as hydrogen cyanide, volatile aldehyde ketones and the like.
The technology for collecting and analyzing particulate matters of main stream smoke of cigarettes is mature, but the technology for collecting gas phase and two-phase coexisting components has a plurality of problems. The gas phase-vapor phase component collecting method mainly comprises an air bag, a cold trap, a thermal desorption tube and a filter disc dipping. The gas pocket collection method has adsorption, deposition and side reaction, and the vapor phase component can not be measured almost. The cold trap trapping method has complex operation and lower sensitivity, and is mainly used for detecting partial vapor phase components. The thermal desorption tube has large resistance, affects the suction curve, and is incomplete in desorption and even decomposition of partial smoke components. The filter impregnation method is only suitable for specific smoke components, for example, a filter impregnated with 2, 4-Dinitrophenylhydrazine (DNPH) reagent can effectively trap aldehyde ketones in the gas phase and the vapor phase. In general, current methods for detecting total components of main stream smoke of cigarettes are roughly divided into 3 main categories according to trapping methods: (1) a particulate phase, (2) a gas phase, and (3) a vapor phase. At present, a method for measuring the total components (including vapor phase materials with two coexisting phases) of main stream smoke gas and particle two phases of cigarettes is not available.
Therefore, there is a strong need for an analytical method that is simple to operate and that can determine the total composition of the mainstream smoke of a cigarette.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, an object of the present invention is to provide a method for analyzing the composition of mainstream smoke of a cigarette.
To achieve the above and other related objects, the present invention is achieved by the following technical means.
The invention provides a method for analyzing components of main stream smoke of cigarettes, which comprises the steps of firstly capturing the main stream smoke of the cigarettes, then forming the captured components of the main stream smoke of the cigarettes into a sample to be tested, and then completing detection analysis of the components of the main stream smoke of the cigarettes by using a gas chromatograph-mass spectrometer.
According to the analysis method, the working conditions of the gas chromatography-mass spectrometer comprise: two DB-WAX capillary columns (120 m. Times.0.32 mm. Times.0.25 μm) were connected in series. The single DB-WAX chromatographic column (60 m multiplied by 0.32mm multiplied by 0.25 mu m) has poor separation effect on low boiling point components, cannot realize the full component analysis in cigarette smoke, has good separation effect on the low boiling point components when the serial chromatographic columns are used for smoke component analysis, and the boiling point of detected compounds is covered at-10-350 ℃.
According to the analysis method, the main stream smoke of the cigarettes is captured by adopting the Cambridge filter disc and then captured by adopting the adsorption tube, and the adsorption tube is filled with the adsorbent. The method for collecting the smoke by connecting the Cambridge filter disc and the self-made adsorption tube in series and the analysis method for optimizing the use of the gas chromatography-mass spectrometer realize the determination of the total composition of the main stream smoke of the cigarettes for the first time, and the determination result has high sensitivity, accuracy and good repeatability. In addition, the adsorption tube device used in the analysis method is simple, high in trapping efficiency, free from influencing the suction curve and reusable.
According to the analysis method, the process of forming the sample to be tested comprises separation, and the separation comprises solvent elution and extraction of the flue gas.
According to the analysis method, the solvent in the separation process is an organic solvent. Preferably, the organic solvent comprises one or more of methanol, n-hexane, methylene chloride, methyl tert-butyl ether.
According to the analysis method, the extraction mode is oscillation extraction. Preferably, the extraction is carried out at a speed of 200r/min for 30min.
According to the analysis method, an internal standard solution needs to be added during the extraction, and the configuration of the internal standard solution comprises taking isopropanol as a solvent and ethyl undecanoate, isobutyl acetate, isobutyl caproate and ethyl heptadecanoate as internal standards. The concentration of the internal standard solution is 2-4 mg/mL. Preferably, the concentration of the internal standard solution may be 2 to 3mg/mL, or 3 to 4mg/mL, and in some embodiments, 2mg/mL.
