CN103439443A - Method for simultaneously measuring 16 polyaromatic hydrocarbons in mainstream smoke of cigarettes - Google Patents
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Abstract
The invention discloses a method for simultaneously measuring 16 polyaromatic hydrocarbons in mainstream smoke of cigarettes. The method comprises the following steps of (1) trapping dry particulate matters in the mainstream smoke of the cigarettes through a Cambridge filter, then transferring the Cambridge filter into an extraction container, adding an internal standard mixed solution, and then adding methyl alcohol for oscillation extraction to obtain a methyl alcohol extracting liquid; (2) diluting the methyl alcohol extracting liquid through super-pure water to obtain a diluent, and performing selective extraction on the diluent through an immersion type solid phase microextraction technology to obtain a smoke sample; (3) detecting the smoke sample through a GC-MS (gas chromatography-mass spectrometer) to detect the smoke sample, and detecting the content of the 16 polyaromatic hydrocarbons through an internal standard quantification method. The method can be used for simultaneously measuring the content of the 16 polyaromatic hydrocarbons in the mainstream smoke of the cigarettes by the GC-MS method, has the advantages of high detection speed, high sensitivity, high selectivity and high precision and is suitable for measurement of the content of polyaromatic hydrocarbon in smoke of low-tar cigarettes.
Description
Technical field
The invention belongs to palycyclic aromatic detection technique field, be specifically related to a kind of method of simultaneously measuring 16 kinds of palycyclic aromatics in cigarette mainstream flue gas.
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Background technology
Smoking is harmful to your health, and the cigarette healthhazard mainly objectionable impurities in flue gas causes, and the objectionable constituent burst size that detects and control in flue gas is the tobacco business obligation one can't decline.Polycyclic arene compound is objectionable impurities main in flue gas, and human body is had to carcinogenic, teratogenesis.Because smoke components is very complicated, and the content of polycyclic aromatic hydrocarbon compounds in flue gas is trace, substantially prop up magnitude at ng/, matrix interference is serious, detection difficulty is larger, therefore current researcher often only pays close attention to the content of benzo [a] pyrene of cigarette smoke Poisoning maximum, and method commonly used is national standard method " mensuration of benzo in the cigarette smoke TPM [a] pyrene " (GB 21130-2007-T).But, announced 69 kinds of objectionable constituent inventories at HOFFMANN in calendar year 2001, wherein palycyclic aromatic has accounted for 10 kinds.The document of simultaneously measuring at present multiple palycyclic aromatic is less, and it is not ideal enough to detect effect.Therefore, develop that a kind of to measure the new method quick, sensitive, high selectivity of multiple palycyclic aromatic in cigarette smoke be very necessary simultaneously.
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Summary of the invention
The purpose of this invention is to provide a kind of fast detecting, highly sensitive, selectivity good, degree of accuracy is measured the method for 16 kinds of palycyclic aromatics in cigarette mainstream flue gas high the time.
In order to realize above purpose, the technical solution adopted in the present invention is: measure the method for 16 kinds of palycyclic aromatics in cigarette mainstream flue gas simultaneously, comprise the following steps:
1) with after cambridge filter trapping cigarette mainstream flue gas granule phase substance, cambridge filter is proceeded to extraction vessel, add inner mark solution, then add methyl alcohol to shake 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 solutions of 5 kinds of deuteriums for internal standard compound, and 5 kinds of deuteriums are naphthalene-d8, acenaphthene-d10, anthracene-d10, benzo [a] anthracene-d12, benzo [a] pyrene-d12 for internal standard compound, and solvent is methyl alcohol; In inner mark solution, the content of naphthalene-d8 is 200 μ g/mL, and the content of acenaphthene-d10 is 5 μ g/mL, and the content that the content that the content of anthracene-d10 is 5 μ g/mL, benzo [a] anthracene-d12 is 2 μ g/mL, benzo [a] pyrene-d12 is 2 μ g/mL.
