CN103439443B - The method of 16 kinds of palycyclic aromatics in Simultaneously test cigarette mainstream flue gas - Google Patents

The method of 16 kinds of palycyclic aromatics in Simultaneously test cigarette mainstream flue gas Download PDF

Info

Publication number
CN103439443B
CN103439443B CN201310383762.XA CN201310383762A CN103439443B CN 103439443 B CN103439443 B CN 103439443B CN 201310383762 A CN201310383762 A CN 201310383762A CN 103439443 B CN103439443 B CN 103439443B
Authority
CN
China
Prior art keywords
kinds
benzo
flue gas
anthracene
palycyclic
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201310383762.XA
Other languages
Chinese (zh)
Other versions
CN103439443A (en
Inventor
王晓瑜
谢复炜
秦亚琼
夏巧玲
王冰
刘惠民
贾云祯
崔华鹏
陈黎
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Zhengzhou Tobacco Research Institute of CNTC
Original Assignee
Zhengzhou Tobacco Research Institute of CNTC
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Zhengzhou Tobacco Research Institute of CNTC filed Critical Zhengzhou Tobacco Research Institute of CNTC
Priority to CN201310383762.XA priority Critical patent/CN103439443B/en
Publication of CN103439443A publication Critical patent/CN103439443A/en
Application granted granted Critical
Publication of CN103439443B publication Critical patent/CN103439443B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Abstract

The invention discloses the method for 16 kinds of palycyclic aromatics in a kind of Simultaneously test cigarette mainstream flue gas, comprise the following steps: 1) with after cambridge filter trapping cigarette mainstream smoke condensate, cambridge filter is proceeded to extraction vessel, add interior mark mixed solution, add methyl alcohol again and carry out concussion extraction, obtain methanol extract liquid; 2) methanol extract liquid is obtained dilution with after ultrapure water dilution, adopt immersion solid-phase microextraction technology to carry out selective extraction to dilution, obtain fume sample; 3) adopt GC-MS to detect fume sample, detect 16 kinds of polycyclic aromatic hydrocarbon contents by internal standard quanitation.The method of 16 kinds of palycyclic aromatics in Simultaneously test cigarette mainstream flue gas of the present invention, adopt solid-phase microextraction-combined gas chromatography mass spectrometry, can the content of 16 kinds of palycyclic aromatics in Simultaneously test cigarette mainstream flue gas, there is quick detection, highly sensitive, selectivity good, advantage that degree of accuracy is high; Be applicable to the content measuring palycyclic aromatic in low-coke tar cigarette flue gas.

