CN105675757A - Method for determining tobacco-specific N-nitrosamine and polycyclic aromatic hydrocarbons in mainstream smoke of cigarettes simultaneously - Google Patents
Method for determining tobacco-specific N-nitrosamine and polycyclic aromatic hydrocarbons in mainstream smoke of cigarettes simultaneously Download PDFInfo
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Abstract
The invention belongs to the technical field of chemical tests on cigarette smoke and particularly discloses a method for determining tobacco-specific N-nitrosamine and polycyclic aromatic hydrocarbons in mainstream smoke of cigarettes simultaneously. According to the method, a smoking machine smokes cigarettes, a Cambridge filter traps the mainstream smoke of the cigarettes, the filter is filtered by solutions containing interior labels, and an extraction solution is directly detected by an on-line gel chromatography-gas chromatography-tandem mass spectrometer after being filtered. Compared with a standard method, the method has the advantages that two compounds are determined together and the test efficiency is improved; all that is need for detection is to filter the smoke extraction solution, so that the method is convenient to operate, quick and efficient; the on-line gel chromatography-gas chromatography-tandem mass spectrometer is used for detection, and thus the automation degree is high and organic solvent consumption is low.
Description
Technical field
The invention belongs to cigarette smoke chemical analysis technical field, be specifically related to a kind of measure the method for the peculiar N-nitrosamine of Nicotiana tabacum L. and polycyclic aromatic hydrocarbon in cigarette mainstream flue gas simultaneously, detected by online gel chromatography-gas chromatography tandem mass spectrometry combined instrument.
Background technology
Polycyclic aromatic hydrocarbon is Nicotiana tabacum L. products of incomplete combustion when high temperature, in cigarette mainstream flue gas, about 30 condensed-nuclei aromatics having carcinogenecity are identified at present, Hoffmann in 1967 etc. demonstrate the carcinogenecity of polycyclic aromatic hydrocarbon by toxicological experiment, and the medical report delivered subsequently determines that benzo [a] pyrene is most important a kind of carcinogen in polycyclic aromatic hydrocarbon. The peculiar N-nitrosamine of Nicotiana tabacum L. is primarily referred to as N-nitrosonornicotine (NNN), N-nitrosoanatabine (NAT), N-nitroso-group anabasine (NAB) and 4-(nitrosomethylamino)-1-β-pyridine radicals-1-butanone (NNK), it it is ubiquitous carcinogen in cigarette smoke, as far back as 1962, just have in the world in article report Nicotiana tabacum L. containing N-nitrosamine and potential carcinogenecity thereof. Therefore in detection cigarette mainstream flue gas, the burst size of Nicotiana tabacum L. peculiar N-nitrosamine and polycyclic aromatic hydrocarbon is significant with healthy research to smoking.
Smoke components produced by cigarette burning process is sufficiently complex, has been detected as smoke components at present and alreadys more than more than 5000 kinds, and the peculiar N-nitrosamine of Nicotiana tabacum L. therein and polycyclic aromatic hydrocarbon content generally prop up rank at ng/. Therefore, the peculiar N-nitrosamine of the Nicotiana tabacum L. in main flume and polycyclic aromatic hydrocarbon are typically required certain sample pretreatment process when detecting. But, lengthy and tedious time-consuming sample pretreatment process does not occupy most times of whole detection process, is the main source of testing result error yet. The more important thing is, sample pretreatment process and follow-up Instrumental Analysis process are usually offline coupling, and testing efficiency is not high.
Early stage, we successively develop in the main flume based on online gel chromatography-gas chromatography tandem mass spectrometry the assay method of the peculiar N-nitrosamine (201510564296.4) of Nicotiana tabacum L. in benzopyrene (CN104569253A) and electronic cigarette liquid.But there is very big-difference in the instrumental conditions under two kinds of methods and parameter (mobile phase, gel chromatography acquisition time and mass spectrometry parameters etc.) etc. Therefore, it is necessary to exploitation one measures the peculiar N-nitrosamine of Nicotiana tabacum L. in cigarette mainstream flue gas and polycyclic aromatic hydrocarbon method simultaneously.
