CN104049056B - The assay method of benzo [α] pyrene content in smoke's total particulate matter - Google Patents
The assay method of benzo [α] pyrene content in smoke's total particulate matter Download PDFInfo
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Abstract
The invention discloses the assay method of benzo [α] pyrene content in a kind of smoke's total particulate matter, the method comprises the preparation of benzo [α] pyrene methanol extract liquid; The preparation of sample solution; Sample solution GC-MS(gas chromatography-mass spectrography) is analyzed and the calculating of benzo [α] pyrene content in smoke's total particulate matter.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 reduces to each sample of 1mL from each sample of the 50mL ~ 200mL of classic method, and avoids the concentration step in pretreatment process; Under the condition ensureing sensitivity, the recovery, simplify treatment step, greatly reduce the harm of organic solvent to environment and experimenter.
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 smoke's total particulate matter.
Background technology
Palycyclic aromatic is the aromatic organic compounds that a class has multiple phenyl ring, is to find to have one of environmental contaminants that " carcinogenic, teratogenesis, mutagenesis " act on the earliest, is also that the class in cigarette mainstream flue gas mainly contains harmful substances.Be that representational several palycyclic aromatic all belongs to completely carcinogenic compound with benzo [α] pyrene.Chemical Components in Cigarette Smoke is very complicated, and polycyclic aromatic hydrocarbon content is lower, generally in the flue gas often propping up 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 that tobacco quality controls, and direct basis can be provided for the harm of assessment smoking to human health.
Ionic liquid is the material of ionic state, and volatility is very low, nonflammable, Heat stability is good, this guarantees the pollution that it does not have volatile organic solvent in the past to cause to environment.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 widely.In extracting operation process, the standard of slective extraction agent was criterion substantially with effect of extracting in the past, consider less to environmental factor, which results in the organic solvent high volatility of use, toxicity is large, consumption is large, this just causes the various problems such as environmental and human health impacts harm.According to the thought of Green Chemistry, scientific worker must choice for use green solvent, and the shortcoming from extraction process is in the past eliminated in source, becomes whole process into environmental protection technique.
The existing standard method of benzo [α] pyrene in cigarette mainstream flue gas is the mensuration of benzo [α] pyrene " in the GB/T 21130-2007 cigarette smoke condensates ".In existing GB detection method, the mode that cyclohexane adopts silicagel column to purify after extracting benzo [α] pyrene, comprise the steps such as post activation, loading, drip washing, then 40mL eluent vacuum being revolved steaming mode is concentrated into about 1mL; Another kind of common method, purify with Full-automatic solid phase extraction instrument after cyclohexane extracts benzo [α] pyrene and concentrate, 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 condensates, adopt liquid-liquid extraction separation method to obtain sample solution fast.
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 smoke's total particulate matter, 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 as inner mark solution, then adds 40mL methyl alcohol and carries 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 50mL conical bottom plastic centrifuge tube, add 100 μ L ~ 600 μ L limidazolium hexafluorophosphate class ionic liquid and 10 ~ 40mL water, vortex 1 ~ 4min is carried out in vortex instrument, then centrifugal 7 ~ 12min under rotating speed 7000rpm ~ 9000rpm, remove supernatant, add 1 ~ 2mL cyclohexane again, carry out vortex 1 ~ 2min again, then centrifugal 7 ~ 12min under rotating speed 10000rpm ~ 12000rpm, then filter with 0.45 μm of filter membrane, the filtrate of collection is sample solution;
C, gas chromatography-mass spectrography measure
Gas Chromatography-Mass Spectrometry step is as follows:
The preparation of a, series standard solution
Take 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 [α] pyrene peak area in the comparison chromatogram of benzo in standard serial solution [α] pyrene concentration and interior mark concentration is drawn with the ratio of interior mark peak area, typical curve Y=kX+b is obtained 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;
The detection of benzo [α] pyrene content and calculating in c, smoke's total particulate matter
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 smoke's total particulate matter [α] pyrene content:
m＝((A
x/A
is-b)/k×m
is)/n
In formula:
M=often props up benzo [α] the pyrene content in cigarette, and 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 scalar interior in benzo [α] pyrene methanol extract liquid, unit is ng;
N=cigarette quantity, unit is for propping up.
