CN105158392B - The assay method of tobacco peculiar N-nitrosamine in a kind of tobacco juice for electronic smoke - Google Patents
The assay method of tobacco peculiar N-nitrosamine in a kind of tobacco juice for electronic smoke Download PDFInfo
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Abstract
The invention discloses the assay method of tobacco peculiar N nitrosamine in a kind of tobacco juice for electronic smoke, it is characterized in that: extract with dichloromethane after tobacco juice for electronic smoke sample is diluted with the phosphate buffer containing ascorbic acid, extract is measured with online gel permeation chromatography gas-chromatography tandem mass spectrometer after concentrating, and uses inner mark method ration.The present invention is the assay method of tobacco peculiar N content of nitrosamines in brand-new tobacco juice for electronic smoke, has highly sensitive, the removal advantage that matrix is effective and antijamming capability is strong.
Description
Technical field
The invention belongs to the physical and chemical inspection technical field of electronic cigarette, specifically one uses liquid-liquid extraction-gel infiltration
Chromatogram-gas chromatography tandem mass spectrometry measures the method for tobacco peculiar N-content of nitrosamines in tobacco juice for electronic smoke.
Background technology
N-nitrosonornicotine (NNN), N-nitrosoanatabine (NAT), N-nitroso anabasine (NAB) and 4-
(nitrosomethylamino)-1-β-pyridine radicals-1-butanone (NNK) is the carcinogenic substance generally existed in cigarette smoke, due to these N-
Nitrosamine exists only in cigarette smoke or other tobacco products, so being referred to as tobacco peculiar N-nitrosamine.As far back as 1962,
The most just have in article report tobacco containing N-nitrosamine and potential carcinogenicity thereof.At present, tobacco peculiar N-nitrosamine quilt
International cancer research association is classified as carcinogenic and can be with carcinogenic substance blacklist.Therefore, the content pair of tobacco peculiar N-nitrosamine is measured
Correct evaluation bitting midges is significant.But, tobacco peculiar N-nitrosamine is in flue gas and other tobacco system
Content the lowest (usually ng rank) and other Coexisting component in product are complicated, therefore to carry out by N-nitrosamine peculiar to tobacco
Accurate quantitative analysis, it usually needs certain sample pretreatment process, with reach removal coexist matrix interference and enrichment tobacco special
There is the purpose of N-nitrosamine.
Electronic cigarette (electrical cigarette, e-cigarette) is the electronics product that a kind of profile imitates cigarette
Product, its sensation allowing user produce a kind of similar smoking when sucking by being atomized nicotine-containing tobacco juice.In recent years, along with
Management and control measure to traditional cigarette both at home and abroad is constantly strengthened, and electronic cigarette achieves pure development, and production and marketing at home and abroad
Amount is all significantly increased.But, up to now, the most all do not have systematic electronic cigarette safety evaluation data, and its security
Not yet obtain sufficient scientific appraisal.Therefore, the composition in Accurate Determining tobacco juice for electronic smoke is particularly important.Have at present
Containing tobacco peculiar N-nitrosamine in data display tobacco juice for electronic smoke, but when measuring its content, also can run into that content is low and matrix
Complicated problem.
Early stage has document report that after 100 mM ammonium acetate solution dilutions, tobacco juice for electronic smoke is introduced directly into liquid chromatogram-string
Connection mass spectrum is measured;N-nitrosamine peculiar for the tobacco in cigarette mainstream flue gas, current assay method is to use glass
TPM in fiber filter disc trapping cigarette mainstream flue gas, uses ammonium acetate solution ultrasonic extraction, and extract is through miillpore filter mistake
After filter, internal standard method is used to use high performance liquid chromatography-tandem mass combined instrument to carry out quantitative analysis.Although above assay method is simple
Single, but all have much room for improvement, so N-nitrosamine peculiar to some tobacco contains in terms of detection sensitivity and removal matrix interference
Measure low sample can not realize accurately detecting.Therefore, exploitation one is highly sensitive, matrix removal effect is good, antijamming capability
The assay method of tobacco peculiar N-nitrosamine in strong tobacco juice for electronic smoke, the security etc. to correct assessment electronic cigarette has important
Meaning.
Summary of the invention
The purpose of the present invention is primarily to overcome the defect of existing detection technique, and foundation one is sensitive and accurate, matrix is gone
Except the assay method of tobacco peculiar N-nitrosamine in tobacco juice for electronic smoke effective, that antijamming capability is strong, the method can be to electricity
The tobacco peculiar N-nitrosamine that in sub-cigarette tobacco juice, content is extremely low realizes accurate quantitative analysis, and it is good, anti-interference to have matrix removal effect
The advantage that ability is strong.
