CN105866351A - Method for quickly measuring harmful ingredients in main stream smoke of cigarette - Google Patents
Method for quickly measuring harmful ingredients in main stream smoke of cigarette Download PDFInfo
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- CN105866351A CN105866351A CN201610389374.6A CN201610389374A CN105866351A CN 105866351 A CN105866351 A CN 105866351A CN 201610389374 A CN201610389374 A CN 201610389374A CN 105866351 A CN105866351 A CN 105866351A
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- cigarette
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- filter disc
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- 235000019504 cigarettes Nutrition 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 30
- 239000000779 smoke Substances 0.000 title claims abstract description 29
- 239000004615 ingredient Substances 0.000 title abstract 4
- 238000001514 detection method Methods 0.000 claims abstract description 56
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims abstract description 44
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000002904 solvent Substances 0.000 claims abstract description 40
- 230000000391 smoking effect Effects 0.000 claims abstract description 29
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims abstract description 25
- MLUCVPSAIODCQM-NSCUHMNNSA-N crotonaldehyde Chemical compound C\C=C\C=O MLUCVPSAIODCQM-NSCUHMNNSA-N 0.000 claims abstract description 21
- MLUCVPSAIODCQM-UHFFFAOYSA-N crotonaldehyde Natural products CC=CC=O MLUCVPSAIODCQM-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 20
- 229910002091 carbon monoxide Inorganic materials 0.000 claims abstract description 20
- LELOWRISYMNNSU-UHFFFAOYSA-N hydrogen cyanide Chemical compound N#C LELOWRISYMNNSU-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000007789 gas Substances 0.000 claims abstract description 10
- 235000002637 Nicotiana tabacum Nutrition 0.000 claims abstract description 5
- 239000007788 liquid Substances 0.000 claims abstract description 4
- 238000004811 liquid chromatography Methods 0.000 claims abstract 2
- 239000003546 flue gas Substances 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- 239000008367 deionised water Substances 0.000 claims description 18
- 229910021641 deionized water Inorganic materials 0.000 claims description 18
- 239000003517 fume Substances 0.000 claims description 16
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 12
- 239000003153 chemical reaction reagent Substances 0.000 claims description 12
- 238000004128 high performance liquid chromatography Methods 0.000 claims description 10
- 150000002500 ions Chemical class 0.000 claims description 10
- 238000004587 chromatography analysis Methods 0.000 claims description 9
- 238000001212 derivatisation Methods 0.000 claims description 6
- 238000000605 extraction Methods 0.000 claims description 6
- 238000012360 testing method Methods 0.000 claims description 6
- HORQAOAYAYGIBM-UHFFFAOYSA-N 2,4-dinitrophenylhydrazine Chemical compound NNC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O HORQAOAYAYGIBM-UHFFFAOYSA-N 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 4
- 244000061176 Nicotiana tabacum Species 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- 150000001728 carbonyl compounds Chemical class 0.000 claims description 4
- 238000001819 mass spectrum Methods 0.000 claims description 4
- XKLJHFLUAHKGGU-UHFFFAOYSA-N nitrous amide Chemical compound ON=N XKLJHFLUAHKGGU-UHFFFAOYSA-N 0.000 claims description 4
- 239000013618 particulate matter Substances 0.000 claims description 4
- 150000002989 phenols Chemical class 0.000 claims description 4
- 239000000523 sample Substances 0.000 claims description 4
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 239000012488 sample solution Substances 0.000 claims description 3
- FLAQQSHRLBFIEZ-UHFFFAOYSA-N N-Methyl-N-nitroso-4-oxo-4-(3-pyridyl)butyl amine Chemical compound O=NN(C)CCCC(=O)C1=CC=CN=C1 FLAQQSHRLBFIEZ-UHFFFAOYSA-N 0.000 abstract description 18
- 238000004458 analytical method Methods 0.000 abstract description 5
- 241000208125 Nicotiana Species 0.000 abstract 1
- 238000004255 ion exchange chromatography Methods 0.000 abstract 1
- 238000010561 standard procedure Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 24
- 229940105305 carbon monoxide Drugs 0.000 description 16
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 5