Description

The method of 16 kinds of palycyclic aromatics in Simultaneously test cigarette mainstream flue gas
Technical field
The invention belongs to palycyclic aromatic detection technique field, be specifically related to the method for 16 kinds of palycyclic aromatics in a kind of Simultaneously test cigarette mainstream flue gas.
Background technology
Smoking is harmful to your health, and cigarette healthhazard causes primarily of the objectionable impurities in flue gas, detects and the objectionable constituent burst size controlled in flue gas is tobacco business obligation one can't decline.Polycyclic arene compound is objectionable impurities main in flue gas, has carcinogenic, teratogenesis to human body.Because smoke components is very complicated, and the content of polycyclic aromatic hydrocarbon compounds in flue gas is trace, substantially magnitude is propped up at ng/, matrix interference is serious, detection difficulty is larger, therefore at present researcher often only pays close attention to the content of maximum benzo [a] pyrene of cigarette smoke Poisoning, and conventional method is national standard method the mensuration of benzo [a] pyrene " in the cigarette smoke condensates " (GB 21130-2007-T).But disclose 69 kinds of objectionable constituent inventories at HOFFMANN in calendar year 2001, wherein palycyclic aromatic has accounted for 10 kinds.The document of the multiple palycyclic aromatic of current Simultaneously test is less, and Detection results is not ideal enough.Therefore, it is very necessary for developing the new method that is quick, sensitive, high selectivity of multiple palycyclic aromatic in a kind of Simultaneously test cigarette smoke.
Summary of the invention
The object of this invention is to provide a kind of quick detection, highly sensitive, selectivity good, the method for 16 kinds of palycyclic aromatics in Simultaneously test cigarette mainstream flue gas that degree of accuracy is high.
In order to realize above object, the technical solution adopted in the present invention is: the method for 16 kinds of palycyclic aromatics in Simultaneously test cigarette mainstream flue gas, comprises the following steps:
1) with cambridge filter trapping cigarette mainstream smoke condensate after, cambridge filter is proceeded to extraction vessel, adds inner mark solution, then add methyl alcohol carry out concussion extraction, obtain methanol extract liquid;
The amount of inner mark solution used is 50 ~ 200 μ L, and methyl alcohol used is 30 ~ 50ml; The time that described concussion is extracted is 40 ~ 60min.Inner mark solution is the mixed solution of 5 kinds of deuterated internal standard compounds, and 5 kinds of deuterated internal standard compounds are naphthalene-d8, acenaphthene-d10, anthracene-d10, benzo [a] anthracene-d12, benzo [a] pyrene-d12, and solvent is methyl alcohol; In inner mark solution, the content of the content of naphthalene-d8 to be the content of 200 μ g/mL, acenaphthene-d10 be 5 μ g/mL, anthracene-d10 is 5 μ g/mL, the content of benzo [a] anthracene-d12 is 2 μ g/mL, the content of benzo [a] pyrene-d12 is 2 μ g/mL.
2) methanol extract liquid is obtained dilution with after ultrapure water dilution 50 ~ 500 times, adopt immersion solid-phase microextraction technology to carry out selective extraction to dilution, obtain fume sample;
Employing immersion solid-phase microextraction technology to the concrete operations that dilution carries out selective extraction is: dilution is placed in solid-phase microextraction bottle, 50 ~ 70 DEG C, balance 30min under 300 ~ 800rpm rotating speed stirring condition after, insert solid-phase micro-extraction fibre extraction 40 ~ 60min.Described solid-phase micro-extraction fibre is graphite ene-type solid-phase micro-extraction fibre or carbon nano tube type solid-phase micro-extraction fibre.Graphite ene-type solid-phase micro-extraction fibre or carbon nano tube type solid-phase micro-extraction fibre preparation method adopt physics to stick method, concrete grammar referenced patent " preparing the method for the solid-phase micro-extraction coating fast " (patent No.: 201210105077.6).
Described fume sample is the testing sample be adsorbed on solid-phase micro-extraction fibre; During sample introduction, this solid-phase micro-extraction fibre is placed in gas chromatographic sample introduction mouth and carries out Thermal desorption sample introduction.
3) adopt GC-MS to detect fume sample, detect 16 kinds of polycyclic aromatic hydrocarbon contents by internal standard quanitation.