According to the analysis method, the length of the adsorption tube is 8-12 cm, and the inner diameter is 6-8 mm. Preferably, the outer diameter of the adsorption tube is 9mm.
Preferably, the tube length may be 8 to 9cm, may be 9 to 11cm, may be 11 to 12cm, and in some embodiments is 10, 12cm.
Preferably, the inner diameter may be 6 to 7mm, or 7 to 8mm, and in some embodiments 6, 8mm.
Preferably, the adsorption tube is a deactivation glass tube, and the deactivation mode is as follows: firstly, cleaning a glass tube by using 1mol/L HCl, then cleaning the glass tube by using acetone, and drying; then, soaking the glass tube for 12 hours by using 5% DMCS/n-hexane solution, taking out, washing by using the n-hexane solution, and soaking by using methanol for 2 hours after micro-drying; after methanol is dried to a certain degree, soaking the glass tube in n-hexane solution, taking out and air-drying; finally, the mixture is dried in an oven at the temperature of 250-280 ℃ for a plurality of hours and is preserved after being cooled.
The adsorbent comprises one or more of activated carbon, carbon molecular sieve, or Carbotrap349, in certain specific embodiments activated carbon, according to the analytical methods described above.
According to the analysis method, the content of the adsorbent in the single adsorption tube is 0.3-0.6 g, and the particle size of the adsorbent is 60-80 meshes. Preferably, the adsorbent may be present in an amount of 0.3 to 0.4g, 0.4 to 0.5g, or 0.5 to 0.6g, and in some embodiments, 0.4, 0.5 and 0.6g. Too little adsorbent can cause penetration of compounds, and the adsorption effect is reduced; too much amount causes an increase in resistance and thus affects the suction curve.
According to the analysis method, one end of the adsorption tube is connected with the Cambridge filter holder, the other end of the adsorption tube is connected with a piston of the smoking machine, and main stream smoke passes through the Cambridge filter and is trapped by the adsorption tube.
According to the above analysis method, the adsorption tube is suitable for regeneration for recycling, and the regeneration method is as follows: residual solvent in the eluted adsorption tube is volatilized, and then high-temperature treatment is carried out under inert gas.
According to the analysis method, the inert gas is nitrogen, and the flow rate is 20-150 mL/min; preferably, the flow rate may be 20 to 80mL/min, 80 to 100mL/min, or 100 to 150mL/min, and in some embodiments 100mL/min
According to the analysis method, the high temperature is 150-200 ℃; preferably, the elevated temperature may be 150 to 160 ℃, may be 160 to 180 ℃, may be 180 to 200 ℃, and in some specific embodiments, is 190 ℃.
According to the analysis method, the treatment time at the high temperature is 20-120 min; preferably, the treatment time may be 20 to 45 minutes, may be 45 to 80 minutes, may be 80 to 120 minutes, and in some embodiments is 60 minutes.
According to the analysis method, the gas chromatography conditions of the gas chromatography-mass spectrometer comprise the temperature of the sample inlet of 240-260 ℃; preferably, the inlet temperature may be 240 to 250 ℃, or 250 to 260 ℃, in some embodiments 250 ℃.
According to the above analysis method, the gas chromatography conditions of the gas chromatography-mass spectrometer include a column temperature rising procedure: maintaining the temperature at 30-50 ℃ for 10-20 min, raising the temperature to 230-250 ℃ at 2-5 ℃/min, and maintaining the temperature for 3-7 min; preferably, the column temperature increase procedure is 15min at 35 ℃,2 ℃/min to 240 ℃, 5min. The initial temperature of the column temperature is lower, so that the low-boiling-point components are completely separated as far as possible, the peak shape of the chromatographic column is not easy to trailing, the peak width of a sample solvent peak is narrowed, the peak height is high, the separation degree between the solvent peak and a low-boiling-point target peak is effectively improved, the covering of the sample components flowing out in early stage is avoided, and the full-component analysis is realized.