2) by methanol extract liquid with after 50～500 times of ultrapure water dilutions dilution, adopt the immersion solid-phase microextraction technology to carry out selective extraction to dilution, obtain the flue gas sample;
The concrete operations that adopt the immersion solid-phase microextraction technology to carry out selective extraction to dilution are: dilution is placed in to the solid-phase microextraction bottle, after balance 30min, insert solid-phase micro-extraction fibre extraction 40～60min under 50～70 ℃, 300～800rpm rotating speed stirring condition.Described solid-phase micro-extraction fibre is Graphene type solid-phase micro-extraction fibre or carbon nano tube type solid-phase micro-extraction fibre.Graphene 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 " method for preparing fast the solid-phase micro-extraction coating " (patent No.: 201210105077.6).
Described flue gas 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 to the gas chromatographic sample introduction mouth and carries out pyrolysis and analyse sample introduction.
3) adopt GC-MS to be detected the flue gas sample, by interior scalar quantity method, detect 16 kinds of polycyclic aromatic hydrocarbon contents.
Chromatographic condition is: chromatographic column: DB-5ms (30m * 0.25mm * 0.25 μ m); Carrier gas: He; Flow velocity: 1.0ml/min; Injector temperature: 290 ℃; Adopt and do not shunt bushing pipe; The time is analysed in pyrolysis: 2-5min; Heating schedule: since 50 ℃, be raised to 130 ℃ with the programming rate of 10 ℃/min, then be raised to 300 ℃ with the programming rate of 5 ℃/min, keep 5min.
The mass spectrum condition is: adopt single ion detection pattern (SIM), quota ion is in Table 1; Ion source temperature is 300 ℃, and level Four bar temperature is 180 ℃.
16 kinds of polycyclic aromatic hydrocarbon compounds of table 1 and interior entitling claims, quota ion information
| Numbering | Title | Quota ion |
| |
Naphthalene-d8 | 136 |
| 1 | Naphthalene | 128 |
| |
Acenaphthene-d10 | 164 |
| 2 | Naphtho-ethene | 152 |
| 3 | Acenaphthene | 152 |
| 4 | Fluorenes | 166 |
| |
Anthracene-d10 | 188 |
| 5 | Luxuriant and rich with fragrance | 178 |
| 6 | Anthracene | 178 |
| 7 | Fluoranthene | 202 |
| 8 | Pyrene | 202 |
| |
Benzo [a] anthracene-d12 | 240 |
| 9 | Benzo [a] anthracene | 228 |
| 10 | Bend | 228 |
| |
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 interior scalar quantity method detects, in standard operation solution used, in 5 kinds, to mark and 16 kinds of palycyclic aromatic reference materials, solvent is ultrapure water; In in all standard operation 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 operation 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 all equate.
The quantitative curve of 16 kinds of palycyclic aromatics, the range of linearity, detection limit, quantitative limit are as shown in table 2.
The method of simultaneously measuring 16 kinds of palycyclic aromatics in cigarette mainstream flue gas of the present invention, adopt solid-phase microextraction-combined gas chromatography mass spectrometry, but the content of 16 kinds of palycyclic aromatics in the Rapid Simultaneous Determination cigarette mainstream flue gas.Because the Graphene or the carbon nanotube coating solid-phase micro-extraction fibre that adopt have adsorptive selectivity to multiring aromatic hydrocarbon substance, the inventive method clean-up effect is better than traditional Solid-Phase Extraction method.The present invention adopts methanol extraction to Smoke Particulate, and extract carries out solid-phase microextraction after diluting 50-500 times.In the situation that extension rate is 500 times, sensitivity of the present invention has been 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.
