CN104049056A - Method for determining content of benzo [alpha] pyrene in total particulate matters in smoke - Google Patents
Method for determining content of benzo [alpha] pyrene in total particulate matters in smoke Download PDFInfo
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Abstract
The invention discloses a method for determining the content of benzo [alpha] pyrene in total particulate matters in smoke. The method comprises the steps of preparing a benzo [alpha] pyrene methanol extraction solution; preparing a sample solution; analyzing the sample solution by a gas chromatography-mass spectrometry method, and calculating the content of benzo [alpha] pyrene in the total particulate matters in the smoke. The ionic liquid adopted in the method has a better enriching capability on benzo [alpha] pyrene, and has a purifying effect superior to that of a conventional solid-phase extraction method; the consumption of toxic and organic reagents in a purification process is reduced from 50-200 mL per one sample in a conventional method to 1 mL per sample, and a concentration step in a pretreatment process is omitted; under the condition of ensuring the sensitivity and the recovery rate, the treatment step is simplified, and damages of organic solvents to environments and experimenters are greatly reduced.
Description
Technical field
The invention belongs to benzo [α] pyrene detection technique field, be specifically related to the assay method of benzo [α] pyrene content in a kind of flue gas TPM.
Background technology
Palycyclic aromatic is the aromatic organic compounds that a class has multiple phenyl ring, is one of environmental contaminants of finding the earliest to have " carcinogenic, teratogenesis, mutagenesis " effect, is also that the class in cigarette mainstream flue gas mainly contains harmful substances.All belong to carcinogenic compound completely taking benzo [α] pyrene as representational several palycyclic aromatics.Chemical Components in Cigarette Smoke is very complicated, and polycyclic aromatic hydrocarbon content is lower, generally in the flue gas of every cigarette, content is only several to tens nanograms, this detects to the separation of palycyclic aromatic and brings very large difficulty, therefore, set up accurately and reliably, easy Polycyclic Aromatic Hydrocarbons in Cigarette Smoke analytical approach, be not only the important content of tobacco quality control, and can provide direct basis to the harm of human health for assessment smoking.
Ionic liquid is the material of ionic state, and volatility is very low, nonflammable, Heat stability is good, and this has just ensured that it does not have to environment the pollution that volatile organic solvent causes in the past.Because the pressure of environment is strengthening gradually, the research and development of ionic liquid at room temperature are more paid attention to gradually.Its peculiar property makes it can be advantageously applied to liquid-liquid extraction, liquid-phase micro-extraction, solid-phase microextraction, SCF-CO 2 as extraction solvent (organic phase, i.e. extraction phase, hydrophobic phase).
Liquid-liquid extraction detachment process is as the effective separation method of one, and range of application is very extensive.In the past in extracting operation process the standard of slective extraction agent substantially taking effect of extracting as criterion, consider less to environmental factor, this has caused organic solvent high volatility, the toxicity of use large, consumption is large, and this has just caused the variety of issues such as environmental and human health impacts harm.According to the thought of Green Chemistry, scientific worker must choice for use green solvent, eliminates the shortcoming extraction process in the past from source, and whole process is become to environmental protection technique.
The existing standard method of benzo [α] pyrene in cigarette mainstream flue gas is " mensuration of benzo [α] pyrene in GB/T21130-2007 cigarette smoke TPM ".In existing GB detection method, cyclohexane extracts the mode that adopts silicagel column to purify after benzo [α] pyrene, comprises the steps such as post activation, loading, drip washing, then 40mL eluent is revolved to steaming mode by vacuum to be concentrated into about 1mL; Another kind of common method, cyclohexane is used Full-automatic solid phase extraction instrument to purify and concentrates after extracting benzo [α] pyrene, and the method reagent consumption is large.
Summary of the invention
The object of this invention is to provide the assay method of benzo [α] pyrene in a kind of rapid and accurate determination cigarette smoke TPM, adopt liquid-liquid extraction separation method to obtain fast sample solution.