According to the analysis method, the gas chromatography conditions of the gas chromatography-mass spectrometer comprise that the carrier gas is helium (more than or equal to 99.999%).
According to the analysis method, the gas chromatography-mass spectrometer has the advantages that the gas chromatography condition comprises the selection of a constant-current mode, and the flow rate is 1-5 mL/min; preferably, the flow rate may be 1 to 2mL/min, may be 2 to 3mL/min, may be 3 to 5mL/min, and in some embodiments is 2mL/min.
According to the analysis method, the gas chromatography conditions of the gas chromatography-mass spectrometer comprise a split ratio of 5:1-20:1; preferably, the split ratio may be from 5:1 to 10:1, from 10:1 to 15:1, and from 10:1 to 20:1, and in some embodiments, from 5:1. The split ratio is too small, the initial bandwidth is enlarged to affect separation, the peak of the low boiling point component is affected, and the split ratio is too large to affect analysis sensitivity.
According to the analysis method, the gas chromatography-mass spectrometry conditions of the gas chromatography-mass spectrometer comprise the temperature of an ion source of 220-240 ℃; preferably, the ion source temperature may be 220-225 ℃. May be 225 to 235 c or 235 to 240 c, and in some embodiments 230 c.
According to the analysis method, the gas chromatography-mass spectrometry conditions of the gas chromatography-mass spectrometer comprise quadrupole rod temperature 140-160 ℃; preferably, the quadrupole rod temperature may be 140-145 ℃. May be 145 to 155 c or 155 to 160 c, and in some embodiments 150 c.
According to the analysis method, the gas chromatography-mass spectrometry conditions of the gas chromatography-mass spectrometer comprise a transmission line temperature of 230-250 ℃; preferably, the transmission line temperature may be 230-235 ℃. May be 235 to 245 c or 245 to 250 c, and in some embodiments 240 c.
According to the analysis method, the gas chromatography-mass spectrometry conditions of the gas chromatography-mass spectrometer comprise a full scanning mode and a scanning range of 33-350 amu.
In a second aspect, the present invention provides a use of the analysis method described above for differentiating cigarettes of different specifications by the composition of the mainstream smoke of the cigarettes.
At present, the collection technology of the gas phase and the two-phase coexisting components of the main stream smoke of the cigarette has a plurality of problems, and compared with other technical means for capturing the gas phase and the vapor phase of the smoke, the adsorption tube used in the analysis method has a simple structure, is adaptive to a smoking machine and has high capturing efficiency, and the smoking curve is not influenced. In addition, the analysis method of the main stream smoke components of the cigarettes provided by the application fills the blank that the total components of the cigarettes cannot be measured at present for the first time.
As described above, the invention provides a method for analyzing the components of main stream smoke of cigarettes, which has the following beneficial effects:
1) The invention provides an analysis method of total components of main stream smoke of cigarettes, which connects a traditional Cambridge filter disc with a self-made adsorption tube in series, so that synchronous trapping of gas phase, particle phase and vapor phase components of the main stream smoke of cigarettes is realized, and the analysis method is fast and efficient. Meanwhile, through optimizing the use condition of the gas chromatograph-mass spectrometer, the detection rate of low boiling point compounds is effectively improved, the boiling point of the detected compounds is covered at-10 to 350 ℃, the analysis and detection of the total components of the main stream smoke are realized, and the measurement result has high sensitivity and accuracy and good repeatability.
2) The analysis method is not only suitable for detecting the total components of the main stream smoke of the cigarettes, but also suitable for separately detecting and analyzing the components trapped by the Cambridge filter disc or the components trapped by the adsorption tube. At present, different chromatographic analysis methods are generally adopted for gas phase components and particle phase components of main stream smoke of cigarettes, the pretreatment conditions and the chromatographic analysis conditions of the methods are different, and compared with the existing gas phase and particle phase component independent analysis technology, the analysis method can be suitable for detection and analysis of all components of main stream smoke of cigarettes or the components trapped by a Cambridge filter disc or the components trapped by an adsorption tube, and the operability is greatly improved.
