CN103257195A - GC-MS/MS (Gas chromatography-tandem mass spectrometry) method for simultaneously analyzing benzo [a] BaA, chrysene and benzo [a] BaP in main stream smoke of cigarettes - Google Patents
GC-MS/MS (Gas chromatography-tandem mass spectrometry) method for simultaneously analyzing benzo [a] BaA, chrysene and benzo [a] BaP in main stream smoke of cigarettes Download PDFInfo
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- CN103257195A CN103257195A CN2013102268157A CN201310226815A CN103257195A CN 103257195 A CN103257195 A CN 103257195A CN 2013102268157 A CN2013102268157 A CN 2013102268157A CN 201310226815 A CN201310226815 A CN 201310226815A CN 103257195 A CN103257195 A CN 103257195A
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Abstract
The invention discloses a GC-MS/MS (Gas chromatography-tandem mass spectrometry) method for simultaneously analyzing benzo [a] BaA, chrysene and benzo [a] BaP in main stream smoke of cigarettes. The method is characterized by comprising the following steps of: taking out a Cambridge filter disc catching granule phase objects of main stream smoke of cigarettes, adding ethyl acetate and an internal standard, carrying out vibrating extraction, carrying out dispersive solid-phase extraction (d-SPE) on extracting liquid, then, carrying out nitrogen-blowing concentration on supernatant, and measuring by using GC-MS/MS. The method provided by the invention overcomes the deficiency that the existing pretreatment is tedious. A sample pretreatment method and an instrument detection condition are optimized, aiming at the granule phase objects of main stream smoke of cigarettes; the matrix disperse solid phase extraction (d-SPE) is selected to be used as a purification measure in purifying treatment; compared with a national standard method solid phase extract phase, the operation is simple, and the price is low; and the method provided by the invention has the advantages of accurate operation, high sensitivity and good repeatability.
Description
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Technical field
The invention belongs to objectionable impurities detection technique field in the cigarette smoke, relate generally to the determination techniques of benzo [a] anthracene (BaA) in the cigarette mainstream flue gas, (Chrysene) in the wrong and benzo [a] pyrene three kinds of palycyclic aromatics such as (BaP).
Background technology
Palycyclic aromatics such as benzo [a] pyrene are that the class in the cigarette mainstream flue gas mainly contains harmful substances, carcinogenesis is strong, weight analysis in the past animal or human's body toxicologic study shows, the strongest TSNAs just and the PAHs of carcinogenesis in the tobacco, and they always are the focus that people study.
The existing standard determination method of the benzo in the cigarette mainstream flue gas [a] pyrene is " mensuration of benzo [a] pyrene in the GB/T 21130-2007 cigarette smoke TPM ".The method of analyzing BaP mainly is GC/MS, and high performance liquid chromatography also is used to the detection of BaP.
The palycyclic aromatic that the GC/MS method is surveyed in the cigarette mainstream flue gas is general with organic solvent lixiviate flue gas TPMs such as target normal hexane in containing or cyclohexanes, extract silica gel Solid-Phase Extraction column purification, eluent is after concentrating, carrying out GC/MS analyzes, to select ion monitoring (SIM) pattern quantitative, has recovery height, highly sensitive, good reproducibility, characteristics such as quantitatively accurate, but need loaded down with trivial details Solid-Phase Extraction purification process and concentration process in the sample pretreatment process, waste time and energy, and to finding in the GC/MS testing process of tar content less than palycyclic aromatic in the main flume of 1 mg/cig cigarette that the content of benzo [a] pyrene is lower than 1 ng/cig more, this moment, the GC/MS chromatographic peak of benzo [a] pyrene was on the low side, and specified rate brings certain difficulty.
Summary of the invention:
Purpose of the present invention is intended to overcome the prior art defective and benzo [a] anthracene in a kind of while analysis of cigarette main flume is provided, bends and the GC-MS/MS method of benzo [a] pyrene, and this method pre-treatment process is simple, detection sensitivity height, good reproducibility.