In order to reach above-mentioned technique effect, the present invention takes following technical scheme:
The assay method of benzo [α] pyrene content in a kind of flue gas TPM, comprises the following steps:
The preparation of A, benzo [α] pyrene methanol extract liquid
With cambridge filter trapping cigarette smoke granule phase substance, then cambridge filter is proceeded in extraction vessel, add the d of 1mL concentration 201.6ng/mL
12-BaP cyclohexane solution is as inner mark solution, then adds 40mL methyl alcohol to carry out ultrasonic extraction, obtains benzo [α] pyrene methanol extract liquid;
The preparation of B, sample solution
10mL benzo [α] pyrene methanol extract liquid is placed in to 50mL conical bottom plastic centrifuge tube, add 100 μ L～600 μ L imidazoles hexafluorophosphoric acid salt ionic liquid and 10～40mL water, in vortex instrument, carry out vortex 1～4min, then centrifugal 7～12min under rotating speed 7000rpm～9000rpm, remove supernatant, add again 1～2mL cyclohexane, carry out again vortex 1～2min, then centrifugal 7～12min under rotating speed 10000rpm～12000rpm, then filter with 0.45 μ m filter membrane, the filtrate of collection is sample solution;
C, gas chromatography-mass spectrography are measured
Gas Chromatography-Mass Spectrometry step is as follows:
The preparation of a, series standard solution
Taking cyclohexane give as solvent, preparation benzo [α] pyrene concentration 10ng/mL, 20ng/mL, 40ng/mL, 100ng/mL, 200ng/mL and 300ng/mL, and the series standard solution of interior mark concentration 201.6ng/mL;
The drafting of b, typical curve
The standard serial solution that step a obtains carries out gas chromatography-mass spectrography analysis, benzo in chromatogram [α] the pyrene peak area of comparing of benzo in standard serial solution [α] pyrene concentration and interior mark concentration is drawn with the ratio of interior mark peak area, obtain typical curve Y=kX+b by its figure, in formula, k represents the slope of this linear equation, b represents the intercept of this linear equation, X represents the ratio of benzo [α] pyrene and interior target concentration, and Y represents the ratio of benzo [α] pyrene and interior target peak area;
Detection and the calculating of benzo [α] pyrene content in c, flue gas TPM
Under the condition determination identical with step b, the sample solution that step B obtains carries out gas chromatography-mass spectrography analysis, record benzo in sample solution [α] pyrene peak area and interior mark peak area, adopt following computing formula to obtain benzo in flue gas TPM [α] pyrene content:
In formula:
Benzo [α] pyrene content in every cigarette of m=, unit is that ng/ props up;
A
xfor benzo [α] pyrene peak area;
A
isfor interior mark peak area;
B is linear equation intercept;
K is linear equation slope;
M
isfor interior scalar in benzo [α] pyrene methanol extract liquid, unit is ng;
N=cigarette quantity, unit is for propping up.
The gas chromatography of according to one embodiment of present invention, described GC-MS(gas chromatography-mass spectrography) and mass spectrographic test condition are as follows:
Gas Chromatographic Determination condition is as follows: chromatographic column: specification is the Elite-5Ms of 30m × 0.25mm × 0.25 μ m; Injector temperature: 280 DEG C; Sample size: 1 μ L; Carrier gas: helium, purity >=99.999%; Do not shunt; Flow velocity: 1.2mL/min; Heating schedule: 150 DEG C of initial temperatures also keep 1min, then be warming up to 280 DEG C and keep 20min with 6 DEG C/min of speed;
Mass spectrophotometry condition is as follows: transmission line temperature: 280 DEG C; Ionization EI energy 70eV; Ion source temperature: 230 DEG C; Solvent delay time 19min, selects ion scan Mode S IM fractional scanning, carries out quantitative test with characteristic ion.