Chromatographic condition is: chromatographic column: DB-5ms (30m × 0.25mm × 0.25 μm); Carrier gas: He; Flow velocity: 1.0ml/min; Injector temperature: 290 DEG C; Adopt and do not shunt bushing pipe; The Thermal desorption time: 2-5min; Heating schedule: from 50 DEG C, is raised to 130 DEG C with the programming rate of 10 DEG C/min, then is raised to 300 DEG C with the programming rate of 5 DEG C/min, keeps 5min.
Mass Spectrometry Conditions is: adopt single ion detection mode (SIM), quota ion is in table 1; Ion source temperature is 300 DEG C, and level Four bar temperature is 180 DEG C.
Table 1 16 kinds of polycyclic aromatic hydrocarbon compounds and interior entitling claims, quota ion information
Numbering Title Quota ion
Interior mark 1 Naphthalene-d8 136
1 Naphthalene 128
Interior mark 2 Acenaphthene-d10 164
2 Naphtho-ethene 152
3 Acenaphthene 152
4 Fluorenes 166
Interior mark 3 Anthracene-d10 188
5 Luxuriant and rich with fragrance 178
6 Anthracene 178
7 Fluoranthene 202
8 Pyrene 202
Interior mark 4 Benzo [a] anthracene-d12 240
9 Benzo [a] anthracene 228
10 Bend 228
Interior mark 5 Benzo [a] pyrene-d12 264
11 Benzo [b] fluoranthene 252
12 Benzo [k] fluoranthene 252
13 Benzo [a] pyrene 252
14 Indeno [1,2,3-cd] pyrene 276
15 Dibenzo [a, h] anthracene 278
16 Benzo [g, h, i] pyrene 276
In internal standard quanitation detects, mark and 16 kinds of palycyclic aromatic reference materials in 5 kinds in standard working solution used, solvent is ultrapure water; In in all standard working solution, the concentration of mark naphthalene-d8, acenaphthene-d10, anthracene-d10, benzo [a] anthracene-d12, benzo [a] pyrene-d12 is fixed, and is followed successively by 200ng/L, 50ng/L, 50ng/L, 20ng/L, 20ng/L; In standard working solution, palycyclic aromatic concentration magnitude is followed successively by 0.5ng/L, 1ng/L, 5ng/L, 10ng/L, 50ng/L, 100ng/L, 500ng/L from low to high, and the lower 16 kinds of palycyclic aromatic concentration of each concentration magnitude are all equal.
The quantitation curves of 16 kinds of palycyclic aromatics, the range of linearity, detection limit, quantitative limit are as shown in table 2.
The method of 16 kinds of palycyclic aromatics in Simultaneously test cigarette mainstream flue gas of the present invention, adopts solid-phase microextraction-combined gas chromatography mass spectrometry, can the content of 16 kinds of palycyclic aromatics in Rapid Simultaneous Determination cigarette mainstream flue gas.Due to adopt Graphene or carbon nanotube coating solid-phase micro-extraction fibre to multiring aromatic hydrocarbon substance, there is adsorptive selectivity, the inventive method clean-up effect is better than traditional solid phase extraction method.The present invention adopts methanol extraction to Smoke Particulate, carries out solid-phase microextraction after extract dilution 50-500 times.When extension rate is 500 times, sensitivity of the present invention is better than solid phase extraction; Extension rate is 50 times, and sensitivity can promote a magnitude again, can be used for testing low-coke tar cigarette, among the palycyclic aromatic super low loading sample systems such as single port flue gas.
Accompanying drawing explanation
Fig. 1 is the SIM figure of 16 kinds of palycyclic aromatic standard specimens;
Fig. 2 is the SIM figure of the palycyclic aromatic of numbering 1 in the cigarette mainstream flue gas of embodiment 1;
Fig. 3 is the SIM figure of the palycyclic aromatic of numbering 2,3 in the cigarette mainstream flue gas of embodiment 1;
Fig. 4 is the SIM figure of the palycyclic aromatic of numbering 4 in the cigarette mainstream flue gas of embodiment 1;
Fig. 5 is the SIM figure of the palycyclic aromatic of numbering 5,6 in the cigarette mainstream flue gas of embodiment 1;
Fig. 6 is the SIM figure of the palycyclic aromatic of numbering 7,8 in the cigarette mainstream flue gas of embodiment 1;
Fig. 7 is the SIM figure of the palycyclic aromatic of numbering 9,10 in the cigarette mainstream flue gas of embodiment 1;
Fig. 8 is the SIM figure of the palycyclic aromatic of numbering 11,12,13 in the cigarette mainstream flue gas of embodiment 1;
Fig. 9 is the SIM figure of the palycyclic aromatic of numbering 14,15,16 in the cigarette mainstream flue gas of embodiment 1;
Wherein, the corresponding title of the numbering of palycyclic aromatic is as shown in table 1, table 2; The unit of horizontal ordinate time is min.
Embodiment
Below in conjunction with embodiment, the present invention is further illustrated.
Embodiment 1
In the Simultaneously test cigarette mainstream flue gas of the present embodiment, the method for 16 kinds of palycyclic aromatics, comprises the following steps:
1) cigarette of the trade mark 1 after balance and screening is aspirated according to YC/T29-1996 specified standard puffing regimens, after trapping 5 cigarette mainstream smoke condensate with 1 cambridge filter, cambridge filter is proceeded to 100ml ground conical flask and at the bottom of being laid in bottle, add 50 μ L inner mark solutions, add the concussion of 30ml methyl alcohol again and extract 40min, obtain methanol extract liquid;