The objective of the invention is to be achieved through the following technical solutions:
Benzo [a] anthracene, GC-MS/MS method in the wrong and benzo [a] pyrene are after having the cambridge filter of cigarette mainstream flue gas granule phase substance to take out capture in the while analysis of cigarette main flume of the present invention, add ethyl acetate and internal standard compound, after vibration is extracted, get extract through disperseing Solid-Phase Extraction (d-SPE), get then the supernatant liquid nitrogen blow concentrate after, (GC-MS/MS) measures with gas chromatography-tandem mass spectrometry, and concrete steps are as follows:
The preparation of a, inner mark solution: preparation d
12-BaP concentration is the acetone soln of 4 μ g/mL;
B, preparation standard operation solution: take by weighing 0.010 g(respectively and be accurate to 0.1 mg) standard items, place same 10 mL volumetric flasks, with acetone solution and constant volume, also finally be mixed with the series standard working solution of all types of target thing with concentration gradient then with the ethyl acetate dilution;
C, specimen preparation: after pressing the granule phase substance of 5 cigarette of ISO 3308:2000 method collection, take off cambridge filter;
D, oscillation extraction: accurately add 10 mL ethyl acetate solvents and 100 μ L inner mark solutions, on shaker with 200 rpm oscillation extractions, 30 min;
E, matrix disperse Solid-Phase Extraction (d-SPE): get 5 mL extracts and join matrix and disperse (to include 900 mg MgSO in the Solid-Phase Extraction centrifuge tube
4, 250 mg PSA), on the whirlpool mixer oscillator with speed oscillation 2 min of 2000 rpm, on supercentrifuge with centrifugal 3 min of 6000 rpm.
F, get supernatant 3 mL nitrogen in 45 ℃ of waters bath with thermostatic control be concentrated into do after, redissolve with 1 mL ethyl acetate, behind the organic filter membrane of mistake 0.22 μ m, be collected in the auto injection chromatogram bottle;
G, GC-MS/MS measure: the standard operation solution among the b or the sample extracting solution among the f mensuration that is available on the machine;
The calculating of h, measurement result: carry out the quantitative test of object with internal standard method, namely select the quasi-molecular ions area to compare its respective concentration with object and corresponding interior target secondary and carry out regretional analysis, obtain typical curve; Sample after extracting is measured, record detect object and corresponding in the target secondary select the ion peak area ratio, the substitution typical curve is tried to achieve benzo [a] anthracene in the sample, is bent and the content of benzo [a] pyrene.
In the present invention, the manner of formulation of standard operation solution is as follows: take by weighing 0.010 g(respectively and be accurate to 0.1 mg) various standard items, place same 10 mL volumetric flasks, with acetone solution and constant volume, be mixed with the mixed standard solution I that each object concentration is 1 mg/mL; Accurately pipette 1 mL mixed standard solution I then, place 100 mL volumetric flasks, with the acetone constant volume, being mixed with concentration is the mixed standard solution II of 10 μ g/mL; Accurately pipette 1 mL mixed standard solution II then, place 10 mL volumetric flasks, use the ethyl acetate constant volume, being mixed with concentration is the mixed standard solution III of 1 μ g/mL; Accurately pipette the mixed standard solution III of 0.01 mL, 0.02 mL, 0.05 mL, 0.1 mL, 0.2 mL, 0.5 mL and 1 mL, place 10 mL volumetric flasks, accurately add 100 μ L inner mark solutions, use the ethyl acetate constant volume, namely get the series standard working solution.The series standard solution concentration of preparation is: 1 ng/mL, 2 ng/mL, 5 ng/mL, 10 ng/mL, 20 ng/mL, 50 ng/mL, 100 ng/mL.
When GC-MS/MS measured, the chromatographic condition of employing was: chromatographic column: DB-35MS elastic quartz capillary tube chromatographic column (30 m * 0.25 mm * 0.25 μ m); Injector temperature: 250 ℃; Temperature programme: 50 ℃ of initial temperatures keep rising to 150 ℃ with 25 ℃/min behind 1 min; Rise to 260 ℃ with 5 ℃/min then, keep 5 min; Rise to 280 ℃ with 10 ℃/min at last, keep 8 min; Split sampling is not shunted time 1 min; Carrier gas: helium (purity is 99.999%); Constant current mode, flow velocity are 1.0 mL/min; Sample size: 1 μ L.Total run time is 42 min
The mass spectrum condition that adopts is: EI ionization pattern, ionization energy 70 eV; Filament current: 50 μ A; Ion source temperature: 250 ℃; Transmission line temperature: 280 ℃; Q2 collides gas: argon gas (purity 99.999%), and collision pond pressure is 1.0 mTorr; Solvent delay 5 min; Scan mode: multiple-reaction monitoring (MRM).3 kinds of objects and interior target retention time and mass spectrum parameter see Table 1.