3) Compared with the analysis method which can only simply study the gas phase components or the grain phase components, the method avoids the follow-up complex quantitative or conversion process, is simple and efficient, has high accuracy and provides theoretical support for the study of tar reduction, harm reduction and the like of cigarettes; in addition, the analysis method can also distinguish cigarettes with different specifications through the main components of the cigarette smoke.
4) The adsorption tube used in the analysis method has the technical advantages of simple structure, high trapping efficiency, adaptation with a smoking machine and no influence on a smoking curve. The invention also provides a regeneration method of the adsorption tube, so that the adsorption tube can be reused, and the cost is saved.
Drawings
FIG. 1 shows an adsorbent tube particularly useful in embodiments of the present invention.
Fig. 2 shows a main stream smoke trapping apparatus for cigarettes specifically used in the examples of the present invention.
FIG. 3 shows a chromatogram of the capture composition of the main stream smoke of a Kentucky 3R4F reference cigarette in example 1 of the present invention by Cambridge filter and sorbent tube.
Fig. 4 shows a chromatogram of the main stream smoke trapped by the adsorption tube of the kentucky 3R4F reference cigarette in example 2 of the present invention.
Fig. 5 shows a main component load diagram of main stream smoke of conventional, medium-grade and fine-grade cigarettes in example 3 of the present invention.
Fig. 6 is a graph showing the comparison of the distribution ratio of vapor phase substances in the gas phase portion and the particulate phase portion of the mainstream smoke of a cigarette in example 4 of the present invention.
FIG. 7 shows a total ion flow chromatogram after eluting the regenerated adsorption tube with a solvent in example 5 of the present invention.
Wherein reference numerals in fig. 2 are as follows:
1 cigarette holder
2 Cambridge filter disc holder
3 adsorption tube
4 smoking machine piston
Detailed Description
Embodiments of the present invention are described below by way of specific examples for verifying the realistic feasibility of the method of the present invention. Other advantages and effects of the present invention will be readily apparent to those skilled in the art from the present disclosure. The invention may be practiced or carried out in other embodiments that depart from the specific details, and the details of the present description may be modified or varied from the spirit and scope of the present invention.
It should be understood that the process equipment or devices not specifically identified in the examples below are all conventional in the art. Furthermore, it is to be understood that the scope of the invention is not limited to the specific embodiments described below, and that one or more of the method steps mentioned in the invention does not exclude the presence of other method steps before or after the combination step or that other method steps may be inserted between these explicitly mentioned steps, unless otherwise indicated. It is also to be understood that the terminology used in the examples of the invention is for the purpose of describing particular embodiments only, and is not intended to limit the scope of the invention. The test methods in the following examples, in which specific conditions are not noted, are generally conducted under conventional conditions or under conditions recommended by the respective manufacturers.
In the following embodiments of the present application, a main stream smoke trapping device for cigarettes as shown in fig. 2 is specifically adopted. The smoke trapping device comprises a cigarette holder 1, a Cambridge filter holder 2, an adsorption tube 3 and a smoking machine piston 4; the cigarette is fixed on the cigarette holder 1, the Cambridge filter disc is fixed on the Cambridge filter disc holder 2, the cigarette holder 1 is directly connected with the Cambridge filter disc holder 2, the Cambridge filter disc holder 2 is communicated with the adsorption tube 3 through a pipeline, one end of the adsorption tube 3 is connected with the Cambridge filter disc holder 2, and the other end is connected with the piston 4 of the smoking machine.
When the specific cigarette main stream smoke trapping device shown in fig. 2 is adopted for smoke trapping, the cigarettes are fixed on the cigarette holder 1, the Cambridge filter disc is fixed on the Cambridge filter disc holder 2, and a smoking machine is started to smoke the cigarettes after the cigarettes are ignited. The flue gas is captured through the Cambridge filter disc and then is captured through the adsorption tube 3 along the pipeline.
In a preferred embodiment, the sisal filter has a gauge of 92mm.