- 229940079593 drug Drugs 0.000 description 4
- 239000003814 drug Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- FLAQQSHRLBFIEZ-MNYIHESISA-N n-methyl-n-[4-oxo-4-(2,4,5,6-tetradeuteriopyridin-3-yl)butyl]nitrous amide Chemical compound [2H]C1=NC([2H])=C(C(=O)CCCN(C)N=O)C([2H])=C1[2H] FLAQQSHRLBFIEZ-MNYIHESISA-N 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000003556 assay Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 2
- 229910021642 ultra pure water Inorganic materials 0.000 description 2
- 239000012498 ultrapure water Substances 0.000 description 2
- SNICXCGAKADSCV-JTQLQIEISA-N (-)-Nicotine Chemical compound CN1CCC[C@H]1C1=CC=CN=C1 SNICXCGAKADSCV-JTQLQIEISA-N 0.000 description 1
- WDCYWAQPCXBPJA-UHFFFAOYSA-N 1,3-dinitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC([N+]([O-])=O)=C1 WDCYWAQPCXBPJA-UHFFFAOYSA-N 0.000 description 1
- 239000005695 Ammonium acetate Substances 0.000 description 1
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 description 1
- FMMWHPNWAFZXNH-UHFFFAOYSA-N Benz[a]pyrene Chemical compound C1=C2C3=CC=CC=C3C=C(C=C3)C2=C2C3=CC=CC2=C1 FMMWHPNWAFZXNH-UHFFFAOYSA-N 0.000 description 1
- 229940043376 ammonium acetate Drugs 0.000 description 1
- 235000019257 ammonium acetate Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000005252 bulbus oculi Anatomy 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 235000015220 hamburgers Nutrition 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229960002715 nicotine Drugs 0.000 description 1
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000009936 smoking Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/0004—Gaseous mixtures, e.g. polluted air
- G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
- G01N33/0062—General constructional details of gas analysers, e.g. portable test equipment concerning the measuring method or the display, e.g. intermittent measurement or digital display
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/0004—Gaseous mixtures, e.g. polluted air
- G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
- G01N33/0027—General constructional details of gas analysers, e.g. portable test equipment concerning the detector
- G01N33/0031—General constructional details of gas analysers, e.g. portable test equipment concerning the detector comprising two or more sensors, e.g. a sensor array
- G01N33/0032—General constructional details of gas analysers, e.g. portable test equipment concerning the detector comprising two or more sensors, e.g. a sensor array using two or more different physical functioning modes
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/0004—Gaseous mixtures, e.g. polluted air
- G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
- G01N33/0027—General constructional details of gas analysers, e.g. portable test equipment concerning the detector
- G01N33/0036—General constructional details of gas analysers, e.g. portable test equipment concerning the detector specially adapted to detect a particular component
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Food Science & Technology (AREA)
- Combustion & Propulsion (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The invention discloses a method for quickly measuring harmful ingredients in main stream smoke of a cigarette. According to the method, solvent gathering and filter disc gathering are adopted on a smoking machine at the same time, carbon monoxide is detected through a non-scattering infrared detection on the smoking machine, a solvent is used for gathering ammonia, hydrogen cyanide and crotonaldehyde, a filter disc is used for gathering NNK, ammonia, hydrogen cyanide and phenol, and after being collected, samples are detected through efficient high oerformance liquid chromatography, ion chromatography and a liquid chromatogram/gas chromatograph-mass spectrometer. The method integrates six tobacco industry standard methods for harmful ingredient detection in smoke of the cigarette, operation is easy and convenient, the analysis procedure is simplified, the analysis step of repeatedly smoking the cigarette is avoided, precision is good, and the method is suitable for measuring the content of the harmful ingredients in the main stream smoke of the cigarette.
Description
One, technical field
The present invention relates to a kind of detection method, a kind of method of harmful components in quick mensuration cigarette mainstream flue gas.