Table 1The retention time of object and internal standard compound and MRM parameter
Method of the present invention has overcome the loaded down with trivial details deficiency of prior art sample treatment pre-treatment, at the cigarette mainstream flue gas granule phase substance, has optimized sample-pretreating method and instrument testing conditions.Be embodied in: existing national standard method, the mode that adopts silicagel column to purify comprises the post activation, goes up steps such as sample, drip washing, then 40 mL eluents is concentrated into about 0.5 mL with revolving the steaming mode.Among the present invention, adopt matrix to disperse Solid-Phase Extraction (d-SPE) as purification style, only need get 5 mL extracts in the centrifuge tube that contains PSA, vibrate and centrifugally can finish purification, compare with national standard method, consuming timely reduce to 5 min by 30 min.And the nitrogen that the present invention adopts blows concentrated method, handles when can realize batch samples (once can handle 50 samples simultaneously), and revolves the steaming method and can only handle a sample contrast, has improved the pre-treatment flux of sample greatly.
The present invention compared with prior art the inventive method has following excellent results:
⑴ with 10 mL ethyl acetate organic solvents three kinds of objects are extracted simultaneously in the inventive method sample pretreatment process, extraction efficiency is better.Compare with national standard method, can reduce 4 times of organic solvent use amounts.
⑵ the inventive method selects matrix to disperse Solid-Phase Extraction (d-SPE) as the purification means when purified treatment, compares with the national standard method Solid-Phase Extraction, and its operation is simpler, and price is more cheap.
⑶ the inventive method adopted the benzo of the GC-MS/MS of high sensitivity and strong anti-interference ability [a] anthracene, bend and benzo [a] pyrene detects simultaneously, therefore has the advantage of accurate, the highly sensitive and good reproducibility of operation.
1. the quantitative limit of the inventive method:
To the object response signal in the standard solution, calculate quantitative limit (LOQ) with 10 times of signal to noise ratio (S/N ratio)s (S/N=10), benzo [a] anthracene, quantitative limit in the wrong and benzo [a] pyrene are respectively 0.12 ng/cig, 0.12 ng/cig and 0.09 ng/cig.
2. the repeatability of the inventive method and recovery of standard addition:
In blank filter disc, add benzo [a] anthracene, bend and the standard solution of benzo [a] pyrene, carry out pre-treatment and GC-MS/MS then and analyze, and calculate its recovery according to adding the scalar sum measured value, the results are shown in Table 2.As can be seen from Table 2, three's the recovery is between 94%～107%, and average relative standard deviation (RSD) illustrates the recovery height of the inventive method, good reproducibility all less than 3%.
Table 2Benzo [a] anthracene, bend and the recovery and the repeatability (n=6) of benzo [a] pyrene
Description of drawings
Fig. 1 is assay method process flow diagram of the present invention (this figure is as Figure of abstract).
Embodiment
The present invention is described further below in conjunction with example, but is not restriction the present invention.
Example 1:
1. instrument and reagent:
Object: benzo [a] anthracene, in the wrong and benzo [a] pyrene, interior mark: d
12-BaP is standard items; Acetone, ethyl acetate are chromatographically pure reagent.
U.S. Thermo Fisher TSQ Quantum GC gas chromatography-triple level Four bar tandem mass spectrometers; Switzerland Mettler AE 163 electronic balance (sensibility reciprocals: 0.0001g); U.S. Labnet VtexMixer VX200 oscillator; Germany Sigma high speed freezing centrifuge.
2. sample preparation:
After pressing the granule phase substance of 5 cigarette of ISO 3308:2000 method collection, take off cambridge filter;
Accurately add 10 mL ethyl acetate solvents and 100 μ L inner mark solutions, on shaker with 200 rpm oscillation extractions, 30 min;
Getting 5 mL extracts joins matrix and disperses (to include 900 mg MgSO in the Solid-Phase Extraction centrifuge tube
4, 250 mg PSA), on the whirlpool mixer oscillator with speed oscillation 2 min of 2000 rpm, on supercentrifuge with centrifugal 3 min of 6000 rpm.