The accompanying drawing explanation
The SIM figure that Fig. 1 is 16 kinds of palycyclic aromatic standard specimens;
The SIM of the palycyclic aromatic of numbering 1 figure in the cigarette mainstream flue gas that Fig. 2 is embodiment 1;
Number the SIM figure of 2,3 palycyclic aromatic in the cigarette mainstream flue gas that Fig. 3 is embodiment 1;
The SIM of the palycyclic aromatic of numbering 4 figure in the cigarette mainstream flue gas that Fig. 4 is embodiment 1;
Number the SIM figure of 5,6 palycyclic aromatic in the cigarette mainstream flue gas that Fig. 5 is embodiment 1;
Number the SIM figure of 7,8 palycyclic aromatic in the cigarette mainstream flue gas that Fig. 6 is embodiment 1;
Number the SIM figure of 9,10 palycyclic aromatic in the cigarette mainstream flue gas that Fig. 7 is embodiment 1;
Number the SIM figure of 11,12,13 palycyclic aromatic in the cigarette mainstream flue gas that Fig. 8 is embodiment 1;
Number the SIM figure of 14,15,16 palycyclic aromatic in the cigarette mainstream flue gas that Fig. 9 is 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.
Measure the method for 16 kinds of palycyclic aromatics in cigarette mainstream flue gas in the time of the present embodiment, comprise 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, with after 5 cigarette mainstream flue gas granule phase substances of 1 cambridge filter trapping, at the bottom of cambridge filter is proceeded to the ground conical flask of 100ml and being laid in bottle, add 50 μ L inner mark solutions, add again the concussion of 30ml methyl alcohol to extract 40min, obtain methanol extract liquid;
Described inner mark solution is the mixed solutions of 5 kinds of deuteriums for internal standard compound, and described 5 kinds of deuteriums are naphthalene-d8, acenaphthene-d10, anthracene-d10, benzo [a] anthracene-d12, benzo [a] pyrene-d12 for internal standard compound, and solvent is methyl alcohol; In described inner mark solution, the content of naphthalene-d8 is 200 μ g/mL, and the content of acenaphthene-d10 is 5 μ g/mL, and the content that the content that the content of anthracene-d10 is 5 μ g/mL, benzo [a] anthracene-d12 is 2 μ g/mL, benzo [a] pyrene-d12 is 2 μ g/mL;
2) by step 1) gained methanol extract liquid with after 50 times of ultrapure water dilutions dilution, adopt the immersion solid-phase microextraction technology to carry out selective extraction to dilution, be about to the 25ml dilution and be placed in solid-phase microextraction bottle (the screw socket sealing gland bottle of 30ml), under 65 ℃, 500rpm rotating speed stirring condition after balance 30min, insert Graphene solid-phase micro-extraction fibre (35 μ m thickness) extraction 60min, obtain flue gas sample (being adsorbed on the testing sample on solid-phase micro-extraction fibre);
3) adopting GC-MS to step 2) gained flue gas sample detected, and the solid-phase micro-extraction fibre that is about to absorption and has testing sample is placed in the gas chromatographic sample introduction mouth to carry out pyrolysis and analyses sample introduction, and the pyrolysis time of analysing is 5min;
The analysis condition that GC-MS detects:
Chromatographic condition is: chromatographic column: DB-5ms (30m * 0.25mm * 0.25 μ m); Carrier gas: He; Flow velocity: 1.0ml/min; Injector temperature: 290 ℃; Adopt and do not shunt bushing pipe; The time is analysed in pyrolysis: 5min; Heating schedule: since 50 ℃, be raised to 130 ℃ with the programming rate of 10 ℃/min, then be raised to 300 ℃ with the programming rate of 5 ℃/min, keep 5min.
The mass spectrum condition is: adopt single ion detection pattern, ion source temperature is 300 ℃, and level Four bar temperature is 180 ℃.
The method of measuring 16 kinds of palycyclic aromatics in cigarette mainstream flue gas in the time of the present embodiment is as shown in table 3 to the cigarette testing result of the trade mark 1.