Two, background technology
In recent years, smoking is constantly subjected to the extensive concern of people with healthy topic, the own generally accreditation by people that Smoking is harmful to your health.Detection method for harmful components such as the NNK in cigarette smoke, phenol, crotonic aldehyde, ammonia, Blausure (German), benzopyrene and carbon monoxides also tends to maturation, and defines national standard and industry standard.At present, the either research and development of analytical tool, or the improvement of the method for analysis, all striding forward to the target saving analysis time and personality resource.And in these examination criterias, in addition to the detection of carbon monoxide can carry out simultaneously and complete detection with cigarette smoke nicotine moisture, the detection of other 6 kinds of harmful components then needs to aspirate on smoking machine respectively supplementary set, carry out detection with different detecting instruments the most respectively to analyze, process is slow, step repeats loaded down with trivial details, only this link of suction supplementary set of smoking machine, the detection of 6 kinds of harmful components is accomplished by repeating 6 cigarette smokings, this detection method is no matter for detection cycle or personality resource, it it is all a drawback the biggest, cannot adapt to the industry requirement that the detection of current fast pace is analyzed.
The distribution situation of the harmful components such as NNK, phenol, crotonic aldehyde, ammonia, Blausure (German) and carbon monoxide in cigarette smoke is respectively had any different, NNK and phenol exist only in Smoke Particulate, crotonic aldehyde and carbon monoxide exist only in flue gas gas gas-phase objects, and ammonia and Blausure (German) the gas phase of flue gas and grain mutually in all have distribution.Chemically character considers, carbon monoxide is insoluble in water, and crotonic aldehyde is the most soluble in water, and the final detection result on carbon monoxide and crotonic aldehyde that connects of the solvent supplementary set bottle therefore used in the method does not affect.
Three, summary of the invention
It is desirable to provide a kind of method of harmful components in quick mensuration cigarette mainstream flue gas, to realize the quick mensuration of carbon monoxide, NNK, phenol, crotonic aldehyde, ammonia and hydrogen cyanide content in cigarette mainstream flue gas.
Detection method equipment therefor is following (Fig. 1):
Fume collector 2 is tightly connected by connecting line 3 with solvent trapping bottle 4；Solvent trapping bottle 4 is tightly connected by connecting line 5 with pump unit 6；Blank filter disc is loaded in Fume collector 2；Solvent trapping bottle 4 built-in 50mL deionized water.
The volume of the deionized water that solvent trapping bottle 4 is built-in is to consider the dissolubility in water of the test substance in the size of solvent supplementary set bottle and flue gas and Negotiation speed and draws, it is ensured that the test substance in flue gas is completely absorbed by water.If it exceeds 50ml, the pump unit of smoking machine can be inhaled into when suction because there being a large amount of bubble.
One end of connecting line 3 is tightly connected with Fume collector 2, and the other end inserts in the deionized water in solvent trapping bottle 4.
One end of connecting line 5 is tightly connected with pump unit 6, and the other end connects with solvent trapping bottle 4.
In apparatus of the present invention, Fume collector 2 is i.e. the Fume collector of smoking machine, and pump unit 6 is i.e. the pump unit of smoking machine, i.e. increases a solvent trapping bottle 4 between Fume collector and the pump unit of conventional smoking machine.
The present invention quickly measures the method for harmful components in cigarette mainstream flue gas, comprises the steps:
1, aspirating 10 Medicated cigarette on smoking machine, take out the filter disc on solvent trapping bottle 4 and Fume collector 2 after suction, filter disc is put in filter disc extraction flask.Carbon monoxide is directly detected by smoking machine and obtains a result.Smoking machine can directly measure CO content, because there being the near-infrared scatter detector carried on Burger watt smoking machine.
Cigarette smoke is trapped by filter disc, then enters solvent trapping bottle 4 by connecting line 3, after the solution absorption of deionized water, is returned by connecting line 5 in the gas circuit circulation of smoking machine.