In a preferred embodiment, the length of the adsorbent tube is 10-12 cm, the inner diameter of the adsorbent tube is 6-8 mm, and the outer diameter is 9mm.
In a preferred embodiment, the adsorbent in the adsorbent tube is activated carbon in an amount of 0.4 to 0.6g.
Example 1
In this embodiment, a method for analyzing components of main stream smoke of a cigarette is provided, including the following steps:
1) Trapping of flue gases
And (3) sucking the Kentucky 3R4F reference cigarettes by a smoking machine, wherein main stream smoke of 20 cigarettes firstly passes through a 92mm Cambridge filter disc, is trapped by the filter disc, and the smoke passing through the filter disc is trapped by an adsorption tube (the adsorption tube has the length of 10cm and the inner diameter of 6mm and is filled with 0.4g of active carbon).
2) Solvent elution and extraction
The filter was transferred to a conical flask, 10mL of methylene chloride was added, the adsorption tube was rinsed with 10mL of methylene chloride, the eluent was also collected in the conical flask, and then 100. Mu.L of an internal standard solution (isopropanol as a solvent, containing 2mg/mL of ethyl undecanoate, isobutyl acetate, isobutyl caproate, ethyl heptadecanoate) was added, followed by shaking extraction at a rate of 200r/min for 30min.
3) Smoke component detection
Taking 1mL of supernatant into a chromatographic bottle, and carrying out smoke component analysis by combining an Agilent 7890B gas chromatograph and an Agilent 5977A mass spectrometer, wherein gas chromatography-mass spectrometry parameters are set as follows:
gas chromatography parameters: the sample injection volume is 2 mu L; the temperature of the sample inlet is 250 ℃; the split ratio is 5:1; column temperature rising procedure: maintaining at 35deg.C for 15min, and increasing at 2deg.C/min to 240 deg.C for 5min; the carrier gas is helium (more than or equal to 99.999 percent); chromatographic column: DB-WAX capillary column (120 m x 0.32mm x 0.25 μm), constant flow mode, flow rate 2.0mL/min.
Mass spectrometry parameters: EI source, voltage 70eV, full scan mode, scan range 33-350 amu, ion source temperature 230 ℃, quadrupole temperature 150 ℃, transmission line temperature 240 ℃, solvent delay 7min,18.3min-20.0min mass spectrum filament closing.
The detection results of the main stream smoke components of the Kentucky 3R4F reference cigarettes are shown in table 1.
TABLE 1
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Note that: "a" represents a gas-phase compound, "b" represents a particulate-phase compound, and "c" represents a gas-particulate two-phase compound
The component chromatogram of the main stream smoke of the Kentucky 3R4F reference cigarette is shown in figure 3. As can be seen from Table 1 and FIG. 3, 269 compounds were identified accurately and qualitatively in this analytical method, of which 153 were the gas phase components, 203 were the grain phase components, and 87 were the two phase common components. The relative deviations of the results of 3 times per day and 6 days in succession and 18 times are shown in Table 1. Wherein, the RSD of 266 components is between 0.56% and 14.93%, and the RSD of 260 components is within 10%.
In conclusion, the method disclosed by the invention has the advantages of high sensitivity, high boiling point coverage of the detected compounds of-10-350 ℃, realization of analysis and detection of the total components of the main stream smoke, good repeatability of detection results and stable and reliable results.
Example 2
In this embodiment, a method for analyzing components of main stream smoke of a cigarette is provided, including the following steps:
1) Trapping of flue gases
And (3) sucking the Kentucky 3R4F reference cigarettes by a smoking machine, wherein main stream smoke of 20 cigarettes firstly passes through a 92mm Cambridge filter disc, is trapped by the filter disc, and the smoke passing through the filter disc is trapped by an adsorption tube (the adsorption tube has the length of 10cm and the inner diameter of 6mm and is filled with 0.4g of active carbon).