Summary of the invention
The purpose of the present invention improves for prior art situation just, and the method for the peculiar N-nitrosamine of Nicotiana tabacum L. and polycyclic aromatic hydrocarbon in the custom-designed cigarette mainstream flue gas of mensuration simultaneously. Compared with the conventional method, the present invention does not need sample pretreatment process, have automaticity high, simple to operate, rapidly and efficiently, organic solvent consumption is few and the test high advantage of flux.
It is an object of the invention to be achieved through the following technical solutions:
A kind of method of the peculiar N-nitrosamine of Nicotiana tabacum L. and polycyclic aromatic hydrocarbon in cigarette mainstream flue gas of mensuration simultaneously, specifically includes following steps:
1) preparation of standard serial solution: with volume ratio be 1:1 ethyl acetate and acetone for solvent, the grow tobacco standard substance of peculiar N-nitrosamine (NAB, NAT, NNN and NNK) of three kinds of polycyclic aromatic hydrocarbons (BaP, BaA and Chry) and four are solute, BaP-d12, NAB-d4, NAT-d4, NNN-d4 and NNK-d4 are interior mark, the standard serial solution of the containing the internal standard of preparation variable concentrations;
2) preparation of sample solution: Medicated cigarette is according to GB/T19609-2004, after the condition linear type smoking machine of ISO4387 2000 regulation aspirates 5 every time, the filter disc of mainstream smoke total particulate matter is had to be placed in container trapping, add extracting solution and mixing inner mark solution extracts, interior mark concentration mark concentration interior with in standard serial solution is identical, more namely obtains sample solution with 0.22 μm of organic membrane filtration. Wherein extracting solution can be ethyl acetate, dichloromethane, hexamethylene, cyclohexane/ethyl acetate (v/v=5/5), it is preferred to ethyl acetate; Extraction pattern is ultrasonic or vibration, and extraction time is 10-60min, it is preferred to 20min; The volume of extracting solution is 10-50mL, it is preferred to 20mL;
3) standard serial solution and sample solution carry out online gel chromatography-gas chromatography tandem mass spectrometry analysis under the same conditions, and whole analysis system is made up of chromatograph of gel permeation and gas chromatogram-tandem mass spectrometer two parts. Wherein, the condition of chromatograph of gel permeation is: chromatographic column is ShodexCLNpakEV-200,16 μm, 2mm*150mm or Silica5SIL4D, 5 μm, 4.6*150mm or Silica5SIL4E, 5 μm, 4.6*250mm, it is preferably ShodexCLNpakEV-200,16 μm, 2mm*150mm; Mobile phase is cyclohexane/ethyl acetate (percentage by volume of ethyl acetate is 10-50%) or cyclohexane/acetone (percentage by volume of acetone is 10-50%), it is preferred to cyclohexane/ethyl acetate, v/v=5/5; Flow velocity is 0.1mL/min; Column temperature is 40 ° of C; Sample size is 10mL; Collecting gel chromatography retention time is the component of 3.0-7.0min, and its all on-line imports the analysis of gas chromatography tandem mass spectrometry instrument; The condition of gas chromatography tandem mass spectrometry instrument is: inertia pre-column is the void column of 5m*0.53mm; Pre-column is DB-35ms, 5m*0.25mm*0.25mm; Detached dowel is DB-35ms, 25m*0.25mm*0.25mm; Chromatographic column heating schedule is: 82 ° of C of initial temperature, keeps 5min, then rises to 300 ° of C with 8 ° of C/min and keep 7.75min, and the operation time is 40min; Adopting Splitless injecting samples mode, sample injection time is 7.0min;With high-purity He for carrier gas, nebulizer gas pressure program is: by 120kPa, rises to 220kPa with 100kPa/min and keeps 6.0min, then recovers to reset pressure with 49.8kPa/min, and keeps 31min; Programmed temperature sampling mouth, injection port heating schedule is: 120 ° of C keep 5min, then rise to 280 ° of C with 100 ° of C/min and keep 33.4min; Purge flow rate program is: initial flow is 5.0mL/min, is down to 0 with the speed of 10mL/min and keeps 7.0min, then rising to initial flow at the same rate, and keeping 32.0min; Interface temperature and ion source temperature be 300 and 200 ° of C respectively; Mass spectrum ionization source is EI source; Ionization voltage is 70ev; The solvent delay time is 18min, and target analytes and interior target multiple-reaction monitoring parameter are as shown in table 1;
4) Nicotiana tabacum L. peculiar N-nitrosamine and polycyclic aromatic hydrocarbon is quantitative: grown tobacco the peak area of peculiar N-nitrosamine by benzo [a] pyrene and four and the ratio of interior mark peak area carries out quantitative, method particularly includes: in standard serial solution, the peak area of Nicotiana tabacum L. peculiar N-nitrosamine and polycyclic aromatic hydrocarbon and the ratio of interior mark peak area are vertical coordinate, the concentration of standard serial solution is abscissa, drawing curve; The ratio of Nicotiana tabacum L. peculiar N-nitrosamine and polycyclic aromatic hydrocarbon peak area and interior mark peak area in solution per sample, according to working curve, obtains the content of the peculiar N-nitrosamine of Nicotiana tabacum L. in sample and polycyclic aromatic hydrocarbon.