Described inner mark solution is the mixed solution of 5 kinds of deuterated internal standard compounds, and described 5 kinds of deuterated internal standard compounds are naphthalene-d8, acenaphthene-d10, anthracene-d10, benzo [a] anthracene-d12, benzo [a] pyrene-d12, and solvent is methyl alcohol; In described inner mark solution, the content of the content of naphthalene-d8 to be the content of 200 μ g/mL, acenaphthene-d10 be 5 μ g/mL, anthracene-d10 is 5 μ g/mL, the content of benzo [a] anthracene-d12 is 2 μ g/mL, the content of benzo [a] pyrene-d12 is 2 μ g/mL;
2) dilution is obtained after step 1) gained methanol extract liquid ultrapure water being diluted 50 times, immersion solid-phase microextraction technology is adopted to carry out selective extraction to dilution, solid-phase microextraction bottle (the screw socket sealing gland bottle of 30ml) is placed in by 25ml dilution, 65 DEG C, balance 30min under 500rpm rotating speed stirring condition after, insert Graphene solid-phase micro-extraction fibre (35 μm of thickness) and extract 60min, obtain fume sample (being namely adsorbed on the testing sample on solid-phase micro-extraction fibre);
3) GC-MS is adopted to step 2) gained fume sample detects, and the solid-phase micro-extraction fibre being about to be adsorbed with testing sample is placed in gas chromatographic sample introduction mouth and carries out Thermal desorption sample introduction, and the Thermal desorption time is 5min;
The analysis condition that GC-MS detects:
Chromatographic condition is: chromatographic column: DB-5ms (30m × 0.25mm × 0.25 μm); Carrier gas: He; Flow velocity: 1.0ml/min; Injector temperature: 290 DEG C; Adopt and do not shunt bushing pipe; The Thermal desorption time: 5min; Heating schedule: from 50 DEG C, is raised to 130 DEG C with the programming rate of 10 DEG C/min, then is raised to 300 DEG C with the programming rate of 5 DEG C/min, keeps 5min.
Mass Spectrometry Conditions is: adopt single ion detection mode, and ion source temperature is 300 DEG C, and level Four bar temperature is 180 DEG C.
In the Simultaneously test cigarette mainstream flue gas of the present embodiment, the cigarette testing result of method to the trade mark 1 of 16 kinds of palycyclic aromatics is as shown in table 3.
Embodiment 2
In the Simultaneously test cigarette mainstream flue gas of the present embodiment, the method for 16 kinds of palycyclic aromatics, comprises the following steps:
1) cigarette of the trade mark 2 after balance and screening is aspirated according to YC/T29-1996 specified standard puffing regimens, after trapping 10 cigarette mainstream smoke condensate with 2 cambridge filters, 2 cambridge filters are proceeded to 100ml conical flask and at the bottom of being laid in bottle, add 50 μ L inner mark solutions, add the concussion of 40ml methyl alcohol again and extract 50min, obtain methanol extract liquid;
Described inner mark solution is the mixed solution of 5 kinds of deuterated internal standard compounds, and described 5 kinds of deuterated internal standard compounds are naphthalene-d8, acenaphthene-d10, anthracene-d10, benzo [a] anthracene-d12, benzo [a] pyrene-d12, and solvent is methyl alcohol; In described inner mark solution, the content of the content of naphthalene-d8 to be the content of 200 μ g/mL, acenaphthene-d10 be 5 μ g/mL, anthracene-d10 is 5 μ g/mL, the content of benzo [a] anthracene-d12 is 2 μ g/mL, the content of benzo [a] pyrene-d12 is 2 μ g/mL;
2) dilution is obtained after step 1) gained methanol extract liquid ultrapure water being diluted 500 times, immersion solid-phase microextraction technology is adopted to carry out selective extraction to dilution, solid-phase microextraction bottle (the screw socket sealing gland bottle of 30ml) is placed in by 25ml dilution, 70 DEG C, balance 30min under 800rpm rotating speed stirring condition after, insert Graphene solid-phase micro-extraction fibre (35 μm of thickness) and extract 40min, obtain fume sample (being namely adsorbed on the testing sample on solid-phase micro-extraction fibre);
3) GC-MS is adopted to step 2) gained fume sample detects, and the solid-phase micro-extraction fibre being about to be adsorbed with testing sample is placed in gas chromatographic sample introduction mouth and carries out Thermal desorption sample introduction, and the Thermal desorption time is 4min;
The analysis condition that GC-MS detects:
Chromatographic condition is: chromatographic column: DB-5ms (30m × 0.25mm × 0.25 μm); Carrier gas: He; Flow velocity: 1.0ml/min; Injector temperature: 290 DEG C; Adopt and do not shunt bushing pipe; The Thermal desorption time: 4min; Heating schedule: from 50 DEG C, is raised to 130 DEG C with the programming rate of 10 DEG C/min, then is raised to 300 DEG C with the programming rate of 5 DEG C/min, keeps 5min.
Mass Spectrometry Conditions is: adopt single ion detection mode, and ion source temperature is 300 DEG C, and level Four bar temperature is 180 DEG C.
In the Simultaneously test cigarette mainstream flue gas of the present embodiment, the cigarette testing result of method to the trade mark 2 of 16 kinds of palycyclic aromatics is as shown in table 3.
Embodiment 3
In the Simultaneously test cigarette mainstream flue gas of the present embodiment, the method for 16 kinds of palycyclic aromatics, comprises the following steps:
1) cigarette of the trade mark 3 after balance and screening is aspirated according to YC/T29-1996 specified standard puffing regimens, after trapping 8 cigarette mainstream smoke condensate with 2 cambridge filters, 2 cambridge filters are proceeded to 100ml conical flask and at the bottom of being laid in bottle, add 100 μ L inner mark solutions, add the concussion of 50ml methyl alcohol again and extract 60min, obtain methanol extract liquid;
Described inner mark solution is the mixed solution of 5 kinds of deuterated internal standard compounds, and described 5 kinds of deuterated internal standard compounds are naphthalene-d8, acenaphthene-d10, anthracene-d10, benzo [a] anthracene-d12, benzo [a] pyrene-d12, and solvent is methyl alcohol; In described inner mark solution, the content of the content of naphthalene-d8 to be the content of 200 μ g/mL, acenaphthene-d10 be 5 μ g/mL, anthracene-d10 is 5 μ g/mL, the content of benzo [a] anthracene-d12 is 2 μ g/mL, the content of benzo [a] pyrene-d12 is 2 μ g/mL;
2) dilution is obtained after step 1) gained methanol extract liquid ultrapure water being diluted 300 times, immersion solid-phase microextraction technology is adopted to carry out selective extraction to dilution, solid-phase microextraction bottle (the screw socket sealing gland bottle of 30ml) is placed in by 25ml dilution, 50 DEG C, balance 30min under 300rpm rotating speed stirring condition after, insert carbon nano-tube solid phase micro-extraction fiber (35 μm of thickness) and extract 50min, obtain fume sample (being namely adsorbed on the testing sample on solid-phase micro-extraction fibre);
3) GC-MS is adopted to step 2) gained fume sample detects, and the solid-phase micro-extraction fibre being about to be adsorbed with testing sample is placed in gas chromatographic sample introduction mouth and carries out Thermal desorption sample introduction, and the Thermal desorption time is 2min;
The analysis condition that GC-MS detects:
Chromatographic condition is: chromatographic column: DB-5ms (30m × 0.25mm × 0.25 μm); Carrier gas: He; Flow velocity: 1.0ml/min; Injector temperature: 290 DEG C; Adopt and do not shunt bushing pipe; The Thermal desorption time: 2min; Heating schedule: from 50 DEG C, is raised to 130 DEG C with the programming rate of 10 DEG C/min, then is raised to 300 DEG C with the programming rate of 5 DEG C/min, keeps 5min.
Mass Spectrometry Conditions is: adopt single ion detection mode, and ion source temperature is 300 DEG C, and level Four bar temperature is 180 DEG C.
In the Simultaneously test cigarette mainstream flue gas of the present embodiment, the cigarette testing result of method to the trade mark 3 of 16 kinds of palycyclic aromatics is as shown in table 3.
The testing result of polycyclic aromatic hydrocarbon content in the cigarette sample of table 3 embodiment 1-3
Experimental example 4
Kentucky reference cigarette 3R4F after balance and screening is aspirated according to YC/T29-1996 specified standard puffing regimens, traps 10 cigarette smoke granule phase substances with 2 cambridge filters.Measure according to the method for embodiment 1, replicate determination 6 groups, the RSD value (see table 4) between 5%-12% of 6 replicate determination values of 16 palycyclic aromatics, proves that precision of method of the present invention is higher, reproducible.
The precision of table 4 solid-phase microextraction-gas chromatography combined with mass spectrometry method
Numbering Title Content (ng/ props up) 1) RSD(n=6, %)
1 Naphthalene 343.9 4.0%
2 Naphtho-ethene 68.9 1.4%
3 Acenaphthene 54.2 7.5%
4 Fluorenes 186.1 6.9%
5 Luxuriant and rich with fragrance 135.8 3.0%
6 Anthracene 59.3 6.0%
7 Fluoranthene 54.4 10.2%
8 Pyrene 45.0 10.5%
9 Benzo [a] anthracene 13.8 2.2%
10 Bend 15.9 1.3%
11 Benzo [b] fluoranthene 5.3 5.3%
12 Benzo [k] fluoranthene 2.1 9.7%
13 Benzo [a] pyrene 6.5 5.6%
14 Indeno [1,2,3-cd] pyrene 3.9 9.5%
15 Dibenzo [a, h] anthracene 1.9 8.7%
16 Benzo [g, h, i] pyrene 3.8 9.8%