2) Solvent elution and extraction
The adsorption tube was rinsed with 10mL of methylene chloride, the rinsed solution was collected in a conical flask, and then 100. Mu.L of an internal standard solution (isopropanol as a solvent, containing 2mg/mL of ethyl undecanoate, isobutyl acetate, isobutyl caproate, ethyl heptadecanoate) was added thereto, followed by shaking extraction at a rate of 200r/min for 30min.
3) Smoke component detection
1mL of the supernatant was taken into a chromatographic bottle, and gas chromatography-mass spectrometry detection analysis was performed. The gas chromatograph-mass spectrometer conditions were the same as in example 1.
The detection results of the smoke components captured by the adsorption tube in the main stream smoke of the Kentucky 3R4F reference cigarette are shown in Table 2.
TABLE 2
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Note that: "a" represents a gas-phase compound and "c" represents a gas-particle two-phase compound
The chromatogram of the smoke components captured by the adsorption tube in the main stream smoke of the Kentucky 3R4F reference cigarette is shown in figure 4. As can be seen from Table 2 and FIG. 4, 153 gas phase components, 87 of which belong to the two-phase common component, were accurately and qualitatively identified by the present analysis method.
The relative deviation of the results was measured 3 times a day in parallel, 6 days in succession, 18 times. The RSD of the 149 components is between 0.86% and 11.29%, and the RSD of the 145 components is within 10%. The analysis method disclosed by the invention can be independently used for measuring the components of the trapped smoke (gas phase-vapor phase) of the adsorption tube, and has the advantages of good repeatability of analysis results and stable and reliable detection results.
Example 3
In this embodiment, the main stream smoke components of conventional, medium-count and fine-count experimental cigarette samples are detected respectively, including the following steps:
1) Trapping of flue gases
The conventional cigarettes are smoked by a smoking machine, main stream smoke of 20 cigarettes firstly passes through a 92mm Cambridge filter disc, is trapped by the filter disc, and the smoke passing through the filter disc is trapped by an adsorption tube (the length of the adsorption tube is 12cm, the inner diameter is 8mm, and 0.6g of active carbon is filled).
2) Solvent elution and extraction
The filter was transferred into a conical flask, 20mL of methylene chloride was added, the adsorption tube was rinsed with 10mL of methylene chloride, the eluent was also collected in the conical flask, and then 100. Mu.L of an internal standard solution (isopropanol as a solvent, containing 2mg/mL of ethyl undecanoate, isobutyl acetate, isobutyl caproate, ethyl heptadecanoate) was added, followed by shaking extraction at a rate of 200r/min for 30min.
3) Smoke component detection
1mL of the supernatant was placed in a chromatographic bottle, and a gas chromatograph of Agilent 7890B and a mass spectrometer of Agilent 5977A were used in combination for smoke analysis. The gas chromatograph-mass spectrometer conditions were the same as in example 1.
The middle and fine experimental cigarette samples were also analyzed using the above-described analysis methods.
3 samples are tested in parallel, the principal component analysis is carried out on the detection result, and a load diagram is obtained by adopting chempatten software. The load diagram is a graphical method for representing the components of a complex mixture, which can present the relative amounts of the various components, thereby presenting the composition of the components of the cigarette smoke and helping people to better understand the components of the mixture. The load diagram is shown in fig. 5, and the detection results of cigarettes with different specifications can be obviously distinguished into 3 groups, which shows that the analysis method of the invention can be used for distinguishing cigarettes with different specifications through the main stream smoke components of the cigarettes.
Example 4
In this embodiment, an analysis method of main stream smoke components of a cigarette is provided, which is used for examining the distribution proportion of vapor phase matters in gas phase and particle phase in main stream smoke components of the cigarette, and includes the following steps:
1) Trapping of flue gases
And (3) sucking the Kentucky 3R4F reference cigarettes by a smoking machine, wherein main stream smoke of 20 cigarettes is firstly trapped by a 92mm Cambridge filter disc, and the smoke passing through the filter disc is trapped by an adsorption tube (the adsorption tube has the length of 10cm and the inner diameter of 6mm and is filled with 0.5g of active carbon).