It is an object of the invention to be achieved through the following technical solutions:
Four assay method growing tobacco peculiar N-nitrosamine (NNN, NAT, NAB and NNK) in a kind of tobacco juice for electronic smoke, specifically
Comprise the following steps that:
A, the preparation of standard working solution: owing to tobacco peculiar N-nitrosamine is in the mixed solution of ethyl acetate and acetone
Dissolubility is preferable, and one of the flowing phase that ethyl acetate is this method, therefore present patent application with ethyl acetate/acetone (1/1,
V/v) it is that standard working solution prepared by solvent.First with ethyl acetate/acetone (1/1, v/v) for solvent, grow tobacco with four peculiar
Isotope (NNN-d4, NAT-d4, NAB-d4 and NNK-d4) standard items of N-nitrosamine are solute, and compound concentration is 1 μ g/mL
Mixing internal standard standard liquid；Again with ethyl acetate/acetone (1/1, v/v) for solvent, grow tobacco peculiar N-nitrosamine with four
(NNN, NAT, NAB and NNK) standard items are solute, the serial mixed standard solution of the variable concentrations of preparation containing the internal standard, Qi Zhongsuo
State the concentration gradient of NNN, NAT and NAB in hybrid standard working solution be 0.200,0.500,1.00,2.00,5.00,
10.0、20.0、50.0 ng/mL；In hybrid standard working solution the concentration gradient of NNK be 0.218,0.545,1.09,2.18,
5.45,10.9,21.8,54.5 ng/mL, wherein interior target concentration is fixed as 10.0 ng/mL；
B, sample pre-treatments: weigh 0.25 g tobacco juice for electronic smoke sample and fill in centrifuge tube in 15-mL tool, add in 100 μ L
Vortex oscillation 3 min after diluting with 2 mL phosphate buffers (20 mM, pH 9, containing 0.05 g/mL ascorbic acid) after mark, then
It is extracted twice with 2 mL dichloromethane and merges organic phase, finally dichloromethane nitrogen at 35 DEG C being blown and be concentrated into 200 μ L, i.e.
For sample liquid to be measured.20 mM phosphate-buffered salts are conventional buffer salt system, owing to tobacco peculiar N-nitrosamine contains pyridine
Ring, can exist with ionic condition in the case of pH value is not more than 7, exist with neutral molecule state when pH value is 9, be conducive to
Follow-up liquid-liquid extraction.Meanwhile, buffer solution adds ascorbic acid, it is possible to be effectively prevented from cigarette during sample pretreatment
The peculiar N-nitrosamine of grass is oxidized；
The pH value of described phosphate buffer is 3.0-12.0, and preferred value is 9.0；Organic solvent is ethyl acetate, dichloro
Methane, n-hexane or methyl tertiary butyl ether(MTBE), preferably dichloromethane.Extracting twice with organic solvent, each extraction volume is 2
mL。
C, Instrument measuring: series standard working solution and the sample solution of containing the internal standard are coagulated the most online
Glue penetration chromatogram-gas chromatography tandem mass spectrometry measures, and wherein gel permeation chromatography condition is: chromatographic column is Shodex CLNpak
EV-200；Flowing is the mixed solution (v/v, 1/1) of hexamethylene and ethyl acetate mutually；Flow velocity is 0.1 mL/min；Column temperature is 40
℃；Sample size is 10 μ L；Collect the component that gel permeation chromatography retention time is 3.0-5.0 min, and it is all existed
Line carries out gas chromatography tandem mass spectrometry analysis；Gas chromatography tandem mass spectrometry condition is: inertia pre-column is 5 m × 0.53
The void column of mm；Pre-column is DB-35 ms, 5 mm × 0.25, m × 0.25 μm；Splitter is DB-35 ms, 25 m ×
0.25 mm × 0.25 μm；
In gas chromatography tandem mass spectrometry is analyzed, chromatographic column heating schedule is: initial temperature 82 DEG C, keeps 5.0 min,
Rising to 300 DEG C with 8 DEG C/min again and keep 7.75 min, the operation time is 40 min；Use Splitless injecting samples mode, sample introduction
Time is 7.0 min；With high-purity He as carrier gas, nebulizer gas pressure program is: by 120 kPa, rises to 100 kPa/min
180 kPa also keep 4.4 min, then recover to reset pressure with 49.8 kPa/min, and keep 33.8 min；Temperature programming is entered
Sample mouth heating schedule is: 120 DEG C keep 5 min, then rise to 250 DEG C with 100 DEG C/min and keep 33.7 min；Interface temperature
It is respectively 300 and 200 DEG C with ion source temperature；Mass spectrum ionization source is EI source；Ionization voltage is 70 ev；The solvent delay time
It is 15 min；Multiple-reaction monitoring pattern, collision gas is Ar, and pressure is 200 kPa, target analytes and interior target multiple-reaction monitoring
Parameter is as shown in table 1.