Claims (4)

1. the method for 16 kinds of palycyclic aromatics in a Simultaneously test cigarette mainstream flue gas, it is characterized in that: 16 kinds of palycyclic aromatics are specially: naphthalene, naphtho-ethene, acenaphthene, fluorenes, phenanthrene, anthracene, fluoranthene, pyrene, benzo [a] anthracene, in the wrong, benzo [b] fluoranthene, benzo [k] fluoranthene, benzo [a] pyrene, indeno [1,2,3-cd] pyrene, dibenzo [a, h] anthracene, benzo [g, h, i] pyrene
Comprise the following steps:
1) with cambridge filter trapping cigarette mainstream smoke condensate after, cambridge filter is proceeded to extraction vessel, adds inner mark solution, then add methyl alcohol carry out concussion extraction, obtain methanol extract liquid;
2) methanol extract liquid is obtained dilution with after ultrapure water dilution 50 ~ 500 times, immersion solid-phase microextraction technology is adopted to carry out selective extraction to dilution, obtain fume sample, concrete operations are: dilution is placed in solid-phase microextraction bottle, 50 ~ 70 DEG C, balance 30min under 300 ~ 800rpm rotating speed stirring condition after, insert solid-phase micro-extraction fibre extraction 40 ~ 60min; Described solid-phase micro-extraction fibre is graphite ene-type solid-phase micro-extraction fibre or carbon nano tube type solid-phase micro-extraction fibre; Described fume sample is the testing sample be adsorbed on solid-phase micro-extraction fibre; During sample introduction, this solid-phase micro-extraction fibre is placed in gas chromatographic sample introduction mouth and carries out Thermal desorption sample introduction;
3) adopt GC-MS to detect fume sample, detect 16 kinds of polycyclic aromatic hydrocarbon contents by internal standard quanitation;
Chromatographic condition is: chromatographic column: DB-5ms, specification 30m × 0.25mm × 0.25 μm; Carrier gas: He; Flow velocity: 1.0ml/min; Injector temperature: 290 DEG C; Adopt and do not shunt bushing pipe; The Thermal desorption time: 2-5min; Heating schedule: from 50 DEG C, is raised to 130 DEG C with the programming rate of 10 DEG C/min, then is raised to 300 DEG C with the programming rate of 5 DEG C/min, keeps 5min;
Mass Spectrometry Conditions is: adopt single ion detection mode, and ion source temperature is 300 DEG C, and level Four bar temperature is 180 DEG C.
2. the method for 16 kinds of palycyclic aromatics in Simultaneously test cigarette mainstream flue gas according to claim 1, is characterized in that: the amount of inner mark solution used is 50 ~ 200 μ L, and methyl alcohol used is 30 ~ 50ml; The time that described concussion is extracted is 40 ~ 60min.
3. the method for 16 kinds of palycyclic aromatics in Simultaneously test cigarette mainstream flue gas according to claim 1 and 2, it is characterized in that: described inner mark solution is the mixed solution of 5 kinds of deuterated internal standard compounds, 5 kinds of deuterated internal standard compounds are naphthalene-d8, acenaphthene-d10, anthracene-d10, benzo [a] anthracene-d12, benzo [a] pyrene-d12, and solvent is methyl alcohol; In inner mark solution, the content of the content of naphthalene-d8 to be the content of 200 μ g/mL, acenaphthene-d10 be 5 μ g/mL, anthracene-d10 is 5 μ g/mL, the content of benzo [a] anthracene-d12 is 2 μ g/mL, the content of benzo [a] pyrene-d12 is 2 μ g/mL.
4. the method for 16 kinds of palycyclic aromatics in Simultaneously test cigarette mainstream flue gas according to claim 1, it is characterized in that: in the internal standard quanitation of step 3) detects, mark and 16 kinds of palycyclic aromatic reference materials in 5 kinds in standard working solution used, solvent is ultrapure water; In in all standard working solution, the concentration of mark naphthalene-d8, acenaphthene-d10, anthracene-d10, benzo [a] anthracene-d12, benzo [a] pyrene-d12 is fixed, and is followed successively by 200ng/L, 50ng/L, 50ng/L, 20ng/L, 20ng/L; In standard working solution, palycyclic aromatic concentration magnitude is followed successively by 0.5ng/L, 1ng/L, 5ng/L, 10ng/L, 50ng/L, 100ng/L, 500ng/L from low to high, and the lower 16 kinds of palycyclic aromatic concentration of each concentration magnitude are all equal.
CN201310383762.XA 2013-08-29 2013-08-29 The method of 16 kinds of palycyclic aromatics in Simultaneously test cigarette mainstream flue gas Active CN103439443B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201310383762.XA CN103439443B (en) 2013-08-29 2013-08-29 The method of 16 kinds of palycyclic aromatics in Simultaneously test cigarette mainstream flue gas