According to one embodiment of present invention, described ionic liquid is 1-hexyl-3-methylimidazole hexafluorophosphate or 1-octyl group-3-methyl-imidazoles hexafluorophosphate.
According to one embodiment of present invention, under being the condition of ultrasonic power 400～500w, the ultrasonic extraction described in steps A carries out ultrasonic processing 35-45min.
According to one embodiment of present invention, the inner mark solution preparation steps of described concentration 201.6ng/mL is as follows:
1) preparation of mark storing solution I in: accurately take 25.2mg D
12-bap, in 100mL volumetric flask, is settled to scale and mixes with cyclohexane, and obtaining concentration is the interior mark storing solution I of 0.252mg/mL;
2) preparation of mark storing solution II in: accurately pipette in 2mL mark storing solution I in 50mL volumetric flask, be settled to scale and shake up with cyclohexane, obtaining concentration is the interior mark storing solution II of 10.08 μ g/mL;
3) preparation of inner mark solution: accurately pipette in 2mL mark storing solution II in 100mL volumetric flask, be settled to scale and shake up with cyclohexane, obtain the inner mark solution that concentration is 201.6ng/mL.
The preparation steps of according to one embodiment of present invention, described standard serial solution is as follows:
1) preparation of standard reserving solution I: accurately take 10mg benzo [α] pyrene in 100mL volumetric flask, dissolve and be settled to scale with cyclohexane, mix and obtain the standard reserving solution I that concentration is 100 μ g/mL;
2) preparation of standard reserving solution II: accurately pipette 1mL standard reserving solution I in 100mL volumetric flask, dissolve and be settled to scale with cyclohexane, mix and obtain the standard reserving solution II that concentration is 1 μ g/mL;
3) preparation of standard serial solution: pipette respectively 0.5mL, 1mL, 2mL, 5mL, 10mL and 15mL standard reserving solution II in 50mL volumetric flask, then add successively the interior mark storing solution II described in 1mL, be settled to scale and shake up with cyclohexane, obtain 6 other standard serial solutions of concentration level, wherein benzo [α] pyrene concentration is followed successively by 10ng/mL, 20ng/mL, 40ng/mL, 100ng/mL, 200ng/mL, 300ng/mL, and interior mark concentration is 201.6ng/mL.
According to one embodiment of present invention, described collect according to the standard of GB/T19609-2004 with cambridge filter trapping cigarette smoke granule phase substance.
In this assay method, obtain methanol extraction liquid with methanol extraction benzo [α] pyrene, add afterwards ionic liquid, ionic liquid is dissolved in methyl alcohol.Due to distribution ratio difference, benzo [α] pyrene can be transferred in ionic liquid from methyl alcohol, and at this moment solution is transparent, and ion liquid dissolving cannot be precipitated out in methyl alcohol.After adding water in this solution, can form emulsion, centrifugal to this emulsion, ionic liquid will be precipitated out, and benzo [α] pyrene has just been enriched in ionic liquid from methyl alcohol like this.The ionic liquid density being precipitated out is larger, cannot directly enter GC-MS analyzes, so mix with holding volatile cyclohexane and ionic liquid, benzo [α] pyrene reaches partition equilibrium in cyclohexane and ionic liquid, part benzo [α] pyrene is transferred in cyclohexane from ionic liquid, finally enters GC-MS with this cyclohexane and analyzes.
The present invention compared with prior art, has following beneficial effect:
The ionic liquid that this method adopts has good accumulation ability to benzo [α] pyrene, clean-up effect is better than traditional Solid-Phase Extraction method, in purification process, the use amount of poisonous organic reagent is reduced to the each sample of 1mL from the each sample of 50mL～200mL of classic method, and has avoided the concentration step in pretreatment process.The present invention, ensureing, under the condition of sensitivity, the recovery, to have simplified treatment step, greatly reduces the harm of organic solvent to environment and experimenter.