According to one embodiment of present invention, gas chromatography and the mass spectrographic test condition of described GC-MS(gas chromatography-mass spectrography) are as follows:
Gas Chromatographic Determination condition is as follows: chromatographic column: specification is the Elite-5Ms of 30m × 0.25mm × 0.25 μm; 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: initial temperature 150 DEG C also keeps 1min, then is warming up to 280 DEG C with speed 6 DEG C/min and keeps 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, Selective ion mode scan pattern SIM 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, ultrasonic process 35-45min is carried out in described in step ultrasonic extraction under the condition of ultrasonic power 400 ~ 500w.
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 with cyclohexane and mixes, and obtains the interior mark storing solution I that concentration is 0.252mg/mL;
2) preparation of mark storing solution II in: accurately pipette mark storing solution I in 2mL and, in 50mL volumetric flask, be settled to scale with cyclohexane and shake up, obtaining the interior mark storing solution II that concentration is 10.08 μ g/mL;
3) preparation of inner mark solution: accurately pipette mark storing solution II in 2mL and, in 100mL volumetric flask, be settled to scale with cyclohexane and shake up, obtaining the inner mark solution that concentration is 201.6ng/mL.
According to one embodiment of present invention, 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 with cyclohexane and be settled to scale, mixing obtains 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 with cyclohexane and be settled to scale, mixing obtains the standard reserving solution II that concentration is 1 μ g/mL;
3) preparation of standard serial solution: pipette 0.5mL, 1mL, 2mL, 5mL, 10mL and 15mL standard reserving solution II respectively in 50mL volumetric flask, then the interior mark storing solution II described in 1mL is added successively, be settled to scale with cyclohexane and shake up, 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 with the standard collection of cambridge filter trapping cigarette smoke granule phase substance according to GB/T 19609-2004.
Obtain methanol extraction liquid with methanol extraction benzo [α] pyrene in this assay method, add ionic liquid afterwards, ionic liquid is dissolved in methyl alcohol.Because distribution ratio is different, 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.Can form emulsion add water in this solution after, centrifugal to this emulsion, ionic liquid will be precipitated out, and such benzo [α] pyrene has just been enriched in ionic liquid from methyl alcohol.The ionic liquid density be precipitated out is larger, directly cannot enter GC-MS to analyze, so mix with the volatile cyclohexane of appearance 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 reduces to each sample of 1mL from each sample of the 50mL ~ 200mL of classic method, and avoids the concentration step in pretreatment process.The present invention, under the condition ensureing sensitivity, the recovery, simplifies treatment step, greatly reduces the harm of organic solvent to environment and experimenter.