2) Solvent elution and extraction
The adsorption tube was rinsed with 10mL of methylene chloride and collected in a conical flask, 100. Mu.L of an internal standard solution (isopropyl alcohol as a solvent, containing 2mg/mL of ethyl undecanoate, isobutyl acetate, isobutyl caproate, ethyl heptadecanoate) was added to obtain an adsorption tube eluent, and then the extraction was performed at a rate of 200r/min with shaking for 30min.
The filter was transferred to another Erlenmeyer flask, 20mL of methylene chloride was added and 100. Mu.L of an internal standard solution (isopropanol as solvent, containing 2mg/mL of ethyl undecanoate, isobutyl acetate, isobutyl caproate, ethyl heptadecanoate) was added to obtain filter eluate, which was then extracted by shaking at 200r/min for 30min.
3) Smoke component detection
Taking 1mL of supernatant extracted by the eluent of the adsorption tube into a chromatographic bottle, and carrying out gas chromatography-mass spectrometry detection analysis, wherein the conditions of a gas chromatography-mass spectrometry instrument are the same as in example 1.
The supernatant 1mL extracted from the filter eluent was put into a chromatographic bottle, and subjected to gas chromatography-mass spectrometry detection analysis, and the gas chromatography-mass spectrometry instrument conditions were the same as in example 1.
The chromatogram of the components trapped by the sorbent tube (gas-vapor phase) and the filter (particulate-vapor phase) in the mainstream cigarette smoke of the kentucky 3R4F reference cigarette is shown in fig. 6. Wherein fig. 6 shows a chromatogram of the components trapped by the sorbent tube in the mainstream smoke. Wherein, the peak of the grain phase part is an internal standard peak; FIG. 6 is a chromatogram of the components captured by the Cambridge filter in mainstream smoke. Wherein the peaks of the gas phase part are internal standard peaks and solvent peaks.
By means of fig. 6, the distribution condition of vapor phase matters in the main stream smoke of the cigarettes in the gas-particle two-phase part can be intuitively judged. Low boiling point substances such as 1, 3-butadiene, isoprene and benzene are found only in the components trapped by the adsorption tube, and high boiling point substances such as 5-hydroxymethylfurfural, nicotine and dihydric phenol are found only in the components trapped by the Cambridge filter; the vapor phase substances such as toluene, pyridine, limonene, styrene, benzaldehyde and the like are trapped by the Cambridge filter and the adsorption tube, but the content difference of the trapped substances is large, and the proportion of the vapor phase substances distributed in the vapor phase part gradually decreases and the proportion of the vapor phase substances distributed in the particle phase part gradually increases as the boiling point of the vapor phase substances increases.
In summary, the analysis method of the application can be used for observing the distribution proportion of vapor phase substances in the main stream smoke of cigarettes in a gas phase part (gas phase-vapor phase) and a particle phase part (gas phase-vapor phase). Compared with an analysis method which can only simply study gas phase components or grain phase components, the method avoids the follow-up complex quantitative or conversion process, is simple and efficient to operate and high in accuracy, provides a more strict means for studying the influence of ventilation dilution on the main stream smoke components of cigarettes, and can be used for designing parameters of cigarettes with different ventilation dilution rates.
Example 5
In this example, the effect of regeneration of the adsorption tube used in the present application was examined.
The adsorption tube eluted in example 4 was placed in a fume hood to allow the residual solvent to evaporate naturally. Then high-temperature regeneration treatment is carried out under the condition of nitrogen, the flow rate of the nitrogen is 100mL/min, the high-temperature is 190 ℃, and the treatment time is 60min.
The regenerated adsorption tube is rinsed with 10mL of dichloromethane, the rinsing liquid is collected in an conical flask, the rinsing liquid is extracted by shaking, 1mL of supernatant is taken into a chromatographic flask, and gas chromatography-mass spectrometry detection analysis is carried out, and the conditions of a gas chromatography-mass spectrometry instrument are the same as in example 1.