In the inventive method, 10 Medicated cigarette of setting suction are through experimental verification, relevant with the volume of the deionized water in solvent trapping bottle 4, to ensure deionized water fully absorbing the determinand in flue gas.
2, the preparation of testing sample solution
1. NNK solution to be measured: add 50ml deionized water and 1mlNNK internal standard (this interior aqueous solution being designated as the most deuterated-4-of NNK-d4 (methyl nitrosamino group)-1-(3-pyridine radicals)-1-butanone) in filter disc extraction flask, filter disc extract is obtained after vibrating 45 minutes, take 1ml and put in chromatogram bottle, to be measured.
2. phenol solution to be measured: take 1ml filter disc extract and put in chromatogram bottle, to be measured.
3. crotonic aldehyde solution to be measured: take the solution in 5ml solvent trapping bottle and add in 50ml tool plug triangular flask, add 15ml derivatization reagent, take 1ml after placing 1 hour in 40 DEG C of water-baths and put in chromatogram bottle, to be measured.Derivatization reagent is the acetonitrile solution of the 2,4 dinitrophenyl hydrazine of 1.0wt%.
4. ammonia solution to be measured: take the solution in 2.5ml solvent trapping bottle and 2.5ml filter disc extract adds in 25ml volumetric flask, deionized water constant volume, to be measured.
5. Blausure (German) solution to be measured: take the solution in 2.5ml solvent trapping bottle and 2.5ml filter disc extract adds in 25ml volumetric flask, deionized water constant volume, to be measured.
3, the detection of sample
1. the detection of CO content is carried out according to " mensuration of carbon monoxide-non-scatter infrared method in GB/T 23356-2009 components in cigarette smoke gas phase ".
2. the detection of NNK content is carried out according to " mensuration-high performance liquid chromatography of Nicotiana tabacum L. peculiar N-nitrosamine/tandem mass spectrum combination method in YQ/T 17-2012 cigarette mainstream smoke total particulate matter ".
3. the detection of phenol content is carried out according to " mensuration-high performance liquid chromatography of YC/T 255-2008 main phenolic compounds in main stream smoke of cigarette ".
4. the detection of crotonic aldehyde content is carried out according to " mensuration-high performance liquid chromatography of YC/T 254-2008 main carbonyl compounds in main stream cigarette smoke ".
5. the detection of ammonia content is carried out according to " mensuration-chromatography of ions of YC/T 377-2010 ammonia of main stream smoke of cigarette ".
6. the detection of hydrogen cyanide content is carried out according to " mensuration-chromatography of ions of Blausure (German) in YC/T 403-2011 cigarette mainstream flue gas ".
Compared with the prior art, beneficial effects of the present invention is embodied in:
1, the assay method of harmful components during the present invention provides a kind of quick mensuration cigarette mainstream flue gas first, achieve the quick mensuration of the carbon monoxide in cigarette mainstream flue gas, NNK, phenol, crotonic aldehyde, ammonia and hydrogen cyanide content, having filled up the technological gap of association area, the product quality supervision and inspection work for relevant departments provides fast and convenient detection method.
2, due to the analysis method of traditional GB and rower, it is the most separate for the assay method of carbon monoxide, NNK, phenol, crotonic aldehyde, ammonia and hydrogen cyanide content in cigarette mainstream flue gas, the detection of one sample to carry out the cigarette smoking process of 6 times, the present invention is reduced to the cigarette smoking process of 6 times 1 time, analyzes method highly efficient.
3, the inventive method pre-treatment is simple, is not required to purify, easy and simple to handle, measures quickly.The results contrast that the present invention and traditional detection method draw, the NNK relative standard deviation (RSD) of trace level (nanogram/prop up) is less than 6.0%, the relative standard deviation (RSD) of other testing results is respectively less than 3.0%, and this shows that the method repeatability and precision are the most fine.