D, result calculate: used internal standard method to carry out quantitatively, specifically by the ratio of target analytes peak area and internal standard peak area
Method be in series standard working solution the ratio of target analytes peak area and internal standard peak area as ordinate, target analytes
Concentration be abscissa, drawing curve.Result calculates specific as follows: the equation of linear regression of NNN, NAT, NAB and NNK divides
Not Wei Y=0.1054X 0.02517, Y=0.09939X 0.008738, Y=0.1702X+0.02063 and Y=
0.1998X-0.1016, linearly dependent coefficient is followed successively by 0.9999,0.9999,0.9985 and 0.9992, and wherein Y represents target
Analyte peak area and the ratio of internal standard peak area, X represents the concentration of target analytes.When sample liquid is measured, will record
Analyte and the ratio of internal standard peak area substitute into corresponding equation of linear regression, can try to achieve containing of target analytes in sample
Amount.
The detection limit of the inventive method and be quantitatively limited to when target analytes signal to noise ratio (S/N) is 3 and 10 corresponding dense
Degree.The range of linearity of NNN, NAT, NAB and NNK, working curve, detection limit and quantitative limit etc. are shown in Table 2.
The present invention is directed to the defect of prior art, tobacco peculiar N-nitrosamine in a kind of tobacco juice for electronic smoke of specialized designs
Assay method: with the phosphate buffer containing ascorbic acid, tobacco juice for electronic smoke is diluted, then carry out liquid-liquid extraction with dichloromethane,
Online gel permeation chromatography-gas chromatography tandem mass spectrometry analysis is carried out after organic phase being concentrated under a nitrogen.With prior art phase
Ratio, having the beneficial effects that of assay method of the present invention:
1) overcome existing determination techniques mesostroma and remove halfway deficiency, for feature and the target of tobacco juice for electronic smoke
The character of analyte, improves method of testing.Particularly as follows: use phosphate buffer that tobacco juice for electronic smoke is diluted, then adopt
Carry out removal of impurities and enrichment with liquid-liquid extraction method, after the most again organic phase being concentrated with online gel permeation chromatography-gas-chromatography-
Tandem mass spectrum detects.Matrix interference can be effectively removed, it is possible to increase method by the sample pretreatment process of liquid-liquid extraction
Antijamming capability；
2) organic phase is carried out nitrogen and blow concentration, target analytes concentration in sample solution can be improved, can raising side
The sensitivity of method, reduces the detection limit of method；
3) with online gel permeation chromatography-gas chromatography tandem mass spectrometry technology as detection means, last sample liquid to be measured
Further interfering material can be separated with target analytes under the centrifugation of gel permeation chromatographic column, only target be divided
Analysis thing proceeds to gas chromatography tandem mass spectrometry online to carry out separating analysis, compensate for liquid-liquid extraction the most to a certain extent and selects
Property difference problem, antijamming capability can be improved；This technology compares the gas-chromatography of routine simultaneously, has higher sample size
(sample size of conventional gas phase chromatogram is 1 μ L, and the sample size of online gel permeation chromatography-gas chromatography tandem mass spectrometry is 10-
20 μ L).Therefore, the method that present patent application is set up has the advantage that antijamming capability is strong, highly sensitive.
Accompanying drawing explanation
Fig. 1 tetra-grows tobacco the typical color spectrogram of peculiar N-nitrosamine standard liquid.
Fig. 2 is the four typical color spectrogram growing tobacco peculiar N-nitrosamine in certain actual sample.
Detailed description of the invention
The present invention is described further below in conjunction with example, but is not to limit the present invention.