The regenerated blank adsorption tube is eluted by solvent, and the gas chromatography-mass spectrometry total ion flow chromatogram is shown in figure 7. As can be seen from fig. 7, the background interference of the regenerated adsorption tube chromatogram is extremely low. This shows that the regenerated adsorption tube has no residual matters, and the original activity is recovered, so that the stable trapping efficiency is ensured. The regeneration method of the invention enables the adsorption tube to be reusable, and has simple and convenient operation and cost saving.
The above embodiments are merely illustrative of the principles of the present invention and its effectiveness, and are not intended to limit the invention. Modifications and variations may be made to the above-described embodiments by those skilled in the art without departing from the spirit and scope of the invention. Accordingly, it is intended that all equivalent modifications and variations of the invention be covered by the claims, which are within the ordinary skill of the art, be within the spirit and scope of the present disclosure.
Claims (10)
1. The analysis method of the main stream smoke components of the cigarettes is characterized in that the main stream smoke of the cigarettes is captured firstly, the captured main stream smoke components of the cigarettes form a sample to be tested, and then qualitative and quantitative analysis is carried out by adopting a gas chromatograph-mass spectrometer; the working conditions of the gas chromatograph-mass spectrometer comprise: two DB-WAX capillary columns were used in series.
2. The analysis method according to claim 1, wherein the main stream smoke of the cigarettes is captured by a Cambridge filter and then captured by an adsorption tube, and the adsorption tube is filled with an adsorbent;
and/or the process for forming the sample to be tested comprises separation, wherein the separation comprises solvent elution and extraction, and an organic solvent is adopted in the separation process.
3. The method of claim 2, wherein the organic solvent comprises one or more of methanol, n-hexane, methylene chloride, methyl tertiary butyl ether;
and/or, the extraction requires the addition of an internal standard solution.
4. The method according to claim 3, wherein the internal standard solution uses isopropyl alcohol as a solvent, and ethyl undecanoate, isobutyl acetate, isobutyl caproate, and ethyl heptadecanoate as internal standards, and the concentration of the internal standard solution is 2-4 mg/mL.
5. The method according to claim 2, wherein the adsorption tube has a length of 8 to 12cm and an inner diameter of 6 to 8mm;
and/or the content of the adsorbent in the single adsorption tube is 0.3-0.6 g;
and/or the particle size of the adsorbent is 60-80 meshes;
and/or the adsorbent comprises one or more of activated carbon, carbon molecular sieve, or Carbotrap 349.
6. The method of claim 1, wherein the gas chromatographic conditions of the gas chromatograph-mass spectrometer include one or more of the following:
the temperature of the sample inlet is 240-260 ℃;
column temperature rising procedure: maintaining the temperature at 30-50 ℃ for 10-20 min, raising the temperature to 230-250 ℃ at 2-5 ℃/min, and maintaining the temperature for 3-7 min;
the carrier gas is helium;
constant flow mode, flow rate is 1-5 mL/min;
the split ratio is 5:1-20:1.
7. The method of claim 1, wherein the mass spectrometry conditions of the gas chromatograph-mass spectrometer include one or more of the following:
the temperature of the ion source is 220-240 ℃;
the temperature of the quadrupole rods is 140-160 ℃;
the temperature of the transmission line is 230-250 ℃;
full scan mode, scan range 33-350 amu.
8. The method of analysis according to claim 2, wherein the adsorbent tube is regenerated for recycling, the method of regeneration comprising: residual solvent in the eluted adsorption tube is volatilized, and then high-temperature treatment is carried out under inert gas.
9. The method according to claim 7, wherein the inert gas is nitrogen at a flow rate of 20 to 150mL/min;
and/or the high-temperature treatment temperature is 150-200 ℃ and the time is 20-120 min.
10. Use of an analysis method according to any one of claims 1 to 9 for differentiating cigarettes of different specifications by the composition of the mainstream smoke of the cigarette.
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