In the present invention, NNN in standard serial solution, NAT, the Concentraton gradient of NAB and BaP is 0.5, 1.0, 2.0, 5.0, 10.0, 20 and 50.0ng/mL, the Concentraton gradient of NNK is 0.545, 1.09, 2.18, 5.45, 10.9, 21.8 and 54.5ng/mL, the Concentraton gradient of BaA is 1.095, 2.19, 4.38, 10.95, 21.9, 43.8 and 109.5ng/mL, the Concentraton gradient of Chry is 1.33, 2.66, 5.32, 13.3, 26.6, 53.2 and 133ng/mL, and NAT-d4 in standard serial solution, in NAB-d4 and NNK-d4, mark concentration is 10ng/mL, the interior mark concentration of NNN-d4 and BaP-d12 respectively 12 and 10.6ng/mL.
The detection limit of the inventive method and be quantitatively limited to Nicotiana tabacum L. peculiar N-nitrosamine and the concentration corresponding when being 3 and 10 of polycyclic aromatic hydrocarbon signal to noise ratio (S/N).
In the present invention, our instrument parameter on affecting testing result and condition, sample solution preparation process have been investigated and have optimized. Being analyzed in order to peculiar for Nicotiana tabacum L. N-nitrosamine and polycyclic aromatic hydrocarbon are transferred to gas chromatography tandem mass spectrometry instrument from all on-line gel permeation chromatography simultaneously, we successively optimize gel permeation chromatographic column, mobile phase and corresponding acquisition time. Result shows ShodexCLNpakEV-200(16 μm, 2mm*150mm) it is that cyclohexane/ethyl acetate (v/v=5/5) has good separating effect at mobile phase, corresponding acquisition time is 3.0-7.0min. Sample solution volume owing to proceeding to gas chromatography tandem mass spectrometry instrument is increased to 400mL by 200mL, therefore sample introduction pressure, injector temperature and purge flow rate are also optimized by we, the nebulizer gas pressure program finally chosen is: by 120kPa, rise to 220kPa with 100kPa/min and keep 6.0min, recover to reset pressure with 49.8kPa/min again, and keep 31min; Injection port heating schedule is: 120 ° of C keep 5min, then rise to 280 ° of C with 100 ° of C/min and keep 33.4min; Purge flow rate program is: initial flow is 5.0mL/min, is down to 0 with the speed of 10mL/min and keeps 7.0min, then rising to initial flow at the same rate, and keeping 32.0min.In order to peculiar for Nicotiana tabacum L. N-nitrosamine and polycyclic aromatic hydrocarbon be extracted from granule phase substance simultaneously, we have investigated the factor (extracting solution type and volume, extraction time and extraction pattern etc.) affecting extraction effect. It is shown that with 20mL ethyl acetate for extracting solution, mechanical shaking extraction 20min is better to the extraction effect of Nicotiana tabacum L. peculiar N-nitrosamine and polycyclic aromatic hydrocarbon. Meanwhile, in order to obtain higher sensitivity, target analytes and interior target multiple-reaction monitoring parameter are optimized by we, including quota ion to collision energy etc., the final target analytes selected and interior target multiple-reaction monitoring parameter are as shown in table 1.