Table 1, GB/T 23356-2009 detection method detect carbon monoxide results contrast with detection method
Table 2, YQ/T 17-2012 detection method detect NNK results contrast with detection method
Table 3, YC/T 255-2008 detection method detect phenol results contrast with detection method
Table 4, YC/T 254-2008 detection method detect crotonic aldehyde results contrast with detection method
Table 5, YC/T 377-2010 detection method detect ammonia results contrast with detection method
Table 6, YC/T 403-2011 detection method detect Blausure (German) results contrast with detection method
Four, accompanying drawing explanation
Fig. 1 is that the present invention uses device schematic diagram.
Wherein 1 cigarette, 2 Fume collectors, 3 connecting lines, 4 solvent supplementary set bottles, 5 connecting lines, 6 pump units.
Fig. 2 is the scale diagrams of solvent trapping bottle 4 of the present invention.Wherein the height of solvent trapping bottle 4 is 170mm, a diameter of 34mm；It is 2-3mm that connecting line 3 inserts the distance from bottom of solvent trapping bottle 4 middle-range solvent trapping bottle 4；In solvent trapping bottle 4 the gas circuit pipe i.e. external diameter of connecting line 5 be 5mm, internal diameter be 3mm；Solvent trapping bottle 4 grinding port plug height 25mm.
Five, detailed description of the invention
The present invention is further described by specific examples below, but is not intended to the present invention.
[instrument, reagent and instrument working condition]
1, instrument: orthoscopic smoking machine or rotating disc type smoking machine, is equipped with carbonmonoxide detector (primary GWAT Co., Ltd of Germany)；High performance liquid chromatography-tandem mass combined instrument, is equipped with electric spray ion source (Waters, US)；Ultimate 3600 high performance liquid chromatograph, joins UV-detector (power & light company of the U.S.)；Ion chromatograph, is equipped with conductance and electrochemical detector (power & light company of the U.S.)；Milli-Q50 ultra-pure water instrument (Millipore company of the U.S.)；AL204-IC analytical balance (sensibility reciprocal scope 0.0001g, Mettler company of Germany).
2, reagent: 2%, the carbon monoxide/nitrogen mixture of 4%, 6%, crotonic aldehyde 2,4-dinitro benzene hydazone derivative, phenol/methanol solution, NNK/ aqueous solution, NNK-d4/ aqueous solution, ammonia water solution, Blausure (German)/aqueous solution, is standard substance；Acetic acid (analytical pure, Solution on Chemical Reagents in Shanghai company of Chinese Medicine group)；Second eyeball (chromatographically pure, Fisher company of the U.S.)；Methanol (chromatographically pure, Fisher company of the U.S.)；Ammonium acetate (chromatographically pure, Fisher company of the U.S.)；Perchloric acid (analytical pure, Solution on Chemical Reagents in Shanghai company of Chinese Medicine group)；Sodium hydroxide (analytical pure, Solution on Chemical Reagents in Shanghai company of Chinese Medicine group)；2,4 dinitrophenyl hydrazine (DNPH) (analytical pure, Solution on Chemical Reagents in Shanghai company of Chinese Medicine group, through recrystallized from acetonitrile before using)；Ultra-pure water.
Embodiment 1:
1, detection device
In the present embodiment, detection method equipment therefor is following (Fig. 1):
Fume collector 2 is tightly connected by connecting line 3 with solvent trapping bottle 4 (Fig. 2)；Solvent trapping bottle 4 is tightly connected by connecting line 5 with pump unit 6；Blank filter disc is loaded in Fume collector 2；Solvent trapping bottle 4 built-in 50mL deionized water.
One end of connecting line 3 is tightly connected with Fume collector 2, and the other end inserts in the deionized water in solvent trapping bottle 4.
One end of connecting line 5 is tightly connected with pump unit 6, and the other end connects with solvent trapping bottle 4.
In apparatus of the present invention, Fume collector 2 is i.e. the Fume collector of smoking machine, and pump unit 6 is i.e. the pump unit of smoking machine, is equivalent to increase a solvent trapping bottle 4 between Fume collector and the pump unit of conventional smoking machine.The concrete size of solvent supplementary set bottle 4 is shown in accompanying drawing 2.