Example 1:
The assay method of tobacco peculiar N-nitrosamine in a kind of tobacco juice for electronic smoke:
1, the preparation of standard working solution: first with ethyl acetate/acetone (1/1, v/v) for solvent, grows tobacco spy with four
Isotope (NNN-d4, NAT-d4, NAB-d4 and NNK-d4) standard items having N-nitrosamine are solute, and compound concentration is 1 μ g/
The mixing internal standard standard liquid of mL；Again with ethyl acetate/acetone (1/1, v/v) for solvent, grow tobacco peculiar N-nitrosamine with four
(NNN, NAT, NAB and NNK) standard items are solute, the serial mixed standard solution of the variable concentrations of preparation containing the internal standard, Qi Zhongsuo
State the concentration gradient of NNN, NAT and NAB in hybrid standard working solution be 0.200,0.500,1.00,2.00,5.00,
10.0、20.0、50.0 ng/mL；In hybrid standard working solution the concentration gradient of NNK be 0.218,0.545,1.09,2.18,
5.45,10.9,21.8,54.5 ng/mL, wherein interior target concentration is fixed as 10.0 ng/mL；
2, sample pre-treatments: weigh 0.25 g tobacco juice for electronic smoke sample and fill in centrifuge tube in 15-mL tool, add in 100 μ L
Vortex oscillation 3 min after diluting with 2 mL phosphate buffers (20 mM, pH 9, containing 0.05 g/mL ascorbic acid) after mark, then
It is extracted twice with 2 mL dichloromethane and merges organic phase, finally dichloromethane nitrogen at 35 DEG C being blown and be concentrated into 200 μ L, i.e.
For sample liquid to be measured；
3, Instrument measuring: series standard working solution and the sample solution of containing the internal standard are coagulated the most online
Glue penetration chromatogram-gas chromatography tandem mass spectrometry measures, and wherein gel permeation chromatography condition is: chromatographic column is Shodex CLNpak
EV-200；Flowing is the mixed solution (v/v, 1/1) of hexamethylene and ethyl acetate mutually；Flow velocity is 0.1 mL/min；Column temperature is 40
℃；Sample size is 10 μ L；Collect the component that gel permeation chromatography retention time is 3.0-5.0 min, and it is all existed
Line carries out gas chromatography tandem mass spectrometry analysis；Gas chromatography tandem mass spectrometry condition is: inertia pre-column is 5 m × 0.53
The void column of mm；Pre-column is DB-35 ms, 5 mm × 0.25, m × 0.25 μm；Splitter is DB-35 ms, 25 m ×
0.25 mm × 0.25 μm；Chromatographic column heating schedule is: initial temperature 82 DEG C, keeps 5.0 min, then rises to 8 DEG C/min
300 DEG C and keep 7.75 min, the operation time is 40 min；Using Splitless injecting samples mode, sample injection time is 7.0 min；With
High-purity He is carrier gas, and nebulizer gas pressure program is: by 120 kPa, rises to 180 kPa with 100 kPa/min and keeps 4.4
Min, then recover to reset pressure with 49.8 kPa/min, and keep 33.8 min；Programmed temperature sampling mouth heating schedule is:
120 DEG C keep 5 min, then rise to 250 DEG C with 100 DEG C/min and keep 33.7 min；Interface temperature and ion source temperature divide
It is not 300 and 200 DEG C；Mass spectrum ionization source is EI source；Ionization voltage is 70 ev；The solvent delay time is 15 min；Many reactions
Monitoring pattern, collision gas is Ar, and pressure is 200 kPa, and target analytes and interior target multiple-reaction monitoring parameter are as shown in table 1.
Under this condition, the chromatogram of the four kinds of objects obtained is as shown in Figure 1.
4, result calculates: used internal standard method to carry out quantitatively, specifically by the ratio of target analytes peak area and internal standard peak area
Method be in series standard working solution the ratio of target analytes peak area and internal standard peak area as ordinate, target analytes
Concentration be abscissa, drawing curve.The detection of the inventive method limits and is quantitatively limited to target analytes signal to noise ratio (S/N)
Concentration corresponding when being 3 and 10.The range of linearity of NNN, NAT, NAB and NNK, working curve, detection limit and quantitative limit etc. are shown in
Table 2.When sample liquid is measured, substitute into corresponding equation of linear regression by recording analyte with the ratio of internal standard peak area,
Try to achieve the content of target analytes in sample, as shown in table 3, the content of four kinds of target analytes after conversion all respective
In the range of linearity.In order to investigate the rate of recovery of method, add in this actual sample low (NNN, NAT and NAB are 1.0 ng/mL,
NNK is 1.09 ng/mL), in (NNN, NAT and NAB are 5.0 ng/mL, and NNK is 5.45 ng/mL), high (NNN, NAT and NAB
Being 20.0 ng/mL, NNK is 21.8 ng/mL) standard specimen of three kinds of concentration, then it is measured.Rate of recovery result is as shown in table 4,
Under variable concentrations, the rate of recovery of target analytes is between 89.3-109.0%, and RSD is not more than 7.9%.