Accompanying drawing explanation
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 Clarus 600GC, PE Clarus SQ8T MS gas chromatograph-mass spectrometer, MettlerToledo electronic balance, IKA MS1Minishaker vortice, Sigma 3K15 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 with cyclohexane and mix, obtain the interior mark storing solution I that concentration is 0.252mg/mL;
2) preparation of mark storing solution II in: accurately pipette mark storing solution I in 2mL and, in 50mL volumetric flask, be settled to scale with cyclohexane and shake up, obtaining the interior mark storing solution II that concentration is 10.08 μ g/mL;
3) preparation of inner mark solution: accurately pipette mark storing solution II in 2mL and, in 100mL volumetric flask, be settled to scale with cyclohexane and shake up, obtaining 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 with cyclohexane and be settled to scale, mixing obtains 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 with cyclohexane and be settled to scale, mixing obtains the hybrid standard storing solution II that concentration is 1 μ g/mL;
3) preparation of standard serial solution: pipette 0.5mL, 1mL, 2mL, 5mL, 10mL, 15mL standard reserving solution II respectively in 50mL volumetric flask, then the interior mark storing solution II of 1mL is added successively, be settled to scale with cyclohexane and shake up, 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
After collecting 20 cigarette smoke granule phase substances with Cambridge filter paper according to the requirement of GB/T 19609, cambridge filter is proceeded to extraction vessel, adds the d of 1mL concentration 201.6ng/mL
12-BaP cyclohexane solution is as inner mark solution, then to add 40mL methyl alcohol be ultrasonic extraction 40min under the condition of 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 50mL conical bottom plastic centrifuge tube, add 100 μ L ionic liquids and 20 ~ 40mL water, vortex 2min is carried out in vortex instrument, then under rotating speed 8000rpm, supernatant is removed after centrifugal 10min, add 1mL cyclohexane again, then carry out vortex 1min, then centrifugal 10min under rotating speed 11000rpm, then filter with 0.45 μm of filter membrane, the filtrate of collection is sample solution.
6, the drafting of typical curve
Standard serial solution is carried out GC-MS(gas chromatography-mass spectrography) analysis, the ratio of benzo [α] pyrene peak area and interior mark peak area in the content of benzo in standard serial solution [α] pyrene and the comparison chromatogram of interior scalar is mapped, obtains 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 μm; 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: initial temperature 150 DEG C, and keep 1min, then with the ramp to 280 DEG C 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, Selective ion mode scan pattern SIM fractional scanning, carries out quantitative test with characteristic ion.
7, the detection of the content of benzo [α] pyrene and calculating in smoke's total particulate matter
With under step b same test condition, sample solution is carried out 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 smoke's total particulate matter [α] pyrene content, computing formula is as follows:
m＝((A
x/A
is-b)/k×m
is)/n
In formula:
M=often props up benzo [α] the pyrene content in cigarette, and 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 scalar interior 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 is: the ionic liquid adding 200 μ L in step 5.
Embodiment 3:
Embodiment 3 difference from Example 1 is: the ionic liquid adding 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 liquid-liquid extraction, can ionic liquid be precipitated out
Embodiment 4:
Embodiment 4 difference from Example 1 is: the ionic liquid adding 400 μ L in step 5.
Embodiment 5:
Embodiment 5 difference from Example 1 is: the ionic liquid adding 500 μ L in step 5.
Embodiment 6:
Embodiment 6 difference from Example 1 is: the ionic liquid adding 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, when adding ionic liquid volume and being 100 μ L, 200 μ L, 300 μ L, separate out the emulsion that ionic liquid cannot be formed from liquid-liquid extraction, so cannot carry out quantitative, have when ionic liquid volume increases to 400 μ L, 500 μ L, 600 μ L and significantly precipitate generation.The content recording benzo [α] pyrene in the cigarette of trade mark A according to the existing national standard method mensuration of benzo [α] pyrene " in the GB/T21130-2007 cigarette smoke condensates " is 7.46ng/mL.In the present invention, when ionic liquid be 400 μ L, water to be 40mL and ionic liquid be 600 μ L, water records result when being 20mL and national standard method error is comparatively large, all the other mean relative deviations are all less than 3%.
The mensuration of the detection limit of this assay method, quantitative limit, repeatability and the recovery
(1) detection limit of the inventive method and quantitative limit:
The standard solution replicate determination of Cmin 10 times, calculate standard deviation, 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 analysis, and calculate its recovery according to adding scalar sum measured value, the results are shown in Table 4.
Measured according to when in case study on implementation 5, the volume of water is 20mL by the cigarette of the trade mark B balanced, 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's deviation (RSD) is less than 3%, illustrates that the recovery of the inventive method is high, reproducible.
The quantitation curves of benzo [α] pyrene, the range of linearity, detection limit, quantitative limit are as shown in table 4.