Brief description of the drawings
Fig. 1 is the process flow diagram of assay method of the present invention.
Embodiment
Below in conjunction with embodiments of the invention, the invention will be further elaborated.
Embodiment 1:
1, instrument and reagent
Reagent: benzo [α] pyrene, interior mark d12-BaP are standard items; Ionic liquid is 1-hexyl-3-methylimidazole hexafluorophosphate, purity >99%; Methyl alcohol, cyclohexane are chromatographically pure reagent; Water is deionized water.
Instrument: Perkin Elmer Clarus600GC, PE Clarus SQ8T MS gas chromatograph-mass spectrometer, Mettler Toledo electronic balance, IKA MS1Minishaker vortice, Sigma3K15 hydro-extractor.
2, the preparation of inner mark solution
1) preparation of mark storing solution I in: accurately take 25.2mg D12-bap in 100mL volumetric flask, be settled to scale and mix with cyclohexane, obtaining concentration is the interior mark storing solution I of 0.252mg/mL;
2) preparation of mark storing solution II in: accurately pipette in 2mL mark storing solution I in 50mL volumetric flask, be settled to scale and shake up with cyclohexane, obtaining concentration is the interior mark storing solution II of 10.08 μ g/mL;
3) preparation of inner mark solution: accurately pipette in 2mL mark storing solution II in 100mL volumetric flask, be settled to scale and shake up with cyclohexane, obtain the inner mark solution that concentration is 201.6ng/mL.
3, the preparation of standard serial solution
1) preparation of standard reserving solution I: accurately take 10mg benzo [α] pyrene in 100mL volumetric flask, dissolve and be settled to scale with cyclohexane, mix and obtain the standard reserving solution I that concentration is 100 μ g/mL;
2) preparation of standard reserving solution II: accurately pipette 1mL standard reserving solution I in 100mL volumetric flask, dissolve and be settled to scale with cyclohexane, mix and obtain the hybrid standard storing solution II that concentration is 1 μ g/mL;
3) preparation of standard serial solution: pipette respectively 0.5mL, 1mL, 2mL, 5mL, 10mL, 15mL standard reserving solution II in 50mL volumetric flask, then add successively the interior mark storing solution II of 1mL, be settled to scale and shake up with cyclohexane, obtain 6 other standard serial solutions of concentration level, wherein benzo [α] pyrene concentration is followed successively by 10ng/mL, 20ng/mL, 40ng/mL, 100ng/mL, 200ng/mL, 300ng/mL, and interior mark concentration is 201.6ng/mL.
4, the preparation of benzo [α] pyrene methanol extract liquid
Collect after 20 cigarette smoke granule phase substances according to the requirement of GB/T19609 with Cambridge filter paper, cambridge filter is proceeded to extraction vessel, add the d of 1mL concentration 201.6ng/mL
12-BaP cyclohexane solution is as inner mark solution, then adds ultrasonic extraction 40min under the condition that 40mL methyl alcohol is 400W at ultrasonic power, obtains benzo [α] pyrene methanol extract liquid.
5, the preparation of sample solution
10mL benzo [α] pyrene methanol extract liquid is placed in to 50mL conical bottom plastic centrifuge tube, add 100 μ L ionic liquids and 20～40mL water, in vortex instrument, carry out vortex 2min, then under rotating speed 8000rpm, after centrifugal 10min, remove supernatant, add again 1mL cyclohexane, then carry out vortex 1min, then centrifugal 10min under rotating speed 11000rpm, then filter with 0.45 μ m filter membrane, the filtrate of collection is sample solution.
6, the drafting of typical curve
Standard serial solution is carried out to GC-MS(gas chromatography-mass spectrography) analysis, by the ratio mapping of comparing benzo in chromatogram [α] pyrene peak area and interior mark peak area of the content of benzo in standard serial solution [α] pyrene and interior scalar, obtain typical curve Y=1.3902X-0.0437.