Example 2:
Assay method as described in example 1, chooses other 21 kinds of commercially available tobacco juice for electronic smoke, measures the peculiar N-of wherein tobacco sub-
The content of nitramine, result is as shown in table 5.
Claims (9)
1. the assay method of tobacco peculiar N-nitrosamine in a tobacco juice for electronic smoke, it is characterised in that comprise the steps:
1) preparation of standard working solution: first with ethyl acetate/acetone as solvent, grows tobacco the same of peculiar N-nitrosamine with four
Position element NNN-d4, NAT-d4, NAB-d4 and NNK-d4 standard items are solute, and compound concentration is the mixing internal standard standard of 1 μ g/mL
Solution；Again with ethyl acetate/acetone as solvent, it is molten with four peculiar N-nitrosamine NNN, NAT, NAB and NNK standard items that grow tobacco
Matter, the serial mixed standard solution of the variable concentrations of preparation containing the internal standard；
2) sample pre-treatments: weigh 0.25 g tobacco juice for electronic smoke sample and fill in centrifuge tube in 15-mL tool, use concentration after adding internal standard
It is 20 mM, vortex oscillation 3 min after the 2 mL phosphate buffer dilutions containing 0.05 g/mL ascorbic acid, then with organic molten
Agent extracts and merges organic phase, is finally blown by organic phase nitrogen at 35 DEG C and is concentrated into 200 μ L, is sample liquid to be measured；
3) Instrument measuring: series standard working solution and the sample solution of containing the internal standard are carried out gel infiltration look under the same conditions
Spectrum-gas chromatography tandem mass spectrometry measures, and gel permeation chromatography condition is: chromatographic column is Shodex CLNpak EV-200；Flowing
It is hexamethylene and the mixed solution of ethyl acetate v/v=1/1 mutually；Flow velocity is 0.1 mL/min；Column temperature is 40 DEG C；Sample size is 10
μL；Collecting gel permeation chromatography retention time is the component of 3.0-5.0 min, and its all on-line is carried out gas-chromatography-
Tandem Mass Spectrometry Analysis；Gas chromatography tandem mass spectrometry condition is: inertia pre-column is the void column of 5 m × 0.53 mm；Pre-column is
DB-35 ms, 5 mm × 0.25, m × 0.25 μm；Splitter is DB-35 ms, 25 mm × 0.25, m × 0.25 μ
m；
4) result calculates: used internal standard method to carry out quantitatively by the ratio of target analytes peak area and internal standard peak area, concrete grammar
Be in series standard working solution the ratio of target analytes peak area and internal standard peak area as ordinate, target analytes dense
Degree is abscissa, drawing curve；According to target analytes peak area in sample liquid and the ratio of internal standard peak area, substitute into work
Curve, obtains the content of target analytes in sample.
2. the assay method of tobacco peculiar N-nitrosamine in tobacco juice for electronic smoke as described in claim 1, it is characterised in that: step
2) pH value of described phosphate buffer is 3.0-12.0.
3. the assay method of tobacco peculiar N-nitrosamine in tobacco juice for electronic smoke as described in claim 2, it is characterised in that: phosphoric acid
The pH value of salt buffer is 9.0.
4. the assay method of tobacco peculiar N-nitrosamine in tobacco juice for electronic smoke as described in claim 1, it is characterised in that: step
2) organic solvent described in is ethyl acetate, dichloromethane, n-hexane or methyl tertiary butyl ether(MTBE).
5. the assay method of tobacco peculiar N-nitrosamine in tobacco juice for electronic smoke as described in claim 4, it is characterised in that: organic
Solvent is dichloromethane.
6. the assay method of tobacco peculiar N-nitrosamine in tobacco juice for electronic smoke as described in claim 1, it is characterised in that: step
2) in, extracting twice with organic solvent, each extraction volume is 2 mL.