The present invention adopts gel chromatography that cigarette mainstream flue gas extract is processed, peculiar for Nicotiana tabacum L. N-nitrosamine is separated with macromole chaff interference by the size exclusion effect utilizing fixing phase with polycyclic aromatic hydrocarbon, again the component containing the peculiar N-nitrosamine of Nicotiana tabacum L. and polycyclic aromatic hydrocarbon is imported gas chromatography tandem mass spectrometry instrument online and be easily separated analysis, finally adopt the content of the peculiar N-nitrosamine of Nicotiana tabacum L. and polycyclic aromatic hydrocarbon in internal mark method determination cigarette mainstream flue gas. The method of the present invention overcome pre-treatment in existing determination techniques lengthy and tedious time-consuming, the deficiencies such as automatic continuous analysis, organic reagent consumption be many cannot be realized, for the character of the feature of cigarette mainstream flue gas extract and target analytes, improve method of testing. The inventive method analyzes organic reagent volume that a sample extracting solution consumes less than 10mL in Instrument measuring process, and the time used is about 50min, and is capable of automatic continuous analysis. Therefore, the inventive method have simple to operate, automaticity is high, rapidly and efficiently, organic reagent consumption is few and the test high advantage of flux, can greatly improve testing efficiency, reduce testing cost.
Accompanying drawing explanation
Fig. 1 is the chromatogram of the peculiar N-nitrosamine of Nicotiana tabacum L. of the present invention and polycyclic aromatic hydrocarbon.
Detailed description of the invention
The present invention is described further in conjunction with example, but is not limiting as the present invention.
Embodiment 1:
The assay method of the peculiar N-nitrosamine of Nicotiana tabacum L. and polycyclic aromatic hydrocarbon in a kind of cigarette mainstream flue gas, concretely comprising the following steps of operation:
The first step, the preparation of standard serial solution: with volume ratio be 1:1 ethyl acetate and acetone for solvent, four standard substance growing tobacco peculiar N-nitrosamine (NAB, NAT, NNN and NNK) and three kinds of polycyclic aromatic hydrocarbons (BaP, BaA and Chry) are solute, NAB-d4, NAT-d4, NNN-d4, NNK-d4 and BaP-d12 are interior mark, the standard serial solution of the containing the internal standard of preparation variable concentrations;
Second step, the preparation of sample solution: by the Medicated cigarette after balance and screening with linear type smoking machine according to GB/T19609-2004, the ISO4387 2000 standard conditions suction specified, 5 Medicated cigarette of experiment suction every time. There is the filter disc of mainstream smoke total particulate matter to be placed in 50mL container trapping, add 20mL ethyl acetate and 200 μ L mixing inner mark solutions, carry out mechanical shaking extraction 20min, more namely extracting solution is obtained sample solution with 0.22 μm of organic membrane filtration;
3rd step, standard serial solution and sample solution carry out online gel chromatography-gas chromatography tandem mass spectrometry analysis under the same conditions: whole analysis system is made up of chromatograph of gel permeation and gas chromatogram-tandem mass spectrometer two parts; Wherein, the condition of chromatograph of gel permeation is: chromatographic column is ShodexCLNpakEV-200 (16 μm, 2mm*150mm); Mobile phase is cyclohexane/ethyl acetate (5/5, v/v);Flow velocity is 0.1mL/min; Column temperature is 40 ° of C; Sample size is 10mL; Collect the component (amounting to 0.4mL) that gel chromatography retention time is 3.0-7.0min, and its all on-line is imported the analysis of gas chromatography tandem mass spectrometry instrument; The condition of gas chromatography tandem mass spectrometry instrument is: inertia pre-column is the void column of 5m*0.53mm; Pre-column is DB-35ms, 5m*0.25mm*0.25mm; Detached dowel is DB-35ms, 25m*0.25mm*0.25mm; Chromatographic column heating schedule is: 82 ° of C of initial temperature, keeps 5min, then rises to 300 ° of C with 8 ° of C/min and keep 7.75min, and the operation time is 40min; Adopting Splitless injecting samples mode, sample injection time is 7.0min; With high-purity He for carrier gas, nebulizer gas pressure program is: by 120kPa, rises to 220kPa with 100kPa/min and keeps 6.0min, then recovers to reset pressure with 49.8kPa/min, and keeps 31min; Programmed temperature sampling mouth, injection port heating schedule is: 120 ° of C keep 5min, then rise to 280 ° of C with 100 ° of C/min and keep 33.4min; Purge flow rate program is: initial flow is 5.0mL/min, is down to 0 with the speed of 10mL/min and keeps 7.0min, then rising to initial flow at the same rate, and keeping 32.0min; Interface temperature and ion source temperature be 300 and 200 ° of C respectively; Mass spectrum ionization source is EI source; Ionization voltage is 70ev; The solvent delay time is 18min, and target analytes and interior target multiple-reaction monitoring parameter are as shown in table 1. Under this condition, the chromatogram of the object obtained is as shown in Figure 1.