Gas chromatography test condition is as follows: chromatographic column: specification is the Elite-5Ms of 30m × 0.25mm × 0.25 μ m; Injector temperature: 280 DEG C; Sample size: 1 μ L; Carrier gas: helium, purity >=99.999%; Do not shunt; Flow velocity: 1.2mL/min; Heating schedule: 150 DEG C of initial temperatures, and keep 1min, then be warming up to 280 DEG C with the speed of 6 DEG C/min, and keep 20min;
Mass spectrophotometry condition is as follows: transmission line temperature: 280 DEG C; Ionization EI energy 70eV; Ion source temperature: 230 DEG C; Solvent delay time 19min, selects ion scan Mode S IM fractional scanning, carries out quantitative test with characteristic ion.
7, detection and the calculating of the content of benzo [α] pyrene in flue gas TPM
With step b same test condition under, sample solution is carried out to GC-MS(gas chromatography-mass spectrography) analysis, record benzo in sample solution [α] pyrene peak area and interior mark peak area, adopt following computing formula to obtain benzo in flue gas TPM [α] pyrene content, computing formula is as follows:
In formula:
Benzo [α] pyrene content in every cigarette of m=, unit is that ng/ props up;
A
xfor benzo [α] pyrene peak area;
A
isfor interior mark peak area;
B is linear equation intercept;
K is linear equation slope;
M
isfor interior scalar in benzo [α] pyrene methanol extract liquid, unit is ng;
N=cigarette quantity, unit is for propping up.
Embodiment 2:
Embodiment 2 difference from Example 1 are: the ionic liquid that adds 200 μ L in step 5.
Embodiment 3:
Embodiment 3 difference from Example 1 are: the ionic liquid that adds 300 μ L in step 5.
The testing result of benzo [α] pyrene content in the cigarette sample of table 1 embodiment 1-3
* after in table, precipitation refers to dispersion liquid extraction, can ionic liquid be precipitated out
Embodiment 4:
Embodiment 4 difference from Example 1 are: the ionic liquid that adds 400 μ L in step 5.
Embodiment 5:
Embodiment 5 difference from Example 1 are: the ionic liquid that adds 500 μ L in step 5.
Embodiment 6:
Embodiment 6 difference from Example 1 are: the ionic liquid that adds 600 μ L in step 6.
The testing result of benzo [α] pyrene content in the cigarette sample of table 2 embodiment 4-6
From table 1 and table 2, in the time adding ionic liquid volume to be 100 μ L, 200 μ L, 300 μ L, the emulsion that ionic liquid cannot form from dispersive liquid-liquid microextraction, separate out, so cannot carry out quantitatively, have remarkable precipitation to generate in the time that ionic liquid volume increases to 400 μ L, 500 μ L, 600 μ L.The content that records benzo [α] pyrene in the cigarette of trade mark A according to existing national standard method " mensuration of benzo [α] pyrene in GB/T21130-2007 cigarette smoke TPM " is 7.46ng/mL.In the present invention, when ionic liquid is that 400 μ L, water are that 40mL and ionic liquid are that 600 μ L, water record result while being 20mL and national standard method error is larger, all the other mean relative deviations are all less than 3%.
The mensuration of detection limit, quantitative limit, repeatability and the recovery of this assay method
(1) detection limit of the inventive method and quantitative limit:
The standard solution replicate determination of Cmin 10 times, calculates standard deviation, and the standard deviation of 3 times is detection limit, and the standard deviation of 10 times is quantitative limit, and detection limit and the quantitative limit of benzo [α] pyrene are respectively 0.4860ng/mL and 1.6200ng/mL.
(2) repeatability of the inventive method and recovery of standard addition:
In blank filter disc, add the standard solution of benzo [α] pyrene, then carry out pre-treatment and GC-MS and analyze, and calculate its recovery according to adding scalar sum measured value, the results are shown in Table 4.