2, detection method
(1) aspirating 10 Medicated cigarette on smoking machine, take out the filter disc on solvent trapping bottle 4 and Fume collector 2 after suction, filter disc is put in filter disc extraction flask.Carbon monoxide is directly detected by smoking machine and obtains a result.
Cigarette smoke is trapped by filter disc, then enters solvent trapping bottle 4 by connecting line 3, after the solution absorption of deionized water, is returned by connecting line 5 in the gas circuit circulation of smoking machine.
(2) preparation of testing sample solution
1. NNK solution to be measured: add 50ml deionized water and 1mlNNK internal standard (this interior aqueous solution being designated as the most deuterated-4-of NNK-d4 (methyl nitrosamino group)-1-(3-pyridine radicals)-1-butanone) in filter disc extraction flask, filter disc extract is obtained after vibrating 45 minutes, take 1ml and put in chromatogram bottle, to be measured.
2. phenol solution to be measured: take 1ml filter disc extract and put in chromatogram bottle, to be measured.
3. crotonic aldehyde solution to be measured: take the solution in 5ml solvent trapping bottle and add in 50ml tool plug triangular flask, add 15ml derivatization reagent, take 1ml after placing 1 hour in 40 DEG C of water-baths and put in chromatogram bottle, to be measured.Derivatization reagent is the acetonitrile solution of the 2,4 dinitrophenyl hydrazine of 1.0wt%.
4. ammonia solution to be measured: take the solution in 2.5ml solvent trapping bottle and 2.5ml filter disc extract adds in 25ml volumetric flask, deionized water constant volume, to be measured.
5. Blausure (German) solution to be measured: take the solution in 2.5ml solvent trapping bottle and 2.5ml filter disc extract adds in 25ml volumetric flask, deionized water constant volume, to be measured.
(3) detection of sample
1. the detection of CO content is carried out according to " mensuration of carbon monoxide-non-scatter infrared method in GB/T 23356-2009 components in cigarette smoke gas phase ".
2. the detection of NNK content is carried out according to " mensuration-high performance liquid chromatography of Nicotiana tabacum L. peculiar N-nitrosamine/tandem mass spectrum combination method in YQ/T 17-2012 cigarette mainstream smoke total particulate matter ".
3. the detection of phenol content is carried out according to " mensuration-high performance liquid chromatography of YC/T 255-2008 main phenolic compounds in main stream smoke of cigarette ".
4. the detection of crotonic aldehyde content is carried out according to " mensuration-high performance liquid chromatography of YC/T 254-2008 main carbonyl compounds in main stream cigarette smoke ".
5. the detection of ammonia content is carried out according to " mensuration-chromatography of ions of YC/T 377-2010 ammonia of main stream smoke of cigarette ".
6. the detection of hydrogen cyanide content is carried out according to " mensuration-chromatography of ions of Blausure (German) in YC/T 403-2011 cigarette mainstream flue gas ".
According to said method, select a kind of Medicated cigarette A, record wherein carbon monoxide in flue gas burst size 10.9 milligrams/, NNK release amount 5.2 nanogram/, phenol release amount 17.2 microgram/, crotonaldehyde release amount 19.3 microgram/, ammonia burst size 8.4 microgram/, Blausure (German) burst size 112.3 microgram/.
Embodiment 2:
According to the detection method described in embodiment 1, select a kind of Medicated cigarette B, record wherein carbon monoxide in flue gas burst size 13.1 milligrams/, NNK release amount 4.2 nanogram/, phenol release amount 15.6 microgram/, crotonaldehyde release amount 18.0 microgram/, ammonia burst size 8.9 microgram/, Blausure (German) burst size 146.2 microgram/.
Embodiment 3:
According to the detection method described in embodiment 1, select a kind of Medicated cigarette C, record wherein carbon monoxide in flue gas burst size 13.5 milligrams/, NNK release amount 4.8 nanogram/, phenol release amount 11.8 microgram/, crotonaldehyde release amount 18.7 microgram/, ammonia burst size 6.8 microgram/, Blausure (German) burst size 125.9 microgram/.