4th step, Nicotiana tabacum L. peculiar N-nitrosamine and polycyclic aromatic hydrocarbon quantitative: the peak area of Nicotiana tabacum L. peculiar N-nitrosamine and polycyclic aromatic hydrocarbon and the ratio of interior mark peak area are vertical coordinate in standard serial solution, the concentration of standard serial solution is abscissa, drawing curve, in Table 2, the wherein detection limit of the inventive method and be quantitatively limited to Nicotiana tabacum L. peculiar N-nitrosamine and the concentration corresponding when being 3 and 10 of polycyclic aromatic hydrocarbon signal to noise ratio (S/N); The ratio of Nicotiana tabacum L. peculiar N-nitrosamine and polycyclic aromatic hydrocarbon peak area and interior mark peak area in solution per sample, according to working curve, obtains the content of the peculiar N-nitrosamine of Nicotiana tabacum L. in sample and polycyclic aromatic hydrocarbon.
Target analytes and interior target multiple-reaction monitoring parameter in table 1. the inventive method
The range of linearity of table 2. the inventive method, working curve, quantitative limit and detection limit
In order to investigate the repeatability of the method, prepare the sample of basic, normal, high three kinds of concentration, be measured with 4 samples of preparation in a day, calculate the in a few days relative standard deviation under variable concentrations; It is measured with the sample prepared for three days on end, calculates the relative standard deviation in the daytime under variable concentrations. Result is as shown in table 3, target analytes under variable concentrations (2,10 and 40 times of value respectively each object range of linearity minimum that basic, normal, high concentration is corresponding) in a few days and day to day precision be respectively smaller than 11.4% and 13.3%, illustrate that the method has good repeatability.
The precision of table 3. the inventive method
The main flume extracting solution of dissimilar Medicated cigarette (mixed type A and fire-cured tobacco type B) adds target analytes standard solution, 2,10 and 40 times of basic, normal, high concentration respectively each object range of linearity minimum, it is analyzed by the inventive method afterwards, the standard working curve that the ratio of the peak area of gained substitutes into target analytes calculates measured concentration, and obtains relative recovery compared with actual addition.As shown in table 4, under variable concentrations the relative recovery of target analytes between 77.1-108.6%, it was shown that the accuracy of method is good, it is possible to meet the requirement that the peculiar N-nitrosamine of Nicotiana tabacum L. in daily cigarette mainstream flue gas and polycyclic aromatic hydrocarbon are analyzed.
The response rate of the peculiar N-nitrosamine of Nicotiana tabacum L. and polycyclic aromatic hydrocarbon in the dissimilar Medicated cigarette of table 4.
Adopt said method and standard method that the peculiar N-nitrosamine of main flume Nicotiana tabacum L. in different trade mark Medicated cigarette and polycyclic aromatic hydrocarbon burst size have been measured. Result is as shown in table 5: the inventive method and standard method testing result are absent from significant difference.
The testing result (ng/ props up, for standard method measurement result in bracket) of the peculiar N-nitrosamine of Nicotiana tabacum L. and polycyclic aromatic hydrocarbon in the different trade mark Medicated cigarette of table 5.