7. the assay method of tobacco peculiar N-nitrosamine in tobacco juice for electronic smoke as described in claim 1, it is characterised in that in step
Rapid 3), during in, gas chromatography tandem mass spectrometry is analyzed, chromatographic column heating schedule is: initial temperature 82 DEG C, keeps 5.0 min, then with 8
DEG C/min rises to 300 DEG C and keeps 7.75 min, the operation time is 40 min；Using Splitless injecting samples mode, sample injection time is
7.0 min；With high-purity He as carrier gas, nebulizer gas pressure program is: by 120 kPa, rises to 180 kPa with 100 kPa/min
And keep 4.4 min, then recover to reset pressure with 49.8 kPa/min, and keep 33.8 min；Programmed temperature sampling mouth rises
Temperature program is: 120 DEG C keep 5 min, then rise to 250 DEG C with 100 DEG C/min and keep 33.7 min；Interface temperature and ion
Source temperature is respectively 300 and 200 DEG C；Mass spectrum ionization source is EI source；Ionization voltage is 70 ev；The solvent delay time is 15
min；Multiple-reaction monitoring pattern, collision gas is Ar, and pressure is 200 kPa, and the quota ion of NNN, NAT, NAB and NNK is to successively
For: 177.0 > 147.0,159.0 > 157.0,161.0 > 133.0 and 177.0 > 146.0, corresponding collision voltage depends on
Secondary it is: 5.0,10.0,15.0 and 5.0 ev；The qualitative ion pair of NNN, NAT, NAB and NNK is followed successively by: 177.0 > 105.0,
20.0,25.0 159.0 > 105.0,161.0 > 106.0 and 177.0 > 118.0, corresponding collision voltage is followed successively by:,
25.0 and 15.0 ev；The quota ion of NNN-d4, NAT-d4, NAB-d4 and NNK-d4 is to being followed successively by: 181.0 > 151.0,
163.0 > 161.0,165.0 > 137.0 and 181.0 > 150.0, corresponding collision voltage is followed successively by: 5.0,10.0,15.0
With 5.0 ev.
8. the assay method of tobacco peculiar N-nitrosamine in tobacco juice for electronic smoke as described in claim 1, it is characterised in that step
4) in, result calculates specific as follows: the equation of linear regression of NNN, NAT, NAB and NNK is respectively Y=0.1054X
0.02517, Y=0.09939X 0.008738, Y=0.1702X+0.02063 and Y=0.1998X-0.1016,
Linearly dependent coefficient is followed successively by 0.9999,0.9999,0.9985 and 0.9992, and wherein Y represents target analytes peak area and interior
The ratio of mark peak area, X represents the concentration of target analytes, when being measured sample liquid, will record analyte and face, internal standard peak
Long-pending ratio substitutes into corresponding equation of linear regression, can try to achieve the content of target analytes in sample.
9. the assay method of tobacco peculiar N-nitrosamine in tobacco juice for electronic smoke as described in claim 1, it is characterised in that step
1) in hybrid standard working solution described in the concentration gradient of NNN, NAT and NAB be 0.200,0.500,1.00,2.00,
5.00、10.0、20.0、50.0 ng/mL；In hybrid standard working solution the concentration gradient of NNK be 0.218,0.545,1.09,
2.18,5.45,10.9,21.8,54.5 ng/mL, wherein interior target concentration is fixed as 10.0 ng/mL.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107064354A (en) * | 2017-04-13 | 2017-08-18 | 国家烟草质量监督检验中心 | The extraction of N nitrosamine and assay method in a kind of solanaceous vegetable that SPE is exchanged based on hydrophobic nonionic |
| CN107064356A (en) * | 2017-04-13 | 2017-08-18 | 国家烟草质量监督检验中心 | The extraction of the peculiar N nitrosamine of tobacco and assay method in a kind of electronic cigarette liquid that SPE is exchanged based on hydrophobic nonionic |
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| CN105675757B (en) * | 2016-01-26 | 2017-10-31 | 国家烟草质量监督检验中心 | 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 |
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| 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 |
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| CN107064354A (en) * | 2017-04-13 | 2017-08-18 | 国家烟草质量监督检验中心 | The extraction of N nitrosamine and assay method in a kind of solanaceous vegetable that SPE is exchanged based on hydrophobic nonionic |
| CN107064356A (en) * | 2017-04-13 | 2017-08-18 | 国家烟草质量监督检验中心 | The extraction of the peculiar N nitrosamine of tobacco and assay method in a kind of electronic cigarette liquid that SPE is exchanged based on hydrophobic nonionic |
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