Measure the method for 16 kinds of palycyclic aromatics in cigarette mainstream flue gas in the time of the present embodiment, comprise 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, with after 10 cigarette mainstream flue gas granule phase substances of 2 cambridge filter trappings, at the bottom of 2 cambridge filters are proceeded to the 100ml conical flask and being laid in bottle, add 50 μ L inner mark solutions, add again the concussion of 40ml methyl alcohol to extract 50min, obtain methanol extract liquid;
Described inner mark solution is the mixed solutions of 5 kinds of deuteriums for internal standard compound, and described 5 kinds of deuteriums are naphthalene-d8, acenaphthene-d10, anthracene-d10, benzo [a] anthracene-d12, benzo [a] pyrene-d12 for internal standard compound, and solvent is methyl alcohol; In described inner mark solution, the content of naphthalene-d8 is 200 μ g/mL, and the content of acenaphthene-d10 is 5 μ g/mL, and the content that the content that the content of anthracene-d10 is 5 μ g/mL, benzo [a] anthracene-d12 is 2 μ g/mL, benzo [a] pyrene-d12 is 2 μ g/mL;
2) by step 1) gained methanol extract liquid with after 500 times of ultrapure water dilutions dilution, adopt the immersion solid-phase microextraction technology to carry out selective extraction to dilution, be about to the 25ml dilution and be placed in solid-phase microextraction bottle (the screw socket sealing gland bottle of 30ml), under 70 ℃, 800rpm rotating speed stirring condition after balance 30min, insert Graphene solid-phase micro-extraction fibre (35 μ m thickness) extraction 40min, obtain flue gas sample (being adsorbed on the testing sample on solid-phase micro-extraction fibre);
3) adopting GC-MS to step 2) gained flue gas sample detected, and the solid-phase micro-extraction fibre that is about to absorption and has testing sample is placed in the gas chromatographic sample introduction mouth to carry out pyrolysis and analyses sample introduction, and the pyrolysis time of analysing is 4min;
The analysis condition that GC-MS detects:
Chromatographic condition is: chromatographic column: DB-5ms (30m * 0.25mm * 0.25 μ m); Carrier gas: He; Flow velocity: 1.0ml/min; Injector temperature: 290 ℃; Adopt and do not shunt bushing pipe; The time is analysed in pyrolysis: 4min; Heating schedule: since 50 ℃, be raised to 130 ℃ with the programming rate of 10 ℃/min, then be raised to 300 ℃ with the programming rate of 5 ℃/min, keep 5min.
The mass spectrum condition is: adopt single ion detection pattern, ion source temperature is 300 ℃, and level Four bar temperature is 180 ℃.
The method of measuring 16 kinds of palycyclic aromatics in cigarette mainstream flue gas in the time of the present embodiment is as shown in table 3 to the cigarette testing result of the trade mark 2.
Measure the method for 16 kinds of palycyclic aromatics in cigarette mainstream flue gas in the time of the present embodiment, comprise 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, with after 8 cigarette mainstream flue gas granule phase substances of 2 cambridge filter trappings, at the bottom of 2 cambridge filters are proceeded to the 100ml conical flask and being laid in bottle, add 100 μ L inner mark solutions, add again the concussion of 50ml methyl alcohol to extract 60min, obtain methanol extract liquid;
Described inner mark solution is the mixed solutions of 5 kinds of deuteriums for internal standard compound, and described 5 kinds of deuteriums are naphthalene-d8, acenaphthene-d10, anthracene-d10, benzo [a] anthracene-d12, benzo [a] pyrene-d12 for internal standard compound, and solvent is methyl alcohol; In described inner mark solution, the content of naphthalene-d8 is 200 μ g/mL, and the content of acenaphthene-d10 is 5 μ g/mL, and the content that the content that the content of anthracene-d10 is 5 μ g/mL, benzo [a] anthracene-d12 is 2 μ g/mL, benzo [a] pyrene-d12 is 2 μ g/mL;