Get supernatant 3 mL nitrogen in 45 ℃ of waters bath with thermostatic control be concentrated into do after, redissolve with 1 mL ethyl acetate, behind the organic filter membrane of mistake 0.22 μ m, be collected in the auto injection chromatogram bottle;
3. prepare standard operation solution: take by weighing 0.01 g(respectively and be accurate to 0.1 mg) standard items, place same 10 mL volumetric flasks, with acetone solution and constant volume, be mixed with benzo [a] anthracene, bend and the concentration of benzo [a] pyrene is the mixed standard solution I of 1 mg/mL; Accurately pipette 1 mL mixed standard solution I then, place 100 mL volumetric flasks, with the acetone constant volume, being mixed with object concentration is the mixed standard solution II of 10 μ g/mL; Accurately pipette 1 mL mixed standard solution II then, place 10 mL volumetric flasks, use the ethyl acetate constant volume, being mixed with concentration is the mixed standard solution III of 1 μ g/mL; Accurately pipette the mixed standard solution III of 0.01 mL, 0.02 mL, 0.05 mL, 0.1 mL, 0.2 mL, 0.5 mL and 1 mL, place 10 mL volumetric flasks, accurately add 100 μ L inner mark solutions, use the ethyl acetate constant volume, namely get the series standard working solution.The series standard solution concentration of preparation is: 1 ng/mL, 2 ng/mL, 5 ng/mL, 10 ng/mL, 20 ng/mL, 50 ng/mL, 100 ng/mL.
4. assay method: the standard solution of the variable concentrations for preparing is injected GC-MS/MS, carry out benzo [a] anthracene, bend and the quantitative test of benzo [a] pyrene with internal standard method, namely selecting the quasi-molecular ions area to compare its respective concentration with object and interior target secondary carries out regretional analysis, obtains typical curve; Sample after extracting is measured, recorded object and interior target secondary and select the ion peak area ratio, the substitution typical curve is tried to achieve benzo in the filter disc [a] anthracene, content in the wrong and benzo [a] pyrene sees Table 3.
Table 3Benzo among the cigarette A [a] anthracene, bend and the testing result of benzo [a] pyrene
| Sequence number | Title | The content of object (ng/cig) |
| 1 | Benzo [a] anthracene | 12.08 |
| 2 | Bend | 14.13 |
| 3 | Benzo [a] pyrene | 7.57 |
When GC-MS/MS measured, the chromatographic condition of employing was: chromatographic column: DB-35MS elastic quartz capillary tube chromatographic column (30 m * 0.25 mm * 0.25 μ m); Injector temperature: 250 ℃; Temperature programme: 50 ℃ of initial temperatures keep rising to 150 ℃ with 25 ℃/min behind 1 min; Rise to 260 ℃ with 5 ℃/min then, keep 5 min; Rise to 280 ℃ with 10 ℃/min at last, keep 8 min; Split sampling is not shunted time 1 min; Carrier gas: helium (purity is 99.999%); Constant current mode, flow velocity are 1.0 mL/min; Sample size: 1 μ L.Total run time is 42 min
The mass spectrum condition that adopts is: EI ionization pattern, ionization energy 70 eV; Filament current: 50 μ A; Ion source temperature: 250 ℃; Transmission line temperature: 280 ℃; Q2 collides gas: argon gas (purity 99.999%), and collision pond pressure is 1.0 mTorr; Solvent delay 5 min; Scan mode: multiple-reaction monitoring (MRM).Object and interior target retention time and mass spectrum parameter see Table 1.
Example 2:
As described in embodiment 1, select another brand cigarette sample B, record sample benzo [a] anthracene, bend and the content of benzo [a] pyrene sees Table 4.
Table 4Benzo among the cigarette B [a] anthracene, bend and the testing result of benzo [a] pyrene
| Sequence number | Title | The content of object (ng/cig) |
| 1 | Benzo [a] anthracene | 2.80 |
| 2 | Bend | 2.62 |
| 3 | Benzo [a] pyrene | 1.25 |
Example 3:
As described in embodiment 1, select another brand cigarette sample C, record benzo in the sample [a] anthracene, bend and the content of benzo [a] pyrene sees Table 5.
Table 5Benzo among the cigarette C [a] anthracene, bend and the testing result of benzo [a] pyrene
| Sequence number | Title | The content of object (ng/cig) |
| 1 | Benzo [a] anthracene | 14.46 |
| 2 | Bend | 15.65 |
| 3 | Benzo [a] pyrene | 8.57 |
Example 4:
As described in embodiment 1, select another brand cigarette sample D, record benzo in the sample [a] anthracene, bend and the content of benzo [a] pyrene sees Table 6.