| Numbering | NNN | NAT | NAB | NNK | BaA | Chry | BaP |
| 1 | 56.2 (62.7) | 63.6 (70.2) | 11.0 (12.6) | 46.2 (57.6) | 30.4 (26.1) | 30.3 (28.6) | 8.8 (8.4) |
| 2 | 5.0 (5.1) | 12.0 (15.0) | 1.8 (1.9) | 4.5 (4.1) | 28.2 (27.1) | 30.8 (28.9) | 8.0 (8.1) |
| 3 | 3.9 (3.6) | 10.9 (9.3) | 1.2 (1.1) | 2.8 (2.9) | 29.4 (31.1) | 32.7 (34.2) | 8.1 (8.9) |
| 4 | 44.6 (51.3) | 47.0 (51.8) | 9.5 (11.1) | 9.7 (12.5) | 21.2 (23.5) | 21.2 (25.4) | 6.5 (7.1) |
| 5 | 5.4 (4.7) | 14.1 (13.5) | 1.9 (1.8) | 5.3 (5.1) | 29.3 (26.8) | 29.0 (28.9) | 8.4 (7.5) |
| 6 | 5.6 (5.5) | 12.7 (15.1) | 2.1 (2.1) | 6.6 (6.0) | 25.1 (24.1) | 24.4 (27.0) | 7.5 (7.3) |
Claims (9)
1. one kind measures the method for the peculiar N-nitrosamine of Nicotiana tabacum L. and polycyclic aromatic hydrocarbon in cigarette mainstream flue gas simultaneously, it is characterised in that: include step in detail below:
1) preparation of standard serial solution: with volume ratio be 1:1 ethyl acetate and acetone for solvent, grow tobacco peculiar N-nitrosamine with three kinds of polycyclic aromatic hydrocarbon: BaP, BaA, Chry and four: the standard substance of NAB, NAT, NNN, NNK are for solute, BaP-d12, NAB-d4, NAT-d4, NNN-d4 and NNK-d4 are interior mark, the standard serial solution of the containing the internal standard of preparation variable concentrations;
2) preparation of sample solution: Medicated cigarette is according to GB/T19609-2004, after the condition linear type smoking machine of ISO4387 2000 regulation aspirates 5 every time, the filter disc of mainstream smoke total particulate matter is had to be placed in container trapping, add extracting solution and mixing inner mark solution extracts, interior mark concentration mark concentration interior with in standard serial solution is identical, more namely obtains sample solution with 0.22 μm of organic membrane filtration;
3) standard serial solution and sample solution carry out online gel chromatography-gas chromatography tandem mass spectrometry analysis under the same conditions, and whole analysis system is made up of chromatograph of gel permeation and gas chromatogram-tandem mass spectrometer two parts; Wherein, the condition of chromatograph of gel permeation is: chromatographic column is ShodexCLNpakEV-200,16 μm, 2mm*150mm or Silica5SIL4D, 5 μm, 4.6*150mm or Silica5SIL4E, 5 μm, 4.6*250mm; Mobile phase is cyclohexane/ethyl acetate, and the percentage by volume of ethyl acetate is 10-50%, or is cyclohexane/acetone, and the percentage by volume of acetone is 10-50%, and flow velocity is 0.1mL/min; Column temperature is 40 ° of C; Sample size is 10mL; Collecting gel chromatography retention time is the component of 3.0-7.0min, and this component all on-line imports the analysis of gas chromatography tandem mass spectrometry instrument; The condition of gas chromatography tandem mass spectrometry instrument is: inertia pre-column is the void column of 5m*0.53mm; Pre-column is DB-35ms, 5m*0.25mm*0.25mm; Detached dowel is DB-35ms, 25m*0.25mm*0.25mm; Chromatographic column heating schedule is: 82 ° of C of initial temperature, keeps 5min, then rises to 300 ° of C with 8 ° of C/min and keep 7.75min, and the operation time is 40min; Adopting Splitless injecting samples mode, sample injection time is 7.0min; With high-purity He for carrier gas, nebulizer gas pressure program is: by 120kPa, rises to 220kPa with 100kPa/min and keeps 6.0min, then recovers to reset pressure with 49.8kPa/min, and keeps 31min; Programmed temperature sampling mouth, injection port heating schedule is: 120 ° of C keep 5min, then rise to 280 ° of C with 100 ° of C/min and keep 33.4min;Purge flow rate program is: initial flow is 5.0mL/min, is down to 0 with the speed of 10mL/min and keeps 7.0min, then rising to initial flow at the same rate, and keeping 32.0min; Interface temperature and ion source temperature be 300 and 200 ° of C respectively; Mass spectrum ionization source is EI source; Ionization voltage is 70ev; The solvent delay time is 18min, and target analytes and interior target multiple-reaction monitoring parameter are as shown in the table;
4) Nicotiana tabacum L. peculiar N-nitrosamine and polycyclic aromatic hydrocarbon is quantitative: undertaken quantitative by the ratio of the peak area of Nicotiana tabacum L. peculiar N-nitrosamine and polycyclic aromatic hydrocarbon and interior mark peak area.