2) by step 1) gained methanol extract liquid with after 300 times of ultrapure water dilutions dilution, adopt the immersion solid-phase microextraction technology to carry out selective extraction to dilution, be about to the 25ml dilution and be placed in solid-phase microextraction bottle (the screw socket sealing gland bottle of 30ml), under 50 ℃, 300rpm rotating speed stirring condition after balance 30min, insert carbon nano-tube solid phase micro-extraction fiber (35 μ m thickness) extraction 50min, obtain flue gas sample (being adsorbed on the testing sample on solid-phase micro-extraction fibre);
3) adopting GC-MS to step 2) gained flue gas sample detected, and the solid-phase micro-extraction fibre that is about to absorption and has testing sample is placed in the gas chromatographic sample introduction mouth to carry out pyrolysis and analyses sample introduction, and the pyrolysis time of analysing is 2min;
The analysis condition that GC-MS detects:
Chromatographic condition is: chromatographic column: DB-5ms (30m * 0.25mm * 0.25 μ m); Carrier gas: He; Flow velocity: 1.0ml/min; Injector temperature: 290 ℃; Adopt and do not shunt bushing pipe; The time is analysed in pyrolysis: 2min; Heating schedule: since 50 ℃, be raised to 130 ℃ with the programming rate of 10 ℃/min, then be raised to 300 ℃ with the programming rate of 5 ℃/min, keep 5min.
The mass spectrum condition is: adopt single ion detection pattern, ion source temperature is 300 ℃, and level Four bar temperature is 180 ℃.
The method of measuring 16 kinds of palycyclic aromatics in cigarette mainstream flue gas in the time of the present embodiment is as shown in table 3 to the cigarette testing result of the trade mark 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, with 10 cigarette smoke granule phase substances of 2 cambridge filter trappings.Method according to embodiment 1 is measured, 6 groups of replicate determinations, and the RSD value of 6 replicate determination values of 16 palycyclic aromatics (in Table 4) between 5%-12%, prove 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 (9)
1. a method of simultaneously measuring 16 kinds of palycyclic aromatics in cigarette mainstream flue gas, is characterized in that: comprise the following steps:
1) with after cambridge filter trapping cigarette mainstream flue gas granule phase substance, cambridge filter is proceeded to extraction vessel, add inner mark solution, then add methyl alcohol to shake extraction, obtain methanol extract liquid;
2) by methanol extract liquid with after 50～500 times of ultrapure water dilutions dilution, adopt the immersion solid-phase microextraction technology to carry out selective extraction to dilution, obtain the flue gas sample;
3) adopt GC-MS to be detected the flue gas sample, by interior scalar quantity method, detect 16 kinds of polycyclic aromatic hydrocarbon contents.
2. the method for simultaneously measuring 16 kinds of palycyclic aromatics in cigarette mainstream flue gas according to claim 1, it 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 simultaneously measuring 16 kinds of palycyclic aromatics in cigarette mainstream flue gas according to claim 1 and 2, it is characterized in that: described inner mark solution is the mixed solutions of 5 kinds of deuteriums for internal standard compound, 5 kinds of deuteriums are naphthalene-d8, acenaphthene-d10, anthracene-d10, benzo [a] anthracene-d12, benzo [a] pyrene-d12 for internal standard compound, and solvent is methyl alcohol; In inner mark solution, the content of naphthalene-d8 is 200 μ g/mL, and the content of acenaphthene-d10 is 5 μ g/mL, and the content that the content that the content of anthracene-d10 is 5 μ g/mL, benzo [a] anthracene-d12 is 2 μ g/mL, benzo [a] pyrene-d12 is 2 μ g/mL.
4. the method for simultaneously measuring 16 kinds of palycyclic aromatics in cigarette mainstream flue gas according to claim 1, it is characterized in that: the concrete operations that adopt the immersion solid-phase microextraction technology to carry out selective extraction to dilution are: dilution is placed in to the solid-phase microextraction bottle, after balance 30min, insert solid-phase micro-extraction fibre extraction 40～60min under 50～70 ℃, 300～800rpm rotating speed stirring condition.