Table 6Benzo among the cigarette D [a] anthracene, bend and the testing result of benzo [a] pyrene
| Sequence number | Title | The content of object (ng/cig) |
| 1 | Benzo [a] anthracene | 11.68 |
| 2 | Bend | 12.49 |
| 3 | Benzo [a] pyrene | 6.65 |
Claims (3)
- One kind simultaneously benzo [a] anthracene in the analysis of cigarette main flume, bend and the GC-MS/MS method of benzo [a] pyrene, it is characterized in that: be after having the cambridge filter of cigarette mainstream flue gas granule phase substance to take out capture, add ethyl acetate and internal standard compound, after vibration is extracted, get extract through disperseing Solid-Phase Extraction (d-SPE), get then the supernatant liquid nitrogen blow concentrate after, (GC-MS/MS) measures with gas chromatography-tandem mass spectrometry, concrete steps are as follows:The preparation of a, inner mark solution: preparation d 12-BaP concentration is the acetone soln of 4 μ g/mL;B, prepare standard operation solution: take by weighing respectively 0.010 g benzo [a] anthracene, bend and the standard items of benzo [a] pyrene, place same 10 mL volumetric flasks, with acetone solution and constant volume, also finally be mixed with the series standard working solution with concentration gradient with the ethyl acetate dilution then;C, specimen preparation: after pressing the granule phase substance of 5 cigarette of ISO 3308:2000 method collection, take off cambridge filter;D, oscillation extraction: accurately add 10 mL ethyl acetate solvents and 100 μ L inner mark solutions, on shaker with 200 rpm oscillation extractions, 30 min;E, matrix disperse Solid-Phase Extraction (d-SPE): get 5 mL extracts and join matrix and disperse (to include 900 mg MgSO in the Solid-Phase Extraction centrifuge tube 4, 250 mg PSA), on the whirlpool mixer oscillator with speed oscillation 2 min of 2000 rpm, on supercentrifuge with centrifugal 3 min of 6000 rpm;F, get supernatant 3 mL nitrogen in 45 ℃ of waters bath with thermostatic control be concentrated into do after, redissolve with 1 mL ethyl acetate, behind the organic filter membrane of mistake 0.22 μ m, be collected in the auto injection chromatogram bottle;G, GC-MS/MS measure: the standard operation solution in the b step or the sample extracting solution among the f mensuration that is available on the machine;The calculating of h, measurement result: carry out the quantitative test of object with internal standard method, namely select the quasi-molecular ions area to compare its respective concentration with object and corresponding interior target secondary and carry out regretional analysis, obtain typical curve; Sample after extracting is measured, record detect object and corresponding in the target secondary select the ion peak area ratio, the substitution typical curve is tried to achieve benzo [a] anthracene in the sample, is bent and the content of benzo [a] pyrene.
- 2. method according to claim 1, it is characterized in that: the series standard working solution concentration of preparation is: 1 ng/mL, 2 ng/mL, 5 ng/mL, 10 ng/mL, 20 ng/mL, 50 ng/mL, 100 ng/mL.
- 3. method according to claim 1, it is characterized in that: when GC-MS/MS measured, the chromatographic condition of employing was: chromatographic column: DB-35MS elastic quartz capillary tube chromatographic column (30 m * 0.25 mm * 0.25 μ m); Injector temperature: 250 ℃; Temperature programme: 50 ℃ of initial temperatures keep rising to 150 ℃ with 25 ℃/min behind 1 min; Rise to 260 ℃ with 5 ℃/min then, keep 5 min; Rise to 280 ℃ with 10 ℃/min at last, keep 8 min; Split sampling is not shunted time 1 min; Carrier gas: helium; Constant current mode, flow velocity are 1.0 mL/min; Sample size: 1 μ L; Total run time is 42 min;The mass spectrum condition that adopts is: EI ionization pattern, ionization energy 70 eV; Filament current: 50 μ A; Ion source temperature: 250 ℃; Transmission line temperature: 280 ℃; Q2 collides gas: argon gas, and collision pond pressure is 1.0 mTorr; Solvent delay 5 min; Scan mode: multiple-reaction monitoring (MRM).
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| CN106093253A (en) * | 2016-05-27 | 2016-11-09 | 国家烟草质量监督检验中心 | The assay method of benzo [a] pyrene in the sample-pretreating method measuring benzo in cigarette smoke [a] pyrene and cigarette smoke |
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| CN110045044A (en) * | 2019-05-24 | 2019-07-23 | 江苏中烟工业有限责任公司 | A method of based on benzo [a] pyrene content in matrix matching solvent calibration measurement cigarette mainstream flue gas |
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