2. the method for the peculiar N-nitrosamine of Nicotiana tabacum L. and polycyclic aromatic hydrocarbon in the cigarette mainstream flue gas of mensuration simultaneously as claimed in claim 1, it is characterised in that: wherein extracting solution is any one in ethyl acetate, dichloromethane, hexamethylene, cyclohexane/ethyl acetate; Extraction pattern is ultrasonic or vibration, and extraction time is 10-60min, and the volume of extracting solution is 10-50mL.
3. the method for the peculiar N-nitrosamine of Nicotiana tabacum L. and polycyclic aromatic hydrocarbon in the cigarette mainstream flue gas of mensuration simultaneously as claimed in claim 1, it is characterized in that: the NNN in described standard serial solution, NAT, the Concentraton gradient of NAB and BaP is 0.5, 1.0, 2.0, 5.0, 10.0, 20 and 50.0ng/mL, the Concentraton gradient of the NNK in described standard serial solution is 0.545, 1.09, 2.18, 5.45, 10.9, 21.8 and 54.5ng/mL, the Concentraton gradient of the BaA in described standard serial solution is 1.095, 2.19, 4.38, 10.95, 21.9, 43.8 and 109.5ng/mL, the Concentraton gradient of the Chry in described standard serial solution is 1.33, 2.66, 5.32, 13.3, 26.6, 53.2 and 133ng/mL, and NAT-d4 in standard serial solution, in NAB-d4 and NNK-d4, mark concentration is 10ng/mL, the interior mark concentration of NNN-d4 and BaP-d12 respectively 12 and 10.6ng/mL.
4. the method for the peculiar N-nitrosamine of Nicotiana tabacum L. and polycyclic aromatic hydrocarbon in the cigarette mainstream flue gas of mensuration simultaneously as claimed in claim 1, it is characterized in that: step 4) method particularly includes: in standard serial solution, the peak area of Nicotiana tabacum L. peculiar N-nitrosamine and polycyclic aromatic hydrocarbon and the ratio of interior mark peak area are vertical coordinate, the concentration of standard serial solution is abscissa, drawing curve; The ratio of Nicotiana tabacum L. peculiar N-nitrosamine and polycyclic aromatic hydrocarbon peak area and interior mark peak area in solution per sample, according to working curve, obtains the content of the peculiar N-nitrosamine of Nicotiana tabacum L. in sample and polycyclic aromatic hydrocarbon.
5. the method for the peculiar N-nitrosamine of Nicotiana tabacum L. and polycyclic aromatic hydrocarbon in the cigarette mainstream flue gas of mensuration simultaneously as claimed in claim 2, it is characterised in that: the ratio of cyclohexane/ethyl acetate used in extracting solution is v/v=5/5.
6. the method for the peculiar N-nitrosamine of Nicotiana tabacum L. and polycyclic aromatic hydrocarbon in the cigarette mainstream flue gas of mensuration simultaneously as claimed in claim 2, it is characterised in that: described extraction time is preferably 20min; The volume of extracting solution is preferably 20mL.
7. the method for the peculiar N-nitrosamine of Nicotiana tabacum L. and polycyclic aromatic hydrocarbon in the cigarette mainstream flue gas of mensuration simultaneously as claimed in claim 1, it is characterised in that: mobile phase used in step 3) is preferably cyclohexane/ethyl acetate, v/v=5/5.
8. as claimed in claim 1 or 2 measure the method for the peculiar N-nitrosamine of Nicotiana tabacum L. and polycyclic aromatic hydrocarbon in cigarette mainstream flue gas simultaneously, it is characterised in that: step 2) in extracting solution be preferably ethyl acetate.