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201310383762.XA CN103439443B (en) 2013-08-29 2013-08-29 The method of 16 kinds of palycyclic aromatics in Simultaneously test cigarette mainstream flue gas

Publications (2)

Publication Number Publication Date
CN103439443A CN103439443A (en) 2013-12-11
CN103439443B true CN103439443B (en) 2015-08-26

Family

ID=49693147

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201310383762.XA Active CN103439443B (en) 2013-08-29 2013-08-29 The method of 16 kinds of palycyclic aromatics in Simultaneously test cigarette mainstream flue gas

Country Status (1)

Country Link
CN (1) CN103439443B (en)

Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104965038B (en) * 2015-04-27 2017-08-15 公安部物证鉴定中心 Using the method for SPME gas chromatography mass spectrometry examination sample Poisoning material
CN104764851B (en) * 2015-05-11 2016-02-24 中国烟草总公司郑州烟草研究院 The assay method of 16 kinds of palycyclic aromatics in a kind of tobacco juice for electronic smoke
CN104931573A (en) * 2015-06-02 2015-09-23 江苏省产品质量监督检验研究院 Analytical method for medium-light tar in biomass gas
CN104865327A (en) * 2015-06-11 2015-08-26 上海衡欣检测技术有限公司 Pretreatment method for detecting polycyclic aromatic hydrocarbon in flue gas
CN106248835B (en) * 2016-09-28 2019-05-31 云南省烟草质量监督检测站 The method for detecting 22 kinds of multiring aromatic hydrocarbon substance contents in cigarette smoke simultaneously
CN106645444B (en) * 2016-09-28 2019-06-04 云南省烟草质量监督检测站 A kind of method of multiring aromatic hydrocarbon substance content in detection smoke-free tobacco product
CN108344831B (en) * 2018-02-08 2020-08-25 国家烟草质量监督检验中心 Method for measuring polycyclic aromatic hydrocarbon in tobacco, main stream smoke or heated non-burning cigarette

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2005008237A1 (en) * 2003-07-17 2005-01-27 Isuzu Motors Limited Device and method for analyzing polycyclic aromatic hydrocarbon having nitro group in diesel particulate
KR100613400B1 (en) * 2004-11-10 2006-08-17 한국과학기술연구원 METHOD FOR DETERMINATION OF PAHs AND PCBs IN SAMPLE BY GC/MS WITH SPME
CN101149359A (en) * 2007-11-09 2008-03-26 西华师范大学 Solid phase micro-extraction probe and its analysis method for polycyclic aromatic hydrocarbon of environmental sample
CN103257194A (en) * 2013-06-08 2013-08-21 国家烟草质量监督检验中心 GC-MS/MS (Gas chromatography - tandem mass spectrometry) method for simultaneously analyzing three polycyclic aromatic hydrocarbons and four tobacco-specific nitrosamines in main stream smoke of cigarettes

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2005008237A1 (en) * 2003-07-17 2005-01-27 Isuzu Motors Limited Device and method for analyzing polycyclic aromatic hydrocarbon having nitro group in diesel particulate
KR100613400B1 (en) * 2004-11-10 2006-08-17 한국과학기술연구원 METHOD FOR DETERMINATION OF PAHs AND PCBs IN SAMPLE BY GC/MS WITH SPME
CN101149359A (en) * 2007-11-09 2008-03-26 西华师范大学 Solid phase micro-extraction probe and its analysis method for polycyclic aromatic hydrocarbon of environmental sample
CN103257194A (en) * 2013-06-08 2013-08-21 国家烟草质量监督检验中心 GC-MS/MS (Gas chromatography - tandem mass spectrometry) method for simultaneously analyzing three polycyclic aromatic hydrocarbons and four tobacco-specific nitrosamines in main stream smoke of cigarettes