5. the method for simultaneously measuring 16 kinds of palycyclic aromatics in cigarette mainstream flue gas according to claim 4, it is characterized in that: described solid-phase micro-extraction fibre is Graphene type solid-phase micro-extraction fibre or carbon nano tube type solid-phase micro-extraction fibre.
6. the method for simultaneously measuring 16 kinds of palycyclic aromatics in cigarette mainstream flue gas according to claim 1, it is characterized in that: described flue gas 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 to the gas chromatographic sample introduction mouth and carries out pyrolysis and analyse sample introduction.
7. the method for simultaneously measuring 16 kinds of palycyclic aromatics in cigarette mainstream flue gas according to claim 1, it is characterized in that: the chromatographic condition detected described in step 3) is: chromatographic column: DB-5ms (30m * 0.25mm * 0.25 μ m); Carrier gas: He; Flow velocity: 1.0ml/min; Injector temperature: 290 ℃; Adopt and do not shunt bushing pipe; The time is analysed in pyrolysis: 2-5min; Heating schedule: since 50 ℃, be raised to 130 ℃ with the programming rate of 10 ℃/min, then be raised to 300 ℃ with the programming rate of 5 ℃/min, keep 5min.
8. the method for simultaneously measuring 16 kinds of palycyclic aromatics in cigarette mainstream flue gas according to claim 1, it is characterized in that: the mass spectrum condition detected described in step 3) is: adopt single ion detection pattern, ion source temperature is 300 ℃, and level Four bar temperature is 180 ℃.
9. the method for simultaneously measuring 16 kinds of palycyclic aromatics in cigarette mainstream flue gas according to claim 1, it is characterized in that: in the interior scalar quantity method of step 3) detects, in standard operation solution used, in 5 kinds, mark and 16 kinds of palycyclic aromatic reference materials, solvent is ultrapure water; In in all standard operation 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 operation 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 all equate.
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| CN104764851A (en) * | 2015-05-11 | 2015-07-08 | 中国烟草总公司郑州烟草研究院 | Method for measuring sixteen polycyclic aromatic hydrocarbons in cigarette liquid of electronic cigarette |
| 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 |
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| CN104965038A (en) * | 2015-04-27 | 2015-10-07 | 公安部物证鉴定中心 | Method for screening toxic substances in sample by using solid phase microextraction-GC-MS |
| CN106248835A (en) * | 2016-09-28 | 2016-12-21 | 云南省烟草质量监督检测站 | The method of 22 kinds of multiring aromatic hydrocarbon substance content in detection cigarette smoke simultaneously |
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| CN108344831A (en) * | 2018-02-08 | 2018-07-31 | 国家烟草质量监督检验中心 | It one grows tobacco, main flume or heating are not burnt the assay method of polycyclic aromatic hydrocarbon in cigarette |
| CN113406238A (en) * | 2021-06-29 | 2021-09-17 | 湖北中烟工业有限责任公司 | Efficient detection method for volatile components in cigarette smoke |
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Citations (4)
| 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 |
-
2013
- 2013-08-29 CN CN201310383762.XA patent/CN103439443B/en active Active
Patent Citations (4)
| 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 (5)
| Title |
|---|
| LARSSON M 等: "Chemical and bioanalytical characterisation of PAHs in risk assessment of remediated PAH-contaminated soils", 《ENVIRONMENT SCIENCE POLLUTION RESEARCH》 * |
| MONICA CULEA 等: "PAHs in Cigarette Smoke by Gas Chromatography–Mass Spectrometry", 《INDOOR AND BUILT ENVIRONMENT》 * |
| 王进 等: "卷烟烟气中多环芳烃的测定", 《环境化学》 * |
| 陶敬奇 等: "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", 《色谱》, vol. 21, no. 6, 30 November 2003 (2003-11-30), pages 599 - 602 * |
| 陶敬奇 等: "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", 《色谱》 * |
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