9. the method for the peculiar N-nitrosamine of Nicotiana tabacum L. and polycyclic aromatic hydrocarbon in the cigarette mainstream flue gas of mensuration simultaneously as claimed in claim 1, it is characterised in that: the chromatographic column of chromatograph of gel permeation is preferably ShodexCLNpakEV-200,16 μm, 2mm*150mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610051476.7A CN105675757B (en) | 2016-01-26 | 2016-01-26 | It is a kind of at the same determine cigarette mainstream flue gas in the peculiar N nitrosamine of tobacco and polycyclic aromatic hydrocarbon method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610051476.7A CN105675757B (en) | 2016-01-26 | 2016-01-26 | It is a kind of at the same determine cigarette mainstream flue gas in the peculiar N nitrosamine of tobacco and polycyclic aromatic hydrocarbon method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105675757A true CN105675757A (en) | 2016-06-15 |
| CN105675757B CN105675757B (en) | 2017-10-31 |
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Cited By (9)
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| 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 |
| CN108387654A (en) * | 2018-02-09 | 2018-08-10 | 深圳瀚星翔科技有限公司 | The detection method of NNN and NNK in a kind of atomization vapour of electronic cigarette release |
| CN108627600A (en) * | 2017-03-20 | 2018-10-09 | 上海烟草集团有限责任公司 | The analysis method of flavor component in a kind of flue gas |
| CN108956802A (en) * | 2018-05-24 | 2018-12-07 | 中国烟草总公司郑州烟草研究院 | The detection method of Multiple components in the processing method of a kind of tobacco and tobacco product, tobacco and tobacco product |
| CN110261517A (en) * | 2019-08-06 | 2019-09-20 | 南通市产品质量监督检验所 | Utilize the method for N- nitrosamine compound in GPC-GC/MS/MS measurement meat products |
| CN110274977A (en) * | 2019-08-06 | 2019-09-24 | 南通市产品质量监督检验所 | The detection method of N- nitrosamine compound in a kind of food |
| CN112730663A (en) * | 2020-12-22 | 2021-04-30 | 华测检测认证集团湖北有限责任公司 | Method for rapidly and accurately measuring volatile nitrosamine in food |
| CN113711007A (en) * | 2019-04-24 | 2021-11-26 | 株式会社岛津制作所 | Method for determining generation source of fine particles in atmosphere |
| CN116660425A (en) * | 2023-07-18 | 2023-08-29 | 山东杰诺检测服务有限公司 | Method for rapidly determining various pesticide residues in fruits and vegetables and application thereof |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106248835B (en) * | 2016-09-28 | 2019-05-31 | 云南省烟草质量监督检测站 | The method for detecting 22 kinds of multiring aromatic hydrocarbon substance contents in cigarette smoke simultaneously |
| 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 |
| CN108627600A (en) * | 2017-03-20 | 2018-10-09 | 上海烟草集团有限责任公司 | The analysis method of flavor component in a kind of flue gas |
| CN108387654A (en) * | 2018-02-09 | 2018-08-10 | 深圳瀚星翔科技有限公司 | The detection method of NNN and NNK in a kind of atomization vapour of electronic cigarette release |
| CN108956802B (en) * | 2018-05-24 | 2021-06-18 | 中国烟草总公司郑州烟草研究院 | Processing method of tobacco and tobacco products and detection method of various components in tobacco and tobacco products |
| CN108956802A (en) * | 2018-05-24 | 2018-12-07 | 中国烟草总公司郑州烟草研究院 | The detection method of Multiple components in the processing method of a kind of tobacco and tobacco product, tobacco and tobacco product |
| CN113711007A (en) * | 2019-04-24 | 2021-11-26 | 株式会社岛津制作所 | Method for determining generation source of fine particles in atmosphere |
| CN110274977A (en) * | 2019-08-06 | 2019-09-24 | 南通市产品质量监督检验所 | The detection method of N- nitrosamine compound in a kind of food |
| CN110261517B (en) * | 2019-08-06 | 2021-10-29 | 南通市产品质量监督检验所 | Method for determining N-nitrosamine compounds in meat products by using GPC-GC/MS/MS |
| CN110261517A (en) * | 2019-08-06 | 2019-09-20 | 南通市产品质量监督检验所 | Utilize the method for N- nitrosamine compound in GPC-GC/MS/MS measurement meat products |
| CN112730663A (en) * | 2020-12-22 | 2021-04-30 | 华测检测认证集团湖北有限责任公司 | Method for rapidly and accurately measuring volatile nitrosamine in food |
| CN116660425A (en) * | 2023-07-18 | 2023-08-29 | 山东杰诺检测服务有限公司 | Method for rapidly determining various pesticide residues in fruits and vegetables and application thereof |
| CN116660425B (en) * | 2023-07-18 | 2023-12-05 | 山东杰诺检测服务有限公司 | Method for rapidly determining various pesticide residues in fruits and vegetables and application thereof |
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