Embodiment 4:
According to the detection method described in embodiment 1, select a kind of Medicated cigarette D, record wherein carbon monoxide in flue gas burst size 11.7 milligrams/, NNK release amount 3.4 nanogram/, phenol release amount 12.4 microgram/, crotonaldehyde release amount 20.5 microgram/, ammonia burst size 7.7 microgram/, Blausure (German) burst size 120.7 microgram/.
[list of references]
1, the mensuration non-scatter infrared method of carbon monoxide in GB/T 23356-2009 components in cigarette smoke gas phase
2, the mensuration high performance liquid chromatography of Nicotiana tabacum L. peculiar N-nitrosamine/tandem mass spectrum combination method in YQ/T 17-2012 cigarette mainstream smoke total particulate matter
3, the mensuration high performance liquid chromatography of YC/T 255-2008 main phenolic compounds in main stream smoke of cigarette
4, the mensuration high performance liquid chromatography of YC/T 254-2008 main carbonyl compounds in main stream cigarette smoke
5, the mensuration chromatography of ions of YC/T 377-2010 ammonia of main stream smoke of cigarette
6, the mensuration chromatography of ions of Blausure (German) in YC/T 403-2011 cigarette mainstream flue gas.
Claims (2)
1. the method for harmful components in a quick mensuration cigarette mainstream flue gas, it is characterised in that comprise the steps:
(1) on smoking machine, aspirate 10 Medicated cigarette, after suction, take out solvent trapping bottle (4) and Fume collector (2)
On filter disc, filter disc is put in filter disc extraction flask, and carbon monoxide is directly detected by smoking machine and obtains a result；
(2) preparation of testing sample solution
1. NNK solution to be measured: add 50ml deionized water and 1mlNNK internal standard in filter disc extraction flask, vibrate 45 minutes
Rear acquisition filter disc extract, takes 1ml and puts in chromatogram bottle, to be measured；
2. phenol solution to be measured: take 1ml filter disc extract and put in chromatogram bottle, to be measured；
3. crotonic aldehyde solution to be measured: take the solution in 5ml solvent trapping bottle and add in 50ml tool plug triangular flask, add 15ml
Derivatization reagent, takes 1ml after placing 1 hour and put in chromatogram bottle in 40 DEG C of water-bath, to be measured；
4. ammonia solution to be measured: take the solution in 2.5ml solvent trapping bottle and 2.5ml filter disc extract adds in 25ml volumetric flask,
Deionized water constant volume, to be measured；
5. Blausure (German) solution to be measured: take the solution in 2.5ml solvent trapping bottle and 2.5ml filter disc extract adds 25ml volumetric flask
In, deionized water constant volume, to be measured；
(3) detection of sample
1. the detection of CO content is according to " in GB/T 23356-2009 components in cigarette smoke gas phase, the mensuration-non-scatter of carbon monoxide is infrared
Method " carry out；
2. the detection of NNK content is according to " Nicotiana tabacum L. peculiar N-nitrosamine in YQ/T 17-2012 cigarette mainstream smoke total particulate matter
Mensuration-high performance liquid chromatography/tandem mass spectrum combination method " carry out；
3. the detection of phenol content is according to " mensuration-the high-efficient liquid of YC/T 255-2008 main phenolic compounds in main stream smoke of cigarette
Phase chromatography " carry out；
4. the detection of crotonic aldehyde content is according to " the mensuration of YC/T 254-2008 main carbonyl compounds in main stream cigarette smoke-efficient
Liquid chromatography " carry out；
5. the detection of ammonia content is carried out according to " mensuration-chromatography of ions of YC/T 377-2010 ammonia of main stream smoke of cigarette "；
6. the detection of hydrogen cyanide content is according to " mensuration-chromatography of ions of Blausure (German) in YC/T 403-2011 cigarette mainstream flue gas "
Carry out.
Method the most according to claim 2, it is characterised in that:
Described derivatization reagent is the acetonitrile solution of the 2,4 dinitrophenyl hydrazine of 1.0wt%.
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