The quantitation curves of table 3 benzo [α] pyrene, detection limit, quantitative limit, the recovery and repeatability (n=5)
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 the present invention's preferably embodiment, 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 embodiment, these amendments and embodiment will drop within spirit disclosed in the present application and spirit.
Claims (2)
1. the assay method of benzo [α] pyrene content in smoke's total particulate matter, 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 as inner mark solution, then adds 40mL methyl alcohol and carries 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 50mL conical bottom plastic centrifuge tube, add 100 μ L ~ 600 μ L limidazolium hexafluorophosphate class ionic liquid and 10 ~ 40mL water, vortex 1 ~ 4min is carried out in vortex instrument, with benzo [α] pyrene in ionic liquid enrichment methanol solution, then centrifugal 7 ~ 12min under rotating speed 7000rpm ~ 9000rpm, remove supernatant, add 1 ~ 2mL cyclohexane again, carry out vortex 1 ~ 2min again, then centrifugal 7 ~ 12min under rotating speed 10000rpm ~ 12000rpm, then filter with 0.45 μm of filter membrane, the filtrate of collecting is sample solution,
C, gas chromatography-mass spectrography measure
Gas Chromatography-Mass Spectrometry step is as follows:
The preparation of a, series standard solution
Take 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 [α] pyrene peak area in the comparison chromatogram of benzo in standard serial solution [α] pyrene concentration and interior mark concentration is drawn with the ratio of interior mark peak area, typical curve Y=kX+b is obtained 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;
The detection of benzo [α] pyrene content and calculating in c, smoke's total particulate matter
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 smoke's total particulate matter [α] pyrene content:
m＝((A
x/A
is-b)/k×m
is)/n
In formula:
M=often props up benzo [α] the pyrene content in cigarette, and 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 scalar interior in benzo [α] pyrene methanol extract liquid, unit is ng;
N=cigarette quantity, unit is for propping up;
Gas chromatography and the mass spectrographic test condition of described GC-MS(gas chromatography-mass spectrography) are as follows:
Gas Chromatographic Determination condition is as follows: chromatographic column: specification is the Elite-5Ms of 30m × 0.25mm × 0.25 μm; 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: initial temperature 150 DEG C also keeps 1min, then is warming up to 280 DEG C with speed 6 DEG C/min and keeps 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, Selective ion mode scan pattern SIM fractional scanning, carries out quantitative test with characteristic ion;
Described ionic liquid is 1-hexyl-3-methylimidazole hexafluorophosphate or 1-octyl group-3-methyl-imidazoles hexafluorophosphate;
In step, ultrasonic process 35-45min is carried out in described ultrasonic extraction under the condition of ultrasonic power 400 ~ 500w;
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 with cyclohexane and mixes, and obtains the interior mark storing solution I that concentration is 0.252mg/mL;
2) preparation of mark storing solution II in: accurately pipette mark storing solution I in 2mL and, in 50mL volumetric flask, be settled to scale with cyclohexane and shake up, obtaining the interior mark storing solution II that concentration is 10.08 μ g/mL;
3) preparation of inner mark solution: accurately pipette mark storing solution II in 2mL and, in 100mL volumetric flask, be settled to scale with cyclohexane and shake up, obtaining the inner mark solution that concentration is 201.6ng/mL;
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 with cyclohexane and be settled to scale, mixing obtains 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 with cyclohexane and be settled to scale, mixing obtains the standard reserving solution II that concentration is 1 μ g/mL;
3) preparation of standard serial solution: pipette 0.5mL, 1mL, 2mL, 5mL, 10mL and 15mL standard reserving solution II respectively in 50mL volumetric flask, then 1mL interior mark storing solution II according to claim 5 is added successively, be settled to scale with cyclohexane and shake up, 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.
2. assay method according to claim 1, is characterized in that the standard collection of described cambridge filter trapping cigarette smoke granule phase substance according to GB/T 19609-2004.
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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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