When the cigarette of trade mark B good balance is 20mL according to the volume of water in case study on implementation 5, measure, parallel 5 times, relative standard deviation is in table 3.
As can be seen from Table 3, the recovery of benzo [α] pyrene is 93%～102%, and average relative standard deviation (RSD) is less than 3%, illustrates that the recovery of the inventive method is high, reproducible.
Quantitative curve, the range of linearity, detection limit, the quantitative limit of benzo [α] pyrene are as shown in table 4.
Quantitative curve, detection limit, quantitative limit, the recovery and the repeatability (n=5) of table 3 benzo [α] pyrene
Note: in linear equation, X represents the ratio of benzo [α] pyrene and interior target concentration, Y represents the ratio of benzo [α] pyrene and interior target peak area
Although with reference to explanatory embodiment of the present invention, invention has been described here, above-described embodiment is only preferably embodiment of the present invention, embodiments of the present invention are not restricted to the described embodiments, should be appreciated that, those skilled in the art can design a lot of other amendment and embodiments, within these amendments and embodiment will drop on the disclosed principle scope and spirit of the application.
Claims (7)
1. an assay method for benzo [α] pyrene content in flue gas TPM, is characterized in that the method comprises the following steps:
The preparation of A, benzo [α] pyrene methanol extract liquid
With cambridge filter trapping cigarette smoke granule phase substance, then cambridge filter is proceeded in extraction vessel, add the d of 1mL concentration 201.6ng/mL
12-BaP cyclohexane solution is as inner mark solution, then adds 40mL methyl alcohol to carry out ultrasonic extraction, obtains benzo [α] pyrene methanol extract liquid;
The preparation of B, sample solution
10mL benzo [α] pyrene methanol extract liquid is placed in to 50mL conical bottom plastic centrifuge tube, add 100 μ L～600 μ L imidazoles hexafluorophosphoric acid salt ionic liquid and 10～40mL water, in vortex instrument, carry out vortex 1～4min, then centrifugal 7～12min under rotating speed 7000rpm～9000rpm, remove supernatant, add again 1～2mL cyclohexane, carry out again vortex 1～2min, then centrifugal 7～12min under rotating speed 10000rpm～12000rpm, then filter with 0.45 μ m filter membrane, the filtrate of collection is sample solution;
C, gas chromatography-mass spectrography are measured
Gas Chromatography-Mass Spectrometry step is as follows:
The preparation of a, series standard solution
Taking cyclohexane give as solvent, preparation benzo [α] pyrene concentration 10ng/mL, 20ng/mL, 40ng/mL, 100ng/mL, 200ng/mL and 300ng/mL, and the series standard solution of interior mark concentration 201.6ng/mL;
The drafting of b, typical curve
The standard serial solution that step a obtains carries out gas chromatography-mass spectrography analysis, benzo in chromatogram [α] the pyrene peak area of comparing of benzo in standard serial solution [α] pyrene concentration and interior mark concentration is drawn with the ratio of interior mark peak area, obtain typical curve Y=kX+b by its figure, in formula, k represents the slope of this linear equation, b represents the intercept of this linear equation, X represents the ratio of benzo [α] pyrene and interior target concentration, and Y represents the ratio of benzo [α] pyrene and interior target peak area;
Detection and the calculating of benzo [α] pyrene content in c, flue gas TPM
Under the condition determination identical with step b, the sample solution that step B obtains carries out gas chromatography-mass spectrography analysis, record benzo in sample solution [α] pyrene peak area and interior mark peak area, adopt following computing formula to obtain benzo in flue gas TPM [α] pyrene content:
In formula:
Benzo [α] pyrene content in every cigarette of m=, unit is that ng/ props up;
A
xfor benzo [α] pyrene peak area;
A
isfor interior mark peak area;
B is linear equation intercept;
K is linear equation slope;
M
isfor interior scalar in benzo [α] pyrene methanol extract liquid, unit is ng;
N=cigarette quantity, unit is for propping up.