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
Chemical and bioanalytical characterisation of PAHs in risk assessment of remediated PAH-contaminated soils;Larsson M 等;《Environment Science Pollution Research》;20130511;第20卷;第8511–8520页 *
PAHs in Cigarette Smoke by Gas Chromatography–Mass Spectrometry;Monica Culea 等;《Indoor and Built Environment》;20051231;第14卷(第3-4期);第283–292页 *
卷烟烟气中多环芳烃的测定;王进 等;《环境化学》;20050131;第24卷(第1期);第101-103页 *
固相微萃取􀀁高效液相色谱联用分析环境水样中的痕量多环芳烃;陶敬奇 等;《色谱》;20031130;第21卷(第6期);第599-602页 *

Also Published As

Publication number Publication date
CN103439443A (en) 2013-12-11

Similar Documents

Publication Publication Date Title
US9914087B2 (en) Sorbent devices and methods of using them
Cowper et al. The analysis of gases by chromatography
Moeder et al. At-line microextraction by packed sorbent-gas chromatography–mass spectrometry for the determination of UV filter and polycyclic musk compounds in water samples
Li et al. Evaluation of multi-walled carbon nanotubes as an adsorbent for trapping volatile organic compounds from environmental samples
Pandey et al. A review of techniques for the determination of polycyclic aromatic hydrocarbons in air
Zlatkis et al. Concentration and analysis of trace volatile organics in gases and biological fluids with a new solid adsorbent
Novotny et al. Some analytical aspects of the chromatographic headspace concentration method using a porous polymer
May et al. Determination of the aqueous solubility of polynuclear aromatic hydrocarbons by a coupled column liquid chromatographic technique
Hou et al. Bis (trifluoromethanesulfonyl) imide-based ionic liquids grafted on graphene oxide-coated solid-phase microextraction fiber for extraction and enrichment of polycyclic aromatic hydrocarbons in potatoes and phthalate esters in food-wrap
Chisvert et al. Simple and commercial readily-available approach for the direct use of ionic liquid-based single-drop microextraction prior to gas chromatography: Determination of chlorobenzenes in real water samples as model analytical application
Hollis et al. Water analysis by gas chromatography using porous polymer columns
Swinnerton et al. Determination of the C1 to C4 hydrocarbons in sea water by gas chromatography
Russell Analysis of air pollutants using sampling tubes and gas chromatography
Jain Direct blood-injection method for gas chromatographic determination of alcohols and other volatile compounds
Zhao et al. Urinary 1-hydroxypyrene as an indicator of human exposure to ambient polycyclic aromatic hydrocarbons in a coal-burning environment
Woolfenden Monitoring VOCs in air using sorbent tubes followed by thermal desorption-capillary GC analysis: summary of data and practical guidelines
Li et al. Zincon-modified activated carbon for solid-phase extraction and preconcentration of trace lead and chromium from environmental samples
Emteborg et al. Speciation of mercury in natural waters by capillary gas chromatography with a microwave-induced plasma emission detector following preconcentration using a dithiocarbamate resin microcolumn installed in a closed flow injection system
Wright et al. On-line supercritical fluid extraction-capillary gas chromatography
Deng et al. Simultaneous determination of eight common odors in natural water body using automatic purge and trap coupled to gas chromatography with mass spectrometry
Cai et al. Determination of organomercury compounds in aqueous samples by capillary gas chromatography-atomic fluorescence spectrometry following solid-phase extraction
Elke et al. Determination of benzene, toluene, ethylbenzene and xylenes in indoor air at environmental levels using diffusive samplers in combination with headspace solid-phase microextraction and high-resolution gas chromatography–flame ionization detection
Pellizzari et al. Determination of trace hazardous organic vapor pollutants in ambient atmospheres by gas chromatography/mass spectrometry/computer
US4180389A (en) Isolation and concentration of sample prior to analysis thereof
Gallego et al. Comparative study of the adsorption performance of a multi-sorbent bed (Carbotrap, Carbopack X, Carboxen 569) and a Tenax TA adsorbent tube for the analysis of volatile organic compounds (VOCs)

Legal Events

Date Code Title Description
PB01 Publication
C06 Publication
SE01 Entry into force of request for substantive examination
C10 Entry into substantive examination
GR01 Patent grant
C14 Grant of patent or utility model