2. assay method according to claim 1, is characterized in that gas chromatography and the mass spectrographic test condition of described GC-MS(gas chromatography-mass spectrography) is as follows:
Gas Chromatographic Determination condition is as follows: chromatographic column: specification is the Elite-5Ms of 30m × 0.25mm × 0.25 μ m; Injector temperature: 280 DEG C; Sample size: 1 μ L; Carrier gas: helium, purity >=99.999%; Do not shunt; Flow velocity: 1.2mL/min; Heating schedule: 150 DEG C of initial temperatures also keep 1min, then be warming up to 280 DEG C and keep 20min with 6 DEG C/min of speed;
Mass spectrophotometry condition is as follows: transmission line temperature: 280 DEG C; Ionization EI energy 70eV; Ion source temperature: 230 DEG C; Solvent delay time 19min, selects ion scan Mode S IM fractional scanning, carries out quantitative test with characteristic ion.
3. assay method according to claim 1, is characterized in that described ionic liquid is 1-hexyl-3-methylimidazole hexafluorophosphate or 1-octyl group-3-methyl-imidazoles hexafluorophosphate.
4. assay method according to claim 1, is characterized in that carrying out ultrasonic processing 35-45min under the ultrasonic extraction described in steps A is the condition of ultrasonic power 400～500w.
5. assay method according to claim 1, is characterized in that the inner mark solution preparation steps of described concentration 201.6ng/mL is as follows:
1) preparation of mark storing solution I in: accurately take 25.2mg D
12-bap, in 100mL volumetric flask, is settled to scale and mixes with cyclohexane, and obtaining concentration is the interior mark storing solution I of 0.252mg/mL;
2) preparation of mark storing solution II in: accurately pipette in 2mL mark storing solution I in 50mL volumetric flask, be settled to scale and shake up with cyclohexane, obtaining concentration is the interior mark storing solution II of 10.08 μ g/mL;
3) preparation of inner mark solution: accurately pipette in 2mL mark storing solution II in 100mL volumetric flask, be settled to scale and shake up with cyclohexane, obtain the inner mark solution that concentration is 201.6ng/mL.
6. assay method according to claim 5, is characterized in that the preparation steps of described standard serial solution is as follows:
1) preparation of standard reserving solution I: accurately take 10mg benzo [α] pyrene in 100mL volumetric flask, dissolve and be settled to scale with cyclohexane, mix and obtain the standard reserving solution I that concentration is 100 μ g/mL;
2) preparation of standard reserving solution II: accurately pipette 1mL standard reserving solution I in 100mL volumetric flask, dissolve and be settled to scale with cyclohexane, mix and obtain the standard reserving solution II that concentration is 1 μ g/mL;
3) preparation of standard serial solution: pipette respectively 0.5mL, 1mL, 2mL, 5mL, 10mL and 15mL standard reserving solution II in 50mL volumetric flask, then add successively 1mL interior mark storing solution II claimed in claim 5, be settled to scale and shake up with cyclohexane, obtain 6 other standard serial solutions of concentration level, wherein benzo [α] pyrene concentration is followed successively by 10ng/mL, 20ng/mL, 40ng/mL, 100ng/mL, 200ng/mL, 300ng/mL, and interior mark concentration is 201.6ng/mL.
7. assay method according to claim 1, is characterized in that described collecting according to the standard of GB/T19609-2004 with cambridge filter trapping cigarette smoke granule phase substance.
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| CN108375641A (en) * | 2018-05-29 | 2018-08-07 | 云南中烟工业有限责任公司 | The detection method of benzo [a] pyrene in a kind of tobacco leaf flue gas |
| CN108375641B (en) * | 2018-05-29 | 2021-02-09 | 云南中烟工业有限责任公司 | Method for detecting benzo [ a ] pyrene in tobacco smoke |
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